3 D Co3 (PO4 )2 -Reduced Graphene Oxide Flowers for Photocatalytic Water Splitting: A Type II Staggered Heterojunction System.

Science.gov (United States)

Samal, Alaka; Swain, Smrutirekha; Satpati, Biswarup; Das, Dipti Prakasini; Mishra, Barada Kanta

2016-11-23

The design, synthesis, and photoelectrochemical characterization of Co 3 (PO 4 ) 2 , a hydrogen evolving catalyst modified with reduced graphene oxide (RGO), is reported. The 3 D flowerlike Co 3 (PO 4 ) 2 heterojunction system, consisting of 3 D flowerlike Co 3 (PO 4 ) 2 and RGO sheets, was synthesized by a one-pot in situ photoassisted method under visible-light irradiation, which was achieved without the addition of surfactant or a structure-directing reagent. For the first time, Co 3 (PO 4 ) 2 is demonstrated to act as a hydrogen evolving catalyst rather than being used as an oxygen evolving photoanode. In particular, 3 D flowerlike Co 3 (PO 4 ) 2 anchored to RGO nanosheets is shown to possess dramatically improved photocatalytic activity. This enhanced photoactivity is mainly due to the staggered type II heterojunction system, in which photoinduced electrons from 3 D flowerlike Co 3 (PO 4 ) 2 transfer to the RGO sheets and result in decreased charge recombination, as evidenced by photoluminescence spectroscopy. The band gap of Co 3 (PO 4 ) 2 was calculated to be 2.35 eV by the Kubelka-Munk method. Again, the Co 3 (PO 4 ) 2 semiconductor displays n-type behavior, as observed from Mott-Schottky measurements. These RGO-Co 3 (PO 4 ) 2 conjugates are active in the visible range of solar light for water splitting and textile dye degradation, and can be used towards the development of greener and cheaper photocatalysts by exploiting solar light. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Redox process catalysed by growing crystal-strengite, FePO4,2H2O, crystallizing from solution with iron(II) and hydroxylamine

Science.gov (United States)

Lundager Madsen, Hans Erik

2014-09-01

In an attempt to grow pure crystals of the iron(II) phosphate vivianite, Fe3(PO4)2,8H2O, from a solution of Mohr's salt, Fe(NH4)2(SO4)2,6H2O, added to a solution of ammonium phosphate, hydroxylammonium chloride, NH3OHCl, was added to the iron(II) stock solution to eliminate oxidation of iron(II) by oxygen from the air. However, the effect turned out to be the opposite of the expected: whereas hydroxylamine reduces iron(III) in bulk solution, it acted as a strong oxidant in the presence of growing iron phosphate crystals, causing the crystallization of the iron(III) phosphate strengite, FePO4,2H2O, as the only solid phase. Evidently the crystal surface catalyses oxidation of iron(II) by hydroxylamine. The usual composite kinetics of spiral growth and surface nucleation was found. The surface-nucleation part yielded edge free energy λ in the range 12-45 pJ/m, virtually independent of temperature and in the range typical for phosphates of divalent metals. The scatter of values for λ presumably arises from contributions from different crystal forms to the overall growth rate. The low mean value points to strong adsorption of iron(II), which is subsequently oxidized at the crystal surface, forming strengite. The state of the system did not tend to thermodynamic equilibrium, but to a metastable state, presumably controlled by the iron(II) rich surface layer of the crystal. In addition to crystal growth, it was possible to measure nucleation kinetics by light scattering (turbidimetry). A point of transition from heterogeneous to homogeneous nucleation was found, and from the results for the homogeneous domain a rather precise value of crystal surface free energy γ=55 mJ/m2 was found. This is a relatively low value as well, indicating that the redox process plays a role already at the nucleation stage.

Mechanism of intercalation in protonic conductors: case of HUP (H3OUO2PO4, 3H2O) and the corresponding xerogel [(UO2)sub(1.5-x) PO4Hsub(2x),2H2O

International Nuclear Information System (INIS)

Colomban, P.; Pham Thi, M.

1985-01-01

Intercalation of acetone alkylammonium, methylviologen and cobalticinium ions in HUP framework (H 3 OUO 2 PO 4 .3H 2 O) have been studied with different methods (IR and Raman spectroscopies, X-ray diffraction, DSC and scanning electron microscopy). Various reactions have been pointed out: i.e. proton transfer from H 3 O + to PO 4 3- , ionisation of cobaltocene into cobalticinium. Species orientation is discussed and its influence on conductivity and phase transitions [fr

Neutralization of Na2PO4: Reaction between Na3PO4 and CaCL2

International Nuclear Information System (INIS)

Xia Shenglan; Wang Luning

1990-01-01

The results of reaction Na 3 PO 4 with CaCl 2 in water at ambient and higher temperature are described. The reaction rate of Na 3 PO 4 with CaCl 2 is slow at ambient temperature and the reaction is complete at 260 deg C after 2 h. The products are Ca(OH) 2 and Ca 5 (PO 4 ) 3 (OH). The quantity of them is dependent upon the quanity of Na 3 PO 4 and CaCl 2 contained in water, all of them control pH of water

H3PO4 imbibed polyacrylamide-graft-chitosan frameworks for high-temperature proton exchange membranes

Science.gov (United States)

Yuan, Shuangshuang; Tang, Qunwei; He, Benlin; Chen, Haiyan; Li, Qinghua; Ma, Chunqing; Jin, Suyue; Liu, Zhichao

2014-03-01

Proton exchange membrane (PEM), transferring protons from anode to cathode, is a key component in a PEM fuel cell. In the current work, a new class of PEMs are synthesized benefiting from the imbibition behavior of three-dimensional (3D) polyacrylamide-graft-chitosan (PAAm-graft-chitosan) frameworks to H3PO4 aqueous solution. Interconnected 3D framework of PAAm-graft-chitosan provides tremendous space for holding proton-conducting H3PO4. The highest anhydrous proton conductivity of 0.13 S cm-1 at 165 °C is obtained. A fuel cell using a thick membrane as a PEM showed a peak power density of 405 mW cm-2 with O2 and H2 as the oxidant and fuel, respectively. Results indicate that the interconnected 3D framework provides superhighway for proton conduction. The valued merits on anhydrous proton conductivity, huge H3PO4 loading, and easy synthesis promise the new membranes to be good alternatives as high-temperature PEMs.

Facile synthesis technology of Li_3V_2(PO_4)_3/C adding H_2O_2 in ball mill process

International Nuclear Information System (INIS)

Min, Xiujuan; Mu, Deying; Li, Ruhong; Dai, Changsong

2016-01-01

Highlights: • Sintering time of Li_3V_2(PO_4)_3 reduced to 6 hours by adding hydrogen peroxide. • Electrochemical performance of Li_3V_2(PO_4)_3 was improved by reducing sintering time. • The Li_3V_2(PO_4)_3 production process was simplified during material synthesis stage. - Abstract: Li_3V_2(PO_4)_3/C has stable structure, high theory specific capacity and good safety performance, therefore it has become the research focus of lithium-ion batteries in recent years. The facile synthesis technology of Li_3V_2(PO_4)_3/C was characterized by adding different amounts of H_2O_2. Structure and morphology characteristics were examined by XRD, TG, Raman Spectroscopy, XPS and SEM. Electrochemical performance was investigated by constant current charging and discharging test. The results revealed that the Li_3V_2(PO_4)_3/C electrochemical performance of adding 15 mL H_2O_2 was better after sintering during 6 h. At the charge cut-off voltage of 4.3 V, the first discharge capacity at 0.2 C rate reached 127 mAh g"−"1. Because of adding H_2O_2 in the ball-mill dispersant, the vanadium pentoxide formed the wet sol. The molecular-leveled mixture increased the homogeneity of raw materials. Therefore, the addition of H_2O_2 shortened the sintering time and significantly improved the electrochemical performance of Li_3V_2(PO_4)_3/C.

Electrochemical behaviours of Eu(III/E(II and Ce(IV/Ce(III in H3PO4-H2O media : solvation and complexation reactions

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Belqat B.

2018-01-01

Full Text Available Many kinds of rare earth elements (REE such as europium and cerium have been make them essential elements in many high-tech components. The electrochemical studies can be presented as an interesting indication for europium and cerium extraction from phosphoric solutions, including solvation and complexation reactions. The normal redox potentials of Eu3+/Eu2+ and Ce4+/Ce3+ systems have been determined in H3PO4-H2O media with various phosphoric acid concentration. The solvation of these elements in phosphoric media is characterized by their transfer activity coefficients "f" calculated from the corresponding normal redox potentials. The corresponding solvation increases with increasing the H3PO4 concentration. For each REE, the electrochemical properties depend on its number of charges and on its basic properties. Results suggest that solvation and complexation of REE phosphates are important in controlling REE concentration.

A new set of K3Fe3(PO4)4·yH2O (0 ≤ y ≤ 1) layered phases obtained by topotactic reactions

Science.gov (United States)

Trad, Khiem; Wattiaux, Alain; Ben Amara, Mongi; Delmas, Claude; Carlier, Dany

2018-06-01

K3Fe3(PO4)4·H2O powder was synthesized by Na+/K+ exchange reaction from Na3Fe3(PO4)4 in aqueous medium. The replacement of the sodium cations by the potassium larger ones and water molecules causes a structural distortion leading to P2/n monoclinic K3Fe3(PO4)4·H2O. This new layered phase was characterized by XRD, Mössbauer spectroscopy and magnetic measurements. The study of its thermal stability reveals that other new layered K3Fe3(PO4)4·yH2O with (0 ≤ y ≤ 1) phases can be stabilized up to 600 °C and finally at higher temperature a new K3Fe3(PO4)4 polymorph with a different structural type is irreversibility formed.

High efficient multifunctional Ag_3PO_4 loaded hydroxyapatite nanowires for water treatment

International Nuclear Information System (INIS)

Li, Yaling; Zhou, Hangyu; Zhu, Genxing; Shao, Changyu; Pan, Haihua; Xu, Xurong; Tang, Ruikang

2015-01-01

Highlights: • The multifunctional Ag_3PO_4 loaded hydroxyapatite (HAP) nanowires were synthesized via a facile in-situ precipitation method. • By optimizing the initial concentration of AgNO_3, the well-distributed Ag_3PO_4/HAP composites could be achieved. • The Ag_3PO_4/HAP composites showed excellent photocatalytic performance for the decomposition of dyes under visible light irradiation. • The maximum absorption capacity of the Ag_3PO_4/HAP composites for Pb(II) was 250 mg/g, approximately three times as that of pure HAP. • The Ag_3PO_4/HAP composites also exhibited excellent antibacterial activities even at relative low concentrations. - Abstract: Organic, inorganic, and biological pollutants are typical water contaminants and they seriously affect water quality. In this study, we suggested that a novel multifunctional Ag_3PO_4 loaded hydroxyapatite (HAP) material can remove the typical pollutants from water. The Ag_3PO_4/HAP composites were synthesized facilely via in-situ precipitation of Ag_3PO_4 on the pre-existing HAP nanowires. By optimizing the composition of Ag_3PO_4 and HAP, the material could achieve an optimal photocatalytic activity to decompose rhodamine B (RhB), methyl orange (MO) and methylene blue (MB) under visible light irradiations with enhanced pH stability. Besides, the adsorption of Pb(II) on the Ag_3PO_4/HAP reached a maximum capacity of 250 mg/g and this value was approximately three times as that of pure HAP. Furthermore, the composite material exhibited excellent antibacterial activities towards gram-negative bacterium (Escherichia coli) and gram-positive bacterium (Stphylococcus aureus). The results highlighted the cooperative effect between Ag_3PO_4 and hydroxyapatite (HAP). The simultaneous removals of dyes, toxic metal ions, and bacteria with a high efficiency followed an easy approach for the purification of contaminated water via the rationally designed material, in which the Ag_3PO_4/HAP composite might be developed

On thermal expansion of RbD2PO4, CsH2PO4 and CsDrPO4 crystals

International Nuclear Information System (INIS)

Vlokh, O.G.; Shchur, Ya.I.; Klymiv, I.M.

1994-01-01

Thermal expansion of RbD 2 PO 4 , CsH 2 PO 4 , CsD 2 PO 4 crystals in a wide range of temperatures embracing points of phase transitions was studied. An explanation of anomalous behaviour of thermal expansion factor along directions b and c in the course of RbD 2 PO 4 transfer into intermediate phase was suggested. 10 refs., 4 figs

Ferroelectric phase transition in hydrogen-bonded 2-aminopyridine phosphate (NC sub 4 H sub 4 NH sub 2)centre dot H sub 3 PO sub 4

CERN Document Server

Czapla, Z; Waskowska, A

2003-01-01

A new crystal of 2-aminopyridine phosphate (NC sub 4 H sub 4 NH sub 2)centre dot H sub 3 PO sub 4 has been grown and its x-ray structure and physical properties were studied. At room temperature the crystals are monoclinic, space group C2/c. The flat 2-aminopyridine cations are hydrogen bonded to the anionic [PO sub 4 ] groups. The interesting feature of the crystal structure is the three-dimensional network of hydrogen bonds including, among others, two strong, symmetrical O centre dot centre dot centre dot H, H centre dot centre dot centre dot O interactions with disordered proton locations. Symmetrically related PO sub 4 anions linked through these protons form infinite (PO sub 4) subinfinity chains along the crystal a-axis. The anomalies in the temperature dependence of the electric permittivity showed that the crystal undergoes ferroelectric phase transition at T sub c = 103.5 K. The spontaneous polarization takes place along the crystal a-axis, being parallel to the chains of the hydrogen-bonded PO sub ...

Corrosion characteristics of an aluminium alloy in the H3PO4 - CO2 mixture

International Nuclear Information System (INIS)

Aljinovic, Lj.; Smith, M.; Gotovac, V.

1998-01-01

The Al 6063 alloy examined in this work contains silicon and magnesium capable of forming Mg 2 Si and iron, which can form an intermetallic second phase (FeAl 3 ). In order to examine the influence of temperature on the corrosion behaviour of the Al 6063 alloy, examinations were carried out in aerated H 3 PO 4 and in H 3 PO 4 saturated with CO 2 at temperatures of 20, 30, 40, and 50 C. The following electrochemical methods were applied: determination of dependence of E OCP on time, recording of anodic and cathodic polarization curves, and cyclic voltammetry. It has been observed that corrosion parameters obtained are strongly temperature dependent. They also depend on CO 2 dissolved in H 3 PO 4 . CO 2 retards cathodic and anodic reactions at all temperatures, which can be attributed to formation of a kind of mechanical passivity as alloy components react with CO 2 . (orig.)

H2O2 rejuvenation-mediated synthesis of stable mixed-morphology Ag3PO4 photocatalysts

Directory of Open Access Journals (Sweden)

Henry Agbe

2018-04-01

Full Text Available Ag3PO4 photocatalyst has attracted interest of the scientific community in recent times due to its reported high efficiency for water oxidation and dye degradation. However, Ag3PO4 photo-corrodes if electron accepter such as AgNO3 is not used as scavenger. Synthesis of efficient Ag3PO4 followed by a simple protocol for regeneration of the photocatalyst is therefore a prerequisite for practical application. Herein, we present a facile method for the synthesis of a highly efficient Ag3PO4, whose photocatalytic efficiency was demonstrated using 3 different organic dyes: Methylene Blue (MB, Methyl orange (MO and Rhodamine B (RhB organic dyes for degradation tests. Approximately, 19 % of Ag3PO4 is converted to Ag0 after 4.30 hours of continuous UV-Vis irradiation in presence of MB organic dye. We have shown that the Ag/Ag3PO4 composite can be rejuvenated by a simple chemical oxidation step after several cycles of photocatalysis tests. At an optimal pH of 6.5, a mixture of cubic, rhombic dodecahedron, nanosphere and nanocrystals morphologies of the photocatalyst was formed. H2O2 served as the chemical oxidant to re-insert the surface metallic Ag into the Ag3PO4 photocatalyst but also as the agent that can control morphology of the regenerated as-prepared photocatalyst without the need for any other morphology controlling Agent (MCA. Surprisingly, the as- regenerated Ag3PO4 was found to have higher photocatalytic reactivity than the freshly made material and superior at least 17 times in comparison with the conventional Degussa TiO2, and some of TiO2 composites tested in this work. Keywords: Materials chemistry, Materials science, Engineering

Structural transitions, ion mobility, and conductivity in CsSbF3(H2PO4)

Science.gov (United States)

Kavun, V. Ya.; Uvarov, N. F.; Slobodyuk, A. B.; Ulihin, A. S.; Kovaleva, E. V.; Zemnukhova, L. A.

2018-02-01

Structural transitions, ion mobility, and conductivity in CsSbF3(H2PO4) (I) have been investigated by the methods of 1H, 19F, 31P NMR (including 1H, 19F, 31P MAS NMR), DSC, X-ray diffraction, and impedance spectroscopy. It was found that the fundamental changes in 1H, 19F, 31P NMR spectra (above 390 K) were associated with the formation of a crystalline disorder phase I with high ionic mobility in the proton and fluoride sublattices, as a result of a phase transition in the 400-420 K range. In the same temperature range, the transition of PO2(OH)2- anions from the "rigid lattice" to fast reorientations takes place. Above 430 K, there occurs a transition from the crystalline disordered phase to the amorphous one. The types of ion mobility in CsSbF3(H2PO4) and its amorphous phase have been established and temperature ranges of their realization have been determined (150-450 K). According to the NMR data, the diffusion in the proton sublattice of the disordered crystalline and amorphous phases is preserved even at room temperature. The ionic conductivity in CsSbF3(H2PO4) reaches the values of 2.6 × 10-4 S/cm in the temperature range 410-425 K and decreases down to 2.0 × 10-5 S/cm upon transition to the amorphous phase (435-445 K).

Formation of condensed phosphates when heating CdO with NH4H2PO4

International Nuclear Information System (INIS)

Atstinya, L.Zh.; Dindune, A.P.; Konstant, Z.A.

1987-01-01

A study was made on process of CdO thermal condensation with NH 4 H 2 PO 4 depending on the ratio of basic substances and temperature synthesis conditions. It was established that reaction between CdO and NH 4 H 2 PO 4 of pure for analysis grade was initiated when basic mixtures were pounded with a pestle. Heating of cadmium-ammonium triphosphate with products of ammonium dihydrophosphate polycondensation in 330-350 deg C range resulted to CdNH 4 (PO 3 ) 3 formation. Exoeffect on DTA curves corresponded at 540 deg C to formation of α-Cd(PO 3 ) 2 . α-Cd(PO 3 ) 2 → β-Cd(PO 3 ) 2 transition took place at 810 deg C with successive melting of β-Cd(PO 3 ) 2 at 850 deg C, which was supported by the DTA curve and sharp change of the relative electric conductivity

Formation and transformations of radicals in frozen aqueous solutions of components of nucleic acids and H3PO4

International Nuclear Information System (INIS)

Minkhadzhidinova, D.R.; Chefranova, O.A.; Sharpatyj, V.A.

1977-01-01

Radiolysis of frozen aqueous solutions of 6-16 M H 3 PO 4 and 5 M NaH 2 PO 4 was studied, as well as radiolysis of these systems in the presence of nitrous bases and glucose. In aqueous solutions of H 3 PO 4 and NaH 2 PO 4 irradiated at 77 K, two groups of radicals formed as a result of interaction of the oxidative component of radiolysis of water with phosphate ions were identified. Their photolytic properties were studied. Primary products of radiolysis of the nitrous bases in phosphoric- acid solutions are anion- and cation-radicals. The molal absorption coefficients of the particles were determined

Separation of the components of the TBP-H2 MBP-HDBP-H3PO4 mixture

International Nuclear Information System (INIS)

Pires, M.A.F.; Abrao, A.

1981-04-01

Several schemes for the separation of dibutylphosphoric acid (HDBP), monobutylphosphoric acid (H 2 MBP) and orthophosphoric acid (H 3 PO 4 ) as hydrolytic and radiolytic degradation products from tri-n-butylphosphate (TBP) were studied. For the resolution of a HDBP, H 2 MPB and H 3 PO 4 mixture in TBP-diluent, or in TBP-diluent-heavy metal nitrate (U-VI, Th-IV or Zr-IV), techniques such as ion exchange chromatography, ion chromatography and separation onto a chromatographic alumina column were investigated. For the identification, determination and analytical resolution following up for the several systems studied, techniques such as refraction index measurement, electrical conductivity measurement, molecular spectrophotometry and gas chromatography were applied. Special emphasys was given to the separation using alumina column where the HDBP acid was retained and eluted selectively for its separation from TBP-varsol-uranyl nitrate mixtures. This analytical procedure was applied to the samples coming from the Uranium Purification Pilot Plant in operation at the Centro de Engenharia Quimica (IPEN). (Author) [pt

Crystal structures and magnetic properties of iron (III)-based phosphates: Na{sub 4}NiFe(PO{sub 4}){sub 3} and Na{sub 2}Ni{sub 2}Fe(PO{sub 4}){sub 3}

Energy Technology Data Exchange (ETDEWEB)

Essehli, Rachid, E-mail: rachid_essehli@yahoo.fr [Laboratory of Mineral Solid and Analytical Chemistry ' LCSMA' , Department of Chemistry, Faculty of Sciences, University Mohamed I, Po. Box 717, 60000 Oujda (Morocco); Bali, Brahim El [Laboratory of Mineral Solid and Analytical Chemistry ' LCSMA' , Department of Chemistry, Faculty of Sciences, University Mohamed I, Po. Box 717, 60000 Oujda (Morocco); Benmokhtar, Said [LCMS, Laboratoire de Chimie des Materiaux Solides, Departement de chimie, Faculte des Sciences Ben M' SIK, Casablanca (Morocco); Bouziane, Khalid [Physics Department, College of Science, Sultan Qaboos University, PO Box 36, Postal Code 123 Al Khod, Sultanate of Oman (Oman); Manoun, Bouchaib [Laboratoire de Physico-Chimie des Materiaux, Departement de Chimie, FST Errachidia, University Moulay Ismail, B.P. 509 Boutalamine, Errachidia (Morocco); Abdalslam, Mouner Ahmed [Materials Science, Technical University Darmstadt, Darmstadt (Germany); Ehrenberg, Helmut [IFW Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany)

2011-01-28

Graphical abstract: A perspective view of the Na{sub 2}Ni{sub 2}Fe(PO{sub 4}){sub 3} structure along the [0 0 1] direction. Both compounds seem to exibit antiferromagnetic interactions between magnetic entities at low temperature. Display Omitted Research highlights: > Nasicon and Alluaudite compounds, Iron(III)-based phosphates, Crystal structures of Na{sub 4}NiFe(PO{sub 4}){sub 3} and Na{sub 2}Ni{sub 2}Fe(PO{sub 4}){sub 3}. > Magnetism behaviours of Na{sub 4}NiFe(PO{sub 4}){sub 3} and Na{sub 2}Ni{sub 2}Fe(PO{sub 4}){sub 3}. > Antiferromagnetism interactions. > Mossbauer spectroscopy. - Abstract: Crystal structures from two new phosphates Na{sub 4}NiFe(PO{sub 4}){sub 3} (I) and Na{sub 2}Ni{sub 2}Fe(PO{sub 4}){sub 3} (II) have been determined by single crystal X-ray diffraction analysis. Compound (I) crystallizes in a rhombohedral system (S. G: R-3c, Z = 6, a = 8.7350(9) A, c = 21.643(4) A, R{sub 1} = 0.041, wR{sub 2}=0.120). Compound (II) crystallizes in a monoclinic system (S. G: C2/c, Z = 4, a = 11.729(7) A, b = 12.433(5) A, c = 6.431(2) A, {beta} = 113.66(4){sup o}, R{sub 1} = 0.043, wR{sub 2}=0.111). The three-dimensional structure of (I) is closely related to the Nasicon structural type, consisting of corner sharing [(Ni/Fe)O{sub 6}] octahedra and [PO{sub 4}] tetrahedra forming [NiFe(PO{sub 4}){sub 3}]{sup 4+} units which align in chains along the c-axis. The Na{sup +} cations fill up trigonal antiprismatic sites within these chains. The crystal structure of (II) belongs to the alluaudite type. Its open framework results from [Ni{sub 2}O{sub 10}] units of edge-sharing [NiO{sub 6}] octahedra, which alternate with [FeO{sub 6}] octahedra that form infinite chains. Coordination of these chains yields two distinct tunnels in which site Na{sup +}. The magnetization data of compound (I) reveal antiferromagnetic (AFM) interactions by the onset of deviations from a Curie-Weiss behaviour at low temperature as confirmed by Moessbauer measurements performed at 4.2 K. The

Complex phosphates in the Li(Na)3PO4-InPO4 systems

International Nuclear Information System (INIS)

Potapova, A.M.; Zimina, G.V.; Smirnova, I.N.; Novoselov, A.V.; Spiridonov, F.M.; Stefanovich, S.Yu.

2008-01-01

Subsolidus sections in the systems Li 3 PO 4 -InPO 4 (950 deg C) and Na 3 PO 4 -InPO 4 (800, 900, and 1000 deg C) have been studied by X-ray powder diffraction. The compound Li 3 In(PO 4 ) 2 has been synthesized, and the NASICON-type solid solution Li 3(1-x) In 2+x (PO 4 ) 3 (0.67 ≤ x ≤ 0.80) has been found to exist. In the system Na 3 PO 4 -InPO 4 , the solid solution Na 3(1-x) In x/3 PO 4 (0 ≤ x ≤ 0.2) and two complex phosphates exist: Na 3 In(PO 4 ) 2 and Na 3 In 2 (PO 4 ) 3 . These complex phosphates are dimorphic, with the irreversible-transition temperature equal to 675 and 820 deg C, respectively. Na 3 In(PO 4 ) 2 degrades at 920 deg C. Ionic conductivity has been measured in some phases in the system [ru

Synthesis, crystal structure, optical and thermal properties of lanthanide hydrogen-polyphosphates Ln[H(PO3)4] (Ln = Tb, Dy, Ho).

Science.gov (United States)

Förg, Katharina; Höppe, Henning A

2015-11-28

Lanthanide hydrogen-polyphosphates Ln[H(PO3)4] (Ln = Tb, Dy, Ho) were synthesised as colourless (Ln = Tb, Dy) and light pink (Ln = Ho) crystalline powders by reaction of Tb4O7/Dy2O3/Ho2O3 with H3PO3 at 380 °C. All compounds crystallise isotypically (P2(1)/c (no. 14), Z = 4, a(Tb) = 1368.24(4) pm, b(Tb) = 710.42(2) pm, c(Tb) = 965.79(3) pm, β(Tb) = 101.200(1)°, 3112 data, 160 parameters, wR2 = 0.062, a(Ho) = 1363.34(5) pm, b(Ho) = 709.24(3) pm, c(Ho) = 959.07(4) pm, β(Ho) = 101.055(1)°, 1607 data, 158 parameters, wR2 = 0.058). The crystal structure comprises two different infinite helical chains of corner-sharing phosphate tetrahedra. In-between these chains the lanthanide ions are located, coordinated by seven oxygen atoms belonging to four different polyphosphate chains. Vibrational, UV/Vis and fluorescence spectra of Ln[H(PO3)4] (Ln = Tb, Dy, Ho) as well as Dy[H(PO3)4]:Ln (Ln = Ce, Eu) and the magnetic and thermal behaviour of Tb[H(PO3)4] are reported.

3.0 V High Energy Density Symmetric Sodium-Ion Battery: Na4V2(PO4)3∥Na3V2(PO4)3.

Science.gov (United States)

Yao, Xuhui; Zhu, Zixuan; Li, Qi; Wang, Xuanpeng; Xu, Xiaoming; Meng, Jiashen; Ren, Wenhao; Zhang, Xinhe; Huang, Yunhui; Mai, Liqiang

2018-03-28

Symmetric sodium-ion batteries (SIBs) are considered as promising candidates for large-scale energy storage owing to the simplified manufacture and wide abundance of sodium resources. However, most symmetric SIBs suffer from suppressed energy density. Here, a superior congeneric Na 4 V 2 (PO 4 ) 3 anode is synthesized via electrochemical preintercalation, and a high energy density symmetric SIB (Na 3 V 2 (PO 4 ) 3 as a cathode and Na 4 V 2 (PO 4 ) 3 as an anode) based on the deepened redox couple of V 4+ /V 2+ is built for the first time. When measured in half cell, both electrodes show stabilized electrochemical performance (over 3000 cycles). The symmetric SIBs exhibit an output voltage of 3.0 V and a cell-level energy density of 138 W h kg -1 . Furthermore, the sodium storage mechanism under the expanded measurement range of 0.01-3.9 V is disclosed through an in situ X-ray diffraction technique.

Singlet ground state in the spin-1/2 weakly coupled dimer compound NH4[ (V2O3)2(4,4'-b p y ) 2(H2PO4)(PO4)2] .0.5 H2O

Science.gov (United States)

Arjun, U.; Kumar, Vinod; Anjana, P. K.; Thirumurugan, A.; Sichelschmidt, J.; Mahajan, A. V.; Nath, R.

2017-05-01

We present the synthesis and a detailed investigation of structural and magnetic properties of polycrystalline NH4[(V2O3)2(4,4'-b p y ) 2(H2PO4) (PO4)2] .0.5 H2O by means of x-ray diffraction, magnetic susceptibility, electron spin resonance, and 31P nuclear magnetic resonance measurements. Temperature-dependent magnetic susceptibility could be described well using a weakly coupled spin-1/2 dimer model with an excitation gap Δ /kB≃26.1 K between the singlet ground state and triplet excited states and a weak interdimer exchange coupling J'/kB≃4.6 K. A gapped chain model also describes the data well with a gap of about 20 K. The electron spin resonance intensity as a function of temperature traces the bulk susceptibility nicely. The isotropic Landé g factor is estimated to be about g ≃1.97 , at room temperature. We are able to resolve the 31P NMR signal as coming from two inequivalent P sites in the crystal structure. The hyperfine coupling constant between 31P nucleus and V4 + spins is calculated to be Ahf(1 ) ≃2963 Oe/μB and Ahf(2 ) ≃1466 Oe/μB for the P(1) and P(2) sites, respectively. Our NMR shift and spin-lattice relaxation rate for both the 31P sites show an activated behavior at low temperatures, further confirming the singlet ground state. The estimated value of the spin gap from the NMR data measured in an applied field of H =9.394 T is consistent with the gap obtained from the magnetic susceptibility analysis using the dimer model. Because of a relatively small spin gap, NH4[(V2O3)2(4,4'-b p y ) 2(H2PO4) (PO4)2] .0.5 H2O is a promising compound for further experimental studies under high magnetic fields.

Analytical resolution of the mixture TBP-HDBP-H2MBP-H3PO4

International Nuclear Information System (INIS)

Pires, M.A.F.

1983-01-01

Several schemes for the separation of dibutylphosphoric acid (HDBP), main degradation product of tributylphosphate (TBP), in TBP/diluent, TBP/diluent-uranyl nitrate and TBP/diluent-thorium nitrate mixture were studied. For the resolution of HDBP-TBP/diluent-heavy metal nitrates (U-VI,Th-IV) systems, techniques such as: in exchange chromatography, ion chromatography using common ion exchangers and chromatographic separation with alumina column were investigated. For the identification, determination and analytical resolution following up the several systems studied, techniques such as refraction index measurement, electrical conductivity measurement, molecular absorption spectrophotometry, gas chromatography and ion chromatography, were applied. The separation of HDBP component was achieved using an alumina column where it was adsorbed from the TBP/diluent-uranyl nitrate and selectively eluted. Several modifications of this procedure for samples from the Uranium Purification Pilot Plant at Instituto de Pesquisas Energeticas e Nucleares (Sao Paulo, Brazil) were made. Special emphasis was given to the determination of HDBP using the ion chromatography technique. HDBP along with any monobutylphosphate acid (H 2 MBP) and phosphoric acid (H 3 PO 4 ) were stripped from the organic phase into dilute sodium hydroxide. HDBP is separated from H 2 MBP and H 3 PO 4 by ion chromatography and determined by its peak height. The determination of degradation products from TBP in TBP/diluent-uranyl nitrate and TBP/diluent-thorium nitrate systems was then performed. The detection limit for dibutylphosphate is 1.0μg HDBP/ml of analyte solution. (Author) [pt

Mixed phosphates of the Na3PO4 - LnPO4 systems

International Nuclear Information System (INIS)

Slivko, T.A.; Smirnova, I.N.; Zimina, G.V.; Spiridonov, F.M.; Chudinova, N.N.

2002-01-01

The phase relationships in the systems Na 3 PO 4 - LnPO 4 (subsolidus 950 Deg C cross-sections), where Ln=Sm, Eu, Tb, Dy, Ho, Tm, Yb, Lu, were studied by X-ray analysis. Reactions of the components were deduced, formed phases were separated and identified. The Na 6 Ln 3 (PO 4 ) 5 (Ln=Dy, Ho, Tm), Na 3 Ln 2 (PO 4 ) 3 (Ln=Tm, Yb, Lu) compounds and phases of the unstable composition Na 6+x Ln 3-x/3 (PO 4 ) 5 (Ln=Yb, Lu, 0 ≤ x ≤ 1.5) were detected for the first time. In all systems the existence of the Na 3-x Ln x/3 PO 4 unstable composition phase on the basis of the high temperature modification of sodium phosphate (sp. gr. Fm3m) is established, suggesting that stabilization of this modification by rare earth ions is possible [ru

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)

High efficient multifunctional Ag{sub 3}PO{sub 4} loaded hydroxyapatite nanowires for water treatment

Energy Technology Data Exchange (ETDEWEB)

Li, Yaling; Zhou, Hangyu; Zhu, Genxing [Center for Biomaterials and Biopathways, Department of Chemistry, Zhejiang University, Hangzhou (China); Shao, Changyu; Pan, Haihua; Xu, Xurong [Center for Biomaterials and Biopathways, Department of Chemistry, Zhejiang University, Hangzhou (China); Qiushi Academy for Advanced Studies, Zhejiang University (China); Tang, Ruikang, E-mail: rtang@zju.edu.cn [Center for Biomaterials and Biopathways, Department of Chemistry, Zhejiang University, Hangzhou (China); Qiushi Academy for Advanced Studies, Zhejiang University (China)

2015-12-15

Highlights: • The multifunctional Ag{sub 3}PO{sub 4} loaded hydroxyapatite (HAP) nanowires were synthesized via a facile in-situ precipitation method. • By optimizing the initial concentration of AgNO{sub 3}, the well-distributed Ag{sub 3}PO{sub 4}/HAP composites could be achieved. • The Ag{sub 3}PO{sub 4}/HAP composites showed excellent photocatalytic performance for the decomposition of dyes under visible light irradiation. • The maximum absorption capacity of the Ag{sub 3}PO{sub 4}/HAP composites for Pb(II) was 250 mg/g, approximately three times as that of pure HAP. • The Ag{sub 3}PO{sub 4}/HAP composites also exhibited excellent antibacterial activities even at relative low concentrations. - Abstract: Organic, inorganic, and biological pollutants are typical water contaminants and they seriously affect water quality. In this study, we suggested that a novel multifunctional Ag{sub 3}PO{sub 4} loaded hydroxyapatite (HAP) material can remove the typical pollutants from water. The Ag{sub 3}PO{sub 4}/HAP composites were synthesized facilely via in-situ precipitation of Ag{sub 3}PO{sub 4} on the pre-existing HAP nanowires. By optimizing the composition of Ag{sub 3}PO{sub 4} and HAP, the material could achieve an optimal photocatalytic activity to decompose rhodamine B (RhB), methyl orange (MO) and methylene blue (MB) under visible light irradiations with enhanced pH stability. Besides, the adsorption of Pb(II) on the Ag{sub 3}PO{sub 4}/HAP reached a maximum capacity of 250 mg/g and this value was approximately three times as that of pure HAP. Furthermore, the composite material exhibited excellent antibacterial activities towards gram-negative bacterium (Escherichia coli) and gram-positive bacterium (Stphylococcus aureus). The results highlighted the cooperative effect between Ag{sub 3}PO{sub 4} and hydroxyapatite (HAP). The simultaneous removals of dyes, toxic metal ions, and bacteria with a high efficiency followed an easy approach for the purification

Study on the Visible-Light Photocatalytic Performance and Degradation Mechanism of Diclofenac Sodium under the System of Hetero-Structural CuBi2O4/Ag3PO4 with H2O2

Directory of Open Access Journals (Sweden)

Xiaojuan Chen

2018-03-01

Full Text Available Two kinds of CuBi2O4/Ag3PO4 with different heterojunction structures were prepared based on the combination of hydrothermal and in-situ precipitation methods with surfactant additives (sodium citrate and sodium stearate, and their characteristics were systematically resolved by X-ray Diffraction (XRD, Brunauer–Emmett–Teller (BET, X-ray Photoelectron Spectroscopy (XPS, Scanning Electron Microscope (SEM/ High-resolution Transmission Electron Microscopy (HRTEM, UV-vis Diffuse Reflectance Spectra (DRS and Photoluminescence (PL. Meanwhile, the photocatalytic properties of the catalysts were determined for diclofenac sodium (DS degradation and the photocatalytic mechanism was also explored. The results indicate that both of the two kinds of CuBi2O4/Ag3PO4 exhibit higher photocatalytic efficiency, mineralization rate, and stability than that of pure CuBi2O4 or Ag3PO4. Moreover, the catalytic activity of CuBi2O4/Ag3PO4 can be further enhanced by adding H2O2. The free radical capture experiments show that in the pure CuBi2O4/Ag3PO4 photocatalytic system, the OH• and O2•− are the main species participating in DS degradation; however, in the CuBi2O4/Ag3PO4 photocatalytic system with H2O2, all OH•, h+, and O2•− take part in the DS degradation, and the contribution order is OH• > h+ > O2•−. Accordingly, the photocatalytic mechanism of CuBi2O4/Ag3PO4 could be explained by the Z-Scheme theory, while the catalysis of CuBi2O4/Ag3PO4 with H2O2 follows the heterojunction energy band theory.

Effect of H3PO4 Concentration and Particle Size of the Eggshell Used in Laying Hens Fed on Bone and Blood

Directory of Open Access Journals (Sweden)

S. Kismiati

2013-06-01

Full Text Available Normal 0 false false false IN X-NONE X-NONE MicrosoftInternetExplorer4 The objective of this research was to evaluate the effect of H3 PO4 concentrations and particle size of eggshell used in the feed of laying hens on bone and blood profiles. Ninety-six laying hens (Isa Brown strain age 25 weeks were kept in individual battery cage and divided into 8 groups randomly. Group 1 was fed using eggshell with out H3PO4 and particle size of <1 mm (feed 1 , group 2 was fed using eggshell that has been soaked in H3PO4 3% and particle size of <1 mm (feed 2, group 3 were fed using eggshell that has been soaked in H3PO4 4% and particle size of <1 mm (feed 3, group 4 was fed using eggshell that has been soaked in H3PO4 5% and particle size of <1 mm (feed 4, group 5 was fed using eggshell that has been soaked in H3PO4 and particle size of <3 mm (feed 5 , group of 6 was fed using eggshell that has been soaked in H3PO4 3% and particle size of <3 mm (feed 6, group 7 was fed using eggshell that has been soaked in H3PO4 4 % and particle size of <3 mm (feed 7 and a group of 8 was fed using eggshell that has been soaked in H3PO4 5% and particle size of <3 mm (feed 8. A Completely Randomized Design patterns factorial 4 x 2 x 3 was used in this research. Result of this research showed that had no interaction effect (P>0.05 between the H3PO4 concentration and particle size of eggshell on weight, volume, diameter of tibia bone and calcium and phosphorus content of the blood. The concentration of H3PO4 or particles size also had no effect (P>0.05 on all variables. Normal 0 false false false IN X-NONE X-NONE MicrosoftInternetExplorer4 /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-qformat:yes; mso-style-parent:""; mso-padding-alt:0cm 5.4pt 0cm 5.4pt; mso-para-margin:0cm; mso-para-margin-bottom:.0001pt; mso-pagination:widow-orphan; font

Batagayite, CaZn2(Zn,Cu)6(PO4)4(PO3OH)3·12H2O, a new phosphate mineral from Këster tin deposit (Yakutia, Russia): occurrence and crystal structure

Science.gov (United States)

Yakovenchuk, Victor N.; Pakhomovsky, Yakov A.; Konopleva, Nataliya G.; Panikorovskii, Taras L.; Bazai, Ayya; Mikhailova, Julia A.; Bocharov, Vladimir N.; Ivanyuk, Gregory Yu.; Krivovichev, Sergey V.

2017-12-01

Batagayite, CaZn2(Zn,Cu)6(PO4)4(PO3OH)3·12H2O, is a new secondary phosphate mineral from the Këster deposit, Arga-Ynnykh-Khai massif, NE Yakutia, Russia. It is monoclinic, P21, a = 8.4264(4), b = 12.8309(6), c = 14.6928(9) Å, β = 98.514(6)o, V = 1571.05(15) Å3 and Z = 2 (from single-crystal X-ray diffraction data). Batagayite crystals are blades up to 2 mm long, flattened on {001} and elongated on [100]; blades often grow in radial aggregates. Associated minerals are arsenolite, native copper, epifanovite, fluorapatite, libethenite, Na-analogue of batagayite, pseudomalachite, quartz, sampleite, tobermorite, and Mg-analogue of hopeite. The streak is white and the luster is vitreous. The mineral is brittle and has a perfect cleavage on {001}, no parting was observed. The Mohs hardness is 3. Density, determined by the float-sink method in Clerici solution, is 2.90(3) g/cm3, and the calculated density is 3.02 g/cm3 (using the empirical formula and single-crystal unit-cell parameters). Batagayite is biaxial, optically negative, α = 1.566 ± 0.002, β = 1.572 ± 0.002, γ = 1.573 ± 0.002 at 589 nm. 2V meas. = 40(5)°, 2V calc = 44.3°. Optical orientation: Z is perpendicular to (001), further details unclear. No dispersion or pleochroism were observed. The mean chemical composition determined by electron microprobe is: Na2O 0.31, MgO 1.39, Al2O3 0.55, SiO2 0.48, P2O5 34.37, K2O 0.17, CaO 2.76, MnO 1.03, CuO 5.80, ZnO 35.62, CdO 0.24 wt%. The H2O content estimated from the crystal-structure refinement is 16.83 wt%, giving a total of 99.55 wt%. The empirical formula calculated on the basis of P + Si = 7 is (Zn6.22Cu1.04Ca0.70Mg0.49Mn0.21Al0.15Na0.14K0.05Cd0.03)Σ9.03(P6.89Si0.11)Σ7.00O24.91(OH)3.09·12.10H2O. The mineral easily dissolves in 10% room-temperature HCl. The eight diagnostic lines in the X-ray powder-diffraction pattern are (I-d[Å]-hkl): 100-14.59-001, 25-6.34-012, 11-6.02-111, 37-4.864-003, 13-4.766-112, 20-3.102-1 \\overline {2} \\overline {4} , 11

Structure of LaH(PO3H)2.3H2O

International Nuclear Information System (INIS)

Loukili, M.; Durand, J.; Larbot, A.; Cot, L.; Rafiq, M.

1991-01-01

Lanthanum hydrogen bis(hydrogenphosphite) trihydrate, LaH(Po 3 H) 2 .3H 2 O, M r =353.8, monoclinic, P2 1 /c, a=9.687 (3), b=7.138 (2), c=13.518 A, β=104.48 (3) deg, V=905.0 (5) A 3 , Z=4, D m =2.56 (2), D x =2.598 Mg m -3 , λ(MoKα)=0.71073 A, μ(MoKα)=5.103 mm -1 , F(000)=672, T=300 K, R=0.032 for 1018 independent observed reflections. The structure contains two phosphite anions connected by a hydrogen bond. The La 3+ cation is eight coordinated by seven O atoms from phosphite anions and one O atom of a water molecule. (orig.)

Betaine Phosphate (CH3)3N+CH2COO-.H3PO4 Modification Using D2O

International Nuclear Information System (INIS)

Saryati; Ridwan; Deswita; Sugiantoro, Sugik

2002-01-01

Betaine fosfate (CH 3 ) 3 N + CH 2 COO - .H 3 PO 4 modification by using D 2 O has been studied. This modification was carried out by slowly evaporation the saturated Betaine phosphat in the D 2 O solution in the dry box at 40 o C, until the dry crystal were formed. Based on the NMR data, can be concluded that the exchange process with D has been runed well and Betaine phosphate-D (CH 3 ) 3 N + CH 2 COO - .H 3 PO 4 has been resulted. From the X-ray diffraction pattern data can be concluded that there are a deference in the crystal structure between Betaine phosphate and Betaine phosphate modification result. From the Differential Scanning Colorimeter (DSC) diagram at the range temperature from 30 o C to 250 o C, can be shown that the Betaine phosphate-H has two endothermic transition phase, at 99 o C with a very little adsorbed calor and at 221.50 o C with -26.75 cal/g. Modified Betaine phosphate has also two endothermic transition phase, at 99.86 o C with -1.94 cal/g and at 171.01 o C with -3.48 cal/g. It can be conclosed that the D atom substitution on the H atoms in Betaine phosphate, to change the crystal and the endothermic fase temperature and energy

Synthesis and characterization of nanoporous anodic oxide film on aluminum in H3PO4 + KMnO4 electrolyte mixture at different anodization conditions

Science.gov (United States)

Verma, Naveen; Jindal, Jitender; Singh, Krishan Chander; Mari, Bernabe

2016-04-01

The micro structural properties of nanoporous anodic oxide film formed in H3PO4 were highly influenced by addition of a low concentration of KMnO4 (0.0005 M) in 1 M H3PO4 solution. The KMnO4 as additive enhanced the growth rate of oxide film formation as well as thickness of pore walls. Furthermore the growth rate was found increased with increase in applied current density. The increase in temperature and lack of stirring during anodization causes the thinness of pore wall which leads to increase in pore volume. With the decrease in concentration of H3PO4 in anodizing electrolyte from 1M to 0.3 M, keeping all other conditions constant, the decrease in porosity was observed. This might be due to the dissolution of aluminium oxide film in highly concentrated acidic solution.

Conductivity of Composite Material Based on System NdPO4·nH2OCsH2PO4

DEFF Research Database (Denmark)

Anfimova, Tatiana; Bjerrum, Niels J.; Li, Qingfeng

2013-01-01

The goal of the present study was to obtain a comprehensive knowledge about synthesis conditions, structure, thermal behavior and conductivity properties of neodymiumorthophosphates in order to analyze of use this material in intermediate temperature fuel cells due to their thermal and chemical...... stability properties.The impedance spectroscopy technique (IS) was used to measure the conductivity. The conductivity of composites observed to be lower than conductivity of pure CsH2PO4 but had improved sufficiently conductivity of pure NdPO4·nH2O...

Partial exchange of the Li+, Na+ and K+ alkaline cations in the HNi(PO4).H2O layered compound

International Nuclear Information System (INIS)

Escobal, Jaione; Mesa, Jose; Pizarro, Jose; Bazan, Begona; Arriortua, Maria; Rojo, Teofilo

2006-01-01

The exchange of the Li + (1), Na + (2) and K + (3) alkaline cations in the layered HNi(PO 4 ).H 2 O was carried out starting from a methanolic solution containing the Li(OH).H 2 O hydroxide for (1) and the M(OH) (M=Na and K) hydroxides together with the (C 6 H 13 NH 2 ) 0.75 HNiPO 4 .H 2 O phases for (2) and (3). The compounds are stable until, approximately, 280 o C for (1) and 400 deg. C for phases (2) and (3), respectively. The IR spectra show the bands belonging to the water molecule and the (PO 4 ) 3- oxoanion. The diffuse reflectance spectra indicate the existence of Ni(II), d 8 , cations in slightly distorted octahedral geometry. The calculated Dq and Racah (B and C) parameters have a mean value of Dq=765, B=905 and C=3895cm -1 , respectively, in accordance with the values obtained habitually for this octahedral Ni(II) cation. The study of the exchange process performed by X-ray powder diffraction indicates that the exchange of the Li + cation in the lamellar HNi(PO 4 ).H 2 O phase is the minor rapid reaction, whereas the exchange of the Na + and K + cations needs the presence of the intermediate (C 6 H 13 NH 2 ) 0.75 HNiPO 4 .H 2 O intercalate in order to obtain the required product with the sodium and potassium ions. The Scanning electronic microscopy (SEM) images show a mean size of particle of 5μm. The Li + exchanged compound exhibits small ionic conductivity (Ωcm -1 is in the 10 -8 -10 -9 range) probably restrained by the methanol solvent. Magnetic measurements carried out from 5K to room temperature indicate antiferromagnetic coupling as the major interaction in the three phases. Notwithstanding the Li and K phases show a weak ferromagnetism at low temperatures

Electric Response and Conductivity Mechanism in H3PO4‑Doped Polybenzimidazole-4N−HfO2 Nanocomposite Membranes for High Temperature Fuel Cells

International Nuclear Information System (INIS)

Nawn, Graeme; Vezzù, Keti; Bertasi, Federico; Pagot, Gioele; Pace, Giuseppe; Conti, Fosca; Negro, Enrico

2017-01-01

Relaxation and polarization phenomena of phosphoric acid-doped [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y nanocomposite membranes for high-temperature proton-exchange membrane fuel cells are studied using Dynamic Mechanical Analysis (DMA) and Broadband Electrical Spectroscopy (BES). The membranes are obtained by casting combinations of a polybenzimidazole polymer (PBI4N) with increasing amounts of hafnium oxide nanofiller, resulting in [PBI4N(HfO 2 ) x ] hybrid systems with 0 ≤ x ≤ 0.32. Phosphoric acid at varying content levels (0 ÷ 18 wt%) is used as a doping agent, giving rise to [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y membranes. DMA and BES studies lead us to determine that the electric response of the membranes is modulated by polarization phenomena and by α and β dielectric relaxation events of the polymer matrix. Additionally, the experimental results suggest that in [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y membranes the conductivity occurs owing to three conductivity pathways: two mechanisms involving inter-domain proton migration phenomena by “hopping” events; and one mechanism in which proton exchange occurs between delocalization bodies. These results highlight the significant effect of the hafnium oxide nanofiller content on the conductivity of [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y where, at x ≥ 0.04, demonstrates conductivity higher (9.0 × 10 −2 S/cm) than that of pristine H 3 PO 4 -doped PBI4N (4.8 × 10 −2 S/cm) at T ≥ 155 °C.

New crystals of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O system

Energy Technology Data Exchange (ETDEWEB)

Makarova, I. P., E-mail: makarova@crys.ras.ru; Grebenev, V. V.; Komornikov, V. A.; Selezneva, E. V. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation)

2016-11-15

Cs{sub 6}H(HSO{sub 4}){sub 3}(H{sub 2}PO{sub 4}){sub 4} crystals, grown for the first time based on an analysis of the phase diagram of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O ternary system, have been investigated by structural analysis using synchrotron radiation. The atomic structure of the crystals is determined and its specific features are analyzed.

Facile synthesis technology of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C adding H{sub 2}O{sub 2} in ball mill process

Energy Technology Data Exchange (ETDEWEB)

Min, Xiujuan [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Mu, Deying [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Department of Environmental Engineering, Harbin University of Commerce, Harbin 150076 (China); Li, Ruhong [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Dai, Changsong, E-mail: changsd@hit.edu.cn [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China)

2016-11-15

Highlights: • Sintering time of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} reduced to 6 hours by adding hydrogen peroxide. • Electrochemical performance of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} was improved by reducing sintering time. • The Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} production process was simplified during material synthesis stage. - Abstract: Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C has stable structure, high theory specific capacity and good safety performance, therefore it has become the research focus of lithium-ion batteries in recent years. The facile synthesis technology of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C was characterized by adding different amounts of H{sub 2}O{sub 2}. Structure and morphology characteristics were examined by XRD, TG, Raman Spectroscopy, XPS and SEM. Electrochemical performance was investigated by constant current charging and discharging test. The results revealed that the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C electrochemical performance of adding 15 mL H{sub 2}O{sub 2} was better after sintering during 6 h. At the charge cut-off voltage of 4.3 V, the first discharge capacity at 0.2 C rate reached 127 mAh g{sup −1}. Because of adding H{sub 2}O{sub 2} in the ball-mill dispersant, the vanadium pentoxide formed the wet sol. The molecular-leveled mixture increased the homogeneity of raw materials. Therefore, the addition of H{sub 2}O{sub 2} shortened the sintering time and significantly improved the electrochemical performance of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C.

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)

Synthesis, structures and properties of the new lithium cobalt(II) phosphate Li4Co(PO4)2

International Nuclear Information System (INIS)

Glaum, R.; Gerber, K.; Schulz-Dobrick, M.; Herklotz, M.; Scheiba, F.; Ehrenberg, H.

2012-01-01

α-Li 4 Co(PO 4 ) 2 has been synthesized and crystallized by solid-state reactions. The new phosphate crystallizes in the monoclinic system (P2 1 /a, Z=4, a=8.117(3) Å, b=10.303(8) Å, c=8.118(8) Å, β=104.36(8) Å) and is isotypic to α-Li 4 Zn(PO 4 ) 2 . The structure of α-Li 4 Co(PO 4 ) 2 has been determined from single-crystal X-ray diffraction data {R 1 =0.040, wR 2 =0.135, 2278 unique reflections with F o >4σ(F o )}. The crystal structure, which might be regarded as a superstructure of the wurtzite structure type, is build of layers of regular CoO 4 , PO 4 and Li1O 4 tetrahedra. Lithium atoms Li2, Li3 and Li4 are located between these layers. Thermal investigations by in-situ XRPD, DTA/TG and quenching experiments suggest decomposition followed by formation and phase transformation of Li 4 Co(PO 4 ) 2 : α-Li 4 Co(PO 4 ) 2 ⟹ 442°C β-Li 3 PO 4 +LiCoPO 4 ⇌ 773°C β-Li 4 Co(PO 4 ) 2 ⟹ quenchingto25°C α-Li 4 Co(PO 4 ) 2 According to HT-XRPD at θ=850°Cβ-Li 4 Co(PO 4 ) 2 (Pnma, Z=2, 10.3341(8) Å, b=6.5829(5) Å, c=5.0428(3) Å) is isostructural to γ-Li 3 PO 4 . The powder reflectance spectrum of α-Li 4 Co(PO 4 ) 2 shows the typical absorption bands for the tetrahedral chromophore [Co II O 4 ]. - Graphical abstract: The complex formation and decomposition behavior of Li 4 Co(PO 4 ) 2 with temperature has been elucidated. The crystal structure of its α-phase was determined from single crystal data, HT-XRPD allowed derivation of a structure model for the β-phase. Both modifications belong to the Li 3 PO 4 structure family. Highlights: ► Li 4 Co(PO 4 ) 2 exhibits complex thermal behavior. ► The new phosphate belongs to the Li 3 PO 4 structure family. ► A single-crystal structure analysis is provided for the metastable α-Li 4 Co(PO 4 ) 2 . ► From HT-XRPD data a cation distribution model is developed for β-Li 4 Co(PO 4 ) 2 . ► No electrochemical delithiation is observed up to 5 V.

Sol–gel synthesis and electrochemical properties of 9LiFePO4·Li3V2(PO4)3/C composite cathode material for lithium ion batteries

International Nuclear Information System (INIS)

Zhong Shengkui; Wu Ling; Liu Jiequn

2012-01-01

Highlights: ► Nano-sized 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C powders are prepared by a sol–gel method. ► Mutual doping in 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C can improve its electronic conductivity. ► The addition of Li 3 V 2 (PO 4 ) 3 can improve the ionic diffusivity of LiFePO 4 . ► LiFePO 4 , Li 3 V 2 (PO 4 ) 3 and LiFePO 4 –Li 3 V 2 (PO 4 ) 3 unit cells coexist in the composite. - Abstract: 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C composite cathode material is prepared by a sol–gel method, using ferric citrate, V 2 O 5 , Li 2 CO 3 , NH 4 H 2 PO 4 and citric acid as raw materials. The composite material is composed of the olivine LiFePO 4 and monoclinic Li 3 V 2 (PO 4 ) 3 phases. XRD results indicate that most of the iron and vanadium in the raw materials tend to form the LiFePO 4 and Li 3 V 2 (PO 4 ) 3 phases, and only small amounts of Fe and V as the dopants enter into the lattice of Li 3 V 2 (PO 4 ) 3 and LiFePO 4 , respectively. The electronic conductivity and Li + diffusion coefficient of 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C are 6.615 × 10 −3 S cm −1 and ∼10 −10 cm 2 s −1 , which are three orders of magnitude and one order of magnitude larger than those of the LiFePO 4 /C, respectively. The composite material shows a first discharge specific capacity of 131.3 mAh g −1 and capacity retention of 95.1% after 200 cycles at 10 C rate. Compared with the LiFePO 4 /C, its rate capability and cycle performance are both remarkably improved.

Hydrothermal synthesis and crystal structure of CsFe23(HPO4)2(PO4)(H2O)

International Nuclear Information System (INIS)

Anisimova, N.Yu.; Ilyukhin, A.B.; Chudinova, N.N.; Serafin, M.

2001-01-01

The double acid iron-cesium orthophosphate CsFe 2 3 (HPO 4 ) 2 (PO 4 )(H 2 O) was prepared by hydrothermal synthesis (from the Fe 2 O 3 , Cs 2 CO 3 and H 3 PO 4 mixture at 290 Deg C during 1 h following by cooling to 25 Deg C). Its crystal structure (a = 5.021(3), b = 15.80(1), c = 13.646(8), β 94.49(4) Deg, sp. gr. P2 1 /n, Z = 4) was analyzed by X-ray diffraction. The structure is formed by the orthophosphate tetrahedrons and the FeO 6 octahedrons, the water molecule is coordinated by the iron atom [ru

Neutron diffraction studies of the Na-ion battery electrode materials NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3}

Energy Technology Data Exchange (ETDEWEB)

Yahia, H. Ben [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar); Essehli, R., E-mail: ressehli@qf.org.qa [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar); Avdeev, M. [Australian Nuclear Science and Technology Organisation, New Illawarra Road, Lucas Heights NSW 2234 (Australia); Park, J-B.; Sun, Y-K. [Department of Energy Engineering Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Al-Maadeed, M.A. [Center for Advanced Materials (CAM), Qatar University, 2713 Doha (Qatar); Belharouak, I., E-mail: ibelharouak@qf.org.qa [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar)

2016-06-15

The new compounds NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} were synthesized by sol-gel method and their crystal structures were determined by using neutron powder diffraction data. These compounds were characterized by galvanometric cycling and cyclic voltammetry. NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} crystallize with a stuffed α-CrPO{sub 4}-type structure. The structure consists of a 3D-framework made of octahedra and tetrahedra that are sharing corners and/or edges generating channels along [100] and [010], in which the sodium atoms are located. Of significance, in the structures of NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} a statistical disorder Ni{sup 2+}/Cr{sup 3+} was observed on both the 8g and 4a atomic positions, whereas in NaCoCr{sub 2}(PO{sub 4}){sub 3} the statistical disorder Co{sup 2+}/Cr{sup 3+} was only observed on the 8g atomic position. When tested as negative electrode materials, NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} delivered specific capacities of 352, 385, and 368 mA h g{sup −1}, respectively, which attests to the electrochemical activity of sodium in these compounds. - Highlights: • NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} were synthesized by sol-gel method. • The crystal structures were determined by using neutron powder diffraction data. • The three compounds crystallize with a stuffed α-CrPO{sub 4}-type structure. • The three compounds were tested as anodes in sodium-ion batteries. • Relatively high specific capacities were obtained for these compounds.

Room temperature metathetic synthesis and characterization of α-hopeite, Zn3(PO4)2.4H2O

International Nuclear Information System (INIS)

Parhi, Purnendu; Manivannan, V.; Kohli, Sandeep; McCurdy, Patrick

2008-01-01

The synthesis of crystalline zinc phosphates (α-hopeite phase) through the metathetic pathway has been investigated. The reaction has been carried out by room-temperature grinding. High lattice energy of the by-product NaCl has driven the reaction in the forward direction, and as a result, stable phosphate phases have been synthesized. Reaction of a different phosphorus source (like Na 3 PO 4 , Na 2 HPO 4 , NaH 2 PO 4 , and K 2 HPO 4 ) with ZnCl 2 has been attempted. The structural, vibrational, thermal, optical, and chemical properties of synthesized powders are determined by powder X-ray diffraction (XRD), scanning electron microscope (SEM), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and diffused reflectance spectra (DR) in the UV-vis range. The direct band gap of the title compound was determined to be 3.6 ± 0.2 eV

CINETIQUE DES IONS PHOSPHORIQUES H2PO4- ET HPO4-2 EN MILIEU GYPSEUX

Directory of Open Access Journals (Sweden)

Hacène BOUZIANE

2011-06-01

Full Text Available L’étude de la fixation des ions H2PO4- et HPO4-2 par les divers types de gypse (tassé ; feuilleté ; fibreux. Donne une réaction positive quelle que soit la solution phosphaté et le type de gypse utilisé. Il convient de noter que l’adsorption est beaucoup plus forte pour les ions H2PO4- que celle des ions HPO4-2 et qu’elle varie d’un type de gypse à l’autre.                 L’étude de l’influence du temps, de la granulométrie et de la concentration des solutions montrent en effet que : plus le diamètre du grain est petit, plus l’adsorption est forte. La fixation se produit même pour une solution phosphatée à très faible concentration ; il se produit toujours une réaction avec précipitation et non un équilibre d’adsorption. La réaction des ions phosphatés augment rapidement dans les premières minutes quel que soit le type de gypse et la concentration utilisée. Nous avons abouti à la formation d’un gel phosphaté, visqueux et non soluble. L’analyse chimique de ce gel donne les résultats suivants : PO4=54,20% ,Ca=11,30% , K=32,94%; si l’on compare ces résultats avec les résultats calculés pour K3CaH,(PO42=PO4=54,59%, Ca=11,19%, K=33,62%, nos valeurs sont très voisines de celles-ci. Il s’agit donc du même sel sur lequel aucun travail sur la formation de K3CaH(PO42 à partir de CaSO42H2O ne semble avoir été publié.

Synthesis and crystal structure of acid indium phosphite In(H3PO3)3

International Nuclear Information System (INIS)

Zakharova, B.S.; Chudinova, N.N.; Ilyhkhin, A.B.

1996-01-01

A group of isostructural acid phosphites of trivalent metals M(H 2 PO 3 ) 3 , where M 3 =V, Fe, Ga, In, was synthesized. Crystal structure of In(H 2 PO 3 ) 3 was determined. The compound crystallizes in hexagonal syngony, a = 8.414(2), c = 7.069(2) A, V = 433.3(2) A 3 , Z = 2, sp.gr. P6 3 . In (H 2 PO 3 ) 3 structure is of frame type. 9 refs.; 3 tabs

Biological reduction-deposition and luminescent properties of nanostructured CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Yu, Xiaoniu [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Research Institute of Green Construction Materials, Southeast University, Nanjing 211189 (China); Qian, Chunxiang, E-mail: cxqian@seu.edu.cn [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Research Institute of Green Construction Materials, Southeast University, Nanjing 211189 (China)

2016-03-01

Nano-sized CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} with hexagonal phase have been prepared by simply varying the reactant P/Ce molar ratio in bacterial liquid. The phase composition of two samples was checked via Fourier transform infrared spectroscopy (FTIR), energy dispersive analysis of X-rays (EDS) and X-ray diffraction (XRD) analyses, displaying the presence of CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} with average crystallite size are 32.34 and 15.61 nm, respectively. The scanning electron microscopy (SEM) images show that nano-clusters and sphere-like in shape with a narrow diameter distribution were observed in two samples. The transmission electron microscopy (TEM) photographs further indicate obtained CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} nanoparticles correspond to nanosheets and nanorods, respectively. The emission spectra of CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} display a broad band of 300–380 nm range with the strongest emission at 342 nm in the violet region. - Highlights: • A new method was found to synthesize CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} nanoparticles. • CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) nanoparticles have good luminescent properties. • Size and luminescent properties of two samples have been studied and compared.

Hydrated aluminophosphate (AlPO/sub 4/. 1. 5H/sub 2/O) with PO/sub 4/, AlO/sub 4/ and AlO/sub 4/(H/sub 2/O)/sub 2/ groups and encapsulated water

Energy Technology Data Exchange (ETDEWEB)

Pluth, J.J.; Smith, J.V.

1986-09-15

Aluminium phosphate hydrate, AlPO/sub 4/ /sub ./ 1.5H/sub 2/O, M/sub r/=148.98, orthorhombic, Pbca, a=19.3525(13), b=9.7272(7), c=9.7621(8) A, V=1837.7(1) A/sup 3/, Z=16, D/sub x/=2.15 g cm/sup -3/, lambda(CuK..cap alpha..)=1.5418 A, ..mu..=68.2 cm/sup -1/, F(000)=1200, Tproportional to 295 K, R=0.033 for 1530 diffractions. A 4-connected framework contains PO/sub 4/ tetrahedra interposed between AlO/sub 4/ tetrahedra and AlO/sub 4/(H/sub 2/O)/sub 2/ octahedra at the nodes of cross-linked alternate 6/sup 3/ and 4.8/sup 2/ nets. A two-dimensional channel system, limited by 8-rings, lies between adjacent 6/sup 3/ nets. One H/sub 2/O of each octahedron lies in a 6-ring, and the other forms a continuous chain with a third H/sub 2/O which is held in place only by hydrogen bonds.

Synthesis of flower-like LiMnPO4/C with precipitated NH4MnPO4·H2O as precursor

International Nuclear Information System (INIS)

Liu Jiali; Hu Dongge; Huang Tao; Yu Aishui

2012-01-01

Highlights: ► Flower-like NH 4 MnPO 4 ·H 2 O is obtained by novel precipitating method. ► It is used as the precursor to synthesize LiMnPO 4 /C. ► Subsequent heat treatment would not destroy the precursor morphology. ► As-prepared LiMnPO 4 /C showed discharge capacity of 85 mAh/g at 0.05 C. - Abstract: Ammonium magnesium phosphate monohydrate (NH 4 MnPO 4 ·H 2 O) precursor was prepared by a novel precipitating process with manganese citrate complexes as intermediate. The morphology of the precursor observed by Scanning Electron Microscope (SEM) was flower-like which was self-assembled by plate-like particles. Further analysis by X-ray diffraction (XRD) revealed that the lattice of the plate crystal was orientated along (0 1 0) plane. By solid-state reaction of the precursor, with lithium acetate and glucose as carbon source, pure olivine structured LiMnPO 4 /C composite was obtained and meanwhile, the original flower-like morphology could be retained.

Zn(3)(4-OOCC(6)H(4)PO(3))(2): A polar metal phosphonate with pillared layered structure showing SHG-activity and large dielectric anisotropy.

Science.gov (United States)

Li, Jin-Tang; Cao, Deng-Ke; Akutagawa, Tomoyuki; Zheng, Li-Min

2010-10-07

A new metal phosphonate Zn(3)(4-OOCC(6)H(4)PO(3))(2) (1) is reported which crystallizes in orthorhombic space group Pca2(1). It shows a pillared layered structure in which the {ZnO(4)}, {ZnO(5)} and {PO(3)C} polyhedra are connected through corner- or edge-sharing to form an inorganic layer in the ab plane which contains 4- and 5-member rings. These layers are pillared by the uni-oriented 4-carboxylatephenylphosphonate ligands, thus leading to a polar 3D architecture. The dielectric anisotropy measurements of a single crystal of 1 reveal that dielectric constant along the inter-layer is larger than that along the intra-layer with a ratio of about 2.3. Second harmonic generation (SHG) activity is observed.

Preparation and characterization of activated carbon from reedy grass leaves by chemical activation with H{sub 3}PO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Xu, Jianzhong, E-mail: xjz8112@sina.com [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Chen, Lingzhi [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Department of Applied Chemistry, Hengshui University, Hengshui 053000, Hebei (China); Qu, Hongqiang; Jiao, Yunhong; Xie, Jixing [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Xing, Guangen [Department of Applied Chemistry, Hengshui University, Hengshui 053000, Hebei (China)

2014-11-30

Highlights: • Activated carbons were produced from reedy grass leaves by activation with phosphoric acid. • The activated carbons have a large number of oxygen- and phosphorus-containing surface groups. • The structure of activated carbons was bight fibers features on the surface and the external surface of the activated carbons was slightly corrugated and abundant pores. - Abstract: Activated carbons were produced from reedy grass leaves by chemical activation with H{sub 3}PO{sub 4} in N{sub 2} atmosphere and their characteristics were investigated. The effects of activation temperature and time were examined. Adsorption capacity was demonstrated with BET and iodine number. Micropore volume and pore size distribution of activated carbons were characterized by N{sub 2} adsorption isotherms. The surface area and iodine number of the activated carbons produced at 500 °C for 2 h were 1474 m{sup 2}/g and 1128 mg/g, respectively. Thermal decomposition of pure reedy grass leaves and H{sub 3}PO{sub 4}-impregnated reedy grass leaves have been investigated with thermogravimetric/mass spectroscopy (TG–MS) technique. It was found that the temperature and intensity of maximum evolution of H{sub 2}O and CO{sub 2} of H{sub 3}PO{sub 4}-impregnated reedy grass leaves were lower than that of pure reedy grass leaves. This implies that H{sub 3}PO{sub 4} as an activating reagent changed the thermal degradation of the reedy grass leaves, stabilized the cellulose structure, leading to a subsequent change in the evolution of porosity. The results of X-ray photoelectron spectroscopy and Fourier-infrared spectroscopy analysis indicate that the produced activated carbons have rich functional groups on surface.

Copper(II) manganese(II) orthophosphate, Cu_0.5Mn_2.5(PO₄)₂

DEFF Research Database (Denmark)

Warner, Terence Edwin; Bond, Andrew; Foghmoes, Søren Preben Vagn

2011-01-01

The title compound, Cu0.5Mn2.5(PO4)2, is a copper-manganese phosphate solid solution with the graftonite-type structure, (Mn,Fe,Ca,Mg)3(PO4)2. The structure has three distinct metal cation sites, two of which are occupied exclusively by MnII, and one of which accommodates CuII. Incorporation of C......II into the structure distorts the coordination geometry of the metal cation site from 5-coordinate square-pyramidal towards 4-coordinate flattened tetrahedral, and serves to contract the structure principally along the c axis....

Morphology and conductivity study of solid electrolyte Li{sub 3}PO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Prayogi, Lugas Dwi, E-mail: ldprayodi@gmail.com; Faisal, Muhamad [Engineering Physics, Sepuluh Nopember Institute of Technology ITS Campus, Sukolilo, Surabaya 6011 (Indonesia); Kartini, Evvy, E-mail: kartini@batan.go.id; Honggowiranto, Wagiyo; Supardi [Center for Science and Technology of Advanced Materials, National Nuclear Energy Agency Kawasan Puspiptek Serpong, Tangerang Selatan15314, Banten (Indonesia)

2016-02-08

The comparison between two different methods of synthesize of solid electrolyte Li{sub 3}PO{sub 4} as precursor material for developing lithium ion battery, has been performed. The first method is to synthesize Li{sub 3}PO{sub 4} prepared by wet chemical reaction from LiOH and H{sub 3}PO{sub 4} which provide facile, abundant available resource, low cost, and low toxicity. The second method is solid state reaction prepared by Li{sub 2}CO{sub 3} and NH{sub 4}H{sub 2}PO{sub 4.} In addition, the possible morphology identification of comparison between two different methods will also be discussed. The composition, morphology, and additional identification phase and another compound of Li{sub 3}PO{sub 4} powder products from two different reaction are characterized by SEM, EDS, and EIS. The Li{sub 3}PO{sub 4} powder produced from wet reaction and solid state reaction have an average diameter of 0.834 – 7.81 µm and 2.15 – 17.3 µm, respectively. The density of Li{sub 3}PO{sub 4} prepared by wet chemical reaction is 2.238 gr/cm{sup 3}, little bit lower than the sample prepared by solid state reaction which density is 2.3560 gr/cm{sup 3}. The EIS measurement result shows that the conductivity of Li{sub 3}PO{sub 4} is 1.7 x 10{sup −9} S.cm{sup −1} for wet chemical reaction and 1.8 x 10{sup −10} S.cm{sup −1} for solid state reaction. The conductivity of Li{sub 3}PO{sub 4} is not quite different between those two samples even though they were prepared by different method of synthesize.

Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst

International Nuclear Information System (INIS)

Adamiak, Joanna; Kalinowska-Alichnewicz, Dorota; Szadkowski, Michal; Skupinski, Wincenty

2011-01-01

Highlights: → A novel catalyst H 3 PO 4 /MoO 3 /SiO 2 was characterized and used in nitration. → On the surface domains of phosphomolybdic acid (HPM) are obtained. → Dinitrotoluene is obtained with very high yield i.e. 96 wt.% in mild conditions. → Dinitrochlorobenzene is obtained with only twelve-fold excess of nitric acid. → It is sulfuric acid free and solvent free nitration of aromatic compounds. - Abstract: A new catalyst, H 3 PO 4 /MoO 3 /SiO 2 , was prepared by modification of MoO 3 /SiO 2 using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds.

Preparation and physical properties of (PVA0.7(NaBr0.3(H3PO4xM solid acid membrane for phosphoric acid – Fuel cells

Directory of Open Access Journals (Sweden)

F. Ahmad

2013-03-01

Full Text Available A solid acid membranes based on poly (vinyl alcohol (PVA, sodium bromide (NaBr and phosphoric acid (H3PO4 were prepared by a solution casting method. The morphological, IR, electrical and optical properties of the (PVA0.7(NaBr0.3(H3PO4xM solid acid membranes where x = 0.00, 0.85, 1.7, 3.4, 5.1 M were investigated. The variation of film morphology was examined by scanning electron microscopy (SEM studies. FTIR spectroscopy has been used to characterize the structure of polymer and confirms the complexation of phosphoric acid with host polymeric matrix. The temperature dependent nature of ionic conductivity and the impedance of the polymer electrolytes were determined along with the associated activation energy. The ionic conductivity at room temperature was found to be strongly depends on the H3PO4 concentration which it has been achieved to be of the order 4.3 × 10−3 S/cm at ambient temperature. Optical measurements showed a decrease in optical band gap and an increase in band tail width with the increase of phosphoric acid. The data shows that the (PVA0.7(NaBr0.3(H3PO4xM solid acid membrane is promising for intermediate temperature phosphoric acid fuel cell applications.

In pursuit of the rhabdophane crystal structure: from the hydrated monoclinic LnPO{sub 4}.0.667H{sub 2}O to the hexagonal LnPO{sub 4} (Ln = Nd, Sm, Gd, Eu and Dy)

Energy Technology Data Exchange (ETDEWEB)

Mesbah, Adel, E-mail: adel.mesbah@cea.fr [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France); Clavier, Nicolas [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France); Elkaim, Erik [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, BP 48, 91192 Gif-sur-Yvette Cedex (France); Szenknect, Stéphanie; Dacheux, Nicolas [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France)

2017-05-15

The dehydration process of the hydrated rhabdophane LnPO{sub 4}.0.667H{sub 2}O (Ln = La to Dy) was thoroughly studied over the combination of in situ high resolution synchrotron powder diffraction and TGA experiments. In the case of SmPO{sub 4}.0.667H{sub 2}O (monoclinic, C2), a first dehydration step was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2) with Z =12 and a =17.6264(1) Å, b =6.9704(1) Å, c =12.1141(1) Å, β=133.74(1) °, V =1075.33(1) Å{sup 3}. In agreement with the TGA and dilatometry experiments, all the water molecules were evacuated above 220 °C yielding to the anhydrous form, which crystallizes in the hexagonal P3{sub 1}21 space group with a =7.0389(1) Å, c =6.3702(1) Å and V =273.34(1) Å{sup 3}. This study was extended to selected LnPO{sub 4}.0.667H{sub 2}O samples (Ln= Nd, Gd, Eu, Dy) and the obtained results confirmed the existence of two dehydration steps before the stabilization of the anhydrous form, with the transitory formation of LnPO{sub 4}.0.5H{sub 2}O. - Graphical abstract: The dehydration process of the rhabdophane SmPO{sub 4}.0.667H{sub 2}O was studied over combination of in situ high resolution synchrotron powder diffraction and TGA techniques, a first dehydration was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2). Then above 220 °C, the anhydrous form of the rhabdophane SmPO{sub 4} was stabilized and crystallizes in the hexagonal P3{sub 1}21 space group. - Highlights: • In situ synchrotron powder diffraction was carried out during the dehydration of the rhabdopahe LnPO{sub 4}.0.667H{sub 2}O. • The heat of the rhabdophane LnPO{sub 4}.0.667H{sub 2}O leads to LnPO{sub 4}.0.5H{sub 2}O then to anhydrous rhabdophane LnPO{sub 4}. • LnPO{sub 4}.0.5H{sub 2}O (monoclinic, C2) and LnPO{sub 4} (Hexagonal, P3{sub 1}21) were solved over the use of direct methods.

H3PO4/Al2O3 catalysts: characterization and catalytic evaluation of oleic acid conversion to biofuels and biolubricant

Directory of Open Access Journals (Sweden)

Lucia Regina Raddi de Araujo

2006-06-01

Full Text Available Al2O3 and H3PO4/Al2O3 catalysts were investigated in the conversion of oleic acid to biofuels and biolubricant at 1 atm and at 623 K. The catalytic tests were performed in a fixed bed and continuous flow reactor, using an oleic acid-catalyst ratio of 4 and N2 as the carrier gas. The reaction products were analyzed by gas chromatography and acidity measurements. N2 adsorption-desorption, X ray diffraction, 31P nuclear magnetic resonance and FT-IR spectroscopy were also employed to evaluate the textural, structural and acidic properties of the catalysts. The results showed that phosphoric acid impregnation improved the alumina decarboxylation activities, generating hydrocarbons in the range of gasoline, diesel oil and lubricant oil. The best catalytic performance was achieved with the highest surface area alumina impregnated with H3PO4, which was the solid that allied high total acidity with a large quantity of mesopores.

Synthesis, crystal structure and optical properties of the catena-metaphosphates Ce(PO3)4 and U(PO3)4

International Nuclear Information System (INIS)

Hoeppe, Henning A.; Daub, Michi

2012-01-01

The catena-metaphosphates of tetravalent cerium and tetravalent uranium were obtained as phase pure crystalline powders by reaction of the respective dioxides with phosphoric acid at 500 C. Ce(PO 3 ) 4 and U(PO 3 ) 4 crystallise in space group C2/c (Z = 16, a Ce = 13.7696(3) Aa, b Ce = 29.7120(7) Aa, c Ce = 8.9269(2) Aa, β Ce = 90.00(1) Aa 3 and a U = 13.786(3) Aa, b U = 29.843(6) Aa, c U = 8.9720(18) Aa, β U = 90.01(3) Aa 3 ). The vibrational and optical spectra of pale yellow Ce(PO 3 ) 4 and emerald-greenish U(PO 3 ) 4 are also reported. (orig.)

Hydrothermal synthesis and photoluminescent properties of hierarchical GdPO4·H2O:Ln3+ (Ln3+ = Eu3+, Ce3+, Tb3+) flower-like clusters

Science.gov (United States)

Amurisana, Bao.; Zhiqiang, Song.; Haschaolu, O.; Yi, Chen; Tegus, O.

2018-02-01

3D hierarchical GdPO4·H2O:Ln3+ (Ln3+ = Eu3+, Ce3+, Tb3+) flower clusters were successfully prepared on glass slide substrate by a simple, economical hydrothermal process with the assistance of disodium ethylenediaminetetraacetic acid (Na2H2L, where L4- = (CH2COO)2N(CH2)2N(CH2COO)24-). In this process, Na2H2L was used as both a chelating agent and a structure-director. The hierarchical flower clusters have an average diameter of 7-12 μm and are composed of well-aligned microrods. The influence of the molar ratio of Na2H2L/Gd3+ and reaction time on the morphology was systematically studied. A possible crystal growth and formation mechanism of hierarchical flower clusters is proposed based on the evolution of morphology as a function of reaction time. The self-assembled GdPO4·H2O:Ln3+ superstructures exhibit strong orange-red (Eu3+, 5D0 → 7F1), green (Tb3+, 5D4 → 7F5) and near ultraviolet emissions (Ce3+, 5d → 7F5/2) under ultraviolet excitation, respectively. This study may provide a new channel for building hierarchically superstructued oxide micro/nanomaterials with optical and new properties.

Dissolution mechanism of crystalline cellulose in H3PO4 as assessed by high-field NMR spectroscopy and fast field cycling NMR relaxometry.

Science.gov (United States)

Conte, Pellegrino; Maccotta, Antonella; De Pasquale, Claudio; Bubici, Salvatore; Alonzo, Giuseppe

2009-10-14

Many processes have been proposed to produce glucose as a substrate for bacterial fermentation to obtain bioethanol. Among others, cellulose degradation appears as the most convenient way to achieve reliable amounts of glucose units. In fact, cellulose is the most widespread biopolymer, and it is considered also as a renewable resource. Due to extended intra- and interchain hydrogen bonds that provide a very efficient packing structure, however, cellulose is also a very stable polymer, the degradation of which is not easily achievable. In the past decade, researchers enhanced cellulose reactivity by increasing its solubility in many solvents, among which concentrated phosphoric acid (H(3)PO(4)) played the major role because of its low volatility and nontoxicity. In the present study, the solubilization mechanism of crystalline cellulose in H(3)PO(4) has been elucidated by using high- and low-field NMR spectroscopy. In particular, high-field NMR spectra showed formation of direct bonding between phosphoric acid and dissolved cellulose. On the other hand, molecular dynamics studies by low-field NMR with a fast field cycling (FFC) setup revealed two different H(3)PO(4) relaxing components. The first component, described by the fastest longitudinal relaxation rate (R(1)), was assigned to the H(3)PO(4) molecules bound to the biopolymer. Conversely, the second component, characterized by the slowest R(1), was attributed to the bulk solvent. The understanding of cellulose dissolution in H(3)PO(4) represents a very important issue because comprehension of chemical mechanisms is fundamental for process ameliorations to produce bioenergy from biomasses.

Synthesis of g-C3N4/Ag3PO4 heterojunction with enhanced photocatalytic performance

International Nuclear Information System (INIS)

He, Peizhi; Song, Limin; Zhang, Shujuan; Wu, Xiaoqing; Wei, Qingwu

2014-01-01

Graphical abstract: g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst with visible-light response was prepared by a facile coprecipitation method. The results show that g-C 3 N 4 /Ag 3 PO 4 possesses a much higher activity for the decomposition of RhB than that of the pure Ag 3 PO 4 particles. The most mechanism is that g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst can efficiently separate the photogenerated electron–hole pairs, enhancing the photocatalytic activity of g-C 3 N 4 /Ag 3 PO 4 composites. - Highlights: • g-C 3 N 4 /Ag 3 PO 4 heterojunction showed much higher activity than that of Ag 3 PO 4 . • The high activity could be attributed to g-C 3 N 4 for modifying Ag 3 PO 4 . • More ·OH radicals may be significant reason to improve Ag 3 PO 4 activity. - Abstract: g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst with visible-light response was prepared by a facile coprecipitation method. The photocatalysts were characterized by X-ray powder diffraction, transmission electron microscopy, UV–vis absorption spectroscopy and Fourier transform infrared spectroscopy. The photocatalytic activities of the obtained samples were tested by using Rhodamine B (RhB) as the degradation target under visible light irradiation. g-C 3 N 4 /Ag 3 PO 4 decomposed RhB more effectively than the pure Ag 3 PO 4 particles did, and 2 wt.% g-C 3 N 4 had the highest activity. Furthermore, 2 wt.% g-C 3 N 4 /Ag 3 PO 4 degraded high-concentration RhB more potently than unmodified Ag 3 PO 4 did, probably because g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst enhanced the photocatalytic activity by efficiently separating the photogenerated electron–hole pairs

Enhanced photo-stability and photocatalytic activity of Ag3PO4 via modification with BiPO4 and polypyrrole

Science.gov (United States)

Cai, Li; Jiang, Hui; Wang, Luxi

2017-10-01

Ag3PO4 photocatalysts modified with BiPO4 and polypyrrole (PPy) were successfully synthesized via a combination of co-precipitation hydrothermal technique and oxidative polymerization method. Their morphologies, structures and optical and electronic properties were characterized by means of scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscope (TEM), Brunauer-Emmett-Teller (BET) surface areas, X-ray diffraction (XRD), fourier transform infrared spectra (FT-IR), X-ray photo-electron spectroscopy (XPS), UV-vis diffuse reflection spectra (UV-vis DRS), photocurrent technique and electrochemical impedance spectra (EIS). The typical triphenylmethane dye (malachite green) was chosen as a target organic contaminants to estimate the photocatalytic activities and photo-stabilities of Ag3PO4-BiPO4-PPy heterostructures under visible light irradiation. The results indicated that the existence of BiPO4 and PPy not only showed great influences on the photocatalytic activity, but also significantly enhanced photo-stability of Ag3PO4 in repeated and long-term applications. The degradation conversion of Ag3PO4-BiPO4-PPy heterostructures (ABP-3) was 1.58 times of that of pure Ag3PO4. The photo-corrosion phenomenon of Ag3PO4 was effectively avoided. The photocatalytic activity of up to 87% in the Ag3PO4-BiPO4-PPy heterostructures (ABP-3) can be remained after five repeated cycles, while only about 33% of the degradation efficiency can be reserved in pure Ag3PO4. The possible mechanism of enhanced photo-stability and photocatalytic activity of Ag3PO4-BiPO4-PPy heterostructures was also discussed in this work.

AgI/Ag3PO4 hybrids with highly efficient visible-light driven photocatalytic activity

International Nuclear Information System (INIS)

Katsumata, Hideyuki; Hayashi, Takahiro; Taniguchi, Masanao; Suzuki, Tohru; Kaneco, Satoshi

2015-01-01

Highlights: • AgI/Ag 3 PO 4 hybrid was prepared via an in situ anion-exchange method. • AgI/Ag 3 PO 4 displays the excellent photocatalytic activity under visible light. • AgI/Ag 3 PO 4 readily transforms to be Ag@AgI/Ag 3 PO 4 system. • h + and O 2 ·− play the major role in the AO 7 decolorization over AgI/Ag 3 PO 4 . • The activity enhancement is ascribed to a Z-scheme system composed of Ag 3 PO 4 , Ag and AgI. - Abstract: Highly efficient visible-light-driven AgI/Ag 3 PO 4 hybrid photocatalysts with different mole ratios of AgI were prepared via an in situ anion-exchange method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis diffuse reflectance spectroscopy (DRS) and photoluminescence (PL) technique. Under visible light irradiation (>420 nm), the AgI/Ag 3 PO 4 photocatalysts displayed the higher photocatalytic activity than pure Ag 3 PO 4 and AgI for the decolorization of acid orange 7 (AO 7). Among the hybrid photocatalysts, AgI/Ag 3 PO 4 with 80% of AgI exhibited the highest photocatalytic activity for the decolorization of AO 7. X-ray photoelectron spectroscopy (XPS) results revealed that AgI/Ag 3 PO 4 readily transformed to be Ag@AgI/Ag 3 PO 4 system while the photocatalytic activity of AgI/Ag 3 PO 4 remained after 5 recycling runs. In addition, the quenching effects of different scavengers displayed that the reactive h + and O 2 ·− play the major role in the AO 7 decolorization. The photocatalytic activity enhancement of AgI/Ag 3 PO 4 hybrids can be ascribed to the efficient separation of electron–hole pairs through a Z-scheme system composed of Ag 3 PO 4 , Ag and AgI, in which Ag nanoparticles act as the charge separation center

Synthesis and spectral studies of manganese(II), cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and mercury(II) complexes of 4-oxo-4H-1-benzopyran-3-carboxaldehyde hydrazone derivatives

International Nuclear Information System (INIS)

Nawar, N.; Khattab, M.A.; Bekheit, M.M.; El-Kaddah, A.H.

1996-01-01

A few complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-chlorobenzylhydrazone) (BCBH) and 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-methylbenzylhydrazone) (BMBH) have been synthesised and characterized by elemental analysis, molar conductivities, magnetic measurements and infrared (IR) and visible spectral studies. The IR spectra show that BCBH and BMBH behave as bidentate ligands either in the keto or enol form. (author). 24 refs., 2 tabs

Enhanced electrochemical performance of different morphological C/LiMnPO4 nanoparticles from hollow-sphere Li3PO4 precursor via a delicate polyol-assisted hydrothermal method

Science.gov (United States)

Cui, Yu-Ting; Xu, Ning; Kou, Li-Qin; Wu, Meng-Tao; Chen, Li

2014-03-01

With the hollow-sphere Li3PO4 as precursor, a delicate polyol-assisted hydrothermal method is devised to synthesize high-performance LiMnPO4. Orthorhombic shaped, irregular flaky shaped and sphere-like LiMnPO4 are sequentially prepared by decreasing the water-diethylene glycol (DEG) ratio. The capacity, cycling stability and rate performance of all samples prepared by the new synthesis method are improved significantly. And the C/LiMnPO4 with irregular flaky shape exhibits a capacity of 154.1 mA h g-1 at C/20, 147.4 mA h g-1 at C/10 and 102.5 mA h g-1 at 2 C, which is the best performance ever reported for LiMnPO4 active material with similar carbon additives.

LiFePO4 Nanostructures Fabricated from Iron(III) Phosphate (FePO4 x 2H2O) by Hydrothermal Method.

Science.gov (United States)

Saji, Viswanathan S; Song, Hyun-Kon

2015-01-01

Electrode materials having nanometer scale dimensions are expected to have property enhancements due to enhanced surface area and mass/charge transport kinetics. This is particularly relevant to intrinsically low electronically conductive materials such as lithium iron phosphate (LiFePO4), which is of recent research interest as a high performance intercalation electrode material for Li-ion batteries. Many of the reported works on LiFePO4 synthesis are unattractive either due to the high cost of raw materials or due to the complex synthesis technique. In this direction, synthesis of LiFePO4 directly from inexpensive FePO4 shows promise.The present study reports LiFePO4 nanostructures prepared from iron (III) phosphate (FePO4 x 2H2O) by precipitation-hydrothermal method. The sintered powder was characterized by X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Inductive coupled plasma-optical emission spectroscopy (ICP-OES), and Electron microscopy (SEM and TEM). Two synthesis methods, viz. bulk synthesis and anodized aluminum oxide (AAO) template-assisted synthesis are reported. By bulk synthesis, micro-sized particles having peculiar surface nanostructuring were formed at precipitation pH of 6.0 to 7.5 whereas typical nanosized LiFePO4 resulted at pH ≥ 8.0. An in-situ precipitation strategy inside the pores of AAO utilizing the spin coating was utilized for the AAO-template-assisted synthesis. The template with pores filled with the precipitate was subsequently subjected to hydrothermal process and high temperature sintering to fabricate compact rod-like structures.

Symmetry and topology code of the cluster self-assembly of framework MT structures of alumophosphates AlPO4(H2O)2 (metavariscite and variscite) and Al2(PO4)2(H2O)3 (APC)

Science.gov (United States)

Ilyushin, G. D.; Blatov, V. A.

2017-03-01

The supramolecular chemistry of alumophosphates, which form framework 3D MT structures from polyhedral AlO4(H2O)2 clusters with octahedral O coordination (of M polyhedra) and PO4 and AlO4 with tetrahedral O coordination (of T polyhedra), is considered. A combinatorial-topological modeling of the formation of possible types of linear (six types) and ring (two types) tetrapolyhedral cluster precursors M2T2 from MT monomers is carried out. Different versions of chain formation from linked (MT)2 rings (six types) are considered. The model, which has a universal character, has been used to simulate the cluster selfassembly of the crystal structure of AlPO4(H2O)2 minerals (metavariscite, m-VAR, and variscite, VAR) and zeolite [Al2(PO4)2(H2O)2] · H2O (APC). A tetrapolyhedral linear precursor is established for m-VAR and a ring precursor (MT)2 is established for VAR and APC. The symmetry and topology code of the processes of crystal structure self-assembly from cluster precursors is completely reconstructed. The functional role of the O-H···O hydrogen bonds is considered for the first time. The cluster self-assembly model explains the specific features of the morphogenesis of single crystals: m-VAR prisms, flattened VAR octahedra, and needleshaped APC square-base prisms.

Neutron diffraction, specific heat and magnetic susceptibility of Ni3(PO4)2

International Nuclear Information System (INIS)

Escobal, J.; Pizarro, J.L.; Mesa, J.L.; Rojo, J.M.; Bazan, B.; Arriortua, M.I.; Rojo, T.

2005-01-01

The Ni 3 (PO 4 ) 2 phosphate was synthesized by the ceramic method in air atmosphere. The crystal structure consists of a three-dimensional skeleton constructed from Ni 3 O 14 edge-sharing octahedra, which are interconnected by (PO 4 ) 3- oxoanions with tetrahedral geometry. The magnetic behavior was studied on powdered sample by using susceptibility, specific heat and neutron diffraction data. The nickel(II) orthophosphate exhibits a three-dimensional magnetic ordering at approximately 17.1 K. However, its complex crystal structure hampers any parametrization of the J-exchange parameter. The specific heat measurements of Ni 3 (PO 4 ) 2 exhibit a three-dimensional magnetic ordering (λ-type) peak at 17.1 K. Measurements above T N suggest the presence of a small short-range order in this phase. The total magnetic entropy was found to be 28.1 KJ/mol at 50 K. The magnetic structure of the nickel(II) phosphate exhibits ferromagnetic interactions inside the Ni 3 O 14 trimers which are antiferromagnetically coupled between them, giving rise to a purely antiferromagnetic structure

Luminescence characteristics and glow curves analysis of Cu"+ doped Li_3PO_4 phosphor

International Nuclear Information System (INIS)

Aghalte, G.A.; Dhoble, S.J.; Pawar, N.R.

2016-01-01

Li_3PO_4:Cu exhibits useful TL properties in personnel dosimetry of ionizing radiations. Cu is known to be one of the most efficient activator. The PL intensity is found to increase consistently with the increasing quenching temperature. Cu"+ doped Li_3PO_4 phosphor was synthesized by the wet chemical co-precipitation method. The crystal structure and particle morphology of the phosphor was investigated by using X-ray diffraction and scanning electron microscopy. Li_3PO_4:Cu is excellent phosphor for TL dosimetry. For the synthesis of Li_3PO_4:Cu phosphor the stoichiometric amounts of LiOH·H_2O and CuSO_4·"5H_2O were dissolved separately and then the solutions were mixed together. It was precipitated by using concentrated H_3PO_4. The precipitate was filtered out immediately and kept 12 hours below IR lamp. Prepared dry Li_3PO_4:Cu powder was then put on 2.5 wt% NH_4Cl in graphite crucible in preheated furnace at 800°C and was kept for 1 hour. It was then rapidly quenched to room temperature. Thermoluminescence (TL) glow curves were recorded on Nucleonix TL Reader with a heating rate of 2°C per second in the temperature range of 50-250°C. The PMT voltage was 750 volts. Photoluminescence (PL) studies were carried out by Hitachi F-4000 spectrophotometer with a spectral slit width of 1.5 nm

H3PO4 treated surface modified CuS counter electrodes with high electrocatalytic activity for enhancing photovoltaic performance of quantum dot-sensitized solar cells

Science.gov (United States)

Panthakkal Abdul Muthalif, Mohammed; Sunesh, Chozhidakath Damodharan; Choe, Youngson

2018-05-01

Herein we report a simple synthetic strategy to prepare highly efficient and surface modified CuS counter electrodes (CEs) for quantum dot-sensitized solar cells (QDSSCs) in the presence of phosphoric acid (H3PO4) using the chemical bath deposition method. This is the first report of successful treatment of H3PO4 on the surface of CuS CEs for designing a high-performance QDSSCs with improved photovoltaic properties. After optimization, the 4 ml H3PO4 treated CuS CE-based QDSSC exhibits excellent photovoltaic performance with a conversion efficiency (η) of 4.20% (Voc = 0.592 V, Jsc = 13.35 mA cm-2, FF = 0.532) under one full-sun illumination (100 mW cm-2, AM 1.5 G).

A second polymorph with composition Co3(PO42·H2O

Directory of Open Access Journals (Sweden)

Yang Kim

2008-10-01

Full Text Available Single crystals of Co3(PO42·H2O, tricobalt(II bis[orthophosphate(V] monohydrate, were obtained under hydrothermal conditions. The compound is the second polymorph of this composition and is isotypic with its zinc analogue, Zn3(PO42·H2O. Three independent Co2+ cations are bridged by two independent orthophosphate anions. Two of the metal cations exhibit a distorted tetrahedral coordination while the third exhibits a considerably distorted [5 + 1] octahedral coordination environment with one very long Co—O distance of 2.416 (3 Å. The former cations are bonded to four different phosphate anions, and the latter cation is bonded to four anions (one of which is bidentate and one water molecule, leading to a framework structure. Additional hydrogen bonds of the type O—H...O stabilize this arrangement.

Equilibrium diagram of KPO3-Y(PO3)3 system, chemical preparation and characterization of KY(PO3)4

International Nuclear Information System (INIS)

Jouini, Anis; Ferid, Mokhtar; Trabelsi-Ayadi, Malika

2003-01-01

Microdifferential thermal analysis (μ-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO 3 -Y(PO 3 ) 3 system. The only compound observed within the system was KY(PO 3 ) 4 melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO 3 ) 3 at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO 3 was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO 3 ) 4 polyphosphate has the P2 1 space group with lattice parameters: a=7.183(4) A, b=8.351(6) A, c=7.983(3) A, β=91.75(3) deg. and Z=2 is isostructural with KNd(PO 3 ) 4 . The second allotropic form of KY(PO 3 ) 4 belongs to the P2 1 /n space group with lattice parameters: a=10.835(3) A, b=9.003(2) A, c=10.314(1) A, β=106.09(7) deg. and Z=4 and is isostructural with TlNd(PO 3 ) 4 . The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP 4 O 12 crystallizes in the C2/c space group with lattice parameters: a=7.825(3) A, b=12.537(4) A, c=10.584(2) A, β=110.22(7) deg. and Z=4 is isostructural with RbNdP 4 O 12 and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported

Luminescence and energy transfer of Sm3+ and Eu3+ in Ca2PO4Cl

International Nuclear Information System (INIS)

Wang, Zhijun; Li, Panlai; Yang, Zhiping; Guo, Qinglin

2014-01-01

Sm 3+ , Eu 3+ , and Sm 3+ –Eu 3+ doped Ca 2 PO 4 Cl phosphors are synthesized by a solid-state method. Ca 2 PO 4 Cl:Sm 3+ can produce red emission under the 400 nm radiation excitation, and the emission peak is located at 601 nm, which is assigned to the 4 G 5/2 → 6 H 7/2 transition of Sm 3+ . Ca 2 PO 4 Cl:Eu 3+ can create red emission under the 392 nm radiation excitation, and the strongest peak is located at 620 nm, which is attributed to the 5 D 0 → 7 F 2 transition of Eu 3+ . The energy transfer from Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl has been validated and the critical distance (R c ) of Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl is calculated to be 1.14 nm. With increasing Eu 3+ doping concentration, the energy transfer efficiency (Sm 3+ →Eu 3+ ) gradually increases to 53.7%. The luminescence property of Ca 2 PO 4 Cl:Sm 3+ , Eu 3+ can be tuned by properly tuning the relative ratio of Sm 3+ –Eu 3+ , and the emission intensity of Ca 2 PO 4 Cl:Eu 3+ can be greatly enhanced by codoped Sm 3+ . - Highlights: • Ca 2 PO 4 Cl:Sm 3+ , Eu 3+ can produce red emission under the 400 nm radiation excitation. • The energy transfer from Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl has been validated. • The critical distance of Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl is calculated to be 1.14 nm

Influence of reaction products of K-getter fuel additives on commercial vanadia-based SCR catalysts Part II. Simultaneous addition of KCl, Ca(OH)(2), H3PO4 and H2SO4 in a hot flue gas at a SCR pilot-scale setup

DEFF Research Database (Denmark)

Castellino, Francesco; Jensen, Anker Degn; Johnsson, Jan Erik

2009-01-01

A commercial V2O5-WO3-TiO2 corrugated-type SCR monolith has been exposed for 1000 h in a pilot-scale setup to a flue gas doped with KCl, Ca(OH)(2), H3PO4 and H2SO4 by spraying a water solution of the components into the hot flue gas. The mixture composition has been adjusted in order to have P...... surface and did not proceed at the fast rates known for KCl. This fact indicates that binding K in P-K-Ca compounds is an effective way to reduce the negative influence of alkali metals on the lifetime of the vanadia-based SCR catalysts. On the other hand, P-deposition was favoured by the formation...

Re-entrant spin glass and stepped magnetization in mixed-valence SrFe3(PO4)3

International Nuclear Information System (INIS)

Shang Mingyu; Chen Yan; Tian Ge; Yuan Hongming; Feng Shouhua

2013-01-01

The 2 D channel mixed-valent iron (II/III) monophosphate SrFe 3 (PO 4 ) 3 was synthesized via one step mild hydrothermal method at 210 °C and characterized by X-ray diffraction techniques and magnetization measurements. Coexistence of antiferromagnetic superexchange and ferromagnetic superexchange interactions was supposed to be in the lattice according to the Goodenough-Kanamori-Anderson rules. Temperature dependent DC magnetization measurement shows that SrFe 3 (PO 4 ) 3 is ferrimagnet with three magnetic transitions between 2 and 350 K. Through AC magnetization measurement, re-entrant spin glass was observed due to the competition between ferromagnetic and antiferromagnetic interactions. Furthermore, an interesting field induced stepped magnetization was observed in SrFe 3 (PO 4 ) 3 at 2 K with the saturation magnetization Ms=2.4 μ B /f.u. at 5 T.

Hydrothermal synthesis, structural and physico-chemical characterizations of two Nasicon phosphates: M0.50IITi2(PO4)3 (M = Mn, Co)

International Nuclear Information System (INIS)

Essehli, Rachid; Bali, Brahim El; Benmokhtar, S.; Fejfarova, Karla; Dusek, Michal

2009-01-01

The family of titanium Nasicon-phosphates of generic formula M 0.5 II Ti 2 (PO 4 ) 3 has been revisited using hydrothermal techniques. Two phases have been synthesized: Mn 0.5 II Ti 2 (PO 4 ) 3 (MnTiP) and Co 0.5 II Ti 2 (PO 4 ) 3 (CoTiP). Single crystal diffraction studies show that they exhibit two different structural types. Mn 0.5 II Ti 2 (PO 4 ) 3 phosphate crystallizes in the R-3 space group, with the cell parameters a = 8.51300(10) A and c = 21.0083(3) A (V = 1318.52(3) A 3 and Z = 6). The Co 0.5 II Ti 2 (PO 4 ) 3 phosphate crystallizes in the R-3c space group, with a = 8.4608(9) A and c = 21.174(2) A (V = 1312.7(2) A 3 and Z = 6). These two compounds are clearly related to the parent Nasicon-type rhombohedral structure, which can be described using [Ti 2 (PO 4 ) 3 ] framework composed of two [TiO 6 ] octahedral interlinked via three [PO 4 ] tetrahedra. 31 P magic-angle spinning nuclear magnetic resonance (MAS-NMR) data are presented as supporting data. Curie-Weiss-type behavior is observed in the magnetic susceptibility. The phases are also characterized by IR spectroscopy and UV-visible.

Spectro-photometric determination of niobium in Nb-Ti alloy using in-situ separation of Ti by masking with H3PO4

International Nuclear Information System (INIS)

Ghosh, Prasun; Dutta, M.; Jat, J.R.; Reddy, G.B.; Balaji Rao, Y.; Subba Rao, Y.

2016-01-01

The present paper details a simple procedure for the determination of Nb content in Nb-Ti alloy. The method involves dissolution of alloy in mixture of HNO 3 and HF followed by fuming with H 2 SO 4 . Subsequently, solution is taken for UV-Vis Spectro-photometric measurement after addition of Conc. H 3 PO 4 and H 2 O 2 . Hydrogen peroxide is added as coloring agent. Hydrogen peroxide (H 2 O 2 ) is known to form yellow color peroxo complex with both Niobium and Titanium in sulfuric acid medium and thus Ti will interfere with Nb in absorbance measurement. In view of this practical difficulty, in-situ separation of Ti during measurement has been resorted by masking Ti using Conc. H 3 PO 4 . Standard synthetic sample solution of Nb-Ti was prepared having Niobium and titanium in the ratio of 60:40, 50:50 and 40:60. Quantitative measurement of Niobium was carried out by UV-Visible spectrophotometer at 365 nm. The interference of titanium is prominent from the obtained Niobium concentration. Different ratios of H 3 PO 4 and H 2 SO 4 tried to arrive at optimum ratio to eliminate titanium interference and results are as shown. Quantitative measurement of Niobium was carried out at 355 nm as absorption maxima shifted from 365 nm to 355 nm in presence of phosphoric acid. Results show a good agreement with synthetic standard at 80:20 sulfuric to phosphoric acid ratio

Novel proton conducting polymer electrolytes based on polyparabanic acid doped with H 3PO 4 for high temperature fuel cell

Science.gov (United States)

Aihara, Yuichi; Sonai, Atsuo

Three novel proton conducting polymer electrolytes based on polyparabanic acid doped with H 3PO 4 were synthesized and their use in high temperature fuel cells characterized. The precursor polymers, PMD-Im, POD-Im and PDMDP-Im, were synthesized by cyclization polymerization of diisocynanates. After doping with H 3PO 4, the ionic conductivity and the thermal degradation were studied by using the AC impedance method and thermal gravimetric analysis, respectively. These membranes showed high ionic conductivity of the order of 10 -2 S cm -1 at 423 K with good thermal stability. Their application to fuel cells was demonstrated and polarization curves were obtained at 423 K were obtained without humidification.

Study of the solubility, viscosity and density in Na+, Zn2+/Cl− − H2O, Na+ − Zn2+ − (H2PO2)− − H2O, Na+, Cl−/(H2PO2)− − H2O, and Zn2+, Cl−/(H2PO2)− − H2O ternary systems, and in Na+, Zn2+/Cl−, (H2PO2)−//H2O reciprocal quaternary system at 273.15 K

International Nuclear Information System (INIS)

Adiguzel, Vedat; Erge, Hasan; Alisoglu, Vahit; Necefoglu, Hacali

2014-01-01

Highlights: • The physicochemical properties of ternary and one quaternary have been studied. • Reciprocal quaternary systems’ solubility and phase equilibrium have been studied. • In all systems the solid phases have been found. • It was found that Zn(H 2 PO 2 ) 2 salt contains 70% of the general crystallization field. - Abstract: The solubility and the physicochemical properties (density, viscosity) in the Na-Zn- Cl-H 2 O), (Na + Zn + H 2 PO 2 + H 2 O), (Na + Cl + H 2 PO 2 + H 2 O), and (Zn + Cl + H 2 PO 2 + H 2 O) ternaries, and in Na + , Zn 2+ /Cl − , (H 2 PO 2 ) − //H 2 O reciprocal quaternary systems at T = 273.15 K were investigated by using the isothermal method. The diagrams of ternary salts systems, (NaCl + ZnCl 2 + H 2 O), (NaCl + NaH 2 PO 2 + H 2 O), (NaH 2 PO 2 + Zn(H 2 PO 2 ) 2 + H 2 O), (ZnCl 2 + Zn(H 2 PO 2 ) 2 + H 2 O), are plotted in figures 1–4. However, whole ions of reciprocal quaternary salt systems are plotted in figure 5. Additionally, the density and viscosity values of ternary systems vs. their corresponding composition values in weight per cent are plotted in figures 6–10. At the (i) (ZnCl 2 + Zn(H 2 PO 2 ) 2 + H 2 O), (ii) (NaCl + ZnCl 2 + H 2 O), (iii) (NaCl + NaH 2 PO 2 + H 2 O), (iv) (NaH 2 PO 2 + Zn(H 2 PO 2 ) 2 + H 2 O) ternary systems the solid phase compositions have been determined as: (i) Zn(H 2 PO 2 ) 2 ⋅ H 2 O, Zn(H 2 PO 2 ) 2 , ZnCl 2 ⋅ 2H 2 O, (ii) NaCl, 2NaCl ⋅ ZnCl 2 ⋅ 2H 2 O, and ZnCl 2 ⋅ 2H 2 O, (iii) NaCl and NaH 2 PO 2 ⋅ H 2 O, (iv) Zn(H 2 PO 2 ) 2 ⋅ H 2 O and NaH 2 PO 2 ⋅ H 2 O, respectively. On the other hand reciprocal quaternary system was observed as: ZnCl 2 ⋅ 2H 2 O, 2NaCl ⋅ ZnCl 2 ⋅ 2H 2 O, Zn(H 2 PO 2 ) 2 ⋅ H 2 O, NaH 2 PO 2 ⋅ H 2 O, NaCl. According to results, the least soluble salt was Zn(H 2 PO 2 ) 2 . The crystallization field of this salt, being the largest in comparison with those of other salts, occupied 70% of the general crystallization field

Ion conductivity and phase transitions in the Na3Sc2(PO4)3 - NaGe2(PO4)3 system

International Nuclear Information System (INIS)

Nogaj, A.S.

2002-01-01

Influence of heteropolyvalent substitution on dipole ordering of sodium-scandium phosphate, as well as on ion conductivity and phase transitions in the system Na 3 Sc 2 (PO 4 ) 3 - NaGe 2 (PO 4 ) 3 , was studied using the methods of solid phase synthesis, X-ray diffraction, laser spectroscopy and measurement of electric conductivity. Boundaries of the dipole-ordered and superionic phases existence ranges in the given system were identified. It is shown that expansion of the dipole-ordered phase existence range with increase in substituent cation concentration is characteristic of the phase on the basis of α-Na 3 Sc 2 (PO 4 ) 3 [ru

Pengembangan Adsorben dari Limbah Lumpur Industri Crumb Rubber Yang Diaktivasi dengan H3PO4 Untuk Menyerap Ion Cr(VI

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Salmariza Salmariza

2014-12-01

Full Text Available Developing an adsorbent from activated sludge waste of crumb rubber industry which was activated by H3PO4 for Adsorption of Cr(VI had been done. The research was carried out by characterization of activated carbon in accordance with Indonesia National Standard (SNI 06-3730-1995, involved determination of iodine absorption, water content, and bounded carbon content. The research was conducted in batch system for activated carbon and adsorbent without activation, by observed pH sollution, contact time, and initial concentration of the treatment solution. Determination of maximum absorption capacity of activated carbon on Cr(VI used the Langmuir isotherm equation. From the characterization study of activated carbon was obtained that adsorption of iodine 482.6 mg/g, water content 0.14%, and bonded carbon content 24.925%. The results revealed that H3PO4 activator affected the adsorption of Cr(VI. Research with batch systems were obtained the optimum pH 2, contact time 120 minutes, and the optimum concentration 50 mg/L for adsorbent without activation and optimum pH 3, contact time 60 minutes, and the optimum concentration 50 mg/L for activated carbon. The maximum adsorption capacity was obtained 1.16 mg/g for adsorbent without activation and 1.99 mg/g for activated carbon.ABSTRAK Pengembangan adsorben dari limbah lumpur aktif Industri Crumb Rubber yang diaktivasi dengan H3PO4 untuk menyerap ion Cr(VI telah dilakukan. Pada penelitian dilakukan karakterisasi karbon aktif sesuai dengan Standar Nasional Indonesia (SNI 06-3730-1995, meliputi penentuan daya serap terhadap iodin, kadar air, dan kadar karbon terikat. Penelitian dilakukan dengan sistem batch terhadap karbon aktif dan adsorben tanpa aktivasi, dengan mengamati pH larutan, waktu kontak, dan konsentrasi awal larutan. Penentuan kapasitas serapan maksimum karbon aktif terhadap Cr(VI menggunakan persamaan Isoterm Langmuir. Hasil penelitian karakterisasi karbon aktif didapatkan daya serap terhadap

Topotactic insertion of lithium in the layered structure Li4VO(PO4)2: The tunnel structure Li5VO(PO4)2

International Nuclear Information System (INIS)

Satya Kishore, M.; Pralong, V.; Caignaert, V.; Malo, S.; Hebert, S.; Varadaraju, U.V.; Raveau, B.

2008-01-01

A new V(III) lithium phosphate Li 5 VO(PO 4 ) 2 has been synthesized by electrochemical insertion of lithium into Li 4 VO(PO 4 ) 2 . This phase, which crystallizes in the space group I4/mcm, exhibits a tunnel structure closely related to the layered structure of Li 4 VO(PO 4 ) 2 and to the tunnel structure of VO(H 2 PO 4 ) 2 . The topotactic reactions that take place during lithium exchange and intercalation, starting from VO(H 2 PO 4 ) 2 and going to the final phase Li 5 VO(PO 4 ) 2 are explained on the basis of the flexible coordinations of V 4+ and V 3+ species. The electrochemical and magnetic properties of this new phase are also presented and explained on the basis of the structure dimensionality. - Graphical abstract: Electrochemical synthesis of a new 3D V(III) lithium phosphate, Li 5 VO(PO 4 ) 2 . Starting from the 2D Li 4 VO(PO 4 ) 2 , the topotactic reaction that take place during lithium intercalation is explained on the basis of the flexible coordinations of V 4+ and V 3+ species

Crystal structure of CsTb(PO3)4 compound

International Nuclear Information System (INIS)

Palkina, K.K.; Maksimova, S.I.; Kuznetsov, V.G.; Chibiskova, N.T.

1978-01-01

The X-ray structural study of compounds of the CsLn(PO 3 ) 4 series has been made. Found is the presence of two structural types for CsPr(PO 3 ) 4 (cubic and monoclinic modifications), one type for CsNd(PO 3 ) 4 (cubic modification) and for CsTb(PO 3 ) 4 (monoclinic modification). For the CsTb(PO 3 ) 4 monocrystal the lattice parameters are determined: a=7.032 +- 0.001; b=8.705 +- 0.001; c=9.051 +- 0.001 A; α=90 deg, β=90 deg, γ=100 deg, Z=2, V=545.68 A 3 , dsub(exp)=3.70 g/cm 3 . The structure character is presented as infinite chains of (PO 4 ) tetrahedrons, stretched along the ''C'' period. Tb and Cs atoms are rounded by 8 atoms of oxygen. Tb polyhedron are irregular octaapexes or strongly deformed tetragonal antiprisms. Tb-Tb shortest distance is 6.59 A

Syntheses, crystal structures, NMR spectroscopy, and vibrational spectroscopy of Sr(PO{sub 3}F).H{sub 2}O and Sr(PO{sub 3}F)

Energy Technology Data Exchange (ETDEWEB)

Jantz, Stephan G.; Hoeppe, Henning A. [Lehrstuhl fuer Festkoerperchemie, Institut fuer Physik, Universitaet Augsburg (Germany); Wuellen, Leo van; Fischer, Andreas [Lehrstuhl fuer Chemische Physik und Materialwissenschaften, Institut fuer Physik, Universitaet Augsburg (Germany); Libowitzky, Eugen [Institute for Mineralogy and Crystallography, Faculty of Geosciences, Geography and Astronomy, University of Vienna (Austria); Baran, Enrique J. [Centro de Quimica Inorganica (CEQUINOR/CONICET, UNLP), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina); Weil, Matthias [Institute for Chemical Technologies and Analytics, Division Structural Chemistry, Vienna University of Technology (Austria)

2016-03-15

Single crystals of Sr(PO{sub 3}F).H{sub 2}O {P2_1/c, Z = 4, a = 7.4844(2) Aa, b = 7.0793(2) Aa, c = 8.4265(2) Aa, β = 108.696(1) , V = 422.91(2) Aa"3, 2391 F_o"2, 70 parameters, R_1[F"2 > 2σ(F"2)] = 0.036; wR_2(F"2 all) = 0.049, S = 1.054} were grown from an aqueous solution by a metathesis reaction. The structure comprises [SrO{sub 8}] polyhedra and PO{sub 3}F tetrahedra that form a layered arrangement parallel to (100). The topotactic dehydration of this phase proceeds between 80 and 140 C to afford Sr(PO{sub 3}F). The monazite-type crystal structure of Sr(PO{sub 3}F) was elucidated from the X-ray powder data by simulated annealing [P2{sub 1}/c, Z = 4, a = 6.71689(9) Aa, b = 7.11774(11) Aa, c = 8.66997(13) Aa, β = 128.0063(7) , V = 326.605(8) Aa{sup 3}, R{sub p} = 0.010, R{sub wp} = 0.015, R{sub F} = 0.030]. During dehydration, the structure of Sr(PO{sub 3}F) .H{sub 2}O collapses along [100] from a layered arrangement into a framework structure, accompanied by a change of the coordination number of the Sr{sup 2+} ions from eight to nine. The magic-angle spinning (MAS) NMR and vibrational spectroscopy data of both phases are discussed. (Copyright copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

High pressure experimental studies on Na3Fe(PO4)(CO3) and Na3Mn(PO4)(CO3): Extensive pressure behaviors of carbonophosphates family

Science.gov (United States)

Gao, Jing; Huang, Weifeng; Wu, Xiang; Qin, Shan

2018-04-01

Carbon-bearing phases in the Earth's interior have profound implications for the long-term Earth carbon cycle. Here we investigate high-pressure behaviors of carbonophosphates bonshtedtite Na3Fe(PO4)(CO3) and sidorenkite Na3Mn(PO4)(CO3) in diamond anvil cells up to ∼12 GPa at room temperature. Modifications in in situ synchrotron X-ray diffraction patterns and Raman spectra confirm the structural stability of carbonophosphates within the pressure region. Fitting the third-order Birch-Murnaghan equation of state to the volume compression curve, the isothermal bulk modulus parameters are obtained to be K0 = 56(1) GPa, K0' = 3.3(1), V0 = 303.3(3) Å3 for Na3Fe(PO4)(CO3) and K0 = 54(1) GPa, K0' = 3.4(1), V0 = 313.4(2) Å3 for Na3Mn(PO4)(CO3). Crystallographic axes exhibit an elastic anisotropy with a more compressible c-axis relative to the ab-plane. An inverse linear correlation between the K0 value and the ionic radius of M2+ (M = Mg, Fe, Mn) is well determined for carbonophosphates. The pressure-dependence responsiveness of [PO4] and [CO3] in carbonophosphates show a negative relationship to the M2+ radius. We also discussed the effect of [PO4] group on the structural variations and high-pressure behaviors of carbonates. Furthermore, the geochemical properties of carbonophosphates hold implications to diamond genesis.

Crystal structures of lazulite-type oxidephosphates TiIIITiIV3O3(PO4)3 and MIII4TiIV27O24(PO4)24 (MIII=Ti, Cr, Fe)

International Nuclear Information System (INIS)

Schoeneborn, M.; Glaum, R.; Reinauer, F.

2008-01-01

Single crystals of the oxidephosphates Ti III Ti IV 3 O 3 (PO 4 ) 3 (black), Cr III 4 Ti IV 27 O 24 (PO 4 ) 24 (red-brown, transparent), and Fe III 4 Ti IV 27 O 24 (PO 4 ) 24 (brown) with edge-lengths up to 0.3 mm were grown by chemical vapour transport. The crystal structures of these orthorhombic members (space group F2dd ) of the lazulite/lipscombite structure family were refined from single-crystal data [Ti III Ti IV 3 O 3 (PO 4 ) 3 : Z=24, a=7.3261(9) A, b=22.166(5) A, c=39.239(8) A, R 1 =0.029, wR 2 =0.084, 6055 independent reflections, 301 variables; Cr III 4 Ti IV 27 O 24 (PO 4 ) 24 : Z=1, a=7.419(3) A, b=21.640(5) A, c=13.057(4) A, R 1 =0.037, wR 2 =0.097, 1524 independent reflections, 111 variables; Fe III 4 Ti IV 27 O 24 (PO 4 ) 24 : Z=1, a=7.4001(9) A, b=21.7503(2) A, c=12.775(3) A, R 1 =0.049, wR 2 =0.140, 1240 independent reflections, 112 variables). For Ti III Ti IV O 3 (PO 4 ) 3 a well-ordered structure built from dimers [Ti III,IV 2 O 9 ] and [Ti IV,IV 2 O 9 ] and phosphate tetrahedra is found. The metal sites in the crystal structures of Cr 4 Ti 27 O 24 (PO 4 ) 24 and Fe 4 Ti 27 O 24 (PO 4 ) 24 , consisting of dimers [M III Ti IV O 9 ] and [Ti IV,IV 2 O 9 ], monomeric [Ti IV O 6 ] octahedra, and phosphate tetrahedra, are heavily disordered. Site disorder, leading to partial occupancy of all octahedral voids of the parent lipscombite/lazulite structure, as well as splitting of the metal positions is observed. According to Guinier photographs Ti III 4 Ti IV 27 O 24 (PO 4 ) 24 (a=7.418(2) A, b=21.933(6) A, c=12.948(7) A) is isotypic to the oxidephosphates M III 4 Ti IV 27 O 24 (PO 4 ) 24 (M III : Cr, Fe). The UV/vis spectrum of Cr 4 Ti 27 O 24 (PO 4 ) 24 reveals a rather small ligand-field splitting Δ o =14,370 cm -1 and a very low nephelauxetic ratio β=0.72 for the chromophores [Cr III O 6 ] within the dimers [Cr III Ti IV O 9 ]. - Graphical abstract: Single crystals of the oxidephosphates Ti III Ti IV 3 O 3 (PO 4 ) 3 (black), Cr III 4 Ti IV 27 O

Synthesis and luminescence properties of novel Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphor

Energy Technology Data Exchange (ETDEWEB)

Xu, Qiguang; Sun, Jiayue, E-mail: Jiayue_sun@126.com; Cui, Dianpeng; Di, Qiumei; Zeng, Junhui

2015-02-15

Sr{sub 3}(Gd{sub 1−x}Dy{sub x})(PO{sub 4}){sub 3} phosphors for white light-emitting diodes (w-LEDs) were prepared by the conventional solid-state reaction. X-ray diffraction (XRD) and photoluminescence spectra were utilized to characterize the structure and luminescence properties of the as-synthesized phosphors. Luminescence properties shows that the phosphor can be efficiently excited by the ultraviolet visible light in the region from 300 to 450 nm, and it exhibits blue (483 nm) and yellow (575 nm) emission corresponding to {sup 4}F{sub 9/2}→{sup 6}H{sub 15/2} transition and {sup 4}F{sub 9/2}→{sup 6}H{sub 13/2} transition, respectively. It has been found that concentration quenching occurs via dipole–dipole interaction according to Dexter's theory. The temperature dependence of photoluminescence properties is investigated from 25 to 250 °C and the prepared Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphors show good thermal quenching properties. - Highlights: • Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphors were synthesized by a solid-state reaction method. • The phosphor could be efficiently excited by the UV–vis light region from 300 to 450 nm. • Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphors exhibited blue (483 nm) and yellow (575 nm) emission. • The Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphors concentration quenching occurred as a result of dipole–dipole interaction. • Sr{sub 3}Gd(PO{sub 4}){sub 3}:Dy{sup 3+} phosphors showed good thermal quenching properties.

Uncommon potential hysteresis in the Li/Li2xVO(H2-xPO4)2 (0 ≤ x ≤ 2) system

International Nuclear Information System (INIS)

Dubarry, M.; Gaubicher, J.; Guyomard, D.; Wallez, G.; Quarton, M.; Baehtz, C.

2008-01-01

Physical and electrochemical investigations of vanadium phosphates, Li 2x VO(H 2-x PO 4 ) 2 (0 + /Li + ionic exchange from VO(H 2 PO 4 ) 2 to Li 2 VO(HPO 4 ) 2 leads to grain decrepitation. Further ionic exchange toward formation of Li 4 VO(PO 4 ) 2 lowers the symmetry. As inferred from potentiodynamic cycling correlated to ex situ and in situ X-ray diffraction (XRD), the system Li/Li 4 VO(PO 4 ) 2 shows several phase transformations that are associated with thermodynamical potential hysteresis that span from roughly 15 mV to more than 1.8 V. Small hysteresis are associated with topotactic reactions and with V V /V IV and V III /V II redox couples. Large potential hysteresis values (>1 V) were observed when oxidation of V III to V IV is involved

Resolution of the mixture TBP-H2 MPB-HDB-PH3PO4

International Nuclear Information System (INIS)

Pires, M.A.F.; Abrao, A.

1980-01-01

Tributylphosphate (TBP) is presently the most used extractant for uranium, thorium and zirconium technologies, both for the purification of these elements from their concentrates and for the recovery of heavy metals in the reprocessing of irradiated fuels. Nevertheless, in the presence of phosphoric acid, some degradation products are formed, such as: di-n-butylphosphoric acid (HDBP), monobutylphosphoric ancd (H 2 MBP) and ortophosphoric acid. The accumulation of these degradation products in the organic phase of the liquid-liquid extraction processes is highly undesirable. In order to avoid this problem, the separation of the mixture HDBP, H 2 MBP and H 3 PO 4 in TBP-dilutent or TBP-diluent-uranyl, thorium of zirconyl nitrate was then studied. Several separation techniques were investigated: adsorption using a cationic resin saturated with U(VI), chromatogtraphy in macroporous polymers, chromatography in alumina columns. Refractive index and condutimetric measurements were carried out to follow up the separation processes. The best results were obtained in an alumina column. (C.L.B.) [pt

Selective detection of Fe2+ by combination of CePO4:Tb3+ nanocrystal-H2O2 hybrid system with synchronous fluorescence scan technique.

Science.gov (United States)

Chen, Hongqi; Ren, Jicun

2012-04-21

A new method for quenching kinetic discrimination of Fe(2+) and Fe(3+), and sensitive detection of trace amount of Fe(2+) was developed by using synchronous fluorescence scan technique. The principle of this assay is based on the quenching kinetic discrimination of Fe(2+) and Fe(3+) in CePO(4):Tb(3+) nanocrytals-H(2)O(2) hybrid system and the Fenton reaction between Fe(2+) and H(2)O(2). Stable, water-soluble and well-dispersible CePO(4):Tb(3+) nanocrystals were synthesized in aqueous solutions, and characterized by transmission electron microscopy (TEM) and electron diffraction spectroscopy (EDS). We found that both Fe(2+) and Fe(3+) could quench the synchronous fluorescence of CePO(4):Tb(3+) nanocrytals-H(2)O(2) system, but their quenching kinetics velocities were quite different. In the presence of Fe(3+), the synchronous fluorescent intensity was unchanged after only one minute, but in the presence of Fe(2+), the synchronous fluorescent intensity decreased slowly until 28 min later. The Fenton reaction between Fe(2+) and H(2)O(2) resulted in hydroxyl radicals which effectively quenched the synchronous fluorescence of the CePO(4):Tb(3+) nanocrystals due to the oxidation of Ce(3+) into Ce(4+) by hydroxyl radicals. Under optimum conditions, the linear range for Fe(2+) is 3 nM-2 μM, and the limit of detection is 2.0 nM. The method was used to analyze water samples.

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, a new very complex Ba-Sc phosphate mineral from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia)

Science.gov (United States)

Yakovenchuk, Victor N.; Ivanyuk, Gregory Yu.; Pakhomovsky, Yakov A.; Panikorovskii, Taras L.; Britvin, Sergei N.; Krivovichev, Sergey V.; Shilovskikh, Vladimir V.; Bocharov, Vladimir N.

2018-02-01

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, is a new Ba-Sc phosphate from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia). It is orthorhombic, Pnma, a = 11.256(1), b = 8.512(1), c = 27.707(4) Å, V = 2654.6(3) Å3 and Z = 4 (from powder diffraction data) or a = 11.2261(9), b = 8.5039(6), c = 27.699(2) Å, V = 2644.3(3) Å3 (from single-crystal diffraction data). The mineral was found in a void within the calcite-magnetite phoscorite (enriched in hydroxylapatite and Sc-rich baddeleyite) inside the axial zone of the Kovdor phoscorite-carbonatite pipe. Kampelite forms radiated aggregates (up to 1.5 mm in diameter) of platy crystals grown on the surfaces of crystals of quintinite-2 H in close association with pyrite, bobierrite and quintinite-3 R. Kampelite is colourless, with a pearly lustre and a white streak. The cleavage is perfect on {001}, the fracture is smooth. Mohs hardness is about 1. In transmitted light, the mineral is colourless without pleochroism or dispersion. Kampelite is biaxial + (pseudouniaxial), α ≈ β = 1.607(2), γ = 1.612(2) (589 nm), and 2 V calc = 0°. The calculated and measured densities are 3.28 and 3.07(3) g·cm-3, respectively. The mean chemical composition determined by electron microprobe is: MgO 4.79, Al2O3 0.45, P2O5 31.66, K2O 0.34, Sc2O3 16.17, Mn2O3 1.62, Fe2O3 1.38, SrO 3.44, and BaO 29.81 wt%. The H2O content estimated from the crystal-structure refinement is 7.12 wt%, giving a total of 96.51 wt%. The empirical formula calculated on the basis of P = 6 apfu (atoms per formula unit) is (Ba2.62Sr0.45K0.10Ca0.06)Σ3.23Mg1.60Mn0.28(Sc3.15Fe3+ 0.23Al0.12)Σ3.50(PO4)6(OH)2.61·4.01H2O. The simplified formula is Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O. The mineral easily dissolves in 10% cold HCl. The strongest X-ray powder-diffraction lines [listed as d in Å ( I) ( hkl)] are as follows: 15.80(100)(001), 13.86(45)(002), 3.184(18)(223), 3.129(19)(026), 2.756(16)(402), 2.688(24)(10 10). The crystal structure of kampelite was

Separative recovery with lime of phosphate and fluoride from an acidic effluent containing H3PO4, HF and/or H2SiF6.

Science.gov (United States)

Gouider, Mbarka; Feki, Mongi; Sayadi, Sami

2009-10-30

Fluoride content and flow-rate of fertilizer plant wastewater from phosphoric acid and/or triple superphosphate (TSP) production lead to the discharge of several thousand tons of fluoride (F(-)) per year and even more for phosphate (PO4(3-)). Since sustainability is an important environmental concern, the removal methods should allow phosphorus and fluoride to be recycled as a sustainable products for use as raw materials either in agricultural or industrial applications. In the present work, separative recovery with lime of these two target species was investigated. A preliminary speciation study, carried out on the crude effluent, showed that two forms of fluoride: HF and H2SiF6 are present in a highly acidic medium (pH approximately 2). Evidence that fluoride is present under both free (HF) and combined (H2SiF6) forms, in the phosphate-containing effluent, was provided by comparing potentiometric titration curves of a crude wastewater sample and synthetic acid mixtures containing H3PO4, HF and H2SiF6. In a second step synthetic effluent containing mixtures of the following acids: HF, H2SiF6 and H3PO4, were treated with lime. The behaviour of these compounds under lime treatment was analysed. The data showed that fluoride has a beneficial effect on phosphate removal. Moreover, by acting on the precipitation pH, a "selective" recovery of fluoride and phosphate ions was possible either from phosphoric acid/hydrofluoric acid or phosphoric acid/hexafluorosilicic acid mixtures. Indeed, the first stage of the separative recovery, led to a fluoride removal efficiency of 97-98% from phosphoric acid/hydrofluoric acid mixture. It was of 93-95% from phosphoric acid/hexafluorosilicic acid mixture. During the second stage, the phosphate precipitation reached 99.8% from both acidic mixtures whereas it did not exceed 82% from a solution containing H3PO4 alone. The XRD and IR analyses showed that during lime treatment, a H2SiF6 hydrolysis occurred, instead of CaSiF6 solid

Americium and plutonium in phosphates of trigonal structure (NZP type) Am1/3[Zr2(PO4)3] and Pu1/4[Zr2(PO4)3

International Nuclear Information System (INIS)

Bykov, D.M.; Orlova, A.I.; Tomilin, S.V.; Lizin, A.A.; Lukinykh, A.N.

2006-01-01

Am 1/3 [Zr 2 (PO 4 ) 3 ] and Pu 1/4 [Zr 2 (PO 4 ) 3 ] phosphates are synthesized and are investigated by X-ray diffraction method. Compounds have triclinic lattices and lattice parameters are determined. Possibility of actinide inclusion into hollows of framework of NZP type is shown for the first time. It is proposed that inclusion of Pu and Am highly-charged cations into framework hollows decreases crystal structure symmetry up to primitive trigonal one. Rate of Pu leaching from ceramics on Pu 1/4 [Zr 2 (PO 4 ) 3 ] basis are measured [ru

Synthesis, crystal structure and spectroscopy properties of Na 3AZr(PO 4) 3 ( A=Mg, Ni) and Li 2.6Na 0.4NiZr(PO 4) 3 phosphates

Science.gov (United States)

Chakir, M.; El Jazouli, A.; de Waal, D.

2006-06-01

Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates were prepared at 750 °C by coprecipitation route. Their crystal structures have been refined at room temperature from X-ray powder diffraction data using Rietveld method. Li 2.6Na 0.4NiZr(PO 4) 3 was synthesized through ion exchange from the sodium analog. These materials belong to the Nasicon-type structure. Raman spectra of Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates present broad peaks in favor of the statistical distribution in the sites around PO 4 tetrahedra. Diffuse reflectance spectra indicate the presence of octahedrally coordinated Ni 2+ ions.

Neodymium-doped Sr5(PO4)3F and Sr5(VO4)3F

International Nuclear Information System (INIS)

Corker, D.L.; Nicholls, J.; Loutts, G.B.

1995-01-01

Neodymium-doped Sr 5 (PO 4 ) 3 F [neodymium strontium fluoride phosphate, (Nd,Sr) 5 (PO 4 ) 3 F] and neodymium-doped Sr 5 (VO 4 ) 3 F [neodymium strontium fluoride vanadate, (Nd,Sr) 5 (VO 4 ) 3 F] crystallize in space group P6 3 /m and are isostructural with calcium fluorophosphate, Ca 5 (PO 4 ) 3 F. There are two different Sr sites in Sr 5 (XO 4 ) 3 F, denoted Sr(1) and Sr(2). Using single-crystal X-ray diffraction the two structures were refined to R factors of 2.3 and 2.2%, respectively, showing that Nd is present at both Sr sites in (Sr,Nd) 5 (VO 4 ) 3 F but only at the Sr(2) site in (Sr,Nd) 5 (PO 4 ) 3 F. (orig.)

Synthesis and luminescence properties of novel LiSrPO{sub 4}:Dy{sup 3+} phosphor

Energy Technology Data Exchange (ETDEWEB)

Sun, Jiayue, E-mail: jiayue_sun@126.com [School of Science, Beijing Technology and Business University, Beijing 100048 (China); Zhang, Xiangyan [School of Science, Beijing Technology and Business University, Beijing 100048 (China); Xia, Zhiguo, E-mail: xiazg426@yahoo.com.cn [School of Materials Sciences and Technology, China University of Geosciences, Beijing 100083 (China); Du, Haiyan [School of Science, Beijing Technology and Business University, Beijing 100048 (China)

2011-11-15

Graphical abstract: Novel LiSrPO4:Dy{sup 3+} phosphors were synthesized by solid-state reaction, and Dy{sup 3+}-doped concentration dependent luminescence properties, concentration quenching effect and the decay times were investigated in detail. Highlights: {yields} LiSrPO{sub 4}:Dy{sup 3+} could be excited by UV light and exhibited blue and yellow emission. {yields} Concentration quenching effect of LiSrPO{sub 4}:Dy{sup 3+} samples were investigated in detail. {yields} Decay times are estimated to be 0.57-0.89 ms for Dy{sup 3+} in LiSrPO{sub 4} host. -- Abstract: Novel LiSrPO{sub 4}:Dy{sup 3+} phosphors for white light-emitting diodes (w-LEDs) were synthesized by the conventional solid-state reaction. X-ray powder diffraction (XRD) analysis confirmed the phase formation of LiSrPO{sub 4}:Dy{sup 3+} materials. Luminescence properties results showed that the phosphor could be efficiently excited by the UV-vis light region from 250 to 460 nm, and it exhibited blue (483 nm) and yellow (574 nm) emission corresponding to {sup 4}F{sub 9/2} {yields} {sup 6}H{sub 15/2} transitions and {sup 4}F{sub 9/2} {yields} {sup 6}H{sub 13}/{sub 2} transitions, respectively. The luminescence intensity of LiSrPO{sub 4}:xDy{sup 3+} phosphor firstly increased and then decreased with increasing Dy{sup 3+} concentration, and reached the maximum at x = 0.03. It was found that concentration quenching occurred as a result of dipole-dipole interaction according to the Dexter's theory. The decay time was also determined for various concentrations of Dy{sup 3+} in LiSrPO{sub 4}.

Improvement of the mechanical properties and corrosion resistance of biodegradable β-Ca3(PO4)2/Mg-Zn composites prepared by powder metallurgy: the adding β-Ca3(PO4)2, hot extrusion and aging treatment.

Science.gov (United States)

Yan, Yang; Kang, Yijun; Li, Ding; Yu, Kun; Xiao, Tao; Deng, Youwen; Dai, Han; Dai, Yilong; Xiong, Hanqing; Fang, Hongjie

2017-05-01

In this study, 10%β-Ca 3 (PO 4 ) 2 /Mg-6%Zn (wt.%) composites with Mg-6%Zn alloy as control were prepared by powder metallurgy. After hot extrusion, the as-extruded composites were aged for 72h at 150°C. The effects of the adding β-Ca 3 (PO 4 ) 2 , hot extrusion and aging treatment on their microstructure, mechanical properties and corrosion resistance were investigated. The XRD results identified α-Mg, MgZn phase and β-Ca 3 (PO 4 ) 2 phase in these composites. After hot extrusion, grains were significantly refined, and the larger-sized β-Ca 3 (PO 4 ) 2 particles and coarse MgZn phases were broken into linear-distributed β-Ca 3 (PO 4 ) 2 and MgZn phases along the extrusion direction. After aging treatment, the elements of Zn, Ca, P and O presented a more homogeneous distribution. The compressive strengths of the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites were approximately double those of natural bone, and their densities and elastic moduli matched those of natural bone. The immersion tests and electrochemical tests revealed that the adding β-Ca 3 (PO 4 ) 2 , hot extrusion and aging treatment could promote the formation of protective corrosion product layer on the sample surface in Ringer's solution, which improved corrosion resistance of the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites. The XRD results indicated that the corrosion product layer contained Mg(OH) 2 , β-Ca 3 (PO 4 ) 2 and hydroxyapatite (HA). The cytotoxicity assessments showed the as-extruded β-Ca 3 (PO 4 ) 2 /Mg-Zn composite aged for 72h was harmless to L-929 cells. These results suggested that the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites prepared by powder metallurgy were promising to be used for bone tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Photoluminescence properties of Eu(3+)/ Sm(3+) activated CaZr4(PO4)6 phosphors.

Science.gov (United States)

Nair, Govind B; Dhoble, S J

2016-09-01

Solid state reaction method was employed for the synthesis of a series of CaZr4(PO4)6: Eu(3+)/Sm(3+) phosphors. The red-emitting CaZr4(PO4)6:Eu(3+) phosphors can be efficiently excited at 396 nm and thereby, exhibit a strong red luminescence predominantly corresponding to the electric dipole transition at 615 nm. Under 405 nm excitation, CaZr4(PO4)6:Sm(3+) phosphors display orange emission with color temperatures approximately around 2200 K. The acquired results reveal that CaZr4(PO4)6: RE(3+) (RE = Eu, Sm) phosphors could be potential candidates for red and orange emitting phosphor, respectively, for UV/blue-pump LEDs.

Role of PO4 tetrahedron in LiFePO4 and FePO4 system.

Science.gov (United States)

Zeng, Yuewu

2015-06-01

Using high resolution transmission electron microscopy with image simulation and Fourier analysis, the Li1- x FePO4 (x < 0.01), Li1- x FePO4 (x ∼ 0.5), and FePO4 particles, prepared by charging or discharging the 053048 electrochemical cells (thickness: 5 mm, width: 30 mm, height: 48 mm) and dismantled inside an Ar-filled dry box, were investigated. The high resolution images reveal: (1) the solid solution of Li1- x FePO4 (x < 0.01) contains some missing Li ions leading PO4 group distorted around M1 tunnel of the unit cell; (2) the texture of the particles of Li1- x FePO4 (x ∼0.5) has homogeneously distributed compositional domains of LiFePO4 and FePO4 resulting from spinodal decomposition which promote Li ion easily getting into the particle due to uphill diffusion, (3) the particles of FePO4 formed in charging have heavily distorted lattice and contain some isolated LiFePO4 , (4) interface between LiFePO4 and FePO4 and between amorphous and crystal region provides the lattice distortion of small polarons. © 2015 Wiley Periodicals, Inc.

Photoluminescent properties of LiSrxBa1-xPO4:RE3+ (RE = Sm3+, Eu3+) f-f transition phosphors

International Nuclear Information System (INIS)

Tu Dong; Liang Yujun; Liu Rong; Cheng Zheng; Yang Fan; Yang Wenlong

2011-01-01

Highlights: → Novel phosphors LiSr x Ba 1-x PO 4 : Sm 3+ and LiSr x Ba 1-x PO 4 : Eu 3+ have been synthesized by solid-state reaction method. → The LiSr x Ba 1-x PO 4 : Sm 3+ and LiSr x Ba 1-x PO 4 : Eu 3+ phosphors may be potential f-f transition phosphors used in LED. → The emission intensity of the LiSr x Ba 1-x PO 4 : Sm 3+ and LiSr x Ba 1-x PO 4 : Eu 3+ phosphors can be enhanced by increasing the value of x. - Abstract: Rare-earth ions (Sm 3+ or Eu 3+ ) doped LiSr x Ba 1-x PO 4 (x = 0, 0.2, 0.4, 0.6, 0.8, 1.0) f-f transition phosphor powders were prepared by a high temperature solid-state reaction. The resulted phosphors were characterized by X-ray diffraction (XRD) and photoluminescence (PL) spectroscopy. The results of XRD indicate that the phase structure of the sample changes from LiBaPO 4 to LiSrPO 4 when x changes from 0 to 1.0. The excitation spectra indicate that only direct excitation of rare earth ions (Sm 3+ or Eu 3+ ) can be observed. The doped rare earth ions show their characteristic emission in LiSr x Ba 1-x PO 4 , i.e., Eu 3+5 D 0 - 7 F J (J = 0, 1, 2, 3, 4), Sm 3+4 G 5/2 → 6 H J (J = 5/2, 7/2, 9/2, 11/2), respectively. The dependence of the emission intensities of the LiSr x Ba 1-x PO 4 :Sm 3+ and LiSr x Ba 1-x PO 4 :Eu 3+ phosphors on the x value and Ln 3+ (Ln 3+ = Sm 3+ , Eu 3+ ) concentration is also investigated.

Synthesis and Characterization of New Nickel Phosphates, ANi4(PO4)3 (A=K, Rb)

International Nuclear Information System (INIS)

Im, Yoonmi; Kim, Pilsoo; Yun, Hoseop

2014-01-01

Quaternary nickel orthophosphates, ANi 4 (PO 4 ) 3 (A=Alkali metals) have been extensively investigated because they show interesting properties such as ionic conductivities, optical, and magnetic behaviors. They are built up from NiO 6 octahedra and PO 4 tetrahedra. These basic building blocks are connected via common oxygen atoms to form the three-dimensional frameworks and the alkali metal ions reside in the empty space. For NaNi 4 (PO 4 ) 3 , two different structures have been reported and this can be caused by the different reaction conditions. While NaNi 4 (PO 4 ) 3 prepared as single crystals with the use of NaCl flux at 1373 K crystallizes in the space group Amam and show a partial disorder of one of the PO 4 tetrahedra, NaNi 4 (PO 4 ) 3 and KNi 4 (PO 4 ) 3 synthesized with alkali metal nitrate at 1073 K as powders adopt an ordered structure with the space group Pnnm. As far as we know, no structural studies of KNi 4 (PO 4 ) 3 from single crystal diffraction data have been reported yet and RbNi 4 (PO 4 ) 3 is a new compound. In this paper we report on the synthesis and structural investigations using single crystals of two nickel orthophosphates, KNi 4 (PO 4 ) 3 and RbNi 4 (PO 4 ) 3

Poly[bis[μ-4-(4-carboxyphenoxybenzoato](μ-4,4′-oxydibenzoatobis[μ-3-(pyridin-4-yl-5-(pyridin-3-yl-1H-1,2,4-triazole]dicadmium(II

Directory of Open Access Journals (Sweden)

Xiao-Jin Qi

2016-07-01

Full Text Available Three kinds of bridging ligands, 4,4′-oxydibenzoate, 4-(4-carboxyphenoxybenzoate and 3-(pyridin-4-yl-5-(pyridin-3-yl-1H-1,2,4-triazole, link the CdII cations to form the title polymeric complex, [Cd2(C14H8O5(C14H9O52(C12H9N52]n, in which each CdII cation is in a distorted N2O5 pentagonal–bipyramidal coordination geometry. The 4,4′-oxydibenzoate dianion exhibits point group symmetry 2, with the central O atom located on a twofold rotation axis. Classical N—H...O, O—H...N hydrogen bonds and weak C—H...O hydrogen bonds link the complex molecules into a three-dimensional supramolecular architecture. A solvent-accessible void of 53 (2 Å3 is observed, but no solvent molecule could reasonably located there.

Synthesis and characterization of Ru(II) complexes with polyfunctional quinazoline-(3H)-4-ones

International Nuclear Information System (INIS)

Prabhakar, B.; Lingaiah, P.; Laxma Reddy, K.

1991-01-01

Few Ru(II) complexes of the type Ru(O-N-O) 2 with tridentate O-N-O donors and of the type RuCl 2 (O-N) 2 with bidentate O-O and O-N donors have been synthesized and characterized on the basis of analytical, conductivity, thermal, magnetic, IR, electronic and PMR spectral data. The IR and PMR spectral data of the metal complexes indicate that the lignads like 2-methyl/phenyl-3-(2'-hydroxybenzalamino) quinazoline-(3H)-4-one(MHBQ/PHBQ) act as uninegative tridentate, 2-methyl/phenyl-3-(carboxymethyl) quinazoline(3H)-4-one (MCMQ/PCMQ) as uninegative bidentate and 2-methyl/phenyl-3-(furfuralamino) quinazoline-(3H)-4-one (MFQ/PFQ), 2-methyl/phenyl-3-(acetamino) quinazoline-(3H)-4-one (MAQ/PAQ), 2-methyl/phenyl3-(uramino)quinazoline-(3H)-4-one (MUQ/PUQ) and 2-methyl/phenyl-3-thiouramino)quinazoline-(3H)-4-one-(MTUQ/PTUQ) as neutral bidentate ligands. The electronic spectral data of the complexes indicate that the arrangement around Ru(II) is octahedral. (author). 25 refs., 2 tabs

The hydrogen dynamics of CsH5(PO4)2 studied by means of nuclear magnetic resonance

International Nuclear Information System (INIS)

Gradisek, A; Dimnik, B; Vrtnik, S; Dolinsek, J; Wencka, M; Zdanowska Fraczek, M; Lavrova, G V

2011-01-01

We have investigated the hydrogen dynamics of cesium pentahydrogen diphosphate, CsH 5 (PO 4 ) 2 , by means of nuclear magnetic resonance (NMR) spectroscopy, in order to address the question of why there is no superprotonic phase transition in this compound, in contrast to other structurally similar hydrogen-bonded ionic salts, where a superprotonic transition is frequently found to be present. The analysis of the NMR spectrum and the spin-lattice relaxation rate revealed that the temperature-dependent hydrogen dynamics of CsH 5 (PO 4 ) 2 involves motional processes (the intra-H-bond jumps and the inter-H-bond jumps at elevated temperatures, as a mechanism of the ionic conductivity) identical to those for the other H-bonded superprotonic salts. The considerably stronger H-bond network in CsH 5 (PO 4 ) 2 prompts the search for a higher superprotonic transition temperature. However, due to the relatively weak bonding between the {[H 2 PO 4 ]} ∞ planes in the [100] direction of the CsH 5 (PO 4 ) 2 structure by means of the ionic bonding via the cesium atoms and the small number of H bonds in that direction (where out of five H bonds in the unit cell, four are directed within the {[H 2 PO 4 ]} ∞ planes and only one is between the planes), the bonds between the planes become thermally broken and the crystal melts before the H-bond network rearranges via water release into an open structure typical of the superprotonic phase. Were the coupling between the {[H 2 PO 4 ]} ∞ planes in the CsH 5 (PO 4 ) 2 somewhat stronger, the superprotonic transition would occur in the same manner as it does in other structurally related hydrogen-bonded ionic salts.

Photoluminescence and thermoluminescence characterization of Eu3+- and Dy3+ -activated Ca3(PO4)2 phosphor

International Nuclear Information System (INIS)

Nagpure, I.M.; Saha, Subhajit; Dhoble, S.J.

2009-01-01

Rare-earth-doped polycrystalline Ca 3 (PO 4 ) 2 :Eu, Ca 3 (PO 4 ) 2 :Dy and Ca 3 (PO 4 ) 2 :Eu,Dy phosphors prepared by a modified solid-state synthesis has been studied for its X-ray diffraction, thermoluminescence (TL) and photoluminescence (PL) characteristics. The PL emission spectra of the phosphor suggest the presence of Eu 3+ ion in Ca 3 (PO 4 ) 2 :Eu and Dy 3+ ion in Ca 3 (PO 4 ) 2 :Dy lattice sites. The TL glow curve of the Ca 3 (PO 4 ) 2 :Eu compounds has a simple structure with a prominent peak at 228 deg. C, while Ca 3 (PO 4 ) 2 :Dy peaking at 146 and 230 deg. C. TL sensitivity of phosphors are compared with CaSO 4 : Dy and found 1.52 and 1.20 times less in Ca 3 (PO 4 ) 2 :Eu and Ca 3 (PO 4 ) 2 :Dy phosphors, respectively. The Ca 3 (PO 4 ) 2 :Eu,Dy phosphors shows switching behavior under two different excitation wavelengths and enhancement in PL intensity of Dy 3+ ions were reported. The paper discusses the photoluminescence and thermoluminescence behavior of Eu 3+ and Dy 3+ ion in Ca 3 (PO 4 ) 2 hosts, it may be applicable to solid-state lighting as well as thermoluminescence dosimetry applications.

Crystal structures of Th(OH)PO4, U(OH)PO4 and Th2O(PO4)2. Condensation mechanism of M(IV)(OH)PO4 (M= Th, U) into M2O(PO4)2

International Nuclear Information System (INIS)

Dacheux, N.; Clavier, N.; Wallez, G.; Quarton, M.

2007-01-01

Three new crystal structures, isotypic with β-Zr 2 O(PO 4 ) 2 , have been resolved by the Rietveld method. All crystallize with an orthorhombic cell (S.G.: Cmca) with a = 7.1393(2) Angstroms, b = 9.2641(2) Angstroms, c 12.5262(4) Angstroms, V = 828.46(4) (Angstroms) 3 and Z = 8 for Th(OH)PO 4 ; a = 7.0100(2) Angstroms, b = 9.1200(2) Angstroms, c = 12.3665(3) Angstroms, V 790.60(4) (Angstroms) 3 and Z = 8 for U(OH)PO 4 ; a 7.1691(3) Angstroms, b 9.2388(4) Angstroms, c = 12.8204(7) Angstroms, V 849.15(7) (Angstroms) 3 and Z = 4 for Th 2 O(PO 4 ) 2 . By heating, the M(OH)PO 4 (M Th, U) compounds condense topotactically into M 2 O(PO 4 ) 2 , with a change of the environment of the tetravalent cation that lowers from 8 to 7 oxygen atoms. The lower stability of Th 2 O(PO 4 ) 2 compared to that of U 2 O(PO 4 ) 2 seems to result from this unusual environment for tetravalent thorium. (authors)

Crystal chemistry of M{sup II}M′{sup IV}(PO{sub 4}){sub 2} double monophosphates

Energy Technology Data Exchange (ETDEWEB)

Bregiroux, Damien, E-mail: damien.bregiroux@upmc.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Collège de France, Laboratoire de Chimie de la Matière Condensée de Paris, 11 place Marcelin Berthelot, 75005 Paris (France); Popa, Karin [“Al.I. Cuza” University, Department of Chemistry, 11-Carol I Blvd., 700506 Iasi (Romania); Wallez, Gilles [Institut de Recherche de Chimie Paris (IRCP), CNRS – Chimie ParisTech – Paris Sciences et Lettres PSL UMR8247, 11 rue Pierre et Marie Curie, 75005 Paris (France); Sorbonne Universités, UPMC Univ Paris 06 (France)

2015-10-15

M{sup II}M′{sup IV}(PO{sub 4}){sub 2} compounds have been extensively studied for several decades for their potential applications in the field of several domains such as matrices for actinides conditioning, phosphors etc. In this paper, the relationships between composition and crystal structure of these compounds are established. A review of the various processes used for the synthesis of these compounds is also proposed, as well as their most reported properties. M{sup II}M′{sup IV}(PO{sub 4}){sub 2} structures stem from two different archetypes: the cheralite and the yavapaiite structures, with some exceptions that are also described in this article. The ratio of the cations radii appears to be the most relevant parameter. The high ratio between the ionic radii of the divalent and tetravalent cations in yavapaiite derivates results in the ordering of these cations into well-differentiated polyhedra whereas cheralite is the only non-ordered structure encountered for M{sup II}M′{sup IV}(PO{sub 4}){sub 2} compounds. - Graphical abstract: In this paper, the relationships between composition and crystal structure of M{sup II}M′{sup IV}(PO{sub 4}){sub 2} compounds are established. A review of the various processes used for the synthesis of these compounds is also proposed, as well as their most reported properties. - Highlights: • Crystal structure–composition relationships of MIIM′IV(PO4)2 compounds. • Review of the various processes used for the synthesis of these compounds. • Their most reported properties are described and discussed.

Investigation of the synergistic effect of alcoholic compounds on the extraction of H3PO4 from Syrian wet phosphoric acid by TBP

International Nuclear Information System (INIS)

Abdulbaki, M. K.; Shino, O.; Wahoud, A.

2006-01-01

This paper studies the synergistic effects of alcoholic compounds such as isoamyl alcohol. Pentanol, hexanol and heptanol on the extraction of H 3 PO 4 from Syrian phosphoric acid by (TBP). The possibility to use these alcoholic compounds as a diluent instead of kerosene was also studied. The results show that the alcoholic compounds has bigger extraction yield than (TBP) diluted in kerosene. The alcoholic compounds has an important synergistic effect, when it was used as a diluent instead of kerosene, on the extraction of H 3 PO 4 by (TBP) and they have a bigger extraction yield and the quicker phase separation comparing with kerosene. Extraction of uranium, fluoride, sulfate and heavy metals is relatively small. (Authors)

Synthesis and performance of Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} cathode materials

Energy Technology Data Exchange (ETDEWEB)

Dai, Changsong; Chen, Zhenyu; Jin, Haizu; Hu, Xinguo [School of Chemical Engineering and Technology, Harbin Institute of Technology, Harbin 150001 (China)

2010-09-01

In order to search for cathode materials with better performance, Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} (0, 0.04, 0.07, 0.10 and 0.13) is prepared via a carbothermal reduction (CTR) process with LiOH.H{sub 2}O, V{sub 2}O{sub 5}, Mg(CH{sub 3}COO){sub 2}.4H{sub 2}O, NH{sub 4}H{sub 2}PO{sub 4}, and sucrose as raw materials and investigated by X-ray diffraction (XRD), scanning electron microscopic (SEM) and electrochemical impedance spectrum (EIS). XRD shows that Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} (x = 0.04, 0.07, 0.10 and 0.13) has the same monoclinic structure as undoped Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} while the particle size of Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} is smaller than that of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} according to SEM images. EIS reveals that the charge transfer resistance of as-prepared materials is reduced and its reversibility is enhanced proved by the cyclic votammograms. The Mg{sup 2+}-doped Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} has a better high rate discharge performance. At a discharge rate of 20 C, the discharge capacity of Li{sub 3}(V{sub 0.9}Mg{sub 0.1}){sub 2}(PO{sub 4}){sub 3} is 107 mAh g{sup -1} and the capacity retention is 98% after 80 cycles. Li{sub 3}(V{sub 0.9}Mg{sub 0.1}){sub 2}(PO{sub 4}){sub 3}//graphite full cells (085580-type) have good discharge performance and the modified cathode material has very good compatibility with graphite. (author)

Equilibrium diagram of KPO{sub 3}-Y(PO{sub 3}){sub 3} system, chemical preparation and characterization of KY(PO{sub 3}){sub 4}

Energy Technology Data Exchange (ETDEWEB)

Jouini, Anis; Ferid, Mokhtar; Trabelsi-Ayadi, Malika

2003-04-17

Microdifferential thermal analysis ({mu}-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO{sub 3}-Y(PO{sub 3}){sub 3} system. The only compound observed within the system was KY(PO{sub 3}){sub 4} melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO{sub 3}){sub 3} at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO{sub 3} was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO{sub 3}){sub 4} polyphosphate has the P2{sub 1} space group with lattice parameters: a=7.183(4) A, b=8.351(6) A, c=7.983(3) A, {beta}=91.75(3) deg. and Z=2 is isostructural with KNd(PO{sub 3}){sub 4}. The second allotropic form of KY(PO{sub 3}){sub 4} belongs to the P2{sub 1}/n space group with lattice parameters: a=10.835(3) A, b=9.003(2) A, c=10.314(1) A, {beta}=106.09(7) deg. and Z=4 and is isostructural with TlNd(PO{sub 3}){sub 4}. The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP{sub 4}O{sub 12} crystallizes in the C2/c space group with lattice parameters: a=7.825(3) A, b=12.537(4) A, c=10.584(2) A, {beta}=110.22(7) deg. and Z=4 is isostructural with RbNdP{sub 4}O{sub 12} and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported.

(Solid + liquid) phase equilibria of (Ca(H2PO2)2 + CaCl2 + H2O) and (Ca(H2PO2)2 + NaH2PO2 + H2O) ternary systems at T = 323.15 K

International Nuclear Information System (INIS)

Cao, Hong-yu; Zhou, Huan; Bai, Xiao-qin; Ma, Ruo-xin; Tan, Li-na; Wang, Jun-min

2016-01-01

Graphical abstract: Solubility diagram of the (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) system at T = (323.15 and 298.15) K. - Highlights: • Phase diagrams of Ca 2+ -H 2 PO 2 − -Cl − -H 2 O, Ca 2+ -Na + -H 2 PO 2 − -H 2 O at 323.15 K were obtained. • Incompatible double salt of NaCa(H 2 PO 2 ) 3 in Ca 2+ -Na + -H 2 PO 2 − -H 2 O system was determined. • Density diagram of the corresponding liquid were simultaneously measured. - Abstract: Calcium hypophosphite has been widely used as an anti-corrosive agent, flame retardant, fertilizer, assistant for Ni electroless plating, and animal nutritional supplement. High purity calcium hypophosphite can be synthesized via the replacement reaction of sodium hypophosphite and calcium chloride. In this work, the (solid + liquid) phase equilibria of (Ca(H 2 PO 2 ) 2 + CaCl 2 + H 2 O) and (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) ternary systems at T = 323.15 K were studied experimentally via the classical isothermal solubility equilibrium method, and the phase diagrams for these two systems were obtained. It was found that two solid salts of CaCl 2 ·2H 2 O and Ca(H 2 PO 2 ) 2 exist in the (Ca(H 2 PO 2 ) 2 + CaCl 2 + H 2 O) system, and three salts of Ca(H 2 PO 2 ) 2 , NaH 2 PO 2 ·H 2 O and one incompatible double salt, NaCa(H 2 PO 2 ) 3 occur in the (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) system.

Analysis of (NH4)2SO4/(NH4)H2PO4 mixtures by thermogravimetry and X-ray diffraction

International Nuclear Information System (INIS)

Perez, Jose; Perez, Eduardo; Vas, Beatriz del; Garcia, Luis; Serrano, Jose Luis

2006-01-01

(NH 4 ) 2 SO 4 and (NH 4 )H 2 PO 4 are the principal components in the powder material used in fire extinguishers. In this paper the mutual influence in their thermal decomposition is investigated by thermogravimetry. Two methods for the quantification of both salts in mixtures (NH 4 ) 2 SO 4 /(NH 4 )H 2 PO 4 are proposed. The first employs thermogravimetry and is based on the measurement of the mass fraction in the 500-550 deg. C interval, once (NH 4 ) 2 SO 4 has totally decomposed to yield gaseous products. The second uses some selected peaks in the X-ray diffractogram

A fast synthesis of Li 3V 2(PO 4) 3 crystals via glass-ceramic processing and their battery performance

Science.gov (United States)

Nagamine, Kenta; Honma, Tsuyoshi; Komatsu, Takayuki

A synthesis of Li 3V 2(PO 4) 3 being a potential cathode material for lithium ion batteries was attempted via a glass-ceramic processing. A glass with the composition of 37.5Li 2O-25V 2O 5-37.5P 2O 5 (mol%) was prepared by a melt-quenching method and precursor glass powders were crystallized with/without 10 wt% glucose in N 2 or 7%H 2/Ar atmosphere. It was found that heat treatments with glucose at 700 °C in 7%H 2/Ar can produce well-crystallized Li 3V 2(PO 4) 3 in the short time of 30 min. The battery performance measurements revealed that the precursor glass shows the discharge capacity of 14 mAh g -1 at the rate of 1 μA cm -2 and the glass-ceramics with Li 3V 2(PO 4) 3 prepared with glucose at 700 °C in 7%H 2/Ar show the capacities of 117-126 mAh g -1 (∼96% of the theoretical capacity) which are independent of heat treatment time. The present study proposes that the glass-ceramic processing is a fast synthesizing route for Li 3V 2(PO 4) 3 crystals.

Uncommon potential hysteresis in the Li/Li{sub 2x}VO(H{sub 2-x}PO{sub 4}){sub 2} (0 {<=} x {<=} 2) system

Energy Technology Data Exchange (ETDEWEB)

Dubarry, M. [Institut des Materiaux Jean Rouxel, 2 rue de la Houssiniere, BP32229, 44322 Nantes Cedex 3 (France); Gaubicher, J. [Institut des Materiaux Jean Rouxel, 2 rue de la Houssiniere, BP32229, 44322 Nantes Cedex 3 (France)], E-mail: joel.gaubicher@cnrs-imn.fr; Guyomard, D. [Institut des Materiaux Jean Rouxel, 2 rue de la Houssiniere, BP32229, 44322 Nantes Cedex 3 (France); Wallez, G.; Quarton, M. [Laboratoire de Cristallochimie du Solide, Universite Pierre et Marie Curie-Paris VI, 4 place Jussieu, 75252 Paris Cedex 05 (France); Baehtz, C. [Deutsches Elektronen Synchrotron HASYLAB, Notkestr. 85, 22607 Hamburg (Germany)

2008-05-20

Physical and electrochemical investigations of vanadium phosphates, Li{sub 2x}VO(H{sub 2-x}PO{sub 4}){sub 2} (0 < x < 2), have been undertaken. H{sup +}/Li{sup +} ionic exchange from VO(H{sub 2}PO{sub 4}){sub 2} to Li{sub 2}VO(HPO{sub 4}){sub 2} leads to grain decrepitation. Further ionic exchange toward formation of Li{sub 4}VO(PO{sub 4}){sub 2} lowers the symmetry. As inferred from potentiodynamic cycling correlated to ex situ and in situ X-ray diffraction (XRD), the system Li/Li{sub 4}VO(PO{sub 4}){sub 2} shows several phase transformations that are associated with thermodynamical potential hysteresis that span from roughly 15 mV to more than 1.8 V. Small hysteresis are associated with topotactic reactions and with V{sup V}/V{sup IV} and V{sup III}/V{sup II} redox couples. Large potential hysteresis values (>1 V) were observed when oxidation of V{sup III} to V{sup IV} is involved.

One-pot syntheses of Li3V2(PO4)3/C cathode material for lithium ion batteries via ascorbic acid reduction approach

International Nuclear Information System (INIS)

Huang, J.S.; Yang, L.; Liu, K.Y.

2011-01-01

Highlights: → Ascorbic acid (C 6 H 8 O 6 ) was used as reducing agent and organic carbon source. → The strategy shortened the period of material preparation and lowered energy cost. → Li 3 V 2 (PO 4 ) 3 /C was obtained with enhanced electrochemical performance. → Effects of reagents on electrochemical performance of Li 3 V 2 (PO 4 ) 3 were evaluated. - Abstract: Monoclinic Li 3 V 2 (PO 4 ) 3 /C composite synthesized by ascorbic acid reduction method is examined as a cathode material for Li-ion batteries. Transmission electron microscopy (TEM) images show that the nano-size particles are obtained. The reversible capacity of Li 3 V 2 (PO 4 ) 3 /C prepared with LiOH and H 3 PO 4 is 141.2 mAh g -1 after 100 cycles at 1C discharge rate between 3 V and 4.8 V, and the retention rates of discharge capacity is 93.4%. Ascorbic acid plays not only as reduction reagent, but also as carbon sources. This strategy shortens the time of solid state reaction and facilitates the procedure of synthesis. Effects of different precursors materials on the performance of the Li 3 V 2 (PO 4 ) 3 /C are investigated.

Development of a lymphscintigraphy agent: Tc-99m-Sn-PO4

International Nuclear Information System (INIS)

Gilliland, D.L.; Basmadjian, G.P.; Kirschner, A.S.; Leonard, J.C.; Ice, R.D.

1979-01-01

Stannous chloride dissolved in a solution of Na 2 HO 4 pH 9.0 gives a stable solution of Sn(II) ions. When pertechnetate-99m is added to such a solution, a stable, soluble complex of technetium-99m-Sn-PO 4 results. This is a mixed metal complex in which the Tc is present in the (III) + oxidation state and the Sn is an integral part of the complex. This complex, when injected I.V., localizes in the RES due to the formation of an in-vivo colloid with Ca(II) ions in the blood. When injected subcutaneously (SC), the complex travels through the lymphatic channels and localizes in the lymph nodes. In rabbits, axillary and popliteal nodes were visualized after injecting SC into the dorsum of the hind and fore paws. In addition, uptake by the liver, kidneys and bone marrow was noted. After intratesticular injection in dogs, the para-aortic lymph nodes were imaged at 3 to 30 minutes

Toluene and chlorobenzene dinitration over solid H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2} catalyst

Energy Technology Data Exchange (ETDEWEB)

Adamiak, Joanna, E-mail: jadamiak@ch.pw.edu.pl [Warsaw University of Technology, Faculty of Chemistry, Division of High Energetic Materials, Noakowskiego 3, 00-664 Warsaw (Poland); Kalinowska-Alichnewicz, Dorota; Szadkowski, Michal; Skupinski, Wincenty [Warsaw University of Technology, Faculty of Chemistry, Division of High Energetic Materials, Noakowskiego 3, 00-664 Warsaw (Poland)

2011-11-15

Highlights: {yields} A novel catalyst H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2} was characterized and used in nitration. {yields} On the surface domains of phosphomolybdic acid (HPM) are obtained. {yields} Dinitrotoluene is obtained with very high yield i.e. 96 wt.% in mild conditions. {yields} Dinitrochlorobenzene is obtained with only twelve-fold excess of nitric acid. {yields} It is sulfuric acid free and solvent free nitration of aromatic compounds. - Abstract: A new catalyst, H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2}, was prepared by modification of MoO{sub 3}/SiO{sub 2} using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds.

Synthesis and electrochemical properties of xLiMn0.9Fe0.1PO4·yLi3V2(PO4)3/C composite cathode materials for lithium–ion batteries

International Nuclear Information System (INIS)

Wu, Ling; Lu, JiaJia; Wei, Gui; Wang, Pengfei; Ding, Hao; Zheng, Junwei; Li, Xiaowei; Zhong, Shengkui

2014-01-01

Highlights: • xLiMn 0.9 Fe 0.1 PO4·yLi 3 V 2 (PO 4 ) 3 /C composites are prepared by a solid-state method. • The addition of Li 3 V 2 (PO 4 ) 3 can improve the properties of LiMn 0.9 Fe 0.1 PO 4 . • Mutual doping occurrs between the LiMn 0.9 Fe 0.1 PO 4 and Li 3 V 2 (PO 4 ) 3 phases. • 5LiMn 0.9 Fe 0.1 PO 4 ·Li 3 V 2 (PO 4 ) 3 /C shows the best electrochemical properties. - Abstract: The xLiMn 0.9 Fe 0.1 PO 4 ·yLi 3 V 2 (PO 4 ) 3 /C (x:y=1:0, 9:1 5:1, 3:1, 1:1 and 0:1) cathode materials are synthesized by a ball–milling and post–calcination method. XRD results reveal that the xLiMn 0.9 Fe 0.1 PO 4 ·yLi 3 V 2 (PO 4 ) 3 /C (x,y≠0) composites are composed of LiMn 0.9 Fe 0.1 PO 4 and Li 3 V 2 (PO 4 ) 3 phases, and no impurities are detected. In LiMn 0.9 Fe 0.1 PO 4 –Li 3 V 2 (PO 4 ) 3 system, most of the manganese, iron and vanadium elements in the raw materials tend to form the two major phases, and only small amounts of V, Mn and Fe as dopants enter into the lattice of LiMn 0.9 Fe 0.1 PO 4 and Li 3 V 2 (PO 4 ) 3 . Electrochemical tests show that the xLiMn 0.9 Fe 0.1 PO 4 ·yLi 3 V 2 (PO 4 ) 3 /C (x,y≠0) composites exhibit much better performance than the single LiMn 0.9 Fe 0.1 PO 4 /C. Among the samples, 5LiMn 0.9 Fe 0.1 PO 4 ·Li 3 V 2 (PO 4 ) 3 /C shows the best electrochemical performance. The sample delivers the specific capacities of 158.1, 140.7 and 100.2 mAh g −1 at 0.05, 1 and 4 C rates in the potential range of 2.5–4.5 V, and exhibits very long and flat discharge plateau around 4.0 V up to 1 C rate. The sample also shows good cycling performance at various C–rates

Modeling Li-ion conductivity in LiLa(PO3)4 powder

International Nuclear Information System (INIS)

Mounir, Ferhi; Karima, Horchani-Naifer; Khaled, Ben Saad; Mokhtar, Férid

2012-01-01

Polycrystalline powder and single-crystal of LiLa(PO 3 ) 4 are synthesized by solid state reaction and flux technique, respectively. A morphological description of the obtained product was made based on scanning electron microscopy micrographs. The obtained powder was characterized by X-ray powder diffraction, FTIR and Raman spectroscopies. Ionic conductivity of the LiLa(PO 3 ) 4 powder was measured and evaluated over a temperature range from 553 to 913 K. Single crystals of LiLa(PO 3 ) 4 are characterized by single-crystal X-ray diffraction. The LiLa(PO 3 ) 4 structure was found to be isotypic with LiNd(PO 3 ) 4 . It crystallizes in the monoclinic system with space group C2/c and cell parameters: a=16.635(6) Å, b=7.130(3) Å, c=9.913(3) Å, β=126.37(4)°, V=946.72(6) Å 3 and Z=4. The LiLa(PO 3 ) 4 structure was described as an alternation between spiraling chains (PO 3 ) n and (La 3+ , Li + ) cations along the b direction. The small Li + ions, coordinated to four oxygen atoms, were located in the large connected cavities created between the LaO 8 polyhedra and the polyphosphate chains. The jumping of Li + through tunnels of the crystalline network was investigated using complex impedance spectroscopy. The close value of the activation energies calculated through the analysis of conductivity data and loss spectra indicate that the transport in the investigated system is through hopping mechanism. The correlation between ionic conductivity of LiLa(PO 3 ) 4 and its crystallographic structure was investigated and the most probably transport pathway model was determined.

Effect of synthesizing method on the properties of LiFePO4/C composite for rechargeable lithium-ion batteries

Science.gov (United States)

Yoon, Man-Soon; Islam, Mobinul; Park, Young Min; Ur, Soon-Chul

2013-03-01

Olivine-type LiFePO4/C cathode materials are fabricated with FePO4 powders that are pre-synthesized by two different processes from iron chloride solution. Process I is a modified precipitation method which is implemented by the pH control of a solution using NH4OH to form FePO4 precipitates at room temperature. Process II is a conventional precipitation method, of which H3PO4 (85%) solution is gradually added to a FeCl3 solution during the process to maintain a designated mole ratio. The solution is subsequently aged at 90°C in a water bath until FePO4 precipitates appear. In order to synthesize LiFePO4/C composites, each batch of FePO4 powders is then mixed with pre-milled lithium carbonate and glucose (8 wt. %) as a carbon source in a ball-mill. The structural characteristics of both LiFePO4/C composites fabricated using iron phospates from two different routes have been examined employing XRD and SEM. The modified precipitation process is considered to be a relatively simple and effective process for the preparation of LiFePO4/C composites owing to their excellent electrochemical properties and rate capabilities.

Energy transfer mechanism from Gd3+ to Sm3+ in K3Gd(PO4)2:Sm3+ phosphor

International Nuclear Information System (INIS)

Gupta, Palvi; Bedyal, A K; Kumar, Vinay; Khajuria, Y; Sharma, Vishal; Ntwaeaborwa, O M; Swart, H C

2015-01-01

Undoped K 3 Gd(PO 4 ) 2 and trivalent samarium (0.5–2.5 mol%) doped K 3 Gd(PO 4 ) 2 phosphors were synthesized by the solid-state method. The phase formation, optical and luminescence properties were investigated by x-ray diffraction (XRD), diffuse reflectance (DR) spectroscopy, and photoluminescence (PL) spectroscopy. The fluorescence decay spectra of the obtained phosphors were also recorded to study the energy transfer from sensitizer (Gd 3+ ) to activator (Sm 3+ ). Energy transfer effects from sensitizer to activator caused by rare-earth ions were mainly observed in the obtained PL and lifetime spectra. The decay curves of K 3 Gd(PO 4 ) 2 phosphor with different Sm 3+ ions concentrations were found to be non-exponential and the data is well fitted with the Inokuti–Hirayama (I–H) model. The energy transfer parameters such as critical distance for the transfer processes were determined. The Commission Internationale de l’Eclairage (CIE) chromatic coordinates and color-correlated temperature were also determined for the prepared phosphor. (paper)

Calcioferrite with composition (Ca3.94Sr0.06Mg1.01(Fe2.93Al1.07(PO46(OH4·12H2O

Directory of Open Access Journals (Sweden)

Barbara Lafuente

2014-03-01

Full Text Available Calcioferrite, ideally Ca4MgFe3+4(PO46(OH4·12H2O (tetracalcium magnesium tetrairon(III hexakis-phosphate tetrahydroxide dodecahydrate, is a member of the calcioferrite group of hydrated calcium phosphate minerals with the general formula Ca4AB4(PO46(OH4·12H2O, where A = Mg, Fe2+, Mn2+ and B = Al, Fe3+. Calcioferrite and the other three known members of the group, montgomeryite (A = Mg, B = Al, kingsmountite (A = Fe2+, B = Al, and zodacite (A = Mn2+, B = Fe3+, usually occur as very small crystals, making their structure refinements by conventional single-crystal X-ray diffraction challenging. This study presents the first structure determination of calcioferrite with composition (Ca3.94Sr0.06Mg1.01(Fe2.93Al1.07(PO46(OH4·12H2O based on single-crystal X-ray diffraction data collected from a natural sample from the Moculta quarry in Angaston, Australia. Calcioferrite is isostructural with montgomeryite, the only member of the group with a reported structure. The calcioferrite structure is characterized by (Fe/AlO6 octahedra (site symmetries 2 and -1 sharing corners (OH to form chains running parallel to [101]. These chains are linked together by PO4 tetrahedra (site symmetries 2 and 1, forming [(Fe/Al3(PO43(OH2] layers stacking along [010], which are connected by (Ca/Sr2+ cations (site symmetry 2 and Mg2+ cations (site symmetry 2; half-occupation. Hydrogen-bonding interactions involving the water molecules (one of which is equally disordered over two positions and OH function are also present between these layers. The relatively weaker bonds between the layers account for the cleavage of the mineral parallel to (010.

Photoluminescence characteristics of Sm{sup 3+} doped Ba{sub 3}La(PO{sub 4}){sub 3} as new orange-red emitting phosphors

Energy Technology Data Exchange (ETDEWEB)

Yu, Ruijin [College of Science, Northwest A and F University, Yangling, Shaanxi 712100 (China); Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of); Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Mi Noh, Hyeon; Kee Moon, Byung; Chun Choi, Byung [Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of); Hyun Jeong, Jung, E-mail: jhjeong@pknu.ac.kr [Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of); Sueb Lee, Ho [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Jang, Kiwan, E-mail: kwjang@changwon.ac.kr [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Soo Yi, Soung [Department of Electronic Material Engineering, Silla University, Busan 617-736 (Korea, Republic of)

2014-01-15

A series of orange-red emitting Ba{sub 3}La(PO{sub 4}){sub 3}:xSm{sup 3+} (0.01≤x≤0.30) phosphors was synthesized by the convenient solid-state reaction. X-ray diffraction and photoluminescence spectra were utilized to characterize the structure and luminescence properties of the as-synthesized phosphors. The emission spectra of the Ba{sub 3}La(PO{sub 4}){sub 3}:Sm{sup 3+} phosphors consisted of some sharp emission peaks of Sm{sup 3+} ions centered at 563 nm, 600 nm, 647 nm, 710 nm. The strongest one is located at 600 nm due to {sup 4}G{sub 5/2}–{sup 6}H{sub 7/2} transition of Sm{sup 3+}, generating bright orange-red light. The optimum dopant concentration of Sm{sup 3+} ions in Ba{sub 3}La(PO{sub 4}):xSm{sup 3+} is around 5 mol% and the critical transfer distance of Sm{sup 3+} is calculated as 22 Å. The CIE chromaticity coordinates of the Ba{sub 3}La(PO{sub 4}){sub 3}:0.05Sm{sup 3+} phosphors was is located in the orange reddish region. The Ba{sub 3}La(PO{sub 4}){sub 3}:Sm{sup 3+} phosphors may be potentially used as red phosphors for white light-emitting diodes. -- Highlights: • A new Sm{sup 3+}-doped Ba{sub 3}La(PO{sub 4}){sub 3} phosphor was firstly synthesized. • Its structure, luminescent properties are well studied and characterized. • The Ba{sub 3}La(PO{sub 4}){sub 3}:Sm{sup 3+} shows bright orange reddish emissions under UV excitation.

Crystal structure of Na3Sc2(PO4)3 at 60 deg C

International Nuclear Information System (INIS)

Lazoryak, B.I.; Kalinin, V.B.; Stefanovich, S.Yu.; Efremov, V.A.

1980-01-01

The structure of the ferroelectric phase of Na 3 Sc 2 (PO 4 ) 3 compound was studied. Na 3 Sc 2 (PO 4 ) 3 monocrystal heated by a jet of warm N 2 was investigated at 60 deg C. The rhombohedron modification was determined: a=8.927(3), c=22.34(4) A, Z=6, space group R anti 3c. Interatomic distances and inner angles of polyhedrons in Na 3 Sc 2 (PO 4 ) 3 structure were determined

Microwave assisted synthesis of core–shell LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C nanocomposite cathode for high-performance lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Li, Huanhuan [Automotive Engineering Research Institute, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013 (China); Li, Yunxing [School of Material Science and Engineering, Jiangsu University, Zhenjiang 212013 (China); Chen, Long; Jiang, Haobin [Automotive Engineering Research Institute, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013 (China); Wei, Jinping [Institute of New Energy Material Chemistry, Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Nankai University, Tianjin 300071 (China); Wang, Hongbo [China Aviation Lithium Battery Co. Ltd., Luoyang 471003 (China); Wang, Yaping, E-mail: wangyaping@ujs.edu.cn [School of Material Science and Engineering, Jiangsu University, Zhenjiang 212013 (China)

2014-12-25

Highlights: • We firstly report a fast microwave heating way to prepare LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C. • The reversible discharge capacity of LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C is about 169 mA h g{sup −1}. • LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C nanocomposite elucidates excellent cyclic stability. • LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C nanocomposite exhibits attractive rate capability. - Abstract: A microwave assisted method is developed for synthesizing pure LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4} and LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C nanocomposite. Olivine LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4} coated with uniform amorphous carbon film of ∼5 nm in thickness with an average size of ∼200 nm is successfully obtained. Compared with pure LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}, LiFe{sub 1/3}Mn{sub 1/3}Co{sub 1/3}PO{sub 4}/C composite presents enhanced electrochemical Li-ion intercalation performances. It exhibits a high discharge capacity of 169 mA h g{sup −1} at 0.1 C (theoretical capacity is 170 mA h g{sup −1}). The capacity retention is 99% after 30 cycles. Furthermore, the capacities are still retained 101 at 5 C and 76 mA h g{sup −1} and 20 C, respectively. Carbon coating can significantly improve the Li-ion diffusion, the reversibility of lithium extraction/insertion and electrical conductivity of LiCo{sub 1/3}Mn{sub 1/3}Fe{sub 1/3}PO{sub 4}.

A novel inorganic-organic compound: Synthesis and structural characterization of tin(II) phenylbis(phosphonate), Sn2(PO3C6H4PO3)

International Nuclear Information System (INIS)

Subbiah, Ayyappan; Bhuvanesh, Nattamai; Clearfield, Abraham

2005-01-01

A novel tin(II) phenylbis(phosphonate) compound has been synthesized hydrothermally and its structure has been determined by single crystal X-ray diffraction. The structure is monoclinic, space group P2 1 /c (no. 14), a=4.8094(4), b=16.2871(13), c=6.9107(6)A; β=106.292(6) o , V=519.59(7)A 3 , Z=2. The three-dimensional structure consists of 3-coordinated tin and 4-coordinated phosphorus double layers separated (pillared) by phenyl rings. These phenyl rings are placed 4.8A apart along the a-axis in the structure resulting in lower surface area (∼14m 2 /g). The porosity has been increased by replacing phenyl groups by methyl groups (∼31m 2 /g)

Luminescent properties of Mg3Ca3(PO4)4: Eu2+ blue-emitting phosphor for white light emitting diodes

International Nuclear Information System (INIS)

Li Yinqun; Deng Degang; Wang Qian; Li Gaofeng; Hua Youjie; Jia Guohua; Huang Lihui; Zhao Shilong; Wang Huanping; Li Chenxia; Xu Shiqing

2012-01-01

A blue-emitting phosphor, Eu 2+ -activated Mg 3 Ca 3 (PO 4 ) 4 phosphor was synthesized by conventional solid-state reaction. X-ray powder diffraction (XRD) analysis confirmed the phase formation. Photoluminescence (PL) results showed that Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ could be efficiently excited by UV–visible light from 250 to 430 nm, which matched well with the emission wavelengths of near-UV and UV LED chips. The effects of the doped-Eu 2+ concentration in Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ on the PL were also investigated. The result reveals that Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ is a potential blue-emitting phosphor for white LEDs. - Graphical Abstract: The excitation spectra show a broad peak from 250 to 430 nm, which means Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ phosphor can be suitable for application in white LEDs excited by the near-UV and UV LEDs. The emission spectrum peaked at 456 nm with the full-width half-maximum (FWHM) of 102 nm is attributed to the 4f 6 5d 1 –4f 7 transition of the Eu 2+ ion. The asymmetric emission spectra show that Eu 2+ has more one emission center in Mg 3 Ca 3 (PO 4 ) 4 , which can be deconvoluted into at least four Gaussian components peaked at 423, 446, 483 and 510 nm. Highlights: ► Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ phosphor could be effectively excited by UV chips (360–430 nm). ► Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ phosphor is a potential blue-emitting phosphor for white LEDs. ► Mg 3 Ca 3 (PO 4 ) 4 : Eu 2+ phosphor shows a broadband emission.

Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst.

Science.gov (United States)

Adamiak, Joanna; Kalinowska-Alichnewicz, Dorota; Szadkowski, Michał; Skupiński, Wincenty

2011-11-15

A new catalyst, H(3)PO(4)/MoO(3)/SiO(2), was prepared by modification of MoO(3)/SiO(2) using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

Investigation on pseudosymmetry, twinning and disorder in crystal structure determinations: Ba(H2O)M2III[PO3(OH)]4 (M=Fe, V) as examples

International Nuclear Information System (INIS)

Sun Wei; Huang Yaxi; Pan Yuanming; Mi Jinxiao

2012-01-01

Twinning commonly occurs in monoclinic crystals with dimensionally similar a and c axes and results in pseudo-orthorhombic symmetries with overlapping diffractions. For example, twinning in the new synthetic compound Ba(H 2 O)Fe 2 [PO 3 (OH)] 4 , which varies in space group from P2 1 to P2 1 /c with approximately equal a and c axial lengths, gives rise to a pseudosymmetry of C222 1 . Similarly, the related compound Ba(H 2 O)V 2 [PO 3 (OH)] 4 is commonly twinned and varies in space groups as well, arising from ordered to disordered distributions of the barium cations and water molecules in the cavities. Moreover, analyses of these and other twinned structures show that the small average standard uncertainty of bond distances is a sensitive criterion for structure determinations, especially for those involving crystal twinning as well as order–disorder. A proper structure determination leads to small standard uncertainties of the atomic displacement parameters, which further result in the small standard uncertainties of bond distances. - Graphical abstract: Ba(H 2 O)M 2 III [PO 3 (OH)] 4 (M=Fe, V) varies in space group from P2 1 to P2 1 /c, arising from ordered to disordered distributions of Ba 2+ and H 2 O in the cavities. Highlights: ► Twinning commonly occurs in monoclinic crystals with a≈c. ► Overlapping diffractions from twin domains hamper with the determination of real space groups. ► Conventional criteria for evaluating the real space groups are not effective in this case. ► Small standard uncertainty of bond distances is proposed as a sensitive criterion. ► Using this criterion we determined the order–disorder structures of Ba(H 2 O)M 2 III [PO 3 (OH)] 4 (M=Fe, V) from twinned crystals.

Cation mobility in NASICON compounds Li1-xZr2-xNbx(PO4)3 and Li1+xZr2-xScx(PO4)3

International Nuclear Information System (INIS)

Stenina, I.A.; Yaroslavtsev, A.B.; Aliev, A.D.; Antipov, E.V.; Velikodnyj, Yu.A.; Rebrov, A.I.

2002-01-01

Compounds featuring NASICON structure of the composition Li 1-x Zr 2-x Nb x (PO 4 ) 3 and Li 1+x Zr 2-x Sc x (PO 4 ) 3 were studied by the method of X-ray phase analysis and 7 Li and 31 P NMR. Structure of Li 0.8 Zr 1.8 Nb 0.2 (PO 4 ) 3 was refined on the basis of X-ray powder pattern. It is shown that cationic disordering in LiZr 2 (PO 4 ) 3 is stimulated both by cationic vacancies and interstitial atoms formation. The cationic vacancies are characterized by a higher mobility. The level of intrinsic disordering was estimated and the Frenkel constant for the compound was calculated [ru

Effect of VO43− substitution for PO43− on electrochemical properties of the Li3Fe2(PO4)3 cathode materials

International Nuclear Information System (INIS)

Yang, Yonggang; Zhang, Yongguang; Hua, Zhengshen; Wang, Xin; Peng, Huifen; Bakenov, Zhumabay

2016-01-01

Graphical abstract: VO 4 3− –substituted Li 3 Fe 2 (PO 4 ) 3 samples were prepared by sol-gel method. The VO 4 3− substitution remarkably improves the rate capability and cycling performance of the Li 3 Fe 2 (PO 4 ) 3 due to improved conductivity and enhanced lithium ion diffusion. - Highlights: • Mixed anion effect was used to improve electrochemical properties of Li 3 Fe 2 (PO 4 ) 3 . • The VO 4 3− substitution improved rate capability and cyclability of Li 3 Fe 2 (PO 4 ) 3 . • The Li 3 Fe 2 (PO 4 ) 2.55 (VO 4 ) 0.45 material shows the excellent electrochemical performance. - Abstract: In this research, VO 4 3− substitution was used to improve electrochemical properties of the Nasicon Li 3 Fe 2 (PO 4 ) 3 cathode material. The VO 4 3− substitution resulted in formation of a homogeneous compound Li 3 Fe 2 (PO 4 ) 3-x (VO 4 ) x in a composition range of x ≤ 0.45; further introduction of VO 4 3− led to precipitation of some other phases. It was shown that the VO 4 3− substituted samples presented discharging capacity higher than that of bare non-substituted Nasicon and the reported Ti 4+ and Mn 2+ doped ones. The Li 3 Fe 2 (PO 4 ) 2.55 (VO 4 ) 0.45 material exhibited excellent cycling stability and rate capability, and retained a capacity of 91.8 mAh g −1 after 60 cycles at 2C charge-discharge rate. This value is one of the highest reported to date for the Li 3 Fe 2 (PO 4 ) 3 compound, and was about 48% higher than that of the latter. The electrochemical performance enhancements for the VO 4 3− substituted samples were attributed to the reduction of charge transfer resistance, increase of electrical conductivity, and fast lithium ion diffusion behavior. Hence, the obtained results proved that the VO 4 3− anion substitution for PO 4 3− is a powerful technique to improve the electrochemical performance of the studied Nasicon compound.

Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

Science.gov (United States)

Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

Optical and crystal chemistry studies of Na3Ln(PO4)2-K3Ln(PO4)2 (Ln=Eu, Gd)

International Nuclear Information System (INIS)

Mesnaoui, M.; Maazaz, M.

1987-01-01

In these systems, large single phase domains are separated by two phase regions. The structural evolution as a function of composition is analysed both by X-ray diffraction and by using Eu 3+ and Gd 3+ as luminescent local structural probes. Due to layer type structure of the K 3 Ln(PO 4 ) 2 phases an exchange reaction resulting in total substitution of sodium for potassium can be carried out with formation of metastable Na 3 Ln(PO 4 ) 2 phases, the structure of which is close to those of the potassium compounds. 10 refs.; 18 figs [fr

Phase equilibria in the NaF-CdO-NaPO{sub 3} system at 873 K and crystal structure and physico-chemical characterizations of the new Na{sub 2}CdPO{sub 4}F fluorophosphate

Energy Technology Data Exchange (ETDEWEB)

Aboussatar, Mohamed [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Laboratoire de Physico-Chimie de l’État Solide, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax (Tunisia); Mbarek, Aïcha [Laboratoire de Chimie Industrielle, Ecole Nationale d’Ingénieurs de Sfax, Université de Sfax, BP W3038, 3000 Sfax (Tunisia); Naili, Houcine [Laboratoire de Physico-Chimie de l’État Solide, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax (Tunisia); El-Ghozzi, Malika [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Chadeyron, Geneviève [Université Clermont Auvergne, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS/UBP/SIGMA, BP 10448, F-63000 Clermont-Ferrand (France); Avignant, Daniel [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Zambon, Daniel, E-mail: Daniel.Zambon@univ-bpclermont.fr [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France)

2017-04-15

Isothermal sections of the diagram representing phase relationships in the NaF-CdO-NaPO{sub 3} system have been investigated by solid state reactions and powder X-ray diffraction. This phase diagram investigation confirms the polymorphism of the NaCdPO{sub 4} side component and the structure of the ß high temperature polymorph (orthorhombic, space group Pnma and unit cell parameters a=9.3118(2), b=7.0459(1), c=5.1849(1) Å has been refined. A new fluorophosphate, Na{sub 2}CdPO{sub 4}F, has been discovered and its crystal structure determined and refined from powder X-ray diffraction data. It exhibits a new 3D structure with orthorhombic symmetry, space group Pnma and unit cell parameters a=5.3731(1), b=6.8530(1), c=12.2691(2) Å. The structure is closely related to those of the high temperature polymorph of the nacaphite Na{sub 2}CaPO{sub 4}F and the fluorosilicate Ca{sub 2}NaSiO{sub 4}F but differs essentially in the cationic repartition since the structure is fully ordered with one Na site (8d) and one Cd site (4c). Relationships with other Na{sub 2}M{sup II}PO{sub 4}F (M{sup II}=Mg, Ca, Mn, Fe, Co, Ni) have been examined and the crystal-chemical and topographical analysis of these fluorophosphates is briefly reviewed. IR, Raman, optical and {sup 19}F, {sup 23}Na, {sup 31}P MAS NMR characterizations of Na{sub 2}CdPO{sub 4}F have been investigated. - Graphical abstract: The structure of the compound Na{sub 2}CdPO{sub 4}F, discovered during the study of the phase relationships in the NaF-CdO-NaPO{sub 3} system, has been determined and compared with other Na{sub 2}M{sup II}PO{sub 4}F fluorophosphates. - Highlights: • XRD analysis of the isothermal section of the NaF-CdO-NaPO{sub 3} system at 923 K. • Rietveld refinement of the high temperature polymorph β-NaCdPO{sub 4}. • Crystal structure of the new Na{sub 2}CdPO{sub 4}F fluorophosphate determined from powder XRD. • Crystal structure - composition relationships of Na{sub 2}M{sup II}PO{sub 4}F compounds

Synthesis and regulation of α-LiZnPO4.H2O via a solid-state reaction at low-heating temperatures

International Nuclear Information System (INIS)

Liao Sen; Chen Zhipeng; Tian Xiaozhen; Wu Wenwei

2009-01-01

A simple and novel route for the synthesis of a lithium zinc phosphate hydrate, α-LiZnPO 4 .H 2 O, was studied, and the target product was obtained with LiH 2 PO 4 .H 2 O and ZnCO 3 as raw materials and polyethylene glycol-400 (PEG-400) as a surfactant via a one step solid-state reaction at room temperature (25 deg. C). The product was characterized with X-ray powder diffraction (XRD), thermogravimetric analysis and the 1st derivativative of thermogravimetric analysis (TG/DTG) and Fourier transform infrared spectroscopy (FTIR). The comparison experimental results suggested that aging temperature controlled the products of the synthesis, that is, the α-LiZnPO 4 .H 2 O was formed when the reaction mixture was aged at room temperature, and the α-LiZnPO 4 was obtained when the reaction mixture was aged at 80 deg. C.

Synthesis and luminescence characteristics of Dy{sup 3+} doped KLa(PO{sub 3}){sub 4}

Energy Technology Data Exchange (ETDEWEB)

Chemingui, S.; Ferhi, M., E-mail: ferhi.mounir@gmail.com; Horchani-Naifer, K.; Férid, M.

2015-10-15

Polycrystalline powders of KLa{sub (1−x)}Dy{sub x}(PO{sub 3}){sub 4} (x=0.5%, 1%, 5% and 10%) with linear chain have been grown by solid state reaction. The obtained powders are characterized by X-ray powder diffraction, FTIR and Raman spectroscopies. Emission, excitation spectra and decay curves analysis have been used to study the spectroscopic properties of Dy{sup 3+} in KLa(PO{sub 3}){sub 4}. The photoluminescence spectra show two characteristic blue and yellow bands of Dy{sup 3+}. The yellow-to-blue emission intensity ratios and CIE chromaticity coordinates have been determined from emission spectra to evaluate the emitted light as function of Dy{sup 3+} concentration. The measured decay rates for {sup 4}F{sub 9/2}→{sup 6}H{sub 15/2} deviated from exponential to non-exponential shape with increase of Dy{sup 3+} concentration. The observed non-exponential behavior of the decay curve has been fitted to Inokuti–Hirayama model, which indicates that the energy transfer between the donor and the acceptor is of dipole–dipole nature. The energy transfer, between the donor (excited Dy{sup 3+}) and the acceptor (unexcited Dy{sup 3+}), increases with Dy{sup 3+} ions concentration. - Highlights: • Polycrystalline powders of KLa{sub (1−x)}Dy{sub x}(PO{sub 3}){sub 4} were grown by solid state reaction. • The obtained samples are characterized by XRD, FTIR and Raman spectroscopies. • The luminescent properties of Dy{sup 3+} in KLa(PO{sub 3}){sub 4} are investigated. • Lifetime and chromatic coordinates depend strongly on Dy{sup 3+} concentration. • White and blue emissions are obtained at high and low concentration, respectively.

Inhibition effect of tetradecylpyridinium bromide on the corrosion of cold rolled steel in 7.0 M H3PO4

Directory of Open Access Journals (Sweden)

Xianghong Li

2017-05-01

Full Text Available Inhibition effect of cationic surfactant of tetradecylpyridinium bromide (TDPB on the corrosion of cold rolled steel (CRS in phosphoric acid produced by dihydrate wet method process (7.0 M H3PO4 was investigated by weight loss and potentiodynamic polarization methods and electrochemical impedance spectroscopy (EIS and scanning electron microscopy (SEM. Quantum chemical calculation was applied to elucidate the adsorption mode of the inhibitor molecule on steel surface. The results show that TDPB acts as a good inhibitor, and its maximum inhibition efficiency is higher than 90% even at low concentration. The adsorption of TDPB obeys the Langmuir adsorption isotherm equation. Polarization curves indicate that TDPB behaves as a mixed-type inhibitor in H3PO4. EIS spectra exhibit one capacitive loop which indicates that the corrosion reaction is controlled by charge transfer process. The inhibition action of TDPB could also be evidenced by surface SEM images. Density functional theory (DFT calculations suggest that the pyridine ring is the active adsorption center. Depending on the results, the inhibitive mechanism is proposed from the viewpoint of adsorption theory.

Preparation of powders Ag3PO4 and study of their photocatalytic activity

International Nuclear Information System (INIS)

Badurova, K.

2014-01-01

In our thesis we dealt with preparing powders of Ag 3 PO 4 by using Na 2 HPO 4 ·12H 2 O and Na 3 PO 4 ·12H 2 O as two different precursors. Samples were prepared by precipitation and mechanochemical methods. Photocatalytic efficiency of individual samples was studied by irradiation of suspensions of prepared powders with methylene blue (MB) solution and with phenol solution using source of light similar to solar light. Photocatalytic efficiency was determined via method of determination of total organic carbon (TOC) as the time dependence of phenol concentration and also via monitoring spectrophotometric parameters of solution as the time dependence of MB solution colouring intensity. Effect of sample preparation method on photocatalytic efficiency and morphology of particles was studied. After that, samples were characterised by X-ray powder diffraction method (XRD), scanning electron microscopy (SEM) and Raman spectroscopy (authors)

Surfactant mediated hydrothermal synthesis, characterization and luminescent properties of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} core shell nanorods

Energy Technology Data Exchange (ETDEWEB)

Khajuria, Heena; Ladol, Jigmet; Khajuria, Sonika; Shah, Mohd Syed; Sheikh, H.N., E-mail: hnsheikh@rediffmail.com

2016-08-15

Highlights: • Core shell nanorods were synthesised by surfactant assisted hydrothermal method. • Morphology of core shell nanorods resembles those of core nanorods indicating coating of shell on cores. • More uniform and non-aggregated core shell nanorods were prepared in presence of surfactants. • Surfactant assisted prepared core shell nanorods show intense emission as compared to uncoated core nanorods. - Abstract: Core shell GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} nanorods were synthesized via hydrothermal route in the presence of different surfactants [cetyltrimethyl ammonium bromide (CTAB) and Sodium dodecyl sulphate (SDS)]. The nanorods were characterized by powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and photoluminescence (PL) studies. The X-ray diffraction results indicate good crystallinity and effective doping in core and core shell nanorods. SEM and TEM micrographs show that all of the as prepared gadolinium phosphate products have rod like shape. The compositional analysis of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} core was done by EDS. The emission intensity of the GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} @ GdPO{sub 4} core shell increased significantly with respect to those of GdPO{sub 4}: Ce{sup 3+}/Tb{sup 3+} core nanorods. The effect of surfactant on the uniformity, thickness and luminescence of the core shell nanorods was investigated.

Synthesis and electrochemical properties of KPb_4_−_xCa_x(PO_4)_3 (0 ≤ x ≤ 1.5) for oxidation of cadmium at graphite electrode

International Nuclear Information System (INIS)

Lahrich, Sara; Manoun, Bouchaib; El Mhammedi, Moulay Abderrahim

2017-01-01

Chemically modified carbon paste electrode (CPE) for cadmium (II) analysis has been constructed by mixing KPb_4_−_xCa_x(PO_4)_3 (0 ≤ x ≤ 1.5) (CaLA) and graphite powder. The lacunar apatite was synthesized using solid reaction and characterized by X-ray diffraction (XRD), infrared spectroscopy (IR) and Raman spectroscopy. The refinement study was carried out using Rietveld method where the obtained results show a good agreement between the observed and calculated patterns. The detection of cadmium (II) was investigated in acetate buffer (pH 4.5) using differential pulse anodic stripping voltammetry (DPASV). The limit of detection obtained under the optimized experimental conditions was 5.35 × 10"−"7 mol L"−"1 with a relative standard deviation of 2.37%. Possible interferences were tested and evaluated in 5.0 × 10"−"5 mol L"−"1 cadmium (II) in the presence of other inorganic ions. Finally, the proposed method was successfully applied to determine cadmium (II) in seawater and mussel samples. Hence, the satisfactory results confirm the applicability of this sensor in practical analysis. - Highlights: • Synthesis and characterization of new lacunar apatites KPb_4_−_xCa_x(PO_4)_3 (0 ≤ x ≤ 1.5). • Structural refinement of these compounds using Rietveld method. • A study of Ca doping effect in lacunar apatites for detecting Cd (II). • The electrochemical oxidation of Cd (II) was performed at CaLA-CPE using DPASV. • The proposed method was evaluated to detect cadmium in seawater and mussel samples.

Preparation and characterization of high surface area activated carbon from Fox nut (Euryale ferox shell by chemical activation with H3PO4

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Arvind Kumar

Full Text Available Activated carbons were prepared from Fox nutshell by chemical activation with H3PO4 in N2 atmosphere and their characteristics were studied. The effects of activation temperature and impregnation ratio were examined. N2 adsorption isotherms characterized the surface area, total pore volume, micropore volume and pore size distribution of activated carbons. Activated carbon was produced at 700 °C with a 1.5 impregnation ratio and one hour of activation time has found 2636 m2/g and 1.53 cm3/g of highest BET surface area and total pore volume, respectively. The result of Fourier-infrared spectroscopy analysis of the prepared activated carbon confirmed that the carbon has abundant functional groups on the surface. Field emission scanning electron micrographs of the prepared activated carbon showed that a porous structure formed during activation. Keywords: Activated carbons, Fox nutshell, Chemical activation, H3PO4, Activated carbon, Surface chemistry, Porous structure

Ag3PO4/ZnO: An efficient visible-light-sensitized composite with its application in photocatalytic degradation of Rhodamine B

International Nuclear Information System (INIS)

Liu, Wei; Wang, Mingliang; Xu, Chunxiang; Chen, Shifu; Fu, Xianliang

2013-01-01

Graphical abstract: The free OH radicals generated in the VB of ZnO play the primary role in the visible-light photocatalytic degradation of RhB in Ag 3 PO 4 /ZnO system. The accumulated electrons in the CB of Ag 3 PO 4 can be transferred to O 2 adsorbed on the surface of the composite semiconductors and H 2 O 2 yields. H 2 O 2 reacts with electrons in succession to produce active ·OH to some extent. Display Omitted Highlights: ► Efficient visible-light-sensitized Ag 3 PO 4 /ZnO composites were successfully prepared. ► Effect of Ag 3 PO 4 content on the catalytic activity of Ag 3 PO 4 /ZnO is studied in detail. ► Rate constant of RhB degradation over Ag 3 PO 4 (3.0 wt.%)/ZnO is 3 times that of Ag 3 PO 4 . ► The active species in RhB degradation are examined by adding a series of scavengers. ► Visible light degradation mechanism of RhB over Ag 3 PO 4 /ZnO is systematically studied. -- Abstract: The efficient visible-light-sensitized Ag 3 PO 4 /ZnO composites with various weight percents of Ag 3 PO 4 were prepared by a facile ball milling method. The photocatalysts were characterized by XRD, DRS, SEM, EDS, XPS, and BET specific area. The ·OH radicals produced during the photocatalytic reaction was detected by the TA–PL technique. The photocatalytic property of Ag 3 PO 4 /ZnO was evaluated by photocatalytic degradation of Rhodamine B under visible light irradiation. Significantly, the results revealed that the photocatalytic activity of the composites was much higher than that of pure Ag 3 PO 4 and ZnO. The rate constant of RhB degradation over Ag 3 PO 4 (3.0 wt.%)/ZnO is 3 times that of single-phase Ag 3 PO 4 . The optimal percentage of Ag 3 PO 4 in the composite is 3.0 wt.%. It is proposed that the ·OH radicals produced in the valence band of ZnO play the leading role in the photocatalytic degradation of Rhodamine B by Ag 3 PO 4 /ZnO systems under visible light irradiation.

Photoluminescence and thermoluminescence properties of Tb3+ doped K3Gd(PO4)2 nanophosphor

International Nuclear Information System (INIS)

Gupta, Palvi; Bedyal, A.K.; Kumar, Vinay; Khajuria, Y.; Lochab, S.P.; Pitale, S.S.; Ntwaeaborwa, O.M.; Swart, H.C.

2014-01-01

Energy level diagram of Tb 3+ ion in the K 3 Gd(PO 4 ) 2 host lattice. - Highlights: • First time, a detailed TL and PL study on undoped and Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor. • Combustion method was employed to synthesize the Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor. • Mechanism of excitation and emission in undoped and Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor was given. - Abstract: Tb 3+ doped nanoparticulate K 3 Gd(PO 4 ) 2 phosphor was prepared by combustion method using urea as a fuel. The structure, optical and luminescent properties of the phosphor were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (DRS), photoluminescence spectroscopy (PL), and thermoluminescence (TL) spectroscopy. In undoped K 3 Gd(PO 4 ) 2 , the excitation and emission peaks at 273 nm and 323 nm belongs to the 8 S 7/2 → 6 I J(J=7/2) and 6 P J(J=7/2) → 8 S 7/2 transitions of Gd 3+ while green emission was observed in the Tb 3+ doped K 3 Gd(PO 4 ) 2 . TL study was carried out after exposing the samples to γ-radiations (0.1–5 kGy) in the K 3 Gd(PO 4 ) 2 :Tb 3+ (1.5 mol%). The calculated kinetic parameters were compared with different methods. The band gap of the phosphor was estimated as 5.80 eV. The green shade of the Tb 3+ ion with the CIE coordinates (x, y) as (0.29, 0.54) was in good agreement with the well known green phosphors

Proton-conducting solid acid electrolytes based upon MH(PO3H)

NARCIS (Netherlands)

Zhou, W.

2011-01-01

Solid acids, such as CsHSO4 and CsH2PO4, are a novel class of anhydrous proton-conducting compounds that can be used as electrolyte in H2/O2 and direct methanol fuel cells. The disordering of the hydrogen-bonded network above the so-called superprotonic phase transition results in an increase of the

Thermodynamics, dielectric permittivity and phase diagrams of the Rb1-x(NH4xH2PO4 type proton glasses

Directory of Open Access Journals (Sweden)

S.I. Sorokov

2010-01-01

Full Text Available The cluster pseudospin model of proton glasses, which takes into account the energy levels of protons around the PO4 group, the long-range interactions between the hydrogen bonds, and an internal random deformational field is used to investigate thermodynamical characteristics, longitudinal and transverse dielectric permittivities of Rb1-x(ND4xD2PO4 and Rb1-x(NH4xH2AsO4 compounds. A review of experimental and theoretical works on the Rb1-x(NH4xH2PO4 type crystals is presented.

First-principles study of paraelectric and ferroelectric CsH2PO4 including dispersion forces: Stability and related vibrational, dielectric, and elastic properties

Science.gov (United States)

Van Troeye, Benoit; van Setten, Michiel Jan; Giantomassi, Matteo; Torrent, Marc; Rignanese, Gian-Marco; Gonze, Xavier

2017-01-01

Using density functional theory (DFT) and density functional perturbation theory (DFPT), we investigate the stability and response functions of CsH2PO4 , a ferroelectric material at low temperature. This material cannot be described properly by the usual (semi)local approximations within DFT. The long-range e--e- correlation needs to be properly taken into account, using, for instance, Grimme's DFT-D methods, as investigated in this work. We find that DFT-D3(BJ) performs the best for the members of the dihydrogenated alkali phosphate family (KH2PO4 , RbH2PO4 , CsH2PO4 ), leading to experimental lattice parameters reproduced with an average deviation of 0.5%. With these DFT-D methods, the structural, dielectric, vibrational, and mechanical properties of CsH2PO4 are globally in excellent agreement with the available experiments (<2 % MAPE for Raman-active phonons). Our study suggests the possible existence of a new low-temperature phase of CsH2PO4 , not yet reported experimentally. Finally, we report the implementation of DFT-D contributions to elastic constants within DFPT.

Blue photoluminescence and long lasting phosphorescence properties of a novel chloride phosphate phosphor: Sr5(PO4)3Cl:Eu2+

International Nuclear Information System (INIS)

Wu, Chuanqiang; Zhang, Jiachi; Feng, Pengfei; Duan, Yiming; Zhang, Zhiya; Wang, Yuhua

2014-01-01

A novel blue emitting long lasting phosphorescence phosphor Sr 5 (PO 4 ) 3 Cl:Eu 2+ is synthesized by solid state method at 1223 K in reducing atmosphere. The afterglow emission spectrum shows one broad band centered at 441 nm due to the 5d–4f transition of Eu 2+ at six coordinated Sr(II) sites and the color coordinates are calculated to be (0.149, 0.095) which is close to the light blue region. The excitation band is in 240–430 nm and partly overlaps the solar irradiation on Earth's surface. The long lasting phosphorescence of the optimal sample doping by 0.1 mol%Eu 2+ can be recorded for about 1040 s (0.32 mcd/m 2 ). Thermoluminescence shows that there are at least three types of traps corresponding to peaks at 340 K, 382 K, 500 K, respectively. The filling and fading experiments reveal that the traps in Sr 5 (PO 4 ) 3 Cl:Eu 2+ are independent. The shallow traps (340 K) essentially contribute to the visible long lasting phosphorescence, while the deep traps (382 K and 500 K) are proved to be very stable. Thus, the Sr 5 (PO 4 ) 3 Cl:Eu 2+ material shows potential applications as not only a long lasting phosphorescence phosphor, but also an optical storage material. -- Highlights: • The blue long lasting phosphorescence of Sr 5 (PO 4 ) 3 Cl:Eu 2+ is first reported. • Filling and fading experiments are carried out for revealing natures of traps. • The afterglow mechanism for independent traps of Sr 5 (PO 4 ) 3 Cl:Eu 2+ is proposed

1H and 2H NMR relaxation study on the phase transitions of (NH4)3H(SO4)2 and (ND4)3D(SO4)2 single crystals

International Nuclear Information System (INIS)

Lim, Ae Ran; Jeong, Se-Young

2006-01-01

T 1 , T 1ρ and T 2 for the 1 H and 2 H nuclei in (NH 4 ) 3 H(SO 4 ) 2 and (ND 4 ) 3 D(SO 4 ) 2 single crystals grown using the slow evaporation method were measured for phases I, II, III, IV and V. The 1 H T 1 , T 1ρ , and T 2 values were found to exhibit different trends in phases II and III: T 1 , T 1ρ and T 2 for 1 H do not change significantly near the phase transition at 265 K, whereas near 413 K they change discontinuously. We conclude that the NH 4 + and H(SO 4 ) 2 - ions do not play an important role in the III-II phase transition, but do play important roles in the II-I phase transition. The liquid-like nature of the 1 H T 1ρ and T 2 above 413 K is indicative of the destruction and reconstruction of hydrogen bonds. Moreover, the phase transitions of the (NH 4 ) 3 H(SO 4 ) 2 crystal are accompanied by changes in the molecular motion of the (NH 4 ) + ions. The variations with temperature of the 2 H T 1 and T 2 of (ND 4 ) 3 D(SO 4 ) 2 crystals are not similar to those observed for the 1 H T 1 and T 2 . Our comparison of the results for (NH 4 ) 3 H(SO 4 ) 2 and (ND 4 ) 3 D(SO 4 ) 2 crystals indicates the following: the 1 H T 1ρ and T 2 of the (NH 4 ) + and H(SO 4 ) 2 - ions above T C1 are characteristic of fast, liquid-like motion, which is not the case for (ND 4 ) 3 D(SO 4 ) 2 ; and the 2 H T 1 of D(SO 4 ) 2 - in (ND 4 ) 3 D(SO 4 ) 2 is longer than the 2 H T 1 of (ND 4 ) + in contrast to the results for (NH 4 ) 3 H(SO 4 ) 2 crystals

Synthesis and some properties of hydrogen phosphites M3(H2PO3)3, where M = Ga, V, Fe, or In

International Nuclear Information System (INIS)

Zakharova, B.S.; Tarnopol'skij, V.A.; Chudinova, N.N.

2001-01-01

The conditions on production and the properties of the acid phosphites M 3 (H 2 PO 3 ) 3 (M = Ga, V, Fe, In) are demonstrated. The compounds were investigated by X-ray diffraction, thermal gravimetric analysis, IR spectroscopy and conductometry. Interaction of M 2 O 3 (M = Ga, V, Fe, In) with the melt of phosphorous acid was studied in the P : M = 1. 5 : 1 - 10 : 1 interval of compositions. The lattice parameters are given, the hypothesis on the available of superstructure in the M 3 (H 2 PO 3 ) 3 compounds is corroborated. From the measurements the proton conductivity in vanadium and indium phosphites is comprised of 2.5 x 10 -5 and 1.9 x 10 8- S/cm correspondingly. Acid vanadium and indium phosphites are behaved similarly during heating. The limit of thermal stability of the acid phosphites V(H 2 PO 3 ) 3 , V(H 2 PO 3 ) 3 grows [ru

Enhanced electrochemical performance of LiMnPO4 by Li+-conductive Li3VO4 surface coatings

International Nuclear Information System (INIS)

Dong, Youzhong; Zhao, Yanming; Duan, He; Liang, Zhiyong

2014-01-01

By a simple wet ball-milling method, Li 3 VO 4 -coated LiMnPO 4 samples were prepared successfully for the first time. The thin Li 3 VO 4 coating layer with a three-dimensional Li + -ion transport path and high mobility of Li + -ion strongly adhered to the LiMnPO 4 material reduces Mn dissolution and increases the Li + flux through the surface of the LiMnPO 4 itself by preventing formation of phases on the surface that would normally block Li + as well as Li + -ion permeation into the surface of the LiMnPO 4 electrode and therefore improve the rate capability as well as the cycling stability of LiMnPO 4 materials. The electrochemical testing shows that the 5% Li 3 VO 4 -coated LiMnPO 4 sample shows a clear voltage plateau in the charge curves and a much higher reversible capacity at different discharge rates compared with the pristine LiMnPO 4 . EIS results also show that the surface charge transfer resistance and Warburg impedance of the Li 3 VO 4 -coated LiMnPO 4 samples significantly decreased. The surface charge transfer resistance and Warburg impedance for the pristine LiMnPO 4 are 955.1 Ω and 400.3 Ω, respectively. While, for the 5% Li 3 VO 4 -coated LiMnPO 4 , the value are only 400.2 Ω and 283.6 Ω, respectively. The surface charge transfer resistance decreases more than half. All of the improved performance will be favorable for application of the LiMnPO 4 in high-power lithium ion batteries

Preventing structural degradation from Na3V2(PO4)3 to V2(PO4)3: F-doped Na3V2(PO4)3/C cathode composite with stable lifetime for sodium ion batteries

Science.gov (United States)

Chen, Yanjun; Xu, Youlong; Sun, Xiaofei; Zhang, Baofeng; He, Shengnan; Li, Long; Wang, Chao

2018-02-01

A prospective NASICON-type F-doped Na3V2(PO4)2.93F0.07/C (F-0.07-NVP/C) composite is synthesized by a solid-state reaction method. F-doping can restrain the structural degradation from Na3V2(PO4)3 to V2(PO4)3 and enhance the structural stability. Meanwhile, it can decrease the particle size to diminish the pathway of Na+ diffusion, which can increase ionic conductivity efficiently. The kinetic behavior is significantly improved and it is beneficial to reinforcing the electrochemical performance of F-doping composites. Compared with Undoped-NVP/C sample, F-0.07-NVP/C composite delivers a 113 mAh g-1 discharge capacity at 10 mA g-1, which is very close to the theoretical capacity (117 mAh g-1). As for cycle performance, a reversible capacity of 97.8 mAh g-1 can be obtained and it retains 86% capacity after 1000 cycles at 200 mA g-1. F-0.07-NVP/C composite presents the highest DNa+ (2.62 × 10-15 cm2s-1), two orders of magnitude higher than the undoped sample (4.8 × 10-17 cm2s-1). This outstanding electrochemical performance is ascribed to the synergetic effect from improved kinetic behavior and enhanced structural stability due to F-doping. Hence, the F-doped composite would be a promising cathode material in SIB for energy storage and conversion.

Hydrothermal synthesis, thermal, structural, spectroscopic and magnetic studies of the Mn5-x Co x (HPO4)2(PO4)2(H2O)4 (x=1.25, 2, 2.5 and 3) finite solid solution

International Nuclear Information System (INIS)

Larrea, Edurne S.; Mesa, Jose L.; Pizarro, Jose L.; Arriortua, Maria I.; Rojo, Teofilo

2007-01-01

The Mn 5- x Co x (HPO 4 ) 2 (PO 4 ) 2 (H 2 O) 4 (x=1.25, 2, 2.5, 3) finite solid solution has been synthesized by mild hydrothermal conditions under autogeneous pressure. The phases crystallize in the C2/c space group with Z=4, belonging to the monoclinic system. The unit-cell parameters obtained from single crystal X-ray diffraction are: a=17.525(1), b=9.0535(6), c=9.4517(7) A, β=96.633(5) o being R1=0.0436, wR2=0.0454 for Mn75Co25; a=17.444(2), b=9.0093(9), c=9.400(1) A, β=96.76(1) o being R1=0.0381, wR2=0.0490 for Mn60Co40; a=17.433(2), b=8.9989(9), c=9.405(1) A, β=96.662(9) o being R1=0.0438, wR2=0.0515 for Mn50Co50 and a=17.4257(9), b=8.9869(5), c=9.3935(5) A, β=96.685(4) o being R1=0.0296, wR2=0.0460 for Mn40Co60. The structure consists of a three dimensional network formed by octahedral pentameric entities (Mn,Co) 5 O 16 (H 2 O) 6 sharing vertices with the (PO 4 ) 3- and (HPO 4 ) 2- tetrahedra. The limit of thermal stability of these compounds is, approximately, 165 deg. C, near to this mean temperature the phases loose their water content in two successive steps. IR spectra show the characteristic bands of the water molecules and the phosphate and hydrogen-phosphate oxoanions. The diffuse reflectance spectra are consistent with the presence of MO 6 octahedra environments in slightly distorted octahedral geometry, except for the M(3)O 6 octahedron which presents a remarkable distortion and so a higher Dq parameter. The mean value for the Dq and B-Racah parameter for the M(1),(2)O 6 octahedra is 685 and 850 cm -1 , respectively. These parameters for the most distorted M(3)O 6 polyhedron are 825 and 880 cm -1 , respectively. The four phases exhibit antiferromagnetic couplings as the major magnetic interactions. However, a small spin canting phenomenon is observed at low temperatures for the two phases with major content in the anisotropic-Co(II) cation. - Graphical abstract: Crystal structure of the finite solid solution Mn 5-x Co x (HPO 4 ) 2 (PO 4 ) 2 (H

Synergistic inhibition effect of 5-aminotetrazole and 4,6-dihydroxypyrimidine on the corrosion of cold rolled steel in H{sub 3}PO{sub 4} solution

Energy Technology Data Exchange (ETDEWEB)

Li, Xianghong, E-mail: xianghong-li@163.com [Yunnan Key Laboratory of Wood Adhesives and Glue Products, Southwest Forestry University, Kunming 650224 (China); Faculty of Science, Southwest Forestry University, Kunming 650224 (China); Deng, Shuduan [Yunnan Key Laboratory of Wood Adhesives and Glue Products, Southwest Forestry University, Kunming 650224 (China); Xie, Xiaoguang [School of Chemical Science and Technology, Yunnan University, Kunming 650091 (China); Du, Guanben [Yunnan Key Laboratory of Wood Adhesives and Glue Products, Southwest Forestry University, Kunming 650224 (China)

2016-09-15

The synergistic inhibition effect of 5-aminotetrazole (AT) and 4,6-dihydroxypyrimidine (DHP) on the corrosion of cold rolled steel (CRS) in H{sub 3}PO{sub 4} solution was studied by weight loss, potentiodynamic polarization curves, electrochemical impedance spectroscopy (EIS), scanning electron microscope (SEM), quantum chemical calculation and molecular dynamics (MD) methods. The results show that AT exhibits a moderate inhibitive effect, and DHP has a poor effect. However, incorporation AT with DHP significantly improves the inhibitive performance, and yields synergism. The adsorption of AT in the absence and presence of DHP obeys Langmuir adsorption isotherm. AT/DHP mixture acts as a mixed-type inhibitor. The combined AT and DHP molecules co-adsorb on the Fe (001) surface in the nearly flat manner, and the adsorption energy is larger than individual AT or DHP. - Highlights: • There is a synergistic inhibition effect of AT and DHP for steel in H{sub 3}PO{sub 4} solution. • The adsorption of AT whether it is mixed with DHP or not obeys Langmuir isotherm. • The AT/DHP mixture behaves as a mixed-type inhibitor. • E{sub HOMO} increases and E{sub LUMO} decreases in the combined AT and DHP. • AT and DHP co-adsorb on Fe (001) surface with the nearly flat manner.

Synthesis and electrochemical properties of Ti4+ doped Li3-xFe2-xTix(PO4)3/C cathode materials

International Nuclear Information System (INIS)

Liu Zhanqiang; Huang Fuqiang; Sun Junkang

2011-01-01

Highlights: → Li 3-x Fe 2-x Ti x (PO 4 ) 3 /C composite cathodes were prepared by ball-milling method. Ti-doping can improve the electrochemical property of Li 3 Fe 2 (PO 4 ) 3 . → The optimized doping level was found to be x = 0.2. → The second phase of LiTi 2 (PO 4 ) 3 will emerge if the doping level higher than 0.2. - Abstract: Li 3-x Fe 2-x Ti x (PO 4 ) 3 /C (x = 0-0.4) cathodes designed with Fe doped by Ti was studied. Both Li 3 Fe 2 (PO 4 ) 3 /C (x = 0) and Li 2.8 Fe 1.8 Ti 0.2 (PO 4 ) 3 /C (x = 0.2) possess two plateau potentials of Fe 3+ /Fe 2+ couple (around 2.8 V and 2.7 V vs. Li + /Li) upon discharge observed from galvanostatic charge/discharge and cyclic voltammetry. Li 2.8 Fe 1.8 Ti 0.2 (PO 4 ) 3 /C has higher reversibility and better capacity retention than that of the undoped Li 3 Fe 2 (PO 4 ) 3 /C. A much higher specific capacity of 122.3 mAh/g was obtained at C/20 in the first cycle, approaching the theoretical capacity of 128 mAh/g, and a capacity of 100.1 mAh/g was held at C/2 after the 20th cycle.

Activated Carbon from the Chinese Herbal Medicine Waste by H3PO4 Activation

Directory of Open Access Journals (Sweden)

Tie Mi

2015-01-01

Full Text Available Large amounts of Chinese herbal medicine wastes produced by the medicinal factories have been mainly landfilled as waste. In this study, via phosphoric acid activation, a Chinese herbal medicine waste from Magnolia officinalis (CHMW-MO was prepared for activated carbon (CHMW-MO-AC. The effect of preparation conditions (phosphoric acid/CHMW-MO impregnation ratio, activation temperature, and time of activated carbon on yield of CHMW-MO-AC was investigated. The surface area and porous texture of the CHMW-MO-ACs were characterized by nitrogen adsorption at 77 K. The SBET and pore volume were achieved in their highest value of 920 m2/g and 0.703 cm3/g, respectively. Thermal gravity analysis and scanning electron microscope images showed that CHMW-MO-ACs have a high thermal resistance and pore development. The results indicated that CHMW-MO is a good precursor material for preparing activated carbon, and CHMW-MO-AC with well-developed mesopore volume can be prepared by H3PO4 activation.

Evaluation and characterization of β -tricalcium phosphate powder prepared by CaCO3/H3PO4 system

International Nuclear Information System (INIS)

Shah Rizal Kasim; Yeong Meng Yee; Hazizan Md Akil; Zainal Arifin Ahmad

2007-01-01

Many attempts have been focused in the past on preparing of synthetic β-tricalcium (β-TCP), which being employed as bone substitute due to its biocompatibility and resorbability. Low temperature synthesize such as sol-gel method become popular due to the high product purity and homogenous composition. Sol-gel method is less economical towards commercialization because the cost of raw materials and the yield of the product that can be achieved. This paper describes the synthesis of β-TCP via mixing of CaCO 3 and H 3 PO 4 followed by calcinations process at 750 degree C - 1050 degree C. X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimeter (DSC), fourier transformation infra-red (FTIR) were used for characterization and evaluation of the phase composition, morphology, particle size and thermal behavior of the product. β-TCP phase start to occur after calcinations at 750 degree C. (Author)

A research on shape-controllable synthesis of Ag3PO4/AgBr and its degradation of ciprofloxacin.

Science.gov (United States)

Chen, Jingran; Yang, Xingyu; Zhu, Chenyu; Xie, Xin; Lin, Cuiping; Zhao, Yalei; Yan, Qishe

2018-03-01

Antibiotic ciprofloxacin is one of the commonly used broad spectrum fluoroquinolone human and veterinary drugs. Because of the overuse of human beings, the presence of ciprofloxacin has been detected in a variety of environmental matrices. To solve this problem, a facile, environmentally-friendly Ag 3 PO 4 /AgBr composite photocatalyst was synthesized by a simple precipitation method at room temperature in the presence of cetyltrimethyl ammonium bromide (CTAB). CTAB was served as surfactant and the source of bromide ions. The as-prepared Ag 3 PO 4 /AgBr microspheres were characterized by means of powder X-ray diffraction (XRD), scanning electron microscope (SEM) and UV-visible diffuse reflectance spectroscopy (UV-vis DRS). The results revealed that the Ag 3 PO 4 /AgBr sample (synthesized with CTAB, 0.8 g) exhibited the highest photocatalytic activity to the photodegradation rate of 96.36%. Moreover, mechanism detection experiment indicated that h + was the major active species in the degradation process. So the enhanced photocatalytic activity of Ag 3 PO 4 /AgBr composites is attributed to its excellent separation of photogenerated electron-hole pairs through Ag 3 PO 4 /AgBr heterojunction. Also, Ag 3 PO 4 /AgBr heterojunction has a lower band gap compared to pure Ag 3 PO 4 and pure AgBr, so higher efficiency of light harvesting is equipped.

Luminescence properties and energy transfer investigations of Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ phosphors

International Nuclear Information System (INIS)

Yang, Zaifa; Xu, Denghui; Sun, Jiayue; Du, Jiangnan; Gao, Xuedong

2016-01-01

Highlights: • A phosphor Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ for UV-based white LEDs was firstly synthesized successfully. • The phase structure and photoluminescence properties of samples were studied in detail. • The energy transfer process from Ce"3"+ to Tb"3"+ ions was illustrated in detail. • Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ phosphor has potential applications as an UV-convertible phosphor for white light emitting diodes. - Abstract: A series of Ce"3"+ or Tb"3"+ doped and Ce"3"+/Tb"3"+ co-doped Sr_3Lu(PO_4)_3 phosphors were prepared via the conventional high temperature solid-state reaction. The phase structure, photoluminescence and energy transfer properties of samples were studied in detail. The optimal proportion of Ce"3"+ single doping is 4 mol% with maximal fluorescence intensity. The Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ phosphor shows both a blue emission (428 nm) from Ce"3"+ and a yellowish-green emission (545 nm) from Tb"3"+ with considerable intensity under ultraviolet (UV) excitation (268 nm). The energy transfer from Ce"3"+ to Tb"3"+ ions takes place in the Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ phosphor on the basis of the analysis of the luminescence spectra. The energy transfer mechanism from Ce"3"+ to Tb"3"+ ions was proved to be dipole–dipole interaction. The energy transfer behaviors in Sr_3Lu(PO_4)_3:Ce"3"+, Tb"3"+ phosphor is also investigated by the lifetime measurement. The results show that this phosphor has potential applications for UV white-light LEDs.

Luminescence properties of phosphate phosphor Ba{sub 3}Y(PO{sub 4}){sub 3}:Sm{sup 3+}

Energy Technology Data Exchange (ETDEWEB)

Yang, Fu [College of Science, Hebei North University, Zhangjiakou 075000 (China); Liu, Yufeng, E-mail: liuyufeng4@126.com [State Key Lab of Power Systems, Department of Thermal Engineering, Tsinghua University, Beijing 100084 (China); Tian, Xiaodong; Dong, Guoyi [College of Physics Science and Technology, Hebei University, Baoding 071002 (China); Yu, Quanmao [Institute of Functional Materials, Jiangxi University of Finance & Economics, Nanchang 330013 (China)

2015-05-15

A series of reddish orange-emitting phosphate phosphors Ba{sub 3}Y{sub 1−x}(PO{sub 4}){sub 3}:xSm{sup 3+}(0.01≤x≤0.20) were synthesized by solid-state reaction. X-ray diffraction and photoluminescence spectra were utilized to characterize the structure and luminescence properties of as-synthesized phosphors. The optimized phosphors Ba{sub 3}Y{sub 0.95}(PO{sub 4}){sub 3}:0.05Sm{sup 3+} present several excitation bands from 300 to 500 nm, and exhibit intense reddish orange-emitting properties. The energy transfer type between Sm{sup 3+} ions was confirmed as d–d interaction by using Van Uitert model. The chromatic properties of the typical sample Ba{sub 3}Y(PO{sub 4}){sub 3}:0.05Sm{sup 3+} phosphor have been found to have chromaticity coordinates of (0.583, 0.405), which are located in reddish orange region under the excitation of 401 nm. These results indicated that Ba{sub 3}Y(PO{sub 4}){sub 3}:Sm{sup 3+} phosphors have potential applications in the field of lighting and display due to their effective excitation in the near-ultraviolet range. - Graphical abstract: The color coordinates for 5 mol% Sm{sup 3+} doped Ba{sub 3}Y(PO{sub 4}){sub 3} phosphor were calculated to be (0.583, 0.405), which are located in reddish orange region under the excitation of 401 nm. The peaks of Ba{sub 3}Y{sub 0.95}(PO{sub 4}){sub 3}:0.05Sm{sup 3+} phosphor with the highest emission intensity at 600 nm are broader than those of Y{sub 2}O{sub 3}:Eu{sup 3+} and Y{sub 2}O{sub 2}S:Eu{sup 3+} phosphors. All these characteristics suggest that Ba{sub 3}Y(PO{sub 4}){sub 3}:Sm{sup 3+} phosphors are suitable for near-UV (370–410 nm) excitation and can be applicable to near UV-based WLEDs. ▪ - Highlights: • Different concentration Sm{sup 3+}-doped Ba{sub 3}Y(PO{sub 4}){sub 3} phosphors were fabricated by solid state method. • The optimized phosphors present the several excitation bands from 300 to 500 nm. • The Ba{sub 3}Y(PO{sub 4}){sub 3}:Sm{sup 3+} shows bright reddish orange

Thermal expansion of phosphates with the NaZr2(PO4)3 structure containing lanthanides and zirconium: R0.33Zr2(PO4)3 (R = Nd, Eu, Er) and Er0.33(1–x) Zr0.25xZr2(PO4)3

International Nuclear Information System (INIS)

Volgutov, V. Yu.; Orlova, A. I.

2015-01-01

Phosphates R 0.33 Zr 2 (PO 4 ) 3 (R = Nd, Eu, or Er) and Er 0.33(1–x) Zr 0.25 Zr 2 (PO 4 ) 3 (x = 0, 0.25, 0.5, 0.75, 1.0) of the NaZr 2 (PO 4 ) 3 family have been synthesized and investigated by high-temperature X-ray diffraction. The crystallochemical approach is used to obtain compounds with expected small and controllable thermal-expansion parameters. Phosphates with close-to-zero thermal-expansion parameters, including those with low thermal-expansion anisotropy, have been obtained: Nd 0.33 Zr 2 (PO 4 ) 3 with α a =–2.21 × 10 −6 °C −1 , α c = 0.81 × 10 −6 °C −1 , and Δα = 3.02 × 10 −6 °C –1 and Er 0.08 Zr 0.19 Zr 2 (PO 4 ) 3 with α a =–1.86 × 10 −6 °C −1 , α c = 1.73 × 10 −6 °C −1 , and Δα = 3.58 × 10 −6 °C −1

Study of the influence of the amount of PBI-H{sub 3}PO{sub 4} in the catalytic layer of a high temperature PEMFC

Energy Technology Data Exchange (ETDEWEB)

Lobato, Justo; Canizares, Pablo; Rodrigo, Manuel A.; Linares, Jose J.; Pinar, F. Javier [Chemical Engineering Department, Enrique Costa Building, University of Castilla-La Mancha, Av. Camilo Jose Cela, n 12, 13071, Ciudad Real (Spain)

2010-02-15

The influence of the amount of polybenzimidazole (PBI)-H{sub 3}PO{sub 4} (normalized with respect to the PBI loading, which expressed as C/PBI weight ratio) content in both the anode and cathode has been studied for a PBI-based high temperature proton exchange membrane (PEM) fuel cell. The electrodes prepared with different amounts of PBI have been characterized physically, by measuring the pore size distribution, and visualizing the surface microstructure. Afterwards, the electrochemical behaviour of the electrodes has been evaluated. The catalytic electrochemical activity has been measured by voltamperometry for each electrode prepared with a different PBI content, and the cell performance results have been studied, supported by the impedance spectra, in order to determine the influence of the PBI loading in each electrode. The best results have been achieved with a C/PBI weight ratio of 20, for both the anode and the cathode. A lower C/PBI weight ratio (larger amount of PBI in the catalytic layer) reduced the electrocatalytic activity, and impaired the mass transport processes, due to the large amount of polymer covering the catalyst particle, lowering the cell performance. A higher C/PBI weight ratio (lower amount of PBI in the catalytic layer) reduced the electrocatalytic activity, and slightly increased the ohmic resistance. The low amount of the polymeric ionic carrier PBI-H{sub 3}PO{sub 4} limited the proton mobility, despite of the presence of large amounts of ''free'' H{sub 3}PO{sub 4} in the catalytic layer. (author)

Synthesis, structure, and photoluminescence properties of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors for white-light-emitting diodes.

Science.gov (United States)

Jiao, Mengmeng; Lü, Wei; Shao, Baiqi; Zhao, Lingfei; You, Hongpeng

2015-08-24

A series of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors are prepared using a solid-state reaction. X-ray diffraction analysis and Rietveld structure refinement are used to check the phase purity and crystal structure of the prepared samples. Ce(3+) - and Eu(2+) -doped phosphors both have broad excitation and emission bands, owing to the spin- and orbital-allowed electron transition between the 4f and 5d energy levels. By co-doping the KBaSc2 (PO4 )3 :Eu(2+) and KBaSc2 (PO4 )3 :Ce(3+) phosphors with Tb(3+) ions, tunable colors from blue to green can be obtained. The critical distance between the Eu(2+) and Tb(3+) ions is calculated by a concentration quenching method and the energy-transfer mechanism for Eu(2+) →Tb(3+) is studied by utilizing the Inokuti-Hirayama model. In addition, the quantum efficiencies of the prepared samples are measured. The results indicate that KBaSc2 (PO4 )3 :Eu(2+) ,Tb(3+) and KBaSc2 (PO4 )3 :Ce(3+) ,Tb(3+) phosphors might have potential applications in UV-excited white-light-emitting diodes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Photoluminescence Properties of Red-Emitting Ca3Sr3-x(PO4)4:xEu3+ Phosphors for White Light-Emitting Diodes.

Science.gov (United States)

Hakeem, D A; Park, K

2015-07-01

The photoluminescent properties of the Eu(3+)-activated Ca3Sr3(PO4)4 phosphors prepared by a solution combustion method were investigated. The excitation spectra of Ca3Sr3-x(PO4)4:xEu3+ (0.05 ≤ x ≤ 0.6) phosphors under 614 nm wavelength showed a broad band centered at 266 nm along with other peaks at 320, 362, 381, 394, 414, 464, and 534 nm. The emission spectra observed in the range of 450 to 750 nm under excitation at 394 nm were ascribed to the 5D0-7F1-4 transitions of Eu3+ ions. The Ca3Sr3-x(PO4)4:xEu3+ phosphors showed the strongest red emission at 614 nm due to the electric dipole 5DO -->7F2 transition of Eu3+. The strongest emission intensity was obtained for the Eu3+ ions of x = 0.5. The prepared Ca3Sr3-x(PO4)4:xEu3+ can be used as an efficient red phosphor for UV-based white LEDs.

Origin of Activity and Stability Enhancement for Ag3PO4 Photocatalyst after Calcination

Directory of Open Access Journals (Sweden)

Pengyu Dong

2016-11-01

Full Text Available Pristine Ag3PO4 microspheres were synthesized by a co-precipitation method, followed by being calcined at different temperatures to obtain a series of calcined Ag3PO4 photocatalysts. This work aims to investigate the origin of activity and stability enhancement for Ag3PO4 photocatalyst after calcination based on the systematical analyses of the structures, morphologies, chemical states of elements, oxygen defects, optical absorption properties, separation and transfer of photogenerated electron-hole pairs, and active species. The results indicate that oxygen vacancies (VO˙˙ are created and metallic silver nanoparticles (Ag NPs are formed by the reaction of partial Ag+ in Ag3PO4 semiconductor with the thermally excited electrons from Ag3PO4 and then deposited on the surface of Ag3PO4 microspheres during the calcination process. Among the calcined Ag3PO4 samples, the Ag3PO4-200 sample exhibits the best photocatalytic activity and greatly enhanced photocatalytic stability for photodegradation of methylene blue (MB solution under visible light irradiation. Oxygen vacancies play a significantly positive role in the enhancement of photocatalytic activity, while metallic Ag has a very important effect on improving the photocatalytic stability. Overall, the present work provides some powerful evidences and a deep understanding on the origin of activity and stability enhancement for the Ag3PO4 photocatalyst after calcination.

Removal of FePO4 and Fe3(PO4)2 crystals on the surface of passive fillers in Fe0/GAC reactor using the acclimated bacteria

International Nuclear Information System (INIS)

Lai, Bo; Zhou, Yuexi; Yang, Ping; Wang, Juling; Yang, Jinghui; Li, Huiqiang

2012-01-01

Highlights: ► Fe 3 (PO 4 ) 2 and FePO 4 crystals would weaken treatment efficiency of Fe 0 /GAC reactor. ► Fe 3 (PO 4 ) 2 and FePO 4 crystals could be removed by the acclimated bacteria. ► FeS and sulfur in the passive film would be removed by the sulfur-oxidizing bacteria. ► Develop a cost-effective bio-regeneration technology for the passive fillers. - Abstract: As past studies presented, there is obvious defect that the fillers in the Fe 0 /GAC reactor begin to be passive after about 60 d continuous running, although the complicated, toxic and refractory ABS resin wastewater can be pretreated efficiently by the Fe 0 /GAC reactor. During the process, the Fe 3 (PO 4 ) 2 and FePO 4 crystals with high density in the passive film are formed by the reaction between PO 4 3− and Fe 2+ /Fe 3+ . Meanwhile, they obstruct the formation of macroscopic galvanic cells between Fe 0 and GAC, which will lower the wastewater treatment efficiency of Fe 0 /GAC reactor. In this study, in order to remove the Fe 3 (PO 4 ) 2 and FePO 4 crystals on the surface of the passive fillers, the bacteria were acclimated in the passive Fe 0 /GAC reactor. According to the results, it can be concluded that the Fe 3 (PO 4 ) 2 and FePO 4 crystals with high density in the passive film could be decomposed or removed by the joint action between the typical propionic acid type fermentation bacteria and sulfate reducing bacteria (SRB), whereas the PO 4 3− ions from the decomposition of the Fe 3 (PO 4 ) 2 and FePO 4 crystals were released into aqueous solution which would be discharged from the passive Fe 0 /GAC reactor. Furthermore, the remained FeS and sulfur (S) in the passive film also can be decomposed or removed easily by the oxidation of the sulfur-oxidizing bacteria. This study provides some theoretical references for the further study of a cost-effective bio-regeneration technology to solve the passive problems of the fillers in the zero-valent iron (ZVI) or Fe 0 /GAC reactor.

Synthesis and Electrochemical Properties of LiFePO4/C for Lithium Ion Batteries.

Science.gov (United States)

Gao, Hong; Wang, Jiazhao; Yin, Shengyu; Zheng, Hao; Wang, Shengfu; Feng, Chuanqi; Wang, Shiquan

2015-03-01

LiFePO4/C was prepared through a facile rheological phase reaction method by using Fe3(PO4)2, Li3PO4 · 8H2O, and glucose as reactants. The LiFePO4/C samples were characterized by X-ray diffraction, scanning electron microscopy, and thermogravimetric analysis. The electrochemical properties of the samples were investigated. The results show that the LiFePO4/C samples have single-phase olivine-type structure, and their particles feature a spherical shape. The carbon coating on the particles of LiFePO4 is about 1.8% of the LiFePO4/C by weight. The particle size was distributed from 0.2 to 1 µm. The initial discharge capacity of LiFePO4/C reached 154 mA h/g at 0.1 C. The retained discharge capacity of LiFePO4/C was 152.9 mA h g(-1) after 50 cycles. The LiFePO4/C also showed better cycling performance than that of the bare LiPeO4 at a higher charge/discharge rate (1 C). The LIFePO4/C prepared in this way could be a promising cathode material for lithium ion battery application.

Improved cycling and high rate performance of core-shell LiFe1/3Mn1/3Co1/3PO4/carbon nanocomposites for lithium-ion batteries: Effect of the carbon source

International Nuclear Information System (INIS)

Li, Huanhuan; Chen, Yi; Chen, Long; Jiang, Haobin; Wang, Yaping; Wang, Hongbo; Li, Guochun; Li, Yunxing; Yuan, Yuan

2014-01-01

Highlights: • We report a fast microwave heating way to prepare LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /C. • The effects of different carbon sources were discussed in detail. • LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP2000 shows a discharge capacity of 160 mA h g −1 at 0.1 C. • LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP2000 elucidates excellent cyclic stability. • LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP2000 exhibits attractive rate capability. - Abstract: Core-shell type olivine solid solutions, LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /C, are synthesized via a very simple and rapid microwave heating route with different carbon sources. The obatined LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /C materials are characterized thoroughly by various analytical techniques such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy and energy-dispersive spectroscopy instrument. The particle sizes and distribution of the carbon layer of BP2000 carbon black coated LiFe 1/3 Mn 1/3 Co 1/3 PO 4 (LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP) are more uniform than that obtained from acetylene black (LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /AB) and Super P (LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /SP). Moreover, the LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP nanocomposite shows superior electrochemical properties such as high discharge capacity of 160 mA h g −1 at 0.1 C, excellent cyclic stability (143 mA h g −1 at 0.1 C after 30 cycles) and rate capability (76 mAh g −1 at 20 C), which are better than other two samples. Cyclic voltammetric and electrical tests disclose that the Li-ion diffusion, the reversibility of lithium extraction/insertion and electrical conductivity are significantly improved in LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP composite. Electrochemical impedance spectroscopy illustrates that LiFe 1/3 Mn 1/3 Co 1/3 PO 4 /BP composite electrode possesses low contact and charge-transfer impedances, which can lead to rapid electron transport during the electrochemical lithium insertion/extraction reaction. It is believed that olivine solid

Li3-xNaxV2(PO4)3 (0≤x≤3): Possible anode materials for rechargeable lithium-ion batteries

International Nuclear Information System (INIS)

Wang, Pengfei; Shao, Lianyi; Qian, Shangshu; Yi, Ting-Feng; Yu, Haoxiang; Yan, Lei; Li, Peng; Lin, Xiaoting; Shui, Miao; Shu, Jie

2016-01-01

Highlights: • Li 3-x Na x V 2 (PO 4 ) 3 (0 ≤ x ≤ 3) series are firstly evaluated as anode materials. • Li 3-x Na x V 2 (PO 4 ) 3 anodes show lithium storage activity in 1.0–3.0 V. • The lithium storage capability of different Li 3-x Na x V 2 (PO 4 ) 3 is compared. • Structural reversibility of Li 3-x Na x V 2 (PO 4 ) 3 is studied by in-situ XRD. - Abstract: In this paper, a series of Li 3-x Na x V 2 (PO 4 ) 3 (0 ≤ x ≤ 3) are prepared by a solid state reaction and systematically evaluated as anode materials for lithium-ion batteries. Structural analysis shows that the phase structure of Li 3-x Na x V 2 (PO 4 ) 3 changes along with the evolution of Na content. Charge-discharge tests exhibit that Li 3 V 2 (PO 4 ) 3 shows the highest initial charge specific capacity as high as 88.3 mAh g −1 among all the seven samples, and the reversible capacity is kept at 68.3 mAh g −1 after 45 cycles, corresponding to 77.3% of the initial charge capacity. With increasing of Na content in Li 3-x Na x V 2 (PO 4 ) 3 , the as-obtained sample show poorer lithium storage capability than Li 3 V 2 (PO 4 ) 3 . As a result, Na 3 V 2 (PO 4 ) 3 shows the inferior cycling performance than other Li 3-x Na x V 2 (PO 4 ) 3 . It can only deliver a reversible capacity of 20.9 mAh g −1 after 45 cycles, corresponding to 45.9% of the initial charge capacity. In-situ X-ray diffraction observations demonstrate that the poor electrochemical property of Na 3 V 2 (PO 4 ) 3 anode is due to the irreversible structural evolution during charge-discharge process. Therefore, reducing the Na 3 V 2 (PO 4 ) 3 phase in as-obtained sample is a feasible route to improve the lithium storage capability of Li 3-x Na x V 2 (PO 4 ) 3 .

Nanocomposite of exfoliated bentonite/g-C3N4/Ag3PO4 for enhanced visible-light photocatalytic decomposition of Rhodamine B.

Science.gov (United States)

Ma, Jianfeng; Huang, Daiqin; Zhang, Wenyi; Zou, Jing; Kong, Yong; Zhu, Jianxi; Komarneni, Sridhar

2016-11-01

Novel visible-light-driven heterojunction photocatalyst comprising exfoliated bentonite, g-C3N4 and Ag3PO4 (EB/g-C3N4/Ag3PO4) was synthesized by a facile and green method. The composites EB/g-C3N4/Ag3PO4 were characterized by X-ray diffraction, Transmission electron microscopy, Fourier transform infrared spectroscopy, UV-Vis diffuse reflectance spectroscopy and the Brunauer, Emmett, and Teller (BET) surface area method. Under visible light irradiation, EB/g-C3N4/Ag3PO4 composites displayed much higher photocatalytic activity than that of either pure g-C3N4 or pure Ag3PO4 in the degradation of Rhodamine B (RhB). Among the hybrid photocatalysts, EB/g-C3N4/Ag3PO4 composite containing 20 wt% Ag3PO4 exhibited the highest photocatalytic activity for the decolorization of RhB. Under the visible-light irradiation, the RhB dye was completely decolorized in less than 60 min. The enhanced photocatalytic performance is attributed to the stable structure, enlarged surface area, strong adsorbability, strong light absorption ability, and high-efficiency separation rate of photoinduced electron-hole pairs. Our finding paves a way to design highly efficient and stable visible-light-induced photocatalysts for practical applications in wastewater treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Physicochemical properties of 3,4,5-trimethoxybenzoates of Mn(II, Co(II, Ni(II and Zn(II

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W. FERENC

2005-09-01

Full Text Available The complexes of Mn(II, Co(II, Ni(II, Cu(II and Zn(II with 3,4,5-trimethoxybenzoic acid anion of the formula: M(C10H11O52·nH2O, where n = 6 for Ni(II, n = 1 for Mn(II, Co(II, Cu(II, and n = 0 for Zn, have been synthesized and characterized by elemental analysis, IR spectroscopy, X–ray diffraction measurements, thermogravimetry and magnetic studies. They are crystalline compounds characterized by various symmetry. They decompose in various ways when heated in air to 1273 K. At first, they dehydrate in one step and form anhydrous salts. The final products of decomposition are oxides of the respective metals (Mn2O3, Co3O4, NiO, CuO, ZnO. The solubilities of the analysed complexes in water at 293 K are in the orders of 10-2 – 10-4 mol dm-3. The magnetic susceptibilities of the Mn(II, Co(II, Ni(II and Cu(II complexes were measured over the range of 76–303 K and the magnetic moments were calculated. The results show that the 3,4,5-trimethoxybenzoates of Mn(II, Co(II and Ni(II are high-spin complexes but that of Cu(II forms a dimer [Cu2(C10H11O54(H2O2]. The carboxylate groups bind as monodentate or bidentate chelating or bridging ligands.

Structural and electrochemical characterization of 0.7LiFePO4·0.3Li3V2(PO4)3/C cathode materials using PEG and glucose as carbon sources

International Nuclear Information System (INIS)

Ma, Pingping; Hu, Pu; Liu, Zhijian; Xia, Jianhua; Xia, Dingguo; Chen, Yu; Liu, Zhengang; Lu, Zhichao

2013-01-01

0.7LiFePO 4 ·0.3Li 3 V 2 (PO 4 ) 3 /C composites (LFVP/C) were synthesized via spray-drying technique followed by solid-state reaction approach using polyethylene glycol (PEG) and glucose as carbon sources. The samples were characterized by X-ray diffraction (XRD), X-ray absorption fine-structure spectroscopy (XAFS) and Raman spectroscopy. The results show that the bi-phase composite structure of LFVP/C contains olivine LiFePO 4 (LFP) and monoclinic Li 3 V 2 (PO 4 ) 3 (LVP). The lower intensity ratio of the I D /I G and A sp 3 /A sp 2 for PEG-200 indicates the formation of higher degree of graphitized carbon during the process, which would enhance the electronic conductivity. The composite obtained using PEG-200 as carbon source show excellent rate performance, delivering the discharge capacity of 120 mAh/g at the current density of 1.5 A/g

Evaluation of the phase composition of (NH4)2SO4 + (NH4)H2PO4 mixtures by X-ray diffractometry

International Nuclear Information System (INIS)

Ortiz, Angel L.; Cumbrera, Francisco L.; Perez, Jose; Vas, Beatriz del; Perez, Eduardo

2009-01-01

The phase composition of standard (NH 4 ) 2 SO 4 + (NH 4 )H 2 PO 4 mixtures was investigated by X-ray diffractometry (XRD) using the internal-standard, reference-intensity-ratio, and Rietveld methods. It was found that the Rietveld method yields the most accurate phase-composition measurements, with an average error of ∼2 wt.%. It was also found that the internal-standard method is only effective in determining the phase composition if the calibration curve for (NH 4 )H 2 PO 4 is used, giving an average error of ∼6.5 wt.%. On the contrary, the internal-standard method with the calibration curve of the (NH 4 ) 2 SO 4 phase and the reference-intensity-ratio method are not valid. The inappropriateness of these two methods was attributed to graininess in the (NH 4 ) 2 SO 4 phase, with the attendant deviation of its diffracted intensities from the theoretical values. Direct scanning electron microscopy observations of the morphology of the powder particles in the mixtures showed clear evidence of the large agglomerates formed because the individual powder particles are partially sintered together during milling, thus corroborating the graininess determined by the XRD analyses. Finally, the implications of the present study for the quantitative phase-composition analysis of (NH 4 ) 2 SO 4 + (NH 4 )H 2 PO 4 mixtures, which are of great technological importance for the fire prevention industry, are discussed.

Modeling Li-ion conductivity in LiLa(PO{sub 3}){sub 4} powder

Energy Technology Data Exchange (ETDEWEB)

Mounir, Ferhi, E-mail: ferhi.mounir@gmail.com [Laboratoire de Physicochimie des Materiaux Mineraux et leurs Applications, Centre National des Recherches en Sciences des Materiaux, BP No. 73, 8027 Soliman (Tunisia); Karima, Horchani-Naifer [Laboratoire de Physicochimie des Materiaux Mineraux et leurs Applications, Centre National des Recherches en Sciences des Materiaux, BP No. 73, 8027 Soliman (Tunisia); Khaled, Ben Saad [Laboratoire de Photovoltaieque, Centre des Recherches et des Technologies de l' Energie, Technopole Borj Cedria, BP No. 95, 2050 Hammam Lif (Tunisia); Mokhtar, Ferid [Laboratoire de Physicochimie des Materiaux Mineraux et leurs Applications, Centre National des Recherches en Sciences des Materiaux, BP No. 73, 8027 Soliman (Tunisia)

2012-07-01

Polycrystalline powder and single-crystal of LiLa(PO{sub 3}){sub 4} are synthesized by solid state reaction and flux technique, respectively. A morphological description of the obtained product was made based on scanning electron microscopy micrographs. The obtained powder was characterized by X-ray powder diffraction, FTIR and Raman spectroscopies. Ionic conductivity of the LiLa(PO{sub 3}){sub 4} powder was measured and evaluated over a temperature range from 553 to 913 K. Single crystals of LiLa(PO{sub 3}){sub 4} are characterized by single-crystal X-ray diffraction. The LiLa(PO{sub 3}){sub 4} structure was found to be isotypic with LiNd(PO{sub 3}){sub 4}. It crystallizes in the monoclinic system with space group C2/c and cell parameters: a=16.635(6) A, b=7.130(3) A, c=9.913(3) A, {beta}=126.37(4) Degree-Sign , V=946.72(6) A{sup 3} and Z=4. The LiLa(PO{sub 3}){sub 4} structure was described as an alternation between spiraling chains (PO{sub 3}){sub n} and (La{sup 3+}, Li{sup +}) cations along the b direction. The small Li{sup +} ions, coordinated to four oxygen atoms, were located in the large connected cavities created between the LaO{sub 8} polyhedra and the polyphosphate chains. The jumping of Li{sup +} through tunnels of the crystalline network was investigated using complex impedance spectroscopy. The close value of the activation energies calculated through the analysis of conductivity data and loss spectra indicate that the transport in the investigated system is through hopping mechanism. The correlation between ionic conductivity of LiLa(PO{sub 3}){sub 4} and its crystallographic structure was investigated and the most probably transport pathway model was determined.

On the effect of the Fe(2+)/Fe(3+) redox couple on oxidation of carbon in hot H3PO4

Science.gov (United States)

Dhar, H. P.; Christner, L. G.; Kush, A. K.

1986-01-01

Oxidation studies of graphite:glassy carbon composites have been carried out at 1 and 4.7 atm. pressures in conc. H3PO4 in the presence and absence of iron ions. The concentration of the acid was varied over 85-100 wt pct, and of the iron ions over 30-300 ppm; the temperature varied over 190-210 C. Unlike the effect of Fe, which has been observed to increase the corrosion of carbon in sulphuric acid, the corrosion in phosphoric acid was observed to be slightly decreased or not at all affected. This result arises because of the catalytic reduction of the oxidized surface groups of carbon by Fe(2+) ions. The catalytic reduction is possible because under the experimental conditions the redox potential of the Fe(2+)/Fe(3+) couple is lower than the open-circuit voltage of carbon.

Combustion synthesized nanocrystalline Li3V2(PO4)3/C cathode for lithium-ion batteries

International Nuclear Information System (INIS)

Nathiya, K.; Bhuvaneswari, D.; Gangulibabu; Kalaiselvi, N.

2012-01-01

Graphical abstract: Nanocrystalline Li 3 V 2 (PO 4 ) 3 /C compound has been synthesized using a novel corn assisted combustion (CAC) method, wherein the composite prepared at 850 °C is found to exhibit superior physical and electrochemical properties than the one synthesized at 800 °C (Fig. 1). Despite the charge disproportionation of V 4+ and a possible solid solution behavior of Li 3 V 2 (PO 4 ) 3 cathode upon insertion and de-insertion of Li + ions, the structural stability of the same is appreciable, even with the extraction of third lithium at 4.6 V (Fig. 2). An appreciable specific capacity of 174 mAh g −1 with an excellent columbic efficiency (99%) and better capacity retention upon high rate applications have been exhibited by Li 3 V 2 (PO 4 ) 3 /C cathode, thus demonstrating the feasibility of CAC method in preparing the title compound to best suit with the needs of lithium battery applications. Display Omitted Highlights: ► Novel corn assisted combustion method has been used to synthesize Li 3 V 2 (PO 4 ) 3 /C. ► Corn is a cheap and eco benign combustible fuel to facilitate CAC synthesis. ► Li 3 V 2 (PO 4 ) 3 /C exhibits an appreciable specific capacity of 174 mAh g −1 (C/10 rate). ► Currently observed columbic efficiency of 99% is better than the reported behavior. ► Suitability of Li 3 V 2 (PO 4 ) 3 /C cathode up to 10C rate is demonstrated. -- Abstract: Nanocrystalline Li 3 V 2 (PO 4 ) 3 /C composite synthesized using a novel corn assisted combustion method at 850 °C exhibits superior physical and electrochemical properties than the one synthesized at 800 °C. Despite the charge disproportionation of V 4+ and a possible solid solution behavior of Li 3 V 2 (PO 4 ) 3 cathode upon insertion and extraction of Li + ions, the structural stability of the same is appreciable, even with the extraction of third lithium at 4.6 V. An appreciable specific capacity of 174 mAh g −1 and better capacity retention upon high rate applications have been

Photoluminescence and Energy Transfer Properties with Y+SiO4 Substituting Ba+PO4 in Ba3Y(PO4)3:Ce(3+)/Tb(3+), Tb(3+)/Eu(3+) Phosphors for w-LEDs.

Science.gov (United States)

Li, Kai; Liang, Sisi; Shang, Mengmeng; Lian, Hongzhou; Lin, Jun

2016-08-01

A series of Ce(3+), Tb(3+), Eu(3+) doped Ba2Y2(PO4)2(SiO4) (BYSPO) phosphors were synthesized via the high-temperature solid-state reaction route. X-ray diffraction, high-resolution transmission electron microscopy, Fourier transform infrared, solid-state NMR, photoluminescence (PL) including temperature-dependent PL, and fluorescent decay measurements were conducted to characterize and analyze as-prepared samples. BYSPO was obtained by the substitution of Y+SiO4 for Ba+PO4 in Ba3Y(PO4)3 (BYPO). The red shift of PL emission from 375 to 401 nm occurs by comparing BYSPO:0.14Ce(3+) with BYPO:0.14Ce(3+) under 323 nm UV excitation. More importantly, the excitation edge can be extended from 350 to 400 nm, which makes it be excited by UV/n-UV chips (330-410 nm). Tunable emission color from blue to green can be observed under 365 nm UV excitation based on the energy transfer from Ce(3+) to Tb(3+) ions after codoping Tb(3+) into BYSPO:0.14Ce(3+). Moreover, energy transfer from Tb(3+) to Eu(3+) ions also can be found in BYSPO:Tb(3+),Eu(3+) phosphors, resulting in the tunable color from green to orange red upon 377 nm UV excitation. Energy transfer properties were demonstrated by overlap of excitation spectra, variations of emission spectra, and decay times. In addition, energy transfer mechanisms from Ce(3+) to Tb(3+) and Tb(3+) to Eu(3+) in BYSPO were also discussed in detail. Quantum yields and CIE chromatic coordinates were also presented. Generally, the results suggest their potential applications in UV/n-UV pumped LEDs.

X-ray and neutron single crystal diffraction on (NH4)3H(SO4)2. II. Refinement of crystal structure of phase II at room temperature

International Nuclear Information System (INIS)

Reehuis, M.; Wozniak, K.; Dominiak, P.; Smirnov, L.S.; Natkaniec, I.; Baranov, A.I.; Dolbinina, V.V.

2006-01-01

The (NH 4 ) 3 H(SO 4 ) 2 is of special interest due to the possible influence of ammonium ions on a series of phase transitions: I => II => III => IV => V => VII. Earlier, the X-ray single crystal diffraction study of phase II of (NH 4 ) 3 H(SO 4 ) 2 showed that the crystal structure of this compound has two crystallographically independent groups of ammonium ions NH 4 (1) and NH 4 (2), but orientational positions of these ammonium ions were not determined exactly. The refinement of NH 4 (1) and NH 4 (2) orientational positions in phase II is carried out with the help of the X-ray and neutron single crystal diffraction study. The analyses of differential Fourier maps of electron charge density and nuclear density point out the possibility of disordering of NH 4 (2) ammonium ions

Di-μ-chlorido-bis(chlorido{2,2′-[3-(1H-imidazol-4-ylmethyl-3-azapentane-1,5-diyl]diphthalimide}copper(II

Directory of Open Access Journals (Sweden)

Xi-Xi Wang

2009-12-01

Full Text Available The centrosymmetric dinuclear CuII complex, [Cu2Cl4(C24H21N5O42], was synthesized by the reaction of CuCl2·2H2O with the tripodal ligand 2,2′-[3-(1H-imidazol-4-ylmethyl-3-azapentane-1,5-diyl]diphthalimide (L. Each of the CuII ions is coordinated by two N atoms from the ligand, two bridging Cl atoms and one terminal Cl atom. The CuII coordination can be best be described as a transition state between four- and five-coordination, since one of the bridging Cl atoms has a much longer Cu—Cl bond distance [2.7069 (13 Å] than the other [2.2630 (12 Å]. In addition, the Cu...Cu distance is 3.622 (1 Å. The three-dimensional structrure is generated by N—H...O, C—H...O and C—H...Cl hydrogen bonds and π–π interactions [centroid–centroid distances = 3.658 (4 and 4.020 (4 Å].

Microwave synthesis of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C as positive-electrode materials for rechargeable lithium batteries

Energy Technology Data Exchange (ETDEWEB)

Xi, Yupeng; Zhang, Yanhui; Su, Zhi, E-mail: suzhixj@sina.com

2015-04-15

Highlights: • High performance LVP/C synthesized by self-assembly microwave oven. • TEM showed the carbon layer is consisted of two kinds of concrete components. • The fast and efficient method make the process feasible commercially. - Abstract: The paper reports a microwave irradiation method to rapidly synthesize Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C materials as cathode for lithium ion batteries by the self-assembly microwave reaction oven with carbon seal reactor, using LiH{sub 2}PO{sub 4}, V{sub 2}O{sub 5} and sucrose as raw materials. Sucrose was used to be reducer and carbon source. Thermogravimetric (TG) analysis, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were used to characterize its structure and morphology. Electrochemical properties of the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C materials were studied by cyclic voltammetry (CV) and charge–discharge cycling performance. The results showed that the diffraction peaks of the sample correspond to a single-phase, and can be indexed as monoclinic structure with a space group of P2{sub 1}/n. An electrochemical test showed that Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C demonstrated an excellent electrochemical capacity of 138 mA h g{sup −1} at 0.2 C rate and 124.1 mA h g{sup −1} at 5 C rate with stable cycle ability.

Hydroxyapatite supported Ag3PO4 nanoparticles with higher visible light photocatalytic activity

International Nuclear Information System (INIS)

Hong Xiaoting; Wu Xiaohui; Zhang Qiuyun; Xiao Mingfeng; Yang Gelin; Qiu Meirong; Han Guocheng

2012-01-01

Hydroxyapatite supported Ag 3 PO 4 nanocomposites have been synthesized by a wet impregnation process. UV-vis absorption spectra show a red shift of the absorption edges for the composite systems compared to pure hydroxyapatite support. The surface structure and morphology of the nanocomposites were characterized by Brunauer-Emmett-Teller (BET) apparatus, X-ray diffraction (XRD), transmission electron microscopy (TEM). The results suggest that Ag 3 PO 4 nanoparticles (6-17 nm in diameter) are well dispersed on the hydroxyapatite support and Ag 3 PO 4 nanoparticles density is larger for the higher Ag + loading sample. The as-prepared nanocomposite photocatalysts showed a pronounced photocatalytic activity upon decomposition of methylene blue dye in aqueous solution under both visible light (wavelength > 400 nm) and UV-vis light irradiation. A synergic mechanism of inherent photocatalytic capability of Ag 3 PO 4 and the accelerated electron/hole separation resulting from the photoinduced electrons captured by the slow-released Ag + at the interface of Ag 3 PO 4 and hydroxyapatite is proposed for the nanocomposites on the enhancement of photocatalytic performance in comparison to that of pure Ag 3 PO 4 nanoparticles. The support of hydroxyapatite may also act as an absorbent which favors the mass transfer in heterogeneous photocatalysis reaction.

A comparative structural and electrochemical study of monoclinic Li3V2(PO4)3/C and rhombohedral Li2.5Na0.5V(2−2x/3)Nix(PO4)3/C

International Nuclear Information System (INIS)

Wang, Wenhui; Chen, Zhenyu; Zhang, Jiaolong; Dai, Changsong; Li, Jiajie; Ji, Dalong

2013-01-01

In order to synthesize pure derivative of rhombohedral Li 3 V 2 (PO 4 ) 3 (LVP), lithium-ion batteries materials Li 2.5 Na 0.5 V (2−2x/3) Ni x (PO 4 ) 3 /C (x = 0.03, 0.06, 0.09) and its control, monoclinic Li 3 V 2 (PO 4 ) 3 /C (LVP/C), were prepared by sol–gel method. The samples were investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), Raman spectroscopy, and electrochemical methods. The XRD patterns of Li 2.5 Na 0.5 V (2−2x/3) Ni x (PO 4 ) 3 /C are in good agreement with that of rhombohedral LVP, which indicates that the Na + –Ni 2+ composite doping can change the structure of monoclinic LVP. All the composite doping samples displayed a single flat plateau at 3.7 V in the charge/discharge voltage profile, which is caused by transformation of multi-phase mechanism to single-phase mechanism. For Li 2.5 Na 0.5 V 1.98 Ni 0.03 (PO 4 ) 3 /C, a specific discharge capacity of 108 mAh g −1 was achieved at a 0.5 C charge rate and a 1 C discharge rate, and a 99.0% retention rate of the initial capacity was obtained after 50 cycles