WorldWideScience

Sample records for pyrazolines preparation structure

  1. Synthesis, quantitative structure-property relationship study of novel fluorescence active 2-pyrazolines and application

    Science.gov (United States)

    Girgis, Adel S.; Basta, Altaf H.; El-Saied, Houssni; Mohamed, Mohamed A.; Bedair, Ahmad H.; Salim, Ahmad S.

    2018-03-01

    A variety of fluorescence-active fluorinated pyrazolines 13-33 was synthesized in good yields through cyclocondensation reaction of propenones 1-9 with aryl hydrazines 10-12. Some of the synthesized compounds provided promising fluorescence properties with quantum yield (Φ) higher than that of quinine sulfate (standard reference). Quantitative structure-property relationship studies were undertaken supporting the exhibited fluorescence properties and estimating the parameters governing properties. Five synthesized fluorescence-active pyrazolines (13, 15, 18, 19 and 23) with variable Φ were selected for treating two types of paper sheets (Fabriano and Bible paper). These investigated fluorescence compounds, especially compounds 19 and 23, provide improvements in strength properties of paper sheets. Based on the observed performance they can be used as markers in security documents.

  2. Spectral studies of 2-pyrazoline derivatives: structural elucidation through single crystal XRD and DFT calculations.

    Science.gov (United States)

    Chinnaraja, D; Rajalakshmi, R; Srinivasan, T; Velmurugan, D; Jayabharathi, J

    2014-04-24

    A series of biologically active N-thiocarbamoyl pyrazoline derivatives have been synthesized using anhydrous potassium carbonate as the catalyst. All the synthesized compounds were characterized by FT-IR, (1)H NMR, (13)C NMR spectral studies, LCMS, CHN Analysis and X-ray diffraction analysis (compound 7). In order to supplement the XRD parameters, molecular modelling was carried out by Gaussian 03W. From the optimized structure, the energy, dipolemoment and HOMO-LUMO energies of all the systems were calculated. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Synthesis, Crystal Structural Characterization and Biological Properties of Thiosemicarbazones of Schiff Bases Derived from 4-Acyl-2-pyrazoline-5-one

    Directory of Open Access Journals (Sweden)

    Arjunsinh Rana

    2011-01-01

    Full Text Available A novel synthesis, single crystal and biological activity of 4-acylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one by condensation of 4-acyl-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one with thiosemicarbazide was carried out. The compounds were characterized on the basis of elemental analysis, IR, 1H NMR, Mass, DSC and 13C NMR spectral data. The compounds were tested for their antibacterial activity against various gram +ve and -ve bacteria. The results were compared with the marketed drugs. The crystal structure was determined by single x-ray diffraction. 4-Acetyl thiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one(AcPTMP-ths crystallizes in the monoclinic system, space group P21/n with a=6.0828(7Å, b=29.547(4Å, c=7.9101(15Å, α=90°, γ=95.602(15°, γ=90°, V=1414.9(4 Å3, Z=4, Dc=1.429 mg/m3 and 4-Propionylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one (PropPTMP-ths crystallizes in the monoclinic system, space group P21/c with a=13.5622(10Å, b=13.3671(12Å, c=22.151(2Å, α=90°, β=93.13(7°, γ=90°, V=4010.1(6 Å3, Z=8, Dc=1.310 mg/m3. The compounds were screened for antibacterial properties and exhibited potential activity.

  4. Synthesis, X-ray crystal structure and optical properties research of novel diphenyl sulfone-based bis-pyrazoline derivatives

    International Nuclear Information System (INIS)

    Gong Zhongliang; Zheng Liangwen; Zhao Baoxiang

    2012-01-01

    A series of novel bis-pyrazoline derivatives were synthesized by the reaction of chalcone and (sulfonylbis(3,1-phenylene))bis(hydrazine) in 20–34% yields. The structures of the compounds were determined by IR, 1 H NMR, HRMS spectra, and a representative compound 3b was confirmed based on the X-ray crystallographic analysis. Absorption and fluorescence spectra of these compounds in dichloromethane solution were investigated. The results showed that the emission maxima varied from 415 to 444 nm mainly depending on C3 substituents of pyrazoline moiety. The compounds had higher quantum yields, when C3 substituent was an electron-withdrawing p-chlorophenyl group. Moreover, absorption spectra and emission spectra exhibited a blue-shift and a red-shift with increasing the polarity of solvents, respectively. Fluorescent molecules happened to collide with each other and resulted in quench of the fluorescence when the concentration increased over to 10 −5 M. - Highlights: ► A series of novel diphenyl sulfone-based bis-pyrazoline derivatives were designed and synthesized. ► Their UV–vis absorption and fluorescence emission spectra were investigated. ► The relationship of substituents and the optical properties were discussed. ► With increasing the solvent polarity, fluorescence emission displayed a red-shift and fluorescence quantum yields decreased. ► Fluorescence was quenched when the concentration increased over to 10 −5 M.

  5. Synthesis, crystal structure, and spectra of 3,3- dimethyl-1-N-(1'-phenyl-2',3'-dimethyl-5'-oxo-3'- pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline

    International Nuclear Information System (INIS)

    Sokol, V.I.; Ryabov, M.A.; Merkur'eva, N.Yu.; Davydov, V.V.; Zaitsev, B.E.; Shklyaev, Yu.V.; Sergienko, V.S.; Zaitsev, B.E.

    1996-01-01

    The synthesis and the crystal and molecular structure of 3,3-dimethyl-1-N-(1'-phenyl-2',3'- dimethyl-5'-oxo-3'-pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline are reported. As is evidenced by the 1H NMR, IR, and electron spectra, the tautomeric form of the compounds observed in the crystal is also retained in solutions

  6. 1-Acetyl-5-ferrocenyl-3-phenyl-2-pyrazoline

    Directory of Open Access Journals (Sweden)

    Orhan Büyükgüngör

    2009-02-01

    Full Text Available In the title compound, [Fe(C5H5(C16H15N2O], the pyrazoline ring and the phenyl ring are nearly coplanar, making a dihedral angle of 6.54 (2°, while the substituted cyclopentadienyl ring is twisted out of the pyrazoline ring plane by 81.32 (1°. The molecules in the crystal structure are held together by weak C—H...O intermolecular hydrogen bonds and two C—H...π interactions.

  7. 1-Acetyl-3-ferrocenyl-5-(2-nitrophenyl-2-pyrazoline

    Directory of Open Access Journals (Sweden)

    Orhan Büyükgüngör

    2008-04-01

    Full Text Available In the title compound, [Fe(C5H5(C16H14N3O3], the pyrazoline ring and the substituted cyclopentadienyl ring are nearly coplanar, with a dihedral angle of 8.17 (2°, while the nitro-substituted benzene ring is twisted out of the pyrazoline ring plane by 70.76 (1°. The molecules in the crystal structure are held together by three intermolecular C—H...O hydrogen bonds. There is also an intramolecular C—H...N hydrogen bond. The H atoms of the methyl group are disordered equally over two positions.

  8. 1-[3-(2-Nitrophenyl-5-phenyl-2-pyrazolin-1-yl]ethanone

    Directory of Open Access Journals (Sweden)

    Huan-Mei Guo

    2010-07-01

    Full Text Available The title compound, C17H15N3O3, was prepared from 1-(2-nitrophenyl-3-phenylprop-2-en-1-one and hydrazine. The dihedral angle between the benzene and phenyl rings is 74.55 (2°. The pyrazoline ring is in a slight envelope conformation with the C atom bonded to the phenyl ring forming the flap. In the crystal structure, weak intermolecular C—H...O hydrogen bonds connect molecules into chains along [100].

  9. Metal Complexes of New Bioactive Pyrazolone Phenylhydrazones; Crystal Structure of 4-Acetyl-3-methyl-1-phenyl-2-pyrazoline-5-one phenylhydrazone Ampp-Ph

    Directory of Open Access Journals (Sweden)

    Omoruyi G. Idemudia

    2016-05-01

    Full Text Available The condensation reaction of phenylhydrazine and dinitrophenylhydrazine with 4-acetyl and 4-benzoyl pyrazolone precipitated air-stable acetyldinitrophenylhydrazone Ampp-Dh, benzoylphenylhydrazone Bmpp-Ph and benzoyldinitrophenylhydrazone Bmpp-Dh in their keto imine form; a study inspired by the burning interest for the development of new bioactive materials with novel properties that may become alternative therapeutic agents. Elemental analysis, FTIR, 1H, and 13C NMR, and mass spectroscopy have been used to justify their proposed chemical structures, which were in agreement with the single crystal structure of Bmpp-Dh earlier reported according to X-ray crystallography. The single crystal structure of 4-acetyl-3-methyl-1-phenyl--pyrazoline-5-one phenylhydrazone Ampp-Ph, which crystallizes in a triclinic crystal system with a P-1 (No. 2 space group is presented. Octahedral Mn(II, Ni(II, Co(II, and Cu(II complexes of these respective ligands with two molecules each of the bidentate Schiff base, coordinating to the metal ion through the azomethine nitrogen C=N and the keto oxygen C=O, which were afforded by the reaction of aqueous solutions of the corresponding metal salts with the ligands are also reported. Their identity and proposed structures were according to elemental analysis, FTIR spectroscopy, UV-VIS spectrophotometry (electronic spectra and Bohr magnetic moments, as well as thermogravimetric analysis (TGA results. A look at the antibacterial and antioxidant activities of synthesized compounds using the methods of the disc diffusion against some selected bacterial isolates and 1,1-diphenyl-2-picryl-hydrazil (DPPH respectively, showed biological activities in relation to employed standard medicinal drugs.

  10. Synthesis, structure characterization, in vitro and in silico biological evaluation of a new series of thiazole nucleus integrated with pyrazoline scaffolds

    Science.gov (United States)

    Sadashiva, Rajitha; Naral, Damodara; Kudva, Jyothi; Madan Kumar, S.; Byrappa, K.; Mohammed Shafeeulla, R.; Kumsi, Manjunatha

    2017-10-01

    In the current study, a series of 2,4-disubstituted-1,3-thiazoles linked with pyrazoline scaffolds 3a-o were rationally designed and synthesized. The structures of the title compounds were elucidated by spectroscopic data (UV-Vis, IR, NMR and Mass spectra) and elemental analysis. Single crystal X-Ray diffraction studies revealed that, the compounds 3i and 3k crystallized in monoclinic crystal system with P21/n space group and Z = 4. The molecules 3i and 3k were connected with intermolecular hydrogen bonds N2-H2 … O1, N3sbnd H3 … Cl1 and short contacts (Csbnd H … π and Csbnd Cl … π). Intramolecular hydrogen bonds, N3sbnd H3 … N5 and C5sbnd H5 ….N1 were also existed. The compounds were evaluated for their anticancer activity against A549 and MCF-7 human cancer cell lines and in vitro antimicrobial activity against pathogenic microbial strains. The compounds bearing chloro atom at the para position of phenyl ring A like 3f, 3j and 3k with the IC50: 7.5, 5.0 and 5.0 μM respectively, exhibited better activity than standard drug Cisplatin (IC50: 10.0 μM). In addition, the compounds 3a, 3f, 3j and 3l have exhibited the similar antimicrobial activity as that of standard drug Ciprofloxacin and Fluconazole. Furthermore, to support the biological potency of the compounds, in silico molecular docking studies were carried out against the E. coli MurB (PDB code: pdb:2MBR)

  11. Synthesis of merocyanines analogues based on the pyrazolin-5-one system

    International Nuclear Information System (INIS)

    Park, Soo Youl; Oh, Sea Wha

    2003-01-01

    The majority of dyes belong to the chromophoric class known as donor-acceptor systems. The essential structural feature of such systems is the presence of one or more electron donating groups conjugated to one or more electron withdrawing groups via an unsaturated bridge. The pyrazolin-5-one system is an effective electron acceptor residue, and can also act as a weak electron donor. In our experiments, the various symmetrical and unsymmetrical H-chromophores were synthesized in the indoxyl, imidazo(1,2-a)pyridin-2-one, pyrazolin-5-one, and pyridin-2-6-dione residues, resulting in cross-conjugated donor-acceptor systems. And the visible light absorption was then associated with the migration of electron density from the donor region of the molecule to the acceptor region. Also, it was useful to prepare related non-cross-conjugated donor acceptor chromophores by combining these residues with other electron donor or acceptor moieties. For convenience such chromophores are referred to as merocyanines

  12. Synthesis and Spectroscopic Characterization of Some New Biological Active Azo–Pyrazoline Derivatives

    Directory of Open Access Journals (Sweden)

    Farouq E. Hawaiz

    2012-01-01

    Full Text Available A number of 3-[4-(benzyloxy-3-(2-Chlorophenylazo-phenyl]-5-(substituted-phenyl-1-substituted-2-pyrazolines( 4a-j and (5a-j have been synthesized by diazotization of 2-chloroaniline and its coupling reaction with 4-hydroxy acetophenone, followed by benzyloxation of the hydroxyl group to give the substrate [4-benzyloxy-3-(2-chlorophenylazo-acetophenone (1].The prepared starting material (1 has been reacted with different substituted benzaldehydes to give a new series of chalcone derivatives 1-[(4-benzyloxy-3-(2-chloro-phenylazo-phenyl]-3-(substituted phenyl-2-propen-1-one (3a-j, in high yields and in a few minutes, and the later compounds were treated with hydrazine hydrate according to Michael addition reaction to afford a new biolological active target compounds (4a-j and (5a-j. Furthermore, The structures of the newly synthesized compounds were confirmed by FT-IR, 13C-NMR,13C-DEPT & 1H-NMR spectral data. The chalcone and pyrazoline derivatives were evaluated for their anti bacterial activity against Escherichia coli as gram negative and Staphylococcus aureus as gram positive, the results showed significant activity against both types of bacteria.

  13. Synthesis and anticonvulsant activity of certain chalcone based pyrazoline compounds

    Directory of Open Access Journals (Sweden)

    Sudhakara Rao Gerapati

    2015-09-01

    Full Text Available Convulsions are involuntary, violent, spasmodic and prolonged contractions of skeletal muscles. That means a patient may have epilepsy without convulsions and vice versa. Epilepsy is a common neurological abnormality affecting about 1% of the world population. The primary objectives of these synthesized compounds are to suppress seizures and provide neuroprotection by minimizing the effects from seizure attacks. Here some of the chalcones and chalcone based various pyrazolines were evaluated for anticonvulsant activity. Their structures have been elucidated on the basis of elemental analyses and spectroscopic studies (IR, 1H-NMR & Mass spectroscopy. A preliminary evaluation of the prepared compounds has indicated that some of them exhibit moderate to significant anticonvulsant activity compared to a diazepam standard1-3.  All compounds were tested for their anticonvulsant activity using maximal electroshock induced convulsions (MES in mice at a dose level of 4 mg/kg.b.w. The compounds  Ph1, Ph2 , Py2 ,Py3 and Py4 have shown  to  good anticonvulsant activity when doses are administered as 25mg/ kg.b.w  , reduced the phases of seizures severity and  found to be active and also  increased survival rate. Remaining compounds are less efficacious.

  14. Microwave assisted synthesis of some new coumarin-pyrazoline hybrids and their antimicrobial activity

    OpenAIRE

    Ashok Dongamanti; Lakshmi Bommidi Vijaya; Ravi Sidda; Ganesh Arram

    2015-01-01

    A series of pyrazolines 4a-g have been synthesized by Michael addition of chalcones 3a-g with hydrazine hydrate in presence of sodium acetate under conventional heating and microwave irradiation. Structures of the newly synthesized chalcones 3a-g and pyrazolines 4a-g have been established on the basis of IR, 1H & 13C NMR and mass spectral data. All the synthesized compounds were screened for their antimicrobial activity. Some of the compounds shown very goo...

  15. Microwave assisted synthesis of some new coumarin-pyrazoline hybrids and their antimicrobial activity

    Directory of Open Access Journals (Sweden)

    Ashok Dongamanti

    2015-01-01

    Full Text Available A series of pyrazolines 4a-g have been synthesized by Michael addition of chalcones 3a-g with hydrazine hydrate in presence of sodium acetate under conventional heating and microwave irradiation. Structures of the newly synthesized chalcones 3a-g and pyrazolines 4a-g have been established on the basis of IR, 1H & 13C NMR and mass spectral data. All the synthesized compounds were screened for their antimicrobial activity. Some of the compounds shown very good activity compared to standard drugs against all pathogenic bacteria and fungi.

  16. Synthesis, characterization, antimicrobial and anticancer studies of new steroidal pyrazolines

    Directory of Open Access Journals (Sweden)

    Shamsuzzaman

    2016-01-01

    Full Text Available A convenient synthesis of 2′-(2″,4″-dinitrophenyl-5α-cholestano [5,7-c d] pyrazolines 4–6 from cholest-5-en-7-one 1–3 was performed and structural assignment of the products was confirmed on the basis of IR, 1H NMR, 13C NMR, MS and analytical data. The synthesized compounds were screened for in vitro antimicrobial activity against different strains during which compound 6 showed potent antimicrobial behaviour against Corynebacterium xerosis and Staphylococcus epidermidis. The synthesized compounds were also screened for in vitro anticancer activity against human cancer cell lines during which compound 5 exhibited significant anticancer activity.

  17. A new pyrazoline-based fluorescent sensor for Al3+ in aqueous solution.

    Science.gov (United States)

    Hu, Shengli; Song, Jingjing; Wu, Gongying; Cheng, Cuixia; Gao, Qing

    2015-02-05

    A new pyrazoline-based fluorescent sensor was synthesized and the structure was confirmed by single crystal X-ray diffraction. The sensor responds to Al(3+) with high selectivity among a series of cations in aqueous methanol. This sensor forms a 1:1 complex with Al(3+) and displays fluorescent quenching. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. An improved synthesis of 1,3,5-triaryl-2-pyrazolines in acetic acid aqueous solution under ultrasound irradiation

    Directory of Open Access Journals (Sweden)

    Lin Zhi-Ping

    2007-03-01

    Full Text Available Abstract Background Pyrazoline derivatives have been found to possess a broad spectrum of biological activities. Among various pyrazoline derivatives, 2-pyrazolines seem to be the most frequently studied. A variety of methods have been reported for the preparation of this class of compound. However, in spite of their potential utility, some of the reported methods suffer from drawbacks such as long reaction times, cumbersome product isolation procedures and environmental concerns. Organic reactions in aqueous media have attracted increasing interest recently because of environmental issues and the understanding of biochemical processes. Ultrasound has increasingly been used in organic synthesis in the last three decades. A large number of organic reactions can be carried out in higher yields, shorter reaction time or milder conditions under ultrasound irradiation. Results Preparation of a series of 1,3,5-triaryl-2-pyrazolines through the reaction of chalcones and phenylhydrazine hydrochloride was carried out in 83–96% yield within 1.5–2 h in sodium acetate-acetic acid aqueous solution under ultrasound irradiation. Conclusion We have described a practical and convenient procedure for the synthesis of 1,3,5-triaryl-2-pyrazolines in sodium acetate-acetic acid aqueous solution at room temperature under ultrasound irradiation.

  19. Antinociceptive effect of novel pyrazolines in mice

    Directory of Open Access Journals (Sweden)

    Tabarelli Z.

    2004-01-01

    Full Text Available The antinociceptive effect of six novel synthetic pyrazolines (3-ethoxymethyl-5-ethoxycarbonyl-1H-pyrazole (Pz 1 and its corresponding 1-substituted methyl (Pz 2 and phenyl (Pz 3 analogues, and 3-(1-ethoxyethyl-5-ethoxycarbonyl-1H-pyrazole (Pz 4 and its corresponding 1-substituted methyl (Pz 5 and phenyl (Pz 6 analogues was evaluated by the tail immersion test in adult male albino mice. The animals (N = 11-12 in each group received vehicle (5% Tween 80, 10 ml/kg, sc or 1.5 mmol/kg of each of the pyrazolines (Pz 1-Pz 6, sc. Fifteen, thirty and sixty minutes after drug administration, the mice were subjected to the tail immersion test. Thirty minutes after drug administration Pz 2 and Pz 3 increased tail withdrawal latency (vehicle = 3.4 ± 0.2; Pz 2 = 5.2 ± 0.4; Pz 3 = 5.9 ± 0.4 s; mean ± SEM, whereas the other pyrazolines did not present antinociceptive activity. Dose-effect curves (0.15 to 1.5 mmol/kg were constructed for the bioactive pyrazolines. Pz 2 (1.5 mmol/kg, sc impaired motor coordination in the rotarod and increased immobility in the open-field test. Pz 3 did not alter rotarod performance and spontaneous locomotion, but increased immobility in the open field at the dose of 1.5 mmol/kg. The involvement of opioid mechanisms in the pyrazoline-induced antinociception was investigated by pretreating the animals with naloxone (2.75 µmol/kg, sc. Naloxone prevented Pz 3- but not Pz 2-induced antinociception. Moreover, naloxone pretreatment did not alter Pz 3-induced immobility. We conclude that Pz 3-induced antinociception involves opioid mechanisms but this is not the case for Pz 2.

  20. Tautomerism of pyrazolinones in the solid state: the case of 1-aryl-3-methyl-3-pyrazolin-5-ones. An X-ray and CPMAS NMR study

    Energy Technology Data Exchange (ETDEWEB)

    Foces-Foces, C. [Departamento de Cristalografia. Instituto de Quimica Fisica. Rocasolano. Madrid (Spain); Fontenas, Ch.; Elguero, J. [Instituto de Quimica Medica. Madrid (Spain); Sobrados, I. [Instituto de Ciencia de Materiales. CSIC. Madrid (Spain)

    1997-10-01

    The tautomerism of pyrazolines in solution is one of the best-studied cases of tautomerism. Although there are many X-ray structures of these compounds, no systematic study of their tautomerism in the solid state has been carried out. In this paper we present the results obtained by X-ray crystallography and ``13 C CPMAS NMR on two related compounds, 1-phenyl-and 1-p-bromo phenyl-3-methyl pyrazoline, as well as the result of a search in the CSD. Some general conclusions about the tautomerism of pyrazolines have been drawn. (Author) 22 refs.

  1. Synthesis, Characterization and Chelating Properties of 4-Butyrylsemicarbazone-1-phenyl-3-methyl-2-pyrazolin-5-one

    Directory of Open Access Journals (Sweden)

    J. D. Patel

    2010-01-01

    Full Text Available 4-Butyrylsemicarbazone-1-phenyl-3-methyl-2-pyrazolin-5-one (BUMP-SC was prepared and its metal chelates of Cu2+, Ni2+, Co2+, Mn2+, Fe2+, Fe3+, Cr3+, UO2 and OV were prepared. The ligands and its chelates were characterized by elemental analysis, metal:ligand (M:L stoichiometry, IR-electronic spectral studies and magnetic properties. The compounds also were screened for their antimicrobial activity.

  2. REGIOSELECTIVE REACTIONS OF 3-ALKYL-1-PHENYL-2-PYRAZOLIN-5-ONES WITH ACYL HALIDES IN THE PRECENCE OF NONOSIZED MAGNESIUM HYDROXIDE AS A HIGHLY EFFECTIVE HETEROGENOUS BASE CATALYST Regioselektive Reaktionen von 3-Alkyl-1-PHENYL-2-pyrazolin-5-ONES Mit Acylhalogeniden IN DER PRECENCE DER NONOSIZED MAGNESIUM HYDROXIDE als hochwirksame heterogene BASE CATALYST

    OpenAIRE

    Hassan Sheibani and Bahman Massomi Nejad

    2012-01-01

    4-Acyl-3-alkyl-1-phenyl-2-pyrazolin-5-one derivatives were prepared by the regioselective acylation of 3-alkyl-1-phenyl-2-pyrazolin-5-ones in the presence of base catalysts such as calcium hydroxide [Ca(OH)2], magnesium hydroxide [Mg(OH)2] and nanosized magnesium hydroxide. In the presence of nanosized magnesium hydroxide, excellent yields of products were obtained and reaction times were significantly reduced.

  3. Solid-phase synthesis of 3-amino-2-pyrazolines

    DEFF Research Database (Denmark)

    Nielsen, John

    1998-01-01

    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to alpha,beta-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2...

  4. Synthesis and antioxidant activity study of pyrazoline carrying arylfuran/thiophene moiety

    Directory of Open Access Journals (Sweden)

    Jois Vidyashree H.S.

    2014-01-01

    Full Text Available A novel series of N-acetyl-3-aryl-5-(5-(p/o-nitrophenyl-2-arylfuryl/thienyl substituted pyrazoline (3a-o were synthesized by the reaction of 1-aryl-3-(5-(p/o-nitrophenyl-2-furyl/thienyl-2-propene-1-one with hydrazine hydrate in acetic acid medium. The structures of the newly synthesized compounds were established by IR, 1H NMR, mass spectra and single crystal X-ray study. The synthesized compounds were subjected to antioxidant activity using DPPH scavenging assay. The compounds 3a, 3f, 3h and 3o showed moderate activity.

  5. Design, synthesis, and in vivo SAR of a novel series of pyrazolines as potent selective androgen receptor modulators.

    Science.gov (United States)

    Zhang, Xuqing; Li, Xiaojie; Allan, George F; Sbriscia, Tifanie; Linton, Olivia; Lundeen, Scott G; Sui, Zhihua

    2007-08-09

    A novel series of pyrazolines 2 have been designed, synthesized, and evaluated by in vivo screening as tissue-selective androgen receptor modulators (SARMs). Structure-activity relationships (SAR) were investigated at the R1 to R6 positions as well as the core pyrazoline ring and the anilide linker. Overall, strong electron-withdrawing groups at the R1 and R2 positions and a small group at the R5 and R6 position are optimal for AR agonist activity. The (S)-isomer of 7c exhibits more potent AR agonist activity than the corresponding (R)-isomer. (S)-7c exhibited an overall partial androgenic effect but full anabolic effect via oral administration in castrated rats. It demonstrated a noticeable antiandrogenic effect on prostate in intact rats with endogenous testosterone. Thus, (S)-7c is a tissue-selective nonsteroidal androgen receptor modulator with agonist activity on muscle and mixed agonist and antagonist activity on prostate.

  6. Solution-phase parallel synthesis of a library of delta(2)-pyrazolines.

    Science.gov (United States)

    Manyem, Shankar; Sibi, Mukund P; Lushington, Gerald H; Neuenswander, Benjamin; Schoenen, Frank; Aubé, Jeffrey

    2007-01-01

    A parallel synthesis of a library (80 members) of 2-pyrazolines in solution phase is described. The 2-pyrazoline core was accessed through the [3 + 2] cycloaddition of nitrilimines with enoyl oxazolidinones. The cycloaddition provided two regioisomers, the major product being the C regioisomer. The oxazolidinone moiety was further reduced to the primary alcohol, producing another library of 5-hydroxymethyl-2-pyrazolines. The Lipinski profiles and calculated ADME properties of the compounds are also reported.

  7. Dioxomolybdenum(VI chelates of bioinorganic, catalytic, and medicinal relevance: Studies on some cis-dioxomolybdenum(VI complexes involving O, N-donor 4-oximino-2-pyrazoline-5-one derivatives

    Directory of Open Access Journals (Sweden)

    R.C. Maurya

    2015-05-01

    Full Text Available A new series of five mixed-ligand complexes of dioxomolybdenum(VI of the general composition [MoO2(L2(H2O2], where LH = 4-acetyloxime-3-methyl-1-phenyl-2-pyrazolin-5-one (aomppH, 3-methyl-1-phenyl-4-propionyloxime-2-pyrazolin-5-one (mppopH, 4-butyryloxime-3-methyl-1-phenyl-2-pyrazolin-5-one (buomppH, 4-iso-butyryloxime-3-methyl-1-phenyl-2-pyrazolin-5-one (ibuomppH or 4-benzoyloxime-3-methyl-1-phenyl-2-pyrazolin-5-one (bomppH has been synthesized by the interaction of [MoO2(acac2] with the said ligands in ethanol medium. The complexes so obtained were characterized by elemental analyses, molar conductance, decomposition temperature and magnetic measurements, thermogravimetric analyses, 1H NMR, IR, mass, and electronic spectral studies. The 3D molecular modeling and analysis for bond lengths and bond angles have also been carried out for one of the representative compound, [MoO2(aomppH2(H2O2] (1 to substantiate the proposed structure.

  8. Development of potential selective and reversible pyrazoline based MAO-B inhibitors as MAO-B PET tracer precursors and reference substances for the early detection of Alzheimer's disease.

    Science.gov (United States)

    Neudorfer, Catharina; Shanab, Karem; Jurik, Andreas; Schreiber, Veronika; Neudorfer, Carolina; Vraka, Chrysoula; Schirmer, Eva; Holzer, Wolfgang; Ecker, Gerhard; Mitterhauser, Markus; Wadsak, Wolfgang; Spreitzer, Helmut

    2014-09-15

    Since high MAO-B levels are present in early stages of AD, the MAO-B system can be designated as an appropriate and prospective tracer target of molecular imaging biomarkers for the detection of early AD. According to the preceding investigations of Mishra et al. the aim of this work was the development of a compound library of selective and reversible MAO-B inhibitors by performing bioisosteric modifications of the core structure of 3-(anthracen-9-yl)-5-phenyl-4,5-dihydro-1H-pyrazoles. In conclusion, 13 new pyrazoline based derivatives have been prepared, which will serve as precursor substances for future radiolabeling as well as reference compounds for the investigation of increased MAO-B levels in AD. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Redox-Enabled, pH-Disabled Pyrazoline-Ferrocene INHIBIT Logic Gates.

    Science.gov (United States)

    Scerri, Glenn J; Cini, Miriam; Schembri, Jonathan S; da Costa, Paola F; Johnson, Alex D; Magri, David C

    2017-07-05

    Pyrazoline-ferrocene conjugates with an "electron-donor-spacer-fluorophore-receptor" format are demonstrated as redox-fluorescent two-input INHIBIT logic gates. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Synthesis, Antibacterial and Antifungal Activity of Some New Pyrazoline and Pyrazole Derivatives

    Directory of Open Access Journals (Sweden)

    Seham Y. Hassan

    2013-02-01

    Full Text Available A series of 2-pyrazolines 5–9 have been synthesized from α,β-unsaturated ketones 2–4. New 2-pyrazoline derivatives 13–15 bearing benzenesulfonamide moieties were then synthesized by condensing the appropriate chalcones 2–4 with 4-hydrazinyl benzenesulfonamide hydrochloride. Ethyl [1,2,4] triazolo[3,4-c][1,2,4]triazino[5,6-b]-5H-indole-5-ethanoate (26 and 1-(5H-[1,2,4]triazino[5,6-b] indol-3-yl-3-methyl-1H-pyrazol-5(4H-one (32 were synthesized from 3-hydrazinyl-5H-[1,2,4]triazino[5,6-b]indole (24. On the other hand ethyl[1,2,4]triazolo[3,4-c][1,2,4]triazino[5,6-b]-5,10-dihydroquinoxaline- 5-ethanoate (27 and 1-(5,10-dihydro-[1,2,4]triazino[5,6-b]quinoxalin-3-yl-3-methyl-1H-pyrazol-5(4H-one (33 were synthesized from 3-hydrazinyl-5,10-dihydro-[1,2,4]triazino[5,6-b]quinoxaline (25 by reaction with diethyl malonate or ethyl acetoacetate, respectively. Condensation of 6,6-dimethyl-4-oxo-4,5,6,7-tetrahydro-1H-indole-2-carbaldehyde (1' with compound 24 or 25 afforded the corresponding Schiff's bases 36 and 37, respectively. Reaction of the Schiff's base 37 with benzoyl hydrazine or acetic anhydride afforded benzohydrazide derivative 39 and the cyclized compound 40, respectively. Furthermore, the pyrazole derivatives 42–44 were synthesized by cyclization of hydrazine derivative 25 with the prepared chalcones 2–4. All the newly synthesized compounds have been characterized on the basis of IR and 1H-NMR spectral data as well as physical data. Antimicrobial activity against the organisms E. coli ATCC8739 and P. aeruginosa ATCC 9027 as examples of Gram-negative bacteria, S. aureus ATCC 6583P as an example of Gram-positive bacteria and C. albicans ATCC 2091 as an example of a yeast-like fungus have been studied using the Nutrient Agar (NA and Sabouraud Dextrose Agar (SDA diffusion methods. The best performance was found for the compounds 16, 17, 19 and 20.

  11. Biological synthesis of ZnO nanoparticles using C. albicans and studying their catalytic performance in the synthesis of steroidal pyrazolines

    Directory of Open Access Journals (Sweden)

    Shamsuzzaman

    2017-05-01

    Full Text Available In this study, we describe a green and simple procedure for biosynthesis of ZnO nanoparticles using Candida albicans as eco-friendly reducing and capping agent. The synthesized ZnO nanoparticles were characterized by UV–vis spectroscopy, powder X-ray diffraction, scanning electron microscopy (SEM, transmission electron microscopy (TEM, photoluminescence (PL, thermo gravimetric analysis (TGA and differential thermal analysis (DTA. The prepared nano-particles were used as catalyst for the fast and efficient synthesis of steroidal pyrazolines (4–9 from α, β-unsaturated steroidal ketones (1–3. The target molecules were obtained in good to excellent yields applying the current method.

  12. STRUCTURAL ANALYSIS OF CONDITIONAL PREPARATION IN JUDO

    Directory of Open Access Journals (Sweden)

    Slavko Obadov

    2006-06-01

    Full Text Available Conditional preparation is a constituent part of overall sports preparation. Conditional training might be defined as a process of improvement of a sportsman’s functional and motor abilities, morphological characteristics, health, as well as the required motor knowledge. Conditional preparation can be might be classified as: general, basic and situational conditional preparation. Programs of the conditional training might be classified as: developing, resuming, recovering, preventive and recovering ones. High level of the general physical preparation enables maximum demonstration of the physical abilities of a sportsman during the stage of improvement of the specific motor abilities. Good general preparation of a sportsman enables him to push beyond his functional limits in order to cope with heavy loads easier, which subsequently enables him to achieve top performance level. Basic conditional preparation assumes the development of the most important judo abilities. Specific conditional preparation is related directly to the execution of different structural elements under the conditional requirements. Situational conditional preparation enables integration of the tactical and conditional training.

  13. Studies on Synthesis of Some Novel Heterocyclic Chalcone, Pyrazoline, Pyrimidine - 2 - One, Pyrimidine - 2 - Thione, para-Acetanilide Sulphonyl and Benzoyl Derivatives and their Antimicrobial Activity

    Directory of Open Access Journals (Sweden)

    Rakesh N. Mistry

    2005-01-01

    Full Text Available 1, 2 - Dichloro benzene on chlorosulphonation by chlorosulphonic acid gives 1, 2 - [dichloro] - benzene sulphonyl chloride which on condensation with p –amino acetophenone gives 1-[acetyl] - 1’ , 2’ - [dichloro] - dibenz sulphonamide derivative. This derivative undergo condensation with 2,4- dichloro benzaldehyde gives 1- [3” - (sub. phenyl - 2” - propene - 1” - one] - 1’ , 2’ - [dichloro] - dibenz sulphonamide derivative which on reaction with 99% hydrazine hydrate and glacial acetic acid gives 1-[acetyl]-3- [1’ , 2’ - (dichloro - dibenz sulphonamide] -5 - [2” , 4” - dichloro phenyl] - 2 - pyrazoline derivative. This derivative reacts with various substituted aldehydes to give corresponding substituted chalcone derivatives [1(a-j]. Now, these chalcone derivatives [1(a-j] on condensation with urea gives corresponding substituted pyrimidine - 2 - one derivatives [2(a-j] and on condensation with thio-urea gives corresponding substituted pyrimidine- 2 -thione derivatives [3(a-j]. Further, these chalcone derivatives [1(a-j] on reaction with 99% hydrazine hydrate gives 1 - [1’ - (H - 5’ - (sub. phenyl - 2’ - pyrazoline]- 3 - [1” , 2” - (dichloro - dibenz sulphonamide] - 5 - [2’’’ , 4’’’ - dichloro phenyl]-2- pyrazoline derivatives [4(a-j] as an intermediate compounds, which on condensation with p-acetanilide sulphonyl chloride gives corresponding substituted p - acetanilide sulphonyl derivatives [5(a-j] and on condensation with benzoyl chloride gives corresponding substituted benzoyl derivatives [6(a-j]. Structure elucidation of synthesised compounds has been made on the basis of elemental analysis, I.R. spectral studies and 1H N.M.R. spectral studies. The antimicrobial activity of the synthesised compounds has been studied against the cultures “Staphylococcus aureus”, “Escherichia coli” and “Candela albicans”.

  14. An eco-friendly synthesis of 2-pyrazoline derivatives catalysed by

    Indian Academy of Sciences (India)

    PRABHAT BHAT

    2017-07-07

    Jul 7, 2017 ... nagel synthesised 2-pyrazolines by the reaction of α,β- unsaturated aldehydes and ketones (chalcones) with hydrazine.12 This remains ..... 2011 Solvent-free reductive amination of aromatic alde- hydes catalyzed by CeCl3 ...

  15. Discovery of new antitubercular agents by combining pyrazoline and benzoxazole pharmacophores: design, synthesis and insights into the binding interactions

    Czech Academy of Sciences Publication Activity Database

    Rana, D. N.; Chhabria, M. T.; Shah, N. K.; Brahmkshatriya, Pathik

    2014-01-01

    Roč. 23, č. 5 (2014), s. 2218-2228 ISSN 1054-2523 Institutional support: RVO:61388963 Keywords : antitubercular * benzoxazole * interaction energy * molecular docking * pharmacophore * pyrazoline Subject RIV: CC - Organic Chemistry Impact factor: 1.402, year: 2014

  16. Synthesis and antimicrobial evaluation of some new pyrazole, pyrazoline and chromeno[3,4-c]pyrazole derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Abunada, Nada M.; Miqdad, Omar A. [Al-Aqsa University, Gaza (Palestinian Territory, Occupied). Faculty of Applied Sciences. Dept. of Chemistry; Hassaneen, Hamdi M. [Cairo University, Cairo (Egypt). Faculty of Science. Dept. of Chemistry; Samaha, Ahmed S. M. Abu [Al-Aqsa University, Gaza (Palestinian Territory, Occupied). Faculty of Applied Sciences. Dept. of Biology

    2009-07-01

    Some new pyrazole-5-carbonitrile derivatives 8,9 and pyrazole-5-carboxamide 13 were synthesized by the cycloaddition reaction of nitrilimines 3,4 to alpha-cyanocinnamonitriles 5a-f and alpha-cyanocinnamamide 12a,b respectively. On the other hand 3,4 add to ethyl alpha-cyanocinnamate 14a-f to give ethyl 2-pyrazoline-5-carboxylate derivatives 15,16. Also, cycloaddition of 3,4 to 3-cyanocoumarin 19a or 3-phenylsulphonylcoumarin 19b or 3-bromocoumarin 19c give chromeno[3,4-c]pyrazol-4(3H)-one derivatives 20. In the same direction, the cycloaddition of 3,4 to 3-acetylcoumarin 22 and 3-benzoylcoumarin 23 gives the corresponding dihydrochromeno[3,4-]pyrazol-4(3H)-one 24 and 25 respectively. Oxidation of 24 and 25 give 20. Most of the prepared compounds showed good to moderate antibacterial and antifungal activities. (author)

  17. Inorganic nanolayers: structure, preparation, and biomedical applications.

    Science.gov (United States)

    Saifullah, Bullo; Hussein, Mohd Zobir B

    2015-01-01

    Hydrotalcite-like compounds are two-dimensional inorganic nanolayers also known as clay minerals or anionic clays or layered double hydroxides/layered hydroxy salts, and have emerged as a single type of material with numerous biomedical applications, such as drug delivery, gene delivery, cosmetics, and biosensing. Inorganic nanolayers are promising materials due to their fascinating properties, such as ease of preparation, ability to intercalate different type of anions (inorganic, organic, biomolecules, and even genes), high thermal stability, delivery of intercalated anions in a sustained manner, high biocompatibility, and easy biodegradation. Inorganic nanolayers have been the focus for researchers over the last decade, resulting in widening application horizons, especially in the field of biomedical science. These nanolayers have been widely applied in drug and gene delivery. They have also been applied in biosensing technology, and most recently in bioimaging science. The suitability of inorganic nanolayers for application in drug delivery, gene delivery, biosensing technology, and bioimaging science makes them ideal materials to be applied for theranostic purposes. In this paper, we review the structure, methods of preparation, and latest advances made by inorganic nanolayers in such biomedical applications as drug delivery, gene delivery, biosensing, and bioimaging.

  18. Synthesis, studies and in-vitro antibacterial activity of N-substituted 5-(furan-2-yl-phenyl pyrazolines

    Directory of Open Access Journals (Sweden)

    Mamta Rani

    2015-03-01

    Full Text Available Novel compounds with antibacterial properties: pyrazoline derivatives were synthesized by the cyclization of various -1-[2-(alkoxyphenyl]-3-(furan-2-yl prop-2-en-1-one 1a–1d with N-substituted phenyl hydrazine in the presence of CH3COOH in ethanol. The structures of these compounds were elucidated by, IR, 1H NMR, 13C NMR, ESI-MS spectral data and their purities were confirmed by elemental analyses. The in vitro antibacterial activity of these compounds was evaluated against two Gram-positive and two Gram-negative bacteria Aeromonas hydrophila, Yersinia enterocolitica, Listeria monocytogenes, and Staphylococcus aureus by microdilution method and then the minimum inhibitory concentration (MIC of compounds were determined. The results showed that compounds (5R-5-(furan-2-yl-1-phenyl-3-[2-(benzyloxyphenyl]-4, 5-dihydro-1H-pyrazole (2b and (5R-5-(furan-2-yl-1-phenyl-3-[2-(naphthalen-2-ylmethoxy prop-2-en-1-yloxyphenyl]-4,5-dihydro-1H-pyrazole (2d showing most promising antibacterial activities as compared to Gentamicin and Tetracycline are given.

  19. Synthesis and Antimicrobial Studies of New Series of Pyrazoline Bearing Bis-Heterocycles via 1,3-Dipolar Cycloaddition Reactions

    Directory of Open Access Journals (Sweden)

    B. Jayashankara

    2008-01-01

    Full Text Available Biologically interesting bis-heterocycles bearing pyrazoline and imidazole moieties have been synthesized. 1H NMR, 13C NMR, IR and elemental analyses characterized the newly synthesized compounds. All the synthesized compounds were evaluated for their antimicrobial activity and were compared with the standard drugs. All the compounds demonstrated potent to weak antimicrobial activity.

  20. Synthesis and anticonvulsant activity of some 2-pyrazolines derived from chalcones

    Directory of Open Access Journals (Sweden)

    Nagihan Beyhan

    2017-05-01

    All compounds were tested for their anticonvulsant activity using pentylenetetrazole induced seizure (PTZ and maximal electroshock seizure (MES tests in mice at a dose level of 50 mg/kg. Among the 2-pyrazoline-1-carbothioamide derivatives, 5-(2,6-dichlorophenyl-3-(thiophen-2-yl-4,5-dihydro-1H-pyrazole-1-carbothioamide (2e reduced grade-5 seizure activity and also increased survival rate in PTZ test. In MES test, 5-(4-methoxyphenyl-3-[4-(methylsulphonylphenyl]-4,5-dihydro-1H-pyrazole-1-carbothioamide(2g has not only decreased seizure severity, but also increased survival rate. Among the 2-pyrazoline-1-carboxamide derivatives, 3-(5-bromothiophen-2-yl-N-(4-chlorophenyl-5-(2,6-dichlorophenyl-4,5-dihydro-1H-pyrazole-1-carboxamide (3d having 5-bromothiophen and 2,6-dichlorophenyl moieties and N-(4-chlorophenyl-5-(2,6-dichlorophenyl-3-(5-chlorothiophen-2-yl-4,5-dihydro-1H-pyrazole-1-carboxamide (3e having 5-chlorothiophen and 2,6-dichlorophenyl moieties showed remarkable activities in PTZ test. Among all tested derivatives, compound 3d was found to be the most active one and reduced grade-5 seizure severity and also increased survival rate.

  1. Preparation, Structure Characterization and Thermal Decomposition ...

    African Journals Online (AJOL)

    NJD

    Decomposition Process of the Dysprosium(III) m-Methylbenzoate 1 ... A dinuclear complex [Dy(m-MBA)3phen]2·H2O was prepared by the reaction of DyCl3·6H2O, m-methylbenzoic acid and .... ing rate of 10 °C min–1 are illustrated in Fig. 4.

  2. Pulse radiolysis study on free radical scavenger edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one). 2: A comparative study on edaravone derivatives

    International Nuclear Information System (INIS)

    Hata, Kuniki; Katsumura, Yosuke; Lin, M.; Yamashita, Shinichi; Muroya, Yusa; Fu Haiying; Nakagawa, Hidehiko

    2011-01-01

    A comparative study using the pulse radiolysis technique was carried out to investigate transient absorption spectra and rate constants for the reactions of OH radical and N 3 radical with edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one) and its four analogue compounds, 1,3-dimethyl-2-pyrazolin-5-one, 3-methyl-1-(pyridin-2-yl)-2-pyrazolin-5-one, 1-phenyl-3-trifluoromethyl-2-pyrazolin-5-one and 1-(4-chlorophenyl)-3-methyl-2-pyrazolin-5-one. The results showed that, unlike reaction mechanisms previously proposed, the phenyl group of edaravone played an important role in the reaction with OH radical and OH adducts to the phenyl group were formed. Quantum chemical calculations also strongly supported this attribution and suggested that the most favorable site for attacks by OH radical is the ortho position of the phenyl group. Moreover, the rate constants for the reactions of edaravone and its analogues towards OH radical and N 3 radical were about 8.0 x 10 9 , and 4.0 x 10 9 dm 3 mol -1 s -1 , respectively. Edaravone displayed higher reactivity compared to the others, in contrast to a previous report in which 3-methyl-1-(pyridin-2-yl)-2-pyrazolin-5-one showed the highest reactivity towards Hydroxyl radical OH. (author)

  3. Pulse radiolysis study on free radical scavenger edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one). 2: A comparative study on edaravone derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Hata, Kuniki; Katsumura, Yosuke [Tokyo Univ., School of Engineering, Tokyo (Japan); Lin, M; Yamashita, Shinichi [Japan Atomic Energy Agency, Advanced Science Research Center, Tokai, Ibaraki (Japan); Muroya, Yusa [Tokyo Univ., Nuclear Professional School, Tokai, Ibaraki (Japan); Haiying, Fu [Chinese Academy of Sciences, Shanghai (China); Nakagawa, Hidehiko [Nagoya City Univ., Graduate School of Pharmaceutical Sciences, Nagoya, Aichi (Japan)

    2011-01-15

    A comparative study using the pulse radiolysis technique was carried out to investigate transient absorption spectra and rate constants for the reactions of OH radical and N{sub 3} radical with edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one) and its four analogue compounds, 1,3-dimethyl-2-pyrazolin-5-one, 3-methyl-1-(pyridin-2-yl)-2-pyrazolin-5-one, 1-phenyl-3-trifluoromethyl-2-pyrazolin-5-one and 1-(4-chlorophenyl)-3-methyl-2-pyrazolin-5-one. The results showed that, unlike reaction mechanisms previously proposed, the phenyl group of edaravone played an important role in the reaction with OH radical and OH adducts to the phenyl group were formed. Quantum chemical calculations also strongly supported this attribution and suggested that the most favorable site for attacks by OH radical is the ortho position of the phenyl group. Moreover, the rate constants for the reactions of edaravone and its analogues towards OH radical and N{sub 3} radical were about 8.0 x 10{sup 9}, and 4.0 x 10{sup 9} dm{sup 3} mol{sup -1} s{sup -1}, respectively. Edaravone displayed higher reactivity compared to the others, in contrast to a previous report in which 3-methyl-1-(pyridin-2-yl)-2-pyrazolin-5-one showed the highest reactivity towards Hydroxyl radical OH. (author)

  4. Synthesis and Antimicrobial Studies of Some Novel Pyrazoline and Isoxazoline Derivatives

    Directory of Open Access Journals (Sweden)

    S. B. jadhav

    2009-01-01

    Full Text Available A new series of 1H-3-(4’-substituted phenyl-5-(6’’-methoxy napthaline-2-pyrazolines (4a-e and 1H-3-(4’-substituted phenyl-5-(6’’-methoxynapthaline-2-isoxazolines (5a-e were synthesized by reacting 1-(4’-substituted phenyl-3-(6’’-methoxynapthaline-2-propene-1-one (3a-e with hydrazine hydrate and hydroxylamine hydrochloride respectively. All these compounds were characterized by means of their IR, 1H NMR, spectroscopic data and microanalysis. All the synthesized products were evaluated for their antimicrobial activity. All the compounds exhibited significant to moderate antimicrobial activity.

  5. Design, Synthesis and the Biological Evaluation of New 1,3-Thiazolidine-4-ones Based on the 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one Scaffold

    Directory of Open Access Journals (Sweden)

    Maria Apotrosoaei

    2014-09-01

    Full Text Available New thiazolidine-4-one derivatives based on the 4-aminophenazone (4-amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one scaffold have been synthesized as potential anti-inflammatory drugs. The pyrazoline derivatives are known especially for their antipyretic, analgesic and anti-inflammatory effects, but recently there were synthesized new compounds with important antioxidant, antiproliferative, anticancer and antidiabetic activities. The beneficial effects of these compounds are explained by nonselective inhibition of cyclooxygenase izoenzymes, but also by their potential scavenging ability for reactive oxygen and nitrogen species. The structure of the new compounds was proved using spectroscopic methods (FR-IR, 1H-NMR, 13C-NMR, MS. The in vitro antioxidant potential of the synthesized compounds was evaluated according to the ferric reducing antioxidant power, phosphomolydenum reducing antioxidant power, DPPH and ABTS radical scavenging assays. The chemical modulation of 4-aminophenazone (6 through linkage to thiazolidine-propanoic acid derivatives 5a–l led to improved antioxidant potential, all derivatives 7a–l being more active than phenazone. The most active compounds are the derivatives 7e, and 7k, which showed the higher antioxidant effect depending on the antioxidant assay considered.

  6. Synthesis and Anticancer Activity of Some Novel Tetralin-6-yl-pyrazoline, 2-Thioxopyrimidine, 2-Oxopyridine, 2-Thioxo-pyridine and 2-Iminopyridine Derivatives

    Directory of Open Access Journals (Sweden)

    Ebtehal S. Al-Abdullah

    2011-04-01

    Full Text Available The title compounds were prepared by reaction of 6-acetyltetralin (1 with different aromatic aldehydes 2a-c, namely 2,6-dichlorobenzaldehyde, 2,6-diflouro-benzaldehyde, and 3-ethoxy-4-hydroxybenzaldehyde, to yield the corresponding a,b-unsaturated ketones 3a-c. Compound 3b was reacted with hydrazine hydrate to yield the corresponding 2-pyrazoline 4, while compounds 3a,b reacted with thiourea to afford the 2-thioxopyrimidine derivatives 5a,b, respectively. The reaction of 1, and the aromatic aldehydes 2a-c with ethyl cyanoacetate, 2-cyano-thioacetamide or malononitrile in the presence of ammonium acetate yielded the corresponding 2-oxopyridines 6a,b, 2-thioxopyridines 7a-c or 2-iminopyridines 8a,b, respectively. The newly prepared compounds were evaluated for anticancer activity against two human tumor cell lines. Compound 3a showed the highest potency with IC50 = 3.5 and 4.5 μg/mL against a cervix carcinoma cell line (Hela and breast carcinoma cell line (MCF7, respectively.

  7. Regiospecific synthesis of new fatty N-acyl trihalomethylated pyrazoline derivatives from fatty acid methyl esters (FAMEs)

    Energy Technology Data Exchange (ETDEWEB)

    Beck, Paulo; Santos, Juliane M. dos; D' Oca, Marcelo G. M.; Piovesan, Luciana A., E-mail: lpiovesan@gmail.com [Universidade Federal do Rio Grande (UFRS), RS (Brazil). Escola de Quimica e Alimentos; Kuhn, Bruna L.; Moreira, Dayse N.; Flores, Alex F.C.; Martins, Marcos A.P. [Universidade Federal de Santa Maria (UFSM), RS (Brazil). Dept. de Quimica

    2012-11-15

    A series of new fatty N-acyl trihalomethylated pyrazoline derivatives from fatty acid methyl esters was synthesized by the cyclo condensation of respective fatty hydrazides with 4-alkoxy- 1,1,1-trial omethyl-3-alquen-2-ones. Efficient and regiospecific cyclizations catalyzed by BF{sub 3}-MeOH gave the desired products in good to excellent yields and at high purity. (author)

  8. Structural and magnetic characterization of YIG particles prepared using microemulsions

    International Nuclear Information System (INIS)

    Teijeiro, A.G.; Baldomir, D.; Rivas, J.; Paz, S.; Vaqueiro, P.; Lopez Quintela, A.

    1995-01-01

    Yttrium-iron-garnet (YIG) particles have been synthesized using the microemulsion technique. A comparison of ferrite powders obtained by this method and those prepared by sol-gel and solid state reactions is reported. We have studied both the magnetic and structural properties and have found a dependence on annealing temperatures. ((orig.))

  9. Influence of preparation method on structural and magnetic ...

    Indian Academy of Sciences (India)

    Administrator

    Influence of preparation method on structural and magnetic properties of nickel ferrite nanoparticles. BINU P JACOB, ASHOK KUMAR†, R P PANT†, SUKHVIR SINGH† and. E M MOHAMMED*. Department of Physics, Maharaja's College, Ernakulam 681 011, India. †National Physical Laboratory, New Delhi 110 012, India.

  10. An Efficient Synthesis of New Pyrazolines and Isoxazolines Bearing Thiazolyl and Etheral Pharmacophores

    Energy Technology Data Exchange (ETDEWEB)

    Bhosle, Manisha R.; Mali, Jyotirling R.; Pratap, Umesh R.; Mane, Ramrao A. [Ambedkar Marathwada University, Aurangabad (India)

    2012-06-15

    A convenient synthetic route has been developed to synthesize 5-(4-((2-phenylthiazol-4-yl) methoxy)phenyl)- 3-(4-sustituted phenyl)pyrazolines (5a-f) and 5-(4-((2-phenylthiazol-4-yl)methoxy)phenyl)-3-(4-substituted phenyl)isoxazolines (6a-f) starting from 2-phenyl-4-chloromethylthiazole (1). The chloromethylthiazole (1) was first condensed with 4-hydroxy benzaldehyde (2) for obtaining 4-((2-phenylthiazol-4-yl)methoxy)benzaldehyde (3). Claisen-Smidth condensation of 4-((2-phenylthiazol-4-yl)methoxy)benzaldehyde (3) and acetophenones has been carried in alkaline alcohol and obtained 3-(4-((2-phenylthiazol-4-yl)methoxy)phenyl)-1-(4- substituted phenyl)prop-2-en-1-ones (4a-f). The cyclocondensation of 2-propen-1-ones has been first time carried separately with hydrazine hydrate and hydroxylamine hydrochloride in aqueous micellar tetradecyltrimethylammonium bromide (TTAB) medium for getting the titled heterocycles with good to excellent yields

  11. Study of structural relaxation in amorphous alloys prepared by sputtering

    International Nuclear Information System (INIS)

    Habibi, S.; Banaee, N.; Majidy, S.

    2004-01-01

    Full text: We have prepared amorphous alloy of Al x Cu 1-x (with X= 93, 90, 80, 70, 30) using sputtering system. The rate of growth was 0.7 nm/sec. X-ray diffractometer was used to conform the amorphous nature of the prepared specimens. High temperature annealing can change amorphous to crystalline structure, while low temperature annealing may transform amorphous state to a more stable amorphous state via structural relaxation of the specimen and enhancing the properties of the alloys, such as mechanical ductility etc. Here we have annealed the alloys at temperatures 100, 150, 200, 250, 300 and 350 C for 1 hour. We observed that microhardness of the specimen increases with annealing and gets maximum value at 300 C. Our XRD experiments and also earlier Moessbauer studies show that while the average interatomic distances reduces due to annealing, structure remains amorphous

  12. Nano-structured polymer composites and process for preparing same

    Science.gov (United States)

    Hillmyer, Marc; Chen, Liang

    2013-04-16

    A process for preparing a polymer composite that includes reacting (a) a multi-functional monomer and (b) a block copolymer comprising (i) a first block and (ii) a second block that includes a functional group capable of reacting with the multi-functional monomer, to form a crosslinked, nano-structured, bi-continuous composite. The composite includes a continuous matrix phase and a second continuous phase comprising the first block of the block copolymer.

  13. A Facile Solvent Free Microwave Induced Synthesis and Antibacterial Activity of Some 3-(2’-Hydroxyphenyl-5-(Substituted Aryl-2-Pyrazoline-N1-Caboxaldehydes

    Directory of Open Access Journals (Sweden)

    Birbal Bajia

    2007-01-01

    Full Text Available A novel one pot formylation of 3-(2’-hydroxyphenyl-5-(substituted 2-pyrazolines has been carried out using microwave irradiation with formic acid. solvent free reaction afforded title compounds in 80-90% yield with high purity.synthesized compounds were tested for their antibacterial activity using standard drug.

  14. Syntheses, experimental and theoretical studies on absorption/emission properties of pyrazoline-containing aryl/methoxy naphthyl substituents

    Energy Technology Data Exchange (ETDEWEB)

    Trilleras, Jorge; González-López, Edwin; León-Jaramillo, Jhair; Pérez-Gamboa, Alfredo; Puello-Polo, Esneyder, E-mail: jorgetrilleras@mail.uniatlantico.edu.co [Universidad del Atlántico (Colombia); Romo, Pablo; Ortíz, Alejandro; Quiroga, Jairo [Centre for Bioinformatics and Photonics, Cali (Colombia)

    2018-05-01

    5-Aryl-3-(2-methoxynaphthalen-6-yl)-1-phenylpyrazoline derivatives were synthesized starting from (E)-1-(3-aryl)-(2-methoxynaphthalen-6-yl)-prop-2-en-1-one and phenylhydrazine. The compounds were characterized by {sup 1} H and {sup 13}C nuclear magnetic resonance (NMR), elemental analyses and mass spectrometry. Some compounds showed promising luminescence properties in solution and in solid state; the absorption and emission characteristics were measured and the fluorescence quantum yield of two of the derivatives [4,5-dihydro-3-(2-methoxynaphthalen6-yl)-5-(3,4,5-trimethoxyphenyl)-1- phenyl-1H-pyrazoline and 5-(4-chlorophenyl)-4,5-dihydro3-(2-methoxynaphthalen-6-yl)-1-phenyl-1H- pyrazoline] were found to have excellent values compared to rhodamine B standard. Theoretical calculations at time-dependent density functional theory (TD-DFT) level are in agreement with the experimental measurements and are helpful to explain the electronic behavior. (author)

  15. Preparation, structure and properties of potassium neodymium tetraphosphate monocrystals

    International Nuclear Information System (INIS)

    Litvin, B.N.; Dorokhova, G.I.; Filipenko, O.S.

    1981-01-01

    To prepare KNd(PO 3 ) 4 in the form of monocrystals its crystallization in the aqueous solution of phosphoric acid is studied at 280-600 deg C. It is found that tetrapolyphosphate is formed higher than 350 deg C (KNd(P 3 ) 4 ), and lower than the temperature its polymorphous modification (tetrametaphosphate KNd(P 4 O 12 )) is crystallized. The main properties of the crystals of both modifications: habit, density, crystal structure, the Fedorov group, parameters of the elementary cell, refractive indices, interatomic distances, are presented. The life time of the metastable level Ndsup(3+)Esub(3/2) in the crystals prepared is measured. The decrease of life time value with the temperature and concentrational quenching is observed for both modifications [ru

  16. Preparation of porous carbon particle with shell/core structure

    Directory of Open Access Journals (Sweden)

    2007-05-01

    Full Text Available Porous carbon particles with a shell/core structure have been prepared successfully by controlled precipitation of the polymer from droplets of oil-in-water emulsion, followed by curing and carbonization. The droplets of the oil phase are composed of phenolic resin (PFR, a good solvent (ethyl acetate and porogen (Poly(methyl methacrylate, PMMA. The microstructure was characterized in detail by scanning electron microscopy (SEM, transmission electron microscopy (TEM, nitrogen adsorption, and thermo gravimetric analysis (TGA. The obtained carbon particles have a capsular structure with a microporous carbon shell and a mesoporous carbon core. The BET surface area and porous volume are calculated to be 499 m2g-1 and 0.56 cm3g-1, respectively. The effects of the amount of porogen (PMMA, co-solvent (acetone and surfactant on the resultant structure were studied in detail.

  17. [Preparation and structural analysis of diatomite-supported SPFS flocculant].

    Science.gov (United States)

    Zheng, Huai-li; Fang, Hui-li; Jiang, Shao-jie; Yang, Chun; Ma, Jiang-ya; Zhang, Zhao-qing

    2011-07-01

    In the presetn study, polymerized ferric sulphate (PFS) flocculant was prepared and tested. In the preparation of PFS flocculant, industrial by-product ferrous sulfate heptahydrate (FeSO4.7H2O) was reused as the main material. By composition with diatomite and drying up at certain temperature in vacuum drying oven, solid PFS flocculant was produced. Structural characteristics of the new flocculant product were examined through infrared spectroscopy and scanning electron microscopy (SEM), which showed that by compositing with diatomite, new group bridging emerged in the structure of PFS, which made the bond of groups stronger. In addition, part of the metalic contents in diatomite was polymerized with PFS, the product of which was polymerized ferric complex. Furthermore, the absorbing and agglomerating capacity of the diatomite carrier was significant. Considering the factors listed above, the new solid polymerized ferric sulphate (SPFS) flocculant was characterized with a larger molecule structure and enhanced absorbing, bridging and rolling sweep capacities. Through orthogonal experiment, optimum conditions of synthesis were as follows: the ratio of FeSO4.7H2O/diatomite in weight was 43/1, the reaction time is 1 h and the reaction temperature is 55 degrees C. By wastewater treatment experiment, it was found that the synthetic products showed good flocculation performance in the treatment of domestic sewage, the removal of COD was 80.00% and the removal of turbidity was 99.98%.

  18. Preparation of refractory cermet structures for lithium compatibility testing

    Science.gov (United States)

    Heestand, R. L.; Jones, R. A.; Wright, T. R.; Kizer, D. E.

    1973-01-01

    High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.

  19. Selective fluorescence resonance energy transfer from serum albumins to a bio-active 3-pyrazolyl-2-pyrazoline derivative: A spectroscopic analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, Arindam [Department of Chemistry, Jadavpur University, Kolkata 700032 (India); Bhattacharya, Subhash Chandra, E-mail: sbjuchem@yahoo.com [Department of Chemistry, Jadavpur University, Kolkata 700032 (India)

    2012-10-15

    A novel fluorescent probe and pharmaceutically significant: 3-pyrazolyl-2-pyrazoline derivative (PYZ) has been selected as an acceptor molecule for fluorescence resonance energy transfer (FRET) interaction with serum albumins. Steady state and time resolved fluorescence techniques were applied to elucidate the nature of interaction of PYZ with serum albumins (BSA and HSA). Negligible FRET mediated emission occurred in the case of HSA but an efficient FRET mediated emission resulted in case of BSA. To gain further insight into the FRET selectivity of PYZ with the proteins, FRET from L-tryptophan (donor; native tryptophan) to PYZ (acceptor) was performed with the aim of getting an idea about the steric restrictions imposed on PYZ by the other groups present in BSA and HSA. The studies revealed that the surface bound Trp-134 in BSA allows an efficient FRET process with PYZ while the buried Trp-214 in HSA does not. The unusual selectivity for FRET in case of PYZ and the serum albumins has also been attributed to the complex structure of PYZ due to the presence of bulkier phenyl moieties in it. The complex nature of the excited state photophysics of tryptophan (Trp) in proteins also accounts for this FRET selectivity of PYZ with BSA and HSA. - Highlights: Black-Right-Pointing-Pointer FRET from BSA/HSA to PYZ was monitored using steady state and time resolved fluorescence methods. Black-Right-Pointing-Pointer Efficient FRET process resulted in BSA-PYZ system in contrast with the HSA-PYZ system. Black-Right-Pointing-Pointer Surface bound Trp-134 in BSA facilitates the FRET process with PYZ than the buried Trp-214 in HSA. Black-Right-Pointing-Pointer Rigid and complex structure of PYZ also accounts for the FRET selectivity of PYZ with BSA/HSA.

  20. Irregular bilayer structure in vesicles prepared from Halobacterium cutirubrum lipids

    Science.gov (United States)

    Lanyi, J. K.

    1974-01-01

    Fluorescent probes were used to study the structure of the cell envelope of Halobacterium cutirubrum, and, in particular, to explore the effect of the heterogeneity of the lipids in this organism on the structure of the bilayers. The fluorescence polarization of perylene was followed in vesicles of unfractionated lipids and polar lipids as a function of temperature in 3.4 M solutions of NaCl, NaNO3, and KSCN, and it was found that vesicles of unfractionated lipids were more perturbed by chaotropic agents than polar lipids. The dependence of the relaxation times of perylene on temperature was studied in cell envelopes and in vesicles prepared from polar lipids, unfractionated lipids, and mixtures of polar and neutral lipids.

  1. Preparation, structural analysis, and properties of tenoxicam cocrystals.

    Science.gov (United States)

    Patel, Jagdishwar R; Carlton, Robert A; Needham, Thomas E; Chichester, Clinton O; Vogt, Frederick G

    2012-10-15

    Cocrystals of tenoxicam, a non-steroidal anti-inflammatory drug, are screened, prepared, and characterized in this study. Nine tenoxicam cocrystals were identified using solvent-drop grinding (SDG) techniques. Structural characterization was performed using powder X-ray diffraction (PXRD), differential scanning calorimetry, and multinuclear solid-state NMR (SSNMR). Thermal analysis, PXRD, and 1D SSNMR are used to detect solvates and phase mixtures encountered in SDG cocrystal screening. 2D SSNMR methods are then used to confirm cocrystal formation and determine structural aspects for selected cocrystals formed with saccharin, salicylic acid, succinic acid, and glycolic acid in comparison to Forms I and III of tenoxicam. Molecular association is demonstrated using cross-polarization heteronuclear dipolar correlation (CP-HETCOR) methods involving (1)H and (13)C nuclei. Short-range (1)H-(13)C CP-HETCOR and (1)H-(1)H double-quantum interactions between atoms of interest, including those engaged in hydrogen bonding, are used to reveal local aspects of the cocrystal structure. (15)N SSNMR is used to assess ionization state and the potential for zwitterionization in the selected cocrystals. The tenoxicam saccharin cocrystal was found to be similar in structure to a previously-reported cocrystal of piroxicam and saccharin. The four selected cocrystals yielded intrinsic dissolution rates that were similar or reduced relative to tenoxicam Form III. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Preparation of Ferroelectric Thin Films of Bismuth Layer Structured Compounds

    Science.gov (United States)

    Watanabe, Hitoshi; Mihara, Takashi; Yoshimori, Hiroyuki; Araujo, Carlos

    1995-09-01

    Ferroelectric thin films of bismuth layer structured compounds, SrBi2Ta2O9, SrBi2Nb2O9, SrBi4Ti4O15 and their solid solutions, were formed onto a sputtered platinum layer on a silicon substrate using spin-on technique and metal-organic decomposition (MOD) method. X-ray diffraction (XRD) analysis and some electrical measurements were performed on the prepared thin films. XRD results of SrBi2(Ta1- x, Nb x)2O9 films (0≤x≤1) showed that niobium ions substitute for tantalum ions in an arbitrary ratio without any change of the layer structure and lattice constants. Furthermore, XRD results of SrBi2 xTa2O9 films (0≤x≤1.5) indicated that the formation of the bismuth layer structure does not always require an accurate bismuth content. The layer structure was formed above 50% of the stoichiometric bismuth content in the general formula. SrBi2(Ta1- x, Nb x)2O9 films with various Ta/Nb ratios have large enough remanent polarization for nonvolatile memory application and have shown high fatigue resistance against 1011 cycles of full switching of the remanent polarization. Mixture films of the three compounds were also investigated.

  3. Structural and impedance characterization of ceramics prepared from NPK fertilizer

    Directory of Open Access Journals (Sweden)

    Diouma Kobor

    2015-06-01

    Full Text Available One of the main objectives of this work was to study the possibilities of valorising the phosphates through the development of a conductive ceramics using NPK fertilizer as a precursor. Phosphorus based powders were synthesized using solid state technique from NPK fertilizer, lithium chloride and iron chloride at different temperatures up to 900 °C and ceramic samples were prepared by the powder pressing and sintering at 1100 °C. XRD spectra of the calcined powders show various sharp peaks indicating a relatively high degree of crystallinity and presence of different crystalline phases, such as: phosphorus based crystalline compounds (AlPO4 and LiFePO4, ferrite (Fe3O4 and DyFeO3, CaSO4 and K3DyCl6. The prepared phosphorus based ceramics showed very interesting electrical and dielectric properties. Thus, in the future the obtained ceramics could find application in electronic or energy storage devices. However, further investigations are necessary to understand the exact chemical composition and structural characteristics of this material, to better understand the origin of the obtained electrical and dielectric behaviour.

  4. Inorganic nanolayers: structure, preparation, and biomedical applications

    Directory of Open Access Journals (Sweden)

    Saifullah B

    2015-09-01

    Full Text Available Bullo Saifullah, Mohd Zobir B HusseinMaterials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA, Universiti Putra Malaysia, Serdang, MalaysiaAbstract: Hydrotalcite-like compounds are two-dimensional inorganic nanolayers also known as clay minerals or anionic clays or layered double hydroxides/layered hydroxy salts, and have emerged as a single type of material with numerous biomedical applications, such as drug delivery, gene delivery, cosmetics, and biosensing. Inorganic nanolayers are promising materials due to their fascinating properties, such as ease of preparation, ability to intercalate different type of anions (inorganic, organic, biomolecules, and even genes, high thermal stability, delivery of intercalated anions in a sustained manner, high biocompatibility, and easy biodegradation. Inorganic nanolayers have been the focus for researchers over the last decade, resulting in widening application horizons, especially in the field of biomedical science. These nanolayers have been widely applied in drug and gene delivery. They have also been applied in biosensing technology, and most recently in bioimaging science. The suitability of inorganic nanolayers for application in drug delivery, gene delivery, biosensing technology, and bioimaging science makes them ideal materials to be applied for theranostic purposes. In this paper, we review the structure, methods of preparation, and latest advances made by inorganic nanolayers in such biomedical applications as drug delivery, gene delivery, biosensing, and bioimaging.Keywords: inorganic nanolayers, layered double hydroxides, layered hydroxy salts, drug delivery, biosensors, bioimaging

  5. Pd-Ni-MWCNT nanocomposite thin films: preparation and structure

    Science.gov (United States)

    Kozłowski, Mirosław; Czerwosz, ElŻbieta; Sobczak, Kamil

    2017-08-01

    The properties of nanocomposite palladium-nickel-multi-walled (Pd-Ni-MWCNT) films deposited on aluminum oxide (Al2O3) substrate have been prepared and investigated. These films were obtained by 3 step process consisted of PVD/CVD/PVD methods. The morphology and structure of the obtained films were characterized by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) techniques at various stages of the film formation. EDX spectrometer was used to measurements of elements segregation in the obtained film. TEM and STEM (Scanning Transmission Electron Microscopy) observations showed MWCNTs decorated with palladium nanoparticles in the film obtained in the last step of film formation (final PVD process). The average size of the palladium nanoparticles observed both on MWCNTs and carbonaceous matrix does not exceed 5 nm. The research was conducted on the use of the obtained films as potential sensors of gases (e.g. H2, NH3, CO2) and bio-sensors or optical sensors.

  6. Preparation, structure and thermal stability of Cu/LDPE nanocomposites

    International Nuclear Information System (INIS)

    Xia Xianping; Cai Shuizhou; Xie Changsheng

    2006-01-01

    Copper/low-density-polyethylene (Cu/LDPE) nanocomposites have been prepared using a melt-blending technique in a single-screw extruder. Their structure and thermal characteristics are characterized by using X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results of XRD, SEM and SEM-EDS Cu-mapping show that the nanocomposites are a hybrid of the polymer and the copper nanoparticles, and the copper nanoparticles aggregates were distributed uniformly in general. The results also show that the nanocomposites and the base resin, the pure LDPE, have a different crystalline structure and the same oriented characteristics owing to the presence of copper nanoparticles and the same cooling condition. The results of DSC show that the incorporation of copper nanoparticles can decrease the melting temperatures but increase the crystallization temperatures, and can lower the crystallinity degree of the matrix of the composites. The results of TGA show that the presence of copper nanoparticles can improve the thermal stability of the nanocomposites, a maximum increment of 18 deg. C is obtained comparing with the pure LDPE in this experiment. The results of TGA also show that the influence of the incorporation of the copper nanoparticles on the thermal stability of the Cu/LDPE nanocomposites is different from that of the non-metal nanoparticles on the polymer/non-metal nanocomposites and the copper microparticles on the Cu/LDPE microcomposites. The increase of the thermal stability of the Cu/LDPE nanocomposites will decrease when the content of the copper nanoparticles is more than 2 wt.%. The difference might be caused by the fact that the activity of the metal nanoparticles is much more higher than that of the non-metal nanoparticles, and the different size effect the different copper particles has

  7. Electric-Arc Plasma Installation for Preparing Nanodispersed Carbon Structures

    International Nuclear Information System (INIS)

    Stefanov, P.; Garlanov, D.; Vissokov, G.

    2008-01-01

    An electric-arc plasma installation operated in the hidden anode arrangement is constructed and used for the preparation of carbon nanostructures. A contracted plasma arc generated by a plasma torch using an inert gas is used as heat source. The average mass temperature of arc is higher than 10 4 K, while its power density, which is directly transferred onto the electrode (anode), is ∼ 2 kW/mm 2 . The anode contact area formed on the electrode moves against the arc by way of shifting the electrode and is hidden completely in the interior of plasma gas stream moving towards it. As a result of both the direct plasma attack and the opposite movement of streams in the hidden anode contact area, a temperature higher than 6000 K is reached. Thus, intensive vaporization takes place, which forms a saturated plasma-gas-aerosol phase of the initial material of electrode (anode). This gas phase is mixed in and carried by the plasma stream. Over that mixed plasma stream, a controlled process of quenching (fixation) is carried out by twisted turbulent fluid streams. After the fixation, the resultant carbon nano-structures are caught by a filter and collected in a bunker.

  8. In vivo radioprotection of mice by 3-methyl-1-phenyl-2-pyrazolin-5-one (edaravone; Radicut), a clinical drug

    International Nuclear Information System (INIS)

    Anzai, Kazunori; Furuse, Masako; Yoshida, Akira; Matsuyama, Azusa; Moritake, Takashi; Ikota, Nobuo; Tsuboi, Koji

    2004-01-01

    Edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one; Radicut) is a brain-protecting agent used clinically to treat acute ischemic stroke with a reaction mechanism of free radical scavenging. Since the initial stage of radiation damage involves the formation of free radicals, edaravone is expected to be effective in preventing lethal damage from ionizing radiation. In the present study, we used mice to examine in vivo the radioprotective effect of edaravone on whole body X-ray irradiation. A solution of edaravone was administered intraperitoneally to C3H mice (male, 10 weeks old), and they were irradiated with a total dose of 8.0 Gy. Edaravone exhibited dose-dependent and injection time-dependent radioprotection. When injected 30 min before the X-ray irradiation, it had the greatest radioprotective effect, whereas an injection after the irradiation showed no protective effect. The LD 50/30 was about 8.8 Gy for edaravone-injected mice and 6.6 Gy for control mice, yielding a DRF for edaravone (450 mg/kg body weight) of 1.3. Edaravone decreased the body temperature transiently about 3-6deg C, but this did not seem to be responsible for the radioprotection. Since the radioprotection was observed only when the reagent was administered before the irradiation, the primary action of edaravone might be the quenching of free radicals with a short lifetime generated by the irradiation. (author)

  9. In vivo radioprotection of mice by 3-methyl-1-phenyl-2-pyrazolin-5-one (edaravone; Radicut), a clinical drug

    Energy Technology Data Exchange (ETDEWEB)

    Anzai, Kazunori; Furuse, Masako; Yoshida, Akira; Matsuyama, Azusa; Moritake, Takashi; Ikota, Nobuo [National Inst. of Radiological Sciences, Chiba (Japan). Research Center for Radiation Safety; Tsuboi, Koji [Tsukuba Univ., Ibaraki (Japan). Inst. of Clinical Medicine

    2004-06-01

    Edaravone (3-methyl-1-phenyl-2-pyrazolin-5-one; Radicut) is a brain-protecting agent used clinically to treat acute ischemic stroke with a reaction mechanism of free radical scavenging. Since the initial stage of radiation damage involves the formation of free radicals, edaravone is expected to be effective in preventing lethal damage from ionizing radiation. In the present study, we used mice to examine in vivo the radioprotective effect of edaravone on whole body X-ray irradiation. A solution of edaravone was administered intraperitoneally to C3H mice (male, 10 weeks old), and they were irradiated with a total dose of 8.0 Gy. Edaravone exhibited dose-dependent and injection time-dependent radioprotection. When injected 30 min before the X-ray irradiation, it had the greatest radioprotective effect, whereas an injection after the irradiation showed no protective effect. The LD{sub 50/30} was about 8.8 Gy for edaravone-injected mice and 6.6 Gy for control mice, yielding a DRF for edaravone (450 mg/kg body weight) of 1.3. Edaravone decreased the body temperature transiently about 3-6deg C, but this did not seem to be responsible for the radioprotection. Since the radioprotection was observed only when the reagent was administered before the irradiation, the primary action of edaravone might be the quenching of free radicals with a short lifetime generated by the irradiation. (author)

  10. Chitosan-Based Matrices Prepared by Gamma Irradiation for Tissue Regeneration: Structural Properties vs. Preparation Method.

    Science.gov (United States)

    Casimiro, Maria Helena; Lancastre, Joana J H; Rodrigues, Alexandra P; Gomes, Susana R; Rodrigues, Gabriela; Ferreira, Luís M

    2017-02-01

    In the last decade, new generations of biopolymer-based materials have attracted attention, aiming its application as scaffolds for tissue engineering. These engineered three-dimensional scaffolds are designed to improve or replace damaged, missing, or otherwise compromised tissues or organs. Despite the number of promising methods that can be used to generate 3D cell-instructive matrices, the innovative nature of the present work relies on the application of ionizing radiation technology to form and modify surfaces and matrices with advantage over more conventional technologies (room temperature reaction, absence of harmful initiators or solvents, high penetration through the bulk materials, etc.), and the possibility of preparation and sterilization in one single step. The current chapter summarizes the work done by the authors in the gamma radiation processing of biocompatible and biodegradable chitosan-based matrices for skin regeneration. Particular attention is given to the correlation between the different preparation conditions and the final polymeric matrices' properties. We therefore expect to demonstrate that instructive matrices produced and improved by radiation technology bring to the field of skin regenerative medicine a supplemental advantage over more conservative techniques.

  11. Structural and compositional gradients: basic idea, preparation, applications

    International Nuclear Information System (INIS)

    Ilschner, B.

    1993-01-01

    The term gradient materials refers to gradients of chemical composition and/or microstructural parameters which are intentionally introduced into components of any kind of homogeneous or heterogeneous materials, including metallic alloys, ceramics, glasses, polymers, and composites. After a short review of the development of the gradient materials technology since 1972, some fundamental aspects concerning the effects of such gradients on physical or mechanical properties are discussed. A selection of technical applications which have been discussed recently is presented. Finally, different methods for the preparation of gradients from gaseous, liquid or powder precursors are reviewed. (orig.)

  12. Preparation and mounting of adult Drosophila structures in Canada balsam.

    Science.gov (United States)

    Stern, David L; Sucena, Elio

    2012-03-01

    The Drosophila cuticle carries a rich array of morphological details. Thus, cuticle examination has had a central role in the history of genetics. To prepare fine "museum-quality," permanent slides, it is best to mount specimens in Canada Balsam. It is difficult to give precise recipes for Canada Balsam, because every user seems to prefer a slightly different viscosity. Dilute solutions spread easily and do not dry too rapidly while mounting specimens. The disadvantage is that there is actually less Balsam in a "drop" of the solution, and when dried, it can contract from the sides of the coverslip, sometimes disturbing the specimen. Unfortunately, there is no substitute for experience when using Canada Balsam. This protocol describes a procedure for mounting adult cuticles in Canada Balsam.

  13. Structural characterization of pharmaceutical heparins prepared from different animal tissues.

    Science.gov (United States)

    Fu, Li; Li, Guoyun; Yang, Bo; Onishi, Akihiro; Li, Lingyun; Sun, Peilong; Zhang, Fuming; Linhardt, Robert J

    2013-05-01

    Although most pharmaceutical heparin used today is obtained from porcine intestine, heparin has historically been prepared from bovine lung and ovine intestine. There is some regulatory concern about establishing the species origin of heparin. This concern began with the outbreak of mad cow disease in the 1990s and was exacerbated during the heparin shortage in the 2000s and the heparin contamination crisis of 2007-2008. Three heparins from porcine, ovine, and bovine were characterized through state-of-the-art carbohydrate analysis methods with a view profiling their physicochemical properties. Differences in molecular weight, monosaccharide and disaccharide composition, oligosaccharide sequence, and antithrombin III-binding affinity were observed. These data provide some insight into the variability of heparins obtained from these three species and suggest some analytical approaches that may be useful in confirming the species origin of a heparin active pharmaceutical ingredient. Copyright © 2013 Wiley Periodicals, Inc.

  14. Preparation of interconnected highly porous polymeric structures by a replication and freeze-drying process

    NARCIS (Netherlands)

    Hou, Q.; Grijpma, Dirk W.; Feijen, Jan

    2003-01-01

    Three-dimensional degradable porous polymeric structures with high porosities (93-98%) and well-interconnected pore networks have been prepared by freeze-drying polymer solutions in the presence of a leachable template followed by leaching of the template. Templates of the pore network were prepared

  15. Preparation and crystal structure of Ca4Sb2O

    International Nuclear Information System (INIS)

    Eisenmann, B.; Limartha, H.; Schaefer, H.

    1980-01-01

    The formerly described compound Ca 2 Sb is to be corrected to Ca 4 Sb 2 O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K 2 NiF 4 structure type. (orig.)

  16. Structure of nanocomposites of Al–Fe alloys prepared by ...

    Indian Academy of Sciences (India)

    Wintec

    This difference in the product structure can be attributed to the difference in alloying mechanisms in MA and RSP. Keywords. Nanocomposites; Al–Fe; mechanical alloying; rapid solidification; quasicrystalline. 1. Introduction. Al–Fe alloys are attractive for applications at temperatures beyond those normally associated with ...

  17. A model of Piron's preparation-question structures in Ludwig's selection structures

    Science.gov (United States)

    Cattaneo, Gianpiero; Nisticò, Giuseppe

    1993-03-01

    We give a model of the basic Jauch-Piron (JP) approach to quantum physics, i.e., of “preparation-question structure” (with four basic axioms and without axioms C, P, A), in terms of Ludwig's “selection structure”; in the latter structure the primitive notion of “individual sample” of a physical entity is formally described (without making reference to any probability concept). Once we interpret Piron's concept of “question” in Ludwig's context of a selection structure, we find that there is no difficulty in formalizing notions such as “performable together questions”; moreover, results such as “ α ˜˜= α” or “( αδ Β)˜= α ˜▽ Β˜” can be formally proved. We develop the theory along the lines of the JP approach; the set of JP propositions is derived and it turns out to be a complete lattice, as happens in Piron's theory, but with a different physical interpretation of the lattice operations. Finally, we study some connections between the standard Ludwig foundation and our approach.

  18. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

    KAUST Repository

    Xue, Zheng; Lu, Huijie; Liu, Wen-Tso

    2014-01-01

    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses

  19. V-amylose structural characteristics, methods of preparation, significance, and potential applications

    CSIR Research Space (South Africa)

    Obiro, WC

    2012-02-01

    Full Text Available , and postprandial hyperglycaemia in diabetics. Various aspects of V-amylose structure, methods of preparation, factors that affect its formation, and the significance and potential applications of the V-amylose complexes are reviewed....

  20. Physical content of preparation-question structures and Brouwer-Zadeh lattices

    Science.gov (United States)

    Cattaneo, Gianpiero; Nisticó, Giuseppe

    1992-10-01

    We give a criterion to compare the physical content of different mathematical structures derived from a preparation-question structure. Then this criterion is used in order to compare the physical content of the (Jauch-Piron's) property lattice with the physical content of the poset of testable properties. We prove that for complete preparation-question structures these two structures carry the same physical content; moreover the set of testable properties has the algebraic structure of the Brouwer-Zadeh lattice. For more general preparation-question structures the physical content of the poset of testable property can be larger than that of the property lattice. Physically relevant examples of the possible cases are given.

  1. Structures of nanoparticles prepared from oil-in-water emulsions.

    Science.gov (United States)

    Sjöström, B; Kaplun, A; Talmon, Y; Cabane, B

    1995-01-01

    Hydrophobic substances were dissolved in an organic solvent and emulsified with an aqueous solution at very high shear. Droplets of very small sizes (50-100 nm) were obtained by using surfactants which were combinations of lecithins and bile salts. After emulsification, the organic solvent was removed by evaporation, yielding stable dispersions of solid particles. The sizes, shapes, and structures of the particles were examined through quasi-elastic light scattering, small-angle neutron scattering and cryotransmission electron microscopy. Cholesterol acetate particles stabilized by lecithin and bile salts were found to be platelets of 10-20 nm thickness and 80 nm diameter. Cholesteryl acetate particles stabilized with POE-(20)-sorbitan monolaurate were dense spherical globules of diameter 100 nm. Particles with a composition similar to the endogenously occurring, lipoprotein, LDL, were large spherical globules studded with small vesicles. The subsequent evolution of the cholesteryl acetate dispersion upon aging was examined. There was no transfer of cholesteryl acetate between particles nor to large crystals. However, some aggregation of the particles was observed when the volume fraction of the particles in the aqueous dispersion exceeded 0.05. Thus, the structure of the nanoparticles obtained through deswelling of emulsion droplets changes according to the nature of the emulsifiers and to the composition of the hydrophobic substances which they contain.

  2. Pore Structure Characterization in Concrete Prepared with Carbonated Fly Ash

    Science.gov (United States)

    Sahoo, Sanjukta

    2018-03-01

    Carbon dioxide capture and storage (CCS) is a technique to address the global concern of continuously rising CO2 level in the atmosphere. Fly ash is considered as a suitable medium for CCS due to presence of metal oxides. The fly ash which has already sequestered carbon dioxide is referred to as carbonated fly ash. Recent research reveals better durability of concretes using carbonated fly ash as part replacement of cement. In the present research pore structure characterization of the carbonated fly ash concrete has been carried out. Mercury Intrusion porosimetry test has been conducted on control concrete and concrete specimens using fly ash and carbonated fly ash at replacement levels of 25% and 40%. The specimens have been water cured for 28 days and 90 days. It is observed that porosity reduction rate is more pronounced in carbonated fly ash concrete compared to control concrete at higher water curing age. Correlation analysis is also carried out which indicates moderately linear relationship between porosity % and pore distribution with particle size and water curing.

  3. Methanol-Sensing Property Improvement of Meso structured Zinc Oxide Prepared by the Nano casting Strategy

    International Nuclear Information System (INIS)

    Gao, Q.; Zheng, W.T.; Wei, C.D.; Lin, H.M.

    2013-01-01

    The specific structure and morphology often play a critical role in governing the excellent intrinsic properties of the compound semiconductor. Herein, meso structured ZnO with excellent methanol-sensing properties was prepared by a structure replication procedure through the incipient wetness technique. The investigation on the crystal structure and morphology of the resultant material shows that the product consists of hexagonally arranged meso pores and crystalline walls, and its structure is an ideal replication of CMK-3 template. Consequently, meso structured ZnO was fabricated as a gas sensor for methanol. The excellent methanol-sensing performance was achieved at a relatively low operating temperature of 120°C. In comparison with the non porous ZnO prepared through conventional coprecipitation approach, meso structured ZnO material shows the higher sensitivity and stability. Furthermore, it shows the discrimination between methanol and ethanol sensitivity, which makes it a good candidate in fabricating selective methanol sensor in practice

  4. Structural and morphological characterization of fullerite crystals prepared from the vapor phase

    International Nuclear Information System (INIS)

    Haluska, M.; Fejdi, P.; Vybornov, M.; Kuzmany, H.

    1993-01-01

    Crystal structure, habits and surface structures of fullerite crystals prepared from vapor phase were characterized by X-ray analysis, interfacial angle measurements and optical and scanning electron microscopy (SEM). The study of selected C 60 crystals confirmed the fcc structure at room temperature. The crystal habit is determined by two types of morphological faces, namely {100} and {111}. SEM was used for the observation of thermal etched surfaces. (orig.)

  5. Structure-activity relationship of surfactant for preparing DMFC anodic catalyst

    International Nuclear Information System (INIS)

    Su Yi; Xue Xinzhong; Xu Weilin; Liu Changpeng; Xing Wei; Zhou Xiaochun; Tian Tian; Lu Tianhong

    2006-01-01

    Three kinds of surfactants as stabilizer were applied to the preparation of electrocatalysts for direct methanol fuel cell (DMFC). The catalysts have been characterized by examining their catalytic activities, morphologies and particle sizes by means of cyclic voltammetry, chronoamperometry, X-ray diffraction and transmission electron microscopy (TEM). It is found that the surfactants with different structures have a significantly influence on the catalyst shape and activity. The catalysts prepared with non-ionic surfactants as the stabilizer show higher activity for direct oxidation of methanol. The structure-activity relationship (SAR) analysis has been explored and the effect of hydrophile-lipophile balance (HLB value) has also been discussed

  6. Tuning of Preparational Factors Affecting the Morphological Structure and Gas Separation Property of Asymmetric Polysulfone Membranes

    Science.gov (United States)

    Yuenyao, C.; Ruangdit, S.; Chittrakarn, T.

    2017-09-01

    The aim of this work was to study the effect of preparational factors such as solvent type, evaporation time (ET) and non-solvent additive, on the morphological structure, physical and gas separation properties of the prepared membrane samples by tuning of these parameters. Flat sheet asymmetric polysulfone (PSF) membranes were prepared by the dry/wet phase inversion process combined with the double coagulation bath method. The alteration of the prepared membranes were analyzed through scientific techniques such as Scanning Electron Microscope (SEM) and Dynamic Mechanical Thermal Analysis (DMTA). Furthermore, gas separation performance of membrane samples was measured in term of gas permeation and ideal selectivity of CO2/CH4. Experimental results showed that the change of preparational factors affected to the gas permeation of asymmetric PSF membranes. For example, the selective layer thickness increased with increasing of ET. This lead to increase significantly of ideal selectivity of CO2/CH4. The CO2/CH4 ideal selectivity was also increased with increase of ethanol (non-solvent additive) concentration in casting solution. In summary, the tuning of preparational factors affected to morphological structure, physical and gas separation properties of PSF membranes.

  7. Copper(II Complexes with Ligands Derived from 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one: Synthesis and Biological Activity

    Directory of Open Access Journals (Sweden)

    Raluca Cernat

    2006-11-01

    Full Text Available The synthesis of Cu(II complexes derived from Schiff base ligands obtainedby the condensation of 2-hydroxybenzaldehyde or terephtalic aldehyde with 4-amino-antipyrine (4-amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one is presented. The newlyprepared compounds were characterized by 1H-NMR, UV-VIS, IR and ESRspectroscopy. The determination of the antimicrobial activity of the ligands and of thecomplexes was carried out on samples of Escherichia coli, Klebsiella pneumoniae,Acinetobacter boumanii, Pseudomonas aeruginosa, Staphylococcus aureus and Candidasp. The qualitative and quantitative antimicrobial activity test results proved that all theprepared complexes are very active, especially against samples of Ps. aeruginosa, A.Boumanii, E. coli and S. aureus.

  8. Preparation of BiOBr thin films with micro-nano-structure and their photocatalytic applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Rui [College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024 (China); Fan, Caimei, E-mail: fancm@163.com [College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024 (China); Zhang, Xiaochao, E-mail: zhang13598124761@163.com [College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024 (China); Wang, Yawen; Wang, Yunfang [College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024 (China); Zhang, Hui [Particle Technology Research Centre, Department of Chemical and Biochemical Engineering, The University of Western Ontario, London, Ontario N6A 5B9 (Canada)

    2014-07-01

    A series of micro-nano-structure BiOBr thin films were prepared at a low temperature by the alcoholysis-coating method using BiBr{sub 3} as precursor. The as-prepared films were characterized by X-ray powder diffraction, scanning electron microscopy, and Brunauer–Emmett–Teller surface area. The obtained results indicated that micro-nano-structure tetragonal BiOBr films with different intensity ratios of (110) to (102) characteristic peaks could be synthesized through controlling the reaction temperature and the calcination temperatures. Furthermore, the photocatalytic activities of BiOBr thin films with different preparation conditions have been evaluated by the degradation of methyl orange (MO) under UV light irradiation, suggesting that the photocatalytic activity should be closely related to the solvent, the alcoholysis reaction temperature, and the calcining temperature. The best photocatalytic degradation efficiency of MO for BiOBr thin films reaches 98.5% under 2.5 h UV irradiation. The BiOBr thin films display excellent stability and their photocatalytic activity still remains above 90% after being used five times. The main reasons for the higher photocatalytic activity of micro-nano-structure BiOBr microspheres have been investigated. In addition, the possible formation mechanism of BiOBr thin films with micro-nano-structure and excellent photocatalytic activity was proposed and discussed. - Highlights: • The BiOBr film was prepared at low temperature via alcoholysis-coating method. • The optimum process conditions of preparing BiOBr film were discussed. • As-prepared BiOBr films were composed of micro-nano flake structures. • The BiOBr films demonstrated excellent photocatalytic activity. • The formation mechanism of BiOBr films with high activity was proposed.

  9. Synthesis of novel pyrazoline based bis (1,2,3-triazole scaffolds via click chemistry

    Directory of Open Access Journals (Sweden)

    Kiran Kothuri

    2017-01-01

    Full Text Available A series of novel bis(1,2,3-triazoles derivatives 7a–m were synthesized by the 1,3-dipolar cycloaddition (click-reaction of 1-methyl-3,5-bis(2- -(prop-2-yn-1-yloxyphenyl-4,5-dihydro-1H-pyrazole (5 with various aralkyl azides 6a–m in the presence of sodium ascorbate and copper sulphate with good yields. The required precursor 5 was synthesized by reacting (E-1,3- -bis(2-hydroxyphenylprop-2-en-1-one (3 with methylhydrazine hydrate via 2,2′-(1-methyl-4,5-dihydro-1H-pyrazole-3,5-diyldiphenol 4, followed by reaction with propargyl bromide. The homogeneity of all the newly synthesized compounds was checked by TLC. The IR, NMR, mass spectral data and elemental analysis were in accord with the assigned structure. The title compounds were evaluated for their antibacterial activity against various bacterial strains, i.e., Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus subtilis; compounds 7f–7h and 7j were found to be moderately active against the bacteria, when compared with that of the standard drug. Furthermore, the same library of compounds was evaluated for their antioxidant activity using the nitric oxide radical scavenging activity. The results of the study showed that compounds 7e–7h and 7k–7m showed good radical scavenging activity.

  10. Influence of Professional Preparation and Class Structure on HIV, STD, and Pregnancy Prevention Education

    Science.gov (United States)

    Rhodes, Darson L.; Jozkowski, Kristen N.; Hammig, Bart J.; Ogletree, Roberta J.; Fogarty, Erin C.

    2014-01-01

    Objective: The purpose of this study was to determine if education about human immunodeficiency virus (HIV)/sexually transmitted disease (STD) and pregnancy prevention is dependent on professional preparation and/or class structure. Design: A secondary data analysis of the 2006 School Health Policies and Programmes Study (SHPPS) was conducted.…

  11. Nuclear structure data file. A manual for preparation of data sets

    International Nuclear Information System (INIS)

    Ewbank, W.B.; Schmorak, M.R.; Bertrand, F.E.; Feliciano, M.; Horen, D.J.

    1975-06-01

    The Nuclear Data Project at ORNL is building a computer-based file of nuclear structure data, which is intended for use by both basic and applied users. For every nucleus, the Nuclear Structure Data File contains evaluated nuclear structure information. This manual describes a standard input format for nuclear structure data. The format is sufficiently structured that bulk data can be entered efficiently. At the same time, the structure is open-ended and can accommodate most measured or deduced quantities that yield nuclear structure information. Computer programs have been developed at the Data Project to perform consistency checking and routine calculations. Programs are also used for preparing level scheme drawings. (U.S.)

  12. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

    KAUST Repository

    Xue, Zheng

    2014-07-15

    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community. © 2014 © 2014 Taylor & Francis.

  13. Influence of preparation conditions on structural elements ordering in vanadium pentaoxide xerogels

    International Nuclear Information System (INIS)

    Peryshkov, D.V.; Grigor'eva, A.V.; Gudilin, E.A.; Semenenko, D.A.; Volkov, V.V.; Dembo, K.A.; Tret'yakov, Yu.D.

    2006-01-01

    Complex analysis of vanadium pentaoxide xerogel films prepared by three different methods, i.e. by V 2 O 5 dissolution in H 2 O 2 , by hydrolysis of VO(t-Bu) 3 and by ion exchange, has been carried out for the first time using the methods of small-angle X-ray scattering, IR spectroscopy, scanning electron microscopy and thermal analysis. A correlation between chemical prehistory of the samples prepared and their structural features has been established. It is shown that the prehistory influence stems from the differences in gelation process when different precursors are used [ru

  14. Studying the structural and optical properties of Zn O:Cu prepared by APCVD technique

    International Nuclear Information System (INIS)

    Manssor, M.

    2012-01-01

    Undoped and Cu-doped Zn O ant (3-9 wt.%) thin films have been prepared by APCVD technique on glass substrates at 500 degree.The structural and optical properties of these films were studied. The results of the structural tests showed that these films are of a polycrystalline hexagonal structure with a preferred orientation in the (002) direction, the optical properties included transmittance, energy gap, ob sorption coefficient, reflectance, refractive index and extinction coefficient, the energy gap values were found to decrease from (3.25 to 3.15 eV) and the average transmittance was found about (90%) in the visible region. (author).

  15. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    Science.gov (United States)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-11-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound.

  16. Novel preparation and photocatalytic activity of one-dimensional TiO2 hollow structures

    International Nuclear Information System (INIS)

    Yu Huogen; Yu Jiaguo; Cheng Bei; Liu Shengwei

    2007-01-01

    Usually, templated methods include two important steps: the coating of nanocrystals on the surface of the templates and the removal of the templates. In this study, one-dimensional TiO 2 hollow structures, based on the template-directed deposition and then in situ template-sacrificial reaction (or dissolution), were prepared by a one-step template method using vanadium oxide nanobelts as the templates and TiF 4 as the precursor at 60 deg. C. The coating of TiO 2 nanoparticles on the surface of the templates was accompanied with the dissolution of vanadium oxide nanobelts by HF produced during the hydrolysis of TiF 4 in the reaction solution. It was found that the prepared one-dimensional TiO 2 hollow structures with a mesoporous wall were composed of TiO 2 nanoparticles with a diameter of 10-55 nm, resulting in a large specific surface area (77.2 m 2 g -1 ) and high pore volume (0.13 cm 3 g -1 ), and the wall thickness of the TiO 2 hollow structures could be easily controlled by adjusting the precursor concentration of TiF 4 . The photocatalytic activity experiment indicated that the prepared one-dimensional TiO 2 hollow structures, which could be readily separated from a slurry system after photocatalytic reaction, exhibited obvious photocatalytic activity for the photocatalytic degradation of methyl orange aqueous solution

  17. Study of the structural evolutions of crystalline tungsten oxide films prepared using hot-filament CVD

    International Nuclear Information System (INIS)

    Feng, P X; Wang, X P; Zhang, H X; Yang, B Q; Wang, Z B; Gonzalez-BerrIos, A; Morell, G; Weiner, B

    2007-01-01

    Structural evolutions of tungsten oxide(WO 3 ) samples on different substrates are studied using Raman spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, x-ray diffraction and x-ray photoelectron spectroscopy. The WO 3 samples are prepared using hot-filament CVD techniques. The focus of the study is on the evolutions of nano structures at different stages following deposition time. The experimental measurements reveal evolutions of the surface structures from uniform film to fractal-like structures, and eventually to nano particles, and crystalline structures from mono (0 1 0) crystalline thin film to polycrystalline thick film developments. The effect of high temperature on the nanostructured WO 3 is also investigated. Well-aligned nanoscale WO 3 rod arrays are obtained at a substrate temperature of up to 1400 deg. C. Further increasing the substrate temperature yields microscale crystalline WO 3 particles

  18. MnFe(PGe) compounds: Preparation, structural evolution, and magnetocaloric effects

    International Nuclear Information System (INIS)

    Yue Ming; Zhang Hong-Guo; Zhang Jiu-Xing; Liu Dan-Min

    2015-01-01

    The interdependences of preparation conditions, magnetic and crystal structures, and magnetocaloric effects (MCE) of the MnFePGe-based compounds are reviewed. Based upon those findings, a new method for the evaluation of the MCE in these compounds, based on differential scanning calorimetry (DSC), is proposed. The MnFePGe-based compounds are a group of magnetic refrigerants with giant magnetocaloric effect (GMCE), and as such, have drawn tremendous attention, especially due to their many advantages for practical applications. Structural evolution and phase transformation in the compounds as functions of temperature, pressure, and magnetic field are reported. Influences of preparation conditions upon the homogeneity of the compounds’ chemical composition and microstructure, both of which play a key role in the MCE and thermal hysteresis of the compounds, are introduced. Lastly, the origin of the “virgin effect” in the MnFePGe-based compounds is discussed. (paper)

  19. Strong composite films with layered structures prepared by casting silk fibroin-graphene oxide hydrogels

    Science.gov (United States)

    Huang, Liang; Li, Chun; Yuan, Wenjing; Shi, Gaoquan

    2013-04-01

    Composite films of graphene oxide (GO) sheets and silk fibroin (SF) with layered structures have been prepared by facile solution casting of SF-GO hydrogels. The as-prepared composite film containing 15% (by weight, wt%) of SF shows a high tensile strength of 221 +/- 16 MPa and a failure strain of 1.8 +/- 0.4%, which partially surpass those of natural nacre. Particularly, this composite film also has a high modulus of 17.2 +/- 1.9 GPa. The high mechanical properties of this composite film can be attributed to its high content of GO (85 wt%), compact layered structure and the strong hydrogen bonding interaction between SF chains and GO sheets.Composite films of graphene oxide (GO) sheets and silk fibroin (SF) with layered structures have been prepared by facile solution casting of SF-GO hydrogels. The as-prepared composite film containing 15% (by weight, wt%) of SF shows a high tensile strength of 221 +/- 16 MPa and a failure strain of 1.8 +/- 0.4%, which partially surpass those of natural nacre. Particularly, this composite film also has a high modulus of 17.2 +/- 1.9 GPa. The high mechanical properties of this composite film can be attributed to its high content of GO (85 wt%), compact layered structure and the strong hydrogen bonding interaction between SF chains and GO sheets. Electronic supplementary information (ESI) available: XPS spectrum of the SF-GO hybrid film, SEM images of lyophilized GO dispersion and the failure surface of GO film. See DOI: 10.1039/c3nr00196b

  20. Evaporation-based method for preparing gelatin foams with aligned tubular pore structures

    International Nuclear Information System (INIS)

    Frazier, Shane D.; Srubar, Wil V.

    2016-01-01

    Gelatin-based foams with aligned tubular pore structures were prepared via liquid-to-gas vaporization of tightly bound water in dehydrated gelatin hydrogels. This study elucidates the mechanism of the foaming process by investigating the secondary (i.e., helical) structure, molecular interactions, and water content of gelatin films before and after foaming using X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry and thermogravimetric analysis (TGA), respectively. Experimental data from gelatin samples prepared at various gelatin-to-water concentrations (5–30 wt.%) substantiate that resulting foam structures are similar in pore diameter (approximately 350 μm), shape, and density (0.05–0.22 g/cm"3) to those fabricated using conventional methods (e.g., freeze-drying). Helical structures were identified in the films but were not evident in the foamed samples after vaporization (~ 150 °C), suggesting that the primary foaming mechanism is governed by the vaporization of water that is tightly bound in secondary structures (i.e., helices, β-turns, β-sheets) that are present in dehydrated gelatin films. FTIR and TGA data show that the foaming process leads to more disorder and reduced hydrogen bonding to hydroxyl groups in gelatin and that no thermal degradation of gelatin occurs before or after foaming. - Highlights: • A new method is presented for fabricating gelatin foams with aligned, tubular pores. • Gelatin hydrogels were dehydrated then heated to 150 °C to induce foaming. • Vaporization of tightly (vs. loosely) bound water is the primary foaming mechanism • Foaming induced no thermal degradation but caused disorder in secondary structures • Foam microstructures are similar to those prepared using conventional methods.

  1. Evaporation-based method for preparing gelatin foams with aligned tubular pore structures

    Energy Technology Data Exchange (ETDEWEB)

    Frazier, Shane D.; Srubar, Wil V., E-mail: wsrubar@colorado.edu

    2016-05-01

    Gelatin-based foams with aligned tubular pore structures were prepared via liquid-to-gas vaporization of tightly bound water in dehydrated gelatin hydrogels. This study elucidates the mechanism of the foaming process by investigating the secondary (i.e., helical) structure, molecular interactions, and water content of gelatin films before and after foaming using X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry and thermogravimetric analysis (TGA), respectively. Experimental data from gelatin samples prepared at various gelatin-to-water concentrations (5–30 wt.%) substantiate that resulting foam structures are similar in pore diameter (approximately 350 μm), shape, and density (0.05–0.22 g/cm{sup 3}) to those fabricated using conventional methods (e.g., freeze-drying). Helical structures were identified in the films but were not evident in the foamed samples after vaporization (~ 150 °C), suggesting that the primary foaming mechanism is governed by the vaporization of water that is tightly bound in secondary structures (i.e., helices, β-turns, β-sheets) that are present in dehydrated gelatin films. FTIR and TGA data show that the foaming process leads to more disorder and reduced hydrogen bonding to hydroxyl groups in gelatin and that no thermal degradation of gelatin occurs before or after foaming. - Highlights: • A new method is presented for fabricating gelatin foams with aligned, tubular pores. • Gelatin hydrogels were dehydrated then heated to 150 °C to induce foaming. • Vaporization of tightly (vs. loosely) bound water is the primary foaming mechanism • Foaming induced no thermal degradation but caused disorder in secondary structures • Foam microstructures are similar to those prepared using conventional methods.

  2. Structural properties of pure and Fe-doped Yb films prepared by vapor condensation

    Energy Technology Data Exchange (ETDEWEB)

    Rojas-Ayala, C., E-mail: chachi@cbpf.br [Centro Brasileiro de Pesquisas Físicas, Rio de Janeiro 22290-180, RJ (Brazil); Facultad de Ciencias Físicas, Universidad Nacional Mayor de San Marcos, Lima, P.O.B. 14-149, Lima 14 (Peru); Passamani, E.C. [Departamento de Física, Universidade Federal do Espírito Santo, Vitória 29075-910, ES (Brazil); Suguihiro, N.M. [Centro Brasileiro de Pesquisas Físicas, Rio de Janeiro 22290-180, RJ (Brazil); Litterst, F.J. [Centro Brasileiro de Pesquisas Físicas, Rio de Janeiro 22290-180, RJ (Brazil); Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38106 Braunschweig (Germany); Baggio Saitovitch, E. [Centro Brasileiro de Pesquisas Físicas, Rio de Janeiro 22290-180, RJ (Brazil)

    2014-10-15

    Ytterbium and iron-doped ytterbium films were prepared by vapor quenching on Kapton substrates at room temperature. Structural characterization was performed by X-ray diffraction and transmission electron microscopy. The aim was to study the microstructure of pure and iron-doped films and thereby to understand the effects induced by iron incorporation. A coexistence of face centered cubic and hexagonal close packed-like structures was observed, the cubic-type structure being the dominant contribution. There is an apparent thickness dependence of the cubic/hexagonal relative ratios in the case of pure ytterbium. Iron-clusters induce a crystalline texture effect, but do not influence the cubic/hexagonal volume fraction. A schematic model is proposed for the microstructure of un-doped and iron-doped films including the cubic- and hexagonal-like structures, as well as the iron distribution in the ytterbium matrix. - Highlights: • Pure and Fe-doped Yb films have been prepared by vapor condensation. • Coexistence of fcc- and hcp-type structures was observed. • No oxide phases have been detected. • Fe-clustering does not affect the fcc/hcp ratio, but favors a crystalline texture. • A schematic model is proposed to describe microscopically the microstructure.

  3. Structure and stability of human hemoglobin microparticles prepared with a double emulsion technique.

    Science.gov (United States)

    Cedrati, N; Bonneaux, F; Labrude, P; Maincent, P

    1997-09-01

    Hemoglobin solutions can be used as blood substitutes but they present some disadvantages often due to their rapid removal from the bloodstream after injection. A possible way of overcoming this problem is to trap hemoglobin inside particles. This study deals with the preparation, structure and stability of poly(lactic acid) and ethylcellulose microparticles containing human hemoglobin obtained with a double emulsion technique. We investigated the manufacturing process of these particles in order to increase the encapsulation ratio of hemoglobin. For this purpose, some parameters involved in the procedure were optimized, such as hemoglobin concentration and duration of stirring: hemoglobin loading increases with its concentration in the preparation and well-defined stirring time avoids a leakage of hemoglobin. Hemoglobin concentration, surfactant concentration i.e. poly(vinylic alcohol), amounts of polymer and solvent (methylene chloride), duration and speed of stirring. The microparticles were prepared with satisfactory yields (60 to 73%). They were spherical and their mean size was lower than 200 microns. The functional properties of entrapped hemoglobin were studied. The encapsulation did not alter hemoglobin and the oxygen affinity of the hemoglobin remained unmodified (P50 about 13.9 mm Hg in a Bis-Tris buffer pH 7.4 at 37 degrees C). Moreover, only low levels of methemoglobin could be detected (less than 3%). Besides, about 90% of encapsulated hemoglobin could be released from microparticles, with a speed related to the internal structure of the particles. The prepared microparticles were stored during one month at +4 degrees C. No degradation of the particle structure occurred and the functional properties of hemoglobin were preserved. These particles could provide a potential source of oxygen in the field of biotechnologies but any application for a transfusional purpose would first require a drastic reduction in particle size.

  4. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    Energy Technology Data Exchange (ETDEWEB)

    Popova, Margarita, E-mail: mpopova@orgchem.bas.bg [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Szegedi, Agnes [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Mavrodinova, Vesselina [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Novak Tušar, Natasa [National Institute of Chemistry, Ljubljana (Slovenia); Mihály, Judith; Klébert, Szilvia [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Benbassat, Niko; Yoncheva, Krassimira [Faculty of Pharmacy, 2 Dunav Str., 1000 Sofia (Bulgaria)

    2014-11-15

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol.

  5. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    International Nuclear Information System (INIS)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-01-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol

  6. Stable preparations of tyrosine hydroxylase provide the solution structure of the full-length enzyme

    Science.gov (United States)

    Bezem, Maria T.; Baumann, Anne; Skjærven, Lars; Meyer, Romain; Kursula, Petri; Martinez, Aurora; Flydal, Marte I.

    2016-01-01

    Tyrosine hydroxylase (TH) catalyzes the rate-limiting step in the biosynthesis of catecholamine neurotransmitters. TH is a highly complex enzyme at mechanistic, structural, and regulatory levels, and the preparation of kinetically and conformationally stable enzyme for structural characterization has been challenging. Here, we report on improved protocols for purification of recombinant human TH isoform 1 (TH1), which provide large amounts of pure, stable, active TH1 with an intact N-terminus. TH1 purified through fusion with a His-tagged maltose-binding protein on amylose resin was representative of the iron-bound functional enzyme, showing high activity and stabilization by the natural feedback inhibitor dopamine. TH1 purified through fusion with a His-tagged ZZ domain on TALON is remarkably stable, as it was partially inhibited by resin-derived cobalt. This more stable enzyme preparation provided high-quality small-angle X-ray scattering (SAXS) data and reliable structural models of full-length tetrameric TH1. The SAXS-derived model reveals an elongated conformation (Dmax = 20 nm) for TH1, different arrangement of the catalytic domains compared with the crystal structure of truncated forms, and an N-terminal region with an unstructured tail that hosts the phosphorylation sites and a separated Ala-rich helical motif that may have a role in regulation of TH by interacting with binding partners. PMID:27462005

  7. SEM studies of the structure of the gels prepared from untreated and radiation modified potato starch

    International Nuclear Information System (INIS)

    Cieśla, Krystyna; Sartowska, Bożena; Królak, Edward

    2015-01-01

    Potato starch was irradiated with a 60 Co gamma rays using doses of 5, 10, 20 and 30 kGy. Gels containing ca. 9.1% of starch were prepared by heating the starch suspensions in the heating chamber stabilized at 100 °C. Four procedures were applied for preparation of the samples in regard to SEM studies and the ability to observe the radiation effect by SEM was assessed for each method. Differences were observed between the SEM images recorded for the non-irradiated samples prepared using all the methods, and those irradiated. Images of the non-irradiated gels indicate generally a honey-comb structure, while smooth areas but with oriented fractures has appeared after irradiation. Modification of gel structure corresponds to the applied dose. The results were related to the process of gel formation (as observed by means of the hot stage microscope) to decrease in swelling power of the irradiated starch and to decreased viscosity of the resulting gels. It can be concluded that the differences in structural properties of gels shown by SEM result probably due to the better homogenization of the gels formed after radiation induced degradation. - Highlights: • Four procedures of the preservation of starch gels for SEM studies were applied. • The ability to observe the radiation effect by SEM was assessed for each method. • Dose dependent changes in the gel structure were discovered. • It was related to decrease in the swelling power and decreased viscosity of the gels. • A hot-stage microscope was applied in order to follow the gelatinization process

  8. Structure investigations on zirconium phosphate preparates by means of DTA, ETA, and TG

    International Nuclear Information System (INIS)

    Herbell, J.D.; Specht, S.; Born, H.J.

    1976-01-01

    The simultanous DTA, ETA and TG inorganic ion exchanger based on zirconium phosphate enables the clear interpretation of the effects occuring. In particular it can be seen that the fast transition in amorphous preparates at high temperature of a badly defined form of pyrophosphate into the cubic crystalline substances, however a measurable energy release by means of DTA is not observed due to the slight mobility of the atoms in the crystal lattice. This effect on the other hand may be seen using ETA. In addition, an exothermal reaction occuring in some preparates, especially in cation charged ones, was traced back to the forming of part-crystalline structures which could be especially fast and sensitively characterized using DTA. (orig.) [de

  9. Preparation and structural characterization of the thermoluminescent material CaSO4: Dy

    International Nuclear Information System (INIS)

    Sanchez R, A.; Azorin, J.; Gonzalez M, P.R.; Rivera, T.

    2005-01-01

    The grade of crystallinity of a material is important so that the one is presented the thermoluminescence phenomenon; for what is necessary to study those structural characteristic of a TL material and to correlate them with its TL response when being irradiated with ionizing radiation. The calcium sulfate activated with Dysprosium (CaSO 4 : Dy) it is a material that has demonstrated its efficiency in the dosimetry of the ionizing radiation for the thermoluminescence method. In this work the structural characterization of this prepared material for the recrystallization method by means of the evaporation of the solvent and their relationship with their TL response is presented. The results showed that the best material to be used in thermoluminescent dosimetry presents a crystalline structure in orthorhombic phase and a particle size in the interval of 80 μm to 200 μm. (Author)

  10. Preparation and study on the structure of keratin/PVA membrane containing wool fibers

    Science.gov (United States)

    Wu, Min; Shen, Shuming; Yang, Xuhong; Tang, Rencheng

    2017-10-01

    The urea / sodium sulfide / sodium dodecyl sulfate (SDS) method was used to dissolve the wool in this study. Then the Wool fiber/keratin/PVA composites with different proportions were prepared, and the surface morphology, molecular structure, mechanical property of the composite films and the influence of the proportions on their structure and properties were studied. The results showed that, there are α-helix structure, β-sheet and random coil conformations in the pure keratin film, as well as in the wool fiber. Compared with wool fiber, the crystallinity of keratin decreased. PVA can obviously improve the mechanical property of the blended film. When the blended ratio of keratin/PVA is 20/80, the mechanical property of the blended film is greatly improved. The composite films with 8%-16% of wool fibers have better flexibility than those without wool fibers.

  11. Core/shell structured ZnO/SiO2 nanoparticles: Preparation, characterization and photocatalytic property

    International Nuclear Information System (INIS)

    Zhai Jing; Tao Xia; Pu Yuan; Zeng Xiaofei; Chen Jianfeng

    2010-01-01

    ZnO nanoparticles were prepared by a simple chemical synthesis route. Subsequently, SiO 2 layers were successfully coated onto the surface of ZnO nanoparticles to modify the photocatalytic activity in acidic or alkaline solutions. The obtained particles were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectrometry (EDS) and zeta potential. It was found that ultrafine core/shell structured ZnO/SiO 2 nanoparticles were successfully obtained. The photocatalytic performance of ZnO/SiO 2 core/shell structured nanoparticles in Rhodamine B aqueous solution at varied pH value were also investigated. Compared with uncoated ZnO nanoparticles, core/shell structured ZnO/SiO 2 nanoparticles with thinner SiO 2 shell possess improved stability and relatively better photocatalytic activity in acidic or alkaline solutions, which would broaden its potential application in pollutant treatment.

  12. Optical and structural properties of colloidal zirconia nanoparticles prepared by arc discharge in liquid

    Science.gov (United States)

    Peymani forooshani, Reza; Poursalehi, Reza; Yourdkhani, Amin

    2018-01-01

    Zirconia is one of the important ceramic materials with unique properties such as high melting point, high ionic conductivity, high mechanical properties and low thermal conductivity. Therefore, zirconia is one of the useful materials in refractories, thermal barriers, cutting tools, oxygen sensors electrolytes, catalysis, catalyst supports and solid oxide fuel cells. Recently, direct current (DC) arc discharge is extensively employed to synthesis of metal oxide nanostructures in liquid environments. The aim of this work is the synthesis of colloidal zirconia nanoparticles by DC arc discharge method in water as a medium. Arc discharge was ignited between two pure zirconium electrodes in water. Optical and structural properties of prepared colloidal nanoparticles were investigated. Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and UV-visible spectroscopy, were employed for characterization of particle size, morphology, crystal structure and optical properties, respectively. SEM images demonstrate that the nanoparticles are spherical in shape with an average size lower than 38 nm. The XRD patterns of the nanoparticles were consistent with tetragonal and monoclinic zirconia crystal structures. The optical transmission spectra of the colloidal solution show optical characteristic of zirconia nanoparticles as a wide band gap semiconductor with no absorption peak in visible wavelength with the considerable amount of oxygen deficiency. Oxidation of colloidal nanoparticles in water could be explained via reaction with either dissociated oxygen from water in hot plasma region or with dissolved oxygen in water. The results provide a simple and flexible method for preparation of zirconia nanoparticles with a capability of mass production without environmental footprints.

  13. Porous poly(vinyl alcohol)/sepiolite bone scaffolds: Preparation, structure and mechanical properties

    International Nuclear Information System (INIS)

    Killeen, Derek; Frydrych, Martin; Chen Biqiong

    2012-01-01

    Porous poly(vinyl alcohol) (PVA)/sepiolite nanocomposite scaffolds containing 0–10 wt.% sepiolite were prepared by freeze-drying and thermally crosslinked with poly(arylic acid). The microstructure of the obtained scaffolds was characterised by scanning electron microscopy and micro-computed tomography, which showed a ribbon and ladder like interconnected structure. The incorporation of sepiolite increased the mean pore size and porosity of the PVA scaffold as well as the degree of anisotropy due to its fibrous structure. The tensile strength, modulus and energy at break of the PVA solid material that constructed the scaffold were found to improve with additions of sepiolite by up to 104%, 331% and 22% for 6 wt.% clay. Such enhancements were attributed to the strong interactions between the PVA and sepiolite, the good dispersion of sepiolite nanofibres in the matrix and the intrinsic properties of the nanofibres. However, the tensile properties of the PVA scaffold deteriorated in the presence of sepiolite because of the higher porosity, pore size and degree of anisotropy. The PVA/sepiolite nanocomposite scaffold containing 6 wt.% sepiolite was characterised by an interconnected structure, a porosity of 89.5% and a mean pore size of 79 μm and exhibited a tensile strength of 0.44 MPa and modulus of 14.9 MPa, which demonstrates potential for this type of materials to be further developed as bone scaffolds. - Highlights: ► Novel PAA-crosslinked PVA/sepiolite nanocomposite scaffolds were prepared. ► They were highly porous with interconnected structures and exhibited good mechanical properties. ► The effects of sepiolite nanofibres on structure and properties of the scaffolds were investigated. ► Sepiolite nanofibres improved the mechanical properties of the solid material significantly.

  14. Structure and hardness of a hard metal alloy prepared with a WC powder synthesized at low temperature

    Energy Technology Data Exchange (ETDEWEB)

    Costa, F.A. da [Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais, UFRN, Campus Universitario, 59072-970 Natal, RN (Brazil)], E-mail: francineac@yahoo.com; Medeiros, F.F.P. de [Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais, UFRN, Campus Universitario, 59072-970 Natal, RN (Brazil); Silva, A.G.P. da [Laboratorio de Materiais Avancados, UENF, 28015-620 Campos de Goytacazes, RJ (Brazil); Gomes, U.U. [Departamento de Fisica Teorica e Experimental, UFRN, Campus Universitario, 59072-970 Natal, RN (Brazil); Filgueira, M. [Laboratorio de Materiais Avancados, UENF, 28015-620 Campos de Goytacazes, RJ (Brazil); Souza, C.P. de [Laboratorio de Termodinamica e Reatores, UFRN, Campus Universitario, 59072-970 Natal, RN (Brazil)

    2008-06-25

    The structure and hardness of a WC-10 wt% Co alloy prepared with an experimental WC powder are compared with those of another alloy of the same composition produced under the same conditions and prepared with a commercial WC powder. The experimental WC powder was synthesized by a gas-solid reaction between APT and methane at low temperature and the commercial WC powder was conventionally produced by a solid-solid reaction between tungsten and carbon black. WC-10 wt% Co alloys with the two powders were prepared under the same conditions of milling and sintering. The structure of the sample prepared with the experimental WC powder is homogeneous and coarse grained. The structure of the sample prepared with the commercial powder is heterogeneous. Furthermore the size and shape of the WC grains are significantly different.

  15. Preparation of novel polyamine-type chelating resin with hyperbranched structures and its adsorption performance

    Science.gov (United States)

    Zhao, Wei; Wang, Huan; Li, Yuhong; Li, Chenxi

    2018-01-01

    This paper explored the method of combining atom transfer radical polymerization (ATRP) technology and hyperbranched polymer principle to prepare the high capacity chelating resin. First, surface-initiated atom transfer radical polymerization (SI-ATRP) method was used to graft glycidyl methacrylate (GMA) on chloromethylated cross-linked styrene-divinylbenzene resin, and then the novel polyamine chelating resin with a kind of hyperbranched structure was prepared through the amination reaction between amino group of (2-aminoethyl) triamine and epoxy group in GMA. This resin had a selective effect on As(V) and Cr(VI) at a relatively low pH and can be used for the disposal of waste water containing As(V) and Cr(VI). It had a relatively strong adsorption effect on Cu(II), Pb(II), Cd(II) and Cr(III) and can be used for the disposal of heavy metal ion waste water. The finding was that, the adsorption capacity of resin on the studied heavy metal ions was higher than that of the chelating resin synthesized by traditional technology and also higher than that of the resin modified by ATRP technology and bifunctional chelator, indicating that the combination of ATRP and hyperbranched polymer concept is an effective method to prepare chelating resin with high capacity. PMID:29515875

  16. Preparation of novel polyamine-type chelating resin with hyperbranched structures and its adsorption performance

    Science.gov (United States)

    Chen, Youning; Zhao, Wei; Wang, Huan; Li, Yuhong; Li, Chenxi

    2018-02-01

    This paper explored the method of combining atom transfer radical polymerization (ATRP) technology and hyperbranched polymer principle to prepare the high capacity chelating resin. First, surface-initiated atom transfer radical polymerization (SI-ATRP) method was used to graft glycidyl methacrylate (GMA) on chloromethylated cross-linked styrene-divinylbenzene resin, and then the novel polyamine chelating resin with a kind of hyperbranched structure was prepared through the amination reaction between amino group of (2-aminoethyl) triamine and epoxy group in GMA. This resin had a selective effect on As(V) and Cr(VI) at a relatively low pH and can be used for the disposal of waste water containing As(V) and Cr(VI). It had a relatively strong adsorption effect on Cu(II), Pb(II), Cd(II) and Cr(III) and can be used for the disposal of heavy metal ion waste water. The finding was that, the adsorption capacity of resin on the studied heavy metal ions was higher than that of the chelating resin synthesized by traditional technology and also higher than that of the resin modified by ATRP technology and bifunctional chelator, indicating that the combination of ATRP and hyperbranched polymer concept is an effective method to prepare chelating resin with high capacity.

  17. Super-hydrophobic nickel films with micro-nano hierarchical structure prepared by electrodeposition

    International Nuclear Information System (INIS)

    Hang Tao; Hu Anmin; Ling Huiqin; Li Ming; Mao Dali

    2010-01-01

    Super-hydrophobic nickel films were prepared by a simple and low cost electrodepositing method. The surface morphologies of the films characterized by scanning electronic microscope exhibit hierarchical structure with micro-nanocones array, which can be responsible for their super-hydrophobic characteristic (water contact angle over 150 o ) without chemical modification. The wettability of the film can be varied from super-hydrophobic (water contact angle 154 o ) to relatively hydrophilic (water contact angle 87 o ) by controlling the size of the micro-nanocones. The mechanism of the hydrophobic characteristic of nickel films with this unique structure was illustrated by several models. Such micro-nanostructure and its special wettability are expected to be applied in the practical industry.

  18. Preparation and structural study of LaMnO3 magnetic material

    International Nuclear Information System (INIS)

    Moreno, L.C.; Valencia, J.S.; Landinez Tellez, D.A.; Arbey Rodriguez M, J.; Martinez, M.L.; Roa-Rojas, J.; Fajardo, F.

    2008-01-01

    We report the crystallographic parameters of LaMnO 3 obtained from X-ray diffraction data and electronic properties predictions using the density functional theory (DFT). LaMnO 3 was prepared by the citrate precursor method (CPM). The initial solution was 0.1 M of each cation and the citrate nitrate relation was one. The solution was dried at 373 K; the yielded foam was annealed at 873 K and then was characterized by X-ray diffraction. Diffraction peaks show that the space group is R-3c (no. 167) with a=b =5.523 A and c=13.324 A (rhombohedrally distorted perovskite). Structural results of the Rietveld method have a matching of 97% with that obtained from the Structure Prediction Diagnostic Software. DFT calculation reveals a half-metallic character and its magnetic moment is about 2.0 μ B

  19. Structural and electrical properties of epitaxial Si layers prepared by E-beam evaporation

    Energy Technology Data Exchange (ETDEWEB)

    Dogan, P. [Hahn-Meitner-Institut Berlin, Kekulestr. 5, 12489 Berlin (Germany)], E-mail: pinar.dogan@hmi.de; Rudigier, E.; Fenske, F.; Lee, K.Y.; Gorka, B.; Rau, B.; Conrad, E.; Gall, S. [Hahn-Meitner-Institut Berlin, Kekulestr. 5, 12489 Berlin (Germany)

    2008-08-30

    In this work, we present structural and electrical properties of thin Si films which are homoepitaxially grown at low substrate temperatures (T{sub s} 450-700 deg. C) by high-rate electron beam evaporation. As substrates, monocrystalline Si wafers with (100) and (111) orientations and polycrystalline Si (poly-Si) seed layers on glass were used. Applying Secco etching, films grown on Si(111) wafers exhibit a decreasing etch pit density with increasing T{sub s}. The best structural quality of the films was obtained on Si(100) wafers. Defect etching on epitaxially grown poly-Si absorbers reveal regions with different crystalline quality. Solar cells have been prepared on both wafers and seed layers. Applying Rapid Thermal Annealing (RTA) and Hydrogen plasma passivation an open circuit voltage of 570 mV for wafer based and 346 mV for seed layer based solar cells have been reached.

  20. Preparing a Health Care White Paper: Providing Structure to the Writing Process.

    Science.gov (United States)

    Rotarius, Timothy; Rotarius, Velmarie

    2016-01-01

    Health care leaders operate in a very complex and turbulent business environment. Both government regulations and market forces are very active in the industry. Thus, health care managers have many multifaceted and, sometimes, contradictory expectations placed upon them and their organizations. To ensure professional accountability, health care executives often join professional associations and strive for licenses and certifications that are intended to place the professional above the rest. One important avenue to achieve various licensing and certification accomplishments involves writing a white paper about a specific topic of interest to the industry and organization. Presented herein are structural processes that facilitate the creation and preparation of a health care white paper. Both conceptual and empirical structures of white papers are presented, with the similarities and the differences between conceptual and empirical papers highlighted.

  1. Polarized Raman study on the lattice structure of BiFeO3 films prepared by pulsed laser deposition

    KAUST Repository

    Yang, Yang; Yao, Yingbang; Zhang, Q.; Zhang, Xixiang

    2014-01-01

    Polarized Raman spectroscopy was used to study the lattice structure of BiFeO3 films on different substrates prepared by pulsed laser deposition. Interestingly, the Raman spectra of BiFeO3 films exhibit distinct polarization dependences

  2. Structural characterization of nanocrystalline cadmium sulphide powder prepared by solvent evaporation technique

    Science.gov (United States)

    Pandya, Samir; Tandel, Digisha; Chodavadiya, Nisarg

    2018-05-01

    CdS is one of the most important compounds in the II-VI group of semiconductor. There are numerous applications of CdS in the form of nanoparticles and nanocrystalline. Semiconductors nanoparticles (also known as quantum dots), belong to state of matter in the transition region between molecules and solids, have attracted a great deal of attention because of their unique electrical and optical properties, compared to bulk materials. In the field of optoelectronic, nanocrystalline form utilizes mostly in the field of catalysis and fluid technology. Considering these observations, presented work had been carried out, i.e. based on the nanocrystalline material preparation. In the present work CdS nano-crystalline powder was synthesized by a simple and cost effective chemical technique to grow cadmium sulphide (CdS) nanoparticles at 200 °C with different concentrations of cadmium. The synthesis parameters were optimized. The synthesized powder was structurally characterized by X-ray diffraction and particle size analyzer. In the XRD analysis, Micro-structural parameters such as lattice strain, dislocation density and crystallite size were analysed. The broadened diffraction peaks indicated nanocrystalline particles of the film material. In addition to that the size of the prepared particles was analyzed by particle size analyzer. The results show the average size of CdS particles ranging from 80 to 100 nm. The overall conclusion of the work can be very useful in the synthesis of nanocrystalline CdS powder.

  3. A novel approach to preparing magnetic protein microspheres with core-shell structure

    International Nuclear Information System (INIS)

    Jiang Wei; Sun Zhendong; Li Fengsheng; Chen Kai; Liu Tianyu; Liu Jialing; Zhou Tianle; Guo Rui

    2011-01-01

    Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe 3 O 4 cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe 3 O 4 nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail. - Research Highlights: → Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method.→ The microspheres are composed of the oleic acid and undecylenic acid modified Fe 3 O 4 cores and coated with globular bovine serum albumin (BSA).→ 57.8 wt% of approximately 10 nm superparamagnetic Fe 3 O 4 nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides the abundant functional groups.

  4. A novel approach to preparing magnetic protein microspheres with core-shell structure

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Wei, E-mail: climentjw@126.co [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Sun Zhendong; Li Fengsheng [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Chen Kai; Liu Tianyu; Liu Jialing [Department of Physics, Nanjing University of Science and Technology, Nanjing 210094 (China); Zhou Tianle [Department of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Guo Rui [Department of Mechanical Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China)

    2011-03-15

    Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe{sub 3}O{sub 4} cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe{sub 3}O{sub 4} nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail. - Research Highlights: Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe{sub 3}O{sub 4} cores and coated with globular bovine serum albumin (BSA). 57.8 wt% of approximately 10 nm superparamagnetic Fe{sub 3}O{sub 4} nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides the abundant functional groups.

  5. Structure of hybrid organic-inorganic sols for the preparation of hydrothermally stable membranes

    Energy Technology Data Exchange (ETDEWEB)

    Castricum, H.L.; Sah, A; Blank, D.H.A.; Ten Elshof, J.E. [Inorganic Materials Science, MESA Institute for Nanotechnology, University of Twente, P.O. Box 217, 7500 AE Enschede (Netherlands); Geenevasen, J.A.J. [Van ' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018 WV Amsterdam (Netherlands); Kreiter, R.; Vente, J.F. [ECN Energy Efficiency in the Industry, Petten (Netherlands)

    2008-06-15

    A procedure for the preparation of hybrid sols for the synthesis of organic-inorganic microporous materials and thin film membranes is reported. We describe silane reactivity and sol structure for acid-catalysed colloidal sols from mixtures of either tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES), or bis(triethoxysilyl)ethane (BTESE) and MTES. Early-stage hydrolysis and condensation rates of the individual silane precursors were followed with 29Si liquid NMR and structural characteristics of more developed sols were studied with Dynamic Light Scattering. Condensation was found to proceed at more or less similar rates for the different precursors. Homogeneously mixed hybrid colloids can therefore be formed from precursor mixtures. The conditions of preparation under which clear sols with low viscosity could be formed from BTESE/MTES were determined. These sols were synthesised at moderate water/silane and acid/silane ratios and could be applied for the coating of defect-free microporous membranes for molecular separations under hydrothermal conditions.

  6. The performance of double layer structure membrane prepared from flowing coagulant

    Science.gov (United States)

    Mieow Kee, Chan; Xeng, Anthony Leong Chan; Regal, Sasiskala; Singh, Balvinder; Raoo, Preeshaath; Koon Eu, Yap; Sok Choo, Ng

    2017-12-01

    Membrane with double layer structure is favourable as it exhibits smooth surface and macrovoids free structure. However, its’ performance in terms of permeability, porosity and strength has not been studied thoroughly. Additionally, the effect of flowing coagulant on the formation of double layer membrane has not been reported. Thus, the objective of this study is to investigate the performance of double layer membranes, which were prepared using flowing coagulant. Results showed that when the coagulant flow changed from laminar to turbulent, the pure water permeation of the membrane increased. It was due to the higher porosity in the membrane, which prepared by turbulent flow (CA-Turbulent) compared to the membrane which fabricated under laminar condition (CA-Laminar). This can be explained by the rapid solvent-coagulant exchange rate between the polymer solution and the turbulent coagulant. In term of strength, the tensile strength of the CA-Turbulent was ~32 MPa, which was 100% higher compared to CA-Laminar. This may due to the presence of large amount of nodules on its surface, which reduced the surface integrity. In conclusion, flowing coagulant altered the membrane properties and adopting turbulent coagulant flow in membrane fabrication would improve the porosity, surface roughness and the strength of the membrane.

  7. A survey of the mechanical properties of concrete for structural purposes prepared on construction sites

    Directory of Open Access Journals (Sweden)

    R. R. J. RIBEIRO

    Full Text Available Abstract This paper aims to study the concrete dosage conditions for structural purposes in construction sitesl, and the impacts of non-compliance of structural concrete for structural safety, having as study case the city of Angicos / RN. Were analyzed the dynamic elasticity modulus, static elasticity modulus and the compressive strength of concrete samples. Was conducted to collect the survey data, a field research aiming to gather information about dosage of concrete used in the works, as well as the collection of cylindrical specimens of 150 mm diameter by 300 mm of height, prepared according to practice of those professionals. The study indicated a clear necessity to reflection on the subject, since there is no concern, or even, a lack of knowledge by the interviewed professionals regarding the care and procedures necessary for the production of concrete with satisfactory quality, once at least 50% of evaluated construction sites presented compressive strength lower than 20 MPa, minimal strength to structural concrete, as recommended by ABNT-NBR 6118:2014.

  8. Preparation of mesoporous carbon nitride structure by the dealloying of Ni/a-CN nanocomposite films

    Science.gov (United States)

    Zhou, Han; Shen, Yongqing; Huang, Jie; Liao, Bin; Wu, Xianying; Zhang, Xu

    2018-05-01

    The preparation of mesoporous carbon nitride (p-CN) structure by the selective dealloying process of Ni/a-CN nanocomposite films is investigated. The composition and structure of the Ni/a-CN nanocomposite films and porous carbon nitride (p-CN) films are determined by scan electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Phase separated structure including nickel carbide phase and the surrounding amorphous carbon nitride (a-CN) matrix are detected for the as-deposited films. Though the bulk diffusion is introduced in the film during the annealing process, the grain sizes for the post-annealed films are around 10 nm and change little comparing with the ones of the as-deposited films, which is associated with the thermostability of the CN surrounding in the film. The p-CN skeleton with its pore size around 12.5 nm is formed by etching the post-annealed films, indicative of the stability of the phase separated structure during the annealing process.

  9. Structural characteristics and properties of the regenerated silk fibroin prepared from formic acid.

    Science.gov (United States)

    Um, I C; Kweon, H Y; Park, Y H; Hudson, S

    2001-08-20

    Structural characteristics and thermal and solution properties of the regenerated silk fibroin (SF) prepared from formic acid (FU) were compared with those of SF from water (AU). According to the turbidity and shear viscosity measurement, SF formic acid solution was stable and transparent, no molecular aggregations occurred. The sample FU exhibited the beta-sheet structure, while AU random coil conformation using Fourier transform infrared (FTIR), X-ray diffraction (XRD), and differential scanning calorimetry. The effects of methanol treatment on samples were also examined. According to the measurement of crystallinity (XRD) and crystallinity index (FTIR), the concept of long/short-range ordered structure formation was proposed. Long-range ordered crystallites are predominantly formed for methanol treated SF film while SF film cast from formic acid favors the formation of short-range ordered structure. The relaxation temperatures of SF films measured by dynamic thermomechanical analysis supported the above mechanism due to the sensitivity of relaxation temperature on the short-range order.

  10. Structural and Optical Properties of Eu Doped ZnO Nanorods prepared by Pulsed Laser Deposition

    KAUST Repository

    Alarawi, Abeer

    2014-06-23

    Nano structured wide band gap semiconductors have attracted attention of many researchers due to their potential electronic and optoelectronic applications. In this thesis, we report successful synthesis of well aligned Eu doped ZnO nano-rods prepared, for the first time to our knowledge, by pulsed laser deposition (PLD) without any catalyst. X-ray diffraction (XRD) patterns shows that these Eu doped ZnO nanorods are grown along the c-axis of ZnO wurtzite structure. We have studied the effect of the PLD growth conditions on forming vertically aligned Eu doped ZnO nanorods. The structural properties of the material are investigated using a -scanning electron microscope (SEM). The PLD parameters must be carefully controlled in order to obtain c-axis oriented ZnO nanorods on sapphire substrates, without the use of any catalyst. The experiments conducted in order to identify the optimal growth conditions confirmed that, by adjusting the target-substrate distance, substrate temperature, laser energy and deposition duration, the nanorod size could be successfully controlled. Most importantly, the results indicated that the photoluminescence (PL) properties reflect the quality of the ZnO nanorods. These parameters can change the material’s structure from one-dimensional to two-dimensional however the laser energy and frequency affect the size and the height of the nanorods; the xygen pressure changes the density of the nanorods.

  11. Intragranular cellular segregation network structure strengthening 316L stainless steel prepared by selective laser melting

    Energy Technology Data Exchange (ETDEWEB)

    Zhong, Yuan; Liu, Leifeng [Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University, 10691 Stockholm (Sweden); Wikman, Stefan [Fusion for Energy, Torres Diagonal Litoral B3, Josep Pla 2, 08019 Barcelona (Spain); Cui, Daqing [Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University, 10691 Stockholm (Sweden); Shen, Zhijian, E-mail: shen@mmk.su.se [Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University, 10691 Stockholm (Sweden)

    2016-03-15

    A feasibility study was performed to fabricate ITER In-Vessel components by Selective Laser Melting (SLM) supported by Fusion for Energy (F4E). Almost fully dense 316L stainless steel (SS316L) components were prepared from gas-atomized powder and with optimized SLM processing parameters. Tensile tests and Charpy-V tests were carried out at 22 °C and 250 °C and the results showed that SLM SS316L fulfill the RCC-MR code. Microstructure characterization reveals the presence of hierarchical macro-, micro- and nano-structures in as-built samples that were very different from SS316L microstructures prepared by other established methods. The formation of a characteristic intragranular cellular segregation network microstructure appears to contribute to the increase of yield strength without losing ductility. Silicon oxide nano-inclusions were formed during the SLM process that generated a micro-hardness fluctuation in the building direction. The combined influence of a cellular microstructure and the nano-inclusions constraints the size of ductile dimples to nano-scale. The crack propagation is hindered by a pinning effect that improves the defect-tolerance of the SLM SS316L. This work proves that it was possible to manufacture SS316L with properties suitable for ITER First Wall panels. Further studies on irradiation properties of SLM SS316L and manufacturing of larger real-size components are needed. - Highlights: • The mechanical properties of SS316L made by selective laser melting fulfill RCC-MR. • SLM SS316L consists hierarchical structures of high heterogeneity. • Silicon rich oxide nano-inclusions are formed unexpectedly during SLM process. • Cellular structure and oxide nano-inclusions strengthen SLM SS316L.

  12. In vitro biological characterization of macroporous 3D Bonelike structures prepared through a 3D machining technique

    International Nuclear Information System (INIS)

    Laranjeira, M.S.; Dias, A.G.; Santos, J.D.; Fernandes, M.H.

    2009-01-01

    3D bioactive macroporous structures were prepared using a 3D machining technique. A virtual 3D structure model was created and a computer numerically controlled (CNC) milling device machined Bonelike samples. The resulting structures showed a reproducible macroporosity and interconnective structure. Macropores size after sintering was approximately 2000 μm. In vitro testing using human bone marrow stroma showed that cells were able to adhere and proliferate on 3D structures surface and migrate into all macropore channels. In addition, these cells were able to differentiate, since mineralized globular structures associated with cell layer were identified. Results obtained showed that 3D structures of Bonelike successfully allow cell migration into all macropores, and allow human bone marrow stromal cells to proliferate and differentiate. This innovative technique may be considered as a step-forward preparation for 3D interconnective macroporous structures that allow bone ingrowth while maintaining mechanical integrity.

  13. Structure and superconducting properties of Nb3Ge prepared in a UHV system

    International Nuclear Information System (INIS)

    Habermeier, H.U.; Stuttgart Univ.

    1981-01-01

    Nb 3 Ge films are prepared by coevaporation of Nb and Ge under well defined and controlled conditions. The formation of the A15 Nb 3 Ge phase is studied by varying the processing parameters - composition, deposition temperature, and impurity gas background - systematically. Single phase samples with Tsub(c) onsets as high as 21.5 K and lattice parameters of 0.5148 nm only be obtained in an environment with no added impurities and a Ge concentration of 23.8 at%. Oxygen as impurity gas enhances Tsub(c) slightly in samples of the optimal composition, whereas hydrogen as impurity gas does not affect the formation and the Tsub(c) of the A15 phase at all. The structure, (lattice parameters, grain sizes, and phases present) and the superconducting properties (Tsub(c), Hsub(c2)(0)) of the samples show a systematic correlation of the preparation parameters and the physical properties. The experimental results are explained qualitatively within the frame of the linear chain model of A15 superconductors combined with the introduction of anti-site defects. (author)

  14. Structural and adsorptive properties of activated carbons prepared by carbonization and activation of resins.

    Science.gov (United States)

    Leboda, R; Skubiszewska-Zieba, J; Tomaszewski, W; Gun'ko, V M

    2003-07-15

    Four activated carbons (S1-S4) possessing different structural characteristics were prepared by carbonization of commercial resins (used for ion exchange) and subsequent activation. Their textural parameters were determined on the basis of nitrogen adsorption-desorption at 77.4 K, analyzed by applying several local and overall adsorption isotherm equations. The nature of carbon surface functionalities was analyzed by FTIR spectroscopy. The GC and solid-phase extraction (SPE) techniques were applied to study the influence of the texture of carbonaceous materials on their adsorptive properties. The adsorption efficiency of synthesized carbons with respect to alkylhalides used as probe compounds in the GC measurements varied over a range from 28% (C(2)H(3)Cl(3)/S2) to 85% (CHBr(3)/S1) depending on the type of adsorbates and adsorbents. The concentrating efficiency of these carbons in SPE of explosive materials changed over a larger range from 12% (trinitroglycerin/S4) and 13% (trinitrotoluene/S2) up to 100% (octogen/S1). Active carbon prepared using Zerolite 225x8 as a precursor demonstrated better results than other carbons in two types of adsorption with average values of the efficiency of 75.4% for explosives and 60.8% for alkylhalides.

  15. Structure and Properties of Multiwall Carbon Nanotubes/Polystyrene Composites Prepared via Coagulation Precipitation Technique

    Directory of Open Access Journals (Sweden)

    I. N. Mazov

    2011-01-01

    Full Text Available Coagulation technique was applied for preparation of multiwall carbon nanotube- (MWNT-containing polystyrene (PSt composite materials with different MWNT loading (0.5–10 wt.%. Scanning and transmission electron microscopies were used for investigation of the morphology and structure of produced composites. It was shown that synthesis of MWNT/PSt composites using coagulation technique allows one to obtain high dispersion degree of MWNT in the polymer matrix. According to microscopy data, composite powder consists of the polystyrene matrix forming spherical particles with diameter ca. 100–200 nm, and the surface of MWNT is strongly wetted by the polymer forming thin layer with 5–10 nm thickness. Electrical conductivity of MWNT/PSt composites was investigated using a four-probe technique. Observed electrical percolation threshold of composite materials is near to 10 wt.%, mainly due to the insulating polymer layer deposited on the surface of nanotubes. Electromagnetic response of prepared materials was investigated in broadband region (0.01–4 and 26–36 GHz. It was found that MWNT/PSt composites are almost radiotransparent for low frequency region and possess high absorbance of EM radiation at higher frequencies.

  16. Intragranular cellular segregation network structure strengthening 316L stainless steel prepared by selective laser melting

    Science.gov (United States)

    Zhong, Yuan; Liu, Leifeng; Wikman, Stefan; Cui, Daqing; Shen, Zhijian

    2016-03-01

    A feasibility study was performed to fabricate ITER In-Vessel components by Selective Laser Melting (SLM) supported by Fusion for Energy (F4E). Almost fully dense 316L stainless steel (SS316L) components were prepared from gas-atomized powder and with optimized SLM processing parameters. Tensile tests and Charpy-V tests were carried out at 22 °C and 250 °C and the results showed that SLM SS316L fulfill the RCC-MR code. Microstructure characterization reveals the presence of hierarchical macro-, micro- and nano-structures in as-built samples that were very different from SS316L microstructures prepared by other established methods. The formation of a characteristic intragranular cellular segregation network microstructure appears to contribute to the increase of yield strength without losing ductility. Silicon oxide nano-inclusions were formed during the SLM process that generated a micro-hardness fluctuation in the building direction. The combined influence of a cellular microstructure and the nano-inclusions constraints the size of ductile dimples to nano-scale. The crack propagation is hindered by a pinning effect that improves the defect-tolerance of the SLM SS316L. This work proves that it was possible to manufacture SS316L with properties suitable for ITER First Wall panels. Further studies on irradiation properties of SLM SS316L and manufacturing of larger real-size components are needed.

  17. A Review of the Structure, Preparation, and Application of NLCs, PNPs, and PLNs

    Directory of Open Access Journals (Sweden)

    Qianwen Li

    2017-05-01

    Full Text Available Nanostructured lipid carriers (NLCs are modified solid lipid nanoparticles (SLNs that retain the characteristics of the SLN, improve drug stability and loading capacity, and prevent drug leakage. Polymer nanoparticles (PNPs are an important component of drug delivery. These nanoparticles can effectively direct drug delivery to specific targets and improve drug stability and controlled drug release. Lipid–polymer nanoparticles (PLNs, a new type of carrier that combines liposomes and polymers, have been employed in recent years. These nanoparticles possess the complementary advantages of PNPs and liposomes. A PLN is composed of a core–shell structure; the polymer core provides a stable structure, and the phospholipid shell offers good biocompatibility. As such, the two components increase the drug encapsulation efficiency rate, facilitate surface modification, and prevent leakage of water-soluble drugs. Hence, we have reviewed the current state of development for the NLCs’, PNPs’, and PLNs’ structures, preparation, and applications over the past five years, to provide the basis for further study on a controlled release drug delivery system.

  18. A Review of the Structure, Preparation, and Application of NLCs, PNPs, and PLNs.

    Science.gov (United States)

    Li, Qianwen; Cai, Tiange; Huang, Yinghong; Xia, Xi; Cole, Susan P C; Cai, Yu

    2017-05-27

    Nanostructured lipid carriers (NLCs) are modified solid lipid nanoparticles (SLNs) that retain the characteristics of the SLN, improve drug stability and loading capacity, and prevent drug leakage. Polymer nanoparticles (PNPs) are an important component of drug delivery. These nanoparticles can effectively direct drug delivery to specific targets and improve drug stability and controlled drug release. Lipid-polymer nanoparticles (PLNs), a new type of carrier that combines liposomes and polymers, have been employed in recent years. These nanoparticles possess the complementary advantages of PNPs and liposomes. A PLN is composed of a core-shell structure; the polymer core provides a stable structure, and the phospholipid shell offers good biocompatibility. As such, the two components increase the drug encapsulation efficiency rate, facilitate surface modification, and prevent leakage of water-soluble drugs. Hence, we have reviewed the current state of development for the NLCs', PNPs', and PLNs' structures, preparation, and applications over the past five years, to provide the basis for further study on a controlled release drug delivery system.

  19. Preparation, Structural and Dielectric Properties of Solution Grown Polyvinyl Alcohol(PVA) Film

    Science.gov (United States)

    Nangia, Rakhi; Shukla, Neeraj K.; Sharma, Ambika

    2017-08-01

    Flexible dielectrics with high permittivity have been investigated extensively due to their applications in electronic industry. In this work, structural and electrical characteristics of polymer based film have been analysed. Poly vinyl alcohol (PVA) film was prepared by solution casting method. X-ray diffraction (XRD) characterization technique is used to investigate the structural properties. The semi-crystalline nature has been determined by the analysis of the obtained XRD pattern. Electrical properties of the synthesized film have been analysed from the C-V and I-V curves obtained at various frequencies and temperatures. Low conductivity values confirm the insulating behaviour of the film. However, it is found that conductivity increases with temperature. Also, the dielectric permittivity is found to be higher at lower frequencies and higher temperatures, that proves PVA to be an excellent dielectric material which can be used in interface electronics. Dielectric behaviour of the film has been explained based on dipole orientations to slow and fast varying electric field. However further engineering can be done to modulate the structural, electrical properties of the film.

  20. Preparation and crystal and molecular structure of tris(diethyldithiocarbamato)dimethylphenylphosphinetechnetium(III)

    International Nuclear Information System (INIS)

    Batsanov, A.S.; Struchkov, Yu.T.; Lorenz, B.; Wahren, M.

    1984-01-01

    The title compound Tc(S 2 CNEt 2 ) 3 (Me 2 PhP) I has been prepared by the reaction of TcCl 3 (Me 2 PhP) 3 with NaS 2 CNEt 2 . The crystal structure of I has been determined by single-crystal X-ray diffraction methods at room temperature. Crystals are rhombic, space group P2 1 2 1 2 1 , with a = 8.708(1), b = 12.012(1), c = 29.626(3) A and Z = 4. The compound consists of discrete I molecules. The technetium atom has a seven-coordinated environment which is best described as a distorted pentagonal bipyramid. The Tc-P distance (2.330(3) A) is remarkably short compared with other technetium complexes with mono-dentate phosphine ligands. (author)

  1. Influence of the preparation route on the magnetic and structural properties of cobalt ferrites

    International Nuclear Information System (INIS)

    Revoredo Junior, Frederico Alves; Silva Junior, Jose Holanda da; Hernandez, Eduardo Padron

    2014-01-01

    Cobalt ferrite nanoparticles were produced using two methods of preparation, co-precipitation and reaction in the solid state. In synthesis made by solid state reaction was performed by heat treatment at 1200 ° C for four hours alternating with triturations to increase the efficiency of the process. The synthesis by coprecipitation was made with different flows of addition of alkali (NaOH). All samples were structurally characterized by X-ray diffraction and the average size of the crystals was obtained by Scherrer's formula and the Williamson-Hall method. The magnetic measurements were made as a function of applied magnetic field and temperature. Qualitative analyzes of energy dispersive spectroscopy defined the elements of sampling and analysis. Finally, Mössbauer spectroscopy analysis defined the magnetic character of the samples. (author)

  2. Preparation and characterization of CBN ternary compounds with nano-structure

    International Nuclear Information System (INIS)

    Xiong, Y.H.; Yang, S.; Xiong, C.S.; Pi, H.L.; Zhang, J.; Ren, Z.M.; Mai, Y.T.; Xu, W.; Dai, G.H.; Song, S.J.; Xiong, J.; Zhang, L.; Xia, Z.C.; Yuan, S.L.

    2006-01-01

    CBN ternary compounds with nano-structure have been prepared directly by a mechanical alloying technique at room temperature. The characteristic and formation mechanism of CBN are discussed. The nano-sheets and nano-layered rods of CBN are observed according to the morphology of scanning electron microscopy. It is substantiated that the microstructure of CBN was closely related to the ball milling time and the ball milling condition according to the results of X-ray diffraction of CBN with different ball milling time. After ball milling for 60 and 90 h, some new diffraction peaks are observed, which implies that some unknown microstructure and phase separation are induced in the reactive ball milling of CBN. The results of XRD are in accordance with that of X-ray photoelectron spectroscopy of CBN before ball milling and after ball milling for 90 h

  3. Structural and optical characteristics of SnS thin film prepared by SILAR

    Directory of Open Access Journals (Sweden)

    Mukherjee A.

    2015-12-01

    Full Text Available SnS thin films were grown on glass substrates by a simple route named successive ion layer adsorption and reaction (SILAR method. The films were prepared using tin chloride as tin (Sn source and ammonium sulfide as sulphur (S source. The structural, optical and morphological study was done using XRD, FESEM, FT-IR and UV-Vis spectrophotometer. XRD measurement confirmed the presence of orthorhombic phase. Particle size estimated from XRD was about 45 nm which fitted well with the FESEM measurement. The value of band gap was about 1.63 eV indicating that SnS can be used as an important material for thin film solar cells. The surface morphology showed a smooth, homogenous film over the substrate. Characteristic stretching vibration mode of SnS was observed in the absorption band of FT-IR spectrum. The electrical activation energy was about 0.306 eV.

  4. A novel approach to preparing magnetic protein microspheres with core-shell structure

    Science.gov (United States)

    Jiang, Wei; Sun, Zhendong; Li, Fengsheng; Chen, Kai; Liu, Tianyu; Liu, Jialing; Zhou, Tianle; Guo, Rui

    2011-03-01

    Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe 3O 4 cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe 3O 4 nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail.

  5. Preparation and properties of crystals of mixed refractory oxides with perovskite structure

    Energy Technology Data Exchange (ETDEWEB)

    Melekh, B T; Andreev, A A; Kartenko, N F; Pevtsov, A B; Trepakov, V A; Filin, Yu N [AN SSSR, Moscow. Fiziko-Tekhnicheskij Inst.

    1982-10-01

    Peculiar features of crystal growth of some complex refractory oxides with perovskite structure using the method of direct high-frequency melting in a cold container are studied. Melting, synthesis and directed crystallization have been conducted in the air. X-ray diffraction investigations of the prepared SrTiO/sub 3/, CaZrO/sub 3/, BaZrO/sub 3/, BaHFO/sub 3/, LaCrO/sub 3/, YCrO/sub 3/, ErCrO/sub 3/, La/sub 2/Ti/sub 2/O/sub 7/, LaTaO/sub 3/ and other oxides are conducted, lattice parameters are given. Optical spectra of absorption, photo- and thermoluminescence and thermostimulated currents are studied.

  6. Structure and magnetic properties of nanocrystalline Fe75Si25 powders prepared by mechanical alloying

    International Nuclear Information System (INIS)

    Kalita, M.P.C.; Perumal, A.; Srinivasan, A.

    2008-01-01

    Nanocrystalline Fe 75 Si 25 powders were prepared by mechanical alloying in a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling process were studied by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer measurements. The evolution of non-equilibrium solid solution Fe (Si) during milling was accompanied by refinement of crystallite size down to 10 nm and the introduction of high density of dislocations of the order of 10 17 m -2 . During the milling process, Fe sites get substituted by Si. This structural change and the resulting disorder are reflected in the lattice parameters and average magnetic moment of the powders milled for various time periods. A progressive increase of coercivity was also observed with increasing milling time. The increase of coercivity could be attributed to the introduction of dislocations and reduction of powder particle size as a function of milling time

  7. Study on the Reactivity of Amino Acid Chemosensor, NPFNP, with Ethanol: Structural Elucidation through Single Crystal XRD and DFT Calculations

    Directory of Open Access Journals (Sweden)

    Beena Varghese

    2017-01-01

    Full Text Available A novel ethoxy derivative of an amino acid chemosensor, 3-naphthyl-1-phenyl-5-(2ʹ-fluoro-5ʹ-nitrophenyl-2-pyrazoline (NPFNP, has been synthesized and characterized by different spectroscopic methods.  A single crystal of the ethoxy derivative, 3-naphthyl-1-phenyl-5-(2ʹ-ethoxy-5ʹ-nitrophenyl-2-pyrazoline NPENP, has been obtained and characterized.  The structure holds interest as it carries biologically active pyrazoline as a central ring attaching to electron donating and withdrawing substituents. The major motivation for this work was to gain detailed insight into the structural parameters of this compound for investigating the influence of crystal packing and geometrical dimensions on optical properties. Time-dependent DFT calculations have been employed for comparing the XRD data with theoretical parameters. The results show that the DFT method at B3LYP/6-31G level can well reproduce the structure of the title compound.

  8. Manganese ferrite prepared using reverse micelle process: Structural and magnetic properties characterization

    Energy Technology Data Exchange (ETDEWEB)

    Hashim, Mohd, E-mail: md.hashim09@gmail.com [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India); Shirsath, Sagar E. [Spin Device Technology Centre, Department of Engineering, Shinshu University, Nagano 380-8553 (Japan); Meena, S.S. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Mane, M.L. [Department of Physics, S.G.R.G. Shinde Mahavidyalaya, Paranda 413502, MS (India); Kumar, Shalendra [School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773 (Korea, Republic of); Bhatt, Pramod [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Kumar, Ravi [Centre for Material Science Engineering, National Institute of Technology, Hamirpur, HP (India); Prasad, N.K.; Alla, S.K. [Deptartment of Metallurgical Engineering, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005 (India); Shah, Jyoti; Kotnala, R.K. [National Physical Laboratory (CSIR), Dr. K.S. Krishnan Road, New Delhi 110012 (India); Mohammed, K.A. [Department of Mathematics & Physics Sciences, College of Arts and Sciences, University of Nizwa, Nizwa (Oman); Şentürk, Erdoğan [Department of Physics, Sakarya University, Esentepe, 54187 Sakarya (Turkey); Alimuddin [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India)

    2015-09-05

    Highlights: • Preparation of Mn{sup 3+} substituted MnFe{sub 2}O{sub 4} ferrite by Reverse microemulsion process. • Characterization by XRD, SEM, VSM, Mössbauer spectroscopy and dielectric measurements techniques. • Magnetic properties of MnFe{sub 2}O{sub 4} enhanced after Mn{sup 3+} substitution. • The dielectric constant and ac conductivity increased with Mn{sup 3+} substitution. - Abstract: Reverse microemulsion process was employed to prepare of nanocrystalline Mn{sup 3+} substituted MnFe{sub 2−x}Mn{sub x}O{sub 4} ferrites. The structural, magnetic and dielectric properties were studied for different concentrations of Mn{sup 3+}. The structural and microstructural properties were analyzed using X-ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy techniques. The phase identification of the materials was studied by Rietveld refined XRD patterns which reveals single phase with cubic symmetry for the samples. The lattice parameters were ranged in between 8.369 and 8.379 Å and do not show any significant change with the substitution of Mn{sup 3+}. The average particles size was found to be around 11 ± 3 nm. Magnetization results obtained from the vibrating sample magnetometer (VSM) confirm that the substitution of Mn{sup 3+} in MnFe{sub 2}O{sub 4} ferrite caused an increase in the saturation magnetization and coercivity. The dependence of Mössbauer parameters on Mn{sup 3+} substitution has been analyzed. Magnetic behavior of the samples were also studied at field cooled (FC) and zero field cooled (ZFC) mode. The dependence of Mössbauer parameters on Mn{sup 3+} substitution was also analyzed. All the magnetic characterization shows that Mn{sup 3+} substitution enhance the magnetic behavior of MnFe{sub 2}O{sub 4} ferrite nanoparticles.

  9. Influence of Process Control Agent on Characterization and Structure of Micron Chitosan Powders Prepared by Ball Milling Method

    Directory of Open Access Journals (Sweden)

    ZHANG Chuan-jie

    2016-12-01

    Full Text Available With ethyl alcohol or distilled water as process control agent (PCA, micron chitosan powder was prepared by ball milling method. The yield rate, particle size distribution, micro morphology, viscosity average molecular mass, chemical and crystal structures, and thermal properties of these different micron chitosan powders were measured. The results indicate that the yield rate of micron chitosan powders prepared with ethyl alcohol as PCA increases significantly, and improves to 94.7% from 25% while the amount of ethyl alcohol is 0.75mL/g. The particle size distribution of micron chitosan powder prepared with ethyl alcohol as PCA is concentrated, while the D50 and D90 in size are 824nm and 1629nm respectively. Chitosan do not react with ethyl alcohol used as PCA, but the viscosity average molecular mass of prepared micron chitosan powder decreases by 23%, the crystal structures are destroyed slightly, and its thermal stability is slightly weakened.

  10. NiFe epitaxial films with hcp and fcc structures prepared on bcc-Cr underlayers

    Energy Technology Data Exchange (ETDEWEB)

    Higuchi, Jumpei, E-mail: higuchi@futamoto.elect.chuo-u.ac.jp [Faculty of Science and Engineering, Chuo University, 1-13-27 Kasuga, Bunkyo-ku, Tokyo 112-8551 (Japan); Ohtake, Mitsuru; Sato, Yoichi [Faculty of Science and Engineering, Chuo University, 1-13-27 Kasuga, Bunkyo-ku, Tokyo 112-8551 (Japan); Kirino, Fumiyoshi [Graduate School of Fine Arts, Tokyo National University of Fine Arts and Music, 12-8 Ueno-koen, Taito-ku, Tokyo 110-8714 (Japan); Futamoto, Masaaki [Faculty of Science and Engineering, Chuo University, 1-13-27 Kasuga, Bunkyo-ku, Tokyo 112-8551 (Japan)

    2011-09-30

    NiFe epitaxial films are prepared on Cr(211){sub bcc} and Cr(100){sub bcc} underlayers grown hetero-epitaxially on MgO single-crystal substrates by ultra-high vacuum rf magnetron sputtering. The film growth behavior and the crystallographic properties are studied by reflection high energy electron diffraction and pole figure X-ray diffraction. Metastable hcp-NiFe(11-bar 00) and hcp-NiFe(112-bar 0) crystals respectively nucleate on Cr(211){sub bcc} and Cr(100){sub bcc} underlayers, where the hcp-NiFe crystals are stabilized through hetero-epitaxial growth. The hcp-NiFe(11-bar 00) crystal is a single-crystal with the c-axis parallel to the substrate surface, whereas the hcp-NiFe(112-bar 0) crystal is a bi-crystal with the respective c-axes lying in plane and perpendicular each other. With increasing the film thickness, the hcp structure in the NiFe films starts to transform into more stable fcc structure by atomic displacement parallel to the hcp(0001) close packed plane. The resulting films consist of hcp and fcc crystals.

  11. Preparation and Photoluminescence of ZnO Comb-Like Structure and Nanorod Arrays

    Science.gov (United States)

    Yin, Song; Chen, Yi-qing; Su, Yong; Zhou, Qing-tao

    2007-06-01

    A large quantity of Zinc oxide (ZnO) comb-like structure and high-density well-aligned ZnO nanorod arrays were prepared on silicon substrate via thermal evaporation process without any catalyst. The morphology, growth mechanism, and optical properties of the both structures were investigated using XRD, SEM, TEM and PL. The resulting comb-teeth, with a diameter about 20 nm, growing along the [0001] direction have a well-defined epitaxial relationship with the comb ribbon. The ZnO nanorod arrays have a diameter about 200 nm and length up to several micrometers growing approximately vertical to the Si substrate. A ZnO film was obtained before the nanorods growth. A growth model is proposed for interpreting the growth mechanism of comb-like zigzag-notch nanostructure. Room temperature photoluminescence measurements under excitation wavelength of 325 nm showed that the ZnO comb-like nanostructure has a weak UV emission at around 384 nm and a strong green emission around 491 nm, which correspond to a near band-edge transition and the singly ionized oxygen vacancy, respectively. In contrast, a strong and sharp UV peak and a weak green peak was obtained from the ZnO nanorod arrays.

  12. Preparation and structural studies on organotin(IV) complexes with flavonoids

    International Nuclear Information System (INIS)

    Nagy, L.; Christy, A.A.; Sletten, E.; Andersen, Q.M.; Edelmann, F.T.

    1998-01-01

    Fourteen complexes of di-n-butyltin(IV) 2+ cations with flavonoid glycosides (rutin, hesperidin, 2',4',3-trihydroxy-5',4-dimetoxychalkone 4-rutinoside) and flavonoid aglycones (quercetin, morin, hesperitin and sorte flavones) were prepared. The composition of the complexes was determined by standard analytical methods. The results showed that complexes containing diorganotin(IV) 2+ moiety and the ligand in 1:1, 2:1 or 3:1 ratio are formed. The FTIR spectra were consistent with the presence of Sn-O (phenol or carbohydrate) vibration in the compounds. The structure of the complexes was measured by Moessbauer spectroscopy. Comparison of the experimental quadrupole splitting with those calculated on the basis of partial quadrupole splitting concept revealed that the complexes are of four types: with the central tin atoms surrounded by donor atoms in a purely trigonal-bipyramidal, octahedral+trigonal-bipyramidal, trigonal-bipyramidal+tetrahedral and octahedral+tetrahedral arrangement. This procedure also distinguished between the different structural isomers of both trigonal-bipyramidal and octahedral complexes. Conclusions could therefore be drawn on the factors determining which of the isomers are formed in the systems. The Moessbauer parameters obtained for organotin(IV)-flavonoid complexes were compared with those measured for organotin(IV)-carbohydrate complexes. (author)

  13. Preparation and Application of Conductive Textile Coatings Filled with Honeycomb Structured Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Filip Govaert

    2014-01-01

    Full Text Available Electrical conductive textile coatings with variable amounts of carbon nanotubes (CNTs are presented. Formulations of textile coatings were prepared with up to 15 wt % of CNT, based on the solid weight of the binder. The binders are water based polyacrylate dispersions. The CNTs were mixed into the binder dispersion starting from a commercially available aqueous CNT dispersion that is compatible with the binder dispersion. Coating formulations with variable CNT concentrations were applied on polyester and cotton woven and knitted fabrics by different textile coating techniques: direct coating, transfer coating, and screen printing. The coatings showed increasing electrical conductivity with increasing CNT concentration. The coatings can be regarded to be electrically conductive (sheet resistivity<103 Ohm/sq starting at 3 wt% CNT. The degree of dispersion of the carbon nanotubes particles inside the coating was visualized by scanning electron microscopy. The CNT particles form honeycomb structured networks in the coatings, proving a high degree of dispersion. This honeycomb structure of CNT particles is forming a conductive network in the coating leading to low resistivity values.

  14. Preparation and investigation of structural, magnetic and microwave absorption properties of cerium doped barium hexaferrite

    Directory of Open Access Journals (Sweden)

    P Kameli

    2015-01-01

    Full Text Available In this study the structure, magnetic and microwave absorption properties of cerium (Ce doped barium hexaferrite with general formulae BaCexFe12-xO19 (x=0.0, 0.05, 0.1, 0.15, 0.2 have been investigated. These samples have been prepared by sol- gel method. Influence of replacing Fe+3 ion by rare- earth Ce+3 ion on the structural, magnetic and microwave absorption properties have been investigated by X- ray diffraction (XRD, Fourier transform infrared (FT-IR, Vibrating sample magnetometer (VSM and vector network analyzer (VNA. X-ray diffraction analysis indicated that the samples are of single phase with space group p63/mmc. The magnetic properties of samples indicated that with the Ce doping the saturation magnetization show no regular behavior. Moreover, coercivity (Hc first decreased and reached to the minimum value for x=0.1 sample and then increased with Ce content increasing. Also, measurement of electromagnetic wave absorption in X and Ku frequency bands indicated that the maximum of reflection loss obtained for x=0.15 sample. Moreover, result indicated that absorption peak shifted toward a lower frequency when thickness was increased.

  15. Chitin and Chitosan Preparation from Marine Sources. Structure, Properties and Applications

    Science.gov (United States)

    Younes, Islem; Rinaudo, Marguerite

    2015-01-01

    This review describes the most common methods for recovery of chitin from marine organisms. In depth, both enzymatic and chemical treatments for the step of deproteinization are compared, as well as different conditions for demineralization. The conditions of chitosan preparation are also discussed, since they significantly impact the synthesis of chitosan with varying degree of acetylation (DA) and molecular weight (MW). In addition, the main characterization techniques applied for chitin and chitosan are recalled, pointing out the role of their solubility in relation with the chemical structure (mainly the acetyl group distribution along the backbone). Biological activities are also presented, such as: antibacterial, antifungal, antitumor and antioxidant. Interestingly, the relationship between chemical structure and biological activity is demonstrated for chitosan molecules with different DA and MW and homogeneous distribution of acetyl groups for the first time. In the end, several selected pharmaceutical and biomedical applications are presented, in which chitin and chitosan are recognized as new biomaterials taking advantage of their biocompatibility and biodegradability. PMID:25738328

  16. Preparation of activated carbon aerogels with hierarchically porous structures for electrical double layer capacitors

    International Nuclear Information System (INIS)

    Liu, Dong; Shen, Jun; Liu, Nianping; Yang, Huiyu; Du, Ai

    2013-01-01

    Activated carbon aerogels (ACAs) with hierarchically porous structures and high specific surface area have been prepared via CO 2 and KOH activation processes. The pore structures of ACAs are characterized by N 2 adsorption/desorption and scanning electron microscopy. The experimental results show that the ACAs contain three types of pores: micropores with diameters below 2 nm, small mesopores with diameters from 2 to 4 nm and large pores or channels with diameters over 30 nm. The typical sample ACAs-4, which possess pore volume of 2.73 cm 3 g −1 and specific surface area of 2119 m 2 g −1 , exhibits high specific capacitances of 250 F g −1 and 198 F g −1 at the current densities of 0.5 A g −1 and 20 A g −1 respectively in 6 M KOH aqueous solution. Furthermore, the resultant ACAs electrode materials also exhibit high power density, good cycling stability and long lifetime. With these features, ACAs are expected to be promising electrode materials for electrical double layer capacitors

  17. Structural and magnetic properties of Mn nanoparticles prepared by arc-discharge

    International Nuclear Information System (INIS)

    Si, P.Z.; Brueck, E.; Zhang, Z.D.; Tegus, O.; Zhang, W.S.; Buschow, K.H.J.; KlAsse, J.C.P.

    2005-01-01

    Mn nanoparticles are prepared by arc discharge technique. MnO, α-Mn, β-Mn, and γ-Mn are detected by X-ray diffraction, while the presence of Mn 3 O 4 and MnO 2 is revealed by X-ray photoelectron spectroscopy. Transmission electron microscopy observations show that most of the Mn nanoparticles have irregular shapes, rough surfaces and a shell/core structure, with sizes ranging from several nanometers to 80 nm. The magnetic properties of the Mn nanoparticles are investigated between 2 and 350 K at magnetic fields up to 5 T. A magnetic transition occurring near 43 K is attributed to the formation of the ferrimagnetic Mn 3 O 4 . The coercivity of the Mn nanoparticles, arising mainly from Mn 3 O 4 , decreases linearly with increasing temperature below 40 K. Below the blocking temperature T B ∼ 34 K, the hysteresis loops exhibit large coercivity (up to 500 kA/m), owing to finite size effects, and irreversibility in the loops is found up to 4 T, and magnetization is not saturated up to 5 T. The relationship between structure and the magnetic properties are discussed

  18. NiFe epitaxial films with hcp and fcc structures prepared on bcc-Cr underlayers

    International Nuclear Information System (INIS)

    Higuchi, Jumpei; Ohtake, Mitsuru; Sato, Yoichi; Kirino, Fumiyoshi; Futamoto, Masaaki

    2011-01-01

    NiFe epitaxial films are prepared on Cr(211) bcc and Cr(100) bcc underlayers grown hetero-epitaxially on MgO single-crystal substrates by ultra-high vacuum rf magnetron sputtering. The film growth behavior and the crystallographic properties are studied by reflection high energy electron diffraction and pole figure X-ray diffraction. Metastable hcp-NiFe(11-bar 00) and hcp-NiFe(112-bar 0) crystals respectively nucleate on Cr(211) bcc and Cr(100) bcc underlayers, where the hcp-NiFe crystals are stabilized through hetero-epitaxial growth. The hcp-NiFe(11-bar 00) crystal is a single-crystal with the c-axis parallel to the substrate surface, whereas the hcp-NiFe(112-bar 0) crystal is a bi-crystal with the respective c-axes lying in plane and perpendicular each other. With increasing the film thickness, the hcp structure in the NiFe films starts to transform into more stable fcc structure by atomic displacement parallel to the hcp(0001) close packed plane. The resulting films consist of hcp and fcc crystals.

  19. Use of Calcium and Alendronic Acid Preparations in Correction of Structural and Functional Disorders of Bone Tissue in Thyrotoxicosis

    Directory of Open Access Journals (Sweden)

    O.B. Oliynyk

    2012-02-01

    Full Text Available Impact of calcium and alendronic acid preparations on disorders of structural and functional state of bone tissue in experimental animals at exogenic thyrotoxicosis was studied. It was defined that introduction of calcium preparations reduces bone mineral density loss in female rats with drug thyrotoxicosis, and combined use of calcium and alendronic acid prevents bone tissue loss regardless of thyrotoxicosis duration and presence of ovariectomy.

  20. Comparative analysis of structure of sporting preparation in a boat-racing, rowing on kayaks and canoe

    Directory of Open Access Journals (Sweden)

    Zhirnov A.V.

    2011-07-01

    Full Text Available In the article information of expert estimation of different types of preparation is presented in boating. On the basis of analysis of literary sources the structure of the sporting training is certain. Principles of application of quantitative methods of estimation of quality are considered in sport. The most priority types of sporting preparation are exposed in different disciplines of rowing. On the basis of opinions of experts the comparative analysis of influence on the sporting result of different types of preparation is conducted in a boat-racing and rowing on kayaks and canoe.

  1. Nano-Ag complexes prepared by γ-radiolysis and their structures and physical properties

    International Nuclear Information System (INIS)

    Kim, Hwa-Jung; Choi, Seong-Ho; Park, Hae-Jun

    2012-01-01

    In this study, nano-silver (nano-Ag) complexes showing different properties have been synthesized as follows. Polypyrrolidone (PVP)-stabilized silver colloids (NAg), nano-Ag bound to silica (SiO 2 ) (NSS), and nano-Ag bound to a complex of SiO 2 and polyaniline (PANI) (NSSPAI) were prepared via γ-irradiation at room temperature. NAg and NSS used PVP as a colloidal stabilizer, while NSSPAI did not use PVP as a colloidal stabilizer. Interesting bonding properties occurred in the nano-Ag complex and anticipated structural changes were clearly shown through a surface analysis of x-ray photoelectron spectroscopy (XPS). The morphologies by field emission-scanning electron microscopy (FE-SEM) analysis showed that nano-Ag complexes have various particle sizes ranging from 10 to 30 nm. NSS (average, 10 nm) and NSSPAI (average, 30 nm) showed a uniformly spherical shape and size, while NAg did not. From the reflection peaks in the x-ray diffraction (XRD) patterns, surface crystallinity of the nano-Ag complexes was indicated to be in the same degree as that of NSSPAI>NSS>NAg. Also, in the contact angle (CA) determination, surface hydrophobicity of NSSPAI was stronger than those of NSS and NAg, relatively. The different nano-Ag complexes prepared by γ-irradiation can be applicable in various industry fields due to the increase in specific property. - Highlights: ► Nano-Ag complexes showing different properties have been synthesized via γ-irradiation. ► Nano-Ag colloid (NAg), nano-Ag bound to SiO 2 (NSS), nano-Ag bound to SiO 2 and PANI complex (NSSPAI). ► Nano-Ag complexes were the same based on Ag metal. ► Results clearly showed fascinating/different physical properties. ► Different nano-Ag complexes can be applicable in various industry fields.

  2. Synthesis and structural characterization of nano-hydroxyapatite biomaterials prepared by microwave processing

    Science.gov (United States)

    Ramli, Rosmamuhamadani; Arawi, Ainaa Zafirah Omar; Talari, Mahesh Kumar; Mahat, Mohd Muzamir; Jais, Umi Sarah

    2012-07-01

    Synthetic hydroxyapatite, (HA, Ca10(PO4)6(OH)2), is an attractive and widely utilized bio-ceramic material for orthopedic and dental implants because of its close resemblance of native tooth and bone crystal structure. Synthetic HA exhibits excellent osteoconductive properties. Osteoconductivity means the ability to provide the appropriate scaffold or template for bone formation. Calcium phosphate biomaterials [(HA), tri-calcium phosphate (TCP) and biphasic calcium phosphate (HA/TCP)] with appropriate three-dimensional geometry are able to bind and concentrate endogenous bone morphogenetic proteins in circulation, and may become osteoinductive and can be effective carriers of bone cell seeds. This HA can be used in bio-implants as well as drug delivery application due to the unique properties of HA. Biomaterials synthesized from the natural species like mussel shells have additional benefits such as high purity, less expensive and high bio compatibility. In this project, HA-nanoparticles of different crystallite size were prepared by microwave synthesis of precursors. High purity CaO was extracted from the natural mussel shells for the synthesis of nano HA. Dried nano HA powders were analyzed using X-Ray Diffraction (XRD) technique for the determination of crystal structure and impurity content. Scanning Electron Microscopic (SEM) investigation was employed for the morphological investigation of nano HA powders. From the results obtained, it was concluded that by altering the irradiation time, nano HA powders of different crystallite sizes and morphologies could be produced. Crystallite sizes calculated from the XRD patterns are found to be in the range of 10-55 nm depending on the irradiation time.

  3. The crystal structure and morphology of NiO-YSZ composite that prepared from local zircon concentrate of Bangka Island

    Energy Technology Data Exchange (ETDEWEB)

    Rahmawati, F., E-mail: fitria@mipa.uns.ac.id; Apriyani, K.; Heraldy, E. [Research Group of Solid State Chemistry & Catalysis, Department of Chemistry, Sebelas Maret University, Jl. Ir. Sutami 36A Kentingan Surakarta (Indonesia); Soepriyanto, S. [Department of Metallurgical Engineering, Faculty of Mining and Petroleum Engineering, Institut Teknologi Bandung, Jl. Ganesha 10 Bandung 40132 (Indonesia)

    2016-03-29

    In order to increase the economic value of local zircon concentrate from Bangka Island, NiO-YSZ was synthesized from Zirconia, ZrO{sub 2} that was prepared from local zircon concentrate. The NiO-YSZ composite was synthesized by solid state reaction method. XRD analysis equipped with Le Bail refinement was carried out to analyze the crystal structure and cell parameters of the prepared materials. The result showed that zirconia was crystallized in tetragonal structure with a space group of P42/NMC. Yttria-Stabilized-Zirconia (YSZ) was prepared by doping 8% mol yttrium oxide into zirconia and then sintered at 1250°C for 3 hours. Doping of 8% mol Yttria allowed phase transformation of zirconia from tetragonal into the cubic structure. Meanwhile, the composite of NiO-YSZ consists of two crystalline phases, i.e. the NiO with cubic structure and the YSZ with cubic structure. SEM analysis of the prepared materials shows that the addition of NiO into YSZ allows the morphology to become more roughness with larger grain size.

  4. Enzymatic preparation of "functional oil" rich in feruloylated structured lipids with solvent-free ultrasound pretreatment.

    Science.gov (United States)

    Zhang, Haiping; Zheng, Mingming; Shi, Jie; Tang, Hu; Deng, Qianchun; Huang, Fenghong; Luo, Dan

    2018-05-15

    In this study, a series of functional oils rich in feruloylated structured lipids (FSLs) was prepared by enzymatic transesterification of ethyl ferulate (EF) with triglycerides under ultrasound pretreatment. A conversion of more than 92.7% and controllable FSLs (3.1%-26.3%) can be obtained under the following conditions: 16% enzyme, substrate ratio 1:5 (oil/EF, mol/mol), 85 °C, ultrasound 1 h, pulse mode 3 s/3s (working/waiting), and 17.0 W/mL. Compared to conventional mechanical stirring, the activation energy decreased from 50.0 kJ/mol to 40.7 kJ/mol. The apparent kinetic constant increased by more than 13 times, and the time required for the maximum conversion reduced sharply from 20-60 h to 4-6h, which was the fastest rate for enzymatic synthesis of FSLs. The antioxidant activities of the functional oil significantly increased 1.0- to 8.1-fold more than that of the raw oil. The functional oil could be widely applied in various fields of functional foods. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Structure and composition of chemically prepared and vacuum annealed InSb(0 0 1) surfaces

    International Nuclear Information System (INIS)

    Tereshchenko, O.E.

    2006-01-01

    The InSb(0 0 1) surfaces chemically treated in HCl-isopropanol solution and annealed in vacuum were studied by means of X-ray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED) and electron energy-loss spectroscopy (EELS). The HCl-isopropanol treatment removes indium and antimony oxides and leaves on the surface about 3 ML of physisorbed overlayer, containing indium chlorides and small amounts of antimony, which can be thermally desorbed at 230 deg. C. The residual carbon contaminations were around 0.2-0.4 ML and consisted of the hydrocarbon molecules. These hydrocarbon contaminations were removed from the surface together with the indium chlorides and antimony overlayer. With increased annealing temperature, a sequence of reconstructions were identified by LEED: (1 x 1), (1 x 3), (4 x 3), and (4 x 1)/c(8 x 2), in the order of decreasing Sb/In ratio. The structural properties of chemically prepared InSb(0 0 1) surface were found to be similar to those obtained by decapping of Sb-capped epitaxial layers

  6. Preparation and structure of porous dielectrics by plasma enhanced chemical vapor deposition

    International Nuclear Information System (INIS)

    Gates, S. M.; Neumayer, D. A.; Sherwood, M. H.; Grill, A.; Wang, X.; Sankarapandian, M.

    2007-01-01

    The preparation of ultralow dielectric constant porous silicon, carbon, oxygen, hydrogen alloy dielectrics, called 'pSiCOH', using a production 200 mm plasma enhanced chemical vapor deposition tool and a thermal treatment is reported here. The effect of deposition temperature on the pSiCOH film is examined using Fourier transform infrared (FTIR) spectroscopy, dielectric constant (k), and film shrinkage measurements. For all deposition temperatures, carbon in the final porous film is shown to be predominantly Si-CH 3 species, and lower k is shown to correlate with increased concentration of Si-CH 3 . NMR and FTIR spectroscopies clearly detect the loss of a removable, unstable, hydrocarbon (CH x ) phase during the thermal treatment. Also detected are increased cross-linking of the Si-O skeleton, and concentration changes for three distinct structures of carbon. In the as deposited films, deposition temperature also affects the hydrocarbon (CH x ) content and the presence of C=O and C=C functional groups

  7. Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

    International Nuclear Information System (INIS)

    Yasukawa, Akemi; Kandori, Kazuhiko; Tanaka, Hidekazu; Gotoh, Keiko

    2012-01-01

    Highlights: ► LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. ► The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln 3+ contents. ► A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0–0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y 3+ , Gd 3+ , Dy 3+ , Er 3+ and Yb 3+ ) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X Ln ]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X Y ] ≤ 0.10 for substituting Y system and at [X Ln ] ≤ 0.01–0.03 for substituting the other Ln systems. LnPO 4 was mixed with LnCaHap at higher [X Ln ] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X Y ] = 0–0.10 were investigated using XRD, TEM, ICP-AES, IR and TG–DTA in detail.

  8. Influence of preparation conditions on porous structures of olive stone activated by H3PO4

    International Nuclear Information System (INIS)

    Yavuz, Reha; Akyildiz, Hanife; Karatepe, Nilguen; Cetinkaya, Eda

    2010-01-01

    An olive factory residue was used as a precursor in the preparation of granular activated carbon by chemical activation with H 3 PO 4 . Effects of final activation temperature, time, and H 3 PO 4 concentration used in the impregnation stage on the porous development were investigated. SO 2 adsorption experiments were also performed for some of the activated carbon samples to represent their adsorption performance. Activation at low temperature represented that micropores were developed first at early stages of the temperatures. Mesoporosity developed at around 250 C, enhanced up to 400 C, and then started to decrease due to possibly shrinking of pores. The optimum temperature for olive stone was found to be around 400 C on the basis of total pore volume and BET surface area. It was clearly demonstrated that H 3 PO 4 concentration used in the impregnation stage was not only effective for development of surface area and pore volumes but also an effective tool for tailoring the pore structure and size distribution. (author)

  9. Preparation and structural characterization of zwitterionic surfactant intercalated into NiZn-layered hydroxide salts

    Science.gov (United States)

    Liu, Jiexiang; Wang, Jianlong; Zhang, Xiaoguang; Fang, Binbin; Hu, Pan; Zhao, Xuyang

    2015-10-01

    Three zwitterionic surfactants, dodecyl dimethyl carboxylbetaine (DCB), dodecyl dimethyl sulfobetaine (DSB) and N-dodecyl-β-aminoprpionate (DAP), intercalated into NiZn-layered hydroxide salts (NZL-DCB, NZL-DSB and NZL-DAP) were synthesized by the coprecipitation method. The effect of surfactant content, pH, temperature and time of hydrothermal treatment on preparation was investigated and discussed. The NZL-DCB, NZL-DSB and NZL-DAP were characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), and thermogravimetry analysis and differential thermal analysis (TGA/DTA). The results showed that basal spacings of NZL-DCB, NZL-DSB and NZL-DAP were around 3.45, 3.68 and 3.94 nm, respectively. DCB, DSB and DAP probably form an overlapped bilayer in the gallery. TGA/DTA data indicated that NZL-DCB, NZL-DSB and NZL-DAP displayed three loss weight stages: loss of adsorbed and structural water, dehydroxylation of matrix and decomposition of nitrate ions, decomposition and combustion of surfactants. Furthermore, chemical analysis data, BET surface area and scanning electron microscopic (SEM) were also measured and analyzed.

  10. Preparation of two series of materials with perovskite structure and investigation of their physical properties

    International Nuclear Information System (INIS)

    Mohamed, H.S.R.

    2010-01-01

    Results on structural, electric transport and magnetic properties of a series of (Al / In) doped Ca-series and (Al / In) doped Sr-series are presented and discussed.The polycrystalline ceramic samples were prepared by the solid state reaction technique. Elemental analysis showed a reasonable agreement between nominal and actual sample compositions. The grain size (G.S) of the Ca doped series increased with In content (G.S. (x = 0.2) = 79.5 nm and G.S. (x = 0.8) = 95.4 nm). For the Sr-series it has values in the range of 40 - 42 nm.Room temperature structural analysis using the Rietveld refinement technique,showed no structural transitions with the variation of the Al / In ratio. The doped Ca-series had an orthorhombic symmetry with space group Pnma. The Sr -doped series is rhombohedral with space group ( R3C ). In both series the Mn-O bond distance was found to increase whereas the mean Mn-O-Mn bond angle decreased with x. This was ascribed to the size mismatch between the divalent A- site ions and the B- site as a result of the introduction of the large In 3+ ion size. The tolerance factor varies from 0.918-0.933 for the Ca-series and from 0.932 - 0.948 for the Sr-series as x varies from 0.0 to 1.0. The temperature dependence of the magnetic susceptibility and electric resistivity of the Ca-doped series showed distinct ferromagnetic metallic (FMM) to a paramagnetic insulator (PMI) transitions near the Curie point (T C ), which ranges from T C ∼ 210 - 100 K for x = 0.0 to 1.0 respectively. The temperature dependence of the resistivity for the Sr-doped series showed distinct FMM to PMI transitions for samples with x = 0.0, 0.2 and 1.0, whereas samples with x = 0.4, 0.6 and 0.8 showed FMM to PMM. The transition temperature variation is not linear and lies within a narrow temperature range T p ∼ 344 - 367 K The results of the Sr-series showed that the size mismatch between the A- and B- sites is the major factor that controls the magnetic and electric properties

  11. Influence of the external heating type in the morphological and structural characteristics of alumina powder prepared by combustion reaction

    International Nuclear Information System (INIS)

    Cordeiro, V.V.; Freitas, N.L.; Viana, K.M.S.; Dias, G.; Costa, A.C.F.M.; Lira, H.L.

    2009-01-01

    The aim of this work is to evaluate the influence of the external heating in the morphological and structural characteristics of the alumina powder prepared by combustion reaction. It was evaluated different types of external heating: muffle oven, microwave oven and ceramic plate with electrical spiral resistance. The powders were prepared according to the propellants and explosives theory, using urea in the stoichiometric proportion (Φe = 1). During the synthesis parameters such as flame combustion time and temperature were measured. The structural and morphological characteristics of the powders were evaluate by XRD, particle size distribution, SEM and nitrogen adsorption (BET). The results showed the production of a-alumina as unique phase and formed by agglomerates with irregular plate shape of thin particles for all studied conditions. The powders prepared by electrical oven presented small particle size, with narrow agglomerates size distribution. (author)

  12. Preparation of TiC/W core–shell structured powders by one-step activation and chemical reduction process

    International Nuclear Information System (INIS)

    Ding, Xiao-Yu; Luo, Lai-Ma; Huang, Li-Mei; Luo, Guang-Nan; Zhu, Xiao-Yong; Cheng, Ji-Gui; Wu, Yu-Cheng

    2015-01-01

    Highlights: • A novel wet chemical method was used to prepare TiC/W core–shell structure powders. • TiC nanoparticles were well-encapsulated by W shells. • TiC phase was present in the interior of tungsten grains. - Abstract: In the present study, one-step activation and chemical reduction process as a novel wet-chemical route was performed for the preparation of TiC/W core–shell structured ultra-fine powders. The XRD, FE-SEM, TEM and EDS results demonstrated that the as-synthesized powders are of high purity and uniform with a diameter of approximately 500 nm. It is also found that the TiC nanoparticles were well-encapsulated by W shells. Such a unique process suggests a new method for preparing X/W (X refers the water-insoluble nanoparticles) core–shell nanoparticles with different cores

  13. Structural and morphological properties of HfxZr 1-xO2 thin films prepared by Pechini route

    KAUST Repository

    Garcí a-Cerda, L. A.; Puente-Urbina, B. A.; Quevedo-Ló pez, Manuel Angel Quevedo; Gnade, Bruce E.; Baldenegro-Pé rez, Leonardo Aurelio; Alshareef, Husam N.; Herná ndez-Landaverde, Martí n Adelaido

    2010-01-01

    In this study, HfxZr1-xO2 (0 < x < 1) thin films were deposited on silicon wafers using a dip-coating technique and by using a precursor solution prepared by the Pechini route. The effects of annealing temperature on the structure and morphological

  14. Do Test Design and Uses Influence Test Preparation? Testing a Model of Washback with Structural Equation Modeling

    Science.gov (United States)

    Xie, Qin; Andrews, Stephen

    2013-01-01

    This study introduces Expectancy-value motivation theory to explain the paths of influences from perceptions of test design and uses to test preparation as a special case of washback on learning. Based on this theory, two conceptual models were proposed and tested via Structural Equation Modeling. Data collection involved over 870 test takers of…

  15. Irregular distribution of metal ions in ferrites prepared by co-precipitation technique structure analysis of Mn-Zn ferrite using extended X-ray absorption fine structure

    International Nuclear Information System (INIS)

    Jeyadevan, B.; Tohji, K.; Nakatsuka, K.; Narayanasamy, A.

    2000-01-01

    The tetrahedral/octahedral site occupancy of non-magnetic zinc ion, added to maximize the net magnetic moment of mixed ferrites has been found to depend on the method of preparation. In this paper, we qualitatively analyze the metal ion distribution in Mn-Zn ferrite particles prepared by co-precipitation and ceramic methods using extended X-ray absorption fine structure (EXAFS) technique. The results suggest that the differences observed in the magnetic properties of the samples prepared by different methods are not only due to the difference in particle size but also due to the difference in cation distribution. The difference in cation distributions between ferrites of similar composition prepared differently has been found to depend on the crystal field stability energies of the metal ion of interest and associated cations

  16. A contribution to preparative micro-chemistry and structural chemistry of element 96, curium

    International Nuclear Information System (INIS)

    Kohl, R.

    1984-01-01

    Ternary oxides of curium are analyzed by preparing a spectrum of different phases and characterizing it by radiography. Physical and thermodynamic data are established on curium trihalogenides. Particular interest is taken in experiments for preparing curium of the higher valency stages IV, V, and VI. (orig./PW) [de

  17. Preparation of designed poly(D,L-lactide)/nanosized hydroxyapatite composite structures by stereolithography

    NARCIS (Netherlands)

    Ronca, A.; Ambrosio, L.; Grijpma, D. W.

    The preparation of scaffolds to facilitate the replacement of damaged tissues and organs by means of tissue engineering has been much investigated. The key properties of the biomaterials used to prepare such scaffolds include biodegradability, biocompatibility and a well-defined three-dimensional

  18. Preparation of designed poly(d,l-lactide)/nanosized hydroxyapatite composite structures by stereolithography

    NARCIS (Netherlands)

    Ronca, A.; Ambrosio, L.; Grijpma, Dirk W.

    2013-01-01

    The preparation of scaffolds to facilitate the replacement of damaged tissues and organs by means of tissue engineering has been much investigated. The key properties of the biomaterials used to prepare such scaffolds include biodegradability, biocompatibility and a well-defined three-dimensional

  19. (E)-3-(2-Alkyl-10H-phenothiazin-3-yl)-1-arylprop-2-en-1-ones: Preparative, IR, NMR and DFT study on their substituent-dependent reactivity in hydrazinolysis and sonication-assisted oxidation with copper(II)nitrate.

    Science.gov (United States)

    Găină, Luiza; Csámpai, Antal; Túrós, György; Lovász, Tamás; Zsoldos-Mády, Virág; Silberg, Ioan A; Sohár, Pál

    2006-12-07

    A series of novel 3(5)-aryl/ferrocenyl-5(3)-phenothiazinylpyrazoles and pyrazolines were obtained by substituent-dependent regioselective condensation of the corresponding (E)-3-(2-alkyl-10H-phenothiazin-3-yl)-1-aryl/ferrocenylprop-2-en-1-one with hydrazine or methylhydrazine in acetic acid. The different propensity of the primary formed beta-hydrazino adducts to undergo competitive retro-Mannich reaction was interpreted in terms of tautomerisation equilibrium constants calculated by DFT using a solvent model. The regioselectivity of the cyclisation reactions with methylhydrazine and the substituent-dependent redox properties of pyrazolines were also rationalized by comparative DFT calculations performed for simplified model molecules. On the effect of ultrasound-promoted oxidation with copper(II)nitrate phenothiazine-containing pyrazolines, enones and oxo-compounds were selectively transformed into sulfoxides. Only one sulfoxide enone was partially converted into an oxirane derivative. The structure of the novel products was determined by IR and NMR spectroscopy including COSY, HSQC, HMBC and DNOE measurements.

  20. Structure and giant magnetoresistance of carbon-based amorphous films prepared by magnetron sputtering

    International Nuclear Information System (INIS)

    Ma, L.; He, M.F.; Liu, Z.W.; Zeng, D.C.; Gu, Z.F.; Cheng, G.

    2014-01-01

    Pure amorphous carbon (a-C) and Co-doped Co x C 1−x films were prepared on n-Si(100) substrates by dc magnetron sputtering. In Co–C films, the nano-sized amorphous Co particles were homogeneously dispersed in the amorphous cross-linked carbon matrix. The structures of a-C and Co x C 1−x films were investigated by X-ray photoelectron spectroscopy and Raman spectroscopy. The results showed that the a-C films were diamond-like carbon (DLC) films. After doping cobalt into DLC film, the sp 3 -hybridized carbon content in DLC composite films almost had no change. The as-deposited Co x C 1−x granular films had larger value of magnetoresistance (MR) than the amorphous carbon film. A very high positive MR, up to 15.5% at magnetic field B = 0.8 T and x = 2.5 at.% was observed in a Co x C 1−x granular film with thickness of 80 nm at room temperature when the external magnetic field was perpendicular to the electric current and the film surface. With increase of the film thickness and Co-doped content, the MR decreased gradually. It remains a challenge to well explain the observed MR effect in the Co x C 1−x granular films. - Highlights: • The amorphous carbon films were diamond-like carbon films. • No carbide appearing, the Co–C composite films form a good metal/insulator system. • A high positive magnetoresistance, up to 15.5% at B = 0.8 T was observed in Co–C films

  1. Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

    Energy Technology Data Exchange (ETDEWEB)

    Yasukawa, Akemi, E-mail: yasukawa@cc.hirosaki-u.ac.jp [School of Home Economics, Faculty of Education, Hirosaki University, 1-bunkyo, Hirosaki, Aomori 036-8560 (Japan); Kandori, Kazuhiko [School of Chemistry, Osaka University of Education, 4-698-1 Asahigaoka, Kashiwara, Osaka 582-8582 (Japan); Tanaka, Hidekazu [Department of Material Science, Faculty of Science and Engineering, Shimane University, 1060 Nishikawatsu, Matsue, Shimane 690-8504 (Japan); Gotoh, Keiko [Faculty of Human Life and Environment, Nara Women' s University, Kita-uoya-nishi, Nara 630-8506 (Japan)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. Black-Right-Pointing-Pointer The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln{sup 3+} contents. Black-Right-Pointing-Pointer A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0-0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y{sup 3+}, Gd{sup 3+}, Dy{sup 3+}, Er{sup 3+} and Yb{sup 3+}) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X{sub Ln}]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X{sub Y}] {<=} 0.10 for substituting Y system and at [X{sub Ln}] {<=} 0.01-0.03 for substituting the other Ln systems. LnPO{sub 4} was mixed with LnCaHap at higher [X{sub Ln}] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X{sub Y}] = 0-0.10 were investigated using XRD, TEM, ICP-AES, IR and TG-DTA in detail.

  2. Preparation of fluoropolymer-based ion-track membranes. Structure of latent tracks and pretreatment effect

    International Nuclear Information System (INIS)

    Yamaki, Tetsuya; Nuryanthi, Nuryanthi; Koshikawa, Hiroshi; Sawada, Shinichi; Hakoda, Teruyuki; Hasegawa, Shin; Asano, Masaharu; Maekawa, Yasunari

    2012-01-01

    High-energy heavy-ion induced damage, called latent tracks m organic polymers can sometimes be etched out chemically to give submicro- and nano-sized pores. Our focus is placed on ion-track membranes of poly(vinylidene fluoride) (PVDF), a type of fluoropolymer, which were previously considered as a matrix of polymer electrolyte fuel-cell membranes. There have been no optimized methods of preparing the PVDF-based ion-track membranes. We thus examined chemical structures of the defects created in the track, and accordingly, presented a pretreatment technique for achieving more efficient track etching. A 25 μm-thick PVDF film was bombarded with 1.1 GeV 238 U or 450 MeV 129 Xe ions. In the multi-purpose chamber, degradation processes were monitored in-situ by FT-IR spectroscopy and residual gas analysis as a function of the fluence up to 6.0 x 10 11 ions/cm 2 . The films irradiated at 8 ions/cm 2 were etched in a 9 M KOH aqueous solution at 80degC. We also performed the conductometric etching, which allows monitoring of pore evolution versus etching time by recording the electrical conductance through the membrane. At fluences above 1 x 10 10 ions/cm 2 , the film showed two new absorption bands identified as double-bond stretching vibrations of in-chain unsaturations -CH=CF- and fluorinated vinyl groups -CF 2 CH=CF 2 . These defects would result from the evolution of HF. The knowledge of the solubility in a permanganate alkaline solution and our preliminary experiment suggested the importance of oxidized tracks for the easy introduction of the etching agent. We finally found that the pretreatment with ozone could oxidize the double bonds in the tracks, thereby vigorously promoting track etching before breakthrough. (author)

  3. Preparation and characterization of perovskite structure lanthanum gallate and lanthanum aluminate based oxides

    OpenAIRE

    Li, Shuai

    2009-01-01

    The present work was initiated to study the synthesis and properties of lanthanum gallate based oxides as intermediate temperature electrolyte for solid oxide fuel cells. The wet chemical method, polymer complexing route, was used to prepare the precursor powders. To further investigate the polymer complexing method, it was also applied to the preparation of lanthanum aluminate based oxides.   Single perovskite phase La0.8Sr0.2Ga0.83Mg0.17O2.815 can be prepared by the polymer complexing meth...

  4. Stacking layered structure of polymer light emitting diodes prepared by evaporative spray deposition using ultradilute solution for improving carrier balance

    International Nuclear Information System (INIS)

    Aoki, Youichi; Shakutsui, Masato; Fujita, Katsuhiko

    2009-01-01

    Polymer light-emitting diodes (PLEDs) with staking layered structures are prepared by the evaporative spray deposition using ultradilute solution (ESDUS) method, which has enabled forming a polymer layer onto another polymer layer even if both polymers are soluble in a solvent used for the preparation. By this method, polymers having various HOMO and LUMO levels can be stacked as a hole transport layer, an emitting layer and an electron transport layer as commonly employed in small molecule-based organic light emitting diodes. Here we demonstrated that a PLED having a tri-layer structure using three kinds of polymers showed significant improvement in quantum efficiency compared with those having a single or bi-layer structure of corresponding polymers.

  5. Oleochemicals I: Studies on the preparation and the structure of lithium soaps.

    Directory of Open Access Journals (Sweden)

    Shoeb, Zein E.

    1999-12-01

    Full Text Available Lithium stéarate, palmitate, myristate, laurate, caprate and caprylate were prepared by means of fusion method. Elementary analysis and the infrared absorptions spectra of the prepared lithium soaps as well as their X-ray diffractions and the thermogravimetric analyses were carried out. The anhydrous lithium salts of fatty acids with 12 carbon atoms or less showed thermal stability up to ca. 300 ± 78 °C depending on the chain length. On other hand the salts with 14 carbon atoms or more were decomposed at 126 ± 4 °C leading to formation of lithium carbonate. The homologous lithium soaps had very similar crystal structure among them and their metal -to- oxygen bonds were similar for the acyl chains between 8 and 18 carbons. However the angle of inclination of the molecular axes to the basal plane increased with the decreasing of the number of carbon atoms of the fatty acid chain, as determined by X-ray diffraction. In addition, the ionic character of the metal -to- oxygen bond was enhanced with the decrease of the number of carbon atoms as shown by infrared spectroscopy.

    Se han preparado estearato, palmitato, miristato, laurato, caprato y caprilato de litio por fusión. Se ha realizado el análisis elemental, los espectros de absorción en el infrarrojo y las difracciones de rayos X de los Jabones de litio preparados, además del análisis termogravimétrico de los mismos. Las sales de litio anhidra de los ácidos con 12 átomos de carbono o menos mostraron una estabilidad térmica hasta los 300 ± 78 °C dependiendo de la longitud de la cadena. Por otro lado las sales con 14 átomos de carbono o más se descompusieron a 126 ± 4 °C formándose carbonato de litio. Los jabones homólogos de litio mostraron una estructura cristalina similar, siendo los enlaces metal-oxígeno del mismo tipo para los ácidos grasos de número de átomos de carbono entre 8 y 18. Sin embargo el ángulo de inclinación que forma la molécula con el plano

  6. Effect of various structure directing agents on the physicochemical properties of the silica aerogels prepared at an ambient pressure

    KAUST Repository

    Sarawade, Pradip; Shao, Godlistennamwel; Quang, Dangviet; Kim, Heetaik

    2013-01-01

    We studied the effects of various surfactants on the textural properties (BET surface area, pore size, and pore volume) of the silica aerogels prepared at an ambient pressure. A simple surface modification of silica gel prepared at an ambient pressure through hydrolysis and polycondensation of TEOS as asilica precursor was conducted using various structure directing agents. The treatment was found to induce a significant difference in the porosity of the silica aerogel. Highly porous silica aerogels with bimodal porous structures were prepared by modifying the surface of the silica wet-gel (alcogel) with trimethylchlorosilane (TMCS) in order to preserve its porosity. The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. In this work, a possible new type of highly porous hydrophobic silica aerogel with a bimodal porous structure is presented. A hydrophilic extremely porous (high surface area and large pore volume) silica aerogel was obtained by heating the as-synthesized hydrophobic silica aerogel at 400°C for 1 h. There was a significant effect of structure directing agent on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the silicaaerogels. © 2013 Elsevier B.V. All rights reserved.

  7. Effect of various structure directing agents on the physicochemical properties of the silica aerogels prepared at an ambient pressure

    KAUST Repository

    Sarawade, Pradip

    2013-12-01

    We studied the effects of various surfactants on the textural properties (BET surface area, pore size, and pore volume) of the silica aerogels prepared at an ambient pressure. A simple surface modification of silica gel prepared at an ambient pressure through hydrolysis and polycondensation of TEOS as asilica precursor was conducted using various structure directing agents. The treatment was found to induce a significant difference in the porosity of the silica aerogel. Highly porous silica aerogels with bimodal porous structures were prepared by modifying the surface of the silica wet-gel (alcogel) with trimethylchlorosilane (TMCS) in order to preserve its porosity. The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. In this work, a possible new type of highly porous hydrophobic silica aerogel with a bimodal porous structure is presented. A hydrophilic extremely porous (high surface area and large pore volume) silica aerogel was obtained by heating the as-synthesized hydrophobic silica aerogel at 400°C for 1 h. There was a significant effect of structure directing agent on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the silicaaerogels. © 2013 Elsevier B.V. All rights reserved.

  8. Evaluated Nuclear Structure data file: a manual for preparation of data sets

    International Nuclear Information System (INIS)

    Ewbank, W.B.; Schmorak, M.R.

    1978-02-01

    A standard input format for nuclear structure data is described. The format is sufficiently structured that bulk data can be entered efficiently. At the same time, the structure is open-ended and can accommodate most measured or deduced quantities that yield nuclear structure information

  9. Preparation of gluten-free bread using a meso-structured whey protein particle system

    NARCIS (Netherlands)

    Riemsdijk, van L.E.; Goot, van der A.J.; Hamer, R.J.; Boom, R.M.

    2011-01-01

    This article presents a novel method for making gluten-free bread using mesoscopically structured whey protein. The use of the meso-structured protein is based on the hypothesis that the gluten structure present in a developed wheat dough features a particle structure on a mesoscopic length scale

  10. Structural and optical properties of surface-hydrogenated silicon nanocrystallites prepared by reactive pulsed laser ablation

    International Nuclear Information System (INIS)

    Makino, Toshiharu; Inada, Mitsuru; Umezu, Ikurou; Sugimura, Akira

    2005-01-01

    Pulsed laser ablation (PLA) in an inert background gas is a promising technique for preparing Si nanoparticles. Although an inert gas is appropriate for preparing pure material, a reactive background gas can be used to prepare compound nanoparticles. We performed PLA in hydrogen gas to prepare hydrogenated silicon nanoparticles. The mean diameter of the primary particles measured using transmission electron microscopy was approximately 5 nm. The hydrogen content in the deposits was very high and estimated to be about 20%. The infrared absorption corresponding to Si-H n (n = 1, 2, 3) bonds on the surface were observed at around 2100 cm -1 . The Raman scattering peak corresponding to crystalline Si was observed, and that corresponding to amorphous Si was negligibly small. These results indicate that the Si nanoparticles were not an alloy of Si and hydrogen but Si nanocrystallite (nc-Si) covered by hydrogen or hydrogenated amorphous silicon. This means that PLA in reactive H 2 gas is a promising technique for preparing surface passivated nc-Si. The deposition mechanism and optical properties of the surface passivated silicon nanocrystallites are discussed

  11. Effect of preparation processes and structural insight into the supermolecular system: Bisacodyl and β-cyclodextrin inclusion complex

    International Nuclear Information System (INIS)

    Li, Shanshan; Zhai, Yuanming; Yan, Jin; Wang, Lili; Xu, Kailin; Li, Hui

    2016-01-01

    In this study, β-cyclodextrin (β-CD) and bisacodyl were chosen as model host and guest molecule to explore the effect of preparation processes on the physicochemical properties of inclusion complexes (ICs) and to gain an insight into the structure of ICs. The influence of temperature and pH on complexation was studied by multiple temperature–pH phase solubility analysis. The most favorable conformation was predicted by molecular modeling using AutoDock. "1H nuclear magnetic resonance and rotating frame nuclear Overhauser effect spectroscopy further confirmed the structure. Moreover, bisacodyl·β-CD ICs in solid state were successfully prepared via three different procedures (co-crystallization, co-evaporation, and co-grinding) and fully characterized by several solid-state techniques, namely, Fourier transform infrared spectroscopy, X-ray powder diffraction, thermogravimetric analysis, differential scanning calorimetry, solid-state NMR spectroscopy, and scanning electron microscopy. It was found that acid solution and low temperature were unfavorable for formation of bisacodyl·β-CD. The pyridine moiety was suggested to be enclosed in the hydrophobic cavity of β-CD. The complexes prepared using co-crystallization showed properties similar to those prepared using co-evaporation. Moreover, ICs obtained by co-evaporation and co-grinding had higher loading efficiency, water solubility, and dissolution rate than ICs obtained by co-crystallization. - Highlights: • The structure of inclusion complex-bisacodyl·β-CD was determined. • Thermodynamic behaviors of complexation under different conditions were discussed. • Products from three different preparation methods were systemically compared. • Co-crystallization and co-evaporation produced similar complexes. • Co-evaporation and co-grinding had better effects than co-crystallization.

  12. Effect of preparation processes and structural insight into the supermolecular system: Bisacodyl and β-cyclodextrin inclusion complex

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shanshan [College of Chemical Engineering, Sichuan University, Chengdu 610065 (China); Zhai, Yuanming [Analytical and Testing Center, Sichuan University, Chengdu 610064 (China); Yan, Jin; Wang, Lili; Xu, Kailin [College of Chemical Engineering, Sichuan University, Chengdu 610065 (China); Li, Hui, E-mail: lihuilab@sina.com [College of Chemical Engineering, Sichuan University, Chengdu 610065 (China)

    2016-01-01

    In this study, β-cyclodextrin (β-CD) and bisacodyl were chosen as model host and guest molecule to explore the effect of preparation processes on the physicochemical properties of inclusion complexes (ICs) and to gain an insight into the structure of ICs. The influence of temperature and pH on complexation was studied by multiple temperature–pH phase solubility analysis. The most favorable conformation was predicted by molecular modeling using AutoDock. {sup 1}H nuclear magnetic resonance and rotating frame nuclear Overhauser effect spectroscopy further confirmed the structure. Moreover, bisacodyl·β-CD ICs in solid state were successfully prepared via three different procedures (co-crystallization, co-evaporation, and co-grinding) and fully characterized by several solid-state techniques, namely, Fourier transform infrared spectroscopy, X-ray powder diffraction, thermogravimetric analysis, differential scanning calorimetry, solid-state NMR spectroscopy, and scanning electron microscopy. It was found that acid solution and low temperature were unfavorable for formation of bisacodyl·β-CD. The pyridine moiety was suggested to be enclosed in the hydrophobic cavity of β-CD. The complexes prepared using co-crystallization showed properties similar to those prepared using co-evaporation. Moreover, ICs obtained by co-evaporation and co-grinding had higher loading efficiency, water solubility, and dissolution rate than ICs obtained by co-crystallization. - Highlights: • The structure of inclusion complex-bisacodyl·β-CD was determined. • Thermodynamic behaviors of complexation under different conditions were discussed. • Products from three different preparation methods were systemically compared. • Co-crystallization and co-evaporation produced similar complexes. • Co-evaporation and co-grinding had better effects than co-crystallization.

  13. Gamma Radiation -Induced Preparation of Polymeric Composite Resins and their Structure Assignments

    International Nuclear Information System (INIS)

    El-Zahhar, A.A.; Abdel-Aziz, H.M.; Siyam, T.

    2005-01-01

    Poly(acrylamide-acrylic acid). ethylenediamine tetra acetic acid disodium salt P(AM-AA). EDTANa2, Poly(acrylamide-acrylic acid)montmorillonite P(AM-AA). montmorillonite, and Poly(acrylamide acrylic acid)-potassium nickel hexacyanoferrate P(AM-AA)-KNiHCF were prepared by gamma radiation- induced template polymerization of (AA) on P(AM) as a template polymer in the presence of EDTANa2, Clay(montmorillonite), KNiHCF and KZnHCF, respectively. The capacity of the prepared P (AM-AA)-EDTANa2 and P (AM-AA)-montmorillonite composites increases with increasing of EDTANa2 and montmorillonite concentration then decreases. While the capacity of P(AM- AA). KNiHCF composites increases with increasing of KNiHCF content. The characteristic properties of prepared polymeric composites resins were studied by using FTIR spectroscopy

  14. Effects of sintering temperature on structural and electrical transport properties of zinc ferrites prepared by sol-gel route

    International Nuclear Information System (INIS)

    Anis-ur-Rehman, M.; Malik, M.A.; Ahmad, I.; Nasir, S.; Mubeen, M.; Abdullah, A.

    2011-01-01

    The effects of sintering temperature on the structural and electrical transport properties of nanocrystalline zinc ferrites are reported. The zinc ferrites were prepared by WOWS sol-gel synthesis route. The prepared sample was sintered at temperatures 500 deg. C, 700 deg. C and 900 deg. C respectively for 2 h. X-ray Diffraction (XRD) technique was used to describe the structural properties. The crystallite size, lattice parameters and porosity of samples were measured from the analysis of XRD data. The average crystallite size for each sample was measured using the Scherrer formula by considering the most intense (3 1 1) peak. The dielectric constant (e), dielectric loss tangent (tan theta ) and AC electrical conductivity of nanocrystalline Zn ferrites are investigated as a function of frequency and sintering temperature. All the electrical properties are explained in accordance with MaxwellWagner model and Koops phenomenological theory. (author)

  15. INFLUENCE OF SUBSTRATE TEMPERATURE ON STRUCTURAL, ELECTRICAL AND OPTICAL PROPERTIES OF ITO THIN FILMS PREPARED BY RF MAGNETRON SPUTTERING

    OpenAIRE

    BO HE; LEI ZHAO; JING XU; HUAIZHONG XING; SHAOLIN XUE; MENG JIANG

    2013-01-01

    In this paper, we investigated indium-tin-oxide (ITO) thin films on glass substrates deposited by RF magnetron sputtering using ceramic target to find the optimal condition for fabricating optoelectronic devices. The structural, electrical and optical properties of the ITO films prepared at various substrate temperatures were investigated. The results indicate the grain size increases with substrate temperature increases. As the substrate temperature grew up, the resistivity of ITO films grea...

  16. Influence of soy protein’s structural modifications on their microencapsulation properties: a-tocopherol microparticles preparation

    OpenAIRE

    Nesterenko, Alla; Alric, Isabelle; Silvestre, Françoise; Durrieu, Vanessa

    2012-01-01

    Enzymatic and chemical modifications of soy protein isolate (SPI) were studied in order to improve SPI properties for their use as wall material for a-tocopherol microencapsulation by spray-drying. The structural modifications of SPI by enzymatic hydrolysis and/or N-acylation were carried out in aqueous media without any use of organic solvent neither surfactant. Emulsions from aqueous solutions of native or modified SPI and hydrophobic a-tocopherol, were prepared and spray-dri...

  17. Effect of Preparation Method on Phase Formation Process and Structural and Magnetic Properties of Mn2.5Ge Samples

    Directory of Open Access Journals (Sweden)

    R. Sobhani

    2016-12-01

    Full Text Available In this paper, the phase formation process of Mn2.5Ge samples, prepared by mechanical alloying of Mn and Ge metal powders and annealing, has been studied. Results showed that in the milled samples the stable phase is Mn11Ge8 compound with orthorhombic structure and Pnam space group. The value of saturation magnetization increases by increasing milling time from 0.2 up to 1.95 (Am2Kg-1. The remanece of the samples increases by increasing the milling time while the coercivity decreases. Annealing of 15-hour milled sample results in disappearance of Mn and Ge and the formation of new phases of Mn3Ge, Mn5Ge2, Mn5Ge3 and Mn2.3Ge. Mn3Ge is the main phase with Do22 tetragonal structure and I4/mmm space group which is stable and dominant. The enhancement of saturation magnetization in the annealed sample is related to the formation of three new magnetic phases and the increase of coercivity is due to the presence of Mn3Ge compound with tetragonal structure. Studies were replicated on samples made by arc melting method to compare the results and to investigate the effect of the preparation method on phase formation and structural and magnetic properties of the materials. In these samples the saturation value was in range of 0.2 up to 1.95 (Am2Kg-1 depending on preparation methods. Rietveld refinement shows that Mn2.3Ge sample prepared from arc melted under 620oC anealing is single phase. Magnetic analysis of this sample show a saturation magnetization of 5.252(Am2Kg-1 and 0.005 T coercive field.

  18. Preparation, structures and magnetic properties of Dy/Zr and Ho/Zr two-layers and multi-layers

    International Nuclear Information System (INIS)

    Luche, M.C.

    1993-01-01

    The first part of the report is devoted to the description of the ultra-vacuum evaporation equipment, to the sample preparation conditions and to the characterization of the two-layers and multi-layers through reflection and glancing incidence X diffraction and transmission electron microscopy. In the second part, the magnetic properties of the samples are studied and relations between properties and structures are examined. 37 fig., 35 ref

  19. Structural specifics of the condensate prepared by thermal evaporation of alloys of As2S3-Yb systems

    International Nuclear Information System (INIS)

    Ehfendiev, Eh.G.; Mamedov, A.I.; Il'yasov, T.M.; Rustamov, P.G.

    1987-01-01

    The problem aimed at preparation of the films of As 2 S 3 -Yb system, at studying their substructure depending on condensation conditions and defining noncrystallinity region of this system in the film state, is formulated. It is shown that in representative samples of As 2 S 3 -Yb system the vitrification region is extended up to 7 at.% Yb, in the films noncrystallinity region is extended up to 30 at.% Yb. With up to 30 at.% increase of ytterbium amount in initial alloys a tendency to crystallization in amorphous condensate structure is noticed. In evaporation of As 2 S 3 + 40 at.% Yb and As 2 S 3 + 50 at.% Yb, unknown in the film state YbAs 2 S 4 , Yb 3 As 4 S 9 and YbAs 4 S 7 phases are prepared, and the latter is formed in case of As 2 S 3 + 50 at.% Yb alloy at small evaporation rates (∼10 A/s). Substructure of As 2 S 3 + 50 at.% Yb alloy prepared condensate is more dependent on evaporation rate than in evaporation of As 2 S 3 + 40 at.% Yb alloy. In this case, evaporation rates being ∼ 100 A/s, the condensate has a polycrystal structure, and at small rates of ∼ 10 A/c, condensate structure is primarily blocked

  20. Structure, Impact, and Deficiencies of Beginning Counselor Educators' Doctoral Teaching Preparation

    Science.gov (United States)

    Waalkes, Phillip L.; Benshoff, James M.; Stickl, Jaimie; Swindle, Paula J.; Umstead, Lindsey K.

    2018-01-01

    The authors utilized the consensual qualitative research method (Hill, Thompson, & Williams, [Hill, C. E., 1997]) to explore beginning counselor educators' (N = 9) experiences of doctoral teaching preparation, including helpful and missing components. Emerging themes included a lack of intentionality in teaching-related program design and a…

  1. Ultra structure of oil-in-water emulsions a comparison of different microscopy- and preparation methods

    DEFF Research Database (Denmark)

    Jensen, Louise Helene Søgaard; Loussert, C.; Humbel, B.M.

    of food grade emulsifiers such as whey protein, sodium caseinate and milk phospholipids; layers that are expected to be in the range of only a few nm. Furthermore, the liquid nature and high water content of the samples further complicates the preparation process;especially since water is a major...

  2. Preparation, structure and properties of uniaxially oriented polyethylene-silver nanocomposites

    NARCIS (Netherlands)

    Dirix, Y.J.L.; Bastiaansen, C.W.M.; Caseri, W.R.; Smith, P.

    1999-01-01

    Uniaxially oriented composites of high-density polyethylene and silver nanoparticles were prepared using solution-casting, melt-extrusion and solid-state drawing techniques. The absorption spectrum in the visible wavelength range of the drawn nanocomposites was observed to strongly depend on the

  3. STRUCTURED LEARNING AND TRAINING ENVIRONMENTS--A PREPARATION LABORATORY FOR ADVANCED MAMMALIAN PHYSIOLOGY.

    Science.gov (United States)

    FIEL, NICHOLAS J.; JOHNSTON, RAYMOND F.

    A PREPARATION LABORATORY WAS DESIGNED TO FAMILIARIZE STUDENTS IN ADVANCED MAMMALIAN PHYSIOLOGY WITH LABORATORY SKILLS AND TECHNIQUES AND THUS SHORTEN THE TIME THEY SPEND IN SETTING UP ACTUAL EXPERIMENTS. THE LABORATORY LASTS 30 MINUTES, IS FLEXIBLE AND SIMPLE OF OPERATION, AND DOES NOT REQUIRE A PROFESSOR'S PRESENCE. THE BASIC TRAINING UNIT IS THE…

  4. DoGlycans-Tools for Preparing Carbohydrate Structures for Atomistic Simulations of Glycoproteins, Glycolipids, and Carbohydrate Polymers for GROMACS

    DEFF Research Database (Denmark)

    Danne, Reinis; Poojari, Chetan; Martinez-Seara, Hector

    2017-01-01

    Carbohydrates constitute a structurally and functionally diverse group of biological molecules and macromolecules. In cells they are involved in, e.g., energy storage, signaling, and cell-cell recognition. All of these phenomena take place in atomistic scales, thus atomistic simulation would...... be the method of choice to explore how carbohydrates function. However, the progress in the field is limited by the lack of appropriate tools for preparing carbohydrate structures and related topology files for the simulation models. Here we present tools that fill this gap. Applications where the tools...

  5. Structure, morphology and optical properties of CuInS2 thin films prepared by modulated flux deposition

    International Nuclear Information System (INIS)

    Guillen, C.; Herrero, J.; Gutierrez, M.T.; Briones, F.

    2005-01-01

    The structure, morphology and optical properties of copper indium sulfide thin films prepared by a novel modulated flux deposition procedure have been investigated for layers from 200 to 400 nm thickness. These polycrystalline CuInS 2 films grown onto glass substrates showed CuAu-like structure, similar to epitaxial CuInS 2 films grown onto monocrystalline substrates, and direct band gap values Eg=1.52-1.55 eV, optimum for single-junction photovoltaic applications. The increase in the layer thickness leads to growth of the average crystallite size and increases slightly the surface roughness and the absorption coefficient

  6. EVALUATED NUCLEAR STRUCTURE DATA FILE. A MANUAL FOR PREPARATION OF DATA SETS

    International Nuclear Information System (INIS)

    TULI, J.K.

    2001-01-01

    This manual describes the organization and structure of the Evaluated Nuclear Structure Data File (ENSDF). This computer-based file is maintained by the National Nuclear Data Center (NNDC) at Brookhaven National Laboratory for the international Nuclear Structure and Decay Data Network. For every mass number (presently, A ≤ 293), the Evaluated Nuclear Structure Data File (ENSDF) contains evaluated structure information. For masses A ≥ 44, this information is published in the Nuclear Data Sheets; for A < 44, ENSDF is based on compilations published in the journal Nuclear Physics. The information in ENSDF is updated by mass chain or by nuclide with a varying cycle time dependent on the availability of new information

  7. Structural and optical characteristics of nano-sized structure of Zn0.5Cd0.5S thin films prepared by dip-coating method

    International Nuclear Information System (INIS)

    Rafea, M. Abdel; Farag, A.A.M.; Roushdy, N.

    2009-01-01

    In this work, a stoichiometry Zn 0.5 Cd 0.5 S nano-structured powder was synthesized. Thin films of different thicknesses of Zn 0.5 Cd 0.5 S were prepared by dip-coating method onto glass substrates. The X-ray diffraction analysis of the prepared powder and films were performed to investigate the crystalline structure. Some structural parameters such as the mean crystallite size and the internal lattice strain were calculated. The composition analysis was made by the energy dispersive X-ray technique, EDX. Scanning electron micrographs, SEM showed that the prepared films are nearly homogeneous and consists of nearly parallel surfaces and the thickness was determined by the cross section imaging. The transmission spectra, T(λ), of the films at normal incidence of light were obtained in the spectral region 190-1100 nm. The optical constants of Zn 0.5 Cd 0.5 S films were determined using the interference maxima and minima of the transmission spectrum. The dispersion of refractive index was discussed in terms of the single-oscillator model and the important oscillating parameters were determined. The dependence of absorption coefficient on the photon energy was determined and the analysis of the result showed that the optical transition in Zn 0.5 Cd 0.5 S is allowed and indirect. The thickness dependence of the obtained optical parameters was also considered.

  8. Recent Advances in Preparation, Structure, Properties and Applications of Graphite Oxide.

    Science.gov (United States)

    Srivastava, Suneel Kumar; Pionteck, Jürgen

    2015-03-01

    Graphite oxide, also referred as graphitic oxide or graphitic acid, is an oxidized bulk product of graphite with a variable composition. However, it did not receive immense attention until it was identified as an important and easily obtainable precursor for the preparation of graphene. This inspired many researchers to explore facts related to graphite oxide in exploiting its fascinating features. The present article culminates up-dated review on different preparative methods, morphology and characterization of physical/chemical properties of graphite oxide by XRD, XPS, FTIR, Raman, NMR, UV-visible, and DRIFT analyses. Finally, recent developments on intercalation and applications of GO in multifaceted areas of catalysis, sensor, supercapacitors, water purification, hydrogen storage and magnetic shielding etc. has also been reviewed.

  9. Preparation of chitosan-ferulic acid conjugate: Structure characterization and in the application of pharmaceuticals.

    Science.gov (United States)

    Li, Chen; Li, Jian-Bin

    2017-12-01

    A novel drug delivery system based on chitosan derivatives was prepared by introducting ferulic acid to chitosan adopting a free radical-induced grafting procedure. This paper used an ascorbic acid/hydrogen peroxide redox pair as radical initiator. The chitosan derivative was characterized by Fourier transformed infrared (FTIR), Ultraviolet-visible spectrum (UV), Differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Electron microscopic scanning (SEM). What is more, preparing microcapsules with the chitosan conjugate as wall material, the drug release propertie of chitosan conjugates were compared with that of a blank chitosan, which treated in the same conditions but in the absence of ferulic acid. The study clearly demonstrates that free radical-induced grafting procedure was an effective reaction methods and chitosan-ferulic acid is a potential functionalized carrier material for drug delivery. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Preparation of activated carbon from sorghum pith and its structural and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Senthilkumar, S.T.; Senthilkumar, B. [Solid State Ionics and Energy Devices Laboratory, Department of Physics, Bharathiar University, Coimbatore 641046 (India); Balaji, S. [Materials Laboratory, Thiagarajar Advanced Research Center, Thiagarajar College of Engineering, Madurai 625015 (India); Sanjeeviraja, C. [Department of Physics, Alagappa University, Karaikudi 630003 (India); Kalai Selvan, R., E-mail: selvankram@buc.edu.in [Solid State Ionics and Energy Devices Laboratory, Department of Physics, Bharathiar University, Coimbatore 641046 (India)

    2011-03-15

    Research highlights: {yields} Sorghum pith as the cost effective raw material for activated carbon preparation. {yields} Physicochemical method/KOH activation for preparation of activated carbon is inexpensive. {yields} Activated carbon having lower surface area surprisingly delivered a higher specific capacitance. {yields} Treated at 500 {sup o}C activated carbon exceeds maximum specific capacitances of 320.6 F/g at 10 mV/s. -- Abstract: The cost effective activated carbon (AC) has been prepared from sorghum pith by NaOH activation at various temperatures, including 300 {sup o}C (AC1), 400 {sup o}C (AC2) and 500 {sup o}C (AC3) for the electrodes in electric double layer capacitor (EDLC) applications. The amorphous nature of the samples has been observed from X-ray diffraction and Raman spectral studies. Subsequently, the surface functional groups, surface morphology, pore diameter and specific surface area have been identified through FT-IR, SEM, histogram and N{sub 2} adsorption/desorption isotherm methods. The electrochemical characterization of AC electrodes has been examined using cyclic voltammetry technique in the potential range of -0.1-1.2 V in 1.0 M H{sub 2}SO{sub 4} electrolyte at different scan rates (10, 20, 30, 40, 50 and 100 mV/s). The maximum specific capacitances of 320.6 F/g at 10 mV/s and 222.1 F/g at 100 mV/s have been obtained for AC3 electrode when compared with AC1 and AC2 electrodes. Based on the characterization studies, it has been inferred that the activated carbon prepared from sorghum pith may be one of the innovative carbon electrode materials for EDLC applications.

  11. Preparation, structure and properties of hafnium compounds in the system Hf-C-N-O

    International Nuclear Information System (INIS)

    Brundiers, G.D.

    1975-08-01

    Highly dense, homogenous and single phase hafnium carbonitride samples (with low oxygen content) were prepared in the whole concentration range of the ternary cubic carbonitrides. Stoichiometric hafnium oxicarbides were also prepared within the range of solubility. The procedure involved the hot pressing of powders of HfC, HfN, Hf, Hf-Oxide and carbon at temperatures of 3,000 0 C and pressures up to 550 kpf/cm 2 using a novel technique. Small single crystals of slightly substoichiometric HfN were also repared. The densification of the powders was studied as a function of the non-metal concentration. Carbonitrides with N/Hf ratio of 0.37 were prepared in a high temperature autoclave operating at medium pressures by the reaction of HfC with nitrogen. All the samples were characterized by density measurements, chemical, X-ray and metallographic analysis and in some cases with the aid of quantitative metallography and microprobe analysis. Typical properties investigated were lattice parameter, thermal expansion, microhardness and electrical resistivity as function of the non-metal content. For specific concentrations extreme values in the properties are attained. With the aid of the valence electron concentration (VEC) parameter, the properties can be correlated with the density of states of electrons at the Fermi level. (orig./HK) [de

  12. Morphologies and wetting properties of copper film with 3D porous micro-nano hierarchical structure prepared by electrochemical deposition

    International Nuclear Information System (INIS)

    Wang, Hongbin; Wang, Ning; Hang, Tao; Li, Ming

    2016-01-01

    Highlights: • A 3D porous micro-nano hierarchical structure Cu films were prepared. • The evolution of morphology and wettability with deposition time was reported. • The effects of EDA on the microscopic morphology were revealed. • A high contact angle of 162.1° was measured when deposition time is 5 s. • The mechanism of super-hydrophobicity was illustrated by two classical models. - Abstract: Three-dimensional porous micro-nano hierarchical structure Cu films were prepared by electrochemical deposition with the Hydrogen bubble dynamic template. The morphologies of the deposited films characterized by Scanning Electronic Microscopy (SEM) exhibit a porous micro-nano hierarchical structure, which consists of three levels in different size scales, namely the honeycomb-like microstructure, the dendritic substructure and the nano particles. Besides, the factors which influenced the microscopic morphology were studied, including the deposition time and the additive Ethylene diamine. By measuring the water contact angle, the porous copper films were found to be super-hydrophobic. The maximum of the contact angles could reach as high as 162.1°. An empirical correlation between morphologies and wetting properties was revealed for the first time. The pore diameter increased simultaneously with the deposition time while the contact angle decreased. The mechanism was illustrated by two classical models. Such super-hydrophobic three-dimensional hierarchical micro-nano structure is expected to have practical application in industry.

  13. A simple structure of Cu2ZnSnS4/CdS solar cells prepared by sputtering

    Science.gov (United States)

    Li, Zhishan; Wang, Shurong; Ma, Xun; Yang, Min; Jiang, Zhi; Liu, Tao; Lu, Yilei; Liu, Sijia

    2017-12-01

    In this work, Cu2ZnSnS4 (CZTS) thin films were grown on Mo-coated Soda-lime-glass (SLG) substrates by annealing of sputtered ZnS/Sn/CuS precursors at 580 ℃ for 15 min. As a try, the CZTS solar cells were fabricated using simple structure of Mo-coated SLG/CZTS/CdS/Al and traditional structure of Mo-coated SLG/CZTS/CdS/i-ZnO/In2O3:SnO2 (ITO)/Al, respectively. The results show that the CZTS device with simple structure can achieve same level of the open circuit voltage (Voc) compared with that of traditional structure. In addition, the power conversion efficiency of 2.95% and 3.59% were obtained with simple structure and traditional structure, respectively. The CZTS solar cell with simple structure provides a promising way and an easy process to prepare high-performance CZTS thin film solar cells which is available to large-scale industrial production in the future.

  14. Key Techniques on Preparing High Aspect Ratio Micro and Nano Structures

    DEFF Research Database (Denmark)

    Jian, Zhao; Lianhe, Dong; Xiaoli, Zhu

    2016-01-01

    effectively. The mechanism of action between NaCl and HSQ was analyzed. The collapse and adhesion of resist structure due to the effect of gas-liquid interfacial capillary surface tension were suppressed by the CO2 supercritical drying method. Large-area dense nano-structures with the aspect ratio of 12...

  15. On the crystal structure of colloidally prepared CsPbBr3 quantum dots.

    Science.gov (United States)

    Cottingham, Patrick; Brutchey, Richard L

    2016-04-18

    Colloidally synthesized quantum dots of CsPbBr3 are highly promising for light-emitting applications. Previous reports based on benchtop diffraction conflict as to the crystal structure of CsPbBr3 quantum dots. We present X-ray diffraction and PDF analysis of X-ray total scattering data that indicate that the crystal structure is unequivocally orthorhombic (Pnma).

  16. Structural and optical properties of nano-structured CdS thin films prepared by chemical bath deposition

    Energy Technology Data Exchange (ETDEWEB)

    Bai, Rekha, E-mail: rekha.mittal07@gmail.com; Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K. [Thin Film Laboratory, Physics Department, Indian Institute of Technology Delhi, New Delhi-110016 (India)

    2016-05-06

    Cadmium sulfide (CdS) thin films have been deposited on conducting glass substrates by chemical bath deposition (CBD) technique. The effect of precursor concentration on the structural, morphological, compositional, and optical properties of the CdS films has been studied. Crystal structure of these CdS films is characterized by X-ray diffraction (XRD) and it reveals polycrystalline structure with mixture of cubic and wurtzite phases with grain size decreasing as precursor concentration is increased. Optical studies reveal that the CdS thin films have high transmittance in visible spectral region reaching 90% and the films possess direct optical band gap that decreases from 2.46 to 2.39 eV with decreasing bath concentration. Our study suggests that growth is nucleation controlled.

  17. Structural and optical properties of nano-structured CdS thin films prepared by chemical bath deposition

    International Nuclear Information System (INIS)

    Bai, Rekha; Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K.

    2016-01-01

    Cadmium sulfide (CdS) thin films have been deposited on conducting glass substrates by chemical bath deposition (CBD) technique. The effect of precursor concentration on the structural, morphological, compositional, and optical properties of the CdS films has been studied. Crystal structure of these CdS films is characterized by X-ray diffraction (XRD) and it reveals polycrystalline structure with mixture of cubic and wurtzite phases with grain size decreasing as precursor concentration is increased. Optical studies reveal that the CdS thin films have high transmittance in visible spectral region reaching 90% and the films possess direct optical band gap that decreases from 2.46 to 2.39 eV with decreasing bath concentration. Our study suggests that growth is nucleation controlled.

  18. Investigation of the composition-structure-property relationship of AsxTe100 - x films prepared by plasma deposition

    Science.gov (United States)

    Mochalov, Leonid; Dorosz, Dominik; Nezhdanov, Aleksey; Kudryashov, Mikhail; Zelentsov, Sergey; Usanov, Dmitry; Logunov, Alexandr; Mashin, Aleksandr; Gogova, Daniela

    2018-02-01

    AsxTe100 - x amorphous films of different chemical content were prepared by Plasma-Enhanced Chemical Vapor Deposition (PECVD). For the first time the optical properties of As-Te chalcogenide materials have been measured in UV-VIS-IR ranges (from 0.2 to 25 μm) for a very wide range of chemical compositions (20-80 at.% As). As-Te films have been tuned from 0.80 to 1.10 eV. The IR results obtained have been juxtaposed with the Raman spectroscopy findings to establish the correlation between optical and structural properties of the materials developed. Reversible and irreversible changes in the phase composition of the As-Te films under annealing of the surface by laser irradiation have been demonstrated and studied. In order to determine the potential areas of application of the prepared As-Te films the thermal and photo sensitivity has been also investigated.

  19. Preparation and structural characterisation of novel and versatile amphiphilic octenyl succinic anhydride-modified hyaluronic acid derivatives

    DEFF Research Database (Denmark)

    Eenschooten, Corinne Diane; Guillaumie, Fanny; Kontogeorgis, Georgios

    2010-01-01

    and structurally characterised by Fourier transform-infrared spectroscopy and proton nuclear magnetic resonance spectroscopy (1H NMR). The influence of four reaction parameters on the DS of the derivatives was studied by means of an experimental design. The results showed that the OSA/HA molar ratio, the buffer......The purpose of the present study was to prepare amphiphilic hyaluronic acid (HA) derivatives and to study the influence of a selection of reaction parameters on the degree of substitution (DS) of the derivatives. Octenyl succinic anhydride (OSA)–modified HA (OSA–HA) derivatives were prepared...... (NaHCO3) concentration and their interaction had the largest influence while the HA concentration and the reaction time only had a negligible effect. According to 1H NMR the maximum DS achieved within the experimental conditions tested was 43% per disaccharide unit. Moreover optimal reaction...

  20. General method of preparation of uniformly 13C, 15N-labeled DNA fragments for NMR analysis of DNA structures

    International Nuclear Information System (INIS)

    Rene, Brigitte; Masliah, Gregoire; Zargarian, Loussine; Mauffret, Olivier; Fermandjian, Serge

    2006-01-01

    Summary 13 C, 15 N labeling of biomolecules allows easier assignments of NMR resonances and provides a larger number of NMR parameters, which greatly improves the quality of DNA structures. However, there is no general DNA-labeling procedure, like those employed for proteins and RNAs. Here, we describe a general and widely applicable approach designed for preparation of isotopically labeled DNA fragments that can be used for NMR studies. The procedure is based on the PCR amplification of oligonucleotides in the presence of labeled deoxynucleotides triphosphates. It allows great flexibility thanks to insertion of a short DNA sequence (linker) between two repeats of DNA sequence to study. Size and sequence of the linker are designed as to create restriction sites at the junctions with DNA of interest. DNA duplex with desired sequence and size is released upon enzymatic digestion of the PCR product. The suitability of the procedure is validated through the preparation of two biological relevant DNA fragments

  1. Structural and morphological properties of HfxZr 1-xO2 thin films prepared by Pechini route

    KAUST Repository

    García-Cerda, L. A.

    2010-03-01

    In this study, HfxZr1-xO2 (0 < x < 1) thin films were deposited on silicon wafers using a dip-coating technique and by using a precursor solution prepared by the Pechini route. The effects of annealing temperature on the structure and morphological properties of the proposed films were investigated. HfxZr1-xO2 thin films with 1, 3 and 5 layers were annealed in air for 2 h at 600 and 800 °C and the structural and morphological properties studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD results show that the films have monoclinic and tetragonal structure depending of the Hf and Zr concentration. SEM photographs show that all films consist of nanocrystalline grains with sizes in the range of 6 - 13 nm. The total film thickness is about 90 nm. © (2010) Trans Tech Publications.

  2. Structural analysis of highly-durable Si-O-C composite anode prepared by electrodeposition for lithium secondary batteries

    International Nuclear Information System (INIS)

    Nara, Hiroki; Yokoshima, Tokihiko; Otaki, Mitsutoshi; Momma, Toshiyuki; Osaka, Tetsuya

    2013-01-01

    The structure of the highly durable silicon-based anode prepared by electrodeposition was investigated for volume change and chemical structure. With repeated charge–discharge cycles, the volume change resulting from the anode film thickness decreased, and, after 100 cycles, essentially no difference was observed between the charged and discharged states. The buffering effect of the volume change was considered to be achieved by the formation of Li 2 O, Li 2 CO 3 , and lithium silicates such as Li 4 SiO 4 , whose existence were supported by STEM, EELS, and XPS analyses. From the structural analyses, the main reactions related to the capacity of the silicon-based anode were considered to be the formation of Li x Si and Li 2 Si 2 O 5 . Li x Si and Li 2 Si 2 O 5 can be delithiated into Si and SiO 2 , respectively

  3. Chemical state and phase structure of (TaNbTiW)N films prepared by combined magnetron sputtering and PBII

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Xingguo [State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001 (China); Tang, Guangze [National Key Laboratory of Materials Behavior and Evaluation in Space Environment, Harbin Institute of Technology, Harbin 150001 (China); Sun, Mingren [National Key Laboratory of Science and Technology on Precision Hot Processing of Metals Harbin Institute of Technology, Harbin Institute of Technology, Harbin 150001 (China); Ma, Xinxin, E-mail: maxin@hit.edu.cn [State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001 (China); Wang, Liqin [School of Mechatronics Engineering, Harbin Institute of Technology, Harbin, 150001 (China)

    2013-09-01

    (TaNbTiW)N films with thickness of ∼1000 nm are prepared on titanium alloy substrate by combined magnetron sputtering deposition and nitrogen plasma based ion implantation (N-PBII). Chemical state of the elements and phase structure of the films are investigated using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), respectively. The bonds of Ta-N, Nb-N, Ti-N-O and Ta-O are detected in the (TaNbTiW)N films, however both W-N and W-O are not found. The initial alloy film has a BCC structure, while the films with N-PBII treatment are composed of BCC and FCC structures. The hardness and elastic modulus of the films can be improved by increasing nitrogen implantation dose and reach maximum values of 9.0 GPa and 154.1 GPa, respectively.

  4. Structural, morphological and catalytic characterization of neutral Ag salt of 12-tungstophosphoric acid: Influence of preparation conditions

    Energy Technology Data Exchange (ETDEWEB)

    Holclajtner-Antunović, Ivanka; Bajuk-Bogdanović, Danica [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Popa, Alexandru [Institute of Chemistry Timişoara, Bl. Mihail Viteazul 24, 300223 Timişoara (Romania); Nedić Vasiljević, Bojana [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Krstić, Jugoslav [Institute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11001 Belgrade (Serbia); Mentus, Slavko [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Uskoković-Marković, Snežana, E-mail: snezaum@pharmacy.bg.ac.rs [Faculty of Pharmacy, University of Belgrade, Vojvode Stepe 450, 11221 Belgrade (Serbia)

    2015-02-15

    Graphical abstract: - Highlights: • Preparation conditions influence to self-assembly of nanocrystallites of Ag{sub 3}PW{sub 12}O{sub 40}. • Ag{sub 3}PW{sub 12}O{sub 40} obtained by filtration is microporous, Ag{sub 3}PW{sub 12}O{sub 40} obtained by evaporation is non-porous. • Thermal properties of Ag{sub 3}PW{sub 12}O{sub 40}, H{sub 3}PW{sub 12}O{sub 40} and its soluble salts are similar. - Abstract: The objective of this study is the structural and morphological characterization of the Ag{sub 3}PW{sub 12}O{sub 40} salts (AgWPA) of 12-tungstophosphoric acid (WPA) obtained under different preparation conditions and testing of their acid catalytic activity in dehydration of ethanol. The structure, morphology and physicochemical characteristics were determined by Fourier transform infrared (FT-IR) and Raman spectroscopy, X-ray diffraction (XRD), nitrogen physisorption at −196 °C, scanning electron microscopy (SEM) and differential thermal (DTA) and thermogravimetric analysis (TGA). It is shown that the preparation process has a significant influence on the morphological properties of the obtained materials which may be explained by the supposed mechanism of the formation of nanocrystallite′s aggregates with more or less epitaxial connection. Neutral AgWPA obtained by filtration from supernatant forms porous aggregates of a symmetric dodecahedral shape, having average sizes about 2 μm. This sample shows higher specific area in comparison with the salt obtained by evaporation due to the higher micropore volume, while mesopore volumes are the same for both salts. Thus conversion of ethanol and selectivities of the main products, ethylene and diethyl ether, are almost the same and constant for both prepared salts, while their values are changed over the reaction time for the parent WPA acid.

  5. Influence of preparation technique of ceramic superconductors on structure, mechanical and electrical properties

    International Nuclear Information System (INIS)

    Tomandl, G.; Kohl, R.

    1991-01-01

    Sol-Gel-like preparation techniques using citrate-, citrate/ethylenglycol- as well as ethylhexanoate precursors and the addition of fluorine were tested with regard to homogeneity and properties of HTSC-ceramics. A few single- and polycrystalline materials were coated with YBaCuOxide- and Bi Sr Ca Cu Oxide-films using ethylhexanoate-precursors. Interdiffusion reactions were investigated affecting the electrical properties. The best results in YBaCuOxide system were obtained using polycrystalline magnesia and silver as substrate materials. Bulk ceramics with a high degree of orientation were fabricated by reaction sintering and simultaneous external pressure. (orig.) With 44 refs., 6 tabs., 81 figs [de

  6. A green method for the preparation of fluorescent hybrid structures of gold and corrole

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Ângela S., E-mail: aspereira@ua.pt; Barata, Joana F. B. [University of Aveiro, CICECO – Chemistry Department, Aveiro Institute of Materials (Portugal); Vaz Serra, Vanda I. R. C. [University of Aveiro, QOPNA Chemistry Department (Portugal); Pereira, Sérgio; Trindade, Tito [University of Aveiro, CICECO – Chemistry Department, Aveiro Institute of Materials (Portugal)

    2015-10-15

    Gold/soap nanostructures were prepared by a green methodology using saponified household sunflower oil, as reducing and organic dispersing agent of auric acid. The incorporation of hydrophobic molecules on the novel water-soluble gold nanoparticles was followed by fluorescence lifetime imaging microscopy, using as model hydrophobic compound 5,10,15-tris-(pentafluorophenyl)corrolatogallium(III)(pyridine) (GaPFC), a highly fluorescent corrole. The results showed the hydrophobic GaPFC located between the organic bilayer surrounding several Au nanoparticles, which in turn were coated with fatty acids salts anchored by the double bond at the gold’s surface.

  7. Facile method for preparing superoleophobic surfaces with hierarchical microcubic/nanowire structures

    Science.gov (United States)

    Kwak, Wonshik; Hwang, Woonbong

    2016-02-01

    To facilitate the fabrication of superoleophobic surfaces having hierarchical microcubic/nanowire structures (HMNS), even for low surface tension liquids including octane (surface tension = 21.1 mN m-1), and to understand the influences of surface structures on the oleophobicity, we developed a convenient method to achieve superoleophobic surfaces on aluminum substrates using chemical acid etching, anodization and fluorination treatment. The liquid repellency of the structured surface was validated through observable experimental results the contact and sliding angle measurements. The etching condition required to ensure high surface roughness was established, and an optimal anodizing condition was determined, as a critical parameter in building the superoleophobicity. The microcubic structures formed by acid etching are essential for achieving the formation of the hierarchical structure, and therefore, the nanowire structures formed by anodization lead to an enhancement of the superoleophobicity for low surface tension liquids. Under optimized morphology by microcubic/nanowire structures with fluorination treatment, the contact angle over 150° and the sliding angle less than 10° are achieved even for octane.

  8. Structural, dielectric and magnetic properties of cobalt ferrite prepared using auto combustion and ceramic route

    International Nuclear Information System (INIS)

    Murugesan, C.; Perumal, M.; Chandrasekaran, G.

    2014-01-01

    Cobalt ferrite is synthesized by using low temperature auto combustion and high temperature ceramic methods. The prepared samples have values of lattice constant equal to 8.40 Å and 8.38 Å for auto combustion and ceramic methods respectively. The FTIR spectrum of samples of the auto combustion method shows a high frequency vibrational band at 580 cm −1 assigned to tetrahedral site and a low frequency vibrational band at 409 cm −1 assigned to octahedral site which are shifted to 590 cm −1 and 412 cm −1 for the ceramic method sample. SEM micrographs of samples show a substantial difference in surface morphology and size of the grains between the two methods. The frequency dependent dielectric constant and ac conductivity of the samples measured from 1 Hz to 2 MHz at room temperature are reported. The room temperature magnetic hysteresis parameters of the samples are measured using VSM. The measured values of saturation magnetization, coercivity and remanent magnetization are 42 emu/g, 1553 Oe, 18.5 emu/g for the auto combustion method, 66.7 emu/g, 379.6 Oe, and 17.3 emu/g for the ceramic method, respectively. The difference in preparation methods and size of the grains causes interesting changes in electrical and magnetic properties

  9. Preparation and Characterization of Surface Photocatalytic Activity with NiO/TiO2 Nanocomposite Structure

    Directory of Open Access Journals (Sweden)

    Jian-Zhi Chen

    2015-07-01

    Full Text Available This study achieved a nanocomposite structure of nickel oxide (NiO/titanium dioxide (TiO2 heterojunction on a TiO2 film surface. The photocatalytic activity of this structure evaluated by decomposing methylene blue (MB solution was strongly correlated to the conductive behavior of the NiO film. A p-type NiO film of high concentration in contact with the native n-type TiO2 film, which resulted in a strong inner electrical field to effectively separate the photogenerated electron-hole pairs, exhibited a much better photocatalytic activity than the controlled TiO2 film. In addition, the photocatalytic activity of the NiO/TiO2 nanocomposite structure was enhanced as the thickness of the p-NiO film decreased, which was beneficial for the migration of the photogenerated carriers to the structural surface.

  10. Preparation and Characterization of Surface Photocatalytic Activity with NiO/TiO₂ Nanocomposite Structure.

    Science.gov (United States)

    Chen, Jian-Zhi; Chen, Tai-Hong; Lai, Li-Wen; Li, Pei-Yu; Liu, Hua-Wen; Hong, Yi-You; Liu, Day-Shan

    2015-07-13

    This study achieved a nanocomposite structure of nickel oxide (NiO)/titanium dioxide (TiO₂) heterojunction on a TiO₂ film surface. The photocatalytic activity of this structure evaluated by decomposing methylene blue (MB) solution was strongly correlated to the conductive behavior of the NiO film. A p -type NiO film of high concentration in contact with the native n -type TiO₂ film, which resulted in a strong inner electrical field to effectively separate the photogenerated electron-hole pairs, exhibited a much better photocatalytic activity than the controlled TiO₂ film. In addition, the photocatalytic activity of the NiO/TiO₂ nanocomposite structure was enhanced as the thickness of the p -NiO film decreased, which was beneficial for the migration of the photogenerated carriers to the structural surface.

  11. Structural and Optical Properties of Eu Doped ZnO Nanorods prepared by Pulsed Laser Deposition

    KAUST Repository

    Alarawi, Abeer

    2014-01-01

    Nano structured wide band gap semiconductors have attracted attention of many researchers due to their potential electronic and optoelectronic applications. In this thesis, we report successful synthesis of well aligned Eu doped ZnO nano

  12. On the structure and surface chemical composition of indium-tin oxide films prepared by long-throw magnetron sputtering

    International Nuclear Information System (INIS)

    Chuang, M.J.; Huang, H.F.; Wen, C.H.; Chu, A.K.

    2010-01-01

    Structures and surface chemical composition of indium tin oxide (ITO) thin films prepared by long-throw radio-frequency magnetron sputtering technique have been investigated. The ITO films were deposited on glass substrates using a 20 cm target-to-substrate distance in a pure argon sputtering environment. X-ray diffraction results showed that an increase in substrate temperature resulted in ITO structure evolution from amorphous to polycrystalline. Field-emission scanning electron microscopy micrographs suggested that the ITO films were free of bombardment of energetic particles since the microstructures of the films exhibited a smaller grain size and no sub-grain boundary could be observed. The surface composition of the ITO films was characterized by X-ray photoelectron spectroscopy (XPS). Oxygen atoms in both amorphous and crystalline ITO structures were observed from O 1 s XPS spectra. However, the peak of the oxygen atoms in amorphous ITO phase could only be found in samples prepared at low substrate temperatures. Its relative peak area decreased drastically when substrate temperatures were larger than 200 o C. In addition, a composition analysis from the XPS results revealed that the films deposited at low substrate temperatures contained high concentration of oxygen at the film surfaces. The oxygen-rich surfaces can be attributed to hydrolysis reactions of indium oxides, especially when large amount of the amorphous ITO were developed near the film surfaces.

  13. Preparation of core-shell structured CaCO3 microspheres as rapid and recyclable adsorbent for anionic dyes

    Science.gov (United States)

    Zhao, Mengen; Chen, Zhenhua; Lv, Xinyan; Zhou, Kang; Zhang, Jie; Tian, Xiaohan; Ren, Xiuli; Mei, Xifan

    2017-09-01

    Core-shell structured CaCO3 microspheres (MSs) were prepared by a facile, one-pot method at room temperature. The adsorbent dosage and adsorption time of the obtained CaCO3 MSs were investigated. The results suggest that these CaCO3 MSs can rapidly and efficiently remove 99-100% of anionic dyes within the first 2 min. The obtained CaCO3 MSs have a high Brunauer-Emmett-Teller surface area (211.77 m2 g-1). In addition, the maximum adsorption capacity of the obtained CaCO3 MSs towards Congo red was 99.6 mg g-1. We also found that the core-shell structured CaCO3 MSs have a high recycling capability for removing dyes from water. Our results demonstrate that the prepared core-shell structured CaCO3 MSs can be used as an ideal, rapid, efficient and recyclable adsorbent to remove dyes from aqueous solution.

  14. Lack of immunogenicity of ice structuring protein type III HPLC12 preparation administered by the oral route to human volunteers

    DEFF Research Database (Denmark)

    Crevel, R W R; Cooper, K J; Poulsen, Lars K.

    2007-01-01

    Before a novel protein can be used in foods, its potential allergenicity must be assessed. In this study, healthy volunteers consumed ice structuring protein (ISP) Type III preparation or a control material 5 days a week for a total of 8 weeks. General measures of health were recorded during...... background against which to interpret the results. Nevertheless, the absence of an immune response using a protocol which could have been expected to result in a response with a strongly immunogenic protein, confirms the conclusions of earlier published work, and attests to the lack of allergenicity of ISP...

  15. Structural and optical characterization of In_2O_3/PANI nanocomposite prepared by in-situ polymerization

    International Nuclear Information System (INIS)

    Janeoo, Shashi; Sharma, Mamta; Goswamy, J.; Singh, Gurinder

    2016-01-01

    Polyaniline-indium oxide (In_2O_3/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In_2O_3 nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In_2O_3/PANI nanocomposite. TEM analysis shows In_2O_3 nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In_2O_3 nanoparticles. The band gap and electronic transitions in In_2O_3/PANI nanocomposite is determined by using UV/Vis spectra.

  16. Novel selenium containing boro-phosphate glasses: Preparation and structural study

    International Nuclear Information System (INIS)

    Ciceo-Lucacel, R.; Radu, T.; Ponta, O.; Simon, V.

    2014-01-01

    We synthesized a new boro-phosphate glass system with different %mol SeO 2 content by conventional melt quenching technique. All samples were obtained in a glassy state with the vitreous structure confirmed by X-ray diffraction analysis. Scanning electron microscopy (SEM) revealed some non-homogeneous domains on the glasses surface, and their tendency to link each other once the selenium oxide content increases. Energy-dispersive X-ray analysis (EDAX) indicated similar elemental composition in different regions of each sample. X-ray photoelectron spectroscopy (XPS) was used to determine the nature of chemical bonding and the elemental composition at the sample surfaces, and Fourier transform infrared (FT-IR) spectroscopy was used to determine the structural groups in the obtained glass structure. Based on FT-IR results, the glass structure at short range order consists mainly of small phosphate units such as pyrophosphate (i.e. P 2 O 7 4− dimmers or terminating groups at the end of phosphate chains) and some metaphosphate (i.e. PO 3 − middle groups in the phosphate chains) units. The boron atoms are mainly placed in three-coordinated sites in BØ 3 or BØ 2 O − units. A small contribution of BØ 4 − units was also detected from the FT-IR spectra of glasses. For SeO 2 content higher than 5 mol%, the modifier role of selenium ions is strongly reflected on the local structure dominated in this case by pyrophosphate units. - Highlights: • New P 2 O 5 -CaO-B 2 O 3 -SeO 2 glasses synthesized by conventional melt quenching method. • Evidences for the Se ions modifier role in the local structure by FT-IR and XPS. • Significant advances in understanding the structural properties of the new system

  17. CdWO4 polymorphs: Selective preparation, electronic structures, and photocatalytic activities

    International Nuclear Information System (INIS)

    Yan, Tingjiang; Li, Liping; Tong, Wenming; Zheng, Jing; Wang, Yunjian; Li, Guangshe

    2011-01-01

    This work explored the selective synthesis of polymorphs of CdWO 4 in either tetragonal or monoclinic phase by optimizing the experimental parameters. Systematic characterization indicated that both polymorphs possessed similar spherical morphologies but different structural building blocks. Electronic structures calculations for both polymorphs demonstrated the same constructions of conduction band or valence band, while the conduction band widths of both polymorphs were quite different. Both CdWO 4 polymorphs exhibited good photocatalytic activity for degradation of methyl orange under UV light irradiation. When comparing to some other well-known tungstate oxide materials, the photocatalytic activity was found to follow such a consequence, monoclinic CdWO 4 ∼monoclinic ZnWO 4 >tetragonal CdWO 4 >tetragonal CaWO 4 . The specific photocatalytic activity of monoclinic CdWO 4 was even higher than that of commercial TiO 2 photocatalyst (Degussa P25). The increased activity from the tetragonal CdWO 4 to the monoclinic was consistent with the trend of the decreased symmetry, and this could be explained in terms of the geometric structures and electronic structures for both polymorphs. -- Graphical abstract: Monoclinic CdWO 4 exhibited a much higher photocatalytic activity than the tetragonal form owing to the lower symmetry, more distorted geometric structure, and the dispersive band configuration. Display Omitted Research highlights: → Polymorphs of CdWO 4 in either tetragonal or monoclinic phase were selectively synthesized. → Both polymorphs possessed similar spherical morphologies, while the relevant structural building blocks were different. → Photocatalytic activities of CdWO 4 polymorphs depended strongly on the symmetry, geometric structure, as well as band configuration.

  18. Properties of three-dimensional structures prepared by Ge dewetting from Si(111) at high temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Shklyaev, Alexander, E-mail: shklyaev@isp.nsc.ru [A. V. Rzhanov Institute of Semiconductor Physics, SB RAS, Novosibirsk 630090 (Russian Federation); Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Bolotov, Leonid; Poborchii, Vladimir; Tada, Tetsuya [National Institute of Advanced Industrial Science and Technology, Higashi 1-1-1, Tsukuba, Ibaraki 305-8562 (Japan)

    2015-05-28

    The formation of three-dimensional (3D) structures during Ge deposition on Si(111) at about 800 °C is studied with scanning tunneling, Kelvin probe and electron microscopies, and scanning tunneling and Raman spectroscopies. The observed surface morphology is formed by dewetting of Ge from Si(111), since it occurs mainly by means of minimization of surface and interfacial energies. The dewetting proceeds through massive Si eroding around growing 3D structures, providing them to be composed of SiGe with about a 30% Ge content, and leads to the significant reduction of the SiGe/Si interface area. It is found that the SiGe top component of 3D structures forms sharp interfaces with the underlying Si. The minimization of interfacial and strain energies occurs on the way that the 3D structures appear to get the dendrite-like shape. The Ge distribution in the 3D SiGe structures is inhomogeneous in the lateral dimension with a higher Ge concentration in their central areas and Ge segregation on their surface.

  19. CTAB assisted hydrothermal preparation of YPO4:Tb3+ with controlled morphology, structure and enhanced photoluminescence

    International Nuclear Information System (INIS)

    Lai, Hua; Du, Ying; Zhao, Min; Sun, Kening; Yang, Lei

    2014-01-01

    Highlights: • A simple and convenient method toward fabrication of YPO 4 :Tb 3+ with controlled structures and morphologies was proposed. • The crucial role of CTAB during the fabrication process that acts as complexing reagent and inducing agent and the mechanism was discussed. • The addition of CTAB enhances the green emission in YPO 4 :Tb phosphors. -- Abstract: In this paper, we report a simple and convenient method toward fabrication of YPO 4 :Tb 3+ with controlled structures, morphologies and enhanced luminescent properties. By simply controlling the amount of the cetyltrimethyl ammonium bromide (CTAB) during the hydrothermal process, tetragonal YPO 4 :Tb 3+ and hexagonal YPO 4 ·0.8H 2 O:Tb 3+ with nanoparticle and olive-like nanoparticle can be obtained, respectively. Meanwhile, we find that the structures and morphologies can affect their luminescent properties obviously and the intensity of the samples with hexagonal phase is evidently higher than that with tetragonal phase. The variation of crystal structures, morphologies of the samples are ascribed to the crucial role of CTAB during the fabrication process that acts as complexing reagent and inducing agent and the mechanism was also discussed. We believe the method reported here will open a novel approach to rare earth phosphates with multiple structures

  20. Properties of three-dimensional structures prepared by Ge dewetting from Si(111) at high temperatures

    International Nuclear Information System (INIS)

    Shklyaev, Alexander; Bolotov, Leonid; Poborchii, Vladimir; Tada, Tetsuya

    2015-01-01

    The formation of three-dimensional (3D) structures during Ge deposition on Si(111) at about 800 °C is studied with scanning tunneling, Kelvin probe and electron microscopies, and scanning tunneling and Raman spectroscopies. The observed surface morphology is formed by dewetting of Ge from Si(111), since it occurs mainly by means of minimization of surface and interfacial energies. The dewetting proceeds through massive Si eroding around growing 3D structures, providing them to be composed of SiGe with about a 30% Ge content, and leads to the significant reduction of the SiGe/Si interface area. It is found that the SiGe top component of 3D structures forms sharp interfaces with the underlying Si. The minimization of interfacial and strain energies occurs on the way that the 3D structures appear to get the dendrite-like shape. The Ge distribution in the 3D SiGe structures is inhomogeneous in the lateral dimension with a higher Ge concentration in their central areas and Ge segregation on their surface

  1. Structural and magnetic properties of Fe-Al silica composites prepared by sequential ion implantation

    International Nuclear Information System (INIS)

    Julian Fernandez, C. de; Tagliente, M.A.; Mattei, G.; Sada, C.; Bello, V.; Maurizio, C.; Battaglin, G.; Sangregorio, C.; Gatteschi, D.; Tapfer, L.; Mazzoldi, P.

    2004-01-01

    The nanostructural and magnetic properties of Fe-Al/SiO 2 granular solids prepared by ion implantation have been investigated. A strong effect of the implantation order of the Fe and Al ions has been evidenced. By implanting first the Al ions and later Fe ions, 5-40 nm core-shell nanoparticles are formed with a magnetic behavior similar to that of Fe. The lattice parameter of the nanoparticles is consistent with that of the α-Fe. By changing the implantation order, 10-15 nm core-shell nanoparticles of a bcc Fe-based phase with a lattice 2.5% smaller than that of α-Fe are formed. The temperature dependence of the magnetization indicates a superparamagnetic behavior

  2. Structural and magnetic properties of Fe-Al silica composites prepared by sequential ion implantation

    Energy Technology Data Exchange (ETDEWEB)

    Julian Fernandez, C. de E-mail: dejulian@padova.infm.it; Tagliente, M.A.; Mattei, G.; Sada, C.; Bello, V.; Maurizio, C.; Battaglin, G.; Sangregorio, C.; Gatteschi, D.; Tapfer, L.; Mazzoldi, P

    2004-02-01

    The nanostructural and magnetic properties of Fe-Al/SiO{sub 2} granular solids prepared by ion implantation have been investigated. A strong effect of the implantation order of the Fe and Al ions has been evidenced. By implanting first the Al ions and later Fe ions, 5-40 nm core-shell nanoparticles are formed with a magnetic behavior similar to that of Fe. The lattice parameter of the nanoparticles is consistent with that of the {alpha}-Fe. By changing the implantation order, 10-15 nm core-shell nanoparticles of a bcc Fe-based phase with a lattice 2.5% smaller than that of {alpha}-Fe are formed. The temperature dependence of the magnetization indicates a superparamagnetic behavior.

  3. Synthesis, structural characterization and scalable preparation of new amino-zinc borates

    Energy Technology Data Exchange (ETDEWEB)

    Imer, M. R. [Departamento Estrella Campos; Facultad de Química; Universidad de la República; Montevideo; Uruguay; González, M. [Departamento Estrella Campos; Facultad de Química; Universidad de la República; Montevideo; Uruguay; Veiga, N. [Departamento Estrella Campos; Facultad de Química; Universidad de la República; Montevideo; Uruguay; Kremer, C. [Departamento Estrella Campos; Facultad de Química; Universidad de la República; Montevideo; Uruguay; Suescun, L. [Laboratorio de Cristalografía; Química del Estado Sólido y Materiales; Cátedra de Física; DETEMA; Facultad de Química; Arizaga, L. [Departamento Estrella Campos; Facultad de Química; Universidad de la República; Montevideo; Uruguay

    2017-01-01

    Zinc borates are important materials. We report the preparation of three novel ones: [Zn(NH3)3B4O5(OH)4]·H2O (ZB1), Zn3(H2B3O7)2·2NH3·4H2O (ZB2), and [Zn(NH3)4][B4O5(OH)4]·4H2O (ZB3).

  4. Structure, morphology and electrochemical behaviour of manganese oxides prepared by controlled decomposition of permanganate

    Energy Technology Data Exchange (ETDEWEB)

    Donne, S.W.; Jones, B.C. [Discipline of Chemistry, University of Newcastle, Callaghan, NSW 2308 (Australia); Hollenkamp, A.F. [CSIRO Energy Technology, Box 312, Clayton South, Vic. 3169 (Australia)

    2010-01-01

    Hydrothermal decomposition of permanganate, conducted in a range of pH-controlled solutions (from strongly acidic to strongly basic), is used to prepare manganese dioxides that are well-suited for use as supercapacitor electrode materials. While permanganate is thermodynamically unstable, the kinetics of its decomposition in an aqueous environment are very slow, until the temperature is raised to {proportional_to}200 C. Although the resultant materials are relatively crystalline and have low total pore volume, their prominent meso-porosity leads to good electrochemical performance. Best behaviour is obtained for material from permanganate decomposition in 0.01 M H{sub 2}SO{sub 4} solution, for which composite electrodes (150 {mu}m thick) yield {proportional_to}150 F g{sup -1} at 5 mV s{sup -1} in a 9 M KOH electrolyte. (author)

  5. Latent structure analysis in the pharmaceutical process of tablets prepared by wet granulation.

    Science.gov (United States)

    Uehara, Naoto; Hayashi, Yoshihiro; Mochida, Hiroshi; Otoguro, Saori; Onuki, Yoshinori; Obata, Yasuko; Takayama, Kozo

    2016-01-01

    Granule characteristics are some of the important intermediate qualities that determine tablet properties. However, the relationships between granule and tablet characteristics are poorly understood. The aim of this study was to elucidate relationships among formulation factors, granule characteristics, and tablet properties using a non-linear response surface method (RSM) incorporating a thin-plate spline interpolation (RSM-S) and a Bayesian network (BN). Tablets containing lactose (Lac), cornstarch (CS), and microcrystalline cellulose (MCC) were prepared by wet granulation. Ten formulations were prepared by an extreme vertices design. The angle of repose (Y 1 ), compressibility (Y 2 ), cohesion force (Y 3 ), internal friction angle (Y 4 ), and mean particle size (Y 5 ) were measured as granule characteristics. Tensile strength (TS) and disintegration time (DT) were measured as tablet properties. RSM-S results showed that TS increased with increasing amounts of MCC and Lac. DT decreased with increasing amounts of MCC and CS. The optimal BN models were predicted using four evaluation indices -Y 3 was shown to be the most important factor for TS, whereas Y 2 , Y 3 , and Y 4 were relatively important for predicting DT. Moreover, tablets with excellent tablet properties (i.e. high TS and low DT) were produced by relatively high Y 1 , low Y 2 , high Y 3 , high Y 4 , and middle Y 5 values, and resulted from the middle of MCC, middle-to-low CS, low Lac, and middle-to-low magnesium stearate (Mg-St) amounts. The RSM-S and BN techniques are useful for revealing complex relationships among formulation factors, granule characteristics, and tablet properties.

  6. Structure and properties of bulk amorphous magnetically soft coatings prepared by plasma spraying

    International Nuclear Information System (INIS)

    Kalita, V.I.; Kekalo, I.B.; Komlev, D.I.; Taranichev, V.E.

    1995-01-01

    Co-Ni-Fe-Si-B composition plasma coatings consisting of amorphous disk-shaped particles forming the bulk of a coating, of crystalline particles and of a threshold space, were studied. Iron and metalloid distribution heterogeneous by the thickness represents a peculiar feature for coating amorphous particles. Structure of coatings and their magnetic properties depend on some technological parameters. Conclusion is made that at annealing the variation of magnetic properties is determined by the processes of directed ordering and stratification of amorphous phase, while the low level of the initial magnetic properties of coatings is caused alongside with structure peculiarities, by occurrence of independent fine-dispersive domain structure in each disk-shaped amorphous phase. 14 refs., 8 figs., 6 tabs

  7. Preparation of disk-like particles with micro/nano hierarchical structures.

    Science.gov (United States)

    Meng, Zhen; Yang, Wenbo; Chen, Pengpeng; Wang, Weina; Jia, Xudong; Xi, Kai

    2013-10-15

    A facile, reproductive method has been successfully developed to produce disk-like microparticles self-assembled from monodispersed hybrid silica nanoparticles under certain circumstance. The disk-like microparticles with micro/nano hierarchical structures could be obtained in large amount under a mild condition and further used to biomimetic design of the superhydrophobic surface of lotus leaf. After traditional surface modification with dodecyltrichlorosiliane, the static contact angle of water on the surface with micro/nano hierarchical structure could reach 168.8°. The method of surface modification could be further simplified by click reaction with the introduction of thiol groups under mild condition. The present strategy for constructing the surface with micro/nano hierarchical structures offers the advantage of simple and large area fabrication, which enables a variety of superhydrophobic applications. Copyright © 2013 Elsevier Inc. All rights reserved.

  8. Structure, optical and electrical properties of indium tin oxide ultra thin films prepared by jet nebulizer spray pyrolysis technique

    Directory of Open Access Journals (Sweden)

    M. Thirumoorthi

    2016-03-01

    Full Text Available Indium tin oxide (ITO thin films have been prepared by jet nebulizer spray pyrolysis technique for different Sn concentrations on glass substrates. X-ray diffraction patterns reveal that all the films are polycrystalline of cubic structure with preferentially oriented along (222 plane. SEM images show that films exhibit uniform surface morphology with well-defined spherical particles. The EDX spectrum confirms the presence of In, Sn and O elements in prepared films. AFM result indicates that the surface roughness of the films is reduced as Sn doping. The optical transmittance of ITO thin films is improved from 77% to 87% in visible region and optical band gap is increased from 3.59 to 4.07 eV. Photoluminescence spectra show mainly three emissions peaks (UV, blue and green and a shift observed in UV emission peak. The presence of functional groups and chemical bonding was analyzed by FTIR. Hall effect measurements show prepared films having n-type conductivity with low resistivity (3.9 × 10−4 Ω-cm and high carrier concentrations (6.1 × 1020 cm−3.

  9. Preparation of Nanofibrous Structure of Mesoporous Bioactive Glass Microbeads for Biomedical Applications

    Directory of Open Access Journals (Sweden)

    Shiao-Wen Tsai

    2016-06-01

    Full Text Available A highly ordered, mesoporous (pore size 2~50 nm bioactive glass (MBG structure has a greater surface area and pore volume and excellent bone-forming bioactivity compared with traditional bioactive glasses (BGs. Hence, MBGs have been used in drug delivery and bone tissue engineering. MBGs can be developed as either a dense or porous block. Compared with a block, microbeads provide greater flexibility for filling different-shaped cavities and are suitable for culturing cells in vitro. In contrast, the fibrous structure of a scaffold has been shown to increase cell attachment and differentiation due to its ability to mimic the three-dimensional structure of natural extracellular matrices. Hence, the aim of this study is to fabricate MBG microbeads with a fibrous structure. First, a sol-gel/electrospinning technique was utilized to fabricate the MBG nanofiber (MBGNF structure. Subsequently, the MBGNF microbeads (MFBs were produced by an electrospraying technology. The results show that the diameter of the MFBs decreases when the applied voltage increases. The drug loading and release profiles and mechanisms of the MFBs were also evaluated. MFBs had a better drug entrapment efficiency, could reduce the burst release of tetracycline, and sustain the release over 10 days. Hence, the MFBs may be suitable drug carriers. In addition, the cellular attachment of MG63 osteoblast-like cells is significantly higher for MFBs than for glass microbeads after culturing for 4 h. The nanofibrous structure of MFBs could provide an appropriate environment for cellular spreading. Therefore, MFBs have great potential for use as a bone graft material in bone tissue engineering applications.

  10. Preparation and Characterization of Surface Photocatalytic Activity with NiO/TiO2 Nanocomposite Structure

    OpenAIRE

    Chen, Jian-Zhi; Chen, Tai-Hong; Lai, Li-Wen; Li, Pei-Yu; Liu, Hua-Wen; Hong, Yi-You; Liu, Day-Shan

    2015-01-01

    This study achieved a nanocomposite structure of nickel oxide (NiO)/titanium dioxide (TiO2) heterojunction on a TiO2 film surface. The photocatalytic activity of this structure evaluated by decomposing methylene blue (MB) solution was strongly correlated to the conductive behavior of the NiO film. A p-type NiO film of high concentration in contact with the native n-type TiO2 film, which resulted in a strong inner electrical field to effectively separate the photogenerated electron-hole pairs,...

  11. Process for depositing an oxide epitaxially onto a silicon substrate and structures prepared with the process

    Science.gov (United States)

    McKee, Rodney A.; Walker, Frederick J.

    1993-01-01

    A process and structure involving a silicon substrate utilizes an ultra high vacuum and molecular beam epitaxy (MBE) methods to grow an epitaxial oxide film upon a surface of the substrate. As the film is grown, the lattice of the compound formed at the silicon interface becomes stabilized, and a base layer comprised of an oxide having a sodium chloride-type lattice structure grows epitaxially upon the compound so as to cover the substrate surface. A perovskite may then be grown epitaxially upon the base layer to render a product which incorporates silicon, with its electronic capabilities, with a perovskite having technologically-significant properties of its own.

  12. Preparation of degradable porous structures based on 1,3-trimethylene carbonate and D,L-lactide (co)polymers for heart tissue engineering

    NARCIS (Netherlands)

    Pego, AP; Siebum, B; Van Luyn, MJA; Van Seijen, XJGY; Poot, AA; Grijpma, DW; Feijen, J

    2003-01-01

    Biodegradable porous scaffolds for heart tissue engineering were prepared from amorphous elastomeric (co)polymers of 1,3-trimethylene carbonate (TMC) and D,L-lactide (DLLA). Leaching of salt from compression-molded polymer-salt composites allowed the preparation of highly porous structures in a

  13. Polarized Raman study on the lattice structure of BiFeO3 films prepared by pulsed laser deposition

    KAUST Repository

    Yang, Yang

    2014-11-01

    Polarized Raman spectroscopy was used to study the lattice structure of BiFeO3 films on different substrates prepared by pulsed laser deposition. Interestingly, the Raman spectra of BiFeO3 films exhibit distinct polarization dependences. The symmetries of the fundamental Raman modes in 50-700 cm-1 were identified based on group theory. The symmetries of the high order Raman modes in 900-1500 cm-1 of BiFeO3 are determined for the first time, which can provide strong clarifications to the symmetry of the fundamental peaks in 400-700 cm-1 in return. Moreover, the lattice structures of BiFeO3 films are identified consequently on the basis of Raman spectroscopy. BiFeO3 films on SrRuO3 coated SrTiO3 (0 0 1) substrate, CaRuO3 coated SrTiO3 (0 0 1) substrate and tin-doped indium oxide substrate are found to be in the rhombohedral structure, while BiFeO3 film on SrRuO3 coated Nb: SrTiO3 (0 0 1) substrate is in the monoclinic structure. Our results suggest that polarized Raman spectroscopy would be a feasible tool to study the lattice structure of BiFeO3 films.

  14. Preparation and crystal structure of Ca/sub 4/Sb/sub 2/O

    Energy Technology Data Exchange (ETDEWEB)

    Eisenmann, B; Limartha, H; Schaefer, H; Graf, H A

    1980-12-01

    The formerly described compound Ca/sub 2/Sb is to be corrected to Ca/sub 4/Sb/sub 2/O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K/sub 2/NiF/sub 4/ type structure.

  15. Structural, optical and electrical properties of ZnO thin films prepared ...

    Indian Academy of Sciences (India)

    Administrator

    of zinc acetate on glass substrates at 450 °C. Effect of precursor concentration on structural and optical pro- perties has ... dependence of photoresponse properties of sprayed ZnO thin films on ... randomly oriented flake-like grains. The grains ...

  16. Structural and multiferroic properties of barium substituted bismuth ferrite nanocrystallites prepared by sol–gel method

    International Nuclear Information System (INIS)

    Anju; Agarwal, Ashish; Aghamkar, Praveen; Lal, Bhajan

    2017-01-01

    Nanocrystalline Bi 1-x Ba x FeO 3 (0≤x≤0.3) multiferroics were efficiently obtained by sol–gel method after sintering at 800 °C for one hour. The Ba substitution in BiFeO 3 (BFO) strongly modifies its structural and multiferroic properties. XRD studies revealed the structural transition from distorted rhombohedral (R3c) to pseudo-cubic (Pm3m) crystal symmetry. The magnetization increases appreciably for x=0.1, which is due to spin canting of magnetic moments at the nanoparticle surfaces and decreases afterward. From the temperature dependent magnetization studies, it is found that magnetic transition temperature (T N ) is 620 K for x=0 and 640 K for x=0.1. Besides, the maximum polarisation value decreases with increasing Ba content. SEM micrographs revealed the formation of cubic nanocrystallites with increased porosity on Ba substitution. FTIR analysis of the samples also supports the structural change towards increased crystal symmetry. - Highlights: • XRD studies revealed the structural transition from distorted rhombohedral (R3c) to pseudo-cubic (Pm3m) crystal symmetry. • The magnetization increases appreciably for x=0.1 and decreases afterward for higher Ba content. • Magnetic transition temperature (T N ) is found to be 620 K for x=0 and 640 K for x=0.1. • Maximum polarisation value is highest for x=0.1.

  17. Influence of Preparation Conditions on Electrical Properties of the Al/Alq3/Si Diode Structures

    Directory of Open Access Journals (Sweden)

    Irina ČERNIUKĖ

    2013-12-01

    Full Text Available Hybrid organic-inorganic diode structures, Al/Alq3/n-Si and Al/Alq3/p-Si based on thin films of tris(8-hydroxyquinoline aluminum (Alq3 have been investigated. The Alq3 films were evaporated in vacuum and spin coated onto patterned areas of crystalline n- and p-type Si substrates with chemically removed native SiO2 layer. Current-voltage characteristics of the diode structures demonstrated improved rectification property compared to similar Al/n-Si and Al/p-Si device structures. Increased barrier height values (0.90 eV ÷ 1.1 eV and 0.77 eV ÷ 0.91 eV for the Al/Alq3/n-Si and Al/Alq3/p-Si device structures, respectively certified presence of an interface dipole induced by the organic interlayer. Non-ideal behavior of forward current-voltage characteristics has been explained assuming non-uniformity of barrier height, presence of interface states, and influence of the organic film on diode series resistance and space charge limited current. DOI: http://dx.doi.org/10.5755/j01.ms.19.4.2733

  18. Healing agent in cement-based materials and structures, and process for its preparation

    NARCIS (Netherlands)

    Jonkers, H.M.

    2009-01-01

    The present invention relates to healing agent in cement-based materials and structures, wherein said healing agent comprises organic compounds and/or bacteria-loaded porous particles, which porous particles comprise expanded clay- or sintered fly ash. Furthermore, said porous particles are intact

  19. Structural and multiferroic properties of barium substituted bismuth ferrite nanocrystallites prepared by sol–gel method

    Energy Technology Data Exchange (ETDEWEB)

    Anju [Materials Science Lab, Department of Physics, Chaudhary Devi Lal University, Sirsa 125055 (India); Agarwal, Ashish [Department of Applied Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001 (India); Aghamkar, Praveen, E-mail: praveenaghamkar@gmail.com [Materials Science Lab, Department of Physics, Chaudhary Devi Lal University, Sirsa 125055 (India); Lal, Bhajan [Department of Applied Sciences, Goverment Polytechnic for Women, Sirsa 125055 (India)

    2017-03-15

    Nanocrystalline Bi{sub 1-x}Ba{sub x}FeO{sub 3} (0≤x≤0.3) multiferroics were efficiently obtained by sol–gel method after sintering at 800 °C for one hour. The Ba substitution in BiFeO{sub 3} (BFO) strongly modifies its structural and multiferroic properties. XRD studies revealed the structural transition from distorted rhombohedral (R3c) to pseudo-cubic (Pm3m) crystal symmetry. The magnetization increases appreciably for x=0.1, which is due to spin canting of magnetic moments at the nanoparticle surfaces and decreases afterward. From the temperature dependent magnetization studies, it is found that magnetic transition temperature (T{sub N}) is 620 K for x=0 and 640 K for x=0.1. Besides, the maximum polarisation value decreases with increasing Ba content. SEM micrographs revealed the formation of cubic nanocrystallites with increased porosity on Ba substitution. FTIR analysis of the samples also supports the structural change towards increased crystal symmetry. - Highlights: • XRD studies revealed the structural transition from distorted rhombohedral (R3c) to pseudo-cubic (Pm3m) crystal symmetry. • The magnetization increases appreciably for x=0.1 and decreases afterward for higher Ba content. • Magnetic transition temperature (T{sub N}) is found to be 620 K for x=0 and 640 K for x=0.1. • Maximum polarisation value is highest for x=0.1.

  20. Structural and electrical properties of Ta2O5 thin films prepared by ...

    Indian Academy of Sciences (India)

    The dielectric constant and leakage current density of the Ta2O5 thin films increase with increasing powers of the UV- lamps. Effects of UV- lamp powers on the structural and electrical properties were discussed. Keywords. Chemical vapour deposition processes; oxides; dielectric material; MOS capacitor. 1. Introduction.

  1. Novel selenium containing boro-phosphate glasses: Preparation and structural study

    Energy Technology Data Exchange (ETDEWEB)

    Ciceo-Lucacel, R.; Radu, T., E-mail: teodora.radu@phys.ubbcluj.ro; Ponta, O.; Simon, V.

    2014-06-01

    We synthesized a new boro-phosphate glass system with different %mol SeO{sub 2} content by conventional melt quenching technique. All samples were obtained in a glassy state with the vitreous structure confirmed by X-ray diffraction analysis. Scanning electron microscopy (SEM) revealed some non-homogeneous domains on the glasses surface, and their tendency to link each other once the selenium oxide content increases. Energy-dispersive X-ray analysis (EDAX) indicated similar elemental composition in different regions of each sample. X-ray photoelectron spectroscopy (XPS) was used to determine the nature of chemical bonding and the elemental composition at the sample surfaces, and Fourier transform infrared (FT-IR) spectroscopy was used to determine the structural groups in the obtained glass structure. Based on FT-IR results, the glass structure at short range order consists mainly of small phosphate units such as pyrophosphate (i.e. P{sub 2}O{sub 7}{sup 4−} dimmers or terminating groups at the end of phosphate chains) and some metaphosphate (i.e. PO{sub 3}{sup −} middle groups in the phosphate chains) units. The boron atoms are mainly placed in three-coordinated sites in BØ{sub 3} or BØ{sub 2}O{sup −} units. A small contribution of BØ{sub 4}{sup −} units was also detected from the FT-IR spectra of glasses. For SeO{sub 2} content higher than 5 mol%, the modifier role of selenium ions is strongly reflected on the local structure dominated in this case by pyrophosphate units. - Highlights: • New P{sub 2}O{sub 5}-CaO-B{sub 2}O{sub 3}-SeO{sub 2} glasses synthesized by conventional melt quenching method. • Evidences for the Se ions modifier role in the local structure by FT-IR and XPS. • Significant advances in understanding the structural properties of the new system.

  2. Preparation, crystal structure, and dielectric characterization of Li2W2O7 ceramic at RF and microwave frequency range

    Directory of Open Access Journals (Sweden)

    Jinwu Chen

    2017-02-01

    Full Text Available Single phase Li2W2O7 with anorthic structure was prepared by the conventional solid-state reaction method at 550∘C and the anorthic structure was stable up to 660∘C. The dielectric properties at radio frequency (RF and microwave frequency range were characterized. The sample sintered at 640∘C exhibited the optimum microwave dielectric properties with a relative permittivity of 12.2, a quality factor value of 17,700GHz (at 9.8GHz, and a temperature coefficient of the resonant frequency of −232ppm/∘C as well as a high relative density ∼94.1%. Chemical compatibility measurement indicated Li2W2O7 did not react with aluminum electrodes when sintered at 640∘C for 4h.

  3. Preparation and crystal structure of carbonyltris (diethyldithiocarbamato) technetium (III): an unexpected source of co-ordinated carbon monoxide

    International Nuclear Information System (INIS)

    Baldas, J.; Bonnyman, J.; Pojer, P.M.; Williams, G.A.

    1981-10-01

    Tc(S 2 CNEt 2 ) 3 CO has been prepared by the reduction of NH 4 TcO 4 with formamidinesulphinic acid in the presence of NaS 2 CNEt 2 . It is suggested that the co-ordinated carbon monoxide is formed after co-ordination of formamidinesulphinic acid, or some decomposition product, with technetium. The crystal structure of Tc(S 2 CNEt 2 ) 3 CO has been determined by single-crystal X-ray diffraction methods at 17 deg. C. Diffractometry has provided significant Bragg intensities for 2045 independent reflections and the structure has been refined by full-matrix least-squares methods to R 0.049. The compound is isostructural with the rhenium analogue and consists of discrete Tc(S 2 CNEt 2 ) 3 CO molecules, each containing a terminal linear CO group. The technetium atom has a seven co-ordinate environment which is best described as a distorted pentagonal bipyramid

  4. Preparation of Sb2S3 nanocrystals modified TiO2 dendritic structure with nanotubes for hybrid solar cell

    Science.gov (United States)

    Li, Yingpin; Wei, Yanan; Feng, Kangning; Hao, Yanzhong; Pei, Juan; Sun, Bao

    2018-06-01

    Array of TiO2 dendritic structure with nanotubes was constructed on transparent conductive fluorine-doped tin oxide glass (FTO) with titanium potassium oxalate as titanium source. Sb2S3 nanocrystals were successfully deposited on the TiO2 substrate via spin-coating method. Furthermore, TiO2/Sb2S3/P3HT/PEDOT:PSS composite film was prepared by successively spin-coating P3HT and PEDOT:PSS on TiO2/Sb2S3. It was demonstrated that the modification of TiO2 dendritic structure with Sb2S3 could enhance the light absorption in the visible region. The champion hybrid solar cell assembled by TiO2/Sb2S3/P3HT/PEDOT:PSS composite film achieved a power conversion efficiency (PCE) of 1.56%.

  5. Structural and magnetic properties of Fe60Al40 alloys prepared by means of a magnetic mill

    International Nuclear Information System (INIS)

    Bernal-Correa, R.; Rosales-Rivera, A.; Pineda-Gomez, P.; Salazar, N.A.

    2010-01-01

    A study on synthesis, structural and magnetic characterization of Fe 60 Al 40 (at.%) alloys prepared by means of mechanical alloying process is presented. The mechanical alloying was performed using a milling device with magnetically controlled ball movement (Uni-Ball-Mill 5 equipment) at several milling times. The characterization was carried out via X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The effects of milling time on the structural state, morphological evolution and magnetic behaviour of the Fe 60 Al 40 (at.%) alloys are discussed. Besides, in this current study we emphasize the result that indicating a ferro-para-ferromagnetic transition from a correlation between X-ray diffraction and magnetization data.

  6. Preparation and Sound Absorption Properties of a Barium Titanate/Nitrile Butadiene Rubber–Polyurethane Foam Composite with Multilayered Structure

    Science.gov (United States)

    Jiang, Xueliang; Yang, Zhen; Wang, Zhijie; Zhang, Fuqing; You, Feng

    2018-01-01

    Barium titanate/nitrile butadiene rubber (BT/NBR) and polyurethane (PU) foam were combined to prepare a sound-absorbing material with an alternating multilayered structure. The effects of the cell size of PU foam and the alternating unit number on the sound absorption property of the material were investigated. The results show that the sound absorption efficiency at a low frequency increased when decreasing the cell size of PU foam layer. With the increasing of the alternating unit number, the material shows the sound absorption effect in a wider bandwidth of frequency. The BT/NBR-PU foam composites with alternating multilayered structure have an excellent sound absorption property at low frequency due to the organic combination of airflow resistivity, resonance absorption, and interface dissipation. PMID:29565321

  7. Preparation and Sound Absorption Properties of a Barium Titanate/Nitrile Butadiene Rubber–Polyurethane Foam Composite with Multilayered Structure

    Directory of Open Access Journals (Sweden)

    Xueliang Jiang

    2018-03-01

    Full Text Available Barium titanate/nitrile butadiene rubber (BT/NBR and polyurethane (PU foam were combined to prepare a sound-absorbing material with an alternating multilayered structure. The effects of the cell size of PU foam and the alternating unit number on the sound absorption property of the material were investigated. The results show that the sound absorption efficiency at a low frequency increased when decreasing the cell size of PU foam layer. With the increasing of the alternating unit number, the material shows the sound absorption effect in a wider bandwidth of frequency. The BT/NBR-PU foam composites with alternating multilayered structure have an excellent sound absorption property at low frequency due to the organic combination of airflow resistivity, resonance absorption, and interface dissipation.

  8. Preparation and Sound Absorption Properties of a Barium Titanate/Nitrile Butadiene Rubber-Polyurethane Foam Composite with Multilayered Structure.

    Science.gov (United States)

    Jiang, Xueliang; Yang, Zhen; Wang, Zhijie; Zhang, Fuqing; You, Feng; Yao, Chu

    2018-03-22

    Barium titanate/nitrile butadiene rubber (BT/NBR) and polyurethane (PU) foam were combined to prepare a sound-absorbing material with an alternating multilayered structure. The effects of the cell size of PU foam and the alternating unit number on the sound absorption property of the material were investigated. The results show that the sound absorption efficiency at a low frequency increased when decreasing the cell size of PU foam layer. With the increasing of the alternating unit number, the material shows the sound absorption effect in a wider bandwidth of frequency. The BT/NBR-PU foam composites with alternating multilayered structure have an excellent sound absorption property at low frequency due to the organic combination of airflow resistivity, resonance absorption, and interface dissipation.

  9. Electronic structure and size of TiO sub 2 nanoparticles of controlled size prepared by aerosol methods

    CERN Document Server

    Soriano, L; Sanchez-Agudo, M; Sanz, J M; Ahonen, P P; Kauppinen, E I; Palomares, F J; Bressler, P R

    2002-01-01

    A complete characterization of nanostructures has to deal both with electronic structure and dimensions. Here we present the characterization of TiO sub 2 nanoparticles of controlled size prepared by aerosol methods. The electronic structure of these nanoparticles was probed by x-ray absorption spectroscopy (XAS), the particle size by atomic force microscopy (AFM). XAS spectra show that the particles crystallize in the anatase phase upon heating at 500 sup o C, whereas further annealing at 700 sup o C give crystallites of 70 % anatase and 30 % rutile phases. Raising the temperature to 900 sup o C results in a complete transformation of the particles to rutile. AFM images reveal that the mean size of the anatase particles formed upon heating at 500 sup o C is 30 nm, whereas for the rutile particles formed upon annealing at 900 sup o C 90 nm were found. The results obtained by these techniques agree with XRD data. (author)

  10. Influence of Zr doping on structure and morphology of TiO2 nanorods prepared using hydrothermal method

    Science.gov (United States)

    Muslimin, Masliana; Jumali, Mohammad Hafizuddin; Tee, Tan Sin; Beng, Lee Hock; Hui, Tan Chun; Chin, Yap Chi

    2018-04-01

    The aim of this work is to investigate the effect of Zr doping on TiO2 nanostructure. TiO2 nanorods thin films with different Zr-doping concentrations (6 × 10-3 M, 13 × 10-3 M and 25 × 10-3 M) were successfully prepared using a simple hydrothermal method. The structural and morphological properties of the samples were evaluated using XRD and FESEM respectively. The XRD results revealed that the TiO2 in all samples stabilized as rutile phase. The FESEM micrographs confirmed that TiO2 exist as square like nanorods with blunt tips. Although the crystallographic nature remains unchanged, the introduction of Zr has altered the surface density, structure and morphology of TiO2 which subsequently will have significant effect on its properties.

  11. Experimental studies on the electronic structure of pyrite FeS2 films prepared by thermally sulfurizing iron films

    International Nuclear Information System (INIS)

    Zhang Hui; Wang Baoyi; Zhang Rengang; Zhang Zhe; Wei Long; Qian Haijie; Su Run; Kui Rexi

    2006-01-01

    Pyrite FeS 2 films have been prepared by thermally sulfurizing iron films deposited by magnetron sputtering. The electronic structures were studies by X-ray absorption near edge structure and X-ray photoemission spectrum. The results show that an S 3p valence band with relatively higher intensity compared to the calculation exists in 2-10 eV range and a high density below the Fermi level of Fe 3d states were detected. A second gap of 2.8 eV in the unoccupied density of states was found above the conduction band which was 2.4 eV by experimentally calculation. The difference between t 2g and e g which were formed in an octahedral crystal field was computed to be 2.1 eV. (authors)

  12. Structural and magnetic properties in Mn-doped ZnO films prepared by pulsed-laser deposition

    International Nuclear Information System (INIS)

    Li, Qiang; Wang, Yuyin; Liu, Jiandang; Kong, Wei; Ye, Bangjiao

    2014-01-01

    We investigated the structural and magnetic properties of Zn 0.95 Mn 0.05 O films prepared on sapphire substrates by pulsed-laser deposition. Only low temperature ferromagnetism (Curie temperature lower than 50 K) was observed in Mn-doped samples, while pure ZnO film shows a typical paramagnetic behavior. Structural analyses indicate that the substitutional Mn 2+ ions play a significant role for the low temperature ferromagnetism. Lattice defects such as V O and V Zn were not proven to be effective factors for the origin of ferromagnetism in the films. The low temperature ferromagnetism might be interpreted as p–d hybridization from indirect coupling of Mn ions (Mn–O–Mn).

  13. Novel selenium containing boro-phosphate glasses: preparation and structural study.

    Science.gov (United States)

    Ciceo-Lucacel, R; Radu, T; Ponta, O; Simon, V

    2014-06-01

    We synthesized a new boro-phosphate glass system with different %mol SeO2 content by conventional melt quenching technique. All samples were obtained in a glassy state with the vitreous structure confirmed by X-ray diffraction analysis. Scanning electron microscopy (SEM) revealed some non-homogeneous domains on the glasses surface, and their tendency to link each other once the selenium oxide content increases. Energy-dispersive X-ray analysis (EDAX) indicated similar elemental composition in different regions of each sample. X-ray photoelectron spectroscopy (XPS) was used to determine the nature of chemical bonding and the elemental composition at the sample surfaces, and Fourier transform infrared (FT-IR) spectroscopy was used to determine the structural groups in the obtained glass structure. Based on FT-IR results, the glass structure at short range order consists mainly of small phosphate units such as pyrophosphate (i.e. P2O7(4-) dimmers or terminating groups at the end of phosphate chains) and some metaphosphate (i.e. PO3(-) middle groups in the phosphate chains) units. The boron atoms are mainly placed in three-coordinated sites in BØ3 or BØ2O(-) units. A small contribution of BØ4(-) units was also detected from the FT-IR spectra of glasses. For SeO2 content higher than 5mol%, the modifier role of selenium ions is strongly reflected on the local structure dominated in this case by pyrophosphate units. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Preparation and magnetic properties of the Sr-hexaferrite with foam structure

    Energy Technology Data Exchange (ETDEWEB)

    Guerrero, A.L., E-mail: azdlobo@gmail.com [Instituto de Física-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico); Facultad de Ingeniería-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico); Espericueta, D.L. [Facultad de Ingeniería-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico); Facultad de Ciencias-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico); Palomares-Sánchez, S.A. [Facultad de Ciencias-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico); Elizalde-Galindo, J.T. [Instituto de Ingeniería y Tecnología-UACJ, Av. Plutarco Elías Calles 1210, Fovissste Chamizal, Ciudad Juárez, Chihuahua (Mexico); Watts, B.E [IMEM-CNR, Parco Area delle Scienze 37/A, 43124 Parma (Italy); Mirabal-García, M. [Instituto de Física-UASLP, Álvaro Obregón 64, Centro. San Luis Potosí, S.L.P. (Mexico)

    2016-12-01

    This work reports an optimal way to fabricate strontium hexaferrite with porous-reticulated structure using a variation of the replication technique and taking two different precursors, one obtained from the coprecipitation and the other from the ceramic method. Changes made to the original replication technique include the addition of Arabic gum as binder, and the addition of ethylene glycol to form the ceramic sludge. In addition, some parameters such as the relation between solid material and liquid phase, the quantity of binder and the heat treatment were varied to obtain high quality magnetic foams. Two polymeric sponges were used as patterns, one with average pore size of 300 μm diameter and the other with 1100 μm. The characterization of the samples included the analysis of the structure and phase purity, the magnetic properties, the remanence properties, magnetic interactions and the microstructural characteristics. Results indicate that both, the powder precursors and the polymeric pattern play an important role in the configuration of the foam structure and this configuration has an important influence on the dipolar interactions which tend to demagnetize the samples. In addition, it was analyzed the behavior between the minimum value of the δM curves and the hysteresis properties. - Highlights: • New way to obtain Sr-hexaferrite with foam structure and high magnetic performance. • Relation between pore structure and the magnetic properties in ceramic foams. • Analysis of magnetostatic interactions with the magnetism of Sr-hexaferrite foams. • Relation between microstructural characteristics and the magnetization of the foams.

  15. Preparation and magnetic properties of the Sr-hexaferrite with foam structure

    International Nuclear Information System (INIS)

    Guerrero, A.L.; Espericueta, D.L.; Palomares-Sánchez, S.A.; Elizalde-Galindo, J.T.; Watts, B.E; Mirabal-García, M.

    2016-01-01

    This work reports an optimal way to fabricate strontium hexaferrite with porous-reticulated structure using a variation of the replication technique and taking two different precursors, one obtained from the coprecipitation and the other from the ceramic method. Changes made to the original replication technique include the addition of Arabic gum as binder, and the addition of ethylene glycol to form the ceramic sludge. In addition, some parameters such as the relation between solid material and liquid phase, the quantity of binder and the heat treatment were varied to obtain high quality magnetic foams. Two polymeric sponges were used as patterns, one with average pore size of 300 μm diameter and the other with 1100 μm. The characterization of the samples included the analysis of the structure and phase purity, the magnetic properties, the remanence properties, magnetic interactions and the microstructural characteristics. Results indicate that both, the powder precursors and the polymeric pattern play an important role in the configuration of the foam structure and this configuration has an important influence on the dipolar interactions which tend to demagnetize the samples. In addition, it was analyzed the behavior between the minimum value of the δM curves and the hysteresis properties. - Highlights: • New way to obtain Sr-hexaferrite with foam structure and high magnetic performance. • Relation between pore structure and the magnetic properties in ceramic foams. • Analysis of magnetostatic interactions with the magnetism of Sr-hexaferrite foams. • Relation between microstructural characteristics and the magnetization of the foams.

  16. Electrical, optical, and structural properties of GaN films prepared by hydride vapor phase epitaxy

    International Nuclear Information System (INIS)

    Polyakov, A.Y.; Smirnov, N.B.; Yakimov, E.B.; Usikov, A.S.; Helava, H.; Shcherbachev, K.D.; Govorkov, A.V.; Makarov, Yu N.; Lee, In-Hwan

    2014-01-01

    Highlights: • GaN films are prepared by hydride vapor phase epitaxy (HVPE). • Residual donors and deep traps show a minimum density versus growth temperature. • This minimum is located close to the HVPE growth temperature of 950 °C. • Good crystalline GaN with residual donor density < 10 16 cm −3 can be grown at 950 °C. - Abstract: Two sets of undoped GaN films with the thickness of 10–20 μm were prepared by hydride vapor phase epitaxy (HVPE) and characterized by capacitance–voltage (C–V) profiling, microcathodoluminescence (MCL) spectra measurements, MCL imaging, electron beam induced current (EBIC) imaging, EBIC dependence on accelerating voltage, deep levels transient spectroscopy, high resolution X-ray diffraction measurements. The difference in growth conditions was mainly related to the lower (850 °C, group 1) or higher (950 °C, group 2) growth temperature. Both groups of samples showed similar crystalline quality with the dislocation density close to 10 8 cm −2 , but very different electrical and optical properties. In group 1 samples the residual donors concentration was ∼10 17 cm −3 or higher, the MCL spectra were dominated by the band-edge luminescence, and the diffusion length of charge carriers was close to 0.1 μm. Group 2 samples had a 2–4.5 μm thick highly resistive layer on top, for which MCL spectra were determined by green, yellow and red defect bands, and the diffusion length was 1.5 times higher than in group 1. We also present brief results of growth at the “standard” HVPE growth temperature of 1050 °C that show the presence of a minimum in the net donor concentration and deep traps density as a function of the growth temperature. Possible reasons for the observed results are discussed in terms of the electrical compensation of residual donors by deep traps

  17. Enzymatic incorporation of caffeoyl into castor oil to prepare the novel castor oil-based caffeoyl structured lipids.

    Science.gov (United States)

    Sun, Shangde; Wang, Ping; Zhu, Sha

    2017-05-10

    In this work, a novel castor oil-based caffeoyl structured lipids was successfully prepared by the enzymatic transesterification using castor oil (CO) as caffeoyl acceptor. During the structured lipids preparation, two competitive reactions, the hydrolysis of CO to form hydrophilic caffeoyl glycerols (CG)+dicaffeoyl glycerols (DCG) and the transesterification of CO with ethyl caffeate (EC) to form lipophilic caffeoyl mono- and di-acylglycerols (CMAG and CDAG), were found. Reaction progress was monitored using HPLC-ESI-MS and HPLC-UV. The effects of by-product ethanol removal and reaction variables on the transesterification and reaction selectivity were evaluated. Results showed that, the activation energies for the transesterification and for the selective formations of CMAG+CDAG and CG+DCG were 57.60kJ/mol, 58.86kJ/mol, and 60.53kJ/mol, respectively. Under the optimal reaction conditions (enzyme load 23%, 90°C, 1:3 molar ratio of EC to CO, and 46.5h), EC conversion and the yield of CMAG+CDAG were 93.68±2.52% and 78.11±1.35%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Preparation and structural characterization of vulcanized natural rubber nanocomposites containing nickel-zinc ferrite nanopowders.

    Science.gov (United States)

    Bellucci, F S; Salmazo, L O; Budemberg, E R; da Silva, M R; Rodríguez-Pérez, M A; Nobre, M A L; Job, A E

    2012-03-01

    Single-phase polycrystalline mixed nickel-zinc ferrites belonging to Ni0.5Zn0.5Fe2O4 were prepared on a nanometric scale (mean crystallite size equal to 14.7 nm) by chemical synthesis named the modified poliol method. Ferrite nanopowder was then incorporated into a natural rubber matrix producing nanocomposites. The samples were investigated by means of infrared spectroscopy, X-ray diffraction, scanning electron microscopy and magnetic measurements. The obtained results suggest that the base concentration of nickel-zinc ferrite nanoparticles inside the polymer matrix volume greatly influences the magnetic properties of nanocomposites. A small quantity of nanoparticles, less than 10 phr, in the nanocomposite is sufficient to produce a small alteration in the semi-crystallinity of nanocomposites observed by X-ray diffraction analysis and it produces a flexible magnetic composite material with a saturation magnetization, a coercivity field and an initial magnetic permeability equal to 3.08 emu/g, 99.22 Oe and 9.42 x 10(-5) respectively.

  19. Structural Characterization of Polymer-Clay Nanocomposites Prepared by Co-Precipitation Using EPR Techniques

    Directory of Open Access Journals (Sweden)

    Udo Kielmann

    2014-02-01

    Full Text Available Polymer-clay nanocomposites (PCNCs containing either a rubber or an acrylate polymer were prepared by drying or co-precipitating polymer latex and nanolayered clay (synthetic and natural suspensions. The interface between the polymer and the clay nanoparticles was studied by electron paramagnetic resonance (EPR techniques by selectively addressing spin probes either to the surfactant layer (labeled stearic acid or the clay surface (labeled catamine. Continuous-wave (CW EPR studies of the surfactant dynamics allow to define a transition temperature T* which was tentatively assigned to the order-disorder transition of the surfactant layer. CW EPR studies of PCNC showed that completely exfoliated nanoparticles coexist with agglomerates. HYSCORE spectroscopy in PCNCs showed couplings within the probe −assigned with DFT computations− and couplings with nuclei of the environment, 1H and 23Na for the surfactant layer probe, and 29Si, 7Li, 19F and 23Na for the clay surface probe. Analysis of these couplings indicates that the integrity of the surfactant layer is conserved and that there are sizeable ionic regions containing sodium ions directly beyond the surfactant layer. Simulations of the very weak couplings demonstrated that the HYSCORE spectra are sensitive to the composition of the clay and whether or not clay platelets stack.

  20. Structural characterization and frictional properties of carbon nanotube/alumina composites prepared by precursor method

    Energy Technology Data Exchange (ETDEWEB)

    Yamamoto, Go [Institute of Fluid Science, Tohoku University, 2-1-1 Katahira, Aobaku, Sendai 980-8577 (Japan); Fracture and Reliability Research Institute, Tohoku University, 6-6-11-707 Aza-Aoba, Aramaki, Aobaku, Sendai 980-8579 (Japan)], E-mail: gyamamoto@rift.mech.tohoku.ac.jp; Omori, Mamoru; Yokomizo, Kenji; Hashida, Toshiyuki [Fracture and Reliability Research Institute, Tohoku University, 6-6-11-707 Aza-Aoba, Aramaki, Aobaku, Sendai 980-8579 (Japan); Adachi, Koshi [Graduate School of Engineering, Tohoku University, 6-6-01 Aza-Aoba, Aramaki, Aobaku, Sendai 980-8579 (Japan)

    2008-02-25

    Multi-walled carbon nanotube (MWCNT)/Al{sub 2}O{sub 3} composites with MWCNTs content up to 10 mass% were prepared by precursor method. XRD analysis revealed that MWCNT/Al{sub 2}O{sub 3} composites were successfully synthesized by the dehydration of aluminum hydroxide-MWCNTs mixture at 1500 deg. C in vacuum. The steady-state friction coefficient ({mu}) of the composites decreased with increasing up to 4 mass% MWCNT and stayed constant ({mu} = 0.33) with further addition of MWCNT, which value was substantially lower than that of MWCNT-free monolithic Al{sub 2}O{sub 3} ({mu} = 0.57). Microstructural observations showed that resultant friction behavior may be related to the smearing of transferred film over the contact area, which was expected to permit easy shear and then help to achieve a lubricating effect during sliding. However, fracture property tests have shown that no improvement of the fracture strength and fracture toughness of the composites was achieved by addition of MWCNTs. It may be mainly due to the agglomeration of MWCNTs and the weak interface between MWCNTs and the Al{sub 2}O{sub 3} matrix.

  1. Structural characterization and frictional properties of carbon nanotube/alumina composites prepared by precursor method

    International Nuclear Information System (INIS)

    Yamamoto, Go; Omori, Mamoru; Yokomizo, Kenji; Hashida, Toshiyuki; Adachi, Koshi

    2008-01-01

    Multi-walled carbon nanotube (MWCNT)/Al 2 O 3 composites with MWCNTs content up to 10 mass% were prepared by precursor method. XRD analysis revealed that MWCNT/Al 2 O 3 composites were successfully synthesized by the dehydration of aluminum hydroxide-MWCNTs mixture at 1500 deg. C in vacuum. The steady-state friction coefficient (μ) of the composites decreased with increasing up to 4 mass% MWCNT and stayed constant (μ = 0.33) with further addition of MWCNT, which value was substantially lower than that of MWCNT-free monolithic Al 2 O 3 (μ = 0.57). Microstructural observations showed that resultant friction behavior may be related to the smearing of transferred film over the contact area, which was expected to permit easy shear and then help to achieve a lubricating effect during sliding. However, fracture property tests have shown that no improvement of the fracture strength and fracture toughness of the composites was achieved by addition of MWCNTs. It may be mainly due to the agglomeration of MWCNTs and the weak interface between MWCNTs and the Al 2 O 3 matrix

  2. Preparation of Fluorine-Doped TiO2 Photocatalysts with Controlled Crystalline Structure

    Directory of Open Access Journals (Sweden)

    N. Todorova

    2008-01-01

    Full Text Available Nanocrystalline F-doped TiO2 powders were prepared by sol-gel route. The thermal behavior of the powders was recorded by DTA/TG technique. The crystalline phase of the fluorinated TiO2 powders was determined by X-ray diffraction technique. It was demonstrated that F-doping using CF3COOH favors the formation of rutile along with anatase phase even at low temperature. Moreover, the rutile's phase content increases with the increase of the quantity of the fluorine precursor in the starting solution. The surface area of the powders and the pore size distribution were studied by N2 adsorption-desorption using BET and BJH methods. X-ray photoelectron spectroscopy (XPS revealed that the fluorine is presented in the TiO2 powders mainly as metal fluoride in quantities ∼16 at %. The F-doped TiO2 showed a red-shift absorption in UV-vis region which was attributed to the increased content of rutile phase in the powders. The powders exhibited enhanced photocatalytic activity in decomposition of acetone.

  3. Structural changes evaluation with Raman spectroscopy in meat batters prepared by different processes.

    Science.gov (United States)

    Kang, Zhuang-Li; Li, Xiang; He, Hong-Ju; Ma, Han-Jun; Song, Zhao-Jun

    2017-08-01

    A comprehensive study was conducted to evaluate the structural changes of meat and protein of pork batters produced by chopping or beating process through the phase-contrast micrograph, laser light scattering analyzer, scanning electronic microscopy and Raman spectrometer. The results showed that the shattered myofibrilla fragments were shorter and particle-sizes were smaller in the raw batter produced by beating process than those in the chopping process. Compared with the raw and cooked batters produced by chopping process, modifications in amide I and amide III bands revealed a significant decrease of α -helix content and an increase of β -sheet, β -turn and random coils content in the beating process. The changes in secondary structure of protein in the batter produced by beating process was thermally stable. Moreover, more tyrosine residues were buried, and more gauche-gauche-trans disulfide bonds conformations and hydrophobic interactions were formed in the batter produced by beating process.

  4. Preparation and Characterization of Nano-structured Ceramic Powders Synthesized by Emulsion Combustion Method

    International Nuclear Information System (INIS)

    Takatori, Kazumasa; Tani, Takao; Watanabe, Naoyoshi; Kamiya, Nobuo

    1999-01-01

    The emulsion combustion method (ECM), a novel powder production process, was originally developed to synthesize nano-structured metal-oxide powders. Metal ions in the aqueous droplets were rapidly oxidized by the combustion of the surrounding flammable liquid. The ECM achieved a small reaction field and a short reaction period to fabricate the submicron-sized hollow ceramic particles with extremely thin wall and chemically homogeneous ceramic powder. Alumina, zirconia, zirconia-ceria solid solutions and barium titanate were synthesized by the ECM process. Alumina and zirconia powders were characterized to be metastable in crystalline phase and hollow structure. The wall thickness of alumina was about 10 nm. The zirconia-ceria powders were found to be single-phase solid solutions for a wide composition range. These powders were characterized as equiaxed-shape, submicron-sized chemically homogeneous materials. The powder formation mechanism was investigated through the synthesis of barium titanate powder with different metal sources

  5. Group constant preparation for the estimate of neutron induced damage in structural materials

    International Nuclear Information System (INIS)

    Panini, G.C.

    1996-01-01

    Neutron heating (kerma), displacement per atom cross sections (DPA), gas and γ-ray production are important parameters for the estimate of the damage produced by neutron induced nuclear reactions in the structural materials. The NJOY System for Nuclear Data Processing has been extensively used in order to compute the above quantities; here the theory, the algorithms and the connected problems are described. (author). 6 refs, 3 tabs

  6. Effect of the conditions of prepreg preparation on the strength of structural plastics

    Science.gov (United States)

    Zaborskaya, L. V.; Yurkevich, O. R.

    1995-05-01

    A study is made of the effect of the temperature and duration of heat treatment of polymer composite prepregs on their strength. It is established that heat treatment under conditions ensuring close to maximal adhesive interaction between the components of the prepreg and subsequent shaping makes it possible to more than double the strength of the plastic (Table 1), A new approach is proposed to optimizing the conditions of formation of structural plastics.

  7. Laser-assisted preparation and photoelectric properties of grating-structured Pt/FTO thin films

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Nai-fei, E-mail: rnf_ujs@126.com [School of Mechanical Engineering, Jiangsu University, Zhenjiang 212013 (China); Jiangsu Provincial Key Laboratory of Center for Photon Manufacturing Science and Technology, Jiangsu University, Zhenjiang 212013 (China); Huang, Li-jing, E-mail: lij_huang@126.com [Jiangsu Provincial Key Laboratory of Center for Photon Manufacturing Science and Technology, Jiangsu University, Zhenjiang 212013 (China); School of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013 (China); Li, Bao-jia [Jiangsu Provincial Key Laboratory of Center for Photon Manufacturing Science and Technology, Jiangsu University, Zhenjiang 212013 (China); School of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013 (China); Zhou, Ming [Jiangsu Provincial Key Laboratory of Center for Photon Manufacturing Science and Technology, Jiangsu University, Zhenjiang 212013 (China); The State Key Laboratory of Tribology, Tsinghua University, Beijing 100084 (China)

    2014-09-30

    Highlights: • Pt layers were deposited by DC magnetron sputtering on commercial FTO glasses. • Pt/FTO films were irradiated by laser for inducing gratings and annealing. • An ideal grating-structured Pt/FTO film was obtained using a fluence of 1.05 J/cm{sup 2}. • The grating-structured Pt/FTO film exhibited excellent photoelectric properties. • Laser-assisted treatment is effective for improving performance of FTO-based films. - Abstract: In order to improve the transparency and conductivity of commercial fluorine-doped tin oxide (FTO) glass, platinum (Pt) layers were deposited on the FTO film by direct current (DC) magnetron sputtering, followed by being irradiating with a 532 nm nanosecond pulsed laser for the dual purpose of inducing grating structures and annealing. Introducing a Pt layer decreased the average transmittance (400–800 nm) and the sheet resistance of the initial FTO film from 80.2% and 8.4 Ω/sq to 68.6% and 7.9 Ω/sq, respectively. The ideal grating-structured Pt/FTO film was obtained by laser irradiation with a fluence of 1.05 J/cm{sup 2}, and X-ray diffraction (XRD) analysis confirmed that this film underwent optimal annealing. As a result, it exhibited an average transmittance (400–800 nm) of 84.1% and a sheet resistance of 6.8 Ω/sq. These results indicated that laser-assisted treatment combined with introduction of metal layer can effectively improve photoelectric properties of FTO single-layer films.

  8. Preparation of Fe-intercalated Graphite Based on Coal Tailings, Dimensional Structure

    Directory of Open Access Journals (Sweden)

    Irfan Gustian

    2015-12-01

    Full Text Available Intercalated graphite from coal tailings have been modified through the intercalation of iron. Coal tailings which is a byproduct of the destruction process and flakes washing results from mining coal. Intercalation of iron goal is to improve the physical properties of graphite and modifying sizes of crystal lattice structure with thermal method. Modification process begins with the carbonization of coal tailings at 500ºC and activated with phosphoric acid. Activation process has done by pyrolysis at 700ºC. The results of pyrolysis was soaked in mineral oil for 24 hours, then pyrolysis again with variations in temperature 800°C and 900ºC for 1 hour and subsequent intercalation iron at 1% and 2%. Material before activated, after activated, and the results of pyrolysis still indicates order nano: 29, 25 and 36 nm respectively. X-ray diffraction characterization results indicate that change in the structure, the sizes crystal lattice structure of the material The greater the concentration of iron was added, the resulting peak at 2θ = 33 and 35 also will be more sharply. The results of SEM showed different morphologies from each treatment.

  9. Development of cobalt ferrite powder preparation employing the sol-gel technique and its structural characterization

    International Nuclear Information System (INIS)

    Sajjia, M.; Oubaha, M.; Prescott, T.; Olabi, A.G.

    2010-01-01

    Research highlights: This work focuses on the sol-gel process and the effects that the initial parameters have on the final product, which is the cobalt ferrite powder, in addition to the heat treatment. Particular interest is devoted to understand how the crosslinker and the chelating agent work and affect the final product. - Abstract: This work focuses on the development of a method to make cobalt ferrite powder using the sol-gel process. A particular emphasis is devoted to the understanding of the role of the chemical parameters involved in the sol-gel technique, and of the heat treatment on the structures and morphologies of the materials obtained. Several samples of cobalt ferrite powder were obtained by varying the initial parameters of the process in addition to the heat treatment temperature. X-ray diffraction and scanning electron microscopy were used to identify the structure and morphology of samples demonstrating the influence of the initial parameters. DTA/TGA was carried out on two standard samples to identify important reaction temperatures during the heat treatment. The average size of the nano crystallites was estimated for a sample by the full width at half maximum (FWHM) of the strongest X-ray diffraction (XRD) peak. It has been found that the chelating agent and the crosslinker have a critical influence on the resultant structure, the particle size and the particle size distribution.

  10. Design and Preparation of a Micro-Pyramid Structured Thin Film for Broadband Infrared Antireflection

    Directory of Open Access Journals (Sweden)

    Shaobo Ge

    2018-05-01

    Full Text Available A micro-pyramid structured thin film with a broad-band infrared antireflection property is designed and fabricated by using the single-point diamond turning (SPDT technique and combined with nano-imprint lithography (NIL. A structure with dimensions of 10 μm pitch and 5 μm height is transferred from the copper mold to the silicon nitride optical film by using NIL and proportional inductively-coupled plasma (ICP etching. Reflectance of the micro-optical surface is reduced below 1.0% over the infrared spectral range (800–2500 nm. A finite-difference-time-domain (FDTD analysis indicates that this micro-structure can localize photons and enhance the absorption inside the micro-pyramid at long wavelengths. As described above, the micro-pyramid array has been integrated in an optical film successfully. Distinguishing from the traditional micro-optical components, considering the effect of refraction and diffraction, it is a valuable and flexible method to take account of the interference effect of optical film.

  11. Photoelectrochemical properties of the TiO2-ZnO nanorod hierarchical structure prepared by hydrothermal process

    Directory of Open Access Journals (Sweden)

    Bao SUN

    2018-02-01

    Full Text Available In order to increase the transport channels of the photogenerated electrons and enhance the photosensitizer loading ability of the electrode, a new TiO2-ZnO nanorod hierarchical structure is prepared through two-step hydrothermal process. First, TiO2 nanorod array is grown on the FTO conductive glass substrate by hydrothermal proess. Then, ZnO sol is coated onto the TiO2 nanorods through dip-coating method and inverted to ZnO seed layer by sintering. Finally, the secondary ZnO nanorods are grown onto the TiO2 nanorods by the sencond hydrothermal method to form the designed TiO2-ZnO nanorod hierarchical structure. A spin-coating assisted successive ionic layer reaction method (SC-SILR is used to deposit the CdS nanocrystals into the TiO2 nanorod array and the TiO2-ZnO nanorod hierarchical structure is used to form the CdS/TiO2 and CdS/TiO2-ZnO nanocomposite films. Different methods, such as SEM, TEM, XRD, UV-Vis and transient photocurrent, are employed to characterize and measure the morphologies, structures, light absorption and photoelectric conversion performance of all the samples, respectively. The results indicate that, compared with the pure TiO2 nanorod array, the TiO2-ZnO nanorod hierarchical structure can load more CdS photosensitizer. The light absorption properties and transient photocurrent performance of the CdS/TiO2-ZnO nanorod hierarchical structure composite film are evidently superior to that of the CdS/TiO2 nanocomposite films. The excellent photoelctrochemical performance of theTiO2-ZnO hierarchical structure reveales its application prospect in photoanode material of the solar cells.

  12. Structure, chemical bonding states, and optical properties of the hetero-structured ZnO/CuO prepared by using the hydrothermal and the electrospinning methods

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Kyong-Soo; Kim, Jong Wook; Bae, Jong-Seong; Hong, Tae Eun; Jeong, Euh Duck; Jin, Jong Sung; Ha, Myoung Gyu; Kim, Jong-Pil, E-mail: jpkim@kbsi.re.kr

    2017-01-01

    ZnO-branched nanostructures have recently attracted considerable attention due to their rich architectures and promising applications in the field of optoelectronics. Contrary to n-type semiconducting metal oxides, cupric oxide is a p-type semiconductor which can be applied to high-critical-temperature superconductors, photovoltaic materials, field emission, and catalysis. We report the synthesis of the ZnO nanorods on the CuO nanofibers prepared by using the electrospinning method along with the hydrothermal method. As the growing time increases, emission spectra of the hetero-structured ZnO/CuO show that the observed band in the UV region is slightly increased, while the intensity of the green emission is highly enhanced. The hetero-structured ZnO/CuO is found to be a promising candidate for developing renewable devices with photoluminescent behavior and the increased surface to volume ratio.

  13. Structural and optical studied of nano structured lead sulfide thin films prepared by the chemical bath deposition technique

    Energy Technology Data Exchange (ETDEWEB)

    Al Din, Nasser Saad, E-mail: nsaadaldin@yahoo.com; Hussain, Nabiha, E-mail: nabihahssin@yahoo.com [Damascus University Faculty of Science, Department of physics, Homs (Syrian Arab Republic); Jandow, Nidhal, E-mail: nidhaljandow@yahoo.com [Al –Mustansiriyah University, College of Education, Department of physics, Baghdad (Iraq)

    2016-07-25

    Lead (II) Sulfide PbS thin films were deposited on glass substrates at 25°C by chemical bath deposition (CBD) method. The structural properties of the films were studied as a function of the concentration of Thiourea (CS (NH{sub 2}){sub 2}) as Source of Sulfide and deposition time. The surface morphology of the films was characterized by X-ray diffraction and SEM. The obtained results showed that the as-deposited films Polycrystalline had cubic crystalline phase that belong to S.G: Fm3m. We found that they have preferred orientation [200]. Also the thickness of thin films decrease with deposition time after certain value and, it observed free sulfide had orthorhombic phase. Optical properties showed that the thin films have high transmission at visible range and low transmission at UV, IR range. The films of PbS have direct band gap (I.68 - 2.32 ev) at 300 K the values of band energy decreases with increases thickness of the Lead (II) Sulfide films.

  14. The relationship of lateral anatomic structures to exiting guide pins during femoral tunnel preparation utilizing an accessory medial portal.

    Science.gov (United States)

    Farrow, Lutul D; Parker, Richard D

    2010-06-01

    Anatomic reconstruction of the anterior cruciate ligament through an accessory medial portal has become increasingly popular. The purpose of this study is to describe the relationship of guide pin exit points to the lateral anatomic structures when preparing the anterior cruciate ligament femoral tunnel through an accessory medial portal. We utilized seven fresh frozen cadaveric knees. Utilizing an anteromedial approach, a guide wire was placed into the center of each bundle's footprint. Each guide wire was advanced through the lateral femoral cortex. The guide pins were passed at 90, 110, and 130 degrees of knee flexion. The distances from each guide pin to the closest relevant structures on the lateral side of the knee were measured. At 90 degrees the posterolateral bundle guide pin was closest to the lateral condyle articular cartilage (mean 5.4 +/- 2.2 mm) and gastrocnemius tendon (mean 5.7 +/- 2.1 mm). At 110 degrees the posterolateral bundle pin was closest to the gastrocnemius tendon (mean 4.5 +/- 3.4 mm). At 130 degrees the posterolateral bundle pin was closest to the gastrocnemius tendon (mean 7.2 +/- 5.5 mm) and lateral collateral ligament (mean 6.8 +/- 2.1 mm). At 90 degrees the anteromedial bundle guide pin was closest to the articular cartilage (mean 2.0 +/- 2.0 mm). At 110 degrees the anteromedial bundle pin was closest to the articular cartilage (mean 7.4 +/- 3.5 mm) and gastrocnemius tendon (mean 12.3 +/- 3.1 mm). At 130 degrees the AM bundle pin was closest to the gastrocnemius tendon (mean 8.2 +/- 3.2 mm) and LCL (mean 15.1 +/- 2.9 mm). Neither guide pin (anteromedial or posterolateral bundle) put the peroneal nerve at risk at any knee flexion angle. At low knee flexion angles the anteromedial and posterolateral bundle guide pins closely approximated multiple lateral structures when using an accessory medial arthroscopic portal. Utilizing higher flexion angles increases the margin of error when preparing both femoral tunnels. During preparation of

  15. Microporous silica prepared by organic templating: relationship between the molecular template and pore structure

    International Nuclear Information System (INIS)

    Brinker, C. Jeffrey; Cao, Guozhong; Kale, Rahul P.; Lopez, Gabriel P.; Lu, Yunfeng; Prabakar, S.

    1999-01-01

    Microporous silica materials with a controlled pore size and a narrow pore size distribution have been prepared by sol-gel processing using an organic-templating approach. Microporous networks were formed by pyrolytic removal of organic ligands (methacryloxypropyl groups) from organic/inorganic hybrid materials synthesized by copolymerization of 3-methacryloxypropylsilane (MPS) and tetraethoxysilane (TEOS). Molecular simulations and experimental measurements were conducted to examine the relationship between the microstructural characteristics of the porous silica (e.g., pore size, total pore volume, and pore connectivity) and the size and amount of organic template ligands added. Adsorption measurements suggest that the final porosity of the microporous silica is due to both primary pores (those present in the hybrid materials prior to pyrolysis) and secondary pores (those created by pyrolytic removal of organic templates). Primary pores were inaccessible to N(sub 2) at 77 K but accessible to CO(sub 2) at 195 K; secondary pores were accessible to both N(sub 2) (at 77 K) and CO(sub 2) (at 195 K) in adsorption measurements. Primary porosity decreases with the amount of organic ligands added because of the enhanced densification of MPS/TEOS hybrid materials as the mole fraction of trifunctional MPS moieties increases. pore volumes measured by nitrogen adsorption experiments at 77 K suggest that the secondary (template-derived) porosity exhibits a percolation behavior as the template concentration is increased. Gas permeation experiments indicate that the secondary pores are approximately 5(angstrom) in diameter, consistent with predictions based on molecular simulations

  16. Structural and magnetic properties of cadmium substituted manganese ferrites prepared by hydrothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Mostafa, Nasser Y., E-mail: nmost69@yahoo.com [Faculty of Science, Taif University, P.O. Box: 888, Al-Haweiah, Taif (Saudi Arabia); Chemistry Department, Faculty of Science, Suez Canal University, Ismailia 41522 (Egypt); Zaki, Z.I. [Faculty of Science, Taif University, P.O. Box: 888, Al-Haweiah, Taif (Saudi Arabia); Advanced Materials Division, Central Metallurgical R and D Institute (CMRDI), P.O. Box: 87 Helwan, Cairo (Egypt); Heiba, Z.K. [Faculty of Science, Taif University, P.O. Box: 888, Al-Haweiah, Taif (Saudi Arabia); Physics Department, Faculty of Science, Ain Shams University, Cairo (Egypt)

    2013-03-15

    Cd-substituted manganese ferrite Mn{sub 1-x}Cd{sub x}Fe{sub 2}O{sub 4} powders with x having values 0.0, 0.1, 0.3 and 0.5 have been synthesized by hydrothermal route at 180 Degree-Sign C in presence of NaOH as mineralizer. The obtained ferrite samples were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The XRD analysis showed that pure single phases of cubic ferrites were obtained with x upto 0.3. However, sample with x{>=}0.5 showed hexagonal phase of cadmium hydroxide (Cd(OH){sub 2}) besides the ferrite phase. The increase in Cd-substitution upto x=0.3 leads to an increase in the lattice parameter as well as the average crystallite size of the prepared ferrites. The average crystallite size increased by increasing the Cd-content and was in the range of 39-57 nm. According to VSM results, the saturation magnetization increased with Cd ion substitution. - Highlights: Black-Right-Pointing-Pointer Hydrothermal synthesized of mono dispersed Cd-substituted MnFe{sub 2}O{sub 4} nanoparticles. Black-Right-Pointing-Pointer The change in Ms with increasing Cd-substitution was investigated Black-Right-Pointing-Pointer Pure single phases of cubic ferrites were obtained with x up to 0.3 Black-Right-Pointing-Pointer Sample with x{>=}0.5 showed hexagonal phase of Cd(OH){sub 2} beside the ferrite.

  17. Building Selectivity for NO Sensing in a NOx Mixture with Sonochemically Prepared CuO Structures

    Directory of Open Access Journals (Sweden)

    Max R. Mullen

    2015-12-01

    Full Text Available Several technologies are available for decreasing nitrogen oxide (NOx emissions from combustion sources, including selective catalytic reduction methods. In this process, ammonia reacts with nitric oxide (NO and nitrogen dioxide (NO2. As the stoichiometry of the two reactions is different, electrochemical sensor systems that can distinguish between NO and NO2 in a mixture of these two gases are of interest. Since NO and NO2 can be brought to equilibrium, depending on the temperature and the surfaces that they are in contact with, the detection of NO and NO2 independently is a difficult problem and has not been solved to date. In this study, we explore a high surface area sonochemically prepared CuO as the resistive sensing medium. CuO is a poor catalyst for NOx equilibration, and requires temperatures of 500 C to bring about equilibration. Thus, at 300 C, NO and NO2 retain their levels after interaction with CuO surface. In addition, NO adsorbs more strongly on the CuO over NO2. Using these two concepts, we can detect NO with minimal interference from NO2, if the latter gas concentration does not exceed 20% in a NOx mixture over a range of 100–800 ppm. Since this range constitutes most of the range of total NOx concentrations in diesel and other lean burn engines, this sensor should find application in selective detection of NO in this combustion application. A limitation of this sensor is the interference with CO, but with combustion in excess air, this problem should be alleviated.

  18. Structure of d-3-hydroxybutyrate dehydrogenase prepared in the presence of the substrate d-3-hydroxybutyrate and NAD+

    International Nuclear Information System (INIS)

    Hoque, Md Mominul; Shimizu, Satoru; Juan, Ella Czarina Magat; Sato, Yoshiteru; Hossain, Md Tofazzal; Yamamoto, Tamotsu; Imamura, Shigeyuki; Suzuki, Kaoru; Amano, Hitoshi; Sekiguchi, Takeshi; Tsunoda, Masaru; Takénaka, Akio

    2009-01-01

    The crystal structure of A. faecalisd-3-hydroxybutyrate dehydrogenase prepared in the presence of d-3-hydroxybutyrate and NAD + reveals the substrate/product-binding geometry as the first example which suggests that the catalytic reaction occurs by shuttle movements of a hydrogen negative ion from the substrate to NAD + and from NADH to the product. d-3-Hydroxybutyrate dehydrogenase from Alcaligenes faecalis catalyzes the reversible conversion between d-3-hydroxybutyrate and acetoacetate. The enzyme was crystallized in the presence of the substrate d-3-hydroxybutyrate and the cofactor NAD + at the optimum pH for the catalytic reaction. The structure, which was solved by X-ray crystallography, is isomorphous to that of the complex with the substrate analogue acetate. The product as well as the substrate molecule are accommodated well in the catalytic site. Their binding geometries suggest that the reversible reactions occur by shuttle movements of a hydrogen negative ion from the C3 atom of the substrate to the C4 atom of NAD + and from the C4 atom of NADH to the C3 atom of the product. The reaction might be further coupled to the withdrawal of a proton from the hydroxyl group of the substrate by the ionized Tyr155 residue. These structural features strongly support the previously proposed reaction mechanism of d-3-hydroxybutyrate dehydrogenase, which was based on the acetate-bound complex structure

  19. Preparations, structures and properties of heterobimetallic complexes based on tetrahydrofuran-2,3,4,5-tetracarboxylate

    International Nuclear Information System (INIS)

    Jia, Tian-Jing; Li, Shu-Mu; Cao, Wei; Li, Li-Cun; Zheng, Xiang-Jun; Yuan, Da-Qiang

    2013-01-01

    Transition heterobimetallic metal-organic frameworks based on tetrahydrofuran-2,3,4,5-tetracarboxylicate (FTA), namely [M(H 2 O) 6 ][Cu 2 M(FTA) 2 (H 2 O) 2 ]·4H 2 O [M=Mn (1), Co (2)], and [CuZn(FTA)(H 2 O) 5 ]·H 2 O (3) have been synthesized and characterized. Single-crystal X-ray diffraction indicates that complexes 1 and 2 are isomorphic. In 1 and 2, FTA ligand links the metal ions to a 2-D wave-like negative-charged layer with a topology of (4;6 2 ) 2 (4;6 3 ;8 2 ) 2 (6). They possess 1-D channels with [M(H 2 O) 6 ] 2+ and lattice water molecules enclathrated. While in the complex 3, Cu 2+ and Zn 2+ ions are bridged by FTA to a 2-D neutral layer structure with a (8) 2 (8 4 ;12 2 ) topology. Magnetic properties of 1–3 were analyzed in connection with their structures, which show that there exist weak antiferromagnetic interactions between metal ions. - Graphical abstract: Three heterobimetallic MOFs were constructed through the size-selectivity of TFA coordination sites for different transition metal ions based on the concept of “Hard and Soft Acids and Bases”. Highlights: ► Complexes 1 and 3 contain 2-D wave-like negative-charged layers. ► Complex 2 is a 2-D neutral layer structure with a (8) 2 (8 4 ;12 2 ) topology. ► Complexes 1–3 are the first example of heterobimetallic MOFs based on FTA. ► The coordination sites of FTA show size-selectivity to metal ions

  20. Preparations, structures and properties of heterobimetallic complexes based on tetrahydrofuran-2,3,4,5-tetracarboxylate

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Tian-Jing; Li, Shu-Mu; Cao, Wei [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Li, Li-Cun [College of Chemistry, Nankai University, Tianjin 300071 (China); Zheng, Xiang-Jun, E-mail: xjzheng@bnu.edu.cn [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Yuan, Da-Qiang [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

    2013-05-01

    Transition heterobimetallic metal-organic frameworks based on tetrahydrofuran-2,3,4,5-tetracarboxylicate (FTA), namely [M(H₂O)₆][Cu₂M(FTA)₂(H₂O)₂]·4H₂O [M=Mn (1), Co (2)], and [CuZn(FTA)(H₂O)₅]·H₂O (3) have been synthesized and characterized. Single-crystal X-ray diffraction indicates that complexes 1 and 2 are isomorphic. In 1 and 2, FTA ligand links the metal ions to a 2-D wave-like negative-charged layer with a topology of (4;6²)₂(4;6³;8²)₂(6). They possess 1-D channels with [M(H₂O)₆]²⁺ and lattice water molecules enclathrated. While in the complex 3, Cu²⁺ and Zn²⁺ ions are bridged by FTA to a 2-D neutral layer structure with a (8)₂(8⁴;12²) topology. Magnetic properties of 1–3 were analyzed in connection with their structures, which show that there exist weak antiferromagnetic interactions between metal ions. - Graphical abstract: Three heterobimetallic MOFs were constructed through the size-selectivity of TFA coordination sites for different transition metal ions based on the concept of “Hard and Soft Acids and Bases”. Highlights: • Complexes 1 and 3 contain 2-D wave-like negative-charged layers. • Complex 2 is a 2-D neutral layer structure with a (8)₂(8⁴;12²) topology. • Complexes 1–3 are the first example of heterobimetallic MOFs based on FTA. • The coordination sites of FTA show size-selectivity to metal ions.

  1. Preparation and properties of GO-PVA composite hydrogel with oriented structure

    Science.gov (United States)

    Liu, Huanqing; Zhang, Gongzheng; Li, Huanjun

    2017-03-01

    We fabricated GO-PVA composite hydrogels with oriented structure by directional freezing and repeated freeze-thawing, which owned superior mechanical property and thermostability than PVA hydrogel. Due to physical interactions such as hydrogen bonding between surface of GO and PVA chains, GO-PVA composite hydrogel possessed higher crosslinking density and smaller pore size and can resist higher temperature and stronger force from outside than PVA hydrogel. These unique properties will endow GO-PVA hydrogel with greater potential application in biomedical materials.

  2. The structure and growth mechanism of Si nanoneedles prepared by plasma-enhanced chemical vapor deposition

    Czech Academy of Sciences Publication Activity Database

    Červenka, Jiří; Ledinský, Martin; Stuchlík, Jiří; Stuchlíková, The-Ha; Bakardjieva, Snejana; Hruška, Karel; Fejfar, Antonín; Kočka, Jan

    2010-01-01

    Roč. 21, č. 41 (2010), 415604/1-415604/7 ISSN 0957-4484 R&D Projects: GA MŠk(CZ) LC06040; GA AV ČR KAN400100701; GA MŠk LC510 EU Projects: European Commission(XE) 240826 - PolySiMode Institutional research plan: CEZ:AV0Z10100521; CEZ:AV0Z40320502 Keywords : nanoneedles * nanowires * silicon * plasma * chemical vapor deposition * crystal structure * growth * phonon * SEM * Raman Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.644, year: 2010

  3. Structure, electrochromic and optical properties of WO3 film prepared by dip coating-pyrolysis

    International Nuclear Information System (INIS)

    Yang Haitao; Shang Fuliang; Gao Ling; Han Haitao

    2007-01-01

    The tungsten oxide (WO 3 ) film was grown by dip coating-pyrolysis method with the PEG-400 as the structure-directing agent. Microstructure of the WO 3 film was characterized by TG-DSC, XRD and SEM techniques. It was found that the film annealed at 350 deg. C for 2 h comprised cubic WO 3 and orthorhombic WO 3 . The measurements of the cyclic voltammetry (CV) and UV-vis spectrum suggested that the WO 3 film had a good electrochromic reversibility performance. The film possessed excellent modulation to the visible light and the maximal average transmittance modulation reached 70.06%

  4. Influence of boat material on the structure, stoichiometry and optical properties of gallium sulphide films prepared by thermal evaporation

    International Nuclear Information System (INIS)

    Rao, Pritty; Kumar, Sanjiv; Sahoo, N.K.

    2015-01-01

    The paper describes the deposition of thin films of gallium sulphide on soda-lime glass substrates by thermal evaporation of chemically synthesized powders consisting of gallium sulphide and gallium oxyhydroxide from a Mo or Ta boat and the evolution of their compositional, structural and optical properties on vacuum annealing. The films deposited from Mo or Ta boats possessed distinctly different properties. The Mo-boat evaporated pristine films were amorphous, transparent (α ∼ 10 3  cm −1 ) in visible region and had a direct band gap of about 3.2 eV. Vacuum annealing at 723 K brought about their crystallization predominantly into cubic γ-Ga 2 S 3 and a blue shift by about 0.2 eV. The Ta-boat evaporated pristine films were also amorphous but were absorbing (α ∼ 10 4  cm −1 ) and had a direct band gap of about 2.1 eV. These crystallized into hexagonal GaS and experienced a blue shift by more than 1.0 eV on vacuum annealing at 723 K. The dissimilar properties of the two kinds of films arose mainly from their different atomic compositions. The Mo-boat evaporated pristine films contained Ga and S in ∼1:1 atomic proportions while those prepared using Ta-boat were Ga rich which impaired their transmission characteristics. The former composition favoured the stabilization of S rich gallium sulphide (Ga 2 S 3 ) phase while the latter stabilised S deficient species, GaS. Besides inducing crystallization, vacuum annealing at 723 K also caused the diffusion of Ga in excess of atomic composition of the phase formed, into soda-lime glass which improved the optical transmission of the films. Gallium oxyhydroxide, an inevitable co-product of the chemical synthetic process, in the evaporant introduced oxygen and hydrogen impurities in the films which do not seem to significantly influence their optical properties. - Highlights: • Gallium sulphide films are prepared by thermal evaporation from a Mo or Ta boat. • Mo-boat prepared pristine film has Ga

  5. Preparation of high purity metallic protactinium. Crystal structure and dissolution enthalpy of the metal

    International Nuclear Information System (INIS)

    Bohet, J.

    1977-01-01

    Some 300 mg of Pa have been produced in a high purity metallic state. Protactinium monocarbide has been obtained by the carboreduction of Pa 2 O 5 . Protactinium iodide, produced by the direct reaction of iodine on the carbide, has been sublimated at 420 0 C and thermally dissociated at 1200 0 C on a W wire. In these conditions Pa metal has been deposited with a yield greater than 85% and presents a bct structure stable at room temperature (a=3.921+-0.001A and c=3.235+-0.001A). The fcc phase (Fm3m type) (a=5.018+-0.001A) has been obtained by quenching metallic samples (bct) heated in argon at 1500 0 C. The chemical analysis and the transformation of the fcc into bct phase by controlled heat treatments show the presence of this high temperature phase in the metal. Protactinium mononitride (5.58% N) produced by direct reaction of N on Pa at 1100 0 C presents the same fcc crystal structure but the lattice parameter is higher (a=5.047+-0.001A). The dissolution heat of metallic Pa (bct) has been determined in the aqueous solution HCl 12M - HF 0.05M at 298.15+-0.05 K. The standard formation enthalpies of the ionic species Pa(IV) and Pa(V) are respectively equal to -672+-15 kJ.mol -1 and -821+-15 kJ.mol -1

  6. Preparation of biomimetic nano-structured films with multi-scale roughness

    Science.gov (United States)

    Shelemin, A.; Nikitin, D.; Choukourov, A.; Kylián, O.; Kousal, J.; Khalakhan, I.; Melnichuk, I.; Slavínská, D.; Biederman, H.

    2016-06-01

    Biomimetic nano-structured films are valuable materials in various applications. In this study we introduce a fully vacuum-based approach for fabrication of such films. The method combines deposition of nanoparticles (NPs) by gas aggregation source and deposition of overcoat thin film that fixes the nanoparticles on a surface. This leads to the formation of nanorough surfaces which, depending on the chemical nature of the overcoat, may range from superhydrophilic to superhydrophobic. In addition, it is shown that by proper adjustment of the amount of NPs it is possible to tailor adhesive force on superhydrophobic surfaces. Finally, the possibility to produce NPs in a wide range of their size (45-240 nm in this study) makes it possible to produce surfaces not only with single scale roughness, but also with bi-modal or even multi-modal character. Such surfaces were found to be superhydrophobic with negligible water contact angle hysteresis and hence truly slippery.

  7. Structure of alumina supported vanadia catalysts for oxidative dehydrogenation of propane prepared by flame spray pyrolysis

    DEFF Research Database (Denmark)

    Høj, Martin; Jensen, Anker Degn; Grunwaldt, Jan-Dierk

    2013-01-01

    .%. The catalysts were subsequently characterized by BET surface area, X-ray diffraction (XRD), Raman, UV–vis diffuse reflectance and X-ray absorption spectroscopy (XAS) as well as measurement of the catalytic performance. The catalysts had specific surface areas from 143 to 169 m2/g corresponding to average......A series of five vanadia on alumina catalysts for oxidative dehydrogenation of propane to propene were synthesized by flame spray pyrolysis (FSP) using vanadium(III)acetylacetonate and aluminium(III)acetylacetonate dissolved in toluene as precursors. The vanadium loading was 2, 3, 5, 7.5 and 10wt...... X-ray absorption near edge structure (XANES) spectroscopy showed that the vanadia can be reduced when operating at low oxygen concentrations. The catalyst performance was determined in fixed bed reactors with an inlet gas composition of C3H8/O2/N2=5/25/70. The main products were propene, CO and CO2...

  8. Structural, optical and electrical properties of indium tin oxide thin films prepared by spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Benamar, E.; Rami, M.; Messaoudi, C.; Sayah, D.; Ennaoui, A. [Deptartmento de Physique, Laboratoire de Physique des Materiaux, Faculte des Sciences, BP 1014, Ave Inb Battouta, Rabat (Morocco)

    1998-11-27

    Spray pyrolysis process has been used to deposit highly transparent and conducting films of tin-doped indium oxide onto glass substrates. The electrical, structural and optical properties have been investigated as a function of various deposition parameters namely dopant concentrations, temperature and nature of substrate. The morphology of the surface as a function of the substrate temperature has been studied using atomic force microscopy. XRD has shown that deposited films are polycrystalline without second phases and have a preferred orientation (4 0 0). Indium tin oxide layers with low resistivity values around 4x10{sup -5} {Omega} cm and transmission coefficients in the visible and near-infrared range of about 85-90% have been easily obtained

  9. Preparation, structural and optical characterization of ZnO, ZnO: Al nanopowder

    Energy Technology Data Exchange (ETDEWEB)

    Mohan, R. Raj [Department of ECE, Gojan School of Business and Technology, Chennai (India); Rajendran, K. [Department of Electronics, Government Arts College for Women, Ramanathapuram, TN (India); Sambath, K. [Department of ECS, Sri Krishna Arts and Science College, Coimbatore, TN (India)

    2014-01-28

    In this paper, ZnO and ZnO:Al nanopowders have been synthesized by low cost hydrothermal method. Zinc nitrate, hexamethylenetetramine (HMT) and aluminium nitrate are used as precursors for ZnO and AZO with different molar ratios. The structural and optical characterization of doped and un-doped ZnO powders have been investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDAX), photoluminescence (PL) and ultra violet visible (UV-Vis) absorption studies. The SEM results show that the hydrothermal synthesis can be used to obtain nanoparticles with different morphology. It is observed that the grain size of the AZO nanoparticles increased with increasing of Al concentration. The PL measurement of AZO shows that broad range of green emission around 550nm with high intensity. The green emission resulted mainly because of intrinsic defects.

  10. Preparation of biomimetic nano-structured films with multi-scale roughness

    International Nuclear Information System (INIS)

    Shelemin, A; Nikitin, D; Choukourov, A; Kylián, O; Kousal, J; Khalakhan, I; Melnichuk, I; Slavínská, D; Biederman, H

    2016-01-01

    Biomimetic nano-structured films are valuable materials in various applications. In this study we introduce a fully vacuum-based approach for fabrication of such films. The method combines deposition of nanoparticles (NPs) by gas aggregation source and deposition of overcoat thin film that fixes the nanoparticles on a surface. This leads to the formation of nanorough surfaces which, depending on the chemical nature of the overcoat, may range from superhydrophilic to superhydrophobic. In addition, it is shown that by proper adjustment of the amount of NPs it is possible to tailor adhesive force on superhydrophobic surfaces. Finally, the possibility to produce NPs in a wide range of their size (45–240 nm in this study) makes it possible to produce surfaces not only with single scale roughness, but also with bi-modal or even multi-modal character. Such surfaces were found to be superhydrophobic with negligible water contact angle hysteresis and hence truly slippery. (paper)

  11. Structural and morphological characterization of TiO2 powders prepared using Pechini and combustion reaction

    International Nuclear Information System (INIS)

    Ribeiro, P.C.; Almeida, E.P.; Costa, A.C.F.M. da; Lira, H.L.; Kiminami, R.H.G.A.

    2010-01-01

    TiO 2 is a semiconductor oxide and polymorphic and can exist in three crystallographic forms: anatase, rutile and broquita, and forms anatase and rutile are the major interests in scientific research. Thus, this study aims to synthesize TiO 2 by Pechini methods and combustion reaction and to evaluate the influence of synthesis methods in structural and morphological characteristics of the samples. The nanopowders were characterized by X-ray diffraction, nitrogen adsorption, and particle size distribution and scanning electron microscopy. The results of X-ray diffraction showed that the samples obtained by the Pechini method showed the single phase anatase with crystallite size of 20 nm and surface area of 49.44 m 2 /g, whereas the samples synthesized by combustion reaction using glycine as fuel showed the rutile phase as major phase and traces of anatase phase, with crystallite size of 65 nm and surface area 4.34 m 2 /g. (author)

  12. Structural characterization of pure and doped calcium phosphate bioceramics prepared by simple solid state method

    International Nuclear Information System (INIS)

    Ahmed, S.; Kabir, H.; Nigar, F.

    2011-01-01

    Calcium Phosphate based bioceramic materials, in pure and doped forms have been successfully synthesized from egg shells by using solid-state method for the first time. Considering the diverse role of zinc and fluoride in biological functions, these two ions were chosen to develop the substituted bioceramic materials. Structural characterizations of these developed bioceramics were performed by using FTIR, XRD, SEM and EDS techniques. The results revealed that the fluoride doped apatite was formed in single phase containing hydroxyapatite while pure and Zinc doped apatites contained -TCP with hydroxyapatite. Experimental results and the crystallographic parameters matched well with the literature values indicating that the present experimental protocol favoured the formation of the desired bioceramics. However, to synthesize the (Ca (PO)) based bioceramic materials, such a simple solid-state approach would obviously be very helpful, not only in making the process economically feasible, but also in creating an effective material recycling technology for waste-management. (author)

  13. 18-Membered cyclic esters derived from glycolide and lactide: preparations, structures and coordination to sodium ions

    Energy Technology Data Exchange (ETDEWEB)

    Chisholm, Malcolm H.; Gallucci, Judith C.; Yin, Hongfeng (OSU)

    2008-06-30

    From reactions between glycolide or lactide (4 equiv.) with 4-dimethylaminopyridine, DMAP (1 equiv.) and NaBPh4 (1 equiv.) in benzene at 70 C the cyclic ester adducts (CH{sub 2}C(O)O){sub 6}NaBPh{sub 4} and (CHMeC(O)O){sub 6}NaBPh{sub 4} are formed respectively. The structures of the salts Na[(S,R,S,R,S,R)-(CH{sub 3}CHC(O)O){sub 6}]{sub 2}BPh{sub 4} {center_dot} CH{sub 3}CN and (CH{sub 2}C(O)O){sub 6}NaBPh{sub 4} {center_dot} (CH{sub 3}CN){sub 2} are reported. The cyclic esters were separated by chromatography and the structures of (CH{sub 2}C(O)O){sub 6}, (S,R,R,R,R,R)-(CHMeC(O)O){sub 6} and (S,S,R,R,R,R)-(CHMeC(O)O){sub 6} were determined. The {sup 1}H and {sup 13}C NMR data are reported for one of each of the six enantiomers of (CHMeC(O)O){sub 6} and the two meso isomers. The mechanism for the formation of these 18-membered rings is discussed in terms of an initial reaction between DMAP and NaBPh{sub 4} in hot benzene that produces NaPh and DMAP:BPh{sub 3} in the presence of the monomer lactide. The cyclic esters (CHMeC(O)O){sub 6} can also be obtained from the reaction between polylactide, PLA, in the presence of DMAP and NaBPh{sub 4}. The cyclic esters 3-methyl-1,4-dioxane-2,5-dione and 3,6,6-trimethyl-1,4-dioxane-2,5-dione undergo similar ring enlarging reactions to give cyclic 18-membered ring esters as determined by ESI-MS.

  14. Preparation, structural and magnetic investigation, and toxicity assays of SPIONs as carriers of nitric oxide

    Energy Technology Data Exchange (ETDEWEB)

    Goncalves, Luana Caroline; Seabra, Amedea Barozzi; Haddad, Paula Silvia, E-mail: luana.unifesp@gmail.com [Universidade Federal de Sao Paulo (UNIFESP), Sao Paulo, SP (Brazil)

    2016-07-01

    Full text: The features of nanoparticles and their biocompatibility are being the subject of great interest in biomedical areas. Structural and magnetic features and the evaluation of cytotoxicity of nanoparticles (NPs) are extremely important in nanomedicine [1]. In this scenario, the present work is focused on the synthesis, characterization and cytotoxic evaluation of superparamagnetic iron oxide nanoparticles (SPIONs). The nanoparticle of magnetite (Fe{sub 3}O{sub 4}) was obtained from thermal decomposition [2] of Fe(acac){sub 3} compound. At first, we investigated the synthetic parameters, such as temperature and reaction time, in order to improve physicochemical properties of the nanoparticles. In addition, the surface of synthesized NPs was functionalized with mercaptosuccinic acid (MSA) to form thiolate nanoparticles. Free thiol groups of thiolate nanoparticles were nitrosated leading to S-nitrosothiol groups (-SNO), which are able to release the free radical nitric oxide (NO), involved in several biological processes. The structural characterization was done by FTIR and XRD techniques, showing the formation of Fe{sub 3}O{sub 4} with size of 11 nm, in solid state. Moreover, magnetization measurements showed superparamagnetic behavior. The amount of free - SH groups onto surface of NPs was found to be 2,81 ± 1.63 μmol SH per gram of NP. Dynamic light scattering revealed the hydrodynamic size of 412.10 ± 3.20 nm, polidispersitivity of 0.32 and zeta potential of -22.10. Upon nitrosation of thiolate NPs, 8.38 ± 4.71 mmol of NO per gram of NPs were obtained, revealing that NPs are able to spontaneously release therapeutic amount of NO suggesting the promising biomedical applications of these materials. References: [1] A. B. SEABRA e P. S. HADDAD 'Cytotoxicity and genotoxicity of iron oxide nanoparticles' in: Nanotoxicology, 1. ed., vol. 1, New York, Springer, p. 265-280, 2014. (author)

  15. Structural and optical studies of nano-structure silica gel doped with different rare earth elements, prepared by two different sol -gel techniques

    International Nuclear Information System (INIS)

    Battisha, I.K.; El Beyally, A.; Seliman, S.I.; El Nahrawi, A.S.

    2005-01-01

    Structural and optical characteristics of pure silica gel (silica-xerogel, SiO 2 ) and doped with different concentrations ranging from 1 up to 6% of some rare earth (REEs) ions such as, praseodymium Pr +3 ,and Europium Eu +3 , Erbium Er +3 and Holmium Ho +3 , ions, in the form of thin film and monolith materials were prepared by sol - gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural and optical features of sol-gel derived monolith and thin films are analyzed and compared, namely the structure of nano-particle monolith and thin film silica-gel samples, based on X-ray diffraction (XRD). The types of structural information obtainable are compared in detail. It is show that the XRD spectra of a-cristobalite are obtained for the two type materials and even by doping with the four REEs ions. Optical measurements of monolith and thin films were also studied and compared, the normal transmission and specular reflection were measured. The refractive index were calculated and discussed

  16. Optical and structural properties of ZnO/ZnMgO composite thin films prepared by sol–gel technique

    International Nuclear Information System (INIS)

    Xu, Linhua; Su, Jing; Chen, Yulin; Zheng, Gaige; Pei, Shixin; Sun, Tingting; Wang, Junfeng; Lai, Min

    2013-01-01

    Highlights: ► ZnMgO thin film and ZnO/ZnMgO composite thin film have been prepared by sol–gel method. ► The intensity of ultraviolet emission of ZnMgO thin film is enhanced two times compared with that of pure ZnO thin film. ► Compared with ZnMgO thin film, ZnO/ZnMgO composite thin film shows better crystallization and optical properties. ► ZnO/ZnMgO composite thin films prepared by sol–gel method have potential applications in many optoelectronic devices. - Abstract: In this study, pure ZnO thin film, Mg-doped ZnO (ZnMgO) thin film, ZnO/ZnMgO and ZnMgO/ZnO composite thin films were prepared by sol–gel technique. The structural and optical properties of the samples were analyzed by X-ray diffraction, scanning electron microscopy, UV–visible spectrophotometer, ellipsometer and photoluminescence spectra, respectively. The results showed that the incorporation of Mg increased the strain, broadened the optical bandgap, and improved the intensity of ultraviolet emission of ZnO thin film. The full width at half maximum (FWHM) of the ultraviolet emission peak was also increased due to Mg-doping at the same time. Compared with pure ZnO and ZnMgO thin films, the ZnO/ZnMgO thin film showed better crystalline quality and ultraviolet emission performance, smaller strains and higher transmittance in the visible range.

  17. Influence of Substrate Temperature on Structural, Electrical and Optical Properties of Ito Thin Films Prepared by RF Magnetron Sputtering

    Science.gov (United States)

    He, Bo; Zhao, Lei; Xu, Jing; Xing, Huaizhong; Xue, Shaolin; Jiang, Meng

    2013-10-01

    In this paper, we investigated indium-tin-oxide (ITO) thin films on glass substrates deposited by RF magnetron sputtering using ceramic target to find the optimal condition for fabricating optoelectronic devices. The structural, electrical and optical properties of the ITO films prepared at various substrate temperatures were investigated. The results indicate the grain size increases with substrate temperature increases. As the substrate temperature grew up, the resistivity of ITO films greatly decreased. The ITO film possesses high quality in terms of electrode functions, when substrate temperature is 480°C. The resistivity is as low as 9.42 × 10-5 Ω•cm, while the carrier concentration and mobility are as high as 3.461 × 1021 atom/cm3 and 19.1 cm2/Vṡs, respectively. The average transmittance of the film is about 95% in the visible region. The novel ITO/np-Silicon frame, which prepared by RF magnetron sputtering at 480°C substrate temperature, can be used not only for low-cost solar cell, but also for high quantum efficiency of UV and visible lights enhanced photodetector for various applications.

  18. Systematic dynamic viscoelasticity measurements for chitin nanofibers prepared with various concentrations, disintegration times, acidities, and crystalline structures.

    Science.gov (United States)

    Suenaga, Shin; Osada, Mitsumasa

    2018-04-17

    Dynamic viscoelasticities were measured for chitin nanofiber (ChNF) dispersions prepared with various concentrations, disintegration times, acidities, and crystalline structures. The 0.05 w/v% dispersions of pH neutral ChNFs continuously exhibited elastic behavior. The 0.05 w/v% dispersions of acidified ChNFs, on the other hand, transitioned from a colloidal dispersion to a critical gel and then exhibited elastic behavior with increasing ChNF concentration. A double-logarithmic chart of the concentration vs. the storage modulus was prepared and indicated the fractal dimension and the nanostructure in the dispersion. The results determined that the neutral α- and β-ChNFs were dispersed but showed some remaining aggregations and that the acidified β-ChNFs were completely individualized. In addition, the α-chitin steadily disintegrated with increasing disintegration time, and the aspect ratio of the β-chitin decreased as a result of the exscessive disintegration. The storage moduli of the ChNFs were greater than those of chitin solutions, nanorods, and nanowhiskers with the same solids concentrations. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Preparation, Surface and Pore Structure of High Surface Area Activated Carbon Fibers from Bamboo by Steam Activation

    Directory of Open Access Journals (Sweden)

    Xiaojun Ma

    2014-06-01

    Full Text Available High surface area activated carbon fibers (ACF have been prepared from bamboo by steam activation after liquefaction and curing. The influences of activation temperature on the microstructure, surface area and porosity were investigated. The results showed that ACF from bamboo at 850 °C have the maximum iodine and methylene blue adsorption values. Aside from the graphitic carbon, phenolic and carbonyl groups were the predominant functions on the surface of activated carbon fiber from bamboo. The prepared ACF from bamboo were found to be mainly type I of isotherm, but the mesoporosity presented an increasing trend after 700 °C. The surface area and micropore volume of samples, which were determined by application of the Brunauer-Emmett-Teller (BET and t-plot methods, were as high as 2024 m2/g and 0.569 cm3/g, respectively. It was also found that the higher activation temperature produced the more ordered microcrystalline structure of ACF from bamboo.

  20. Optimized cryo-focused ion beam sample preparation aimed at in situ structural studies of membrane proteins.

    Science.gov (United States)

    Schaffer, Miroslava; Mahamid, Julia; Engel, Benjamin D; Laugks, Tim; Baumeister, Wolfgang; Plitzko, Jürgen M

    2017-02-01

    While cryo-electron tomography (cryo-ET) can reveal biological structures in their native state within the cellular environment, it requires the production of high-quality frozen-hydrated sections that are thinner than 300nm. Sample requirements are even more stringent for the visualization of membrane-bound protein complexes within dense cellular regions. Focused ion beam (FIB) sample preparation for transmission electron microscopy (TEM) is a well-established technique in material science, but there are only few examples of biological samples exhibiting sufficient quality for high-resolution in situ investigation by cryo-ET. In this work, we present a comprehensive description of a cryo-sample preparation workflow incorporating additional conductive-coating procedures. These coating steps eliminate the adverse effects of sample charging on imaging with the Volta phase plate, allowing data acquisition with improved contrast. We discuss optimized FIB milling strategies adapted from material science and each critical step required to produce homogeneously thin, non-charging FIB lamellas that make large areas of unperturbed HeLa and Chlamydomonas cells accessible for cryo-ET at molecular resolution. Copyright © 2016 Elsevier Inc. All rights reserved.

  1. Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications

    Directory of Open Access Journals (Sweden)

    Venkatesan K

    2015-10-01

    Full Text Available Kaliyamoorthy Venkatesan,1 Dhanakotti Rajan Babu,1 Mane Prabhu Kavya Bai,2 Ravi Supriya,2 Radhakrishnan Vidya,2 Saminathan Madeswaran,1 Pandurangan Anandan,3 Mukannan Arivanandhan,3 Yasuhiro Hayakawa3 1School of Advanced Sciences, 2School of Bio Sciences and Technology, VIT University, Vellore, Tamil Nadu, India; 3Research Institute of Electronics, Shizuoka University, Hamamatsu, Japan Abstract: Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4 magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311 of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed. Keywords: cytotoxicity, HR-TEM, magnetic nanoparticles, VSM 

  2. Two Ti13-oxo-clusters showing non-compact structures, film electrode preparation and photocurrent properties.

    Science.gov (United States)

    Hou, Jin-Le; Luo, Wen; Wu, Yin-Yin; Su, Hu-Chao; Zhang, Guang-Lin; Zhu, Qin-Yu; Dai, Jie

    2015-12-14

    Two benzene dicarboxylate (BDC) and salicylate (SAL) substituted titanium-oxo-clusters, Ti13O10(o-BDC)4(SAL)4(O(i)Pr)16 (1) and Ti13O10(o-BDC)4(SAL-Cl)4(O(i)Pr)16 (2), are prepared by one step in situ solvothermal synthesis. Single crystal analysis shows that the two Ti13 clusters take a paddle arrangement with an S4 symmetry. The non-compact (non-sphere) structure is stabilized by the coordination of BDC and SAL. Film photoelectrodes are prepared by the wet coating process using the solution of the clusters and the photocurrent response properties of the electrodes are studied. It is found that the photocurrent density and photoresponsiveness of the electrodes are related to the number of coating layers and the annealing temperature. Using ligand coordinated titanium-oxo-clusters as the molecular precursors of TiO2 anatase films is found to be effective due to their high solubility, appropriate stability in solution and hence the easy controllability.

  3. Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications.

    Science.gov (United States)

    Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

    2015-01-01

    Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed.

  4. Structural study of thin films prepared from tungstate glass matrix by Raman and X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Montanari, Bianca; Barbosa, Anne J.; Ribeiro, Sidney J.L.; Messaddeq, Younes [Departamento de Quimica Geral e Inorganica, Instituto de Quimica, UNESP, CP 355, CEP 14800-900 Araraquara, SP (Brazil); Poirier, Gael [Departamento de Ciencias Exatas, UNIFAL-MG, CEP 37130-000 Alfenas, MG (Brazil)], E-mail: gael@unifal-mg.edu.br; Li, Maximo S. [Instituto de Fisica, USP, CP 369, CEP 13560-970 Sao Carlos, SP (Brazil)

    2008-06-30

    Thin films were prepared using glass precursors obtained in the ternary system NaPO{sub 3}-BaF{sub 2}-WO{sub 3} and the binary system NaPO{sub 3}-WO{sub 3} with high concentrations of WO{sub 3} (above 40% molar). Vitreous samples have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. Several structural characterizations were performed by Raman spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES) at the tungsten L{sub I} and L{sub III} absorption edges. XANES investigations showed that tungsten atoms are only sixfold coordinated (octahedral WO{sub 6}) and that these films are free of tungstate tetrahedral units (WO{sub 4}). In addition, Raman spectroscopy allowed identifying a break in the linear phosphate chains as the amount of WO{sub 3} increases and the formation of P-O-W bonds in the films network indicating the intermediary behavior of WO{sub 6} octahedra in the film network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed identifying the presence of W-O{sup -} and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO{sub 3} concentrated samples (above 40% molar) attributed to the formation of WO{sub 6} clusters.

  5. Structural and electrical transport properties of La2Mo2O9 thin films prepared by pulsed laser deposition

    Science.gov (United States)

    Paul, T.; Ghosh, A.

    2017-04-01

    We have studied the structure and electrical properties of La2Mo2O9 thin films of different thicknesses prepared by the laser deposition technique at different substrate temperatures. The structural properties of the thin films have been investigated using XRD, XPS, AFM, TEM, SEM, and Raman spectroscopy. The electrical transport properties of the thin films have been investigated in wide temperature and frequency ranges. The cubic nature of the thin films has been confirmed from structural analysis. An enhancement of the oxygen ion conductivity of the films up to five orders of magnitude is obtained compared to that of the bulk La2Mo2O9, suggesting usefulness of the thin films as electrolytes in micro-solid oxide fuel cells. The enhanced dc ionic conductivity of the thin films has been interpreted using the rule of the mixture model, while a power law model has been used to investigate the frequency and temperature dependences of the conductivity. The analysis of the results predicts the three-dimensional oxygen ion conduction in the thin films.

  6. Effects of Thermal Cross-Linking on the Structure and Property of Asymmetric Membrane Prepared from the Polyacrylonitrile

    Directory of Open Access Journals (Sweden)

    Xin Jin

    2018-05-01

    Full Text Available Improving the thermal and chemical stabilities of classical polymer membranes will be beneficial to extend their applications in the high temperature or aggressive environment. In this work, the asymmetric ultrafiltration membranes prepared from the polyacrylonitrile (PAN were used to fabricate the cross-linking asymmetric (CLA PAN membranes via thermal cross-linking in air to improve their thermal and chemical stabilities. The effects of thermal cross-linking parameters such as temperature and holding time on the structure, gas separation performance, thermal and chemical stabilities of PAN membranes were investigated by Fourier transform infrared spectroscopy (FTIR, X-ray photoelectron spectroscopy (XPS, positron annihilation lifetime spectroscopy (PALS, scanning electron microscopy (SEM, thermogravimetic analysis (TGA and gas permeation test. The thermal cross-linking significantly influences the chemical structure, microstructure and pore structure of PAN membrane. During the thermal cross-linking, the shrinkage of membrane and coalescence or collapse of pore and microstructure make large pores diminish, small pores disappear and pore volumes reduce. The gas permeances of CLA-PAN membranes increase as the increasing of cross-linking temperature and holding time due to the volatilization of small molecules. The CLA-PAN membranes demonstrate excellent thermal and chemical stabilities and present good prospects for application in ultrafiltration for water treatment and for use as a substrate for nanofiltration or gas separation with an aggressive and demanding environment.

  7. Present activities for the preparation of a Japanese draft of structural design guidelines for the experimental fusion reactor

    International Nuclear Information System (INIS)

    Miya, K.; Muto, Y.; Takatsu, H.; Hada, K.; Koizumi, K.; Jitsukawa, S.; Arai, T.; Ohkawa, Y.; Shimakawa, T.; Aoto, K.; Shiraishi, H.; Takagi, T.; Miki, N.; Takahashi, S.; Sato, K.; Takemasa, F.; Kasaba, M.; Kudough, F.; Fujita, J.; Kajiura, S.; Kinoshita, S.

    1996-01-01

    Since November 1990, systematic research has been carried out in preparation for a Japanese draft of structural design guidelines for the experimental fusion reactor. This report summarizes the major results of the work and the status of these efforts. A classification of components and definition of operating conditions are proposed on the basis of the ITER-CDA design, in the light of the safety characteristics of the fusion reactor and relevant conventions for the existing fission reactor design code. Specific issues regarding the structural design of the experimental fusion reactor are discussed based on the experimental and analytical work. The validity of the existing structural design method is confirmed for the use of irradiated 316 SS, irrespective of the significant reduction in uniform elongation capability caused by heavy neutron irradiation. Further important phenomena are treated such as magnetic damping, magnetic stiffness and fracture due to electromagnetic forces. Finally, the issues concerned with welding and non-destructive examinations are discussed with relevance to component classification. (orig.)

  8. Optical and structural properties of protein/gold hybrid bio-nanofilms prepared by layer-by-layer method.

    Science.gov (United States)

    Pál, Edit; Hornok, Viktória; Sebok, Dániel; Majzik, Andrea; Dékány, Imre

    2010-08-01

    Lysozyme/gold thin layers were prepared by layer-by-layer (LbL) self-assembly method. The build-up of the films was followed by UV-vis-absorbance spectra, quartz crystal microbalance (QCM) and surface plasmon resonance (SPR) techniques. The structural property of films was examined by X-ray diffraction (XRD) measurements, while their morphology was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). It was found that gold nanoparticles (NPs) had cubic crystalline structure, the primary particles form aggregates in the thin layer due to the presence of lysozyme molecules. The UV-vis measurements prove change in particle size while the colour of the film changes from wine-red to blue. The layer thickness of films was determined using the above methods and the loose, porous structure of the films explains the difference in the results. The vapour adsorption property of hybrid layers was also studied by QCM using different saturated vapours and ammonia gas. The lysozyme/Au films were most sensitive for ammonia gas among the tested gases/vapours due to the strongest interaction between the functional groups of the protein. Copyright 2010 Elsevier B.V. All rights reserved.

  9. Atomic and electronic structure of a copper/graphene interface as prepared and 1.5 years after

    Science.gov (United States)

    Boukhvalov, D. W.; Bazylewski, P. F.; Kukharenko, A. I.; Zhidkov, I. S.; Ponosov, Yu. S.; Kurmaev, E. Z.; Cholakh, S. O.; Lee, Y. H.; Chang, G. S.

    2017-12-01

    We report the results of X-ray spectroscopy and Raman measurements of as-prepared graphene on a high quality copper surface and the same materials after 1.5 years under different conditions (ambient and low humidity). The obtained results were compared with density functional theory calculations of the formation energies and electronic structures of various structural defects in graphene/Cu interfaces. For evaluation of the stability of the carbon cover, we propose a two-step model. The first step is oxidation of the graphene, and the second is perforation of graphene with the removal of carbon atoms as part of the carbon dioxide molecule. Results of the modeling and experimental measurements provide evidence that graphene grown on high-quality copper substrate becomes robust and stable in time (1.5 years). However, the stability of this interface depends on the quality of the graphene and the number of native defects in the graphene and substrate. The effect of the presence of a metallic substrate with defects on the stability and electronic structure of graphene is also discussed

  10. RealityConvert: a tool for preparing 3D models of biochemical structures for augmented and virtual reality.

    Science.gov (United States)

    Borrel, Alexandre; Fourches, Denis

    2017-12-01

    There is a growing interest for the broad use of Augmented Reality (AR) and Virtual Reality (VR) in the fields of bioinformatics and cheminformatics to visualize complex biological and chemical structures. AR and VR technologies allow for stunning and immersive experiences, offering untapped opportunities for both research and education purposes. However, preparing 3D models ready to use for AR and VR is time-consuming and requires a technical expertise that severely limits the development of new contents of potential interest for structural biologists, medicinal chemists, molecular modellers and teachers. Herein we present the RealityConvert software tool and associated website, which allow users to easily convert molecular objects to high quality 3D models directly compatible for AR and VR applications. For chemical structures, in addition to the 3D model generation, RealityConvert also generates image trackers, useful to universally call and anchor that particular 3D model when used in AR applications. The ultimate goal of RealityConvert is to facilitate and boost the development and accessibility of AR and VR contents for bioinformatics and cheminformatics applications. http://www.realityconvert.com. dfourch@ncsu.edu. Supplementary data are available at Bioinformatics online. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

  11. Growth Mechanism and Surface Structure of Ge Nanocrystals Prepared by Thermal Annealing of Cosputtered GeSiO Ternary Precursor

    Directory of Open Access Journals (Sweden)

    Bo Zhang

    2014-01-01

    Full Text Available Ge nanocrystals (Ge-ncs embedded in a SiO2 superlattice structure were prepared by magnetron cosputtering and postdeposition annealing. The formation of spherical nanocrystals was confirmed by transmission electron microscopy and their growth process was studied by a combination of spectroscopic techniques. The crystallinity volume fraction of Ge component was found to increase with crystallite size, but its overall low values indicated a coexistence of crystalline and noncrystalline phases. A reduction of Ge-O species was observed in the superlattice during thermal annealing, accompanied by a transition from oxygen-deficient silicon oxide to silicon dioxide. A growth mechanism involving phase separation of Ge suboxides (GeOx was then proposed to explain these findings and supplement the existing growth models for Ge-ncs in SiO2 films. Further analysis of the bonding structure of Ge atoms suggested that Ge-ncs are likely to have a core-shell structure with an amorphous-like surface layer, which is composed of GeSiO ternary complex. The surface layer thickness was extracted to be a few angstroms and equivalent to several atomic layer thicknesses.

  12. Process for depositing epitaxial alkaline earth oxide onto a substrate and structures prepared with the process

    Science.gov (United States)

    McKee, Rodney A.; Walker, Frederick J.

    1996-01-01

    A process and structure involving a silicon substrate utilize molecular beam epitaxy (MBE) and/or electron beam evaporation methods and an ultra-high vacuum facility to grow a layup of epitaxial alkaline earth oxide films upon the substrate surface. By selecting metal constituents for the oxides and in the appropriate proportions so that the lattice parameter of each oxide grown closely approximates that of the substrate or base layer upon which oxide is grown, lattice strain at the film/film or film/substrate interface of adjacent films is appreciably reduced or relieved. Moreover, by selecting constituents for the oxides so that the lattice parameters of the materials of adjacent oxide films either increase or decrease in size from one parameter to another parameter, a graded layup of films can be grown (with reduced strain levels therebetween) so that the outer film has a lattice parameter which closely approximates that of, and thus accomodates the epitaxial growth of, a pervoskite chosen to be grown upon the outer film.

  13. Structural studies on iron-tellurite glasses prepared by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Rada, S., E-mail: Simona.Rada@phys.utcluj.r [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Dehelean, A. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Stan, M. [Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Chelcea, R. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Culea, E. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania)

    2011-01-05

    Research highlights: {yields} Iron-tellurite glasses obtained using the sol-gel synthesis. - Abstract: In this study, we report structural properties of the iron-tellurite glasses obtained using the sol-gel synthesis. The samples were characterized by X-ray diffraction, FTIR, UV-vis and EPR spectroscopy. Our results indicate dominant presence of iron ions in the trivalent state and the existence some Fe{sup 2+} ions. The analysis of the IR spectra indicates a gradual transformation of iron ions from tetrahedral into octahedral sites when the concentration of Fe(NO{sub 3}){sub 3} is increased beyond 0.64 mol%. EPR studies show that the increase of Fe(NO{sub 3}){sub 3} content in the host matrix induces the growth of the number of effective g values. This can be explained considering that the orbitals of O{sup 2-} ion with a large spin-orbit interaction constant will interact with the 3d orbital of Fe{sup 3+} ion bonded to this O{sup 2-} ion, thus leading to appearance of an orbital angular momentum which contributes to the magnetic moment of Fe{sup 3+} ion. A strong dipolar interaction, which is more predominant in a glass with higher content of Fe(NO{sub 3}){sub 3}, causing a localized magnetic field along the site of the Fe{sup 3+} ions and the increase the effective g values.

  14. Preparation and crystal structure of a nickel (II)-uranyl (VI) binuclear chelate

    Energy Technology Data Exchange (ETDEWEB)

    Graziani, R; Vidali, H [Padua Univ. (Italy). Istituto di Chimica Generale; Casellato, U; Vigato, P A [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

    1978-04-01

    The structure of the heterobinuclear complex of Ni/sup 2/ and (UO/sub 2/)/sup 2/ with the tetraanionic ligand derived from the condensation of 1,2-diaminoethane with o-acetoacetylphenol has been determined from diffractometer data and refined to R = 7.2%. The crystals are monoclinic, P2/sub 1//a, with a = 20.65(2), b = 8.58(1), c = 14.68(2) Angstroem and ..beta.. = 97.78(5)/sup 0/; Z = 4. The ligand employed has two different coordination sets of atoms, N/sub 2/O/sub 2/ and O/sub 2/O/sub 2/, two oxygen atoms being common to both donor sets. In the complex the nickel ion, which is four coordinate but not square planar, is retained in the inner N/sub 2/O/sub 2/ chamber, whilst the uranyl ion is incorporated in the outer O/sub 2/O/sub 2/ chamber. A molecule of solvent is retained to preserve the preffered seven coordination of uranium.

  15. Preparation and crystal and molecular structure of mer-trichlorotris(dimethylphenylphosphine)technetium(III)

    Energy Technology Data Exchange (ETDEWEB)

    Bandoli, G; Clemente, D A; Mazzi, U [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

    1976-01-01

    The crystal and molecular structure of the title compound has been determined from single-crystal X-ray diffractometer data by Fourier methods and refined by anisotropic block-diagonal least-squares to R 0.054 for 4 065 independent observed reflections. Crystals are monoclinic, space group P2/sub 1//n, with cell parameters a = 10.935(9), b = 39.191(11), c = 13.738(7) A, ..beta.. = 107.33(7)/sup 0/, and Z = 8. The two crystallographically independent molecules are stereochemically equivalent (there is only a small difference in the orientation of a benzene ring) and the metal atom has a somewhat distorted octahedral co-ordination, with two pairs of like ligands mutually trans. Technetium-ligand bond distances are: Tc-Cl(trans to P) 2.46(1), Tc-Cl(trans to Cl) both 2.33(1), Tc-P(trans to Cl) 2.42(1) and Tc-P(trans to P) both 2.47(1) A. The noticeable trans-influence of the phosphine ligands on Tc-Cl bonds is discussed.

  16. Preparation and crystal structure of a copper(2) uranyl(6) binuclear chelate

    Energy Technology Data Exchange (ETDEWEB)

    Graziani, R; Vidali, M [Padua Univ. (Italy). Istituto di Chimica Generale; Casellato, U; Vigato, P A [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

    1978-08-01

    The structure of the heterobinuclear complex of Cu/sup 2 +/ and (UO/sub 2/)/sup 2 +/ with the tetraanionic ligand derived from the condensation of 1,2-diamiaminoethane with o-acetoacetylphenol has been determined from diffractometer data and refined to R = 5.2%. The crystals are monoclinic, P2/sub 1//..cap alpha.., with ..cap alpha.. = 26.22(2), b = 14.79(2), c = 8.10(1) A and ..beta.. = 104.65(5)/sup 0/; Z = 4. The ligand employed has two different coordination sets of atoms, N/sub 2/O/sub 2/ and O/sub 2/O/sub 2/, two oxygen atoms being common to both donor sets. In the complex the copper atom, which is retained in the inner N/sub 2/O/sub 2/ chamber, is five coordinate being axially bonded to a solvent molecule, whilst the uranyl ion is incorporated in the outer O/sub 2/O/sub 2/ chamber. Another molecule of solvent is retained to preserve the preferred seven coordination of uranium.

  17. Structural and magnetic characterization of maghemites prepared from Al-substituted magnetites

    Directory of Open Access Journals (Sweden)

    Marcelo Augusto Batista

    2013-12-01

    Full Text Available Synthetic aluminum-substituted maghemites were characterized by total chemical analysis, powder X-ray diffraction (XRD, Mössbauer spectroscopy (ME, and vibrating sample magnetometry (VSM. The aim was to determine the structural, magnetic, and hyperfine properties of γ-Fe2-xAl xO3 as the Al concentration is varied. The XRD results of the synthetic products were indexed exclusively as maghemite. Increasing Al for Fe substitution decreased the mean crystalline dimension and shifted all diffraction peaks to higher º2θ angles. The a0 dimension of the cubic unit cell decreased with increasing Al according to the equation a o = 0.8385 - 3.63 x 10-5 Al (R²= 0.94. Most Mössbauer spectra were composed of one sextet, but at the highest substitution rate of 142.5 mmol mol-1 Al, both a doublet and sextet were obtained at 300 K. All hyperfine parameters from the sub-spectra were consistent with high-spin Fe3+ (0.2 a 0.7 mms-1 and suggested a strong superparamagnetic component associated with the doublet. The magnetic hyperfine field of the sextets decreased with the amount of Al-substitution [Bhf (T = 49.751 - 0.1202Al; R² = 0.94] while the linewidth increased linearly. The saturation magnetization also decreased with increasing isomorphous substitution.

  18. Synthesis, structural characterisation and antibacterial activity of Ag+-doped fluorapatite nanomaterials prepared by neutralization method

    Science.gov (United States)

    Stanić, Vojislav; Radosavljević-Mihajlović, Ana S.; Živković-Radovanović, Vukosava; Nastasijević, Branislav; Marinović-Cincović, Milena; Marković, Jelena P.; Budimir, Milica D.

    2015-05-01

    Silver doped fluorapatite nanopowders were synthesised by neutralization method, which consists of dissolving Ag2O in solution of HF and H3PO4 and addition to suspension of Ca(OH)2. The powder XRD, SEM and FTIR studies indicated the formation of a fluorapatite nanomaterials with average length of the particles is about 80 nm and a width of about 15 nm. The FTIR studies show that carbonate content in samples is very small and carbonte ions substitute both phosphate and hydroxyl groups in the crystal structure of samples, forming AB-type fluorapatite. Antibacterial studies have demonstrated that all Ag+-doped fluorapatite samples exhibit bactericidal effect against pathogens: Staphylococcus aureus, Micrococcus luteus and Kllebsiela pneumoniae. Antibacterial activity increased with the increase of Ag+ in the samples. The atomic force microscopy studies revealed extensive damage to the bacterial cell envelops in the presence of Ag+-doped fluorapatite particles which may lead to their death. The synthesized Ag+-doped fluorapatite nanomaterials are promising as antibacterial biomaterials in orthopedics and dentistry.

  19. Structural and mechanical properties of ZrSiN thin films prepared by reactive magnetron sputtering

    International Nuclear Information System (INIS)

    Freitas, F.G.R.; Conceicao, A.G.S.; Vitoria, E.R.; Carvalho, R.G.; Tentardini, E.K.; Hübler, R.; Soares, G.

    2014-01-01

    Zirconium silicon nitride (ZrSiN) thin films were deposited by reactive magnetron sputtering in order to verify the silicon influence on coating morphology and mechanical properties. The Si/(Zr+Si) ratio was adjusted between 0 to 14.5% just modifying the power applied on the silicon target. Only peaks associated to ZrN crystalline structure were observed in XRD analysis, since Si_3N_4 phase was amorphous. All samples have (111) preferred orientation, but there is a peak intensity reduction and a broadening increase for the sample with the highest Si/(Zr+Si) ratio (14.5%), demonstrating a considerable loss of crystallinity or grain size reduction (about 8 nm calculated by Scherrer). It was also observed that the texture coefficient for (200) increases with silicon addition. Chemical composition and thickness of the coatings were determined by RBS analysis. No significant changes in nano hardness with increasing Si content were found. The thin film morphology observed by SEM presents columnar and non columnar characteristics. The set of results suggests that Si addition is restricting the columnar growth of ZrN thin films. This conclusion is justified by the fact that Si contributes to increase the ZrN grains nucleation during the sputtering process. (author)

  20. Magnetic Properties and Structural Study of Ni-Co/Cu Multilayers Prepared by Electrodeposition Method

    Directory of Open Access Journals (Sweden)

    M. Jafari Fesharaki

    2015-07-01

    Full Text Available Ni-Co/Cu multilayers have been grown by electrodeposition method from a single electrolyte (based on Ni(SO4.6H2O, Co(SO4.7H2O, Cu(SO4 and H3BO3 using galvanostatic control on titanium sublayers. The X-ray diffraction (XRD patterns confirmed the multilayered structure with the nanometer thicknesses. Also, electron diffraction x-ray (EDX  analysis confirmed the purity of deposited samples. The morphology of the samples was estimated by scanning electron microscope (SEM. Magnetoresistance (MR measurements were carried out at room temperature for the Ni-Co/Cu multilayers by measuring the resistivity in a magnetic fields varying between ±6kOe as a function of the Ni-Co and Cu layer thicknesses; (1 dCu(nm 4 and 3 dNi-Cu(nm 5. The Maximum value of giant magnetoresistance (GMR was obtained when the Ni-Co and Cu thicknesses were 4.0nm and 4.0nm respectively. The hysteresis loop of the samples at room temperature was studied using an alternating gradient force magnetometer (AGFM. Finally, the temperature dependence of magnetization for Ni-Co/Cu multilayers; (dNi-Cu(4nm/dCu(2nm and dNi-Cu(3nm/dCu(3nm measured by Faraday balance and decreasing the magnetization with increasing the temperature discussed according to electron scattering due to spin fluctuation.

  1. Investigation on structural and optical properties of ZnO film prepared by simple wet chemical method

    Science.gov (United States)

    Sholehah, Amalia; Mulyadi, Rendi; Haryono, Didied; Muttakin, Imamul; Rusbana, Tb Bahtiar; Mardiyanto

    2018-04-01

    ZnO thin layer has a broad potential application in electronic and optoelectronic devices. In this study, vertically align ZnO layers were deposited on ITO glass using wet chemistry method. The seed layers were prepared using electrodeposition technique at 3°C. The growing process was carried out using chemical bath deposition at 90°C. To improve the structural properties, two different hydrothermal treatment variations were applied separately. From the experiment, it is shown that the hydrothermal process using N2 gas has given the best result, with average diameter, crystallite size, and band-gap energy of 68.83 nm; 56.37 nm; and 3.16 eV, respectively.

  2. Structure and Optical Properties of Titania-PDMS Hybrid Nanocomposites Prepared by In Situ Non-Aqueous Synthesis

    Directory of Open Access Journals (Sweden)

    Antoine R. M. Dalod

    2017-12-01

    Full Text Available Organic-inorganic hybrid materials are attractive due to the combination of properties from the two distinct types of materials. In this work, transparent titania-polydimethylsiloxane hybrid materials with up to 15.5 vol. % TiO2 content were prepared by an in situ non-aqueous method using titanium (IV isopropoxide and hydroxy-terminated polydimethylsiloxane as precursors. Spectroscopy (Fourier transform infrared, Raman, Ultraviolet-visible, ellipsometry and small-angle X-ray scattering analysis allowed to describe in detail the structure and the optical properties of the nanocomposites. Titanium alkoxide was successfully used as a cross-linker and titania-like nanodomains with an average size of approximately 4 nm were shown to form during the process. The resulting hybrid nanocomposites exhibit high transparency and tunable refractive index from 1.42 up to 1.56, depending on the titania content.

  3. Structural and optical properties of Ni-doped CdS thin films prepared by chemical bath deposition method

    Energy Technology Data Exchange (ETDEWEB)

    Premarani, R. [Arumugam Pillai SeethaiAmmal College, Thiruppattur-630211 (India); Saravanakumar, S., E-mail: sarophy84@gmail.com; Chandramohan, R. [SreeSevuganAnnamalai College, Devakottai-630303 (India); Mahalingam, T. [Department of Electrical and Computer Engineering, Ajou University, Suwon 443-749 (Korea, Republic of)

    2015-06-24

    The structural and optical behavior of undoped Cadmiun Sulphide (CdS) and Ni-doped CdS thinfilms prepared by Chemical Bath Deposition (CBD) technique is reported. The crystallite sizes of the thinfilms have been characterized by X-ray diffraction pattern (XRD). The particle sizes increase with the increase of Ni content in the CdS thinfilms. Scanning Electron Microscope (SEM) results indicated that CdS thinfilms is made up of aggregate of spherical-like particles. The composition was estimated by Energy Dispersive Analysis of X-ray (EDX) and reported. Spectroscopic studies revealed considerable improvement in transmission and the band gap of the films changes with addition of Ni dopant that is associated with variation in crystallite sizes in the nano regime.

  4. The influence of the preparation conditions on structure and optical properties of solid films of graphene oxide

    International Nuclear Information System (INIS)

    Seliverstova, E; Ibrayev, N; Dzhanabekova, R; Gladkova, V

    2016-01-01

    In this study, we investigated the physico-chemical properties of graphene oxide monolayers at the interface water-air. Monolayers were formed by the spreading of dispersion of graphene oxide in acetone and THF. It was found than graphene monolayers are in the “liquid” state on the surface of subphase. Monolayers were transferred onto solid substrates according to Langmuir-Blodgett (LB) method. SEM images show that the films have an island structure. The films obtained from acetone solutions are more uniform, which makes them more promising in terms of their use as conductive coatings. Absorption spectrum of graphene LB films exhibits a broad band in the ultraviolet and visible region of the spectrum. The optical density of the film obtained from acetone solution is greater than the optical density of the film prepared from THF. In the visible region of the spectrum both films have high transparency. (paper)

  5. Preparations and crystal structures of 8 coordinate uranyl(VI) complexes having macrocyclic ligands derived from pyrroledicarboxialdehydes and diamines

    International Nuclear Information System (INIS)

    Komagine, J.; Takeda, M.; Takahashi, M.

    2006-01-01

    Six 8-coordinate uranyl(VI) complexes with macrocyclic Schiff base ligands derived from 2,6-pyrroledicarboxialdehyde and diamines are prepared and the crystal structures for two of them are determined focusing on the relation between the size of the ligands and U-N bond distances. No difference in average uranyl bond distances and bond angles are observed between [UO 2 (bipytn)](a) and [UO 2 (bipydmtn)](b). U-N bonds of these complexes are, however, not equal; the U-N(pyrrole) bonds [2.45(a), 2.44(b) A] are much shorter than the U-N(imine) bonds [2.67(a), 2.67(b) A]. (author)

  6. Effect of annealing on the electrical, optical and structural properties of cadmium stannate thin films prepared by spray pyrolysis technique

    International Nuclear Information System (INIS)

    Kumaravel, R.; Krishnakumar, V.; Gokulakrishnan, V.; Ramamurthi, K.; Jeganathan, K.

    2010-01-01

    Polycrystalline thin films of cadmium stannate (Cd 2 SnO 4 ) were deposited by spray pyrolysis method on the Corning substrates at substrate temperature of 525 o C. Further, the films were annealed at 600 o C in vacuum for 30 min. These films were characterized for their structural, electrical and optical properties. The experimental results showed that the post-deposition annealing in vacuum has a significant influence on the properties of the films. The average grain size of the film was increased from 27.3 to 35.0 nm on heat treatment. The average optical transmittance in the visible region (500-850 nm) is decreased from 81.4% to 73.4% after annealing in vacuum. The minimum resistivity achieved in the present study for the vacuum annealed films is the lowest among the reported values for the Cd 2 SnO 4 thin films prepared by spray pyrolysis method.

  7. Structural and mechanical properties of nc-TiC/a-C:H nanocomposite film prepared by dual plasma technique

    International Nuclear Information System (INIS)

    Wang Yaohui; Zhang Xu; Wu Xianying; Li Qiang; Zhang Huixing; Zhang Xiaoji

    2008-01-01

    Nanocomposite nc-TiC/a-C:H film, with an unusual combination of superhardness, high elastic modulus and high elastic recovery, are prepared by using the dual plasma technique. The effects of the filter coil current on the compositional, structural and mechanical properties of the nc-TiC/a-C:H films have been investigated. X-ray photoelectron spectroscopy (XPS) and Raman analyses show that deposition rate, composition and nanostructure of the nc-TiC/a-C:H films could be changed by varying the filter coil current. Fortunately, by selecting the proper value for the filter coil current, 2.5 A, one could remarkably enhance mechanical properties of films such as the superhardness (66.4 GPa), the high elastic modulus (510 GPa) and the high elastic recovery (83.3%)

  8. Structural and electrical properties of CuAlMo thin films prepared by magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Birkett, Martin, E-mail: martin.birkett@northumbria.ac.uk; Penlington, Roger; Wan, Chaoying; Zoppi, Guillaume

    2013-07-01

    The structural and electrical properties of a low resistivity CuAlMo thin film resistor material were investigated. The thin films were grown on Al{sub 2}O{sub 3} and glass substrates by direct current (dc) magnetron sputtering. The key electrical properties of sheet resistance, temperature coefficient of resistance (TCR) and resistance stability were investigated as a function of sputtering pressure and post-deposition heat treatment time and temperature. A low sputtering pressure range of 0.13 to 0.40 Pa produced CuAlMo films with sheet resistance in the range 0.1 to 0.2 Ω/□ and resistance stability of 0.45 to 0.65% with a TCR of − 90 ppm/°C which could be shifted to zero following annealing in air at 425 °C. Films grown at higher sputtering pressures of 0.53 to 0.80 Pa had increased sheet resistance in the range 0.4 to 0.6 Ω/□ and inferior stability of 0.8 to 1.7% with a more negative TCR of − 110 to − 180 ppm/°C which could not be shifted to zero following annealing. The stability of the films grown at 0.13 and 0.40 Pa could be further improved to < 0.25% with heat treatment, due to the formation of a protective aluminium oxide layer. A minimum dwell time of 3 h at 425 °C was required to stabilise the films and set the electrical properties. - Highlights: • Thin films of copper–aluminium–molybdenum were sputtered on alumina substrates. • Film properties were investigated with variation in process conditions. • Low sputtering pressure gave improved electrical performance. • Post deposition annealing in air further improved electrical performance.

  9. Structural and electrical properties of CuAlMo thin films prepared by magnetron sputtering

    International Nuclear Information System (INIS)

    Birkett, Martin; Penlington, Roger; Wan, Chaoying; Zoppi, Guillaume

    2013-01-01

    The structural and electrical properties of a low resistivity CuAlMo thin film resistor material were investigated. The thin films were grown on Al 2 O 3 and glass substrates by direct current (dc) magnetron sputtering. The key electrical properties of sheet resistance, temperature coefficient of resistance (TCR) and resistance stability were investigated as a function of sputtering pressure and post-deposition heat treatment time and temperature. A low sputtering pressure range of 0.13 to 0.40 Pa produced CuAlMo films with sheet resistance in the range 0.1 to 0.2 Ω/□ and resistance stability of 0.45 to 0.65% with a TCR of − 90 ppm/°C which could be shifted to zero following annealing in air at 425 °C. Films grown at higher sputtering pressures of 0.53 to 0.80 Pa had increased sheet resistance in the range 0.4 to 0.6 Ω/□ and inferior stability of 0.8 to 1.7% with a more negative TCR of − 110 to − 180 ppm/°C which could not be shifted to zero following annealing. The stability of the films grown at 0.13 and 0.40 Pa could be further improved to < 0.25% with heat treatment, due to the formation of a protective aluminium oxide layer. A minimum dwell time of 3 h at 425 °C was required to stabilise the films and set the electrical properties. - Highlights: • Thin films of copper–aluminium–molybdenum were sputtered on alumina substrates. • Film properties were investigated with variation in process conditions. • Low sputtering pressure gave improved electrical performance. • Post deposition annealing in air further improved electrical performance

  10. PREPARING THE PUBLIC FOR COMMERCIALIZATION AND GUIDANCE OF STRUCTURAL MEDIA SPACE TOWARDS ITS FUSION WITH ADVERTISING SPACE

    Directory of Open Access Journals (Sweden)

    Marina Đukić

    2015-07-01

    Full Text Available Through genre structure analysis of the Television´s Zagreb First Channel schedule from the beginning of 1970´s till the end of the 1980´s accompanied by analysis of advertising in same period, the paper will examine the ways and intensity of commercialization entrance in Croatian media space dominated then by state media. Television schedule genre change and the broadcast of economic propaganda program will point out the different character of the television. It can be said that it will serve for preparing the public for commercialization entrance and guidance of structural media space towards its fusion with advertising one. The assumption is that in spite of the TV schedule change, which was in economic sense accompanied by economy reforms in order to establish market economy, the public wasn´t yet delivered to advertisers. One of the clarification lies in the role of the media, which then had revolutionary function with main purpose of not the voters’ generation but only to create patriots. The paper will reproduce a kind of public transformation genesis from latent status in state guided media system to same status of latent consumers in dual media model.

  11. Preparation and Study the Electrical, Structural and Gas Sensing Properties of ZnO Thick Film Resistor

    Directory of Open Access Journals (Sweden)

    M. K. DEORE

    2010-08-01

    Full Text Available Thick films of AR grade ZnO were prepared on glass substrate by screen-printing technique. These films were dried and fired at different temperatures between 550 oC, 600 oC and 650 oC for one hour in air atmosphere. The gas sensing performance of thick films was tested for various gases. ZnO films showed larger response (sensitivity to H2S gas (100 ppm at 250 oC for firing temperature 650 oC. The Morphological, Compositional and Structural properties of the ZnO thick films were performed by Scanning electron microscopy (SEM, Energy dispersive spectroscopy (EDX and XRD technique respectively. Chemical composition of ZnO film samples changes with firing temperature showing non-stoichiometric behaviours. XRD study indicated the formation of polycrystalline ZnO films with hexagonal wurtzite structure. The gas response (sensitivity, selectivity, response and recovery time of the sensor were measured and presented.

  12. Temperature effects during Ostwald ripening on structural and bandgap properties of TiO2 nanoparticles prepared by sonochemical synthesis

    International Nuclear Information System (INIS)

    Gonzalez-Reyes, L.; Hernandez-Perez, I.; Diaz-Barriga Arceo, L.; Dorantes-Rosales, H.; Arce-Estrada, E.; Suarez-Parra, R.; Cruz-Rivera, J.J.

    2010-01-01

    Anatase TiO 2 nanocrystalline (6 nm) with BET specific surface area of 300 m 2 /g and direct bandgap of 3.31 eV were prepared sonochemically and then it was subjected to thermal treatment from 400 to 900 deg. C for 2 h, in order to produce variable anatase-rutile ratio. Three stages were considered in the samples thermally treated: (i) anatase grains coarsening as a result of heat treatment temperature increasing the structural homogeneity and crystallinity and both phenomena produce a reduction in the specific surface area, (ii) coexistence of two phases (anatase and rutile) separated by a transition region, called an interface, and (iii) process where the rutile grains evolve into a new equilibrium shape without the presence of anatase phase, minimizing the total surface and the grain boundary energies, by mass transport diffusion. In this last stage the rutile phase has the sole function of growth and densification. The structure evolution, morphology and microstructure characteristics were obtained by X-ray diffraction (XRD) and transmission electron microscopy (TEM). All the stages of phase transformation are subject to thermal effects that stem from the redistribution of energy in the system. The UV-vis absorption spectra show that direct and indirect transitions can take place in the same sample simultaneously. This is attributed to the combined effect of samples with variable anatase-rutile ratio and particle size effect.

  13. Preparation of InSe Thin Films by Thermal Evaporation Method and Their Characterization: Structural, Optical, and Thermoelectrical Properties

    Directory of Open Access Journals (Sweden)

    Sarita Boolchandani

    2018-01-01

    Full Text Available The indium selenium (InSe bilayer thin films of various thickness ratios, InxSe(1-x (x = 0.25, 0.50, 0.75, were deposited on a glass substrate keeping overall the same thickness of 2500 Ǻ using thermal evaporation method under high vacuum atmosphere. Electrical, optical, and structural properties of these bilayer thin films have been compared before and after thermal annealing at different temperatures. The structural and morphological characterization was done using XRD and SEM, respectively. The optical bandgap of these thin films has been calculated by Tauc’s relation that varies within the range of 1.99 to 2.05 eV. A simple low-cost thermoelectrical power measurement setup is designed which can measure the Seebeck coefficient “S” in the vacuum with temperature variation. The setup temperature variation is up to 70°C. This setup contains a Peltier device TEC1-12715 which is kept between two copper plates that act as a reference metal. Also, in the present work, the thermoelectric power of indium selenide (InSe and aluminum selenide (AlSe bilayer thin films prepared and annealed in the same way is calculated. The thermoelectric power has been measured by estimating the Seebeck coefficient for InSe and AlSe bilayer thin films. It was observed that the Seebeck coefficient is negative for InSe and AlSe thin films.

  14. Novel transparent high-performance AgNWs/ZnO electrodes prepared on unconventional substrates with 3D structured surfaces

    Science.gov (United States)

    Lan, Wei; Yang, Zhiwei; Zhang, Yue; Wei, Yupeng; Wang, Pengxiang; Abas, Asim; Tang, Guomei; Zhang, Xuetao; Wang, Junya; Xie, Erqing

    2018-03-01

    With the development of optoelectronic devices with three-dimensional (3D) structured surfaces, transparent electrodes that can be deposited on non-plane substrates have become increasingly important. In this paper, novel transparent silver nanowire (AgNWs)/ZnO film electrodes were uniformly prepared on treated 3D glass and PET substrates with a combination of spin-coating and heat-welding. The AgNWs/ZnO films show a transmittance of ∼88% and a sheet resistance of ∼10 Ω/sq. They are comparable with commercial ITO films. Furthermore, only a small in-plane resistance variation of ∼1 Ω/sq was measured using four-point probe mapping in films with a 10 cm × 10 cm area. These results confirm that these novel film electrodes are very uniform. Both electrical resistance and optical transmittance of the films remain mostly intact after 1000 bending cycles and tape peeling-tests with 10 cycles. The films show high thermal stability for more than one month at 80 °C. The strategy provides a new route for the design and fabrication of optoelectronic devices with 3D structured surfaces.

  15. Substrate temperature effects on the structure and properties of ZnMnO films prepared by pulsed laser deposition

    Science.gov (United States)

    Riascos, H.; Duque, J. S.; Orozco, S.

    2017-01-01

    ZnMnO thin films were grown on silicon substrates by pulsed laser deposition (PLD). Pulsed Nd:YAG laser was operated at a wavelength of 1064 nm and 100 mJ. ZnMnO thin films were deposited at the vacuum pressure of 10-5 Torr and with substrate temperature from room temperature to 600 °C. The effects of substrate temperature on the structural and Optical properties of ZnMnO thin films have been investigated by X-ray diffraction (XRD), Raman spectroscopy and Uv-vis spectroscopy. From XRD data of the samples, it can be showed that temperature substrate does not change the orientation of ZnMnO thin films. All the films prepared have a hexagonal wurtzite structure, with a dominant (002) peak around 2θ=34.44° and grow mainly along the c-axis orientation. The substrate temperature improved the crystallinity of the deposited films. Uv-vis analysis showed that, the thin films exhibit high transmittance and low absorbance in the visible region. It was found that the energy band to 300 ° C is 3.2 eV, whereas for other temperatures the values were lower. Raman reveals the crystal quality of ZnMnO thin films.

  16. Electrochemical and structural characterization of carbon-supported Pt-Pd bimetallic electrocatalysts prepared by electroless deposition

    Energy Technology Data Exchange (ETDEWEB)

    Ohashi, Masato; Beard, Kevin D.; Ma Shuguo; Blom, Douglas A.; St-Pierre, Jean; Van Zee, John W. [Department of Chemical Engineering, University of South Carolina, Columbia, SC 29208 (United States); Monnier, John R., E-mail: monnier@cec.sc.ed [Department of Chemical Engineering, University of South Carolina, Columbia, SC 29208 (United States)

    2010-10-01

    Electrochemical and structural characteristics of various Pt-Pd/C bimetallic catalysts prepared by electroless deposition (ED) methods have been investigated. Structural analysis was conducted by X-ray diffraction spectroscopy, X-ray photoelectron spectroscopy, scanning transmission electron microscopy, and energy dispersive X-ray spectroscopy (EDS). Monometallic Pt or Pd particles were not detected by EDS, indicating the ED methodology formed only bimetallic particles. The size of the Pt-Pd bimetallic particles was smaller than those of a commercially available Pt/C catalyst. The morphology of the Pt on Pd/C catalysts was identified and corresponded to Pd particles partially encapsulated by Pt. The electrochemical characteristics of the lowest Pd loading catalyst (7.0% Pt on 0.5% Pd/C) for the oxygen reduction reaction (ORR) have been investigated by the rotating ring disk electrode technique. The electrochemical activity was equal or lower than the commercially available Pt/C catalyst; however, the amount of hydrogen peroxide observed at the ring was reduced by the Pd, suggesting that such a catalyst has the potential to decrease ionomer degradation in applications. The Pt on Pd/C catalysts also show a higher tolerance to ripening induced by potential cycling. Therefore, catalyst suitability cannot be judged solely by its initial performance; information related to specific degradation mechanisms is also needed for a more complete assessment.

  17. Slowing the Starch Digestion by Structural Modification through Preparing Zein/Pectin Particle Stabilized Water-in-Water Emulsion.

    Science.gov (United States)

    Chen, Jia-Feng; Guo, Jian; Zhang, Tao; Wan, Zhi-Li; Yang, Juan; Yang, Xiao-Quan

    2018-04-25

    Slowing the digestion of starch is one of the dominant concerns in the food industry. A colloidal structural modification strategy for solving this problem was proposed in this work. Due to thermodynamic incompatibility between two biopolymers, water/water emulsion of waxy corn starch (WCS) droplets dispersed in a continuous aqueous guar gum (GG) was prepared, and zein particles (ZPs), obtained by antisolvent precipitation and pectin modification, were used as stabilizer. As the ratio of zein to pectin in the particles was 1:1, their wetting properties in the two polysaccharides were similar, which made them accumulate at the interface and cover the WCS-rich droplets. The analysis of digestibility curves indicated that a rapid (rate constant k 1 : 0.145 min -1 ) and a slow phase ( k 2 : 0.022 min -1 ) existed during WCS digestion. However, only one slow phase ( k 2 : 0.019 min -1 ) was found in the WCS/GG emulsion, suggesting that this structure was effective in slowing starch digestion.

  18. Structural, Optical, Morphological and Microbial Studies on SnO₂ Nanoparticles Prepared by Co-Precipitation Method.

    Science.gov (United States)

    Arularasu, M V; Anbarasu, M; Poovaragan, S; Sundaram, R; Kanimozhi, K; Magdalane, C Maria; Kaviyarasu, K; Thema, F T; Letsholathebe, D; Mola, Genene T; Maaza, M

    2018-05-01

    Nanoparticles of tin oxide (SnO2) powders were prepared by co-precipitation method at 500 °C, 700 °C and 900 °C temperature. The sintered SnO2 nanoparticles, structural, optical, magnetic, morphological properties and microbial activity have been studied. XRD studies reveals that sintered powder which exhibits tetragonal crystal structure and both crystallinity as well as crystal size increase with increase in temperature. The morphological studies reveal randomly arranged grains with compact nature grain size increases with sintering temperature. The compositional analyses of SnO2 nanoparticles have been studied using X-ray photoelectron spectroscopy analysis. The optical band gap values of SnO2 nanoparticles were calculated to be about 4.3 eV in the temperature 500 °C, comparing with that of the bulk SnO2 3.78 eV, by optical absorption measurement. Room temperature M-H curve for pure SnO2 nanoparticles exhibits ferromagnetic behaviour. The tin oxide nanoparticles are acted as potential candidate material for bacterial and fungal activity.

  19. Influence of silane on the structure of polystyrene prepared by sol-gel coatings via UV curing

    Directory of Open Access Journals (Sweden)

    Balbay Senay

    2017-01-01

    Full Text Available Light, heat, oxygen, moisture, ozone, atmospheric pollution and biological effects are the most important effectives wreak to chemical degradation in the polymer structure. In result of chemical degradation on the polymer consist of problems such as discoloration, brittleness, surface cracks, perspiration, crumbling, smell, surface acidity. In this work, it is aimed to improve the problem of the polystyrene (PS material against chemical degradation. For this reason, PS is coated with silica sol-gel hybrid coating. Silica sol-gel was synthesized by using vinyltrimethoxysilane (VTMS as a cross-linker and tetraethylorthosilicate (TEOS as a silica source. Firstly, four different pre-treatment technique (oven, vacuum oven, lyophilizer and freezing was studied to determine the most suitable pre-treatment technique for coating on PS substrate of sol-gel prepared with initial formulation (S1. A freezing technique gave the best results for coating sample. The change of surface colour of coated PS was measured by CIE L*a*b* methods. Secondly, the most suitable curing agent (Irgacure 184, Irgacure 819, Darocur 1173 and TiO2 as crystalline anatase phase was determined to coat the sol-gel on PS. It was determined to the lowest yellowing of PS surface hybrid coated as UV curing of TEOS sol modified by VTMS and TiO2 as photo-initiators. Finally, the chemical and morphological structure of the coated PS samples was determined by FT-IR and SEM instruments, respectively.

  20. Optical and structural properties of carbon dots/TiO2 nanostructures prepared via DC arc discharge in liquid

    Science.gov (United States)

    Biazar, Nooshin; Poursalehi, Reza; Delavari, Hamid

    2018-01-01

    Synthesis and development of visible active catalysts is an important issue in photocatalytic applications of nanomaterials. TiO2 nanostructures coupled with carbon dots demonstrate a considerable photocatalytic activity in visible wavelengths. Extending optical absorption of a wide band gap semiconductor such as TiO2 with carbon dots is the origin of the visible activity of carbon dots modified semiconductor nanostructures. In addition, carbon dots exhibit high photostability, appropriate electron transport and chemical stability without considerable toxicity or environmental footprints. In this study, optical and structural properties of carbon dots/TiO2 nanostructures prepared via (direct current) DC arc discharge in liquid were investigated. Crystal structure, morphology and optical properties of the samples were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV-visible spectroscopy respectively. SEM images show formation of spherical nanoparticles with an average size of 27 nm. In comparison with pristine TiO2, optical transmission spectrum of carbon dots/TiO2 nanostructures demonstrates an absorption edge at longer wavelengths as well a high optical absorption in visible wavelengths which is significant for visible activity of nanostructures as a photocatalyst. Finally, these results can provide a flexible and versatile pathway for synthesis of carbon dots/oxide semiconductor nanostructures with an appropriate activity under visible light.

  1. Effect of thermal annealing on structural properties of SrGa2S4:Ce thin films prepared by flash evaporation

    International Nuclear Information System (INIS)

    Gambarov, E.F.; Bayramov, A.I.

    2009-01-01

    In the present report the preparation technology and structural characterization of Ce 3 +activated SrGa 2 S 4 thin films are given. SrGa 2 S 4 : e thin films are prepared by so called flash evaporation which is simple and inexpensive method for thin film deposition. X-ray diffraction shows that the as deposited films exhibit amorphous behavior, but after annealing in H S stream, the polycrystalline one. EPMA results indicate nearly stoichiometric composition of the thin films

  2. Structural, optical and nonlinear optical studies of AZO thin film prepared by SILAR method for electro-optic applications

    Science.gov (United States)

    Edison, D. Joseph; Nirmala, W.; Kumar, K. Deva Arun; Valanarasu, S.; Ganesh, V.; Shkir, Mohd.; AlFaify, S.

    2017-10-01

    Aluminium doped (i.e. 3 at%) zinc oxide (AZO) thin films were prepared by simple successive ionic layer adsorption and reaction (SILAR) method with different dipping cycles. The structural and surface morphology of AZO thin films were studied by using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The optical parameters such as, transmittance, band gap, refractive index, extinction coefficient, dielectric constant and nonlinear optical properties of AZO films were investigated. XRD pattern revealed the formation of hexagonal phase ZnO and the intensity of the film was found to increase with increasing dipping cycle. The crystallite size was found to be in the range of 29-37 nm. Scanning Electron Microscope (SEM) images show the presence of small sized grains, revealing that the smoothest surface was obtained at all the films. The EDAX spectrum of AZO conforms the presence of Zn, O and Al. The optical transmittance in the visible region is high 87% and the band gap value is 3.23 eV. The optical transmittance is decreased with respect to dipping cycles. The room temperature PL studies revealed that the AZO films prepared at (30 cycles) has good film quality with lesser defect density. The third order nonlinear optical parameters were also studied using Z-scan technique to know the applications of deposited films in nonlinear devices. The third order nonlinear susceptibility value is found to be 1.69 × 10-7, 3.34 × 10-8, 1.33 × 10-7and 2.52 × 10-7 for AZO films deposited after 15, 20, 25 and 30 dipping cycles.

  3. Structure, properties and wear behaviour of multilayer coatings consisting of metallic and covalent hard materials, prepared by magnetron sputtering

    International Nuclear Information System (INIS)

    Schier, V.

    1995-12-01

    Novel multilayer coatings with metallic and covalent layer materials were prepared by magnetron sputtering and characterised concerning structure, properties and application behaviour. At first single layer coatings were deposited for the determination of the material properties. To evaluate relations between structure and properties of the multilayer coatings, different multilayer concepts were realised: - coatings consisting of at most 7 layers of metallic hard materials, - 100-layer coatings consisting of metallic and covalent hard materials, - TiN-TiC multilayer coatings with different numbers of layers (between 10 and 1000), - 150-layer coatings, based on TiN-TiC multilayers, with thin ( 4 C, AlN, SiC, a:C, Si 3 N 4 , SiAlON). X-rays and electron microscopic analysis indicate in spite of nonstoichiometric compositions single phase crystalline structures for nonreactively and reactively sputtered metastable single layer Ti(B,C)-, Ti(B,N)- and Ti(B,C,N)-coatings. These single layer coatings show excellent mechanical properties (e.g. hardness values up to 6000 HV0,05), caused by lattice stresses as well as by atomic bonding conditions similar to those in c:BN and B 4 C. The good tribological properties shown in pin-on-disk-tests can be attributed to the very high hardness of the coatings. The coatings consisting of at most 7 layers of metallic hard materials show good results mainly for the cutting of steel Ck45, due to the improved mechanical properties (e.g. hardness, toughness) of the multilayers compared to the single layer coatings. This improvement is caused by inserting the hard layer materials and the coherent reinforcement of the coatings. (orig.)

  4. Effect of the preparation method on the structural and catalytic properties of spinel cobalt-iron oxide

    Energy Technology Data Exchange (ETDEWEB)

    Hammiche-Bellal, Yasmina, E-mail: yasminahammiche@gmail.com [Laboratoire des Matériaux Catalytiques et Catalyse en Chimie Organique, Faculté de Chimie, USTHB, BP32 El Alia, Bab Ezzouar, 16111, Alger (Algeria); Djadoun, Amar [Laboratoire de Géophysique, FSTGAT, USTHB, BP32 El Alia, Bab Ezzouar, 16111, Alger (Algeria); Meddour-Boukhobza, Laaldja; Benadda, Amel [Laboratoire des Matériaux Catalytiques et Catalyse en Chimie Organique, Faculté de Chimie, USTHB, BP32 El Alia, Bab Ezzouar, 16111, Alger (Algeria); Auroux, Aline [Université Lyon 1, CNRS, UMR 5256, IRCELYON, Institut de Recherches sur la Catalyse et l' Environnement de Lyon, 2 Avenue Albert Einstein, F-69626, Villeurbanne (France); Berger, Marie-Hélène [Centre des Matériaux PIERRE-MARIE Fourt, UMR 7633, Paris (France); Mernache, Fateh [UDEC-CRND, COMENA, BP 43 Draria, 16050, Alger (Algeria)

    2016-07-01

    Spinel cobalt-iron oxide was synthesized by co-precipitation and hydrothermal routes. The effect of the co-precipitation experimental conditions, the calcination temperature and the hydrothermal synthesis time and temperature on the properties of the solids was studied. The prepared powders were evaluated as catalysts in the ethanol combustion reaction, and were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM/EDX), nitrogen adsorption–desorption isotherms (BET, BJH) and temperature programmed reduction (TPR) techniques. Using chloride salts as starting materials and sodium hydroxide as precipitating agent, the CoFe{sub 2}O{sub 4} prepared powders displayed a mesoporous structure with a pore distribution strongly dependent on the experimental conditions. A monophasic spinel phase in the case of the calcined solids was obtained while the hydrothermal process led to the formation of a mixture of single oxides in addition to the spinel phase. The variation of the crystallite size and the lattice parameter as a function of calcination temperature was similar, whereas this variation found to be irregular when the synthesis residence time in autoclave was increased. The hydrothermally treated solids show the best catalytic performance in the total oxidation of ethanol. The catalytic behavior was correlated with the crystallite size and the reduction temperature of cobalt species determined by the TPR analysis. - Highlights: • Pure CoFe{sub 2}O{sub 4} phase is obtained by co-precipitation method at calcination temperatures 500–900 °C. • The temperature of co-precipitation procedure influences strongly the growth of the solids during the calcination step. • The hydrothermal synthesis gives a mixture of oxides; CoFe{sub 2}O{sub 4} is the predominant phase. • The CoFe{sub 2}O{sub 4} spinel showed a good catalytic reactivity in the ethanol combustion reaction. • The catalysts prepared by hydrothermal process are more reactive and

  5. Preparation of composite micro/nano structure on the silicon surface by reactive ion etching: Enhanced anti-reflective and hydrophobic properties

    Science.gov (United States)

    Zeng, Yu; Fan, Xiaoli; Chen, Jiajia; He, Siyu; Yi, Zao; Ye, Xin; Yi, Yougen

    2018-05-01

    A silicon substrate with micro-pyramid structure (black silicon) is prepared by wet chemical etching and then subjected to reactive ion etching (RIE) in the mixed gas condition of SF6, CHF3 and He. We systematically study the impacts of flow rates of SF6, CHF3 and He, the etching pressure and the etching time on the surface morphology and reflectivity through various characterizations. Meanwhile, we explore and obtain the optimal combination of parameters for the preparation of composite structure that match the RIE process based on the basis of micro-pyramid silicon substrate. The composite sample prepared under the optimum parameters exhibits excellent anti-reflective performance, hydrophobic, self-cleaning and anti-corrosive properties. Based on the above characteristics, the composite micro/nano structure can be applied to solar cells, photodetectors, LEDs, outdoor devices and other important fields.

  6. Structural and optical characterization of nanoparticulate manganese doped zinc silicate phosphors prepared by sol–gel and combustion methods

    Energy Technology Data Exchange (ETDEWEB)

    Mbule, P.S., E-mail: mbuleps@gmail.com [Department of Physics, CSET, University of South Africa, Johannesburg, 1710 (South Africa); Ntwaeaborwa, O.M. [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein 9300 (South Africa); Mothudi, B.M.; Dhlamini, M.S. [Department of Physics, CSET, University of South Africa, Johannesburg, 1710 (South Africa)

    2016-11-15

    The present study reports the synthesis, crystallographic structure and optical properties of manganese (Mn{sup 2+}) doped zinc silicate (Zn{sub 2}SiO{sub 4}) nanoparticle phosphors prepared by sol–gel and combustion methods. For samples prepared by sol–gel method, the X-ray diffraction results showed phase transformation from amorphous to α-phase Zn{sub 2}SiO{sub 4} due to annealing temperatures at 600 °C to 1100 °C, whereas for combustion samples an admixture of highly crystalline β-phase and hexagonal wurtzite structure of ZnO was observed at annealing temperature of 600 °C. Photoluminescence spectra with Mn{sup 2+} concentrations ranging from 0.015–0.09 mol% were compared for two methods. Emission band assigned to the {sup 4}T{sub 1}({sup 4}G)→{sup 6}A{sub 1}({sup 6}S) electronic transition of Mn{sup 2+} was observed with maximum intensity at ~573 nm for combustion samples and ~532 nm for sol–gel samples upon UV-excitation by a Xenon lamp. Furthermore, the photoluminescence decay curves of annealed Zn{sub 2}SiO{sub 4}:Mn{sup 2+} samples were observed to be bi-exponential. The fast and slow decay components are due to the pair or cluster formation and isolated ions at higher doping concentration, respectively. - Highlights: • Synthesis, crystallographic and optical properties of Zn{sub 2}SiO{sub 4}:Mn{sup 2+} are presented. • XRD shows amorphous diffraction peak and crystallinity improved by increase of annealing temperature. • Crystallite and particle size from XRD and SAXS techniques, respectively, are compared. • Photoluminescence (PL) spectra are compared for sol-gel and combustion method. • The photoluminescence decay curves of annealed Zn{sub 2}SiO{sub 4}:Mn{sup 2+} samples were observed to be bi-exponential.

  7. Structural, optical and magnetic properties of Mn diffusion-doped CdS thin films prepared by vacuum evaporation

    Energy Technology Data Exchange (ETDEWEB)

    Aksu, S. [SoloPower, Inc., 5981 Optical Ct., San Jose, CA 95138 (United States); Bacaksiz, E., E-mail: eminb@ktu.edu.tr [Department of Physics, Karadeniz Technical University, 61080 Trabzon (Turkey); Parlak, M. [Department of Physics, Middle East Technical University, 06531 Ankara (Turkey); Yilmaz, S.; Polat, I.; Altunbas, M. [Department of Physics, Karadeniz Technical University, 61080 Trabzon (Turkey); Tuerksoy, M.; Topkaya, R. [Department of Physics, Gebze Institute of Technology, Gebze, 41400 Kocaeli (Turkey); Ozdogan, K. [Department of Physics, Yildiz Technical University, 34210 Istanbul (Turkey)

    2011-10-17

    Highlights: {yields} Cadmium sulphide thin films were deposited by vacuum evaporation. {yields} Elemental Mn was deposited onto CdS thin films by using electron beam evaporation and annealed under vacuum at different temperatures. {yields} Structural, optical and magnetic studies of Mn-doped CdS have been investigated. {yields} X-ray diffraction results showed that the undoped CdS film had a zinc-blende structure with a strong preferred orientation along the (1 1 1) direction. {yields} Magnetic measurements show that Mn-doped CdS thin films exhibit a ferromagnetism behavior at room temperature. - Abstract: The effect of Mn-doping on the vacuum deposited CdS thin films has been investigated by studying the changes in the structural, optical and magnetic properties of the films. A thin Mn layer evaporated on the CdS film surface served as the source layer for the diffusion doping. Doping was accomplished by annealing the CdS/Mn stack layers at the temperature range from 300 deg. C to 400 deg. C in step of 50 deg. C for 30 min under vacuum. The X-ray diffraction results showed that the undoped CdS film had a zinc-blende structure with a strong preferred orientation along the (1 1 1) direction. The incorporation of Mn did not cause any change in the texture but reduced the peak intensity and lead to a smaller crystallite size. Investigation of surface morphology using atomic force microscopy confirmed the decrease in the grain size with the Mn diffusion. In addition, a more uniform grain size distribution was observed in the doped films. X-ray photoelectron spectroscopy analysis showed that Mn atoms on the surface of the films were bounded to either sulphur or oxygen atoms. Auger electron spectroscopy of the diffusion-doped CdS sample at 350 deg. C indicated that the atomic Mn concentration was higher close to the surface region and Mn was distributed with a steadily decreasing profile through the bulk of the film with an average atomic concentration value around few

  8. Crystal Structure And Optical Properties Of TiO2 Thin Films Prepared By Reactive RF Magnetron Sputtering

    Directory of Open Access Journals (Sweden)

    Goto S.

    2015-06-01

    Full Text Available In sputtering deposition process of TiO2, metal Ti or sintered TiO2 target is used as deposition source. In this study, we have compared the characteristic of target materials. When TiO2 target was used, stoichiometric TiO2 films was deposited under the Ar atmosphere containing 1.0% of oxygen. The highest sputtering rate under this atmosphere was 3.9nm/min at 3.4W/cm2. But, sintered TiO2 target is fragile and cannot endure higher density of input power than 3.4W/cm2. On the other hand, Ti target needs higher oxygen concentration (8% in sputtering gas atmosphere for obtaining rutile/anatase. Even though Ti target can be input twice power density of 7.9W/cm2, the highest deposition rate for Ti target was 1.4/nm, which was ~35% of the highest rate for TiO2 target. Then we have study out the composite target consisting of Ti plate and TiO2 chips. Using the composite target, stoichiometric TiO2 films were prepared in the rate of 9.6nm/min at 6.8 W/cm2 under the atmosphere of Ar/2.5%O2. Furthermore, we have found that the TiO2 films obtained from the composite target consisted of about 100% anatase, whereas TiO2 films obtained from other target have rutile dominant structure. The optical band gap energy of the film is determined by using the Tauc plot. The calculated band gap energies for the films deposited by Ti target and composite target were 2.95 and 3.24eV, which are equivalent to that of rutile and anatase structure, respectively.

  9. Pore Structure and Fluoride Ion Adsorption Characteristics of Zr (IV) Surface-Immobilized Resin Prepared Using Polystyrene as a Porogen

    Science.gov (United States)

    Mizuki, Hidenobu; Ito, Yudai; Harada, Hisashi; Uezu, Kazuya

    Zr(IV) surface-immobilized resins for removal of fluoride ion were prepared by surface template polymerization using polystyrene as a porogen. At polymerization, polystyrene was added in order to increase mesopores (2-50 nm) and macropore (>50 nm) with large macropores (around 300 nm) formed with internal aqueous phase of W⁄O emulsion. The pore structure of Zr(IV) surface-immobilized resins was evaluated by measuring specific surface area, pore volume, and pore size distribution with volumetric adsorption measurement instrument and mercury porosimeter. The adsorption isotherms were well fitted by Langmuir equation. The removal of fluoride was also carried out with column method. Zr(IV) surface-immobilized resins, using 10 g⁄L polystyrene in toluene at polymerization, possessed higher volume of not only mesopores and macropores but also large macropores. Furethermore, by adding the polystyrene with smaller molecular size, the pore volume of mesopores, macropores and large macropores was significantly increased, and the fluoride ion adsorption capacity and the column utilization also increased.

  10. Preparation, structural and luminescent properties of nanocrystalline ZnO films doped Ag by close space sublimation method

    Science.gov (United States)

    Khomchenko, Viktoriya; Mazin, Mikhail; Sopinskyy, Mykola; Lytvyn, Oksana; Dan'ko, Viktor; Piryatinskii, Yurii; Demydiuk, Pavlo

    2018-05-01

    The simple way for silver doping of ZnO films is presented. The ZnO films were prepared by reactive rf-magnetron sputtering on silicon and sapphire substrates. Ag doping is carried out by sublimation of the Ag source located at close space at atmospheric pressure in air. Then the ZnO and ZnO-Ag films were annealed in wet media. The microstructure and optical properties of the films were compared and studied by atomic force microscopy (AFM), X-ray diffraction (XRD), photoluminescence (PL) and cathodoluminescence (CL). XRD results indicated that all the ZnO films have a polycrystalline hexagonal structure and a preferred orientation with the c-axis perpendicular to the substrate. The annealing and Ag doping promote increasing grain's sizes and modification of grain size distribution. The effect of substrate temperature, substrate type, Ag doping and post-growth annealing of the films was studied by PL spectroscopy. The effect of Ag doping was obvious and identical for all the films, namely the wide visible bands of PL spectra are suppressed by Ag doping. The intensity of ultraviolet band increased 15 times as compared to their reference films on sapphire substrate. The ultraviolet/visible emission ratio was 20. The full width at half maximum (FWHM) for a 380 nm band was 14 nm, which is comparable with that of epitaxial ZnO. The data implies the high quality of ZnO-Ag films. Possible mechanisms to enhance UV emission are discussed.

  11. Structural Characterizations of Palladium Clusters Prepared by Polyol Reduction of [PdCl4]2− Ions

    Directory of Open Access Journals (Sweden)

    Loredana Schiavo

    2016-01-01

    Full Text Available Palladium nanoparticles are of great interest in many industrial fields, ranging from catalysis and hydrogen technology to microelectronics, thanks to their unique physical and chemical properties. In this work, palladium clusters have been prepared by reduction of [PdCl4]2− ions with ethylene glycol, in the presence of poly(N-vinyl-2-pyrrolidone (PVP as stabilizer. The stabilizer performs the important role of nucleating agent for the Pd atoms with a fast phase separation, since palladium atoms coordinated to the polymer side-groups are forced at short distances during nucleation. Quasispherical palladium clusters with a diameter of ca. 2.6 nm were obtained by reaction in air at 90°C for 2 hours. An extensive materials characterization by transmission electron microscopy (TEM, X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS, and other characterizations (TGA, SEM, EDS-SEM, and UV-Vis has been performed in order to evaluate the structure and oxidation state of nanopalladium.

  12. Structural, optical and electrical properties of CuInS{sub 2} thin films prepared by chemical spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Terasako, Tomoaki; Uno, Yuji; Inoue, Seiki; Shirakata, Sho [Faculty of Engineering, Ehime University, 3 Bunkyo-cho, Matsuyama 780-8577 (Japan); Kariya, Tetsuya [Faculty of Science, Kochi University, Akebono-cho, Kochi, 780-8072 (Japan)

    2006-09-15

    Polycrystalline CuInS{sub 2} thin films were prepared by chemical spray pyrolisis (CSP) on glass substrate from the ethanol aqueous solution containing CuCl{sub 2}, InCl{sub 3} and thiourea. Structural, electrical and optical properties were systematically studied in terms of substrate temperature, pH and the ion ratio (Cu/In) of the spray solution. Although the In-rich films were composed of CuInS{sub 2} and In{sub 2}S{sub 3}, the In{sub 2}S{sub 3} content in the film decreased with Cu/In ratio. Appearance of Raman peaks at 288 and 298 cm{sup -1} indicated that the films contained CuInS{sub 2} with chalcopyrite and CuAu phases. Typical grain size in the Cu-rich films was 200 nm. Optical gap energies were approximately 0.1-0.2eV smaller than the bandgap energy of the CuInS{sub 2} bulk crystal. Resistivity of the Cu-rich films without In{sub 2}S{sub 3} secondary phase was 0.2-5 {omega}cm. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  13. PREPARATION,COMPLEX MECHANISM AND STRUCTURE MODEL OF METALLOPHTHALOC- YANINE-Fe3O4 NANOPARTICLES COMPOSITE

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    MPc-Fe3O4-nanoparticles composite(M=Co, Cu, Ni, Mn) have been prepared and the factors that influence their mean size have been studied. The mean size of the nanoparticles composite increase with the increase of complex temperature. The interaction of MPc with Fe3O4 nanoparticles has been studied. There are M-O covalent bonding and ionic bonding between MPc and Fe3O4 nanoparticles. The intensities of M-O bonding and ionic bonding are in vestigated .The complex mechanism of MPc with Fe3O4 nanoparticles have been studied. First, there are complex between MPc and all Fe3O4 nanoparticles. Then, Fe3O4 nanoparticles accumulate together to form the accumulators, MPc have the function of cohering Fe3O4 nanoparticles. A considerable number of MPc combine with Fe3O4 nanoparticles on the surface of the accumulators to form MPc-Fe3O4 nanoparticles composite. All the above proesses take place spontaneously. The structure model of MPc-Fe3O4 nanoparticles composite has also been investigated. Inside the MPc-Fe3O4 nanoparticles composite, Fe3O4 nanoparticles accumulate together without order, on the surface of the composite, MPc form molecular dispersion layer. The threshold of molecular dispersion layer are also investigated.

  14. Magnetic and structural properties of the Nd2(Fe100-xNbx)14B system prepared by arc melting

    International Nuclear Information System (INIS)

    Oyola Lozano, D.; Zamora, L. E.; Perez Alcazar, G. A.; Rojas, Y. A.; Bustos, H.; Greneche, J. M.

    2006-01-01

    In this work the magnetic and structural properties are investigated by Moessbauer spectrometry, Vibrating Sample Magnetometry and X-ray diffraction of Nd 2 (Fe 100-x Nb x ) 14 B powdered alloys with x = 0, 2 and 4 prepared by arc melting. The Moessbauer spectra of the samples were fitted with several contributions from: Nd 2 Fe 14 B, α-Fe and a paramagnetic phase associated with Nd 1.1 Fe 4 B 4 for x = 0 and additionally from NbFeB and Nd 2 Fe 17 for x = 2 and x = 4. The relative fractions of α-Fe and Nd 2 Fe 14 B are smaller for x = 4 than for x = 0, indicating that the amount of these two phases is reduced with increasing Nb content, while the relative fraction of Nd 2 Fe 17 increases. The α-Fe grain size slightly decreases while that of the Nd 2 Fe 14 B phase is increasing, when the Nb content increases. The hysteresis loops indicate that these samples behave as hard ferromagnets, with a coercive field which decreases when the Nb content increases, but with rather low remanent magnetization.

  15. Preparation and structural characterization of FeCo epitaxial thin films on insulating single-crystal substrates

    International Nuclear Information System (INIS)

    Nishiyama, Tsutomu; Ohtake, Mitsuru; Futamoto, Masaaki; Kirino, Fumiyoshi

    2010-01-01

    FeCo epitaxial films were prepared on MgO(111), SrTiO 3 (111), and Al 2 O 3 (0001) single-crystal substrates by ultrahigh vacuum molecular beam epitaxy. The effects of insulating substrate material on the film growth process and the structures were investigated. FeCo(110) bcc films grow on MgO substrates with two type domains, Nishiyama-Wassermann (NW) and Kurdjumov-Sachs (KS) relationships. On the contrary, FeCo films grown on SrTiO 3 and Al 2 O 3 substrates include FeCo(111) bcc crystal in addition to the FeCo(110) bcc crystals with NW and KS relationships. The FeCo(111) bcc crystal consists of two type domains whose orientations are rotated around the film normal by 180 deg. each other. The out-of-plane and the in-plane lattice spacings of FeCo(110) bcc and FeCo(111) bcc crystals formed on the insulating substrates are in agreement with those of the bulk Fe 50 Co 50 (at. %) crystal with small errors ranging between +0.2% and +0.4%, showing that the strains in the epitaxial films are very small.

  16. Structural Characterization and Magnetic Properties of Undoped and Ti-Doped ZnO Nanoparticles Prepared by Modified Oxalate Route

    Directory of Open Access Journals (Sweden)

    Ekane Peter Etape

    2018-01-01

    Full Text Available Ti-doped zinc oxide and pure zinc oxide nanoparticles were synthesized by a modified oxalate route using Averrhoa carambola fruit juice as a natural source of oxalate. The characteristics of the precursors have been investigated by FTIR, TGA, and XRD. The results from the investigation revealed that the precursors are zinc oxalate and Ti-doped zinc oxalate which readily decompose at 450°C. The as-prepared precursors were calcined at 450°C for 4 hours, and the decomposition products have been characterized by XRD, SEM, EDX, and VSM. XRD results revealed crystallinity with hexagonal wurtzite structure, while the average grain size was found to be 26 nm for Ti-doped ZnO and 29 nm for ZnO, using calculations based on Debye-Scherrer equation. Furthermore, the morphological studies by SEM showed particle agglomeration, while the presence of Ti3+ in the zinc oxide lattice is indicated by EDS analysis. Finally the hysteresis loop from VSM results shows that Ti-doped ZnO exhibits ferromagnetism.

  17. Structural, optical and thermal properties of {beta}-SnS{sub 2} thin films prepared by the spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Khelia, C.; Ben Nasrallah, T.; Amlouk, M.; Belgacem, S. [Faculte des Sciences, Tunis (Tunisia). Lab. de Physique de la Matiere Condensee; Maiz, F. [Equipe de Photothermique de Nabeul, Inst. Preparatoire aux Etudes d' Ingenieur de Nabeul (Tunisia); Mnari, M. [Lab. de Chimie Analytique, Campus Univ., Tunis (Tunisia)

    2000-03-01

    Tin disulfide {beta}-SnS{sub 2} thin films have been prepared on pyrex substrates by the spray pyrolysis technique using tin tetrachloride and thiourea as starting materials. The depositions were carried out in the range of substrate temperatures from 240 to 400 C. Highly c-axis oriented {beta}-SnS{sub 2} films, having a strong (001) X-ray diffraction line are obtained at temperature 280 C and using concentration ratio in solution R = [S]/[Sn] = 2.5. Films surfaces were analyzed by contact atomic force microscopy (AFM) and by scanning electron microscopy (SEM) in order to understand the effect of the deposited temperature on the surface structure. On the other hand, from transmission and reflection spectra, the band gap energy determined is about 2.71 eV. Finally using the photodeflection spectroscopy technique, the thermal conductivity K{sub c} and diffusivity D{sub c} were obtained. Their values are 10 Wm{sup -1}K{sup -1} and 10{sup -5} m{sup 2}s{sup -1} respectively. (orig.)

  18. Assessment of residual coronal tooth structure postendodontic cavity preparation using digital dental impressions and micro-computed tomography.

    Science.gov (United States)

    Al-Nuaimi, Nassr; Patel, Shanon; Foschi, Federico; Mannocci, Francesco; Austin, Rupert S

    To evaluate the in vitro accuracy of digital impressions for three-dimensional (3D) volumetric measurement of residual coronal tooth structure postendodontic cavity preparation, with reference to micro-computed tomography (μCT). Quantification of the accuracy and precision of the intraoral digital scanner (3M True Definition Scanner - IOS) was performed using a metrology gauge block and a profilometric calibration model. Thirty-four human extracted molars with endodontic access cavities were scanned using both intraoral scanning (test scanner) in high-resolution mode, and µCT (reference scanner: GE Locus SP μCT scanner) in high- (HiResCT) and low- (LoResCT) resolution modes. Comparisons of volumetric accuracy and 3D profilometric deviations were performed using surface metrology software. One-way repeated measures analysis of variance (ANOVA), in combination with the Bonferroni post hoc test, was implemented to compare the differences in volume measurements between scanning methods. Digital scanning revealed smaller volume measurements by 1.36% and 0.68% compared to HiResCT and LoResCT, respectively. There was a statistically significant difference in the volumetric measurements obtained from the IOS scanner and both HiResCT and LoResCT scans (P digital scanner was able to reliably measure the extra- and intracoronal aspect of the endodontically accessed tooth.

  19. Influence of preparation conditions on porous structures of olive stone activated by H{sub 3}PO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Yavuz, Reha; Akyildiz, Hanife [Istanbul Technical University, Chemical and Metallurgical Engineering Faculty, 34469 Maslak, Istanbul (Turkey); Karatepe, Nilguen; Cetinkaya, Eda [Istanbul Technical University, Institute of Energy, Renewable Energy Division, 34469 Maslak, Istanbul (Turkey)

    2010-01-15

    An olive factory residue was used as a precursor in the preparation of granular activated carbon by chemical activation with H{sub 3}PO{sub 4}. Effects of final activation temperature, time, and H{sub 3}PO{sub 4} concentration used in the impregnation stage on the porous development were investigated. SO{sub 2} adsorption experiments were also performed for some of the activated carbon samples to represent their adsorption performance. Activation at low temperature represented that micropores were developed first at early stages of the temperatures. Mesoporosity developed at around 250 C, enhanced up to 400 C, and then started to decrease due to possibly shrinking of pores. The optimum temperature for olive stone was found to be around 400 C on the basis of total pore volume and BET surface area. It was clearly demonstrated that H{sub 3}PO{sub 4} concentration used in the impregnation stage was not only effective for development of surface area and pore volumes but also an effective tool for tailoring the pore structure and size distribution. (author)

  20. Cold compaction behavior of nano-structured Nd–Fe–B alloy powders prepared by different processes

    International Nuclear Information System (INIS)

    Liu, Xiaoya; Hu, Lianxi; Wang, Erde

    2013-01-01

    Graphical abstract: Relative density enhancement and nanocrystallization of Nd 2 Fe 14 B phase are two major effective means to improve magnetic properties. Since the matrix Nd 2 Fe 14 B phase in the starting Nd–Fe–B alloy can be disproportionated into a nano-structured mixture of NdH 2.7 , Fe 2 B, and α-Fe phases during mechanical milling in hydrogen. It is thus important to study the densification behavior of nanocrystalline powders to evaluate and predict the cold compactibility of powders. By comparison with the as milled as well as melt-spun Nd 16 Fe 76 B 8 alloy powders, we find that the as-disproportionated Nd 16 Fe 76 B 8 alloy powder exhibits the best cold compactibility. As evident from the illustration presented below, compaction parameters (representing the powder compactibility) have been determined by fitting density–pressure data with double logarithm compaction equation. Densification mechanisms involved during cold compaction process are clarified in our work by referring to microstructure observation of samples prepared by various methods. As a result, highly densified green magnet compact can be obtained by cold pressing of as-disproportionated NdFeB alloy powders. Highlights: ► Nano-structured disproportionated Nd–Fe–B alloy powders by mechanical milling in hydrogen. ► Highly densified green magnet compact by cold pressing of as-disproportionated Nd–Fe–B alloy powders. ► Density–pressure data fitted well by an empirical powder compaction model. ► As-disproportionated powder showed better compactibility than as milled and melt-spun counterparts. ► The effects of physical properties on powder compactibility and densification mechanisms are clarified. - Abstract: The compaction behavior of nano-structured Nd 16 Fe 76 B 8 (atomic ratio) alloy powders, which were prepared by three different processing routes including melt spinning, mechanical milling in argon, and mechanically activated disproportionation by milling in

  1. Cold compaction behavior of nano-structured Nd-Fe-B alloy powders prepared by different processes

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiaoya [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Hu, Lianxi, E-mail: hulx@hit.edu.cn [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Wang, Erde [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2013-02-25

    Graphical abstract: Relative density enhancement and nanocrystallization of Nd{sub 2}Fe{sub 14}B phase are two major effective means to improve magnetic properties. Since the matrix Nd{sub 2}Fe{sub 14}B phase in the starting Nd-Fe-B alloy can be disproportionated into a nano-structured mixture of NdH{sub 2.7}, Fe{sub 2}B, and {alpha}-Fe phases during mechanical milling in hydrogen. It is thus important to study the densification behavior of nanocrystalline powders to evaluate and predict the cold compactibility of powders. By comparison with the as milled as well as melt-spun Nd{sub 16}Fe{sub 76}B{sub 8} alloy powders, we find that the as-disproportionated Nd{sub 16}Fe{sub 76}B{sub 8} alloy powder exhibits the best cold compactibility. As evident from the illustration presented below, compaction parameters (representing the powder compactibility) have been determined by fitting density-pressure data with double logarithm compaction equation. Densification mechanisms involved during cold compaction process are clarified in our work by referring to microstructure observation of samples prepared by various methods. As a result, highly densified green magnet compact can be obtained by cold pressing of as-disproportionated NdFeB alloy powders. Highlights: Black-Right-Pointing-Pointer Nano-structured disproportionated Nd-Fe-B alloy powders by mechanical milling in hydrogen. Black-Right-Pointing-Pointer Highly densified green magnet compact by cold pressing of as-disproportionated Nd-Fe-B alloy powders. Black-Right-Pointing-Pointer Density-pressure data fitted well by an empirical powder compaction model. Black-Right-Pointing-Pointer As-disproportionated powder showed better compactibility than as milled and melt-spun counterparts. Black-Right-Pointing-Pointer The effects of physical properties on powder compactibility and densification mechanisms are clarified. - Abstract: The compaction behavior of nano-structured Nd{sub 16}Fe{sub 76}B{sub 8} (atomic ratio) alloy

  2. Comparative study of nano copper aluminate spinel prepared by sol–gel and modified sol–gel techniques: Structural, electrical, optical and catalytic studies

    International Nuclear Information System (INIS)

    Kumar, R. Thinesh; Suresh, P.; Selvam, N. Clament Sagaya; Kennedy, L. John; Vijaya, J. Judith

    2012-01-01

    Highlights: ► A modified sol–gel method for the preparation of nano CuAl 2 O 4 spinel using ethylenediamine was studied. ► Role of ethylenediamine in enhancing the structural, electrical, optical and catalytic properties of copper aluminate is highlighted. ► Effect of preparation method on the activity and selectivity of the samples on the oxidation of benzyl alcohol by CuAl 2 O 4 is studied. - Abstract: The effect of ethylenediamine addition in the sol–gel method for the preparation of nano CuAl 2 O 4 spinel for the enhancement in their structural, electrical, optical and catalytic properties was investigated. The samples were prepared by two different methods: sol–gel and modified sol–gel technique using ethylenediamine. X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), scanning electron microscopy (SEM), high resolution-transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), nitrogen adsorption/desorption isotherms, temperature dependent conductance measurements, thermoelectric power (TEP) measurements and UV–visible diffuse reflectance (UV–vis-DRS) spectra were used to characterize the samples prepared. CuAl 2 O 4 prepared by modified sol–gel technique was found to possess a higher surface area, lower crystallite size, lower activation energy and high porosity than the one prepared by sol–gel method which in turn lead to the improved performance of it towards the selective oxidation of benzyl alcohol to benzaldehyde. Effect of solvent on the catalytic oxidation of benzyl alcohol by the nano CuAl 2 O 4 prepared by modified sol–gel technique was also investigated.

  3. Structural evolution and formation mechanisms of TiC/Ti nanocomposites prepared by high-energy mechanical alloying

    International Nuclear Information System (INIS)

    Gu Dongdong; Meiners, Wilhelm; Hagedorn, Yves-christian; Wissenbach, Konrad; Poprawe, Reinhart

    2010-01-01

    In this work, high-energy ball milling of a micrometre-scaled Ti and TiC powder mixture was performed to prepare TiC/Ti nanocomposites. The constituent phases and microstructural characteristics of the milled powders were studied by an x-ray diffractometer, a scanning electron microscope, an energy dispersive x-ray spectroscope and a transmission electron microscope. Formation mechanisms and theoretical basis of the microstructural development were elucidated. It showed that on increasing the applied milling time, the structures of the Ti constituent experienced a successive change from hcp (5 h) to fcc (10 h) and finally to an amorphous state (≥15 h). The hydrostatic stresses caused by the excess free volume at grain boundaries were calculated to be 3.96 and 5.59 GPa for the Ti constituent in 5 and 10 h milled powders, which was responsible for the hcp to fcc polymorphic change. The amorphization of Ti constituent was due to the large defect concentration induced by severe plastic deformation during milling. The milled powder particles underwent two stages of significant refinement at 10 and 20 h during milling. For a higher milling time above 25 h, powder characteristics and chemical compositions became stable. The competitive action and the final equilibrium between the mechanisms of fracturing and cold welding accounted for the microstructural evolution. The ball milled products were typically nanocomposite powders featured by a nanocrystalline/amorphous Ti matrix reinforced with uniformly dispersed TiC nanoparticles. The finest crystalline sizes of the Ti and TiC constituents were 17.2 nm (after 10 h milling) and 13.5 nm (after 20 h milling), respectively.

  4. Raman and IR spectroscopic structural characterization of LiAlO2 powders prepared using a liquid mix technique

    International Nuclear Information System (INIS)

    Cornilsen, B.C.; Loyselle, P.L.; Saporta, J.D.

    1990-01-01

    γ-LiAlO 2 and β-LiAlO 2 have been characterized using Raman and infrared spectroscopy. Powders have been prepared using two different preparation techniques: a solution method known as the liquid mix technique (LMT) and the traditional ceramic method. The authors find that the LMT allows direct production of single phase γ-LiAlO 2 at 600 degrees C, below that found using other preparation methods. Furthermore, this solution technique appears to avoid formation of the β-LiAlO 2 intermediate phase. At lower temperatures, the LMT product is a disordered precursor of γ- LiAlO 2

  5. Preparation and crystal structure of the phosphato-niobate Tl sub 3 NaNb sub 4 O sub 9 (PO sub 4 ) sub 2

    Energy Technology Data Exchange (ETDEWEB)

    Fakhfakh, M. (Tunis Univ. (Tunisia). Faculte des Sciences); Verbaere, A. (Nantes Univ., 44 (France)); Jouini, N. (Ecole Normale Superieure de l' Enseignement Technique, Tunis (TN))

    1992-01-01

    Chemical preparation and crystal structure are described. The symmetry is orthorhombic, space group C2cm. The crystal structure has been determined using. The structure is built up from NbO{sub 6} octahedra sharing corners and PO{sub 4} tetrahedra sharing three of their corners with octahedra to form chains running along c. These chains are connected together by isolted NbO{sub 6} octahedra leasing to a three-dimensional framework which delimits cavities and tunnels occupied by the Tl and Na ions.

  6. Structure and Properties of Nanocomposites based on PTT-block-PTMO Copolymer and Graphene Oxide prepared by in Situ Polymerization

    OpenAIRE

    Paszkiewicz, Sandra; Szymczyk, Anna; Špitalský, Zdenko; Mosnáček, Jaroslav; Kwiatkowski, Konrad; Rosłaniec, Zbigniew

    2014-01-01

    Poly(trimethylene terephthalate-block-tetramethylene oxide) (PTT-PTMO) copolymer/graphene oxide nanocomposites were prepared by in situ polymerization. From the SEM and TEM images of PTT-PTMO/GO nanocomposite, it can be seen that GO sheets are clearly well-dispersed in the PTT-PTMO matrix. TEM images also showed that graphene was well exfoliated into individual sheets, suggesting that in situ polymerization is a highly efficient method for preparing nanocomposites. The influence of GO on the ...

  7. Synthesis and Characterization of Nano-Structure Metal Oxides and Peroxides Prepared by Laser Ablation in Liquids

    Science.gov (United States)

    Drmosh, Qasem Ahmed Qasem

    Pulsed laser ablation technique was applied for synthesize of ZnO, ZnO 2 and SnO2 nanostructure using metallic target in different liquids. For this purpose, a laser emitting pulsed UV radiations generated by the third harmonic of Nd:YAG (λ= 355 nm) was applied. For the synthesis of ZnO nanoparticles (NPs), a high-purity metallic plate of Zn was fixed at the bottom of a glass cell in the presence of deionized water and was irradiated at different laser energies (80- 100- 120) mJ per pulse. The average sizes and lattice parameters of ZnO produced by this method were estimated by X-ray diffraction (XRD). ZnO nanoparticles were also produced by ablation of zinc target in the presence of deionized water mixed with two types of surfactants: cetyltrimethyl ammonium bromide (CTAB) and octaethylene glycol monododecyl (OGM). The results showed that the average grain sizes decreased from 38 nm in the case of deionized water to 27 nm and 19 nm in CTAB and OGM respectively. The PL emission in CTAB and OGM showed two peaks: the sharp UV emission at 380 nm and a broad visible peak ranging from 450 nm to 600 nm. Zinc peroxide (ZnO2) nanoparticles having grain size less than 5 nm were also synthesized using pulsed laser ablation in aqueous solution in the presence of different surfactants and solid zinc target in 3 % hydrogen peroxide H2O2 for the first time. The effect of surfactants on the optical and structure of ZnO2 was studied by applying different spectroscopic techniques. The presence of the cubic phase of zinc peroxide in all samples was confirmed with XRD, and the grain sizes were 4.7 nm, 3.7 nm, 3.3 nm and 2.8 nm in pure H2O2; and H2O 2 mixed with SDS, CTAB and OGM respectively. For optical characterization, FTIR transmittance spectra of ZnO2 nanoparticles prepared with and without surfactants showed characteristic peaks of ZnO2 absorption at 435-445 cm-1. FTIR spectrum also revealed that the adsorbed surfactants on zinc peroxide disappeared in case of CTAB and OGM

  8. Structural, optical and magnetic properties of Mn doped ZnO thin films prepared by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Aravind, Arun, E-mail: aruncusat@gmail.com [Nanophotonic and Optoelectronic Devices Laboratory, Department of Physics, Cochin University of Science and Technology, Kochi 682 022, Kerala (India); Jayaraj, M.K., E-mail: mkj@cusat.ac.in [Nanophotonic and Optoelectronic Devices Laboratory, Department of Physics, Cochin University of Science and Technology, Kochi 682 022, Kerala (India); Kumar, Mukesh; Chandra, Ramesh [Nano Science Laboratory, Institute Instrumentation Centre, IIT Roorkee, Roorkee 247 667, Uttarakhand (India)

    2012-08-01

    Highlights: Black-Right-Pointing-Pointer Defect induced Raman active modes in Mn doped ZnO thin films. Black-Right-Pointing-Pointer Room temperature ferromagnetism. Black-Right-Pointing-Pointer Morphological variations of ZnO thin films with Mn doping. Black-Right-Pointing-Pointer Variation of refractive index of ZnO thin films with Mn doping. - Abstract: Zn{sub 1-x}Mn{sub x}O thin films were grown by pulsed laser deposition. The phase purity and the structure were confirmed by X-ray diffraction studies. The films have a transmittance more than 80% in the visible region. The refractive index of Zn{sub 0.90}Mn{sub 0.10}O films is found to be 1.77 at 550 nm. The presence of non-polar E{sub 2}{sup high} and E{sub 2}{sup low} Raman modes in thin films indicates that 'Mn' doping does not change the wurtzite structure of ZnO. Apart from the normal modes of ZnO the Zn{sub 1-x}Mn{sub x}O ceramic targets show two additional modes at 332 cm{sup -1} (I{sub 1}) and 524 cm{sup -1} (I{sub 2}). The broad Raman peaks (340-600 cm{sup -1}) observed Zn{sub 0.90}Mn{sub 0.10}O thin films can be deconvoluted into five peaks, denoted as P{sub 1}-P{sub 5}. The possible origins of Raman peaks in Zn{sub 1-x}Mn{sub x}O films are the structural disorder and morphological change caused by the Mn dopant. The B{sub 1}{sup low}, {sup 2}B{sub 1}{sup low}, B{sub 1}{sup high} and A{sub 1}{sup LO} modes as well as the surface phonon mode have been observed in heavily Mn-doped ZnO films. Zn{sub 0.98}Mn{sub 0.02}O thin film shows room temperature ferromagnetism. The saturation magnetic moment of the Zn{sub 0.98}Mn{sub 0.02}O thin film is 0.42{mu}{sub B}/Mn atom. The undoped ZnO film prepared under the same condition shows diamagnetic nature. At higher doping concentrations the formation of Mn clusters suppress the room temperature ferromagnetism in Zn{sub 1-x}Mn{sub x}O thin films and shows paramagnetism. XPS confirms the incorporation of Mn{sup 2+} into the ZnO lattice.

  9. Effects of Preparation Method on the Structure and Catalytic Activity of Ag–Fe2O3 Catalysts Derived from MOFs

    Directory of Open Access Journals (Sweden)

    Xiaodong Zhang

    2017-12-01

    Full Text Available In this work, Ag–Fe2O3 catalysts were successfully prepared using several different methods. Our main intention was to investigate the effect of the preparation methods on the catalysts’ structure and their catalytic performance for CO oxidation. The catalysts were characterized by X-ray diffraction (XRD, N2 adsorption–desorption, transmission electron microscopy (TEM, X-ray photoelectron spectroscopy (XPS, H2-temperature program reduction (H2-TPR and inductively coupled plasma optical emission spectroscopy (ICP-OES. Ag–Fe catalysts prepared by impregnating Ag into MIL-100 (Fe presented the best catalytic activity, over which CO could be completely oxidized at 160 °C. Based on the characterization, it was found that more metallic Ag species and porosity existed on Ag–Fe catalysts, which could efficiently absorb atmospheric oxygen and, thus, enhance the CO oxidation.

  10. Preparation and characterization of structures of oxygen-ion-conductive thin-film membranes; Herstellung und Charakterisierung von sauerstoffionenleitenden Duennschichtmembranstrukturen

    Energy Technology Data Exchange (ETDEWEB)

    Betz, Michael

    2010-07-01

    In power plants using Oxyfuel technology, fossil fuels are combusted with pure oxygen. This leads to carbon dioxide of high purity, which is necessary for its transport and storage. Oxygen separation by means of perovskitic membranes have great potential to decrease the efficiency losses caused by the allocation of the enormous amounts of oxygen. The aim of this work is the preparation and characterisation of thin film membranes on porous substrates and the analysis of their oxygen permeation properties. Therefore the material system A{sub 0,68}Sr{sub 0,3}Fe{sub 0,8}Co{sub 0,2}O{sub 3-{delta}} (A68SFC) was analysed, where the A-site was substituted with Lanthanides (La, Pr, Nd, Eu, Sm, Gd, Dy, Er) or alkaline earth metals (Ba, Ca). After an extensive characterisation, the selection was reduced to the substitutions with La, Pr and Nd. Other compounds could not meet the demands with regard to phase purity, chemical stability or extension behaviour. All analyses were conducted in comparison to Ba{sub 0,5}Sr{sub 0,5}Co{sub 0,8}Fe{sub 0,2}O{sub 3-{delta}} (BSCF) which is known to exhibit higher permeation rates, but is more sensitive to stability issues. The dependency of permeation rates on membrane thickness or oxygen partial pressures on both membrane surfaces is discussed by means of permeation measurements conducted on bulk BSCF membranes. These cannot be described completely by the Wagner equation. This is due to changes of the driving force originating from influences of the surface reaction kinetics and concentration polarisation on the membrane surface, which are not considered. Porous substrates for asymmetric membranes were manufactured by tape casting and warm pressing. The application of the functional layer was performed via screen printing. Permeation measurements show that the asymmetric structures exhibit higher permeation rates in comparison to bulk membranes with L=1 mm. The moderate increase can be attributed to the low gas permeability of the

  11. 3′,7′,7′-Trimethyl-1′-phenyl-5′,6′,7′,8′-tetrahydrospiro[indoline-3,4′-(1H,4H-pyrazolo[3,4-b]chromene]-2,5′-dione

    Directory of Open Access Journals (Sweden)

    Li-Qin Zhao

    2010-12-01

    Full Text Available The title spirooxindole compound, C26H23N3O3, was prepared by the reaction of isatin, 3-methyl-1-phenyl-2-pyrazolin-5-one and 5,5-dimethylcyclohexane-1,3-dione in an ethanol solution. The fused cyclohexene ring adopts an envelope conformation. The dihedral angle between the aromatic and pyrazoline rings is 23.70 (8°. An intramolecular C—H...O interaction occurs. The crystal structure is stabilized by N—H...N hydrogen-bonding interactions, leading to a zigzag chain along the b axis.

  12. Effect of Maleic Acid Content on the Thermal Stability, Swelling Behaviour and Network Structure of Gelatin -Based Hydrogels Prepared by Gamma Irradiation

    International Nuclear Information System (INIS)

    Eid, M.; Dessouki, A.M.; Abdel-Ghaffar, M.A.

    2005-01-01

    The preparation of highly swelling hydrogels containing diprotic acid and gelatin carried out by gamma-irradiation of acrylamide/maleic acid/gelatine/water mixture at ambient temperature. Poly (acrylamide/maleic acid/gelatin) p(AAm/MA/G) hydrogels were prepared in different MA and G contents at low dose rate (0.94 kGy/h), and moderate dose rate (3.84 kGy/h). The prepared hydrogels were confirmed by FT1R . The effect of copolymer composition, dose and dose rate on the swelling behaviour and the type of water diffusion in the network structure of the hydrogels was discussed. Increasing of MA content and G in the initial mixture leads to an increase in the amount of MA and G in the gel system and decrease in the gelation percent. The swelling behaviours of the hydrogel prepared at moderate dose rate increased with increasing MA mole content in the gel system. On the other hand, no systematic dependence of swelling on MA content was observed for the hydrogels obtained at low dose rate. Pore structure of the hydrogels was monitored by using scanning electron microscopy. Systematic swelling of P(AAm/MA/G) hydrogels prepared at moderate dose rates can be explained by the homogeneous pore size distribution of network. Thermogravimetric analysis (TGA) was employed to study the effect of network structure formation on the thermal behavior of the copolymer. To give a better understanding of the thermal stability of polymers, the rate of the thermal decomposition of P(AAm/MA/G) hydrogels has been evaluated

  13. Effects of the preparation method on the structure and the visible-light photocatalytic activity of Ag2CrO4

    Directory of Open Access Journals (Sweden)

    Difa Xu

    2014-05-01

    Full Text Available Silver chromate (Ag2CrO4 photocatalysts are prepared by microemulsion, precipitation, and hydrothermal methods, in order to investigate the effect of preparation methods on the structure and the visible-light photocatalytic activity. It is found that the photocatalytic activity of the prepared Ag2CrO4was highly dependent on the preparation methods. The sample prepared by microemulsion method exhibits the highest photocatalytic efficiency on the degradation of methylene blue (MB under visible-light irradiation. The enhanced photocatalytic activity could be ascribed to the smaller particle size, higher surface area, relatively stronger light absorption, and blue-shift absorption edge, which result in the adsorption of more MB molecules, a shorter diffusion process of more photogenerated excitons, and a stronger oxidation ability of the photogenerated holes. Considering the universalities of microemulsion, precipitation, and hydrothermal methods, this work may also provide a prototype for the comparative study of semiconductor based photocatalysis for water purification and environmental remediation.

  14. Band structure and visible light photocatalytic activity of multi-type nitrogen doped TiO(2) nanoparticles prepared by thermal decomposition.

    Science.gov (United States)

    Dong, Fan; Zhao, Weirong; Wu, Zhongbiao; Guo, Sen

    2009-03-15

    Multi-type nitrogen doped TiO(2) nanoparticles were prepared by thermal decomposition of the mixture of titanium hydroxide and urea at 400 degrees C for 2h. The as-prepared photocatalysts were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (UV-vis DRS), and photoluminescence (PL). The results showed that the as-prepared samples exhibited strong visible light absorption due to multi-type nitrogen doped in the form of substitutional (N-Ti-O and Ti-O-N) and interstitial (pi* character NO) states, which were 0.14 and 0.73 eV above the top of the valence band, respectively. A physical model of band structure was established to clarify the visible light photocatalytic process over the as-prepared samples. The photocatalytic activity was evaluated for the photodegradation of gaseous toluene under visible light irradiation. The activity of the sample prepared from wet titanium hydroxide and urea (TiO(2)-Nw, apparent reaction rate constant k = 0.045 min(-1)) was much higher than other samples including P25 (k = 0.0013 min(-1)). The high activity can be attributed to the results of the synergetic effects of strong visible light absorption, good crystallization, large surface hydroxyl groups, and enhanced separation of photoinduced carriers.

  15. Textured surface structures formed using new techniques on transparent conducting Al-doped zinc oxide films prepared by magnetron sputtering

    International Nuclear Information System (INIS)

    Minami, Tadatsugu; Miyata, Toshihiro; Uozaki, Ryousuke; Sai, Hitoshi; Koida, Takashi

    2016-01-01

    Surface-textured Al-doped ZnO (AZO) films formed using two new techniques based on magnetron sputtering deposition were developed by optimizing the light scattering properties to be suitable for transparent electrode applications in thin-film silicon solar cells. Scrambled egg-like surface-textured AZO films were prepared using a new texture formation technique that post-etched pyramidal surface-textured AZO films prepared under deposition conditions suppressing c-axis orientation. In addition, double surface-textured AZO films were prepared using another new texture formation technique that completely removed, by post-etching, the pyramidal surface-textured AZO films previously prepared onto the initially deposited low resistivity AZO films; simultaneously, the surface of the low resistivity films was slightly etched. However, the obtained very high haze value in the range from the near ultraviolet to visible light in the scrambled egg-like surface-textured AZO films did not contribute significantly to the obtainable photovoltaic properties in the solar cells fabricated using the films. Significant light scattering properties as well as a low sheet resistance could be achieved in the double surface-textured AZO films. In addition, a significant improvement of external quantum efficiency in the range from the near ultraviolet to visible light was achieved in superstrate-type n-i-p μc-Si:H solar cells fabricated using a double surface-textured AZO film prepared under optimized conditions as the transparent electrode. - Highlights: • Double surface-textured AZO films prepared using a new texture formation technique • Extensive light scattering properties with low sheet resistance achieved in the double surface-textured AZO films • Improved external quantum efficiency of μc-Si:H solar cells using a double surface-textured AZO film

  16. Textured surface structures formed using new techniques on transparent conducting Al-doped zinc oxide films prepared by magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Minami, Tadatsugu [Optoelectronic Device System R& D Center, Kanazawa Institute of Technology, Nonoichi, Ishikawa 921-8501 (Japan); Miyata, Toshihiro, E-mail: tmiyata@neptune.kanazawa-it.ac.jp [Optoelectronic Device System R& D Center, Kanazawa Institute of Technology, Nonoichi, Ishikawa 921-8501 (Japan); Uozaki, Ryousuke [Optoelectronic Device System R& D Center, Kanazawa Institute of Technology, Nonoichi, Ishikawa 921-8501 (Japan); Sai, Hitoshi; Koida, Takashi [Research Center for Photovoltaics, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba, Ibaraki 305-8568 (Japan)

    2016-09-01

    Surface-textured Al-doped ZnO (AZO) films formed using two new techniques based on magnetron sputtering deposition were developed by optimizing the light scattering properties to be suitable for transparent electrode applications in thin-film silicon solar cells. Scrambled egg-like surface-textured AZO films were prepared using a new texture formation technique that post-etched pyramidal surface-textured AZO films prepared under deposition conditions suppressing c-axis orientation. In addition, double surface-textured AZO films were prepared using another new texture formation technique that completely removed, by post-etching, the pyramidal surface-textured AZO films previously prepared onto the initially deposited low resistivity AZO films; simultaneously, the surface of the low resistivity films was slightly etched. However, the obtained very high haze value in the range from the near ultraviolet to visible light in the scrambled egg-like surface-textured AZO films did not contribute significantly to the obtainable photovoltaic properties in the solar cells fabricated using the films. Significant light scattering properties as well as a low sheet resistance could be achieved in the double surface-textured AZO films. In addition, a significant improvement of external quantum efficiency in the range from the near ultraviolet to visible light was achieved in superstrate-type n-i-p μc-Si:H solar cells fabricated using a double surface-textured AZO film prepared under optimized conditions as the transparent electrode. - Highlights: • Double surface-textured AZO films prepared using a new texture formation technique • Extensive light scattering properties with low sheet resistance achieved in the double surface-textured AZO films • Improved external quantum efficiency of μc-Si:H solar cells using a double surface-textured AZO film.

  17. A facile dip-coating process for preparing highly durable superhydrophobic surface with multi-scale structures on paint films.

    Science.gov (United States)

    Cui, Zhe; Yin, Long; Wang, Qingjun; Ding, Jianfu; Chen, Qingmin

    2009-09-15

    Superhydrophobic surfaces with multi-scale nano/microstructures have been prepared on epoxy paint surfaces using a feasible dip-coating process. The microstructures with 5-10 microm protuberances were first prepared on epoxy paint surface by sandblast. Then the nanostructures were introduced on the microstructure surface by anchoring 50-100 nm SiO(2) particles (nano-SiO(2)) onto the sandblasted paint surface, which was completed by dip-coating with a nano-SiO(2)/epoxy adhesive solution (M1). At last the surface was further modified for enhancing hydrophobicity by another dip-coating with a solution of a low surface energy polymer, aminopropyl terminated polydimethylsiloxane (ATPS) modified epoxy adhesive (M2). The water contact angle of the as-prepared samples reached as high as 167.8 degrees and the sliding angle was 7 degrees. The prepared superhydrophobic surface exhibited excellent durability to the high speed scouring test and high stability in neutral and basic aqueous solutions and some common organic solvents. In addition, this method can be adopted to fabricate large scale samples with a good homogeneity of the whole surface at very low cost.

  18. Advanced fluidic handling and use of two-phase flow for high throughput structural investigation of proteins on a microfluidic sample preparation platform

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Møller, M.

    2010-01-01

    Research on the structure of proteins can bring forth a wealth of information about biological function and can be used to better understand the processes in living cells. This paper reports a new microfluidic sample preparation system for the structural investigation of proteins by Small Angle X......-ray Scattering (SAXS). The system includes hardware and software features for precise fluidic control, synchrotron beamline control, UV absorbance measurements and automated data analysis. The precise fluidic handling capabilities are used to transport and precisely position samples as small as 500 n...

  19. Emergency Management Span of Control: Optimizing Organizational Structures to Better Prepare Vermont for the Next Major or Catastrophic Disaster

    National Research Council Canada - National Science Library

    Schumacher, Ludwig J

    2008-01-01

    ..., and actionable federal requests for assistance cannot be articulated. Forty-five states have county emergency management structures between municipal and state structures, which regionalize emergency management within those states...

  20. H++ 3.0: automating pK prediction and the preparation of biomolecular structures for atomistic molecular modeling and simulations.

    Science.gov (United States)

    Anandakrishnan, Ramu; Aguilar, Boris; Onufriev, Alexey V

    2012-07-01

    The accuracy of atomistic biomolecular modeling and simulation studies depend on the accuracy of the input structures. Preparing these structures for an atomistic modeling task, such as molecular dynamics (MD) simulation, can involve the use of a variety of different tools for: correcting errors, adding missing atoms, filling valences with hydrogens, predicting pK values for titratable amino acids, assigning predefined partial charges and radii to all atoms, and generating force field parameter/topology files for MD. Identifying, installing and effectively using the appropriate tools for each of these tasks can be difficult for novice and time-consuming for experienced users. H++ (http://biophysics.cs.vt.edu/) is a free open-source web server that automates the above key steps in the preparation of biomolecular structures for molecular modeling and simulations. H++ also performs extensive error and consistency checking, providing error/warning messages together with the suggested corrections. In addition to numerous minor improvements, the latest version of H++ includes several new capabilities and options: fix erroneous (flipped) side chain conformations for HIS, GLN and ASN, include a ligand in the input structure, process nucleic acid structures and generate a solvent box with specified number of common ions for explicit solvent MD.

  1. Preparation and crystal structure of SrCu/sub 2/Sb/sub 2/ and SrZnBi/sub 2/

    Energy Technology Data Exchange (ETDEWEB)

    Cordier, G; Eisenmann, B; Schaefer, H [Technische Hochschule Darmstadt (Germany, F.R.). Fachbereich Anorganische Chemie und Kernchemie

    1976-10-01

    SrCu/sub 2/Sb/sub 2/ and SrZnBi/sub 2/ have been prepared and analytically and structurally characterized. SrCu/sub 2/Sb/sub 2/ crystallizes tetragonal in the CaBe/sub 2/Ge/sub 2/ structure type. SrZnBi/sub 2/ has its own structure type. In both structures the transition metal atoms form with the semimetal atoms tetragonal pyramids, which are connected by common edges of the basis to twodimensional sheets. These sheets are separated in the case of SrCu/sub 2/Sb/sub 2/ by single sheets of strontium atoms, in the case of SrZnBi/sub 2/ by double sheets of strontium atoms in which fourfold nets of Bi atoms are located.

  2. "In situ preparation": new surgical procedure indicated for soft-tissue sarcoma of a lower limb in close proximity to major neurovascular structures.

    Science.gov (United States)

    Matsumoto, Seiichi; Kawaguchi, Noriyoshi; Manabe, Jun; Matsushita, Yasushi

    2002-02-01

    When soft-tissue sarcomas occur near neurovascular structures, preoperative images cannot always reveal the accurate relationship between the tumor and these structures. Therefore, in some patients, neurovascular structures are sacrificed unnecessarily. In other patients, neurovascular structures are preserved with an inappropriate margin, followed by local recurrence. The objective of this study was to evaluate a new surgical method, "in situ preparation" (ISP), which enables the preparation of neurovascular bundles and the intraoperative evaluation of the surgical margin without contamination by tumor cells. With this method, additional procedures, including pasteurization, alcohol soaking, and distilled water soaking of the preserved neurovascular bundle can also be performed to preserve the continuity of vessels. Between April 1992 and December 1998, 18 patients with soft-tissue sarcoma were operated on using ISP. The tumor and neurovascular structure were lifted en bloc from the surgical bed and separated from the field by the use of a vinyl sheet. The consistency of the neurovascular structures was preserved. The tissue block could be freely turned around and the neurovascular structure was separated from the block through the nearest approach. The margin between the tumor and neurovascular structure was evaluated, and an additional procedure, such as pasteurization, alcohol soaking or distilled water soaking, was performed, according to the safety of the surgical margin. Only one patient showed recurrence after ISP. Complications after ISP were arterial occlusion in two patients and nerve palsy in three patients. The main cause of these complications was the long period of pasteurization; modified additional procedures could prevent such complications. ISP is a useful method with which to ensure a safe surgical margin and good functional results.

  3. Structural and magnetic characterization of as-prepared and annealed FeCoCu nanowire arrays in ordered anodic aluminum oxide templates

    Energy Technology Data Exchange (ETDEWEB)

    Rodríguez-González, B., E-mail: jbenito@uvigo.es [CACTI, University of Vigo, E-36310 Vigo (Spain); International Iberian Nanotechnology Laboratory, INL. Av. Mestre J. Veiga, 4715-330 Braga (Portugal); Bran, C.; Warnatz, T.; Vazquez, M. [Institute of Materials Science of Madrid, CSIC, 28049 Madrid (Spain); Rivas, J. [International Iberian Nanotechnology Laboratory, INL. Av. Mestre J. Veiga, 4715-330 Braga (Portugal)

    2014-04-07

    Herein, we report on the preparation, structure, and magnetic characterization of FeCoCu nanowire arrays grown by DC electrodeposition inside self-assembled ordered nanopores of anodic aluminum oxide templates. A systematic study of their structure has been performed both in as-prepared samples and after annealing in the temperature range up to 800 °C, although particular attention has been paid to annealing at 700 °C after which maximum magnetic hardening is achieved. The obtained nanowires have a diameter of 40 nm and their Fe{sub 0.28}Co{sub 0.67}Cu{sub 0.05} composition was confirmed by energy dispersive X-ray spectroscopy (EDS). Focused ion-beam lamellas of two samples (as-prepared and annealed at 700 °C) were prepared for their imaging in the high-resolution transmission electron microscopy (HRTEM) perpendicularly to the electron beam, where the obtained EDS compositional mappings show a homogeneous distribution of the elements. X-ray diffraction analysis, and selected area electron diffraction (SAED) patterns confirm that nanowires exhibit a bcc cubic structure (space group Im-3m). In addition, bright-dark field images show that the nanowires have a polycrystalline structure that remains essentially the same after annealing, but some modifications were observed: (i) an overall increase and sharpening of recrystallized grains, and (ii) an apparent shrinkage of the nanowires diameter. Obtained SAED patterns also show strong textured components with determined <111> and <112> crystalline directions parallel to the wires growth direction. The presence of both directions was also confirmed in the HRTEM images doing Fourier transform analyses. Magnetic measurements show strong magnetic anisotropy with magnetization easy axis parallel to the nanowires in as-prepared and annealed samples. The magnetic properties are tuned by suitable thermal treatments so that, maximum enhanced coercivity (∼2.7 kOe) and normalized remanence (∼0.91 Ms) values are

  4. Structural and magnetic characterization of as-prepared and annealed FeCoCu nanowire arrays in ordered anodic aluminum oxide templates

    International Nuclear Information System (INIS)

    Rodríguez-González, B.; Bran, C.; Warnatz, T.; Vazquez, M.; Rivas, J.

    2014-01-01

    Herein, we report on the preparation, structure, and magnetic characterization of FeCoCu nanowire arrays grown by DC electrodeposition inside self-assembled ordered nanopores of anodic aluminum oxide templates. A systematic study of their structure has been performed both in as-prepared samples and after annealing in the temperature range up to 800 °C, although particular attention has been paid to annealing at 700 °C after which maximum magnetic hardening is achieved. The obtained nanowires have a diameter of 40 nm and their Fe 0.28 Co 0.67 Cu 0.05 composition was confirmed by energy dispersive X-ray spectroscopy (EDS). Focused ion-beam lamellas of two samples (as-prepared and annealed at 700 °C) were prepared for their imaging in the high-resolution transmission electron microscopy (HRTEM) perpendicularly to the electron beam, where the obtained EDS compositional mappings show a homogeneous distribution of the elements. X-ray diffraction analysis, and selected area electron diffraction (SAED) patterns confirm that nanowires exhibit a bcc cubic structure (space group Im-3m). In addition, bright-dark field images show that the nanowires have a polycrystalline structure that remains essentially the same after annealing, but some modifications were observed: (i) an overall increase and sharpening of recrystallized grains, and (ii) an apparent shrinkage of the nanowires diameter. Obtained SAED patterns also show strong textured components with determined and crystalline directions parallel to the wires growth direction. The presence of both directions was also confirmed in the HRTEM images doing Fourier transform analyses. Magnetic measurements show strong magnetic anisotropy with magnetization easy axis parallel to the nanowires in as-prepared and annealed samples. The magnetic properties are tuned by suitable thermal treatments so that, maximum enhanced coercivity (∼2.7 kOe) and normalized remanence (∼0.91 Ms) values are achieved after annealing at

  5. Effect of Nanocomposite Structures on Fracture Behavior of Epoxy-Clay Nanocomposites Prepared by Different Dispersion Methods

    Directory of Open Access Journals (Sweden)

    Mohammad Bashar

    2014-01-01

    Full Text Available The effects of organic modifier and processing method on morphology and mechanical properties of epoxy-clay nanocomposites were investigated. In this study, the preparation of nanocomposites by exfoliation-adsorption method involved an ultrasonic mixing procedure, and mechanical blending was used for in situ intercalative polymerization. The microstructure study revealed that the organoclay, which was ultrasonically mixed with the epoxy, partially exfoliated and intercalated. In contrast, organoclay remained in phase-separated and flocculated state after the mechanical blending process. Tensile stiffness increased significantly for the nanocomposite prepared by ultrasonic dispersion method through realizing the reinforcing potential of exfoliated silicate layers. Nanocomposites with exfoliated and intercalated nanoclay morphology were ineffective in enhancing the fracture toughness whereas nanocomposites with phase-separated and flocculated morphology have improved crack resistance predominantly by crack deflecting and pinning mechanisms.

  6. New synthesis parameters of GGG:Nd nanocrystalline powder prepared by sol–gel method: Structural and spectroscopic investigation

    Energy Technology Data Exchange (ETDEWEB)

    Alshikh Mohamad, Yassin, E-mail: yassinm@mail.ru; Atassi, Yomen; Moussa, Zafer

    2015-09-15

    GGG:Nd nanopowder is synthesized by the sol–gel method using formic acid and acetic acid as chelating agents and ethylene glycol as a cross linking agent. TGA–DSC, XRD, photoluminescence spectroscopy and fluorescence life time analysis (τ) are used to characterize the powder. XRD is used to optimize the synthesis parameters. According to XRD, complete phase of GGG nanopowder is formed at 800 °C for 1 min. Fluorescence life time analyses reveal that the optimum crystallization temperature is 1000 °C. - Highlights: • GGG:Nd nanopowder was prepared using formic acid by the sol gel method. • Optimization of sol gel parameters was done. • GGG phase formation was complete at 800 °C for 1 min • According to τ measurements, optimal temperature treatment is at 1000 °C. • Nanopowder prepared with formic acid was better than that formed with acetic acid.

  7. Structure and strength of aluminum with sub-micrometer/micrometer grain size prepared by spark plasma sintering

    DEFF Research Database (Denmark)

    Le, G.M.; Godfrey, A.; Hansen, Niels

    2013-01-01

    A spark plasma sintering (SPS) technique has been applied to prepare fully dense Al samples from Al powder. By applying a sintering temperature of 600°C and a loading pressure of 50MPa, fully recrystallized samples of nearly 100% density with average grain sizes of 5.2μm, 1.3μm and 0.8μm have bee...... strengthening. © 2013 Elsevier Ltd....

  8. Preparation, structural analysis and bioactivity of ribonuclease A-albumin conjugate: tetra-conjugation or PEG as the linker.

    Science.gov (United States)

    Li, Chunju; Lin, Qixun; Wang, Jun; Shen, Lijuan; Ma, Guanghui; Su, Zhiguo; Hu, Tao

    2012-12-31

    Ribonuclease A (RNase A) is a therapeutic enzyme with cytotoxic action against tumor cells. Its clinical application is limited by the short half-life and insufficient stability. Conjugation of albumin can overcome the limitation, whereas dramatically decrease the enzymatic activity of RNase A. Here, three strategies were proposed to prepare the RNase A-bovine serum albumin (BSA) conjugates. R-SMCC-B (a conjugate of four RNase A attached with one BSA) and R-PEG-B (a mono-conjugate) were prepared using Sulfo-SMCC (a short bifunctional linker) and mal-PEG-NHS (a bifunctional PEG), respectively. Mal-PEG-NHS and hexadecylamine (HDA) were used to prepare the mono-conjugate, R-HDA-B, where HDA was adopted to bind BSA. The PEG linker can elongate the proximity between RNase A and BSA. In contrast, four RNase A were closely located on BSA in R-SMCC-B. R-SMCC-B showed the lowest K(m) and the highest relative enzymatic activity and k(cat)/K(m) in the three conjugates. Presumably, the tetravalent interaction of RNase A in R-SMCC-B can increase the binding affinity to its substrate. In addition, the slow release of BSA from R-HDA-B may increase the enzymatic activity of R-HDA-B. Our study is expected to provide strategies to develop protein-albumin conjugate with high therapeutic potential. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Synthesis, spectroscopic, structural and optical studies of Ru2S3 nanoparticles prepared from single-source molecular precursors

    Science.gov (United States)

    Mbese, Johannes Z.; Ajibade, Peter A.

    2017-09-01

    Homonuclear tris-dithiocarbamato ruthenium(III) complexes, [Ru(S2CNR2)3] were prepared and characterized by spectroscopic techniques and thermogravimetric analyses. The thermogravimetric analyses (TGA) of the ruthenium complexes showed that the complexes decompose to ruthenium(III) sulfide nanoparticles. The ruthenium(III) complexes were dispersed in oleic acid and thermolysed in hexadecylamine to prepared oleic acid/hexadecylamine capped Ru2S3 nanoparticles. FTIR revealed that Ru2S3 nanoparticles are capped through the interaction of the -NH2 group of hexadecylamine HDA adsorbed on the surfaces of nanoparticles and it also showed that oleic acid (OA) is acting as both coordinating stabilizing surfactant and capping agent. EDS spectra revealed that the prepared nanoparticles are mainly composed of Ru and S, confirming the formation of Ru2S3 nanoparticles. Powder XRD confirms that the nanoparticles are in cubic phase. The inner morphology of nanoparticles obtained from transmission electron microscopy (TEM) showed nanoparticles with narrow particle size distributions characterized by an average diameter of 8.45 nm with a standard deviation of 1.6 nm. The optical band gap (Eg) determined from Tauc plot are in the range 3.44-4.18 eV.

  10. Hydrothermal preparation of blue molybdenum bronze nanoribbons: structural changes in mother crystals, related to solid-state conversion and crystallite splitting to nanomorphology

    Science.gov (United States)

    Nishida, Takamasa; Eda, Kazuo

    2018-02-01

    Hydrothermal syntheses of alkali-metal blue molybdenum bronze nanoribbons, which are expected to exhibit unique properties induced by a combined effect of extrinsic and intrinsic low-dimensionalities, from hydrated-alkali-metal molybdenum bronzes were investigated. Nanoribbons grown along the quasi-one-dimensional (1D) conductive direction of Cs0.3MoO3, which is difficult to prepare by the conventional methods, were first synthesized. The nanomorphology formation is achieved by a solid-state conversion (or crystallite splitting) and subsequent crystallite growth, and the structural changes of the starting material related to the conversion were first observed by powder X-ray diffraction and scanning transmission electron microscopy as a result of finely tuned reaction system and preparation conditions. The structural changes were analyzed by model simulations and were attributed to the structural modulations that were concerned with the intralayer packing disorder and with two-dimensional long-range ordered structure, formed in MoO3 sheets of the hydrated molybdenum bronze. Moreover, the modulations were related to displacement defects of the Mo-O framework units generated along the [100] direction in the hydrated molybdenum bronze. Then, it was suggested that the solid-state conversion into blue molybdenum bronze and the crystallite splitting to nanomorphology were initiated by the breaking of the Mo-O-Mo bonds at the defects. [Figure not available: see fulltext.

  11. Pseudocapacitive properties of nano-structured anhydrous ruthenium oxide thin film prepared by electrostatic spray deposition and electrochemical lithiation/delithiation

    Energy Technology Data Exchange (ETDEWEB)

    Park, S.H.; Kim, J.Y.; Kim, K.B. [Division of Materials Science and Engineering, Yonsei University, Seoul (Korea, Republic of)

    2010-10-15

    Nano-structured anhydrous ruthenium oxide (RuO{sub 2}) thin films were prepared using an electrostatic spray deposition (ESD) technique followed by electrochemical lithiation and delithiation. During the electrochemical lithiation process, RuO{sub 2} decomposed to nano-structured metallic ruthenium Ru with the concomitant formation of Li{sub 2}O. Nano-structured RuO{sub 2} was formed upon subsequent electrochemical extraction of Li from the Ru/Li{sub 2}O nanocomposite. Electrochemical lithiation/deliathiation at different charge/discharge rates (C-rate) was used to control the nano-structure of the anhydrous RuO{sub 2}. Electrochemical lithiation/delithiation of the RuO{sub 2} thin film electrode at different C-rates was closely related to the specific capacitance and high rate capability of the nano-structured anhydrous RuO{sub 2} thin film. Nano-structured RuO{sub 2} thin films prepared by electrochemical lithiation and delithiation at 2C rate showed the highest specific capacitance of 653 F g{sup -1} at 20 mV s{sup -1}, which is more than two times higher than the specific capacitance of 269 F g{sup -1} for the as-prepared RuO{sub 2}. In addition, it showed 14% loss in specific capacitance from 653 F g{sup -1} at 20 mV s{sup -1} to 559 F g{sup -1} at 200 mV s{sup -1}, indicating significant improvement in the high rate capability compared to the 26% loss of specific capacitance of the as-prepared RuO{sub 2} electrode from 269 F g{sup -1} at 20 mV s{sup -1} to 198 F g{sup -1} at 200 mV s{sup -1} for the same change in scan rate. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  12. Synthesis, structural investigation and magnetic properties of Zn2+ substituted cobalt ferrite nanoparticles prepared by the sol–gel auto-combustion technique

    International Nuclear Information System (INIS)

    Raut, A.V.; Barkule, R.S.; Shengule, D.R.; Jadhav, K.M.

    2014-01-01

    Structural morphology and magnetic properties of the Co 1−x Zn x Fe 2 O 4 (0.0≤x≥1.0) spinel ferrite system synthesized by the sol–gel auto-combustion technique using nitrates of respective metal ions have been studied. The ratio of metal nitrates to citric acid was taken at 1:3. The as prepared powder of cobalt zinc ferrite was sintered at 600 °C for 12 h after TG/DTA thermal studies. Compositional stoichiometry was confirmed by energy dispersive analysis of the X-ray (EDAX) technique. Single phase cubic spinel structure of Co–Zn nanoparticles was confirmed by XRD data. The average crystallite size (t), lattice constant (a) and other structural parameters of zinc substituted cobalt ferrite nanoparticles were calculated from XRD followed by SEM and FTIR. It is observed that the sol–gel auto-combustion technique has many advantages for the synthesis of technologically applicable Co–Zn ferrite nanoparticles. The present investigation clearly shows the effect of the synthesis method and possible relation between magnetic properties and microstructure of the prepared samples. Increase in nonmagnetic Zn 2+ content in cobalt ferrite nanoparticles is followed by decrease in n B , M s and other magnetic parameters. Squareness ratio for the Co-ferrite was 1.096 at room temperature. - Highlights: • Co–Zn nanoparticles are prepared by sol–gel auto-combustion method. • Structural properties were characterized by XRD, SEM, and FTIR. • Compositional stoichiometry was confirmed by EDAX analysis. • Magnetic parameters were measured by the pulse field hysteresis loop technique

  13. Synthesis, structural investigation and magnetic properties of Zn{sup 2+} substituted cobalt ferrite nanoparticles prepared by the sol–gel auto-combustion technique

    Energy Technology Data Exchange (ETDEWEB)

    Raut, A.V., E-mail: nano9993@gmail.com [Vivekanand Arts and Sardar Dalipsingh Commerce and Science College, Aurangabad, 431004 Maharastra (India); Barkule, R.S.; Shengule, D.R. [Vivekanand Arts and Sardar Dalipsingh Commerce and Science College, Aurangabad, 431004 Maharastra (India); Jadhav, K.M., E-mail: drjadhavkm@gmail.com [Department of Physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad, 431004 Maharastra (India)

    2014-05-01

    Structural morphology and magnetic properties of the Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (0.0≤x≥1.0) spinel ferrite system synthesized by the sol–gel auto-combustion technique using nitrates of respective metal ions have been studied. The ratio of metal nitrates to citric acid was taken at 1:3. The as prepared powder of cobalt zinc ferrite was sintered at 600 °C for 12 h after TG/DTA thermal studies. Compositional stoichiometry was confirmed by energy dispersive analysis of the X-ray (EDAX) technique. Single phase cubic spinel structure of Co–Zn nanoparticles was confirmed by XRD data. The average crystallite size (t), lattice constant (a) and other structural parameters of zinc substituted cobalt ferrite nanoparticles were calculated from XRD followed by SEM and FTIR. It is observed that the sol–gel auto-combustion technique has many advantages for the synthesis of technologically applicable Co–Zn ferrite nanoparticles. The present investigation clearly shows the effect of the synthesis method and possible relation between magnetic properties and microstructure of the prepared samples. Increase in nonmagnetic Zn{sup 2+} content in cobalt ferrite nanoparticles is followed by decrease in n{sub B}, M{sub s} and other magnetic parameters. Squareness ratio for the Co-ferrite was 1.096 at room temperature. - Highlights: • Co–Zn nanoparticles are prepared by sol–gel auto-combustion method. • Structural properties were characterized by XRD, SEM, and FTIR. • Compositional stoichiometry was confirmed by EDAX analysis. • Magnetic parameters were measured by the pulse field hysteresis loop technique.

  14. Preparation and structural characterization of the thermoluminescent material CaSO{sub 4}: Dy; Preparacion y caracterizacion estructural del material termoluminiscente CaSO{sub 4}: Dy

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez R, A.; Azorin, J. [UAM-I, 09340 Mexico D.F. (Mexico); Gonzalez M, P.R. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico); Rivera, T. [CICATA-IPN, Legaria 694, 11500 Mexico D.F. (Mexico)

    2005-07-01

    The grade of crystallinity of a material is important so that the one is presented the thermoluminescence phenomenon; for what is necessary to study those structural characteristic of a TL material and to correlate them with its TL response when being irradiated with ionizing radiation. The calcium sulfate activated with Dysprosium (CaSO{sub 4}: Dy) it is a material that has demonstrated its efficiency in the dosimetry of the ionizing radiation for the thermoluminescence method. In this work the structural characterization of this prepared material for the recrystallization method by means of the evaporation of the solvent and their relationship with their TL response is presented. The results showed that the best material to be used in thermoluminescent dosimetry presents a crystalline structure in orthorhombic phase and a particle size in the interval of 80 {mu}m to 200 {mu}m. (Author)

  15. Structure and magnetism of SmCo5 nanoflakes prepared by surfactant-assisted ball milling with different ball sizes

    International Nuclear Information System (INIS)

    Nie, Junwu; Han, Xianghua; Du, Juan; Xia, Weixing; Zhang, Jian; Guo, Zhaohui; Yan, Aru; Li, Wei; Ping Liu, J.

    2013-01-01

    Anisotropic magnetic SmCo 5 nanoflakes have been fabricated by surfactant-assisted ball milling (SABM) using hardened steel balls of one of the following sizes: 4, 6.5, 9.5 and 12.7 mm in diameters. The magnetic properties of SmCo 5 particles prepared by SABM with different milling ball sizes in diameters were investigated systematically. It was showed that the nanoflakes milled by amount of small size balls had a higher coercivity and lower anisotropy, i.e., worse grain orientation although in a short milling time while the nanoflakes prepared with same weight of big balls tend to have a lower coercivity, better grain orientation. The coercivity mechanism of the nanoflake was studied and it was mainly dominated with the domain-wall pinning. The SEM analysis shows that the morphology of nanoflakes prepared with different ball sizes are almost the same when the balls to powder weight ratio is fixed. The different magnetic properties caused by different ball sizes are mainly due to the different microstructure changes, i.e, grain refinement and c-axis orientation, which are demonstrated by X-ray diffraction (XRD) analysis and transmission electron microscope (TEM). Based on the experiments above, a combined milling process was suggested and done to improve magnetic properties as your need. - Highlights: • We fabricated anisotropic magnetic SmCo 5 nanoflakes by surfactant-assisted ball milling (SABM). • We investigated the magnetic properties of SmCo 5 particles systematically. It was showed that the coercivity, high or low, and grain orientation, good or bad, were influenced strongly by balls size. The different magnetisms caused by different ball sizes is mainly due to the different microstructure changes. • The coercivity mechanism of the nanoflake was studied and it was mainly dominated with the domain-wall pinning

  16. Influence of the preparation method on the structure, optical and photocatalytic properties of nanosized ZnO

    Energy Technology Data Exchange (ETDEWEB)

    Gancheva, M., E-mail: mancheva@svr.igic.bas.bg [Institute of General and Inorganic Chemistry, Bulgarian Academy of Science, Acad. G. Bonchev Str., bl.11, 1113, Sofia (Bulgaria); Uzunov, I.; Iordanova, R. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Science, Acad. G. Bonchev Str., bl.11, 1113, Sofia (Bulgaria); Papazova, K. [University of Sofia, Faculty of Chemistry and Pharmacy, James Bourchier 1 Blvd., 1164, Sofia (Bulgaria)

    2015-08-15

    Mechanochemical activation is the most commonly applied approach for improving the photocatalytic properties of commercial zinc oxide. Here we show that ZnO obtained by two-pathway decomposition of basic zinc carbonate also possesses a very good photocatalytic activity. Nanosized ZnO powders were successfully prepared by thermal and mechanochemical decomposition of Zn{sub 5}(CO{sub 3}){sub 2}(OH){sub 6}, precipitated under soft conditions. The precursor and final products were characterized by X-ray diffraction (XRD), thermal analysis (TG/DTA), infrared spectroscopy (IR) and B.E.T method. The morphology of the ZnO was observed by SEM analysis. The optical and photocatalytic properties of the prepared zinc oxides were also investigated and compared with commercial ZnO. The band gaps of the thermal and mechanochemical obtained ZnO nanopowders are 3.22 and 3.04 eV, respectively. The degree of decomposition of Malachite Green under UV and visible irradiations in the presence of ZnO prepared by both methods reached levels above 90%. Better catalytic activity was found for the visible region. It was established that the process follows second order kinetics. - Graphical abstract: Display Omitted - Highlights: • Synthesis of nanosized ZnO from hydrozincite by thermal and mechanochemical route. • ZnO powders possess high photocatalytic activity under UV and visible irradiation. • The degree of decomposition of Malachite Green is more than 90% for the both ZnO's. • The photodecomposition of MG under UV/Vis irradiation follows second order kinetics.

  17. Preparation and structural, optical, magnetic, and electrical characterization of Mn{sup 2+}/Co{sup 2+}/Cu{sup 2+} doped hematite nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Srikrishna Ramya, S.I., E-mail: ramyaskr@gmail.com; Mahadevan, C.K.

    2014-03-15

    Pure and Mn{sup 2+} / Co{sup 2+} / Cu{sup 2+} doped (1 and 2 at.%) spherical hematite (α-Fe{sub 2}O{sub 3})nanocrystals have been synthesized by a simple solvothermal method using a domestic microwave oven. XRD measurements confirm that all the seven nanocrystals prepared consist of nanocrystalline hematite phase without any other phases. The energy dispersive X-ray and Fourier transform infrared spectral analyses confirm the phase purity of the nanocrystals prepared. TEM analysis shows the average particle sizes within the range 33–51 nm. Optical absorption measurements indicate that all the three dopants enhance the optical transmittance and reflectance. A red shift is observed in the bandgap energy values estimated from optical absorption and reflectance spectra. Results of magnetic measurements made at room temperature using a vibrating sample magnetometer indicate significant changes in the magnetic properties (coercivity, retentivity and saturationmagnetization) due to doping. Results of magnetic measurements indicate significant changes in the magnetic properties. Results of AC electrical measurements made at various temperatures in the range 40–130 °C and frequencies in the range 100 Hz –1 MHz indicate low dielectric constants and AC electrical conductivities and consequently show the occurrence of nanoconfined states. -- Graphical abstract: The indexed X-ray diffraction (XRD) patterns of all the seven nanocrystals indicate the rhombohedral structure of hematite (JCPDS card No.13-0534). No impurity phase like oxides of Mn or Co or Cu was detected above equipment limit. The average crystallite (grain) sizes estimated using the Scherrer's formula. Highlights: • Pure and Mn/Co/Cu-doped hematite nanocrystals have been prepared. • The method adopted for the preparation is simple, economical and scalable. • Prepared nanocrystals are spherical in shape with good crystallinity and phase purity. • Mn/Co/Cu-doping enhances the optical

  18. CoFe2O4 nanocrystalline powders prepared by citrate-gel methods: Synthesis, structure and magnetic properties

    International Nuclear Information System (INIS)

    Cannas, C.; Falqui, A.; Musinu, A.; Peddis, D.; Piccaluga, G.

    2006-01-01

    Nanocrystalline CoFe 2 O 4 powders were prepared by decomposition of metal ion citrate precursors. Four samples were synthesized from precursor solutions having different pH values in the range 2 physisorption and Transmission Electron Microscopy. Magnetic properties were explored by a SQUID magnetometer. Three out of the four samples, coming from solutions of pH 2, 4 and 7, were produced by an autocombustion reaction and are very similar as regards average size of the nanoparticles (about 20 nm), their morphology and the magnetic properties, while the fourth sample was produced by a slower thermal decomposition and is composed of smaller nanoparticles (about 10 nm)

  19. Enantioselective semi-preparative HPLC separation of PCB metabolites and their absolute structures determined by electronic and vibrational circular dichroism

    Energy Technology Data Exchange (ETDEWEB)

    Tuan, H.P.; Larsson, C.; Huehnerfuss, H. [Hamburg Univ. (Germany). Inst. fuer Organische Chemie; Hoffmann, F.; Froeba, M. [Giessen Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie; Bergmann, Aa. [Stockholm Univ. (Sweden). Dept. of Environmental Chemistry

    2004-09-15

    The present paper represents a first result of an ongoing systematic study of atropisomeric methylsulfonyl, methylthionyl, hydroxy, and methoxy metabolites of environmentally most relevant PCBs. This involves semi-preparative enantioselective HPLC separation to obtain pure atropisomers from synthesized PCB metabolite standards, their configuration estimation using the electronic circular dichroism (UV-CD) method and the determination / confirmation of these absolute configurations applying the combined vibrational circular dichroism (VCD) / ab initio approach. The following substances have been investigated: 4-HO-, 4-MeO-, 4-MeS-, 4-MeSO2-, 3-MeS- and 3-MeSO{sub 2}-CB149.

  20. Synthesis and structure of Na-Li-Si-Al-P-O-N glasses prepared by melt nitridation using NH3

    International Nuclear Information System (INIS)

    Kidar, A.; Pomeroy, M.J.; Hampshire, S.; Mercier, C.; Leriche, A.; Revel, B.

    2012-01-01

    Na-Li-Si-Al-P-O-N glasses have been prepared by nitridation of a pre-synthesized Na 2 O-Li 2 O-SiO 2 -P 2 O 5 -Al 2 O 3 glass under anhydrous ammonia. Nitrogen for oxygen substitution increases the network connectivity leading to increases in microhardness and glass transition temperature. Raman and 31 P MAS-NMR spectroscopy indicate sequential nitridation reactions forming PO 3 N and PO 2 N 2 species. The data collected so far show no evidence of N/O substitutions in the silicate sub-network. (authors)

  1. Laser-induced particle size tuning and structural transformations in germanium nanoparticles prepared by stain etching and colloidal synthesis route

    Energy Technology Data Exchange (ETDEWEB)

    Karatutlu, Ali, E-mail: a.karatutlu@qmul.ac.uk, E-mail: ali.karatutlu@bou.edu.tr [Centre for Condensed Matter and Materials Physics, School of Physics and Astronomy, Queen Mary, University of London, London E1 4NS (United Kingdom); Electrical and Electronics Engineering, Bursa Orhangazi University, 16310 Yıldırım/Bursa (Turkey); Little, William; Ersoy, Osman; Zhang, Yuanpeng; Sapelkin, Andrei [Centre for Condensed Matter and Materials Physics, School of Physics and Astronomy, Queen Mary, University of London, London E1 4NS (United Kingdom); Seker, Isa [Bio-Nanotechnology Research and Development Centre, Fatih University, 34500 Buyukcekmece, Istanbul (Turkey)

    2015-12-28

    In this study, with the aid of Raman measurements, we have observed transformations in small (∼3 nm and ∼10 nm) free-standing Ge nanoparticles under laser light exposure. The nanoparticles were obtained by the chemical stain etching of a monocrystalline Ge wafer and of Ge powder and by colloidal synthesis route. We found that the transformation path depends on laser power and exposure time. At relatively low values of the laser power (2 mW) over a period of 100 min, the Raman signal indicates transformation of the sample from a nanocrystaline to bulk-like state, followed by partial oxidation and finally a conversion of the entire sample into alpha-quartz type GeO{sub 2}. However, when the laser power is set at 60 mW, we observed a heat release during an explosive crystallization of the nanocrystalline material into bulk Ge without noticeable signs of oxidation. Together with the transmission electron microscopy measurements, these results suggest that the chemical stain etching method for the preparation of porous Ge may not be a top-down process as has been widely considered, but a bottom up one. Systematic studies of the laser exposure on Ge nanoparticles prepared by colloidal synthesis results in the fact that the explosive crystallisation is common for H-terminated and partially disordered Ge nanoparticles regardless of its particle size. We suggest possible bio-medical applications for the observed phenomena.

  2. Structural and optical properties of {beta}-FeSi{sub 2}/Si(100) prepared by laser ablation method

    Energy Technology Data Exchange (ETDEWEB)

    Kakemoto, H; Makita, Y; Obara, A; Tsai, Y; Sakuragi, S; Ando, S; Tsukamoto, T

    1997-07-01

    {beta}-FeSi{sub 2} is a promising material for the application of various electronic, optoelectronic and energy devices. The authors present here the semiconducting properties of {beta}-FeSi{sub 2} films on Si(100) substrate prepared by laser ablation method. Samples were grown using poly-crystalline bulk {beta}-FeSi{sub 2} prepared by horizontal gradient freeze method. For the monitoring of growth, in-situ observation of ablation plume was made through fluorescence spectroscopy. Reflection of high-energy electron beam diffraction (RHEED) was also made in-situ to see the surface morphology. Characterization of the films by X-ray diffraction presented purely {beta}(220) orientation. Raman scattering measurements at room temperature also indicated that the grown films are semiconducting {beta}-FeSi{sub 2}. Optical absorption spectra at room temperature showed absorption coefficient higher than 10{sup 5} cm{sup {minus}1} above the band-gap ({approximately}1.2 eV). It was revealed that high quality semiconducting {beta}-FeSi{sub 2} films can be fabricated by laser ablation method without post-annealing.

  3. Matrix-assisted laser desorption/ionization sample preparation optimization for structural characterization of poly(styrene-co-pentafluorostyrene) copolymers

    International Nuclear Information System (INIS)

    Tisdale, Evgenia; Kennedy, Devin; Wilkins, Charles

    2014-01-01

    Graphical abstract: -- Highlights: •We optimized sample preparation for MALDI TOF poly(styrene-copentafluorostyrene) co-polymers. •Influence of matrix choice was investigated. •Influence of matrix/analyte ratio was examined. •Influence of analyte/salt ratio (for Ag+ salt) was studied. -- Abstract: The influence of the sample preparation parameters (the choice of the matrix, matrix:analyte ratio, salt:analyte ratio) was investigated and optimal conditions were established for the MALDI time-of-flight mass spectrometry analysis of the poly(styrene-co-pentafluorostyrene) copolymers. These were synthesized by atom transfer radical polymerization. Use of 2,5-dihydroxybenzoic acid as matrix resulted in spectra with consistently high ion yields for all matrix:analyte:salt ratios tested. The optimized MALDI procedure was successfully applied to the characterization of three copolymers obtained by varying the conditions of polymerization reaction. It was possible to establish the nature of the end groups, calculate molecular weight distributions, and determine the individual length distributions for styrene and pentafluorostyrene monomers, contained in the resulting copolymers. Based on the data obtained, it was concluded that individual styrene chain length distributions are more sensitive to the change in the composition of the catalyst (the addition of small amount of CuBr 2 ) than is the pentafluorostyrene component distribution

  4. Matrix-assisted laser desorption/ionization sample preparation optimization for structural characterization of poly(styrene-co-pentafluorostyrene) copolymers

    Energy Technology Data Exchange (ETDEWEB)

    Tisdale, Evgenia; Kennedy, Devin; Wilkins, Charles, E-mail: cwilkins@uark.edu

    2014-01-15

    Graphical abstract: -- Highlights: •We optimized sample preparation for MALDI TOF poly(styrene-copentafluorostyrene) co-polymers. •Influence of matrix choice was investigated. •Influence of matrix/analyte ratio was examined. •Influence of analyte/salt ratio (for Ag+ salt) was studied. -- Abstract: The influence of the sample preparation parameters (the choice of the matrix, matrix:analyte ratio, salt:analyte ratio) was investigated and optimal conditions were established for the MALDI time-of-flight mass spectrometry analysis of the poly(styrene-co-pentafluorostyrene) copolymers. These were synthesized by atom transfer radical polymerization. Use of 2,5-dihydroxybenzoic acid as matrix resulted in spectra with consistently high ion yields for all matrix:analyte:salt ratios tested. The optimized MALDI procedure was successfully applied to the characterization of three copolymers obtained by varying the conditions of polymerization reaction. It was possible to establish the nature of the end groups, calculate molecular weight distributions, and determine the individual length distributions for styrene and pentafluorostyrene monomers, contained in the resulting copolymers. Based on the data obtained, it was concluded that individual styrene chain length distributions are more sensitive to the change in the composition of the catalyst (the addition of small amount of CuBr{sub 2}) than is the pentafluorostyrene component distribution.

  5. Possible detection and preparation for exploratory drilling of new local structures in the Shatlyk-tedzhenskiy gas region

    Energy Technology Data Exchange (ETDEWEB)

    Tachmuradov, B.M.; Orazkuliyev, K.G.; Zargaryants, I.G.

    1981-01-01

    Based on an analysis of geological-geophysical materials, new positive structural forms are outlined within the highly promising Shatlyk-Tedzhenskiy gas region. They are of practical importance for setting up exploratory drilling.

  6. Characterization of nephelium mutabile blume-like structure of carbon nanotubes prepared from palm oil by CVD method

    Science.gov (United States)

    Maryam, M.; Shamsudin, M. S.; Rusop, M.

    2017-09-01

    A new structure of carbon nanotube was produced from the Single furnace Aerosol-assisted Catalytic CVD (SFAACVD) method using Palm Oil (PO) as the precursor and Ferrocene (Fe) as the catalyst. A nephelium mutabile blume (rambutan)-like structure of CNTs was found from the black substance collected from the Alumina boat substrate placed inside the furnace. Temperature of furnace which was heated at 600 °C - 800 °C plays an important role in determining the formation of structure. The formation rambutan-like structure of CNTs was optimized at 700 °C and the samples collected were characterized by Field Emission Scanning Electron Microscope (FE-SEM) to obtain the surface morphologies. Raman Spectroscopy (RS) and Thermogravimetric Analysis (TGA) were then used to further study the Raman Spectra and purity of samples.

  7. Preparation and wear behavior of polymer matrix composites with an interpenetrating network structure derived from natural sponge

    International Nuclear Information System (INIS)

    Wang Tianchi; Zhou Tianle; Xiong Dangsheng

    2010-01-01

    Natural sponge was used as a template to produce carbon/epoxy resin and (carbon+silicon carbide)/epoxy resin composites with interpenetrating network structures. Carbon with a network structure was first obtained by pyrolysis of the natural sponge. The composites were then obtained by injecting epoxy resin and silicone resin into the carbon. Their microstructures and wear properties were analyzed. The results show that the natural structure of sponge controlled the interpenetrating network structures of the composites. The netlike carbon in the composites reduced the wear rate of the epoxy resin. Compared with the carbon/epoxy resin composite, the (carbon+silicon carbide)/epoxy resin composite shows better wear resistance.

  8. Preparation and Characterization of Cyanocobalamin (Vit B12 Microemulsion Properties and Structure for Topical and Transdermal Application

    Directory of Open Access Journals (Sweden)

    Anayatollah Salimi

    2013-07-01

    This study showed that both microemulsions provided good solubility of Vit B12 with a wide range of internal structure. Low water solubilization capacity is a common property of microemulsions that can affect drug release and permeability through the skin. Based on Vit B12 properties, specially, intermediate oil and water solubility, better drug partitioning into the skin may be obtained by traditional formulations with wide range of structure and high amount of free and bounded water.

  9. Structural and Optical Properties of ZnO Thin Film Prepared by Oxidation of Zn Metal Powders

    International Nuclear Information System (INIS)

    Hassan, N.K.; Hashim, M.R.

    2013-01-01

    High quality ZnO nano structures have been fabricated at room temperature by a simple vacuum thermal evaporator from metallic Zn powders (99.999 % purity) on a silicon (100) substrate. The Zn thin films were then transferred into a thermal tube furnace for oxidation at 700 degree Celsius for different time durations. Time was found to be a critical factor in the synthesis. This was followed by characterization of their morphological, structural and optical properties. The morphology of the grown ZnO nano structures exhibited several large grains, which increased gradually with increasing oxidation time. The crystallinity of the grown nano structures was investigated using X-ray diffraction, revealing that the synthesized ZnO was in hexagonal wurtzite phase. The photoluminescence (PL) spectra of the fabricated ZnO nano structures showed high intensity peak in the UV region due to near-band-edge (NBE) emission in which the structures oxidized for 30 min showing highest intensity. (author)

  10. The strain effect in the surface barrier structures prepared on the basis of n-Si and p-Si

    International Nuclear Information System (INIS)

    Mamatkarimov, O.O.; Tuychiev, U.A.

    2004-01-01

    Full text: One of the ways of creation of large deformations in small volume of the semiconductor is the deformation created by a needle. At insignificant change of external influence the large deformation under a needle in small volume of the semiconductor the significant change of electrophysical parameters of the semiconductor in small volume is created. Therefore, in the present work the results of researches of local pressure influence on physical properties of surface barrier structures has been performed on the basis of silicon with Ni and Mn impurity. The relative changes of a direct current made on the basis n-Si and p-Si from a different degree of compensation are given depending on size of local pressure are shown. Change of current in structures Au-Si -Sb with specific resistance of base ρ=80 Ω·cm and ρ=200 Ω·cm are I p /I 0 =3-3.5 times and I P /I ) =2-2.5 times at pressure P=1.6·10 8 Pa respectively. These data show, that in structures received on the basis of initial silicon, change of a direct current with pressure is in inverse proportion to size of resistance of base of the diode. And in structures Au-Si -Sb with specific resistance of base ρ=5·10 2 Ω·cm and ρ=3·10 3 Ω·cm these changes accordingly are I P /I 0 =7 and I P /I 0 =14. Changes of direct current relative to initial value for structures on the basis p-Si with specific resistance ρ=7·10 2 Ω·cm and ρ=4·10 3 Ω·cm) are I P /I 0 =9 and I P /I 0 =16 respectively. The same changes of direct current of structures on the basis P-Si at local pressure are I P /I 0 =2-2.5. The given values I P /I 0 testify that as in structures Au-Si -Sb, and structures Sb-p-Si -Au, unlike structures on the basis of initial silicon, the values I P /I 0 are increased with increase of specific resistance of base of structures

  11. Automated microfluidic sample-preparation platform for high-throughput structural investigation of proteins by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Nielsen, Søren Skou

    2011-01-01

    A new microfluidic sample-preparation system is presented for the structural investigation of proteins using small-angle X-ray scattering (SAXS) at synchrotrons. The system includes hardware and software features for precise fluidic control, sample mixing by diffusion, automated X-ray exposure...... control, UV absorbance measurements and automated data analysis. As little as 15 l of sample is required to perform a complete analysis cycle, including sample mixing, SAXS measurement, continuous UV absorbance measurements, and cleaning of the channels and X-ray cell with buffer. The complete analysis...

  12. Convenient preparation of high molecular weight poly(dimethylsiloxane using thermally latent NHC-catalysis: a structure-activity correlation

    Directory of Open Access Journals (Sweden)

    Stefan Naumann

    2015-11-01

    Full Text Available The polymerization of octamethylcyclotetrasiloxane (D4 is investigated using several five-, six- and seven-membered N-heterocyclic carbenes (NHCs. The catalysts are delivered in situ from thermally susceptible CO2 adducts. It is demonstrated that the polymerization can be triggered from a latent state by mild heating, using the highly nucleophilic 1,3,4,5-tetramethylimidazol-2-ylidene as organocatalyst. This way, high molecular weight PDMS is prepared (up to >400 000 g/mol, 1.6 ÐM 95%, using low catalyst loadings (0.2–0.1 mol %. Furthermore, the results suggest that a nucleophilic, zwitterionic mechanism is in operation, in preference to purely anionic polymerization.

  13. Preparation and structure characterization of SmCo5(0001) epitaxial thin films grown on Cu(111) underlayers

    International Nuclear Information System (INIS)

    Ohtake, Mitsuru; Nukaga, Yuri; Futamoto, Masaaki; Kirino, Fumiyoshi

    2009-01-01

    SmCo 5 (0001) epitaxial films were prepared on Cu(111) single-crystal underlayers formed on Al 2 O 3 (0001) substrates at 500 deg. C. The nucleation and growth mechanism of (0001)-oriented SmCo 5 crystal on Cu(111) underlayer is investigated and a method to control the nucleation is proposed. The SmCo 5 epitaxial thin film formed directly on Cu underlayer consists of two types of domains whose orientations are rotated around the film normal by 30 deg. each other. By introducing a thin Co seed layer on the Cu underlayer, a SmCo 5 (0001) single-crystal thin film is successfully obtained. Nucleation of SmCo 5 crystal on Cu underlayer seems controllable by varying the interaction between the Cu underlayer and the SmCo 5 layer

  14. Influences of ambient gases on the structure and the composition of calcium phosphate films prepared by pulsed laser deposition

    International Nuclear Information System (INIS)

    Kim, Hye-Lee; Kim, Young-Sun; Kim, Dae-Joon; Lee, Won-Jun; Han, Jung-Suk

    2006-01-01

    Calcium phosphate films were prepared by using a pulsed KrF-laser deposition (PLD) method with a hydroxyapatite target in various ambient gases, such as Ar, O 2 and H 2 O. The influence of the ambient gas on the properties of the deposited films was investigated. The chamber pressure and the substrate temperature were fixed at 0.25 Torr and 600 .deg. C, respectively. Calcium-rich amorphous calcium phosphate films were deposited with a low density in Ar due to the preferential resputtering of phosphorus from the growing film. In an O 2 ambient, the density and the Ca/P ratio of the films were similar to those of the target. However, the deposited film was amorphous calcium phosphate and did not contain OH - groups. Polycrystalline hydroxyapatite films can be deposited in a H 2 O ambient because a sufficient supply of OH - groups from the ambient gas is essential for the growth of a hydroxyapatite film.

  15. Structural, optical and photocatalytic properties of flower-like ZnO nanostructures prepared by a facile wet chemical method

    Directory of Open Access Journals (Sweden)

    Sini Kuriakose

    2013-11-01

    Full Text Available Flower-like ZnO nanostructures were synthesized by a facile wet chemical method. Structural, optical and photocatalytic properties of these nanostructures have been studied by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, photoluminescence (PL and UV–vis absorption spectroscopy. SEM and TEM studies revealed flower-like structures consisting of nanosheets, formed due to oriented attachment of ZnO nanoparticles. Flower-like ZnO structures showed enhanced photocatalytic activity towards sun-light driven photodegradation of methylene blue dye (MB as compared to ZnO nanoparticles. XRD, UV–vis absorption, PL, FTIR and TEM studies revealed the formation of Zn(OH2 surface layer on ZnO nanostructures upon ageing. We demonstrate that the formation of a passivating Zn(OH2 surface layer on the ZnO nanostructures upon ageing deteriorates their efficiency to photocatalytically degrade of MB.

  16. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    International Nuclear Information System (INIS)

    Min, Sa Hoon; Jang, Jyongsik; Lee, Kyung Jin; Bae, Joonwon

    2013-01-01

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol–gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant. (paper)

  17. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    Energy Technology Data Exchange (ETDEWEB)

    Min, Sa Hoon; Jang, Jyongsik; Lee, Kyung Jin [School of Chemical and Biological Engineering, College of Engineering, Seoul National University, Shinlimdong 56-1, Seoul, 151-742 (Korea, Republic of); Bae, Joonwon [Department of Applied Chemistry, Dongduk Women' s University, Seoul 136-714 (Korea, Republic of)

    2013-06-28

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol-gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant. (paper)

  18. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    Science.gov (United States)

    Min, Sa Hoon; Bae, Joonwon; Jang, Jyongsik; Lee, Kyung Jin

    2013-06-01

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol-gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant.

  19. Structural and optical properties of Tb and Na-Tb co-doped Ca3V2O8 phosphors prepared by sol-gel process

    Science.gov (United States)

    Parab, Shambhu S.; Salker, A. V.

    2018-01-01

    A malic acid assisted sol-gel route was successfully employed to prepare two distinct series of green emitting Ca3V2O8 phosphors. In the first series, Tb was solely doped whereas in the second series Na and Tb were doped simultaneously in the Ca3V2O8 crystal lattice. X-ray diffraction studies proved the utility of adopted preparative method by confirming the monophasic formation of all compounds from both the series. Spectral analysis like Raman spectroscopy, UV-DRS were undertaken to analyse the local structure, crystallinity and absorptive characteristics. XPS validated the presence of desired oxidation states of all the elements present. Finally, photoluminescence studies were done to elucidate the scope of prepared compounds as green emitting phosphors and also to understand the effect of both doping schemes on the luminescence. Intense green emission was observed in both the cases. Tb concentration of 0.08 was found to be optimum in case of Tb singly doped compounds whereas Tb = 0.12 showed highest intensity among the Na-Tb co-doped samples. Moreover, a red shift in the excitation wavelength was observed after Na doping signifying a change in the local electronic environment which in turn has affected the luminescence pattern. Local crystallinity and vacancy concentrations were found to have a major say on the emission intensities.

  20. Effects of ZnO Seed Layers Prepared with Various Precursor Concentrations on Structural and Defect Emission Properties of ZnO Nanorods Grown by Hydrothermal Method

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Soaram; Nam, Giwoong; Leem, Jae-Young; Kim, Yangsoo [Inje University, Gimhae (Korea, Republic of); Kim, Ghun Sik; Yoon, Sung Pil [Korea Institute of Science and Technology, Seoul (Korea, Republic of)

    2013-07-15

    ZnO nanorods were grown by a hydrothermal method on ZnO seed layers that had previously been prepared from solutions containing various precursor concentrations. The effects of the ZnO seed layers prepared with various precursor concentrations on the structural and defect emissions of the ZnO nanorods were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), and photoluminescence (PL) spectroscopy. The surface morphology of the ZnO seed layers changed with an increasing precursor concentration, and the diameters and densities of the ZnO nanorods depended on the morphologies of the ZnO seed layers. The ZnO seed layers prepared with various precursor concentrations affected the residual stress in the nanorods grown on the seed layers, the intensity and full widths at half maximum of the 2-theta angle in the XRD spectra for the nanorods, and the intensity and position of the defect emission peak in deep-level emission (DLE) PL spectra for the ZnO nanorods.

  1. Structure and phase transition of BiFeO{sub 3} cubic micro-particles prepared by hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Jian-Ping, E-mail: zhoujp@snnu.edu.cn [College of Physics and Information Technology, Shaanxi Normal University, Xi’an 710062 (China); Yang, Ruo-Lin; Xiao, Rui-Juan; Chen, Xiao-Ming [College of Physics and Information Technology, Shaanxi Normal University, Xi’an 710062 (China); Deng, Chao-Yong [Department of Electronic Science, Guizhou University, Guizhou Guiyang 550025 (China)

    2012-11-15

    Graphical abstract: Bismuth ferrite (BiFeO{sub 3}) cubic micro-particles with smooth surfaces were synthesized. BiFeO{sub 3} has a hexagonal perovskite structure with a space group R3c below 370 °C and rhombohedral perovskite structure with a space group R3m below 755 °C, undergoes a phase transition in the temperature range of 755–817 °C to a cubic structure, then decompose to liquid and Fe{sub 2}O{sub 3} above 939 °C. Highlights: ► BiFeO{sub 3} micro-particles with smooth surface were synthesized by hydrothermal method. ► BiFeO{sub 3} enjoys hexagonal structure with well element ratio and chemical valence. ► BiFeO{sub 3} transition from rhombohedral phase to cubic phase lasts 60 °C. -- Abstract: Single-phase bismuth ferrite (BiFeO{sub 3}) powders were synthesized with a hydrothermal method by controlling the experimental conditions carefully. The powder structure, morphology and composition were characterized by using X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscope, Raman measurement and X-ray photoelectron spectroscopy. The particles change from irregular agglomerations to regular cubes with increasing KOH concentration. The large BiFeO{sub 3} cubic particles enjoy much smooth surfaces with well-matched element ratio (Bi:Fe:O = 1:1:3) and chemical valence (Bi{sup 3+}, Fe{sup 3+} and O{sup 2−}). The high temperature XRD and differential scanning calorimetry show that BiFeO{sub 3} powders have a hexagonal perovskite structure with a space group R3c below 370 °C and a rhombohedral structure with a space group R3m below 755 °C. BiFeO{sub 3} undergoes a phase transition in the temperature range of 755–817 °C from rhombohedral structure to a cubic phase, then decomposes to liquid and Fe{sub 2}O{sub 3} above 939 °C.

  2. Structure and phase transition of BiFeO3 cubic micro-particles prepared by hydrothermal method

    International Nuclear Information System (INIS)

    Zhou, Jian-Ping; Yang, Ruo-Lin; Xiao, Rui-Juan; Chen, Xiao-Ming; Deng, Chao-Yong

    2012-01-01

    Graphical abstract: Bismuth ferrite (BiFeO 3 ) cubic micro-particles with smooth surfaces were synthesized. BiFeO 3 has a hexagonal perovskite structure with a space group R3c below 370 °C and rhombohedral perovskite structure with a space group R3m below 755 °C, undergoes a phase transition in the temperature range of 755–817 °C to a cubic structure, then decompose to liquid and Fe 2 O 3 above 939 °C. Highlights: ► BiFeO 3 micro-particles with smooth surface were synthesized by hydrothermal method. ► BiFeO 3 enjoys hexagonal structure with well element ratio and chemical valence. ► BiFeO 3 transition from rhombohedral phase to cubic phase lasts 60 °C. -- Abstract: Single-phase bismuth ferrite (BiFeO 3 ) powders were synthesized with a hydrothermal method by controlling the experimental conditions carefully. The powder structure, morphology and composition were characterized by using X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscope, Raman measurement and X-ray photoelectron spectroscopy. The particles change from irregular agglomerations to regular cubes with increasing KOH concentration. The large BiFeO 3 cubic particles enjoy much smooth surfaces with well-matched element ratio (Bi:Fe:O = 1:1:3) and chemical valence (Bi 3+ , Fe 3+ and O 2− ). The high temperature XRD and differential scanning calorimetry show that BiFeO 3 powders have a hexagonal perovskite structure with a space group R3c below 370 °C and a rhombohedral structure with a space group R3m below 755 °C. BiFeO 3 undergoes a phase transition in the temperature range of 755–817 °C from rhombohedral structure to a cubic phase, then decomposes to liquid and Fe 2 O 3 above 939 °C.

  3. Quaternary chalcogenides of the IVa metals with layered structures: preparation and crystal structures of TlCuTIVQ3 (T=Zr, Hf; Q=S, Se) and their relation to the Re3B structure type

    International Nuclear Information System (INIS)

    Klepp, K.O.; Gurtner, D.

    1996-01-01

    The new compounds TlCuT IV Q 3 (T = Zr, Hf; Q = S, Se) were prepared by reacting intimate mixtures of Tl 2 S or TlSe with stoichiometric amounts of the corresponding Group IV metal, Cu and the corresponding chalcogen at 870 . The four compounds are isostructural and crystallize in Cmcm, Z = 4 with a 3.726(4) A, b = 13.987(9) A, c = 9.783(4) A for TlCuZrS 3 ; a = 3.847(1) A, b 14.381(6) A, c = 10.150(1) A for TlCuZrSe 3 ; a = 3.694(1) A, b = 14.030(3) A, c = 9.750(3) A for TlCuHfS 3 ; and a = 3.831(1) A, b = 14.409(9) A, c = 10.124(2) A for TlCuHfSe 3 . Their crystal structures were determined from single crystal diffractometer data (Mo Kα radiation, ambient temperature) and refined to conventional R values of 0.016, 0.040, 0.019 and 0.031 respectively. An outstanding feature of their crystal structures is the formation of infinite anionic layers, 2 ∞ -[CuT IV Q 3 ] - parallel to (010), which are separated by Tl + cations. These layers are built up by edge sharing TQ 6 octahedra and distorted CuQ 4 tetrahedra. Average T-Q distances are anti d(Zr-S) = 2.586(1) A, anti d(Zr-Se) = 2.707(1) A, anti d(Hf-S) = 2.569(2) A and anti d(Hf-Se) = 2.694(1) A. Cu-chalcogen distances are anti d(Cu-S) = 2.318(2) A and anti d(Cu-Se) = 2.432(3) A respectively. The thallium ions are in bicapped trigonal prismatic chalcogen coordinations. The atomic arrangement corresponds to that of KCuZrS 3 ; based on the thallium-chalcogen partial structure it can be regarded as a filled variant of an anti-Re 3 B structure type. (orig.)

  4. Preparation, structural, dielectric and magnetic properties of LaFeO3-PbTiO3 solid solutions

    Czech Academy of Sciences Publication Activity Database

    Ivanov, S. A.; Tellgren, R.; Porcher, F.; Ericsson, T.; Mosunov, A.; Beran, Přemysl; Korchagina, S. K.; Kumar, P.; Mathieu, R.; Nordblad, P.

    2012-01-01

    Roč. 47, č. 11 (2012), s. 3253-3268 ISSN 0025-5408 Institutional support: RVO:61389005 Keywords : ceramics * electronic materials * neutron scattering * X-ray diffraction * crystal structure * magnetic properties Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.913, year: 2012

  5. Atomic-Scale Structure of Al2O3-ZrO2 Mixed Oxides Prepared by Laser Ablation

    International Nuclear Information System (INIS)

    Yang Xiuchun; Dubiel, M.; Hofmeister, H.; Riehemann, W.

    2007-01-01

    By means of x-ray diffractometry (XRD) and X-ray absorption fine structure spectroscopy, the phase composition and atomic structure of laser evaporated ZrO2 and ZrO2-Al2O3 nanopowders have been studied. The results indicate that pure ZrO2 exists in the form of tetragonal structure, Al2O3 doped ZrO2 nanoparticles, however, have cubic structure. Compared to bulk tetragonal ZrO2, pure tetragonal ZrO2 nanoparticles have a shorter Zr-O- and Zr-Zr shell, indicating that the lattice contracts with decreasing particle size. For Al2O3 doped ZrO2 solid solution, the distances of first Zr-O and Zr-Zr (Al) coordination decrease with increasing solid solubility. The disorder degree of the ZrO2 lattice increases with increasing solid solubility. The coevaporated ZrO2-Al2O3 is quickly solidified into amorphous phase when it is ablated in a higher pressure. The amorphous phase contains Zr-O-Zr (Al) clusters and has shorter Zr-O distance and tower Zr-O coordination number

  6. Composites prepared from the waterborne polyurethane cationomers-modified graphene. Part I. Synthesis, structure, and physicochemical properties

    Czech Academy of Sciences Publication Activity Database

    Król, P.; Król, B.; Pielichowska, K.; Špírková, Milena

    2015-01-01

    Roč. 293, č. 2 (2015), s. 421-431 ISSN 0303-402X R&D Projects: GA ČR(CZ) GA13-06700S Institutional support: RVO:61389013 Keywords : polyurethane films * surface structure * AFM microscopy Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.890, year: 2015

  7. Effect of preparation conditions on fractal structure and phase transformations in the synthesis of nanoscale M-type barium hexaferrite

    Energy Technology Data Exchange (ETDEWEB)

    Pashkova, E.V. [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine); Solovyova, E.D., E-mail: solovyovak@mail.ru [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine); Kotenko, I.E., E-mail: Hab2420@yahoo.com [National Technical University of Ukraine ' KPI' , Pr. Pobedy, 37, Kyiv-57 (Ukraine); Kolodiazhnyi, T.V., E-mail: kolodiazhnyi.taras@nims.go.jp [National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Belous, A.G., E-mail: belous@ionc.kar.net [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine)

    2011-10-15

    The conditions of the synthesis of carbonate-hydroxide precursors (pH of FeOOH precipitation and heat treatment regimes) were studied in terms of their effect on the fractal structure and physical-chemical properties of precursors. Phase transformations which occur during the synthesis of nanosize M-type barium hexaferrite (BHF) were studied as well. The first structural level of precursors' aggregation for mass fractals, the correlation between fractal dimension and precursors' activity during the synthesis of BHF were determined. Synthesis parameters for the precursors with the optimal fractal structure were determined. These data permit an enhancement of the filtration coefficient of the precipitates by a factor of 4-5, obtaining substantial decrease in the temperature required for synthesis of a single-phase BHF, and monodispersed plate-like nanoparticles (60 nm diameter) with the shape anisotropy and good magnetic characteristics (saturation magnetization (M{sub s})=68,7 emu/g and coercitivity (H{sub c})=5440 Oe). - Highlights: > The nanosize M-type BHF obtained by precipitation of hydroxicarbonates technique. > Optimal fractal structure of a precursor for nanosize M-type BHF has been determined. > The precursor precipitated at pH 4.3 allows getting monodisperse particles of BHF.

  8. Size-dependent magnetic and structural properties of CoCrFeO4 nano-powder prepared by solution self-combustion

    Science.gov (United States)

    Sijo, A. K.; Dutta, Dimple P.

    2018-04-01

    The study reports the tuning of magnetic and structural properties of nano-sized CoCrFeO4 via post-annealing treatment. CoCrFeO4 nano-powder has been prepared by solution self-combustion method. The structural and magnetic properties have been studied over a range of annealing temperatures (300-900 °C). The formation of the phase pure CoCrFeO4 spinel has been confirmed from powder XRD analysis. The crystallite size is observed to increase with an increase in annealing temperature. On annealing, the value of magnetic parameters-remanence, coercivity and saturation magnetization have enhanced. All the samples exhibit irreversibility at low-temperature measurements.

  9. The effect of O2 partial pressure on the structure and photocatalytic property of TiO2 films prepared by sputtering

    International Nuclear Information System (INIS)

    Liu Baoshun; Zhao Xiujian; Zhao Qingnan; Li Chunling; He Xin

    2005-01-01

    The TiO 2 films were prepared on slide substrates by dc reactive magnetron sputtering at different oxygen partial pressure, and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and Fourier transform infrared spectrometry (FT-IR). The degradation of methyl orange aqueous solutions was used to evaluate the photocatalytic activity. The results show that all films show crystalline anatase structure irrespective of oxygen partial pressure. The surface oxygen element exists in three forms, the first one is TiO 2 , the second one is OH - and the last one is physical absorbed water. The films deposited at oxygen partial pressure of 0.035 and 0.040 mTorr present better photocatalytic activity, which shows clear tendency to increase with oxygen partial pressure. Such photocatalytic activity results are considered to correlate with the crystalline structure, grain sizes and the OH - concentration

  10. Structural and magnetic properties of Fe{sub 60}Al{sub 40} alloys prepared by means of a magnetic mill

    Energy Technology Data Exchange (ETDEWEB)

    Bernal-Correa, R. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Rosales-Rivera, A., E-mail: arosalesr@unal.edu.c [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Pineda-Gomez, P. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia); Universidad de Caldas, Manizales (Colombia); Salazar, N.A. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Manizales (Colombia)

    2010-04-16

    A study on synthesis, structural and magnetic characterization of Fe{sub 60}Al{sub 40} (at.%) alloys prepared by means of mechanical alloying process is presented. The mechanical alloying was performed using a milling device with magnetically controlled ball movement (Uni-Ball-Mill 5 equipment) at several milling times. The characterization was carried out via X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The effects of milling time on the structural state, morphological evolution and magnetic behaviour of the Fe{sub 60}Al{sub 40} (at.%) alloys are discussed. Besides, in this current study we emphasize the result that indicating a ferro-para-ferromagnetic transition from a correlation between X-ray diffraction and magnetization data.

  11. Structural and optical properties of Co-doped ZnO nanocrystallites prepared by a one-step solution route

    International Nuclear Information System (INIS)

    Li Ping; Wang Sha; Li Jibiao; Wei Yu

    2012-01-01

    Zinc oxide (ZnO) nanocrystallites with different Co-doping levels were successfully synthesized by a simple one-step solution route at low temperature (95 deg. C) in this study. The structure and morphology of the samples thus obtained were characterized by XRD, EDS, XPS and FESEM. Results show that cobalt ions, in the oxidation state of Co 2+ , replace Zn 2+ ions in the ZnO lattice without changing its wurtzite structure. The dopant content varies from 0.59% to 5.39%, based on Co-doping levels. The pure ZnO particles exhibit well-defined 3D flower-like morphology with an average size of 550 nm, while the particles obtained after Co-doping are mostly cauliflower-like nanoclusters with an average size of 120 nm. Both the flower-like pure ZnO and the cauliflower-like Co:ZnO nanoclusters are composed of densely arrayed nanorods. The optical properties of the ZnO nanocrystallites following Co-doping were also investigated by UV-Visible absorption and Photoluminescence spectra. Our results indicate that Co-doping can change the energy-band structure and effectively adjust the luminescence properties of ZnO nanocrystallites. - Highlights: → Co-doped ZnO nanocrystallites were synthesized via a simple one-step solution route. → Co 2+ ions incorporated into the ZnO lattice without changing its wurtzite structure. → Co-doping changed the energy band structure of ZnO. → Co-doping effectively adjusted the luminescence properties of ZnO nanocrystallites.

  12. Structural and optical properties of Co-doped ZnO nanocrystallites prepared by a one-step solution route

    Energy Technology Data Exchange (ETDEWEB)

    Li Ping, E-mail: lipingchina@yahoo.com.cn [Provincial Key Laboratory of Inorganic Nanomaterials, School of Chemistry and Materials Science, Hebei Normal University, 113 Yuhua Road, Shijiazhuang 050016, Hebei (China); Wang Sha; Li Jibiao; Wei Yu [Provincial Key Laboratory of Inorganic Nanomaterials, School of Chemistry and Materials Science, Hebei Normal University, 113 Yuhua Road, Shijiazhuang 050016, Hebei (China)

    2012-01-15

    Zinc oxide (ZnO) nanocrystallites with different Co-doping levels were successfully synthesized by a simple one-step solution route at low temperature (95 deg. C) in this study. The structure and morphology of the samples thus obtained were characterized by XRD, EDS, XPS and FESEM. Results show that cobalt ions, in the oxidation state of Co{sup 2+}, replace Zn{sup 2+} ions in the ZnO lattice without changing its wurtzite structure. The dopant content varies from 0.59% to 5.39%, based on Co-doping levels. The pure ZnO particles exhibit well-defined 3D flower-like morphology with an average size of 550 nm, while the particles obtained after Co-doping are mostly cauliflower-like nanoclusters with an average size of 120 nm. Both the flower-like pure ZnO and the cauliflower-like Co:ZnO nanoclusters are composed of densely arrayed nanorods. The optical properties of the ZnO nanocrystallites following Co-doping were also investigated by UV-Visible absorption and Photoluminescence spectra. Our results indicate that Co-doping can change the energy-band structure and effectively adjust the luminescence properties of ZnO nanocrystallites. - Highlights: > Co-doped ZnO nanocrystallites were synthesized via a simple one-step solution route. > Co{sup 2+} ions incorporated into the ZnO lattice without changing its wurtzite structure. > Co-doping changed the energy band structure of ZnO. > Co-doping effectively adjusted the luminescence properties of ZnO nanocrystallites.

  13. Self-assembled structures of 1,3:2,4-di(3,4-dimethylbenzylidene) sorbitol in hydrophobic polymer matrices prepared using different heat treatments

    Science.gov (United States)

    Lai, Wei-Chi; Tseng, Shen-Jhen; Huang, Po-Hsun

    2015-11-01

    We report a method for tuning the nanoarchitectures of 1,3:2,4-di(3,4-dimethylbenzylidene) sorbitol (DMDBS) with poly(vinylidene fluoride) (PVDF) polymer matrices. Hydrophobic PVDF facilitated the formation of nanofibrils during heating. The self-assembly behaviors of DMDBS were further tuned by altering the different heat treatments. When the samples were prepared with a rapid heating rate (shorter annealing time), smaller amounts of melted PVDF were excluded due to the shorter time for aggregation of DMDBS, leading to larger complex structures of DMDBS and PVDF. Therefore, longer and thicker nanofibrils (around 100 nm) were observed using scanning electron microscopy. As the samples were prepared with a slow heating rate (longer annealing time), DMDBS had more time to aggregate, and therefore, larger amounts of melted PVDF were excluded. Smaller complex structures of DMDBS and PVDF caused the formation of shorter and thinner nanofibrils (around 40 nm). In addition, small-angle X-ray scattering results indicated that the longer and thicker nanofibrils were mostly excluded outside the PVDF crystalline bundles after cooling because they were too large to be easily incorporated between the PVDF crystalline lamellae. However, a large portion of the smaller and thinner nanofibrils was trapped between the crystalline lamellae after cooling due to their smaller sizes. As expected, the PVDF spherulitic morphologies were affected, but the PVDF crystalline microstructures were not significantly altered by the addition of DMDBS, as shown by the results from polarized optical microscopy and Fourier transform infrared spectroscopy.

  14. Properties of nano-structured Ni/YSZ anodes fabricated from plasma sprayable NiO/YSZ powder prepared by single step solution combustion method

    Energy Technology Data Exchange (ETDEWEB)

    Prakash, B. Shri; Balaji, N.; Kumar, S. Senthil; Aruna, S.T., E-mail: staruna194@gmail.com

    2016-12-15

    Highlights: • Preparation of plasma grade NiO/YSZ powder in single step. • Fabrication of nano-structured Ni/YSZ coating. • Conductivity of 600 S/cm at 800 °C. - Abstract: NiO/YSZ anode coatings are fabricated by atmospheric plasma spraying at different plasma powers from plasma grade NiO/YSZ powders that are prepared in a single step by solution combustion method. The process adopted is devoid of multi-steps that are generally involved in conventional spray drying or fusing and crushing methods. Density of the coating increased and porosity decreased with increase in the plasma power of deposition. An ideal nano-structured Ni/YSZ anode encompassing nano YSZ particles, nano Ni particles and nano pores is achieved on reducing the coating deposited at lower plasma powers. The coating exhibit porosities in the range of 27%, sufficient for anode functional layers. Electronic conductivity of the coatings is in the range of 600 S/cm at 800 °C.

  15. Nitrogen- and oxygen-enriched carbon with square tubular structure prepared from polyaniline as electrode for supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, X.; Liu, E.; Wu, Y.; Tian, Y.; Xie, H.; Wu, Z.; Zhu, Y. [Key Laboratory of Environmentally Friendly Chemistry and Applications of Ministry of Education, College of Chemistry, Xiangtan University, Hunan (China)

    2012-10-15

    Square tubular carbon with a large number of surface functional groups are prepared by carbonizing and activating polyaniline, which are synthesized by polymerization of aniline with a template-free self-assembly method in aqueous media. The physicochemical properties of the square tubular carbon is characterized by scanning and transmission electron microscopy, Brunauer-Emmett-Teller surface area measurements, Raman spectroscopy, and X-ray photoelectron spectroscopy measurements. When used as an electrode, the square tubular carbon exhibit a specific capacitance of 223 F g{sup -1} at a scan rate of 2 mV s{sup -1}, which could still stay over 90% when the scan rate increased by 10 times. The specific capacitance even hardly decrease at a current density of 3 A g{sup -1} after 10,000 cycles, which indicates that the square tubular carbon have good cycle durability and may be a promising candidate as an electrode for supercapacitors. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  16. Crystal structure and superconductivity of YBa2(Cu1-xFex)3Oy prepared by various heat treatments

    International Nuclear Information System (INIS)

    Katsuyama, Shigeru; Kosuge, Koji; Ueda, Yutaka

    1989-01-01

    The heat treatments of (a) slow cooling from 850 C in O 2 gas, which is an ordinary one, (b) quenching into liq. N 2 from 930 C in air followed by oxidation below 400 C in O 2 gas and (c) heating at 800 C in N 2 gas followed by oxidation below 400 C in O 2 gas stabilize the orthorhombic phase up to x=0.02, 0.04 and 0.12, respectively. The extension of the orthorhombic region seems to be due to the change of ratio of Fe1 to Fe2 and clustering for Fe ions in the Cu1-0 planes, which has been deduced from the results of 57 Fe Moessbauer measurements etc. The order of T c of the samples with the same iron concentration prepared by the above heat treatments is T c (c) T c (a) T c (b). The experimental results seem to show that one-dimensional Cu1-0 chains play a very important role in superconductivity as well as the two-dimensional Cu2-0 planes

  17. A comparative study of structural and mechanical properties of Al–Cu composites prepared by vacuum and microwave sintering techniques

    Directory of Open Access Journals (Sweden)

    Penchal Reddy Matli

    2018-04-01

    Full Text Available In this paper, the aluminum metal matrix composite reinforced with copper particulates (3, 6 and 9 vol.% were fabricated by high energy ball milling, followed by vacuum sintering (VS and microwave sintering techniques (MS separately. The effects of Cu content and preparation methods on the microstructure and compression mechanical behavior of Al–Cu matrix composites were investigated. The microstructural characterizations revealed a homogeneous distribution of Cu particles in the Al matrix and also fine microstructures of microwave sintered samples. The microwave sintered specimen exhibited the highest hardness and better mechanical properties compared to vacuum sintered specimens. Furthermore, the hardness and compressive strength increased 137.2% and 30.3% for the microwave sintered Al–9 vol.% Cu composite, respectively. The increase in mechanical properties with the increasing volume fraction of Cu particulates can be ascribed to the presence of harder Cu particles reinforcement. The developed materials of the microwave sintered Al–Cu composite in this investigation could be successfully used for industrial applications due to improved mechanical properties. Keywords: Al matrix composites, Microwave sintering, Microstructure, Mechanical behavior

  18. Influences of ambient gases on the structure and the composition of calcium phosphate films prepared by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hye-Lee; Kim, Young-Sun; Kim, Dae-Joon; Lee, Won-Jun [Sejong University, Seoul (Korea, Republic of); Han, Jung-Suk [Seoul National University, Seoul (Korea, Republic of)

    2006-11-15

    Calcium phosphate films were prepared by using a pulsed KrF-laser deposition (PLD) method with a hydroxyapatite target in various ambient gases, such as Ar, O{sub 2} and H{sub 2}O. The influence of the ambient gas on the properties of the deposited films was investigated. The chamber pressure and the substrate temperature were fixed at 0.25 Torr and 600 .deg. C, respectively. Calcium-rich amorphous calcium phosphate films were deposited with a low density in Ar due to the preferential resputtering of phosphorus from the growing film. In an O{sub 2} ambient, the density and the Ca/P ratio of the films were similar to those of the target. However, the deposited film was amorphous calcium phosphate and did not contain OH{sup -} groups. Polycrystalline hydroxyapatite films can be deposited in a H{sub 2}O ambient because a sufficient supply of OH{sup -} groups from the ambient gas is essential for the growth of a hydroxyapatite film.

  19. Matrix-assisted laser desorption/ionization sample preparation optimization for structural characterization of poly(styrene-co-pentafluorostyrene) copolymers.

    Science.gov (United States)

    Tisdale, Evgenia; Kennedy, Devin; Xu, Xiaodong; Wilkins, Charles

    2014-01-15

    The influence of the sample preparation parameters (the choice of the matrix, matrix:analyte ratio, salt:analyte ratio) was investigated and optimal conditions were established for the MALDI time-of-flight mass spectrometry analysis of the poly(styrene-co-pentafluorostyrene) copolymers. These were synthesized by atom transfer radical polymerization. Use of 2,5-dihydroxybenzoic acid as matrix resulted in spectra with consistently high ion yields for all matrix:analyte:salt ratios tested. The optimized MALDI procedure was successfully applied to the characterization of three copolymers obtained by varying the conditions of polymerization reaction. It was possible to establish the nature of the end groups, calculate molecular weight distributions, and determine the individual length distributions for styrene and pentafluorostyrene monomers, contained in the resulting copolymers. Based on the data obtained, it was concluded that individual styrene chain length distributions are more sensitive to the change in the composition of the catalyst (the addition of small amount of CuBr2) than is the pentafluorostyrene component distribution. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. The preparation, cytocompatibility and antimicrobial property of micro/nano structural titanium loading alginate and antimicrobial peptide

    Science.gov (United States)

    Liu, Zhiyuan; Zhong, Mou; Sun, Yuhua; Chen, Junhong; Feng, Bo

    2018-03-01

    Titanium with hybrid microporous/nanotubes (TMNT) structure on its surface was fabricated by acid etching and subsequently anodization at different voltages. Bovine lactoferricin, a kind of antimicrobial peptide, and sodium alginate (NaAlg) were loaded onto titanium surface through layer by layer assembly. The drug release, cytocompatibility and antimicrobial property against S.aureus and E.coil were studied by release experiment, osteoblast and bacterial cultures. Results indicated that samples with nanotubes of bigger diameter carried more drugs and had better biocompatibility, and drug-loaded samples acquired better biocompatibility compared with drug-free samples. Furthermore, the drug-loaded samples exhibited good initial antimicrobial property, but weak long-term antimicrobial property. Therefore, drug-loaded titanium with micro/nano structure, especially, of big diameter nanotubes, could be a promise material for medical implants, such as internal/external fixation devices.

  1. Characterization of the SnO{sub 2}:F/CdS:In structures prepared by the spray pyrolysis technique

    Energy Technology Data Exchange (ETDEWEB)

    Ikhmayies, Shadia J.; Ahmad-Bitar, Riyad N. [University of Jordan, Faculty of Science, Physics Department, Queen Rania Street, Amman 11942 (Jordan)

    2010-05-15

    SnO{sub 2}:F/CdS:In bilayers were spray-deposited on glass substrates. The structures were characterized by recording and investigating their transmittance curves, I-V plots, X-ray diffractograms (XRD) and by observing their scanning electron microscope (SEM) images. From the I-V plots it was found that the SnO{sub 2}:F forms an ohmic or quasi-ohmic contact with CdS:In. XRD patterns show the polycrystalline nature of the films and show that there is a small shift in the position of the (2 0 0) line of SnO{sub 2}:F without the appearance of new peaks. The morphology of the structures are compared with those of SnO{sub 2}:F alone and CdS:In alone on glass substrates. (author)

  2. InAs/GaSb/AlSb composite quantum well structure preparation with help of reflectance anisotropy spectroscopy

    Czech Academy of Sciences Publication Activity Database

    Hospodková, Alice; Hulicius, Eduard; Pangrác, Jiří; Dominec, Filip; Mikhailova, M. P.; Veinger, A.I.; Kochman, I.V.

    2017-01-01

    Roč. 464, Apr (2017), s. 206-210 ISSN 0022-0248 R&D Projects: GA MŠk LM2015087; GA MŠk LO1603 Institutional support: RVO:68378271 Keywords : low dimensional structures * MOVPE * InAs/GaSb composite quantum wells * AlSb Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.751, year: 2016

  3. Evaluation of the structural, optical and electrical properties of AZO thin films prepared by chemical bath deposition for optoelectronics

    Science.gov (United States)

    Kumar, K. Deva Arun; Valanarasu, S.; Rosario, S. Rex; Ganesh, V.; Shkir, Mohd.; Sreelatha, C. J.; AlFaify, S.

    2018-04-01

    Aluminum doped zinc oxide (AZO) thin films for electrode applications were deposited on glass substrates using chemical bath deposition (CBD) method. The influence of deposition time on the structural, morphological, and opto-electrical properties of AZO films were investigated. Structural studies confirmed that all the deposited films were hexagonal wurtzite structure with polycrystalline nature and exhibited (002) preferential orientation. There is no other impurity phases were detected for different deposition time. Surface morphological images shows the spherically shaped grains are uniformly arranged on to the entire film surface. The EDS spectrum confirms the presence of Zn, O and Al elements in deposited AZO film. The observed optical transmittance is high (87%) in the visible region, and the calculated band gap value is 3.27 eV. In this study, the transmittance value is decreased with increasing deposition time. The room temperature PL spectrum exposed that AZO thin film deposited at (60 min) has good optical quality with less defect density. The minimum electrical resistivity and maximum carrier concentration values were observed as 8.53 × 10-3(Ω cm) and 3.53 × 1018 cm-3 for 60 min deposited film, respectively. The obtained figure of merit (ϕ) value 3.05 × 10-3(Ω/sq)- 1 is suggested for an optoelectronic device.

  4. Preparation, structural, dielectric and magnetic properties of LaFeO3–PbTiO3 solid solutions

    International Nuclear Information System (INIS)

    Ivanov, S.A.; Tellgren, R.; Porcher, F.; Ericsson, T.; Mosunov, A.; Beran, P.; Korchagina, S.K.; Kumar, P. Anil; Mathieu, R.; Nordblad, P.

    2012-01-01

    Highlights: ► Solid-solutions of (1−x)LaFeO 3 –(x)PbTiO 3 were synthesized by solid-state reaction. ► XRPD and NPD evidence orthorhombic (x 0.8) crystal structures. ► LaFeO 3 -rich compositions order antiferromagnetically (x 3 -rich compositions exhibit ferroelectric order (x larger than 0.8). ► Magnetic and dielectric (relaxor) ordering coexist near room-temperature around x = 0.4. -- Abstract: Solid solutions of (1−x)LaFeO 3 –(x)PbTiO 3 (0 3+ cations in the B-site with propagation vector k = (0,0,0). Based on the obtained experimental data, a combined structural and magnetic phase diagram has been constructed. The factors governing the structural, dielectric and magnetic properties of (1−x)LaFeO 3 –(x)PbTiO 3 solid solutions are discussed, as well as their possible multiferroicity.

  5. Effect of Precursor Concentration on Structural Optical and Electrical Properties of NiO Thin Films Prepared by Spray Pyrolysis

    Directory of Open Access Journals (Sweden)

    Rafia Barir

    2017-01-01

    Full Text Available Undoped nickel oxide (NiO thin films were deposited on 500°C heated glass substrates using spray pyrolysis method at (0.015–0.1 M range of precursor. The latter was obtained by decomposition of nickel nitrate hexahydrate in double distilled water. Effect of precursor concentration on structural, optical, and electrical properties of NiO thin films was investigated. X-ray diffraction (XRD shows the formation of NiO under cubic structure with single diffraction peak along (111 plane at 2θ=37.24°. When precursor concentration reaches 0.1 M, an increment in NiO crystallite size over 37.04 nm was obtained indicating the product nano structure. SEM images reveal that beyond 0.04 M as precursor concentration the substrate becomes completely covered with NiO and thin films exhibit formation of nano agglomerations at the top of the sample surface. Ni-O bonds vibrations modes in the product of films were confirmed by FT-IR analysis. Transparency of the films ranged from 57 to 88% and band gap energy of the films decreases from 3.68 to 3.60 eV with increasing precursor concentration. Electrical properties of the elaborated NiO thin films were correlated to the precursor concentration.

  6. Preparation of three terbium complexes with p-aminobenzoic acid and investigation of crystal structure influence on luminescence property

    International Nuclear Information System (INIS)

    Ye Chaohong; Sun Haoling; Wang Xinyi; Li Junran; Nie Daobo; Fu Wenfu; Gao Song

    2004-01-01

    Three new rare earth p-aminobenzoic acid complexes, [Tb 2 L 6 (H 2 O) 2 ] n (1), [Tb 2 L 6 (H 2 O) 4 ].2H 2 O (2) and [Tb(phen) 2 L 2 (H 2 O) 2 ](phen)L·4H 2 O (3) (HL: p-aminobenzoic acid; phen: 1, 10-phenanthroline), with different structural forms are reported in this paper. Complex 1 is a polymolecule with a two-dimensional plane structure. Compound 2 is a binuclear molecule, and 3 appears to be a mononuclear complex. The fluorescence intensity, the fluorescence life-time and emission quantum yield of 2, which has two coordination water molecules, is better than those of 1, which has only one coordination water molecule. This is an unusual phenomenon for general fluorescent rare earth complexes. The fluorescence performance of 3 is the most unsatisfactory among the three complexes. Their crystal structures show that the coordination mode of the ligand is an important factor influencing the luminescence properties of a fluorescent rare earth complex

  7. A novel method for preparing pomegranate-structured FePO4/C composite materials as cathode for lithium-ion batteries

    International Nuclear Information System (INIS)

    Hao, Guan-nan; Zhang, Hao; Chen, Xiao-Hong; Cao, Gao-Ping; Yang, Yusheng

    2012-01-01

    Graphical abstract: Display Omitted Highlights: ► We designed and synthesized a pomegranate-structured FePO 4 /C composite. ► We used a combination of electrospinning and solid-state reaction for preparation. ► We showed how the performance of pomegranate-structured FePO 4 is highly enhanced. -- Abstract: A pomegranate-structured FePO 4 /C composite was synthesized via a combination of electrospinning and high temperature reaction using micron-level FePO 4 and polyacrylonitrile (PAN). Systematic studies on synthesis, modification, and characterization of FePO 4 /C composites were conducted. The FePO 4 /C composites delivered a specific discharge capacity of 109 mAh g −1 at 0.2 C and 39 mAh g −1 at 10 C, which were comparable with the reported nanometer-level FePO 4 . We demonstrated that the three-dimensional net-like structure covered by porous carbon layers could highly enhance the electrochemical performance of FePO 4 .

  8. A novel method for preparing pomegranate-structured FePO{sub 4}/C composite materials as cathode for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Guan-nan [Research Institute of Chemical Defense, Beijing 100191 (China); State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Zhang, Hao, E-mail: dr.h.zhang@hotmail.com [Research Institute of Chemical Defense, Beijing 100191 (China); Chen, Xiao-Hong [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Cao, Gao-Ping; Yang, Yusheng [Research Institute of Chemical Defense, Beijing 100191 (China)

    2012-12-15

    Graphical abstract: Display Omitted Highlights: ► We designed and synthesized a pomegranate-structured FePO{sub 4}/C composite. ► We used a combination of electrospinning and solid-state reaction for preparation. ► We showed how the performance of pomegranate-structured FePO{sub 4} is highly enhanced. -- Abstract: A pomegranate-structured FePO{sub 4}/C composite was synthesized via a combination of electrospinning and high temperature reaction using micron-level FePO{sub 4} and polyacrylonitrile (PAN). Systematic studies on synthesis, modification, and characterization of FePO{sub 4}/C composites were conducted. The FePO{sub 4}/C composites delivered a specific discharge capacity of 109 mAh g{sup −1} at 0.2 C and 39 mAh g{sup −1} at 10 C, which were comparable with the reported nanometer-level FePO{sub 4}. We demonstrated that the three-dimensional net-like structure covered by porous carbon layers could highly enhance the electrochemical performance of FePO{sub 4}.

  9. C2x: A tool for visualisation and input preparation for CASTEP and other electronic structure codes

    Science.gov (United States)

    Rutter, M. J.

    2018-04-01

    The c2x code fills two distinct roles. Its first role is in acting as a converter between the binary format .check files from the widely-used CASTEP [1] electronic structure code and various visualisation programs. Its second role is to manipulate and analyse the input and output files from a variety of electronic structure codes, including CASTEP, ONETEP and VASP, as well as the widely-used 'Gaussian cube' file format. Analysis includes symmetry analysis, and manipulation arbitrary cell transformations. It continues to be under development, with growing functionality, and is written in a form which would make it easy to extend it to working directly with files from other electronic structure codes. Data which c2x is capable of extracting from CASTEP's binary checkpoint files include charge densities, spin densities, wavefunctions, relaxed atomic positions, forces, the Fermi level, the total energy, and symmetry operations. It can recreate .cell input files from checkpoint files. Volumetric data can be output in formats useable by many common visualisation programs, and c2x will itself calculate integrals, expand data into supercells, and interpolate data via combinations of Fourier and trilinear interpolation. It can extract data along arbitrary lines (such as lines between atoms) as 1D output. C2x is able to convert between several common formats for describing molecules and crystals, including the .cell format of CASTEP. It can construct supercells, reduce cells to their primitive form, and add specified k-point meshes. It uses the spglib library [2] to report symmetry information, which it can add to .cell files. C2x is a command-line utility, so is readily included in scripts. It is available under the GPL and can be obtained from http://www.c2x.org.uk. It is believed to be the only open-source code which can read CASTEP's .check files, so it will have utility in other projects.

  10. Structural, magnetic and electrical characterization of Mg–Ni nano-crystalline ferrites prepared through egg-white precursor

    Energy Technology Data Exchange (ETDEWEB)

    Gabal, M.A., E-mail: mgabalabdonada@yahoo.com [Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah (Saudi Arabia); Al Angari, Y.M. [Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah (Saudi Arabia); Zaki, H.M. [Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah (Saudi Arabia); Physics Department, Faculty of Science, Zagazig University, Zagazig (Egypt)

    2014-08-01

    Soft Ni–Mg nano-crystalline ferrites with the general formula Ni{sub 1−x}Mg{sub x}Fe{sub 2}O{sub 4} (0≤x≤1) were synthesized through egg-white method. The precursor decomposition was followed by thermal analysis techniques. The obtained ferrites were characterized by X-ray diffraction, Fourier transform infrared and transmission electron microscopy measurements. X-ray diffraction showed the cubic spinel structure with crystallite size variation within the range 20–45 nm. The different structural data obtained were discussed in the view of ionic radii of the entire ions and their distribution within the lattice. The appropriate suggested cation distribution was then confirmed through Fourier transform infrared as well as electrical and magnetic properties measurements. Transmission electron microscopy exhibited a nano-crystal aggregation phenomenon. The observed size of the spherical particles agrees well with that obtained by X-ray diffraction. Hysteresis loop measurements revealed dilution in the obtained magnetic parameters by Mg-substitution due to the preferential occupancy of Mg{sup 2+} ions by the octahedral sites. Ac-electrical conductivity as a function of temperature and frequency exhibited a semi-conducting behavior with conductivity decreases by increasing Mg-content. The change in the slope of the curve indicates the changing in the conduction mechanism from electron hopping to polaron mechanism by increasing temperature. The obtained structural, electrical and magnetic properties were explained based on the cation distribution among tetrahedral and octahedral sites. - Highlights: • Ni–Mg nano-crystalline ferrites were synthesized through egg-white method. • An appropriate cation distribution was suggested. • Conductivity revealed a change in conduction mechanism by increasing temperature. • The effect of Mg-substitution on different properties was studied.

  11. Influence of preparation methods of microwave, sol-gel, and hydrothermal on structural and optical properties of lanthania nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Goharshadi, Elaheh K.; Mahvelati, Tahereh; Yazdanbakhsh, Mohammad [Ferdowsi Univ., Mashhad (Iran, Islamic Republic of). Dept. of Chemistry

    2016-01-15

    In this work, the nearly pure hexagonal phase of lanthania nanoparticles (NPs) was successfully synthesized using three methods: microwave, sol-gel, and hydrothermal. The samples were characterized using nine techniques including powder X-ray powder diffraction, thermogravimetry, transmission electron microscopy, scanning electron microscopy, field emission microscopy, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, far infrared spectroscopy, and ultraviolet-visible absorption spectroscopy. This study showed that the method of synthesizing lanthania NPs can affect the size, which in turn has impact on structural, morphological, and optical properties.

  12. Structure of chlorinated poly(vinyl chloride). III. Preparation of poly(vinyl chloride)-β,β-d2 as a model for the study of the mechanism of chlorination and of the chlorinated poly(vinyl chloride) structure

    International Nuclear Information System (INIS)

    Lukas, R.; Kolinsky, M.

    1976-01-01

    A method for the preparation of poly(vinyl chloride)-β,β-d 2 (PVC-β,β-d 2 ) as a model for the investigation of the mechanism of chlorination and of the CPVC structure has been suggested. The conditions of preparation of deuterated intermediates of a multistage synthesis of vinyl chloride-β,β-d 2 and of suspension-polymerized PVC-β,β-d 2 have been described including the mass balance. Malonic acid was used as the starting compound. Tacticity values of a sample of PVC-β,β-d 2 and its infrared and nuclear magnetic resonance (NMR) spectra are presented and compared with the data already published

  13. Two inorganic-organic hybrid materials based on polyoxometalate anions and methylene blue: Preparations, crystal structures and properties

    International Nuclear Information System (INIS)

    Nie Shanshan; Zhang Yaobin; Liu Bin; Li Zuoxi; Hu Huaiming; Xue Ganglin; Fu Feng; Wang Jiwu

    2010-01-01

    Two novel inorganic-organic hybrid materials based on an organic dye cation methylene blue (MB) and Lindqvist-type POM polyanions, [C 22 H 18 N 3 S] 2 Mo 6 O 19 2DMF (1) and [C 22 H 18 N 3 S] 2 W 6 O 19 2DMF (2) were synthesized under ambient conditions and characterized by CV, IR spectroscopy, solid diffuse reflectance spectrum, UV-vis spectra in DMF solution, luminescent spectrum and single crystal X-ray diffraction. Crystallographic data reveal that compounds 1 and 2 are isostructural and both crystallize in the triclinic space group P1-bar . Their crystal structures present that the layers of organic molecules and inorganic anions array alternatively, and there exist strong π...π stacking interactions between dimeric MB cations and near distance interactions among organic dye cations, Lindqvist-type POM polyanions and DMF molecules. The solid diffuse reflectance spectra and UV-vis spectra in DMF solution appear new absorption bands ascribed to the charge-transfer transition between the cationic MB donor and the POM acceptors. Studies of the photoluminescent properties show that the formation of 1 and 2 lead to the fluorescence quenching of starting materials. -- Graphical abstract: Their crystal structures present that the layers of organic molecules and inorganic anions array alternatively, and there exist strong π...π stacking interactions between dimeric MB cations. Display Omitted

  14. Structural, morphological, wettability and thermal resistance properties of hydro-oleophobic thin films prepared by a wet chemical process

    International Nuclear Information System (INIS)

    Phani, A.R.

    2006-01-01

    The structural properties of fluorine containing polymer compounds make them highly attractive materials for hydro-oleophobic applications. However, most of these exhibit low surface energy and poor adhesion on the substrates. In the present investigation, crack free, smooth and uniform thin films of poly[4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxole] -co-tetrafluoroethylene (TFD-co-TFE) with good adhesion have been deposited by wet chemical spin-coating technique on polished AISI 440C steel substrates. The as-deposited films (xerogel films) have been subjected to annealing for 1 h at different temperatures ranging from 100 to 500 deg. C in an argon atmosphere. The size growth of the nano-hemispheres increased from 8 nm for xerogel film to 28 nm for film annealed at 400 deg. C. It was found that as the annealing temperature increased from 100 to 400 deg. C, nano-hemisphere-like structures were formed, which in turn have shown increase in the water contact angle from 122 deg. to 147 deg. and oil (peanut) contact angle from 85 deg. to 96 deg. No change in the water contact angle (122 deg.) has been observed when the films deposited at room temperature were heated in air from 30 to 80 deg. C as well as exposed to steam for 8 days for 8 h/day indicating thermal stability of the film

  15. Structural and magnetic properties of NiZn-ferrite thin films prepared by radio frequency magnetron sputtering

    International Nuclear Information System (INIS)

    Liu Yingli; Li Yuanxun; Zhang Huaiwu; Chen Daming; Mu Chunhong

    2011-01-01

    Polycrystalline NiZn-ferrite thin films were deposited on Si(100) substrate by rf magnetron sputtering, using targets with a nominal composition of Ni 0.5 Zn 0.5 Fe 2 O 4 . The effects of substrate condition, sputtering pressure, and postannealing on the structure and magnetic properties of thin films have been investigated. Our results show that the preferred orientation of the NiZn spinel film changed from (311) to (400) with increasing the Ar pressure from 0.8 to 1.6 Pa, meanwhile, the grain size also increased. Atomic force microscopy analysis indicates that perfect surface morphology of the film can be obtained at a relatively lower sputtering pressure of 1.0 Pa. The relative percentage of residual oxygen increases significantly on a condition of lower sputtering pressure, and plays an important role in film structure due to the strong molecular adsorption tendency of oxygen on the film surface during the deposition process. A thin film with a typical thickness of 1 μm, a saturation magnetization of 150 emu/cm 3 , and a coercivity of 8.8 kA/m has been obtained after annealing at 800 deg. C, which has the potential application in magnetic integrated circuits.

  16. Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

    Directory of Open Access Journals (Sweden)

    K. Jeyadheepan

    2014-01-01

    Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

  17. Studies on the structural and electrical properties of F-doped SnO{sub 2} film prepared by APCVD

    Energy Technology Data Exchange (ETDEWEB)

    Yang Jingkai; Liu Wenchang; Dong Lizhong; Li Yuanxun; Li Chuan [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Zhao Hongli, E-mail: zhaohongli@ysu.edu.cn [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China)

    2011-10-01

    Fluorine-doped tin oxide films (SnO{sub 2}:F, FTO) were deposited by atmosphere pressure chemical vapor deposition (APCVD) on Na-Ca-Si glass coated with a diffusion barrier layer of SiO{sub x}C{sub y}. The effects of post-heating time at 700 deg. C on the structural and electrical properties of SnO{sub 2}:F films were investigated. The results showed that SnO{sub 2}:F films were polycrystalline with tetragonal SnO{sub 2} structure, SnO phase was present in SnO{sub 2} film, and abnormal grain growth was observed. The element distribution in the film depth was measured with X-ray photoelectron spectroscopy (XPS) and revealed that when the heating time increased from 202 s to 262 s, the oxygen content in the surface increased from 78.63% to 83.38%. The resistivity increased from 3.13 x 10{sup -4} for as-deposited films to 4.73 x 10{sup -4} {Omega} cm when post-heated for 262 s. Hall mobility is limited by the ionized impurity scattering rather than the grain boundary scattering.

  18. Structural and XPS studies of PSi/TiO2 nanocomposites prepared by ALD and Ag-assisted chemical etching

    International Nuclear Information System (INIS)

    Iatsunskyi, Igor; Kempiński, Mateusz; Nowaczyk, Grzegorz; Jancelewicz, Mariusz; Pavlenko, Mykola; Załęski, Karol; Jurga, Stefan

    2015-01-01

    Highlights: • Porous silicon/TiO 2 nanocomposites have been investigated. • Morphology and chemical composition of PSi/TiO 2 nanocomposites were established. • Valence-band XPS maximums for PSi/TiO 2 nanocomposites were found and analyzed. - Abstract: PSi/TiO 2 nanocomposites fabricated by atomic layer deposition (ALD) and metal-assisted chemical etching (MACE) were investigated. The morphology and phase structure of PSi/TiO 2 nanocomposites were studied by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) with an energy dispersive X-ray spectroscopy (EDX) and Raman spectroscopy. The mean size of TiO 2 nanocrystals was determined by TEM and Raman spectroscopy. X-ray photoelectron spectroscopy (XPS) was used to analyze the chemical elemental composition by observing the behavior of the Ti 2p, O 1s and Si 2p lines. TEM, Raman spectroscopy and XPS binding energy analysis confirmed the formation of TiO 2 anatase phase inside the PSi matrix. The XPS valence band analysis was performed in order to investigate the modification of PSi/TiO 2 nanocomposites electronic structure. Surface defects states of Ti 3+ at PSi/TiO 2 nanocomposites were identified by analyzing of XPS valence band spectra

  19. Structural, Optical and Electrical Properties of Transparent Conducting Oxide Based on Al Doped ZnO Prepared by Spray Pyrolysis

    Directory of Open Access Journals (Sweden)

    Abdeslam DOUAYAR

    2014-05-01

    Full Text Available Aluminum doped zinc oxide (AZO thin films were deposited on glass substrates at 350 °C by spray pyrolysis technique. X-ray diffraction patterns show that the undoped and AZO films exhibit the hexagonal wűrtzite crystal structure with a preferential orientation along 2 direction. AFM images showed that AZO film with 3 % of Al has a uniform grain sizes with a surface roughness of about 24 nm. All films present a high transmittance in the visible range. Both undoped and AZO films were n-type degenerate semiconductor and the best electrical resistivity value was around 8.0 ´ 10- 2 W.cm obtained for 3 % Al content.

  20. Structural anomalies induced by the metal deposition methods in 2D silver nanoparticle arrays prepared by nanosphere lithography

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Shengli, E-mail: huangsl@xmu.edu.cn [Fujian Provincial Key Lab of Semiconductors and Applications, Department of Physics, Xiamen University, Xiamen, Fujian 361005 (China); State Key Lab of Silicon Materials, Zhejiang University, Hangzhou 310027 (China); Yang, Qianqian [Fujian Provincial Key Lab of Semiconductors and Applications, Department of Physics, Xiamen University, Xiamen, Fujian 361005 (China); State Key Lab of Silicon Materials, Zhejiang University, Hangzhou 310027 (China); Zhang, Chunjing; Kong, Lingqi; Li, Shuping; Kang, Junyong [Fujian Provincial Key Lab of Semiconductors and Applications, Department of Physics, Xiamen University, Xiamen, Fujian 361005 (China)

    2013-06-01

    Silver nanoparticle arrays with 2-dimensional hexagonal arrangement were fabricated on the silicon substrates by nanosphere lithography. The silver film was deposited either by thermal evaporation or by magnetron sputtering under different conditions. The nanostructures of the achieved sphere template and the array units were characterized by scanning electron microscopy and atomic force microscopy, and were found to be anomalous under different deposition parameters. Comparative study indicated that the formation of the various 2-dimensional silver nanoparticle array structures was dominated by the thermal energy (temperature), kinetic energy and deposition direction of the deposited metal atoms as well as the size and nanocurvature of the colloidal particles and the metal clusters. - Highlights: • Silver nanoparticle arrays with different nanostructures on silicon substrates. • Various deposition parameters in arrays formation systematically examined. • Possible mechanisms and optimization of nanostructures formation addressed.

  1. Structural and optical properties of colloidal InZnO NPs prepared by laser ablation in liquid

    Science.gov (United States)

    khlewee, Maryam M.; Khashan, Khawla S.

    2018-05-01

    In the current work, colloidal of InZnO NPs were produced by pulsed laser ablation in liquid (PLAL) method. The effect of indium content on the structural, morphological and optical of the InZnO NPs was confirmed by Fourier transform infrared spectroscopy, Scanning electron microscopy, and UV-visible spectroscopy. The FTIR spectra showed the presence of the metal-oxide bond. The SEM exhibit different morphological aspects according to the (In/Zn) ratio. The optical transmittance of InZnO NPs has high value around 70 % in the visible region and the band gap value was varied between 3.29 to 3.25 eV.

  2. Structural changes in plasma membranes prepared from irradiated Chinese hamster V79 cells as revealed by Raman spectroscopy

    International Nuclear Information System (INIS)

    Verma, S.P.; Sonwalkar, N.

    1991-01-01

    The effect of gamma irradiation on the integrity of plasma membranes isolated from Chinese hamster V79 cells was investigated by Raman spectroscopy. Plasma membranes of control V79 cells show transitions between -10 and 5 degree C (low-temperature transition), 10 and 22 degree C (middle-temperature transition), and 32 and 40 degree C (high-temperature transition). Irradiation (5 Gy) alters these transitions markedly. First, the low-temperature transition shifts to higher temperature (onset and completion temperatures 4 and 14 degree C). Second, the middle-temperature transition shifts up to the range of about 20-32 degree C, but the width remains unchanged. Third, the higher temperature transition broadens markedly and shifts to the range of about 15-40 degree C. Protein secondary structure as determined by least-squares analysis of the amide I bands shows 36% total helix, 55% total beta-strand, and 9% turn plus undefined for control plasma membrane proteins. Plasma membrane proteins of irradiated V79 cells show an increase in total helix (40 and 45% at 5 and 10 Gy, respectively) and a decrease in the total beta-strand (48 and 44% at 5 and 10 Gy, respectively) structures. The qualitative analysis of the Raman features of plasma membranes and model compounds in the 1600 cm-1 region, assigned to tyrosine groups, revealed that irradiation alters the microenvironment of these groups. We conclude that the radiation dose used in the survival range of Chinese hamster V79 cells can cause damage to plasma membrane proteins without detectable lipid peroxidation, and that the altered proteins react differently with lipids, yielding a shift in the thermal transition properties

  3. Requirements for a new nuclear data structure. Part 2: Implementation Plan Prepared by WPEC Subgroup No.38 (subgroup title: 'A modern nuclear database structure beyond the ENDF format')

    International Nuclear Information System (INIS)

    2014-01-01

    This document summarizes the implementation plan developed during the second meeting of the WPEC Subgroup 38 (SG38), which was organized to develop a new evaluated nuclear data structure 1 and then oversee the transition from the current standard (ENDF-6) to the new structure. Part 1 of this document, adopted by WPEC in May 2013, lays out the vision and goals for the new structure. In this second step, SG38 develops a community plan to address these needs and requirements. The plan laid out here represents a consensus on how to execute the project, what work will be done, and to some degree how it will be done and the people involved. During the development of the vision and goals for the new format it was recognized that the application of modern programming and database practices will have significant benefits for nuclear reaction databases, both for those of us engaged in producing this data and those who utilize the data for applications. It was also appreciated that additional benefits would be realized if the low-level data containers used for storing reaction data were general enough to be shared with other nuclear data products, such as EXFOR, RIPL, and ENSDF, so that codes interfacing with these different databases could share the same set of routines for reading and writing data structures. However, it was also acknowledged that adoption of these new tools and capabilities will be difficult without some supporting infrastructure in place to use the new data structure, specifically open source codes to manipulate, search, plot, and process the data, as well as tools to translate data to other formats in current use and to check the data for quality. In order to address this broad set of goals, the SG38 project decided to organize the work around seven different products: 1. Low-level data structures; 2. Top-level reaction hierarchy; 3. Particle properties hierarchy; 4. Visualization, manipulation, and processing tools; 5. API for reading and writing data

  4. Key insights on the structural characterization of textured Er2O3–ZrO2 nano-oxides prepared by a surfactant-free solvothermal route

    International Nuclear Information System (INIS)

    Julián-López, Beatriz; Luz, Verónica de la; Gonell, Francisco; Cordoncillo, Eloisa; López-Haro, Miguel; Calvino, Jose J.; Escribano, Purificación

    2012-01-01

    Highlights: ► Structural resolution of fluorite vs. pyrochlore in small nanocrystals. ► Simple template-free solvothermal synthesis of Er 2 O 3 –ZrO 2 nanooxides. ► Good control over size, morphology and surface properties (280 m 2 g −1 ). - Abstract: Zirconia-mixed oxides can exhibit cubic fluorite and pyrochlore structure. Their discrimination is not easy in nanooxides with a crystal size close to that of a few unit cells. In this work, high resolution transmission electron microscopy (HRTEM) has been employed to provide key insights on the structural characterization of a nanometric and porous mixed Er 2 O 3 –ZrO 2 oxide. The material was prepared by a simple template-free solvothermal route that provided nanocrystalline powders at low temperature (170 °C) with spherical morphology, and high surface area (∼280 m 2 g −1 ). The porosity was mainly originated from the assembling of organic complexing agents used in the synthesis to limit the crystal growth and to control hydrolysis and condensation reaction rates. The samples were characterized by thermal analysis, X-ray diffraction, scanning electron microscopy and N 2 adsorption measurements. A detailed study by HRTEM was conducted on microtomed samples. It was observed that the material was made of nanocrystals packed into spherical agglomerates. HRTEM simulations indicated that it is not possible to identify the pyrochlore phase in nanoparticles with diameter below 2 nm. In our samples, the analysis of the HRTEM lattice images by means of fast Fourier transform (FFT) techniques revealed well defined spots that can be assigned to different planes of a cubic fluorite-type phase, even in the raw material. Raman spectroscopy was also a powerful technique to elucidate the crystalline phase of the materials with the smallest nanoparticles. HREM and Raman results evidenced that the material is constituted, irrespective of the temperature of the final calcination step, by an ensemble of randomly

  5. The use of gamma irradiation in preparation of polybutadiene rubber nanopowder; Its effect on particle size, morphology and crosslink structure of the powder

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei Abadchi, Majid; Jalali-Arani, Azam, E-mail: ajalali@aut.ac.ir

    2014-02-01

    Highlights: • Vulcanized rubber powders were prepared by spray drying of irradiated rubber latexes. • Influence of absorbed dose on powder structure and characteristics was investigated. • The size of rubber latex particles did not changed by irradiation. • Crosslink density increased by increasing dose and 98% gel was obtained at 150 kGy. • T{sub g} of rubber powder increased with increasing the irradiation dose. -- Abstract: The aim of this work was the preparation and characterization of polybutadiene rubber (BR) powder by irradiating of rubber lattices using {sup 60}Co radiation and spray-drying of them at the appropriate condition. The influences of absorbed dose on the volume swelling ratio, molecular weight between crosslinks, gel fraction, and glass transition temperature of obtained powder were studied. Morphology, size and size distribution of rubber particles were examined by using scanning electron microscopy (SEM) and laser particle size analyzer (LPSA) technique, respectively. Results obtained by LPSA revealed that radiation has no effect on particle size of rubber latex but after drying, adherence properties of rubber particle causes increase in particle size of rubber powder, as shown in SEM photograph. Fourier transform infrared spectroscopy of rubber powders confirmed that with increasing the irradiation dose, characteristic peak corresponds to the >C=C< double bands decreased. Also Charlesby–Pinner equation was used to evaluate radiation yield.

  6. The use of gamma irradiation in preparation of polybutadiene rubber nanopowder; Its effect on particle size, morphology and crosslink structure of the powder

    International Nuclear Information System (INIS)

    Rezaei Abadchi, Majid; Jalali-Arani, Azam

    2014-01-01

    Highlights: • Vulcanized rubber powders were prepared by spray drying of irradiated rubber latexes. • Influence of absorbed dose on powder structure and characteristics was investigated. • The size of rubber latex particles did not changed by irradiation. • Crosslink density increased by increasing dose and 98% gel was obtained at 150 kGy. • T g of rubber powder increased with increasing the irradiation dose. -- Abstract: The aim of this work was the preparation and characterization of polybutadiene rubber (BR) powder by irradiating of rubber lattices using 60 Co radiation and spray-drying of them at the appropriate condition. The influences of absorbed dose on the volume swelling ratio, molecular weight between crosslinks, gel fraction, and glass transition temperature of obtained powder were studied. Morphology, size and size distribution of rubber particles were examined by using scanning electron microscopy (SEM) and laser particle size analyzer (LPSA) technique, respectively. Results obtained by LPSA revealed that radiation has no effect on particle size of rubber latex but after drying, adherence properties of rubber particle causes increase in particle size of rubber powder, as shown in SEM photograph. Fourier transform infrared spectroscopy of rubber powders confirmed that with increasing the irradiation dose, characteristic peak corresponds to the >C=C< double bands decreased. Also Charlesby–Pinner equation was used to evaluate radiation yield

  7. Effect of maleic acid content on the thermal stability, swelling behaviour and network structure of gelatin-based hydrogels prepared by gamma irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Eid, M. [National Center For Radiation Research and Technology, P.O. Box 29, Nasr City, Cairo 11731 (Egypt)], E-mail: mona_eid2000@yahoo.com; Abdel-Ghaffar, M.A. [National Research Center, Dokki, Cairo (Egypt); Dessouki, A.M. [National Center For Radiation Research and Technology, P.O. Box 29, Nasr City, Cairo 11731 (Egypt)

    2009-01-15

    The highly swelling Poly (acrylamide/maleic acid/gelatin) P(AAm/MA/G) hydrogels were prepared by gamma-irradiation at low dose rate (0.94 kGy/h) and moderate dose rate (3.84 kGy/h). The hydrogels were confirmed by FTIR. The effect of copolymer composition, dose and dose rate on the swelling behaviour was discussed. Increasing of MA content and G in the initial mixture leads to an increase in the amount of MA and G in the gel system and decrease in the gelation %. The swelling behaviours of the hydrogel prepared at moderate dose rate increased with increasing MA mole content in the gel system but, there is no systematic dependence of swelling on MA content was observed for the hydrogels obtained at low dose rate. Pore structure of the hydrogels was monitored by using scanning electron microscopy. Thermogravimetric analysis (TGA) and the rate of the thermal decomposition of P(AAm/MA/G) hydrogels has been evaluated to give a better understanding of the thermal stability of polymers, The X-ray data of P(AAm/MA/G) hydrogels was discussed to investigate some features namely the degree of ordering and crystallite size.

  8. Structural characteristics and gasification reactivity of chars prepared from K{sub 2}CO{sub 3} mixed HyperCoals and coals

    Energy Technology Data Exchange (ETDEWEB)

    Atul Sharma; Hiroyuki Kawashima; Ikuo Saito; Toshimasa Takanohashi [National Institute of Advanced Industrial Science and Technology, Ibaraki (Japan). Advanced Fuel Group

    2009-04-15

    HyperCoal is a clean coal with mineral matter content <0.05 wt %. Oaky Creek (C = 82%), and Pasir (C = 68%) coals were subjected to solvent extraction method to prepare Oaky Creek HyperCoal, and Pasir HyperCoal. Experiments were carried out to compare the gasification reactivity of HyperCoals and parent raw coals with 20, 40, 50 and 60% K{sub 2}CO{sub 3} as a catalyst at 600, 650, 700, and 775{sup o}C with steam. Gasification rates of coals and HyperCoals were strongly influenced by the temperature and catalyst loading. Catalytic steam gasification of HyperCoal chars was found to be chemical reaction controlled in the 600-700{sup o}C temperature range for all catalyst loadings. Gasification rates of HyperCoal chars were found to be always higher than parent coals at any given temperature for all catalyst loadings. However, X-ray diffraction results showed that the microstructures of chars prepared from coals and HyperCoals were similar. Results from nuclear magnetic resonance spectroscopy show no significant difference between the chemical compositions of the chars. Significant differences were observed from scanning electron microscopy images, which showed that the chars from HyperCoals had coral-reef like structures whereas dense chars were observed for coals. 26 refs., 8 figs., 2 tabs.

  9. Structural and Luminescence Properties of Lu2O3:Eu3+ F127 Tri-Block Copolymer Modified Thin Films Prepared by Sol-Gel Method

    Science.gov (United States)

    de Jesus Morales Ramírez, Angel; Hernández, Margarita García; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Palmerin, Joel Moreno; Velazquez, Dulce Yolotzin Medina; Jota, María Luz Carrera

    2013-01-01

    Lu2O3:Eu3+ transparent, high density, and optical quality thin films were prepared using the sol-gel dip-coating technique, starting with lutetium and europium nitrates as precursors and followed by hydrolysis in an ethanol-ethylene glycol solution. Acetic acid and acetylacetonate were incorporated in order to adjust pH and as a sol stabilizer. In order to increment the thickness of the films and orient the structure, F127 Pluronic acid was incorporated during the sol formation. Structural, morphological, and optical properties of the films were investigated for different F127/Lu molar ratios (0–5) in order to obtain high optical quality films with enhanced thickness compared with the traditional method. X-ray diffraction (XRD) shows that the films present a highly oriented cubic structure beyond 1073 K for a 3-layer film, on silica glass substrates. The thickness, density, porosity, and refractive index evolution of the films were investigated by means of m-lines microscopy along with the morphology by scanning electron microscope (SEM) and luminescent properties. PMID:28809336

  10. Optical and structural properties of zinc oxide films with different thicknesses prepared by successive ionic layer adsorption and reaction method

    Energy Technology Data Exchange (ETDEWEB)

    Taner, Ahmet, E-mail: ataner@anadolu.edu.tr [Institute of Science and Technology, Anadolu University, Eskisehir 26470 (Turkey); Kul, Metin; Turan, Evren; Aybek, A. Senol; Zor, Muhsin [Department of Physics, Anadolu University, Eskisehir 26470 (Turkey); Taskoeprue, Turan [Department of Physics, Anadolu University, Eskisehir 26470 (Turkey); Department of Physics, Cank Latin-Small-Letter-Dotless-I r Latin-Small-Letter-Dotless-I Karatekin University, Cank Latin-Small-Letter-Dotless-I r Latin-Small-Letter-Dotless-I 18100 (Turkey)

    2011-12-01

    In this work, zinc oxide semiconducting films belonging to the II-VI group have been produced by successive ionic layer adsorption and reaction (SILAR) method on glass substrates with 10, 15, 20 and 25 cycles at room temperature. Following the deposition, the samples were dried in air at 400 Degree-Sign C for 1 h. The films were characterized by X-ray diffraction, field emission scanning electron microscopy and optical absorption measurement techniques. The X-ray diffractions of the films showed that they are hexagonal in structure. The crystallite size of ZnO films varied between 34 and 38 nm accordingly with the number of SILAR cycles. The material has exhibited direct band gap transition with the band gap values lying in the range between 3.13 and 3.18 eV. The red shift is observed in the absorption edge as the cycles increased. Transmission of the films decreased from 65 to 40% with increasing the number of cycles.

  11. Structural, Morphological, and LPG Sensing Properties of Al-Doped ZnO Thin Film Prepared by SILAR

    Directory of Open Access Journals (Sweden)

    Shampa Mondal

    2013-01-01

    Full Text Available Undoped and aluminum doped zinc oxide (AZO thin films were deposited on glass substrates by successive ion layer adsorption and reaction (SILAR technique from ammonium zincate complex. The thin films are characterized by X-ray diffraction (XRD and scanning electron microscopy (SEM for their structural and morphological studies. Both undoped and Al-doped film show strong preferred c-axis orientation. The texture coefficient (TC of the film along (002 direction increases due to Al incorporation. SEM micrograph shows round shaped particles for pure ZnO. However AZO films show particles with off spherical shape and compact interconnected grains. Sensitivity of the film in presence of 80% LEL (lower explosive limit of LPG increases with temperature and is maximum at 325°C. Significantly high sensitivity of 87% with reasonably fast response was observed for 1% Al-doped ZnO (AZO film in presence of 1.6 vol% LPG at 325°C.

  12. Optical and structural properties of zinc oxide films with different thicknesses prepared by successive ionic layer adsorption and reaction method

    International Nuclear Information System (INIS)

    Taner, Ahmet; Kul, Metin; Turan, Evren; Aybek, A. Şenol; Zor, Muhsin; Taşköprü, Turan

    2011-01-01

    In this work, zinc oxide semiconducting films belonging to the II-VI group have been produced by successive ionic layer adsorption and reaction (SILAR) method on glass substrates with 10, 15, 20 and 25 cycles at room temperature. Following the deposition, the samples were dried in air at 400 °C for 1 h. The films were characterized by X-ray diffraction, field emission scanning electron microscopy and optical absorption measurement techniques. The X-ray diffractions of the films showed that they are hexagonal in structure. The crystallite size of ZnO films varied between 34 and 38 nm accordingly with the number of SILAR cycles. The material has exhibited direct band gap transition with the band gap values lying in the range between 3.13 and 3.18 eV. The red shift is observed in the absorption edge as the cycles increased. Transmission of the films decreased from 65 to 40% with increasing the number of cycles.

  13. Load-Direction-Derived Support Structures for Wind Turbines: A Lattice Tower Concept and Preparations for Future Certifications: Preprint

    Energy Technology Data Exchange (ETDEWEB)

    Jonkman, Jason [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Damiani, Rick R [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Struve, Achim [University of Applied Sciences Flensburg; Faber, Torsten [University of Applied Sciences Flensburg; Ummenhofer, Thomas [Karlsruhe Institute of Technology

    2017-11-07

    The call for more cost-effective and environmentally friendly tower concepts is motivated by tower costs [1] and tower CO2-emission contributions [2], which are high relative to the whole wind turbine system. The proposed rotatable tower concept with yaw bearing at the bottom instead of the top of the tower will provide beneficial economic and environmental impacts to the turbine system. This wind alignment capability indicates a load-direction-derived tower design. By combining this approach with a lattice concept, large material and cost savings for the tower can be achieved. This paper presents a way to analyze and verify the proposed design through aero-servo-elastic simulations, which make future certifications of rotatable tower concepts viable. For this reason, the state-of-the-art, open-source lattice-tower finite-element-method (FEM) module SubDyn [10], developed by the National Renewable Energy Laboratory, has been modified to account for arbitrary member cross-sections. Required changes in the beam element stiffness and mass matrix formulation took place according to an energy method [13]. All validated adaptions will be usable within the aero-servo-elastic simulation framework FAST and are also beneficial for other nonrotatable lattice structures.

  14. Study of structural, optical and thermal properties of nanostructured SnSe{sub 2} prepared by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Z.V. [Faculdade de Tecnologia, Universidade Federal do Amazonas, 3000 Japiim, 69077-000 Manaus, Amazonas (Brazil); Poffo, C.M., E-mail: claudio.poffo@ufsc.br [Universidade Federal de Santa Catarina, Campus de Araranguá, 88900-000, Santa Catarina (Brazil); Lima, J.C. de [Departamento de Física, Universidade Federal de Santa Catarina, Campus Trindade, C.P. 476, 88040-900 Florianópolis, Santa Catarina (Brazil); Souza, S.M. de; Trichês, D.M.; Nogueira, T.P.O. [Departamento de Física, Universidade Federal do Amazonas, 3000 Japiim, 69077-000 Manaus, Amazonas (Brazil); Manzato, L. [Instituto Federal de Educação, Ciência e Tecnologia do Amazonas, 1672, 69075-351 Manaus, Amazonas (Brazil); Biasi, R.S. de [Seção de Engenharia Mecânica e de Materiais, Instituto Militar de Engenharia, 22290-270 Rio de Janeiro (Brazil)

    2016-02-01

    A nanostructured SnSe{sub 2} phase was successfully produced by mechanical alloying. The influence of defect centers on the structural, optical and photoacoustic properties of the alloy was investigated by annealing the as-milled SnSe{sub 2} powder. From optical absorbance and photoacoustic absorption measurements, the energy band gap, E{sub g}, and the thermal diffusivity, α, values were determined for as-milled and annealed samples. The thermal conductivity values for the as-milled and annealed samples were estimated by using the α values obtained from the photoacoustic measurements, the density values obtained from the Rietveld refinement of the X-ray diffraction patterns and the specific heat value for the bulk SnSe{sub 2} phase. These values were used to estimate the dimensionless figure of merit ZT. It was evidenced that the ZT parameter of the as-milled nanostructured SnSe{sub 2} sample is almost twice larger than the ZT of the annealed sample. - Highlights: • Nanostructured SnSe{sub 2} was produced using Mechanical Alloying technique. • As milled sample has a high fraction of interfacial component (80%). • Thermal diffusivity value for nanostructured SnSe{sub 2} was a new report in literature.

  15. Azo polymers with electronical push and pull structures prepared via RAFT polymerization and its photoinduced birefringence behavior

    Directory of Open Access Journals (Sweden)

    2008-08-01

    Full Text Available Two methacrylate monomers containing azo and electronical push and pull structure, e.g. 2-Methyl-acrylic-acid-2-{[4-(4-cyano-phenylazo-3-methyl-phenyl]-ethyl-amino-ethyl ester (MACP with cyano substituted and 2-Methylacrylic-acid-2-{ethyl-[4-(4-methoxy-phenylazo-3-methyl-phenyl]-amino}-ethyl ester (MAMP with methoxy substituted, were synthesized and polymerized using 2-cyanoprop-2-yl dithiobenzoate (CPDB as chain transfer agent and 2,2'-azobisisobutyronitrile (AIBN as initiator. The results showed that the polymerization displayed characteristics of ‘living’/controlled free radical polymerization. Thus, the obtained polymers, polyMACP (pMACP and polyMAMP (pMAMP, had controlled molecular weights and narrow molecular weights distribution. The chain extension experiments of pMACP and pMAMP using styrene as the second monomer were successfully carried out. The photo-induced trans-cis-trans isomerization kinetic of pMACP and pMAMP in chloroform solution were described. Marked differences in rate for the trans-cis and cis-trans isomerization of pMACP and pMAMP were observed in chloroform solution due to the different electronic effects in these two polymers. Photoinduced birefringence and surface relief grating (SRG of the pMACP and pMAMP were investigated in thin film state.

  16. Spectral, structural, optical and dielectrical studies of UV irradiated Rose Bengal thin films prepared by spin coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Zeyada, H.M., E-mail: hzeyada@gmail.com [Department of Physics, Faculty of Science at New Damietta, University of Damietta, 34517 (Egypt); Youssif, M.I.; El-Ghamaz, N.A. [Department of Physics, Faculty of Science at New Damietta, University of Damietta, 34517 (Egypt); Aboderbala, M.E.O. [Department of Physics, Faculty of Science at New Damietta, University of Damietta, 34517 (Egypt); Department of Physics, Faculty of Science, AlJabl Al Gharbi University (Libya)

    2017-02-01

    Optical properties of pristine and UV irradiated Rose Bengal (RB) films have been investigated using transmittance and reflectance methods. The refractive index(n) and extinction coefficient (k) have been calculated from the absolute values of transmission and reflection spectrum. Single oscillator parameters and Drude model of free carrier absorption have been applied for analysis of the refractive index dispersion. Within the frame work of the band-to-band electron transitions theory; the fundamental absorption edge data were analyzed. Our results suggest that thickness of RB films has no effect on the absorption or the refractive indices in the investigated thicknesses range and within the experimental error. Structural transformation of films from amorphous to polycrystalline has been observed upon UV irradiation. Accordingly, the decreases of all of the absorption coefficient, the energy gap and the refractive index of RB films have been detected. Furthermore, the dependence of the optical functions on UV exposure times has been discussed based on the spectral distribution of the dielectric constant.

  17. Preparation of Gc protein-derived macrophage activating factor (GcMAF) and its structural characterization and biological activities.

    Science.gov (United States)

    Mohamad, Saharuddin Bin; Nagasawa, Hideko; Uto, Yoshihiro; Hori, Hitoshi

    2002-01-01

    Gc protein has been reported to be a precursor of Gc protein-derived macrophage activation factor (GcMAF) in the inflammation-primed macrophage activation cascade. An inducible beta-galactosidase of B cells and neuraminidase of T cells convert Gc protein to GcMAF. Gc protein from human serum was purified using 25(OH)D3 affinity column chromatography and modified to GcMAF using immobilized glycosidases (beta-galactosidase and neuraminidase) The sugar moiety structure of GcMAF was characterized by lectin blotting by Helix pomatia agglutinin. The biological activities of GcMAF were evaluated by a superoxide generation assay and a phagocytosis assay. We successfully purified Gc protein from human serum. GcMAF was detected by lectin blotting and showed a high biological activity. Our results support the importance of the terminal N-acetylgalactosamine moiety in the GcMAF-mediated macrophage activation cascade, and the existence of constitutive GcMAF in human serum. These preliminary data are important for designing small molecular GcMAF mimics.

  18. Effect of precursor concentration on the structural and optical properties of ZnO nanorods prepared by hydrothermal method

    International Nuclear Information System (INIS)

    Lestari, Amie; Iwan, S.; Djuhana, Dede; Imawan, Cuk; Harmoko, Adhi; Fauzia, Vivi

    2016-01-01

    Zinc oxide (ZnO) nanorods has attractive properties for nanoscale optoelectronic applications, such as optical sensors, ultraviolet laser diodes, and photodetectors. ZnO nanorods, can be fabricated by simple and low cost chemical approach, such as hydrothermal method. In this method, the morphology, microstructure, optical and electrical properties of ZnO nanorods are highly determined by process parameters such as solvent, deposition time, deposition temperature as well as annealing condition. In this paper we report the fabrication of ZnO nanorods that were grown on transparent conducting indium tin oxide coated glass substrates. Initially, ZnO seed layers were deposited on heated substrates with temperature of 450 °C using ultrasonic spray pyrolysis method with frequency of 1.7 MHz and then grown by hydrothermal method with three different precursor concentrations, namely 0.02 M, 0.06 M, and 0.1 M. The surface morphology and structure were investigated by field emission scanning electron microscope (FESEM) and x-ray diffraction (XRD), while the optical properties were observed by photoluminescence (PL) and and UV VIS reflectance spectroscopy.

  19. Optical properties and crystal structure of Eu3+ -doped Y2O3 crystals prepared under different conditions and with different methods

    International Nuclear Information System (INIS)

    Chung, Yong Hwa; Jang, Ki Wan; Kim, Il Gon; Kim Sang Su; Lee, Yong Ill; Park, Seong Tae; Seo, Hyo Jin

    2003-01-01

    The optical properties and the crystal structure of 6-mol% Eu 3+ -doped Y 2 O 3 powders prepared under different conditions and with different methods were studied through emission spectroscopy and X-ray powder diffraction. All samples exhibited the normal fluorescence spectrum of Eu 3+ -doped cubic Y 2 O 3 powders. The peak positions of the 5 D 0 → 7 F 0 transitions of Eu 3+ ions were shifted to the short-wavelength direction as the sintering temperature was lowered or the size of the host particle itself was decreased. The dynamic properties, such as the rise or the decay time of the 5 D 0 → 7 F 2 transition, depended on other factors than the size of the grain contained in each particle and the size of host particle itself. The morphologies of the studied samples were also observed by using a scanning electron microscope

  20. Structural and optical characterization of In{sub 2}O{sub 3}/PANI nanocomposite prepared by in-situ polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Janeoo, Shashi; Sharma, Mamta, E-mail: mamta.phy85@gmail.com; Goswamy, J. [Department of Applied Sciences (Physics), UIET, Panjab University, Chandigarh-160 014 (India); Singh, Gurinder [Department of Applied Sciences (Physics), UIET, PUSSGSRC, Hoshiarpur (Punjab) (India)

    2016-05-23

    Polyaniline-indium oxide (In{sub 2}O{sub 3}/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In{sub 2}O{sub 3} nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In{sub 2}O{sub 3}/PANI nanocomposite. TEM analysis shows In{sub 2}O{sub 3} nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In{sub 2}O{sub 3} nanoparticles. The band gap and electronic transitions in In{sub 2}O{sub 3}/PANI nanocomposite is determined by using UV/Vis spectra.