WorldWideScience

Sample records for anodic alumina films

  1. Titanium nitride stamps replicating nanoporous anodic alumina films

    International Nuclear Information System (INIS)

    Navas, D; Sanchez, O; Asenjo, A; Jaafar, M; Baldonedo, J L; Vazquez, M; Hernandez-Velez, M

    2007-01-01

    Fabrication of nanostructured TiN films by magnetron sputtering using nanoporous anodic alumina films (NAAF) as substrates is reported. These hard nanostructured films could be used for pre-patterning aluminium foils and to obtain nanoporous films replicating the starting NAAF over a wide range of pore diameters and spacings. Pre-patterned Al foils are obtained by compression with pressures lower than those previously reported, then a new NAAF can be fabricated by means of only one anodization process. As an example, one of the TiN stamps was used for pre-patterning an Al foil at a pressure of 200 kg cm -2 and then it was anodized in oxalic acid solution obtaining the corresponding replica of the starting NAAF

  2. Fabrication of porous anodic alumina films by using two-step anodization process

    International Nuclear Information System (INIS)

    Xu Zhan; Zhou Bin; Xu Xiang; Wang Xiaoli; Wu Di; Shen Jun

    2006-01-01

    This article introduces the fabrication of the porous anodic alumina films which have ordered pore arrangement by using a two-step anodization process. The films have a parallel channel structure which nanopore diameter can be 20-100 nm, and depth can reach 50 μm. The change of pore structure in the first and second anodization, moving the alumina layer, widening process was analysed. The effect of the parameters such as different electrolytes, anodization temperature and the voltage on the nanopore structure was studied. The surface and profile structure through FE-SEM (field emission scanning electron microscope), the element composition in tiny area of the anodic aluminum oxide (AAO) surface were studied. The result indicates the pore diameter of AAO which is anodized in oxalic acid solution is larger than which anodized in sulfuric acid solution. The anodization temperature and voltage can enlarge the nanopore diameter of AAO in a range. (authors)

  3. Ordered Nanomaterials Thin Films via Supported Anodized Alumina Templates

    Directory of Open Access Journals (Sweden)

    Mohammed eES-SOUNI

    2014-10-01

    Full Text Available Supported anodized alumina template films with highly ordered porosity are best suited for fabricating large area ordered nanostructures with tunable dimensions and aspect ratios. In this paper we first discuss important issues for the generation of such templates, including required properties of the Al/Ti/Au/Ti thin film heterostructure on a substrate for high quality templates. We then show examples of anisotropic nanostructure films consisting of noble metals using these templates, discuss briefly their optical properties and their applications to molecular detection using surface enhanced Raman spectroscopy. Finally we briefly address the possibility to make nanocomposite films, exemplary shown on a plasmonic-thermochromic nanocomposite of VO2-capped Au-nanorods.

  4. Porous and mesh alumina formed by anodization of high purity aluminum films at low anodizing voltage

    Energy Technology Data Exchange (ETDEWEB)

    Abd-Elnaiem, Alaa M., E-mail: alaa.abd-elnaiem@science.au.edu.eg [KACST-Intel Consortium Center of Excellence in Nano-manufacturing Applications (CENA), Riyadh (Saudi Arabia); Physics Department, Faculty of Science, Assiut University, Assiut 71516 (Egypt); Mebed, A.M. [Physics Department, Faculty of Science, Assiut University, Assiut 71516 (Egypt); Department of Physics, Faculty of Science, Al-Jouf University, Sakaka 2014 (Saudi Arabia); El-Said, Waleed Ahmed [Department of Chemistry, Faculty of Science, Assiut University, Assiut 71516 (Egypt); Abdel-Rahim, M.A. [Physics Department, Faculty of Science, Assiut University, Assiut 71516 (Egypt)

    2014-11-03

    Electrochemical oxidation of high-purity aluminum (Al) films under low anodizing voltages (1–10) V has been conducted to obtain anodic aluminum oxide (AAO) with ultra-small pore size and inter-pore distance. Different structures of AAO have been obtained e.g. nanoporous and mesh structures. Highly regular pore arrays with small pore size and inter-pore distance have been formed in oxalic or sulfuric acids at different temperatures (22–50 °C). It is found that the pore diameter, inter-pore distance and the barrier layer thickness are independent of the anodizing parameters, which is very different from the rules of general AAO fabrication. The brand formation mechanism has been revealed by the scanning electron microscope study. Regular nanopores are formed under 10 V at the beginning of the anodization and then serve as a template layer dominating the formation of ultra-small nanopores. Anodization that is performed at voltages less than 5 V leads to mesh structured alumina. In addition, we have introduced a simple one-pot synthesis method to develop thin walls of oxide containing lithium (Li) ions that could be used for battery application based on anodization of Al films in a supersaturated mixture of lithium phosphate and phosphoric acid as matrix for Li-composite electrolyte. - Highlights: • We develop anodic aluminum oxide (AAO) with small pore size and inter-pore distance. • Applying low anodizing voltages onto aluminum film leads to form mesh structures. • The value of anodizing voltage (1–10 V) has no effect on pore size or inter-pore distance. • Applying anodizing voltage less than 5 V leads to mesh structured AAO. • AAO can be used as a matrix for Li-composite electrolytes.

  5. Porous and mesh alumina formed by anodization of high purity aluminum films at low anodizing voltage

    International Nuclear Information System (INIS)

    Abd-Elnaiem, Alaa M.; Mebed, A.M.; El-Said, Waleed Ahmed; Abdel-Rahim, M.A.

    2014-01-01

    Electrochemical oxidation of high-purity aluminum (Al) films under low anodizing voltages (1–10) V has been conducted to obtain anodic aluminum oxide (AAO) with ultra-small pore size and inter-pore distance. Different structures of AAO have been obtained e.g. nanoporous and mesh structures. Highly regular pore arrays with small pore size and inter-pore distance have been formed in oxalic or sulfuric acids at different temperatures (22–50 °C). It is found that the pore diameter, inter-pore distance and the barrier layer thickness are independent of the anodizing parameters, which is very different from the rules of general AAO fabrication. The brand formation mechanism has been revealed by the scanning electron microscope study. Regular nanopores are formed under 10 V at the beginning of the anodization and then serve as a template layer dominating the formation of ultra-small nanopores. Anodization that is performed at voltages less than 5 V leads to mesh structured alumina. In addition, we have introduced a simple one-pot synthesis method to develop thin walls of oxide containing lithium (Li) ions that could be used for battery application based on anodization of Al films in a supersaturated mixture of lithium phosphate and phosphoric acid as matrix for Li-composite electrolyte. - Highlights: • We develop anodic aluminum oxide (AAO) with small pore size and inter-pore distance. • Applying low anodizing voltages onto aluminum film leads to form mesh structures. • The value of anodizing voltage (1–10 V) has no effect on pore size or inter-pore distance. • Applying anodizing voltage less than 5 V leads to mesh structured AAO. • AAO can be used as a matrix for Li-composite electrolytes

  6. Excitation of anodized alumina films with a light source

    DEFF Research Database (Denmark)

    Aggerbeck, Martin; Canulescu, Stela; Rechendorff, K.

    Optical properties of anodized aluminium alloys were determined by optical diffuse reflectance spectroscopy of such films. Samples with different concentrations of dopants were excited with a white-light source combined with an integrating sphere for fast determination of diffuse reflectance....... The UV-VIS reflectance of Ti-doped anodized aluminium films was measured over the wavelength range of 200 nm to 900 nm. Titanium doped-anodized aluminium films with 5-15 wt% Ti were characterized. Changes in the diffuse light scattering of doped anodized aluminium films, and thus optical appearance......, with doping are discussed. Using the Kubelka-Munk model on the diffuse reflectance spectra of such films, the bandgap Eg of the oxide alloys can be determined....

  7. Fabrication of highly ordered nanoporous alumina films by stable high-field anodization

    International Nuclear Information System (INIS)

    Li Yanbo; Zheng Maojun; Ma Li; Shen Wenzhong

    2006-01-01

    Stable high-field anodization (1500-4000 A m -2 ) for the fabrication of highly ordered porous anodic alumina films has been realized in a H 3 PO 4 -H 2 O-C 2 H 5 OH system. By maintaining the self-ordering voltage and adjusting the anodizing current density, high-quality self-ordered alumina films with a controllable inter-pore distance over a large range are achieved. The high anodizing current densities lead to high-speed film growth (4-10 μm min -1 ). The inter-pore distance is not solely dependent on the anodizing voltage, but is also influenced by the anodizing current density. This approach is simple and cost-effective, and is of great value for applications in diverse areas of nanotechnology

  8. Surface of Alumina Films after Prolonged Breakdowns in Galvanostatic Anodization

    Directory of Open Access Journals (Sweden)

    Christian Girginov

    2011-01-01

    Full Text Available Breakdown phenomena are investigated at continuous isothermal (20∘C and galvanostatic (0.2–5 mA cm−2 anodizing of aluminum in ammonium salicylate in dimethylformamide (1 M AS/DMF electrolyte. From the kinetic (-curves, the breakdown voltage ( values are estimated, as well as the frequency and amplitude of oscillations of formation voltage ( at different current densities. The surface of the aluminum specimens was studied using atomic force microscopy (AFM. Data on topography and surface roughness parameters of the electrode after electric breakdowns are obtained as a function of anodization time. The electrode surface of anodic films, formed with different current densities until the same charge density has passed (2.5 C cm−2, was assessed. Results are discussed on the basis of perceptions of avalanche mechanism of the breakdown phenomena, due to the injection of electrons and their multiplication in the volume of the film.

  9. Hybrid pulse anodization for the fabrication of porous anodic alumina films from commercial purity (99%) aluminum at room temperature

    International Nuclear Information System (INIS)

    Chung, C K; Zhou, R X; Chang, W T; Liu, T Y

    2009-01-01

    Most porous anodic alumina (PAA) or anodic aluminum oxide (AAO) films are fabricated using the potentiostatic method from high-purity (99.999%) aluminum films at a low temperature of approximately 0-10 deg. C to avoid dissolution effects at room temperature (RT). In this study, we have demonstrated the fabrication of PAA film from commercial purity (99%) aluminum at RT using a hybrid pulse technique which combines pulse reverse and pulse voltages for the two-step anodization. The reaction mechanism is investigated by the real-time monitoring of current. A possible mechanism of hybrid pulse anodization is proposed for the formation of pronounced nanoporous film at RT. The structure and morphology of the anodic films were greatly influenced by the duration of anodization and the type of voltage. The best result was obtained by first applying pulse reverse voltage and then pulse voltage. The first pulse reverse anodization step was used to form new small cells and pre-texture concave aluminum as a self-assembled mask while the second pulse anodization step was for the resulting PAA film. The diameter of the nanopores in the arrays could reach 30-60 nm.

  10. Superhydrophilicity of novel anodic alumina nanofibers films and their formation mechanism

    Science.gov (United States)

    Peng, Rong; Yang, Wulin; Fu, Licai; Zhu, Jiajun; Li, Deyi; Zhou, Lingping

    2017-06-01

    A novel anodic alumina nanofibers structure, which is different from the traditional porous anodic structure, has been quickly fabricated via anodizing in a new electrolyte, pyrophosphoric acid. The effects of the solution concentration and the anodizing time on the formation of the anodic alumina nanofibers were analyzed. The results show that the nanostructure of anodic alumina can change to the nanofiber oxide from the porous oxide by increasing the solution concentration. Prolonging the anodizing time is beneficial to obtain alumina nanofibers at high solution concentration. Growth behavior of the alumina nanofibers was also discussed by scanning electron microscopy observations. Owing to the unique hexagonal structure of anodic alumina as well as the preferential chemical dissolution between the porous anodic alumina and the anodic alumina nanotips, the slightly soluble anodic alumina nanotips could form novel alumina nanofibers during anodizing. The results show that the nanofibers-covered aluminum surface exhibits superhydrophilic property, with a near-zero water contact angle. Such alumina nanofibers with superhydrophilic property could be used for various potential applications.

  11. Linear Coefficient of Thermal Expansion of Porous Anodic Alumina Thin Films from Atomic Force Microscopy

    OpenAIRE

    Zhang, Richard X; Fisher, Timothy; Raman, Arvind; Sands, Timothy D

    2009-01-01

    In this article, a precise and convenient technique based on the atomic force microscope (AFM) is developed to measure the linear coefficient of thermal expansion of a porous anodic alumina thin film. A stage was used to heat the sample from room temperature up to 450 K. Thermal effects on AFM probes and different operation modes at elevated temperatures were also studied, and a silicon AFM probe in the tapping mode was chosen for the subsequent measurements due to its temperature insensitivi...

  12. Porous Alumina Films with Width-Controllable Alumina Stripes

    Directory of Open Access Journals (Sweden)

    Huang Shi-Ming

    2010-01-01

    Full Text Available Abstract Porous alumina films had been fabricated by anodizing from aluminum films after an electropolishing procedure. Alumina stripes without pores can be distinguished on the surface of the porous alumina films. The width of the alumina stripes increases proportionally with the anodizing voltage. And the pores tend to be initiated close to the alumina stripes. These phenomena can be ascribed to the electric field distribution in the alumina barrier layer caused by the geometric structure of the aluminum surface.

  13. Porous Alumina Films with Width-Controllable Alumina Stripes

    Science.gov (United States)

    2010-01-01

    Porous alumina films had been fabricated by anodizing from aluminum films after an electropolishing procedure. Alumina stripes without pores can be distinguished on the surface of the porous alumina films. The width of the alumina stripes increases proportionally with the anodizing voltage. And the pores tend to be initiated close to the alumina stripes. These phenomena can be ascribed to the electric field distribution in the alumina barrier layer caused by the geometric structure of the aluminum surface. PMID:21170406

  14. Formation and disruption of current paths of anodic porous alumina films by conducting atomic force microscopy

    International Nuclear Information System (INIS)

    Oyoshi, K.; Nigo, S.; Inoue, J.; Sakai, O.; Kitazawa, H.; Kido, G.

    2010-01-01

    Anodic porous alumina (APA) films have a honeycomb cell structure of pores and a voltage-induced bi-stable switching effect. We have applied conducting atomic force microscopy (CAFM) as a method to form and to disrupt current paths in the APA films. A bi-polar switching operation was confirmed. We have firstly observed terminals of current paths as spots or areas typically on the center of the triangle formed by three pores. In addition, though a part of the current path showed repetitive switching, most of them were not observed again at the same position after one cycle of switching operations in the present experiments. This suggests that a part of alumina structure and/or composition along the current paths is modified during the switching operations.

  15. Formation and disruption of current paths of anodic porous alumina films by conducting atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Oyoshi, K., E-mail: oyoshi.keiji@nims.go.jp [National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305-0047 (Japan); Nigo, S.; Inoue, J.; Sakai, O.; Kitazawa, H.; Kido, G. [National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305-0047 (Japan)

    2010-11-15

    Anodic porous alumina (APA) films have a honeycomb cell structure of pores and a voltage-induced bi-stable switching effect. We have applied conducting atomic force microscopy (CAFM) as a method to form and to disrupt current paths in the APA films. A bi-polar switching operation was confirmed. We have firstly observed terminals of current paths as spots or areas typically on the center of the triangle formed by three pores. In addition, though a part of the current path showed repetitive switching, most of them were not observed again at the same position after one cycle of switching operations in the present experiments. This suggests that a part of alumina structure and/or composition along the current paths is modified during the switching operations.

  16. Influence of the anodizing process variables on the acidic properties of anodic alumina films

    Directory of Open Access Journals (Sweden)

    D.E. Boldrini

    Full Text Available Abstract In the present work, the effect of the different variables involved in the process of aluminum anodizing on the total surface acidity of the samples obtained was studied. Aluminum foils were treated by the electro-chemical process of anodic anodizing within the following variable ranges: concentration = 1.5-2.5 M; temperature = 303-323 K; voltage = 10-20 V; time = 30-90 min. The total acidity of the samples was characterized by two different methods: acid-base titration using Hammett indicators and potentiometric titration. The results showed that anodizing time, temperature and concentration were the main variables that determined the surface acid properties of the samples, and to a lesser extent voltage. Acidity increased with increasing concentration of the electrolytic bath, whereas the rest of the variables had the opposite effect. The results obtained provide a novel tool for variable selection in order to use synthetized materials as catalytic supports, adding to previous research based on the morphology of alumina layers.

  17. Fabrication of Anodic Porous Alumina by Squaric Acid Anodizing

    OpenAIRE

    Kikuchi, Tatsuya; Yamamoto, Tsuyoshi; Natsui, Shungo; Suzuki, Ryosuke O.

    2014-01-01

    The growth behavior of anodic porous alumina formed via anodizing in a new electrolyte, squaric acid (3,4-dihydroxy-3-cyclobutene-1,2-dione), is reported for the first time. A high-purity aluminum foil was anodized in a 0.1 M squaric acid solution at 293 K and a constant applied potential of 100-150 V. Anodic oxides grew on the aluminum foil at applied potentials of 100-120 V, but a burned oxide film was formed at higher voltage. Anodic porous alumina with a cell size of approximately 200-400...

  18. Preparation of mesoporous alumina films by anodization: Effect of pretreatments on the aluminum surface and MTBE catalytic oxidation

    International Nuclear Information System (INIS)

    Vazquez, A.L.; Carrera, R.; Arce, E.; Castillo, N.; Castillo, S.; Moran-Pineda, M.

    2009-01-01

    Mesoporous materials are both scientifically and technologically important because of the presence of voids of controllable dimensions at atomic, molecular, and nanometric scales. Over the last decade, there has been both an increasing interest and research effort in the synthesis and characterization of these types of materials. The purposes of this work are to study the physical and chemical changes in the properties of mesoporous alumina films produced by anodization in sulphuric acid by different pretreatments on the aluminium surface such as mechanical polishing [MP] and electropolishing [EP]; and to compare their properties such as morphology, structure and catalytic activity with those present in commercial alumina. The morphologic and physical characterizations of the alumina film samples were carried out by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The chemical evaluations were performed by the oxidation of methyl-tert-butyl-ether (MTBE) at 400 deg. C under O 2 /He oxidizing conditions (Praxair, 2.0% O 2 /He balance). According to the results, the samples that presented higher activities than those in Al 2 O 3 /Al [MP] and commercial alumina in the MTBE oxidation (69%), were those prepared by Al 2 O 3 /Al [EP]. The average mesoporous diameter was 17 nm, and the morphological shape was equiaxial; thus, that pore distribution was the smallest of all with a homogeneous distribution.

  19. Preparation of mesoporous alumina films by anodization: Effect of pretreatments on the aluminum surface and MTBE catalytic oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, A.L., E-mail: avazquezd@ipn.m [Departamento de Ingenieria Metalurgica, ESIQIE-IPN, AP 75-876, Mexico, D.F. (Mexico); Programa de Ingenieria Molecular, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, C.P. 07730, Mexico, D.F. (Mexico); Carrera, R. [Departamento de Ingenieria Metalurgica, ESIQIE-IPN, AP 75-876, Mexico, D.F. (Mexico); Programa de Ingenieria Molecular, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, C.P. 07730, Mexico, D.F. (Mexico); Arce, E. [Departamento de Ingenieria Metalurgica, ESIQIE-IPN, AP 75-876, Mexico, D.F. (Mexico); Castillo, N. [CINVESTAV, Departamento de Fisica. Av. IPN 2508, 07360, Mexico, D.F (Mexico); Castillo, S. [Departamento de Ingenieria Metalurgica, ESIQIE-IPN, AP 75-876, Mexico, D.F. (Mexico); Programa de Ingenieria Molecular, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, C.P. 07730, Mexico, D.F. (Mexico); Moran-Pineda, M. [Programa de Ingenieria Molecular, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, C.P. 07730, Mexico, D.F. (Mexico)

    2009-08-26

    Mesoporous materials are both scientifically and technologically important because of the presence of voids of controllable dimensions at atomic, molecular, and nanometric scales. Over the last decade, there has been both an increasing interest and research effort in the synthesis and characterization of these types of materials. The purposes of this work are to study the physical and chemical changes in the properties of mesoporous alumina films produced by anodization in sulphuric acid by different pretreatments on the aluminium surface such as mechanical polishing [MP] and electropolishing [EP]; and to compare their properties such as morphology, structure and catalytic activity with those present in commercial alumina. The morphologic and physical characterizations of the alumina film samples were carried out by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The chemical evaluations were performed by the oxidation of methyl-tert-butyl-ether (MTBE) at 400 deg. C under O{sub 2}/He oxidizing conditions (Praxair, 2.0% O{sub 2}/He balance). According to the results, the samples that presented higher activities than those in Al{sub 2}O{sub 3}/Al [MP] and commercial alumina in the MTBE oxidation (69%), were those prepared by Al{sub 2}O{sub 3}/Al [EP]. The average mesoporous diameter was 17 nm, and the morphological shape was equiaxial; thus, that pore distribution was the smallest of all with a homogeneous distribution.

  20. Penetrating the oxide barrier in situ and separating freestanding porous anodic alumina films in one step.

    Science.gov (United States)

    Tian, Mingliang; Xu, Shengyong; Wang, Jinguo; Kumar, Nitesh; Wertz, Eric; Li, Qi; Campbell, Paul M; Chan, Moses H W; Mallouk, Thomas E

    2005-04-01

    A simple method for penetrating the barrier layer of an anodic aluminum oxide (AAO) film and for detaching the AAO film from residual Al foil was developed by reversing the bias voltage in situ after the anodization process is completed. With this technique, we have been able to obtain large pieces of free-standing AAO membranes with regular pore sizes of sub-10 nm. By combining Ar ion milling and wetting enhancement processes, Au nanowires were grown in the sub-10 nm pores of the AAO films. Further scaling down of the pore size and extension to the deposition of nanowires and nanotubes of materials other than Au should be possible by further optimizing this procedure.

  1. Fabrication of porous anodic alumina using normal anodization and pulse anodization

    Science.gov (United States)

    Chin, I. K.; Yam, F. K.; Hassan, Z.

    2015-05-01

    This article reports on the fabrication of porous anodic alumina (PAA) by two-step anodizing the low purity commercial aluminum sheets at room temperature. Different variations of the second-step anodization were conducted: normal anodization (NA) with direct current potential difference; pulse anodization (PA) alternate between potential differences of 10 V and 0 V; hybrid pulse anodization (HPA) alternate between potential differences of 10 V and -2 V. The method influenced the film homogeneity of the PAA and the most homogeneous structure was obtained via PA. The morphological properties are further elucidated using measured current-transient profiles. The absent of current rise profile in PA indicates the anodization temperature and dissolution of the PAA structure were greatly reduced by alternating potential differences.

  2. Electrochemical impedance spectroscopy of nanoporous anodic alumina template

    International Nuclear Information System (INIS)

    Shahzad, K.

    2010-01-01

    Room temperature EIS characterization of nanoporous anodic alumina prepared at 40 V and 60 V has been done in 0.3 M oxalic acid solution. Rapid decrease in impedance was observed for the template prepared at 40 V. EIS study of porous anodic alumina template prepared in 0.3 M oxalic acid has been done in different electrolytes. Templates prepared in 0.3 M sulfuric acid solution were also characterized for comparison. Rapid decrease in the thickness of nonporous anodic film was observed with an increase of aggressiveness of electrolyte. Temperature based systematic study of EIS measurement has been done for porous anodic alumina template at different temperatures. Formation of micropores was observed in the nanoporous anodic alumina film formed on aluminum in 0.3 M oxalic acid solution which accelerates the dissolution rate with increase of measurement temperature. In addition to these, electropolishing behavior of pure aluminum has also been studied in different electrolytes and it was observed that electropolishing conditions prior to anodization are extremely important. (author)

  3. Energy transfer in porous anodic alumina/rhodamine 110 nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Elhouichet, H., E-mail: habib.elhouichet@fst.rnu.tn [Laboratoire de Physico-Chimie des Materiaux Mineraux et leurs Applications, Centre National de Recherches en Sciences des Materiaux, B.P. 95, Hammam-Lif 2050 (Tunisia); Departement de Physique, Faculte des Sciences de Tunis, University of Tunis Elmanar 2092 Tunis (Tunisia); Harima, N.; Koyama, H. [Hyogo University of Teacher Education, Kato, Hyogo 673-1494 (Japan); Gaponenko, N.V. [Belarusian State University of Informatics and Radioelectronics, P. Browki St. 6, 220013 Minsk (Belarus)

    2012-09-15

    We have used porous anodic alumina (PAA) films as templates for embedding rhodamine 110 (Rh110) molecules and examined their photoluminescence (PL) properties in detail. The analysis of the polarization memory (PM) of PL strongly suggests that there is a significant energy transfer from PAA to Rh110 molecules. The effect of annealing the PAA layer on the PL properties of the nanocomposite has been studied. The results show that the energy transfer becomes more efficient in annealed PAA. - Highlights: Black-Right-Pointing-Pointer Porous anodic alumina-rhodamine 110 nanocomposites are elaborated. Black-Right-Pointing-Pointer Efficient energy transfer from the host to Rh110 molecules is evidenced from measurements of photoluminescence and degree of polarization memory spectra. Black-Right-Pointing-Pointer Thermal annealing of porous anodic alumina can improve the process of excitation transfer.

  4. Electronic properties of electrolyte/anodic alumina junction during porous anodizing

    Energy Technology Data Exchange (ETDEWEB)

    Vrublevsky, I. [Department of Microelectronics, Belarusian State University of Informatics and Radioelectronics, 6 Brovka Street, Minsk 220013 (Belarus)]. E-mail: nil-4-2@bsuir.edu.by; Jagminas, A. [Institute of Chemistry, A. Gostauto 9, LT-01108 Vilnius (Lithuania); Schreckenbach, J. [Institut fuer Chemie, Technische Universitaet Chemnitz, Chemnitz D-09107 (Germany); InnoMat GmbH, Chemnitz (Germany); Goedel, Werner A. [Institut fuer Chemie, Technische Universitaet Chemnitz, Chemnitz D-09107 (Germany)

    2007-03-15

    The growth of porous oxide films on aluminum (99.99% purity), formed in 4% phosphoric acid was studied as a function of the anodizing voltage (23-53 V) using a re-anodizing technique and transmission electron microscopy (TEM) study. The chemical dissolution behavior of freshly anodized and annealed at 200 deg. C porous alumina films was studied. The obtained results indicate that porous alumina has n-type semiconductive behavior during anodizing in 4% phosphoric acid. During anodising, up to 39 V in the barrier layer of porous films, one obtains an accumulation layer (the thickness does not exceed 1 nm) where the excess electrons have been injected into the solid producing a downward bending of the conductive and valence band towards the interface. The charge on the surface of anodic oxide is negative and decreases with growing anodizing voltage. At the anodizing voltage of about 39 V, the charge on the surface of anodic oxide equals to zero. Above 39 V, anodic alumina/electrolyte junction injects protons from the electrolyte. These immobile positive charges in the surface layer of oxide together with an ionic layer of hydroxyl ions concentrated near the interface create a field, which produces an upward bending of the bands.

  5. Iron films deposited on porous alumina substrates

    Energy Technology Data Exchange (ETDEWEB)

    Yamada, Yasuhiro, E-mail: yyasu@rs.kagu.tus.ac.jp; Tanabe, Kenichi; Nishida, Naoki [Tokyo University of Science (Japan); Kobayashi, Yoshio [The University of Electro-Communications (Japan)

    2016-12-15

    Iron films were deposited on porous alumina substrates using an arc plasma gun. The pore sizes (120 – 250 nm) of the substrates were controlled by changing the temperature during the anodic oxidation of aluminum plates. Iron atoms penetrated into pores with diameters of less than 160 nm, and were stabilized by forming γ-Fe, whereas α-Fe was produced as a flat plane covering the pores. For porous alumina substrates with pore sizes larger than 200 nm, the deposited iron films contained many defects and the resulting α-Fe had smaller hyperfine magnetic fields. In addition, only a very small amount of γ-Fe was obtained. It was demonstrated that the composition and structure of an iron film can be affected by the surface morphology of the porous alumina substrate on which the film is grown.

  6. Growth behavior of anodic porous alumina formed in malic acid solution

    Science.gov (United States)

    Kikuchi, Tatsuya; Yamamoto, Tsuyoshi; Suzuki, Ryosuke O.

    2013-11-01

    The growth behavior of anodic porous alumina formed on aluminum by anodizing in malic acid solutions was investigated. High-purity aluminum plates were electropolished in CH3COOH/HClO4 solutions and then anodized in 0.5 M malic acid solutions at 293 K and constant cell voltages of 200-350 V. The anodic porous alumina grew on the aluminum substrate at voltages of 200-250 V, and a black, burned oxide film was formed at higher voltages. The nanopores of the anodic oxide were only formed at grain boundaries of the aluminum substrate during the initial stage of anodizing, and then the growth region extended to the entire aluminum surface as the anodizing time increased. The anodic porous alumina with several defects was formed by anodizing in malic acid solution at 250 V, and oxide cells were approximately 300-800 nm in diameter.

  7. Hydrophilicity Reinforced Adhesion of Anodic Alumina Oxide Template Films to Conducting Substrates for Facile Fabrication of Highly Ordered Nanorod Arrays.

    Science.gov (United States)

    Wang, Chuanju; Wang, Guiqiang; Yang, Rui; Sun, Xiangyu; Ma, Hui; Sun, Shuqing

    2017-01-17

    Arrays of ordered nanorods are of special interest in many fields. However, it remains challenging to obtain such arrays on conducting substrates in a facile manner. In this article, we report the fabrication of highly ordered and vertically standing nanorod arrays of both metals and semiconductors on Au films and indium tin oxide glass substrates without an additional layering. In this approach, following the simple hydrophilic treatment of an anodic aluminum oxide (AAO) membrane and conducting substrates, the AAO membrane was transferred onto the modified substrates with excellent adhesion. Subsequently, nanorod arrays of various materials were electrodeposited on the conducting substrates directly. This method avoids any expensive and tedious lithographic and ion milling process, which provides a simple yet robust route to the fabrication of arrays of 1D materials with high aspect ratio on conducting substrates, which shall pave the way for many practical applications in a range of fields.

  8. Effects of Etching Time and NaOH Concentration on the Production of Alumina Nanowires Using Porous Anodic Alumina Template

    Science.gov (United States)

    Sadeghpour-Motlagh, M.; Mokhtari-Zonouzi, K.; Aghajani, H.; Kakroudi, M. Ghassemi

    2014-06-01

    In this work, two-step anodizing of commercial aluminum foil in acid oxalic solution was applied for producing alumina film. Then the anodic alumina film was etched in sodium hydroxide (NaOH) solution resulting dense and aligned alumina nanowires. This procedure leads to splitting of alumina nanotubes. Subsequently nanowires are produced. The effects of NaOH solution concentration (0.2-1 mol/L) and etching time (60-300 s) at constant temperature on characteristic of nanotubes and produced nanowires were investigated using scanning electron microscopy. The results show that an increase in NaOH solution concentration increases the rate of nanowires production and in turn the manipulation process will be more specific.

  9. Self-ordered Porous Alumina Fabricated via Phosphonic Acid Anodizing

    OpenAIRE

    Akiya, Shunta; Kikuchi, Tatsuya; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

    2016-01-01

    Self-ordered periodic porous alumina with an undiscovered cell diameter was fabricated via electrochemical anodizing in a new electrolyte, phosphonic acid (H3PO3). High-purity aluminum plates were anodized in phosphonic acid solution under various operating conditions of voltage, temperature, concentration, and anodizing time. Phosphonic acid anodizing at 150-180 V caused the self-ordering behavior of porous alumina, and an ideal honeycomb nanostructure measuring 370-440 nm in cell diameter w...

  10. Effect of anodizing voltage on the sorption of water molecules on porous alumina

    Energy Technology Data Exchange (ETDEWEB)

    Vrublevsky, I., E-mail: vrublevsky@bsuir.edu.by [Belarusian State University of Informatics and Radioelectronics, Department of Micro and Nanoelectronics, 220013 Minsk (Belarus); Chernyakova, K. [Belarusian State University of Informatics and Radioelectronics, Department of Micro and Nanoelectronics, 220013 Minsk (Belarus); Bund, A.; Ispas, A.; Schmidt, U. [Fachgebiet Elektrochemie und Galvanotechnik, Technische Universitaet Ilmenau, 98693 Ilmenau (Germany)

    2012-05-01

    The amount of water adsorbed on different centers on the surface of oxalic acid alumina films is a function of the anodizing voltage. It is decreased with increasing the anodizing voltage from 20 up to 50 V, came up to maximum value at 20-30 V and slightly increased at voltages above 50 V. Water adsorption by oxide films formed at voltages below 50 V can be due to the negative surface charge that is present on the alumina surface. The negative surface charge disappears in the films formed at voltages higher than 50 V, and thus, the water is adsorbed on aluminum ions in a tetrahedral and octahedral environment. The correlation between anodizing conditions of aluminum in oxalic acid and the structure and composition of anodic alumina was established by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), thermogravimetric and differential thermal analyses (TG/DTA).

  11. Cathodoluminescence study of anodic nanochannel alumina

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Q.X. [Department of Electrical and Electronic Engineering, Saga University, Honjo-1, Saga, 840-8502 (Japan)]. E-mail: guoq@cc.saga-u.ac.jp; Hachiya, Y. [Department of Electrical and Electronic Engineering, Saga University, Honjo-1, Saga, 840-8502 (Japan); Tanaka, T. [Department of Electrical and Electronic Engineering, Saga University, Honjo-1, Saga, 840-8502 (Japan); Nishio, M. [Department of Electrical and Electronic Engineering, Saga University, Honjo-1, Saga, 840-8502 (Japan); Ogawa, H. [Department of Electrical and Electronic Engineering, Saga University, Honjo-1, Saga, 840-8502 (Japan)

    2006-07-15

    Nanochannel alumina (NCA) templates with highly ordered pore arrays were prepared by anodizing pure aluminum foil in acid solutions. Cathodoluminescence measurements reveal that a blue emission band appears at around 2.8 eV and its energy position depends on measurement temperature and pore size of NCA. The shift of the blue emission band energy with temperature is ascribed to the variations of electron-phonon interactions. X-ray absorption near-edge fine structure results show that the blue emission band shift with pore size is due to the local environment change of atoms in NCA.

  12. Electrochemical growth of nanowires in anodic alumina templates: the role of pore branching

    International Nuclear Information System (INIS)

    Noyan, Alexey A.; Leontiev, Alexey P.; Yakovlev, Maxim V.; Roslyakov, Ilya V.; Tsirlina, Galina A.; Napolskii, Kirill S.

    2017-01-01

    Highlights: • The model of metal growth inside the anodic alumina with branched pores is developed. • Model predicts the dependence of anodic alumina filling on deposition regime. • Branched pores affect the uniformity of anodic alumina filling with electrodeposits. • Branched pores make growth front of metal nanowires inside template multimodal. - Abstract: A comparative study of electrochemical growth of nanowires in the anodic alumina templates with various degree of porous structure ordering is performed. Scanning electron microscopy and coulometric analysis are used for experimental evaluation of the average filling of pores with metal. The theoretical model of metal growth inside anodic alumina templates is proposed. The model takes into account the presence of branched channels in the real structure of anodic alumina and operates with completeness of template filling achieved at the moment when metal reaches the external surface of the oxide film. In case of the diffusion-controlled regime the strong dependence of the pore filling factor on the thickness of porous film and the degree of its structure ordering is predicted theoretically and observed experimentally. The influence of the nature of limiting current on the homogeneity and completeness of template filling is discussed.

  13. Electrochemically replicated smooth aluminum foils for anodic alumina nanochannel arrays

    International Nuclear Information System (INIS)

    Biring, Sajal; Tsai, K-T; Sur, Ujjal Kumar; Wang, Y-L

    2008-01-01

    A fast electrochemical replication technique has been developed to fabricate large-scale ultra-smooth aluminum foils by exploiting readily available large-scale smooth silicon wafers as the masters. Since the adhesion of aluminum on silicon depends on the time of surface pretreatment in water, it is possible to either detach the replicated aluminum from the silicon master without damaging the replicated aluminum and master or integrate the aluminum film to the silicon substrate. Replicated ultra-smooth aluminum foils are used for the growth of both self-organized and lithographically guided long-range ordered arrays of anodic alumina nanochannels without any polishing pretreatment

  14. Variation of nanopore diameter along porous anodic alumina channels by multi-step anodization.

    Science.gov (United States)

    Lee, Kwang Hong; Lim, Xin Yuan; Wai, Kah Wing; Romanato, Filippo; Wong, Chee Cheong

    2011-02-01

    In order to form tapered nanocapillaries, we investigated a method to vary the nanopore diameter along the porous anodic alumina (PAA) channels using multi-step anodization. By anodizing the aluminum in either single acid (H3PO4) or multi-acid (H2SO4, oxalic acid and H3PO4) with increasing or decreasing voltage, the diameter of the nanopore along the PAA channel can be varied systematically corresponding to the applied voltages. The pore size along the channel can be enlarged or shrunken in the range of 20 nm to 200 nm. Structural engineering of the template along the film growth direction can be achieved by deliberately designing a suitable voltage and electrolyte together with anodization time.

  15. Structural analysis of anodic porous alumina used for resistive random access memory

    International Nuclear Information System (INIS)

    Lee, Jeungwoo; Nigo, Seisuke; Kato, Seiichi; Kitazawa, Hideaki; Kido, Giyuu; Nakano, Yoshihiro

    2010-01-01

    Anodic porous alumina with duplex layers exhibits a voltage-induced switching effect and is a promising candidate for resistive random access memory. The nanostructural analysis of porous alumina is important for understanding the switching effect. We investigated the difference between the two layers of an anodic porous alumina film using transmission electron microscopy and electron energy-loss spectroscopy. Diffraction patterns showed that both layers are amorphous, and the electron energy-loss spectroscopy indicated that the inner layer contains less oxygen than the outer layer. We speculate that the conduction paths are mostly located in the oxygen-depleted area.

  16. Novel structure formation at the bottom surface of porous anodic alumina fabricated by single step anodization process.

    Science.gov (United States)

    Ali, Ghafar; Ahmad, Maqsood; Akhter, Javed Iqbal; Maqbool, Muhammad; Cho, Sung Oh

    2010-08-01

    A simple approach for the growth of long-range highly ordered nanoporous anodic alumina film in H(2)SO(4) electrolyte through a single step anodization without any additional pre-anodizing procedure is reported. Free-standing porous anodic alumina film of 180 microm thickness with through hole morphology was obtained. A simple and single step process was used for the detachment of alumina from aluminum substrate. The effect of anodizing conditions, such as anodizing voltage and time on the pore diameter and pore ordering is discussed. The metal/oxide and oxide/electrolyte interfaces were examined by high resolution scanning transmission electron microscope. The arrangement of pores on metal/oxide interface was well ordered with smaller diameters than that of the oxide/electrolyte interface. The inter-pore distance was larger in metal/oxide interface as compared to the oxide/electrolyte interface. The size of the ordered domain was found to depend strongly upon anodizing voltage and time. (c) 2010 Elsevier Ltd. All rights reserved.

  17. Synthesis of aluminum oxy-hydroxide nanofibers from porous anodic alumina

    Energy Technology Data Exchange (ETDEWEB)

    Jha, Himendra; Kikuchi, Tatsuya; Sakairi, Masatoshi; Takahashi, Hideaki [Laboratory of Interface Microstructure Analysis (LIMSA), Division of Materials Science and Engineering, Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan)], E-mail: himendra@eng.hokudai.ac.jp

    2008-10-01

    A novel method for the synthesis of aluminum oxy-hydroxide nanofibers from a porous anodic oxide film of aluminum is demonstrated. In the present method, the porous anodic alumina not only acts as a template, but also serves as the starting material for the synthesis. The porous anodic alumina film is hydrothermally treated for pore-sealing, which forms aluminum oxy-hydroxide inside the pores of the oxide film as well as on the surface of the film. The hydrothermally sealed porous oxide film is immersed in the sodium citrate solution, which selectively etches the porous aluminum oxide from the film, leaving the oxy-hydroxide intact. The method is simple and gives highly uniform aluminum oxy-hydroxide nanofibers. Moreover, the diameter of the nanofibers can be controlled by controlling the pore size of the porous anodic alumina film, which depends on the anodizing conditions. Nanofibers with diameters of about 38-85 nm, having uniform shape and size, were successfully synthesized using the present method.

  18. Synthesis of aluminum oxy-hydroxide nanofibers from porous anodic alumina

    International Nuclear Information System (INIS)

    Jha, Himendra; Kikuchi, Tatsuya; Sakairi, Masatoshi; Takahashi, Hideaki

    2008-01-01

    A novel method for the synthesis of aluminum oxy-hydroxide nanofibers from a porous anodic oxide film of aluminum is demonstrated. In the present method, the porous anodic alumina not only acts as a template, but also serves as the starting material for the synthesis. The porous anodic alumina film is hydrothermally treated for pore-sealing, which forms aluminum oxy-hydroxide inside the pores of the oxide film as well as on the surface of the film. The hydrothermally sealed porous oxide film is immersed in the sodium citrate solution, which selectively etches the porous aluminum oxide from the film, leaving the oxy-hydroxide intact. The method is simple and gives highly uniform aluminum oxy-hydroxide nanofibers. Moreover, the diameter of the nanofibers can be controlled by controlling the pore size of the porous anodic alumina film, which depends on the anodizing conditions. Nanofibers with diameters of about 38-85 nm, having uniform shape and size, were successfully synthesized using the present method

  19. Characterization of the porous anodic alumina nanostructures with a metal interlayer on Si substrates

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Chia-Hui; Chen, Hung-Ing; Hsiao, Jui-Ju; Wang, Jen-Cheng; Nee, Tzer-En, E-mail: neete@mail.cgu.edu.tw

    2014-04-15

    Porous anodic alumina (PAA) films produced by the anodization technique have made possible the mass production of porous nano-scale structures where the pore height and diameter are controllable. A metal interlayer is observed to have a significant influence on the characteristics of these PAA nanostructures. In this study, we investigate in-depth the effect of the current density on the properties of porous anodic alumina nanostructures with a metal interlayer. A thin film layer of tungsten (W) and titanium (Ti) was sandwiched between a porous anodic alumina film and a silicon (Si) substrate to form PAA/W/Si and PAA/Ti/Si structures. The material and optical characteristics of the porous anodic alumina nanostructures, with and without a metal interlayer, on silicon substrates were studied using the scanning electron microscopy, X-ray diffraction (XRD), and temperature-dependent photoluminescence (PL) measurements. The current densities of the porous anodic alumina nanostructures with the metal interlayer are higher than for the PAA/Si, resulting in an increase of the growth rate of the oxide layer. It can be observed from the X-ray diffraction curves that there is more aluminum oxide inside the structure with the metal interlayer. Furthermore, it has been found that there is a reduction in the photoluminescence intensity of the oxygen vacancy with only one electron due to the formation of oxygen vacancies inside the aluminum oxide during the re-crystallization process. This leads to competition between the two kinds of different oxygen-deficient defect centers (F+ and F centers) in the carrier recombination mechanism from the PL spectra of the porous anodic alumina nanostructures, with and without a metal interlayer, on silicon substrates. -- Highlights: • Study of porous anodic alumina (PAA) films with metal interlayers on silicon. • The highly ordered PAA film with a fairly regular nano-porous structure. • The luminescence properties of PAA films were

  20. Optimum Exploration for the Self-Ordering of Anodic Porous Alumina Formed via Selenic Acid Anodizing

    OpenAIRE

    Akiya, Shunta; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2015-01-01

    Improvements of the regularity of the arrangement of anodic porous alumina formed by selenic acid anodizing were investigated under various operating conditions. The oxide burning voltage increased with the stirring rate of the selenic acid solution, and the high applied voltage without oxide burning was achieved by vigorously stirring the solution. The regularity of the porous alumina was improved as the anodizing time and surface flatness increased. Conversely, the purity of the 99.5–99.999...

  1. Ultra-High Density Single Nanometer-Scale Anodic Alumina Nanofibers Fabricated by Pyrophosphoric Acid Anodizing

    Science.gov (United States)

    Kikuchi, Tatsuya; Nishinaga, Osamu; Nakajima, Daiki; Kawashima, Jun; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

    2014-12-01

    Anodic oxide fabricated by anodizing has been widely used for nanostructural engineering, but the nanomorphology is limited to only two oxides: anodic barrier and porous oxides. Therefore, the discovery of an additional anodic oxide with a unique nanofeature would expand the applicability of anodizing. Here we demonstrate the fabrication of a third-generation anodic oxide, specifically, anodic alumina nanofibers, by anodizing in a new electrolyte, pyrophosphoric acid. Ultra-high density single nanometer-scale anodic alumina nanofibers (1010 nanofibers/cm2) consisting of an amorphous, pure aluminum oxide were successfully fabricated via pyrophosphoric acid anodizing. The nanomorphologies of the anodic nanofibers can be controlled by the electrochemical conditions. Anodic tungsten oxide nanofibers can also be fabricated by pyrophosphoric acid anodizing. The aluminum surface covered by the anodic alumina nanofibers exhibited ultra-fast superhydrophilic behavior, with a contact angle of less than 1°, within 1 second. Such ultra-narrow nanofibers can be used for various nanoapplications including catalysts, wettability control, and electronic devices.

  2. Cylindrical Three-Dimensional Porous Anodic Alumina Networks

    Directory of Open Access Journals (Sweden)

    Pedro M. Resende

    2016-11-01

    Full Text Available The synthesis of a conformal three-dimensional nanostructure based on porous anodic alumina with transversal nanopores on wires is herein presented. The resulting three-dimensional network exhibits the same nanostructure as that obtained on planar geometries, but with a macroscopic cylindrical geometry. The morphological analysis of the nanostructure revealed the effects of the initial defects on the aluminum surface and the mechanical strains on the integrity of the three-dimensional network. The results evidence the feasibility of obtaining 3D porous anodic alumina on non-planar aluminum substrates.

  3. Enhanced gas separation factors of microporous polymer constrained in the channels of anodic alumina membranes.

    Science.gov (United States)

    Chernova, Ekaterina; Petukhov, Dmitrii; Boytsova, Olga; Alentiev, Alexander; Budd, Peter; Yampolskii, Yuri; Eliseev, Andrei

    2016-08-08

    New composite membranes based on porous anodic alumina films and polymer of intrinsic microporosity (PIM-1) have been prepared using a spin-coating technique. According to scanning electron microscopy, partial penetration of polymer into the pores of alumina supports takes place giving rise to selective polymeric layers with fiber-like microstructure. Geometric confinement of rigid PIM-1 in the channels of anodic alumina causes reduction of small-scale mobility in polymeric chains. As a result, transport of permanent gases, such as CH4, becomes significantly hindered across composite membranes. Contrary, the transport of condensable gases (CO2, С4H10), did not significantly suffer from the confinement due to high solubility in the polymer matrix. This strategy enables enhancement of selectivity towards CO2 and C4H10 without significant loss of the membrane performance and seems to be prospective for drain and sweetening of natural gas.

  4. Fabrication of a novel aluminum surface covered by numerous high-aspect-ratio anodic alumina nanofibers

    OpenAIRE

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

    2015-01-01

    The formation behavior of anodic alumina nanofibers via anodizing in a concentrated pyrophosphoric acid under various conditions was investigated using electrochemical measurements and SEM/TEM observations. Pyrophosphoric acid anodizing at 293 K resulted in the formation of numerous anodic alumina nanofibers on an aluminum substrate through a thin barrier oxide and honeycomb oxide with narrow walls. However, long-term anodizing led to the chemical dissolution of the alumina nanofibers. The de...

  5. Structural Engineering of Nanoporous Anodic Alumina Photonic Crystals by Sawtooth-like Pulse Anodization.

    Science.gov (United States)

    Law, Cheryl Suwen; Santos, Abel; Nemati, Mahdieh; Losic, Dusan

    2016-06-01

    This study presents a sawtooth-like pulse anodization approach aiming to create a new type of photonic crystal structure based on nanoporous anodic alumina. This nanofabrication approach enables the engineering of the effective medium of nanoporous anodic alumina in a sawtooth-like manner with precision. The manipulation of various anodization parameters such as anodization period, anodization amplitude, number of anodization pulses, ramp ratio and pore widening time allows a precise control and fine-tuning of the optical properties (i.e., characteristic transmission peaks and interferometric colors) exhibited by nanoporous anodic alumina photonic crystals (NAA-PCs). The effect of these anodization parameters on the photonic properties of NAA-PCs is systematically evaluated for the establishment of a fabrication methodology toward NAA-PCs with tunable optical properties. The effective medium of the resulting NAA-PCs is demonstrated to be optimal for the development of optical sensing platforms in combination with reflectometric interference spectroscopy (RIfS). This application is demonstrated by monitoring in real-time the formation of monolayers of thiol molecules (11-mercaptoundecanoic acid) on the surface of gold-coated NAA-PCs. The obtained results reveal that the adsorption mechanism between thiol molecules and gold-coated NAA-PCs follows a Langmuir isotherm model, indicating a monolayer sorption mechanism.

  6. Growth of porous anodized alumina on the sputtered aluminum films with 2D-3D morphology for high specific surface area

    Science.gov (United States)

    Liao, M. W.; Chung, C. K.

    2014-08-01

    The porous anodic aluminum oxide (AAO) with high-aspect-ratio pore channels is widely used as a template for fabricating nanowires or other one-dimensional (1D) nanostructures. The high specific surface area of AAO can also be applied to the super capacitor and the supporting substrate for catalysis. The rough surface could be helpful to enhance specific surface area but it generally results in electrical field concentration even to ruin AAO. In this article, the aluminum (Al) films with the varied 2D-3D morphology on Si substrates were prepared using magnetron sputtering at a power of 50 W-185 W for 1 h at a working pressure of 2.5 × 10-1 Pa. Then, AAO was fabricated from the different Al films by means of one-step hybrid pulse anodizing (HPA) between the positive 40 V and the negative -2 V (1 s:1 s) for 3 min in 0.3 M oxalic acid at a room temperature. The microstructure and morphology of Al films were characterized by X-ray diffraction, scanning electron microscope and atomic force microscope, respectively. Some hillocks formed at the high target power could be attributed to the grain texture growth in the normal orientation of Al(1 1 1). The 3D porous AAO structure which is different from the conventional 2D planar one has been successfully demonstrated using HPA on the film with greatly rough hillock-surface formed at the highest power of 185 W. It offers a potential application of the new 3D AAO to high specific surface area devices.

  7. Growth of porous anodized alumina on the sputtered aluminum films with 2D–3D morphology for high specific surface area

    Energy Technology Data Exchange (ETDEWEB)

    Liao, M.W.; Chung, C.K., E-mail: ckchung@mail.ncku.edu.tw

    2014-08-01

    The porous anodic aluminum oxide (AAO) with high-aspect-ratio pore channels is widely used as a template for fabricating nanowires or other one-dimensional (1D) nanostructures. The high specific surface area of AAO can also be applied to the super capacitor and the supporting substrate for catalysis. The rough surface could be helpful to enhance specific surface area but it generally results in electrical field concentration even to ruin AAO. In this article, the aluminum (Al) films with the varied 2D–3D morphology on Si substrates were prepared using magnetron sputtering at a power of 50 W–185 W for 1 h at a working pressure of 2.5 × 10⁻¹ Pa. Then, AAO was fabricated from the different Al films by means of one-step hybrid pulse anodizing (HPA) between the positive 40 V and the negative -2 V (1 s:1 s) for 3 min in 0.3 M oxalic acid at a room temperature. The microstructure and morphology of Al films were characterized by X-ray diffraction, scanning electron microscope and atomic force microscope, respectively. Some hillocks formed at the high target power could be attributed to the grain texture growth in the normal orientation of Al(1 1 1). The 3D porous AAO structure which is different from the conventional 2D planar one has been successfully demonstrated using HPA on the film with greatly rough hillock-surface formed at the highest power of 185 W. It offers a potential application of the new 3D AAO to high specific surface area devices.

  8. Effects of current density and electrolyte temperature on the volume expansion factor of anodic alumina formed in oxalic acid

    International Nuclear Information System (INIS)

    Zhou, F.; Baron-Wiecheć, A.; Garcia-Vergara, S.J.; Curioni, M.; Habazaki, H.; Skeldon, P.; Thompson, G.E.

    2012-01-01

    The formation of porous anodic alumina in 0.4 M oxalic acid is investigated over a range of current density and electrolyte temperature using sputtering-deposited substrates containing tungsten tracer layers. The findings reveal volume expansion factors and efficiencies of film growth that increase with the increase of the current density and decrease of the temperature. Pore generation by the flow of the anodic alumina in the barrier layer toward the pore walls is proposed to dominate at relatively high current densities (above ∼2 mA cm −2 ), with tungsten tracer species being retained within films. Conversely, losses of tungsten species occur at lower current densities, possibly due to increased field-assisted ejection of Al 3+ ions and/or field-assisted dissolution of the anodic alumina.

  9. Understanding focused ion beam guided anodic alumina nanopore development

    International Nuclear Information System (INIS)

    Chen Bo; Lu, Kathy; Tian Zhipeng

    2011-01-01

    Graphical abstract: Display Omitted Highlights: → We study the effect of FIB patterning on pore evolution during anodization. → FIB patterned concaves with 1.5 nm depth can effectively guide nanopore growth. → The edge effect of FIB guided patterns causes nanopores to bend. → Anodization window is enlarged to 50-80 V for 150 nm interpore distance hexagonal arrays. - Abstract: Focused ion beam (FIB) patterning in combination with anodization has shown great promise in creating unique pore patterns. This work is aimed to understand the effect of the FIB patterned sites in guiding anodized pore development. Highly ordered porous anodic alumina has been created with the guidance of FIB created patterns on electropolished aluminum followed by oxalic acid anodization. Shallow concaves created by the FIB with only 1.5 nm depth can effectively guide the growth of ordered nanopore patterns. With the guidance of the FIB pattern, the anodization rate is much faster and the nanopore growth direction bends at the boundary of the FIB patterned and un-patterned regions. FIB patterning also enlarges the anodization window; ordered nanopore arrays with 150 nm interpore distances can be produced under an applied potential from 50 V to 80 V. The fundamental understanding of these unique processes is discussed.

  10. Advanced morphological analysis of patterns of thin anodic porous alumina

    Energy Technology Data Exchange (ETDEWEB)

    Toccafondi, C. [Istituto Italiano di Tecnologia, Department of Nanophysics, Via Morego 30, Genova I 16163 (Italy); Istituto Italiano di Tecnologia, Department of Nanostructures, Via Morego 30, Genova I 16163 (Italy); Stępniowski, W.J. [Department of Advanced Materials and Technologies, Faculty of Advanced Technologies and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Leoncini, M. [Istituto Italiano di Tecnologia, Department of Nanostructures, Via Morego 30, Genova I 16163 (Italy); Salerno, M., E-mail: marco.salerno@iit.it [Istituto Italiano di Tecnologia, Department of Nanophysics, Via Morego 30, Genova I 16163 (Italy)

    2014-08-15

    Different conditions of fabrication of thin anodic porous alumina on glass substrates have been explored, obtaining two sets of samples with varying pore density and porosity, respectively. The patterns of pores have been imaged by high resolution scanning electron microscopy and analyzed by innovative methods. The regularity ratio has been extracted from radial profiles of the fast Fourier transforms of the images. Additionally, the Minkowski measures have been calculated. It was first observed that the regularity ratio averaged across all directions is properly corrected by the coefficient previously determined in the literature. Furthermore, the angularly averaged regularity ratio for the thin porous alumina made during short single-step anodizations is lower than that of hexagonal patterns of pores as for thick porous alumina from aluminum electropolishing and two-step anodization. Therefore, the regularity ratio represents a reliable measure of pattern order. At the same time, the lower angular spread of the regularity ratio shows that disordered porous alumina is more isotropic. Within each set, when changing either pore density or porosity, both regularity and isotropy remain rather constant, showing consistent fabrication quality of the experimental patterns. Minor deviations are tentatively discussed with the aid of the Minkowski measures, and the slight decrease in both regularity and isotropy for the final data-points of the porosity set is ascribed to excess pore opening and consequent pore merging. - Highlights: • Thin porous alumina is partly self-ordered and pattern analysis is required. • Regularity ratio is often misused: we fix the averaging and consider its spread. • We also apply the mathematical tool of Minkowski measures, new in this field. • Regularity ratio shows pattern isotropy and Minkowski helps in assessment. • General agreement with perfect artificial patterns confirms the good manufacturing.

  11. Pore development in anodic alumina in sulphuric acid and borax electrolytes

    International Nuclear Information System (INIS)

    Garcia-Vergara, S.J.; Skeldon, P.; Thompson, G.E.; Habakaki, H.

    2007-01-01

    The formation of porous anodic films on an Al-3.5 at.%W alloy is compared in sulphuric acid and borax electrolytes in order to investigate pore development processes. The findings disclose that for anodizing in sulphuric acid, the pores develop mainly due to the influences of field-induced plasticity of the film and growth stresses; in borax, field-assisted dissolution dominates. The films formed in sulphuric acid are consequently much thicker than the layer of oxidized alloy and tungsten species are retained in the film. In contrast, with borax, the films and oxidized alloy layers are of similar thickness and tungsten species are lost to the electrolyte. Efficiencies of film growth are also significantly different, about 65% in sulphuric acid and about 52% in borax. The retention of tungsten species during anodizing in sulphuric acid is due to the localization of tungsten in the inner regions of the barrier layer and cell walls, with a layer of anodic alumina separating the tungsten-containing regions from the electrolyte. For borax, the tungsten is distributed more uniformly through the film material, enabling loss of tungsten species to the electrolyte from the pore base

  12. Role of metal ion impurities in generation of oxygen gas within anodic alumina

    Energy Technology Data Exchange (ETDEWEB)

    Shimizu, K. [Keio Univ., Yokohama (Japan). Chemical Lab.; Habazaki, H. [Hokkaido Univ., Sapporo (Japan). Graduate School of Engineering; Skeldon, P.; Thompson, G.E.; Wood, G.C. [University of Manchester Inst. of Science and Technology (United Kingdom). Corrosion and Protection Centre

    2002-07-01

    The generation of oxygen gas within an amorphous anodic alumina film is reported. The film was formed by anodizing aluminum, which was first electropolished and then chemically polished in CrO{sub 3}-H{sub 3}PO{sub 4} solution, in sodium tungstate electrolyte. The procedure results in incorporation of mobile Cr{sup 3+} species, from the chemical polishing film, and mobile W{sup 6+} species, from the electrolyte, into the amorphous structure. The tungsten species are present in the outer 27% of the film thickness, while Cr{sup 6+} species occupy a thin layer within the tungsten-containing region. Above the Cr{sup 3+} containing layer, a band develops that contains oxygen bubbles of a few nanometres size. The oxygen is generated by oxidation of O{sup 2-} ions of the alumina. A mechanism of oxygen generation within the alumina is proposed based on the electronic band structure of the oxide, modified by the Cr{sup 3+} and W{sup 6+} species, and on the ionic transport processes during oxide growth. (author)

  13. Fabrication of a novel aluminum surface covered by numerous high-aspect-ratio anodic alumina nanofibers

    Science.gov (United States)

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

    2015-11-01

    The formation behavior of anodic alumina nanofibers via anodizing in a concentrated pyrophosphoric acid under various conditions was investigated using electrochemical measurements and SEM/TEM observations. Pyrophosphoric acid anodizing at 293 K resulted in the formation of numerous anodic alumina nanofibers on an aluminum substrate through a thin barrier oxide and honeycomb oxide with narrow walls. However, long-term anodizing led to the chemical dissolution of the alumina nanofibers. The density of the anodic alumina nanofibers decreased as the applied voltage increased in the 10-75 V range. However, active electrochemical dissolution of the aluminum substrate occurred at a higher voltage of 90 V. Low temperature anodizing at 273 K resulted in the formation of long alumina nanofibers measuring several micrometers in length, even though a long processing time was required due to the low current density during the low temperature anodizing. In contrast, high temperature anodizing easily resulted in the formation and chemical dissolution of alumina nanofibers. The structural nanofeatures of the anodic alumina nanofibers were controlled by choosing of the appropriate electrochemical conditions, and numerous high-aspect-ratio alumina nanofibers (>100) can be successfully fabricated. The anodic alumina nanofibers consisted of a pure amorphous aluminum oxide without anions from the employed electrolyte.

  14. Nanocarbon-Coated Porous Anodic Alumina for Bionic Devices

    Directory of Open Access Journals (Sweden)

    Morteza Aramesh

    2015-08-01

    Full Text Available A highly-stable and biocompatible nanoporous electrode is demonstrated herein. The electrode is based on a porous anodic alumina which is conformally coated with an ultra-thin layer of diamond-like carbon. The nanocarbon coating plays an essential role for the chemical stability and biocompatibility of the electrodes; thus, the coated electrodes are ideally suited for biomedical applications. The corrosion resistance of the proposed electrodes was tested under extreme chemical conditions, such as in boiling acidic/alkali environments. The nanostructured morphology and the surface chemistry of the electrodes were maintained after wet/dry chemical corrosion tests. The non-cytotoxicity of the electrodes was tested by standard toxicity tests using mouse fibroblasts and cortical neurons. Furthermore, the cell–electrode interaction of cortical neurons with nanocarbon coated nanoporous anodic alumina was studied in vitro. Cortical neurons were found to attach and spread to the nanocarbon coated electrodes without using additional biomolecules, whilst no cell attachment was observed on the surface of the bare anodic alumina. Neurite growth appeared to be sensitive to nanotopographical features of the electrodes. The proposed electrodes show a great promise for practical applications such as retinal prostheses and bionic implants in general.

  15. Contact angle studies on anodic porous alumina.

    Science.gov (United States)

    Redón, Rocío; Vázquez-Olmos, A; Mata-Zamora, M E; Ordóñez-Medrano, A; Rivera-Torres, F; Saniger, J M

    2005-07-15

    The preparation of nanostructures using porous anodic aluminum oxide (AAO) as templates involves the introduction of dissolved materials into the pores of the membranes; one way to determine which materials are preferred to fill the pores involves the measurement of the contact angles (theta) of different solvents or test liquids on the AAOs. Thus, we present measurements of contact angles of nine solvents on four different AAO sheets by tensiometric and goniometric methods. From the solvents tested, we found dimethyl sulfoxide (DMSO) and N,N(')-dimethylformamide (DMF) to interact with the AAOs, the polarity of the solvents and the surfaces being the driving force.

  16. Iron migration from the anode surface in alumina electrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Zhuravleva, Elena N.; Drozdova, Tatiana N.; Ponomareva, Svetlana V. [Siberian Federal University, Krasnoyarsk, 660041 (Russian Federation); Kirik, Sergei D., E-mail: kiriksd@yandex.ru [Siberian Federal University, Krasnoyarsk, 660041 (Russian Federation); Institute of Chemistry and Chemical Technology SB RAS, Krasnoyarsk, 660036 (Russian Federation)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer Corrosion destruction of two-component iron-based alloys in high-temperature aluminum electrolysis in the cryolite alumina melt has been studied. Black-Right-Pointing-Pointer It was found that at the first stage oxidative polarization of iron atoms on the anode surface into Fe{sup 2+} takes place. Black-Right-Pointing-Pointer Fe{sup 2+} interacts with cryolite melt producing FeF{sub 2}. Black-Right-Pointing-Pointer FeF{sub 2} gives oxides FeAl{sub 2}O{sub 4}, Fe{sub 3}O{sub 4}, Fe{sub 2}O{sub 3}. Black-Right-Pointing-Pointer The participation of oxygen in the corrosion has not been observed. - Abstract: Corrosion destruction of two-component iron-based alloys used as an anode in high-temperature alumina electrolysis in the melt of NaF/KF/AlF{sub 3} electrolyte has been considered. Ni, Si, Cu, Cr, Mn, Al, Ti in the amount of up to 10% have been tested as the dopants to an anode alloys. The composition of the corrosion products has been studied using X-ray diffraction, scanning electron microscopy and electron microprobe analysis. It has been established that the anode corrosion is induced by a surface electrochemical polarization and iron atom oxidation. Iron ions come into an exchange interaction with the fluoride components of the melted electrolyte, producing FeF{sub 2}. The last interacts with oxyfluoride species transforming into the oxide forms: FeAl{sub 2}O{sub 4}, Fe{sub 3}O{sub 4}, Fe{sub 2}O{sub 3}. Due to the low solubility, the iron oxides are accumulated in the near-electrode sheath. The only small part of iron from anode migrates to cathode that makes an production of high purity aluminum of a real task. The alloy dopants are also subjected to corrosion in accordance with electromotive series resulting corrosion tunnels on the anode surface. The oxides are final compounds which collect in the same area. The corrosion products form an anode shell which is electronic conductor at electrolysis temperature. The

  17. Niobium oxide nanocolumns formed via anodic alumina with modulated pore diameters

    Science.gov (United States)

    Pligovka, A.; Zakhlebayeva, A.; Lazavenka, A.

    2018-03-01

    Niobium oxide nanocolumns with modulated diameters were formed for the first time. An Al/Nb bilayer specimen was prepared by successive sputter-deposition of 300 nm niobium layer and 1200 nm aluminum layer onto silicon wafer. Regular anodic alumina matrix with modulated pore diameters was formed by sequential anodization of initial specimen in tartaric acid at 180 V, and in oxalic acid at 37 V. Further potentiodynamic reanodization of the specimen up to 400 V causes the simultaneous growth of 440 nm continuous niobium oxide layer beneath the alumina film and two types of an array of oxide nanocolumns (thick – with 100 nm width and 630 nm high and thin – with 25 nm width and 170 nm high), which are the filling of the alumina pores. The morphology of the formed anodic niobium oxide nanocolumns with modulated diameters was determined by field emission scanning electron microscopy. The formed nanostructures can be used for perspective devices of nano- and optoelectronics such as photonic crystals.

  18. Nanostructural characterization of large-scale porous alumina fabricated via anodizing in arsenic acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Akiya, Shunta; Kikuchi, Tatsuya, E-mail: kiku@eng.hokudai.ac.jp; Natsui, Shungo; Suzuki, Ryosuke O.

    2017-05-01

    Highlights: • Anodic porous alumina was formed in an arsenic acid solution. • Potential difference (voltage) anodizing at 340 V was achieved. • The porous alumina was slightly ordered under the appropriate conditions. • Pore sealing behavior was not observed in boiling distilled water. • The porous alumina exhibits a white photoluminescence emission under UV irradiation. - Abstract: Anodizing of aluminum in an arsenic acid solution is reported for the fabrication of anodic porous alumina. The highest potential difference (voltage) without oxide burning increased as the temperature and the concentration of the arsenic acid solution decreased, and a high anodizing potential difference of 340 V was achieved. An ordered porous alumina with several tens of cells was formed in 0.1–0.5 M arsenic acid solutions at 310–340 V for 20 h. However, the regularity of the porous alumina was not improved via anodizing for 72 h. No pore sealing behavior of the porous alumina was observed upon immersion in boiling distilled water, and it may be due to the formation of an insoluble complex on the oxide surface. The porous alumina consisted of two different layers: a hexagonal alumina layer that contained arsenic from the electrolyte and a pure alumina honeycomb skeleton. The porous alumina exhibited a white photoluminescence emission at approximately 515 nm under UV irradiation at 254 nm.

  19. Ellipsometry of anodic film growth

    Energy Technology Data Exchange (ETDEWEB)

    Smith, C.G.

    1978-08-01

    An automated computer interpretation of ellisometer measurements of anodic film growth was developed. Continuous mass and charge balances were used to utilize more fully the time dependence of the ellipsometer data and the current and potential measurements. A multiple-film model was used to characterize the growth of films which proceeds via a dissolution--precipitation mechanism; the model also applies to film growth by adsorption and nucleation mechanisms. The characteristic parameters for film growth describe homogeneous and heterogeneous crystallization rates, film porosities and degree of hydration, and the supersaturation of ionic species in the electrolyte. Additional descriptions which may be chosen are patchwise film formation, nonstoichiometry of the anodic film, and statistical variations in the size and orientation of secondary crystals. Theories were developed to describe the optical effects of these processes. An automatic, self-compensating ellipsometer was used to study the growth in alkaline solution of anodic films on silver, cadmium, and zinc. Mass-transport conditions included stagnant electrolyte and forced convection in a flow channel. Multiple films were needed to characterize the optical properties of these films. Anodic films grew from an electrolyte supersatuated in the solution-phase dissolution product. The degree of supersaturation depended on transport conditions and had a major effect on the structure of the film. Anodic reaction rates were limited by the transport of charge carriers through a primary surface layer. The primary layers on silver, zinc, and cadmium all appeared to be nonstoichiometric, containing excess metal. Diffusion coefficients, transference numbers, and the free energy of adsorption of zinc oxide were derived from ellipsometer measurements. 97 figures, 13 tables, 198 references.

  20. Vertical single- and double-walled carbon nanotubes grown from modified porous anodic alumina templates

    International Nuclear Information System (INIS)

    Maschmann, Matthew R; Franklin, Aaron D; Amama, Placidus B; Zakharov, Dmitri N; Stach, Eric A; Sands, Timothy D; Fisher, Timothy S

    2006-01-01

    Vertical single-walled and double-walled carbon nanotube (SWNT and DWNT) arrays have been grown using a catalyst embedded within the pore walls of a porous anodic alumina (PAA) template. The initial film structure consisted of a SiO x adhesion layer, a Ti layer, a bottom Al layer, a Fe layer, and a top Al layer deposited on a Si wafer. The Al and Fe layers were subsequently anodized to create a vertically oriented pore structure through the film stack. CNTs were synthesized from the catalyst layer by plasma-enhanced chemical vapour deposition (PECVD). The resulting structure is expected to form the basis for development of vertically oriented CNT-based electronics and sensors

  1. Optical properties of alumina membranes prepared by anodic oxidation process

    International Nuclear Information System (INIS)

    Li Zhaojian; Huang Kelong

    2007-01-01

    The luminescence property of anodic alumina membranes (AAMs) with ordered nanopore arrays prepared by electrochemically anodizing aluminum in oxalic acid solutions have been investigated. Photoluminescence emission (PL) measurement shows that a blue PL band occurs in the wavelength ranges of 300-600 nm. The PL intensity and peak position of AAMs depend markedly on the excitation wavelength. A new peak located at 518 nm can be observed under a monitoring wavelength at 429 nm in the photoluminescence excitation (PLE) spectra. Convincing evidences have been presented that the PLE would be associated with the residual aluminum ions in the membrane. The PLE and PL of AAMs, as a function of anodizing times, have been discussed. It is found that the oxalic impurities incorporated in the AAMs would have important influences on the optical properties of AAMs in the initial stage of anodization. The PL and PLE spectra obtained show that there are three optical centers, of which the first is originated from the F + centers in AAMs, the second is correlated with the oxalic impurities incorporated in the AAMs, and the third is associated with the excess aluminum ions in the membrane

  2. Optical properties of alumina membranes prepared by anodic oxidation process

    Energy Technology Data Exchange (ETDEWEB)

    Li Zhaojian [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China)], E-mail: lizhaojian_lzj@hotmail.com; Huang Kelong [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China)], E-mail: klhuang@mail.csu.edu.cn

    2007-12-15

    The luminescence property of anodic alumina membranes (AAMs) with ordered nanopore arrays prepared by electrochemically anodizing aluminum in oxalic acid solutions have been investigated. Photoluminescence emission (PL) measurement shows that a blue PL band occurs in the wavelength ranges of 300-600 nm. The PL intensity and peak position of AAMs depend markedly on the excitation wavelength. A new peak located at 518 nm can be observed under a monitoring wavelength at 429 nm in the photoluminescence excitation (PLE) spectra. Convincing evidences have been presented that the PLE would be associated with the residual aluminum ions in the membrane. The PLE and PL of AAMs, as a function of anodizing times, have been discussed. It is found that the oxalic impurities incorporated in the AAMs would have important influences on the optical properties of AAMs in the initial stage of anodization. The PL and PLE spectra obtained show that there are three optical centers, of which the first is originated from the F{sup +} centers in AAMs, the second is correlated with the oxalic impurities incorporated in the AAMs, and the third is associated with the excess aluminum ions in the membrane.

  3. Understanding improved osteoblast behavior on select nanoporous anodic alumina

    Science.gov (United States)

    Ni, Siyu; Li, Changyan; Ni, Shirong; Chen, Ting; Webster, Thomas J

    2014-01-01

    The aim of this study was to prepare different sized porous anodic alumina (PAA) and examine preosteoblast (MC3T3-E1) attachment and proliferation on such nanoporous surfaces. In this study, PAA with tunable pore sizes (25 nm, 50 nm, and 75 nm) were fabricated by a two-step anodizing procedure in oxalic acid. The surface morphology and elemental composition of PAA were characterized by field emission scanning electron microscopy and X-ray photoelectron spectroscopy analysis. The nanopore arrays on all of the PAA samples were highly regular. X-ray photoelectron spectroscopy analysis suggested that the chemistry of PAA and flat aluminum surfaces were similar. However, contact angles were significantly greater on all of the PAA compared to flat aluminum substrates, which consequently altered protein adsorption profiles. The attachment and proliferation of preosteoblasts were determined for up to 7 days in culture using field emission scanning electron microscopy and a Cell Counting Kit-8. Results showed that nanoporous surfaces did not enhance initial preosteoblast attachment, whereas preosteoblast proliferation dramatically increased when the PAA pore size was either 50 nm or 75 nm compared to all other samples (Paluminum by modifying surface nano-roughness alone (and not changing chemistry) through an anodization process to improve osteoblast density, and, thus, should be further studied as a bioactive interface for orthopedic applications. PMID:25045263

  4. Study the effect of striping in two-step anodizing process on pore arrangement of nano-porous alumina

    International Nuclear Information System (INIS)

    Rahimi, M.H.; Saramad, S.; Tabaian, S.H.; Marashi, S.P.; Zolfaghari, A.; Mohammadalinezhad, M.

    2009-01-01

    Two-step anodic oxidation of aluminum is generally employed to produce the ordered porous anodized alumina (PAA). Dissolving away (striping) the oxide film after the first anodizing step plays a key role in the final arrangement of nano-pores. In this work, different striping durations between 1 and 6 h were applied to the sample that was initially anodized at a constant voltage of 40 V at 17 deg. C for 15 h. The striping duration of 3 h was realized as the optimum time for achieving the best ordering degree for the pores. Scanning electron microscopy (SEM) was used during and at the end of the process to examine the cross section and finishing surface of the specimens. Linear-angular fast Fourier transform (LA-FFT), an in-house technique based on MATLAB software, was employed to assess the ordering degree of the anodized samples.

  5. Study the effect of striping in two-step anodizing process on pore arrangement of nano-porous alumina

    Energy Technology Data Exchange (ETDEWEB)

    Rahimi, M.H. [Department of Mining and Metallurgical Engineering, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Saramad, S., E-mail: ssaramad@aut.ac.ir [Department of Physics, Amirkabir University of Technology, Hafez Avenue, Tehran (Iran, Islamic Republic of); Tabaian, S.H.; Marashi, S.P. [Department of Mining and Metallurgical Engineering, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Zolfaghari, A. [Chemistry and Chemical Engineering Research Centre of Iran, Tehran (Iran, Islamic Republic of); Mohammadalinezhad, M. [Department of Mining and Metallurgical Engineering, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of)

    2009-10-15

    Two-step anodic oxidation of aluminum is generally employed to produce the ordered porous anodized alumina (PAA). Dissolving away (striping) the oxide film after the first anodizing step plays a key role in the final arrangement of nano-pores. In this work, different striping durations between 1 and 6 h were applied to the sample that was initially anodized at a constant voltage of 40 V at 17 deg. C for 15 h. The striping duration of 3 h was realized as the optimum time for achieving the best ordering degree for the pores. Scanning electron microscopy (SEM) was used during and at the end of the process to examine the cross section and finishing surface of the specimens. Linear-angular fast Fourier transform (LA-FFT), an in-house technique based on MATLAB software, was employed to assess the ordering degree of the anodized samples.

  6. Study the effect of striping in two-step anodizing process on pore arrangement of nano-porous alumina

    Science.gov (United States)

    Rahimi, M. H.; Saramad, S.; Tabaian, S. H.; Marashi, S. P.; Zolfaghari, A.; Mohammadalinezhad, M.

    2009-10-01

    Two-step anodic oxidation of aluminum is generally employed to produce the ordered porous anodized alumina (PAA). Dissolving away (striping) the oxide film after the first anodizing step plays a key role in the final arrangement of nano-pores. In this work, different striping durations between 1 and 6 h were applied to the sample that was initially anodized at a constant voltage of 40 V at 17 °C for 15 h. The striping duration of 3 h was realized as the optimum time for achieving the best ordering degree for the pores. Scanning electron microscopy (SEM) was used during and at the end of the process to examine the cross section and finishing surface of the specimens. Linear-angular fast Fourier transform (LA-FFT), an in-house technique based on MATLAB software, was employed to assess the ordering degree of the anodized samples.

  7. Effects of a magnetic field on growth of porous alumina films on aluminum

    Energy Technology Data Exchange (ETDEWEB)

    Ispas, Adriana; Bund, Andreas [Technische Universitaet Dresden, Physikalische Chemie und Elektrochemie, 01062 Dresden (Germany); Vrublevsky, Igor, E-mail: vrublevsky@bsuir.edu.b [Belarusian State University of Informatics and Radioelectronics Minsk, Department of Micro and Nanoelectronics, 220013 Minsk (Belarus)

    2010-05-01

    The effects induced by a magnetic field on the oxide film growth on aluminum in sulfuric, oxalic, phosphoric and sulfamic acid, and on current transients during re-anodizing of porous alumina films in the barrier-type electrolyte, were studied. Aluminum films of 100 nm thickness were prepared by thermal evaporation on Si wafer substrates. We could show that the duration of the anodizing process increased by 33% during anodizing in sulfuric acid when a magnetic field was applied (0.7 T), compared to the process without a magnetic field. Interestingly, such a magnetic field effect was not found during anodizing in oxalic and sulfamic acid. The pore intervals were decreased by ca. 17% in oxalic acid. These findings were attributed to variations in electronic properties of the anodic oxide films formed in various electrolytes and interpreted on the basis of the influence of trapped electrons on the mobility of ions migrating during the film growth. The spin dependent tunneling of electrons into the surface layer of the oxide under the magnetic field could be responsible for the shifts of the current transients to lower potentials during re-anodizing of heat-treated oxalic and phosphoric acid alumina films.

  8. Nanoporous Anodic Alumina: A Versatile Platform for Optical Biosensors

    Directory of Open Access Journals (Sweden)

    Abel Santos

    2014-05-01

    Full Text Available Nanoporous anodic alumina (NAA has become one of the most promising nanomaterials in optical biosensing as a result of its unique physical and chemical properties. Many studies have demonstrated the outstanding capabilities of NAA for developing optical biosensors in combination with different optical techniques. These results reveal that NAA is a promising alternative to other widely explored nanoporous platforms, such as porous silicon. This review is aimed at reporting on the recent advances and current stage of development of NAA-based optical biosensing devices. The different optical detection techniques, principles and concepts are described in detail along with relevant examples of optical biosensing devices using NAA sensing platforms. Furthermore, we summarise the performance of these devices and provide a future perspective on this promising research field.

  9. Mirror-finished superhydrophobic aluminum surfaces modified by anodic alumina nanofibers and self-assembled monolayers

    Science.gov (United States)

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2018-05-01

    We demonstrate mirror-finished superhydrophobic aluminum surfaces fabricated via the formation of anodic alumina nanofibers and subsequent modification with self-assembled monolayers (SAMs). High-density anodic alumina nanofibers were formed on the aluminum surface via anodizing in a pyrophosphoric acid solution. The alumina nanofibers became tangled and bundled by further anodizing at low temperature because of their own weight, and the aluminum surface was completely covered by the long falling nanofibers. The nanofiber-covered aluminum surface exhibited superhydrophilic behavior, with a contact angle measuring less than 10°. As the nanofiber-covered aluminum surface was modified with n-alkylphosphonic acid SAMs, the water contact angle drastically shifted to superhydrophobicity, measuring more than 150°. The contact angle increased with the applied voltage during pyrophosphoric acid anodizing, the anodizing time, and the number of carbon atoms contained in the SAM molecules modified on the alumina nanofibers. By optimizing the anodizing and SAM-modification conditions, superhydrophobic behavior could be achieved with only a brief pyrophosphoric acid anodizing period of 3 min and subsequent simple immersion in SAM solutions. The superhydrophobic aluminum surface exhibited a high reflectance, measuring approximately 99% across most of the visible spectrum, similar to that of an electropolished aluminum surface. Therefore, our mirror-finished superhydrophobic aluminum surface based on anodic alumina nanofibers and SAMs can be used as a reflective mirror in various optical applications such as concentrated solar power systems.

  10. Characterization of the microporous HDPE film with alpha alumina

    International Nuclear Information System (INIS)

    Park, Jong Seok; Sung, Hae Jun; Gwon, Hui Jeong; Lim, Youn Mook; Nho, Young Chang

    2010-01-01

    The effects of the addition of the alpha alumina on the properties of the microporous high density polyethylene (HDPE) films were investigated. The particle size and the specific surface area of alpha alumina were 400 nm and 7.3 m 2 g -1 . The HDPE and the alpha alumina were mixed to obtain the precursor film in the twin extruder. The precursor films were uni-axially stretched up to 600% in oven 120 .deg. C and then the stretched HDPE films were irradiated by gamma rays. The pore volume of the microporous HDPE films was increased with an increasing content of the alpha alumina. The mechanical characteristics of the microporous HDPE films were increased with a content of alpha alumina up to 15%, but decreased at 20%. The electrochemical stability of the microporous HDPE film containing alpha alumia was increased with an increased irradiation dose up ti 50 kGy

  11. Surface study of nano-template anodic porous alumina pre-irradiated by ArF laser

    International Nuclear Information System (INIS)

    Jaleh, B.; Saramad, S.; Farshchi-Tabrizi, M.

    2009-01-01

    Nano-porous alumina membranes have widely used as matrix for the fabrication of nanomaterials for many applications including quantum-dot arrays, magnetic storage devices and composites for catalysis, due to their remarkable hardness, thermal and anti corrupted stability, uniform pore size and high pore density. In this experiment three sets of aluminum samples were chosen for fabrication nano-porous anodic alumina. One set has select for laser cleaning before chemical treatment and the two others with and without chemical treatment without laser irradiation. Anodic aluminum oxide (AAO) films were characterized with Scanning Electron Microscope (SEM) and Atomic Force Microscope (AFM) micrograph and the SEM results were analyzed by Linear-Angular Fast Fourier Transform (LA-FFT) technique to investigate the arrangement and ordering of pores. According to these results the laser irradiated sample has much better regularity in comparison with the usual one.

  12. Modelling the growth process of porous aluminum oxide film during anodization

    International Nuclear Information System (INIS)

    Aryslanova, E M; Alfimov, A V; Chivilikhin, S A

    2015-01-01

    Currently it has become important for the development of metamaterials and nanotechnology to obtain regular self-assembled structures. One such structure is porous anodic alumina film that consists of hexagonally packed cylindrical pores. In this work we consider the anodization process, our model takes into account the influence of layers of aluminum and electrolyte on the rate of growth of aluminum oxide, as well as the effect of surface diffusion. In present work we consider those effects. And as a result of our model we obtain the minimum distance between centers of alumina pores in the beginning of anodizing process. (paper)

  13. Modelling the growth process of porous aluminum oxide film during anodization

    Science.gov (United States)

    Aryslanova, E. M.; Alfimov, A. V.; Chivilikhin, S. A.

    2015-11-01

    Currently it has become important for the development of metamaterials and nanotechnology to obtain regular self-assembled structures. One such structure is porous anodic alumina film that consists of hexagonally packed cylindrical pores. In this work we consider the anodization process, our model takes into account the influence of layers of aluminum and electrolyte on the rate of growth of aluminum oxide, as well as the effect of surface diffusion. In present work we consider those effects. And as a result of our model we obtain the minimum distance between centers of alumina pores in the beginning of anodizing process.

  14. Photoluminescent properties of nanoporous anodic alumina doped with manganese ions

    Energy Technology Data Exchange (ETDEWEB)

    Gasenkova, I.V. [State Research and Production Association ' Optic, Optoelectronic and Laser techniques”, 68 Nezavisimosti Ave., Minsk 220072 (Belarus); Mukhurov, N.I., E-mail: n.mukhurov@ifanbel.bas-net.by [State Research and Production Association ' Optic, Optoelectronic and Laser techniques”, 68 Nezavisimosti Ave., Minsk 220072 (Belarus); Zhvavyi, S.P.; Kolesnik, E.E. [State Research and Production Association ' Optic, Optoelectronic and Laser techniques”, 68 Nezavisimosti Ave., Minsk 220072 (Belarus); Stupak, A.P. [B.I.Stepanov Institute of Physics of the National Academy of Sciences of Belarus, 68 Nezavisimosti Ave., Minsk 220072 (Belarus)

    2017-05-15

    The results are presented of a comparative study of photoluminescent (PL) properties of unalloyed and Mn-alloyed porous anodic alumina (PAA) subjected to annealing at temperatures in the range of ГђВў{sub a}=200–1300 °ГђВЎ. The possibility of alloying of PAA with metal atoms is illustrated through an example of Mn atoms, and the effect of this impurity on the optical properties of aluminum oxide is examined. Alloying of PAA with Mn ions leads to the formation of complex defects including manganese ions and oxygen vacancies. The difference observed in the spectral dependences of the PL intensity of alloyed and unalloyed specimens is explained by the change in the valence of manganese ions in the complex defects. A decrease has been discovered in the PL intensity of the PL bands and R-lines of Mn and Cr ions in the α-phase under prolonged UV-exposure of the alloyed samples.

  15. Ultrafast excited state deactivation of doped porous anodic alumina membranes

    International Nuclear Information System (INIS)

    Makhal, Abhinandan; Sarkar, Soumik; Pal, Samir Kumar; Yan, Hongdan; Wulferding, Dirk; Cetin, Fatih; Lemmens, Peter

    2012-01-01

    Free-standing, bi-directionally permeable and ultra-thin anodic aluminum oxide (AAO) membranes establish attractive templates (host) for the synthesis of nano-dots and rods of various materials (guest). This is due to their chemical and structural integrity and high periodicity on length scales of 5–150 nm which are often used to host photoactive nano-materials for various device applications including dye-sensitized solar cells. In the present study, AAO membranes are synthesized by using electrochemical methods and a detailed structural characterization using FEG-SEM, XRD and TGA confirms the porosity and purity of the material. Defect-mediated photoluminescence quenching of the porous AAO membrane in the presence of an electron accepting guest organic molecule (benzoquinone) is studied by means of steady-state and picosecond/femtosecond-resolved luminescence measurements. Using time-resolved luminescence transients, we have also revealed light harvesting of complexes of porous alumina impregnated with inorganic quantum dots (Maple Red) or gold nanowires. Both the Förster resonance energy transfer and the nano-surface energy transfer techniques are employed to examine the observed quenching behavior as a function of the characteristic donor–acceptor distances. The experimental results will find their relevance in light harvesting devices based on AAOs combined with other materials involving a decisive energy/charge transfer dynamics. (paper)

  16. Ultrafast excited state deactivation of doped porous anodic alumina membranes

    Science.gov (United States)

    Makhal, Abhinandan; Sarkar, Soumik; Pal, Samir Kumar; Yan, Hongdan; Wulferding, Dirk; Cetin, Fatih; Lemmens, Peter

    2012-08-01

    Free-standing, bi-directionally permeable and ultra-thin anodic aluminum oxide (AAO) membranes establish attractive templates (host) for the synthesis of nano-dots and rods of various materials (guest). This is due to their chemical and structural integrity and high periodicity on length scales of 5-150 nm which are often used to host photoactive nano-materials for various device applications including dye-sensitized solar cells. In the present study, AAO membranes are synthesized by using electrochemical methods and a detailed structural characterization using FEG-SEM, XRD and TGA confirms the porosity and purity of the material. Defect-mediated photoluminescence quenching of the porous AAO membrane in the presence of an electron accepting guest organic molecule (benzoquinone) is studied by means of steady-state and picosecond/femtosecond-resolved luminescence measurements. Using time-resolved luminescence transients, we have also revealed light harvesting of complexes of porous alumina impregnated with inorganic quantum dots (Maple Red) or gold nanowires. Both the Förster resonance energy transfer and the nano-surface energy transfer techniques are employed to examine the observed quenching behavior as a function of the characteristic donor-acceptor distances. The experimental results will find their relevance in light harvesting devices based on AAOs combined with other materials involving a decisive energy/charge transfer dynamics.

  17. Ultrafast excited state deactivation of doped porous anodic alumina membranes

    Energy Technology Data Exchange (ETDEWEB)

    Makhal, Abhinandan; Sarkar, Soumik; Pal, Samir Kumar [Department of Chemical, Biological and Macromolecular Sciences, S N Bose National Centre for Basic Sciences, Block JD, Sector III, Salt Lake, Kolkata 700 098 (India); Yan, Hongdan; Wulferding, Dirk; Cetin, Fatih; Lemmens, Peter [Institute for Condensed Matter Physics, TU Braunschweig, Mendelssohnstrasse 3, 38106 Braunschweig (Germany)

    2012-08-03

    Free-standing, bi-directionally permeable and ultra-thin anodic aluminum oxide (AAO) membranes establish attractive templates (host) for the synthesis of nano-dots and rods of various materials (guest). This is due to their chemical and structural integrity and high periodicity on length scales of 5-150 nm which are often used to host photoactive nano-materials for various device applications including dye-sensitized solar cells. In the present study, AAO membranes are synthesized by using electrochemical methods and a detailed structural characterization using FEG-SEM, XRD and TGA confirms the porosity and purity of the material. Defect-mediated photoluminescence quenching of the porous AAO membrane in the presence of an electron accepting guest organic molecule (benzoquinone) is studied by means of steady-state and picosecond/femtosecond-resolved luminescence measurements. Using time-resolved luminescence transients, we have also revealed light harvesting of complexes of porous alumina impregnated with inorganic quantum dots (Maple Red) or gold nanowires. Both the Foerster resonance energy transfer and the nano-surface energy transfer techniques are employed to examine the observed quenching behavior as a function of the characteristic donor-acceptor distances. The experimental results will find their relevance in light harvesting devices based on AAOs combined with other materials involving a decisive energy/charge transfer dynamics. (paper)

  18. Understanding improved osteoblast behavior on select nanoporous anodic alumina

    Directory of Open Access Journals (Sweden)

    Ni S

    2014-07-01

    Full Text Available Siyu Ni,1 Changyan Li,1 Shirong Ni,2 Ting Chen,1 Thomas J Webster3,4 1College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai, People’s Republic of China; 2Department of Pathophysiology, Wenzhou Medical University, Wenzhou, People’s Republic of China; 3Department of Chemical Engineering, College of Engineering, Northeastern University, Boston, MA, USA; 4Center of Excellence for Advanced Materials Research, King Abdulaziz University, Jeddah, Saudi Arabia Abstract: The aim of this study was to prepare different sized porous anodic alumina (PAA and examine preosteoblast (MC3T3-E1 attachment and proliferation on such nanoporous surfaces. In this study, PAA with tunable pore sizes (25 nm, 50 nm, and 75 nm were fabricated by a two-step anodizing procedure in oxalic acid. The surface morphology and elemental composition of PAA were characterized by field emission scanning electron microscopy and X-ray photoelectron spectroscopy analysis. The nanopore arrays on all of the PAA samples were highly regular. X-ray photoelectron spectroscopy analysis suggested that the chemistry of PAA and flat aluminum surfaces were similar. However, contact angles were significantly greater on all of the PAA compared to flat aluminum substrates, which consequently altered protein adsorption profiles. The attachment and proliferation of preosteoblasts were determined for up to 7 days in culture using field emission scanning electron microscopy and a Cell Counting Kit-8. Results showed that nanoporous surfaces did not enhance initial preosteoblast attachment, whereas preosteoblast proliferation dramatically increased when the PAA pore size was either 50 nm or 75 nm compared to all other samples (P<0.05. Thus, this study showed that one can alter surface energy of aluminum by modifying surface nano-roughness alone (and not changing chemistry through an anodization process to improve osteoblast density, and, thus, should be

  19. Effect of Aluminum Purity on the Pore Formation of Porous Anodic Alumina

    International Nuclear Information System (INIS)

    Kim, Byeol; Lee, Jin Seok

    2014-01-01

    Anodic alumina oxide (AAO), a self-ordered hexagonal array, has various applications in nanofabrication such as the fabrication of nanotemplates and other nanostructures. In order to obtain highly ordered porous alumina membranes, a two-step anodization or prepatterning of aluminum are mainly conducted with straight electric field. Electric field is the main driving force for pore growth during anodization. However, impurities in aluminum can disturb the direction of the electric field. To confirm this, we anodized two different aluminum foil samples with high purity (99.999%) and relatively low purity (99.8%), and compared the differences in the surface morphologies of the respective aluminum oxide membranes produced in different electric fields. Branched pores observed in porous alumina surface which was anodized in low-purity aluminum and the size; dimensions of the pores were found to be usually smaller than those obtained from high-purity aluminum. Moreover, anodization at high voltage proceeds to a significant level of conversion because of the high speed of the directional electric field. Consequently, anodic alumina membrane of a specific morphology, i. e., meshed pore, was produced

  20. Effect of Aluminum Purity on the Pore Formation of Porous Anodic Alumina

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Byeol; Lee, Jin Seok [Sookmyung Women' s Univ., Seoul (Korea, Republic of)

    2014-02-15

    Anodic alumina oxide (AAO), a self-ordered hexagonal array, has various applications in nanofabrication such as the fabrication of nanotemplates and other nanostructures. In order to obtain highly ordered porous alumina membranes, a two-step anodization or prepatterning of aluminum are mainly conducted with straight electric field. Electric field is the main driving force for pore growth during anodization. However, impurities in aluminum can disturb the direction of the electric field. To confirm this, we anodized two different aluminum foil samples with high purity (99.999%) and relatively low purity (99.8%), and compared the differences in the surface morphologies of the respective aluminum oxide membranes produced in different electric fields. Branched pores observed in porous alumina surface which was anodized in low-purity aluminum and the size; dimensions of the pores were found to be usually smaller than those obtained from high-purity aluminum. Moreover, anodization at high voltage proceeds to a significant level of conversion because of the high speed of the directional electric field. Consequently, anodic alumina membrane of a specific morphology, i. e., meshed pore, was produced.

  1. Synthesis of highly ordered nanopores on alumina by two-step anodization process

    Energy Technology Data Exchange (ETDEWEB)

    Bwana, Nicholas N. [University of Oxford, Department of Engineering Science (United Kingdom)], E-mail: Nicholas.Bwana@eng.ox.ac.uk

    2008-02-15

    Highly ordered anodic alumina was produced, on RF sputtered aluminium on a conductive glass substrate, by two step anodizing process in 0.4 M sulphuric acid at constant cell potentials of between 5 and 25 V and at a constant current density of 20 mA cm{sup -2}. The temperature was kept constant at 15 deg. C during both anodization processes. The effects of the anodizing potential, current density, and time on the pore diameters were established. Longer anodization periods result in wider irregular pores with reduced porosity for both constant potential and constant current density anodization processes. The current density increases with increasing constant anodizing potential and generally remains constant with time after a sharp rise. Potential drop during constant current density anodization behaves in a similar manner. We confirm that sulphuric acid has a self-ordering potential of 25 V above which burning occurs.

  2. Matrix coatings based on anodic alumina with carbon nanostructures in the pores

    Science.gov (United States)

    Gorokh, G. G.; Pashechko, M. I.; Borc, J. T.; Lozovenko, A. A.; Kashko, I. A.; Latos, A. I.

    2018-03-01

    The nanoporous anodic alumina matrixes thickness of 1.5 mm and pore sizes of 45, 90 and 145 nm were formed on Si substrates. The tubular carbon nanostructures were synthesized into the matrixes pores by pyrolysis of fluid hydrocarbon xylene with 1% ferrocene. The structure and composition of the matrix coatings were examined by scanning electron microscopy, Auger analysis and Raman spectroscopy. The carbon nanostructures completely filled the pores of templates and uniformly covered the tops. The structure of carbon nanostructures corresponded to the structure of multiwall carbon nanotubes. Investigations of mechanical and tribological properties of nanostructured oxide-carbon composite performed by scratching and nanoindentation showed nonlinear dependencies of the frictional force, penetration depth of the cantilever, hardness and plane strain modulus on the load. It was found that the microhardness of the samples increases with reduced of alumina pore diameter, and the penetration depth of the cantilever into the film grows with carbon nanostructures size. The results showed the high mechanical strength of nanostructured oxide-carbon composite.

  3. Gas adsorption and capillary condensation in nanoporous alumina films

    Energy Technology Data Exchange (ETDEWEB)

    Casanova, Felix; Chiang, Casey E; Li, Chang-Peng; Roshchin, Igor V; Schuller, Ivan K [Physics Department, University of California-San Diego, La Jolla, CA 92093 (United States); Ruminski, Anne M; Sailor, Michael J [Department of Chemistry and Biochemistry, University of California-San Diego, La Jolla, CA 92093 (United States)], E-mail: casanova@physics.ucsd.edu

    2008-08-06

    Gas adsorption and capillary condensation of organic vapors are studied by optical interferometry, using anodized nanoporous alumina films with controlled geometry (cylindrical pores with diameters in the range of 10-60 nm). The optical response of the film is optimized with respect to the geometric parameters of the pores, for potential performance as a gas sensor device. The average thickness of the adsorbed film at low relative pressures is not affected by the pore size. Capillary evaporation of the liquid from the nanopores occurs at the liquid-vapor equilibrium described by the classical Kelvin equation with a hemispherical meniscus. Due to the almost complete wetting, we can quantitatively describe the condensation for isopropanol using the Cohan model with a cylindrical meniscus in the Kelvin equation. This model describes the observed hysteresis and allows us to use the adsorption branch of the isotherm to calculate the pore size distribution of the sample in good agreement with independent structural measurements. The condensation for toluene lacks reproducibility due to incomplete surface wetting. This exemplifies the relevant role of the fluid-solid (van der Waals) interactions in the hysteretic behavior of capillary condensation.

  4. Gas adsorption and capillary condensation in nanoporous alumina films

    International Nuclear Information System (INIS)

    Casanova, Felix; Chiang, Casey E; Li, Chang-Peng; Roshchin, Igor V; Schuller, Ivan K; Ruminski, Anne M; Sailor, Michael J

    2008-01-01

    Gas adsorption and capillary condensation of organic vapors are studied by optical interferometry, using anodized nanoporous alumina films with controlled geometry (cylindrical pores with diameters in the range of 10-60 nm). The optical response of the film is optimized with respect to the geometric parameters of the pores, for potential performance as a gas sensor device. The average thickness of the adsorbed film at low relative pressures is not affected by the pore size. Capillary evaporation of the liquid from the nanopores occurs at the liquid-vapor equilibrium described by the classical Kelvin equation with a hemispherical meniscus. Due to the almost complete wetting, we can quantitatively describe the condensation for isopropanol using the Cohan model with a cylindrical meniscus in the Kelvin equation. This model describes the observed hysteresis and allows us to use the adsorption branch of the isotherm to calculate the pore size distribution of the sample in good agreement with independent structural measurements. The condensation for toluene lacks reproducibility due to incomplete surface wetting. This exemplifies the relevant role of the fluid-solid (van der Waals) interactions in the hysteretic behavior of capillary condensation

  5. Gas adsorption and capillary condensation in nanoporous alumina films.

    Science.gov (United States)

    Casanova, Fèlix; Chiang, Casey E; Li, Chang-Peng; Roshchin, Igor V; Ruminski, Anne M; Sailor, Michael J; Schuller, Ivan K

    2008-08-06

    Gas adsorption and capillary condensation of organic vapors are studied by optical interferometry, using anodized nanoporous alumina films with controlled geometry (cylindrical pores with diameters in the range of 10-60 nm). The optical response of the film is optimized with respect to the geometric parameters of the pores, for potential performance as a gas sensor device. The average thickness of the adsorbed film at low relative pressures is not affected by the pore size. Capillary evaporation of the liquid from the nanopores occurs at the liquid-vapor equilibrium described by the classical Kelvin equation with a hemispherical meniscus. Due to the almost complete wetting, we can quantitatively describe the condensation for isopropanol using the Cohan model with a cylindrical meniscus in the Kelvin equation. This model describes the observed hysteresis and allows us to use the adsorption branch of the isotherm to calculate the pore size distribution of the sample in good agreement with independent structural measurements. The condensation for toluene lacks reproducibility due to incomplete surface wetting. This exemplifies the relevant role of the fluid-solid (van der Waals) interactions in the hysteretic behavior of capillary condensation.

  6. Nanoporous hard data: optical encoding of information within nanoporous anodic alumina photonic crystals.

    Science.gov (United States)

    Santos, Abel; Law, Cheryl Suwen; Pereira, Taj; Losic, Dusan

    2016-04-21

    Herein, we present a method for storing binary data within the spectral signature of nanoporous anodic alumina photonic crystals. A rationally designed multi-sinusoidal anodisation approach makes it possible to engineer the photonic stop band of nanoporous anodic alumina with precision. As a result, the transmission spectrum of these photonic nanostructures can be engineered to feature well-resolved and selectively positioned characteristic peaks across the UV-visible spectrum. Using this property, we implement an 8-bit binary code and assess the versatility and capability of this system by a series of experiments aiming to encode different information within the nanoporous anodic alumina photonic crystals. The obtained results reveal that the proposed nanosized platform is robust, chemically stable, versatile and has a set of unique properties for data storage, opening new opportunities for developing advanced nanophotonic tools for a wide range of applications, including sensing, photonic tagging, self-reporting drug releasing systems and secure encoding of information.

  7. Mechanical stability of heat-treated nanoporous anodic alumina subjected to repetitive mechanical deformation

    Science.gov (United States)

    Bankova, A.; Videkov, V.; Tzaneva, B.; Mitov, M.

    2018-03-01

    We report studies on the mechanical response and deformation behavior of heat-treated nanoporous anodic alumina using a micro-balance test and experimental test equipment especially designed for this purpose. AAO samples were characterized mechanically by a three-point bending test using a micro-analytical balance. The deformation behavior was studied by repetitive mechanical bending of the AAO membranes using an electronically controlled system. The nanoporous AAO structures were prepared electrochemically from Al sheet substrates using a two-step anodizing technique in oxalic acid followed by heat treatment at 700 °C in air. The morphological study of the aluminum oxide layer after the mechanical tests and mechanical deformation was conducted using scanning electron and optical microscopy, respectively. The experimental results showed that the techniques proposed are simple and accurate; they could, therefore, be combined to constitute a method for mechanical stability assessment of nanostructured AAO films, which are important structural components in the design of MEMS devices and sensors.

  8. Effect of Manganese Content on the Fabrication of Porous Anodic Alumina

    Directory of Open Access Journals (Sweden)

    C. H. Voon

    2012-01-01

    Full Text Available The influence of manganese content on the formation of well-ordered porous anodic alumina was studied. Porous anodic alumina has been produced on aluminium substrate of different manganese content by single-step anodizing at 50 V in 0.3 M oxalic acid at 15°C for 60 minutes. The well-ordered pore and cell structure was revealed by subjecting the porous anodic alumina to oxide dissolution treatment in a mixture of chromic acid and phosphoric acid. It was found that the manganese content above 1 wt% impaired the regularity of the cell and pore structure significantly, which can be attributed to the presence of secondary phases in the starting material with manganese content above 1 wt%. The pore diameter and interpore distance decreased with the addition of manganese into the substrates. The time variation of current density and the thickness of porous anodic alumina also decreased as a function of the manganese content in the substrates.

  9. Density control of electrodeposited Ni nanoparticles/nanowires inside porous anodic alumina templates by an exponential anodization voltage decrease.

    Science.gov (United States)

    Marquardt, B; Eude, L; Gowtham, M; Cho, G; Jeong, H J; Châtelet, M; Cojocaru, C S; Kim, B S; Pribat, D

    2008-10-08

    Porous alumina templates have been fabricated by applying an exponential voltage decrease at the end of the anodization process. The time constant η of the exponential voltage function has been used to control the average thickness and the thickness distribution of the barrier layer at the bottom of the pores of the alumina structure. Depending on the η value, the thickness distribution of the barrier layer can be made very uniform or highly scattered, which allows us to subsequently fine tune the electrodeposition yield of nickel nanoparticles/nanowires at low voltage. As an illustration, the pore filling percentage with Ni has been varied, in a totally reproducible manner, between ∼3 and 100%. Combined with the ability to vary the pore diameter and repetition step over ∼2 orders of magnitude (by varying the anodization voltage and electrolyte type), the control of the pore filling percentage with metal particles/nanowires could bring novel approaches for the organization of nano-objects.

  10. Rapid fabrication of self-ordered porous alumina with 10-/sub-10-nm-scale nanostructures by selenic acid anodizing

    Science.gov (United States)

    Nishinaga, Osamu; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2013-01-01

    Anodic porous alumina has been widely investigated and used as a nanostructure template in various nanoapplications. The porous structure consists of numerous hexagonal cells perpendicular to the aluminum substrate and each cell has several tens or hundreds of nanoscale pores at its center. Because the nanomorphology of anodic porous alumina is limited by the electrolyte during anodizing, the discovery of additional electrolytes would expand the applicability of porous alumina. In this study, we report a new self-ordered nanoporous alumina formed by selenic acid (H2SeO4) anodizing. By optimizing the anodizing conditions, anodic alumina possessing 10-nm-scale pores was rapidly assembled (within 1 h) during selenic acid anodizing without any special electrochemical equipment. Novel sub-10-nm-scale spacing can also be achieved by selenic acid anodizing and metal sputter deposition. Our new nanoporous alumina can be used as a nanotemplate for various nanostructures in 10-/sub-10-nm-scale manufacturing. PMID:24067318

  11. Highly ordered porous alumina with tailor-made pore structures fabricated by pulse anodization

    International Nuclear Information System (INIS)

    Lee, Woo; Kim, Jae-Cheon

    2010-01-01

    A new anodization method for the preparation of nanoporous anodic aluminum oxide (AAO) with pattern-addressed pore structure was developed. The approach is based on pulse anodization of aluminum employing a series of potential waves that consist of two or more different pulses with designated periods and amplitudes, and provides unique tailoring capability of the internal pore structure of anodic alumina. Pores of the resulting AAOs exhibit a high degree of directional coherency along the pore axes without branching, and thus are suitable for fabricating novel nanowires or nanotubes, whose diameter modulation patterns are predefined by the internal pore geometry of AAO. It is found from microscopic analysis on pulse anodized AAOs that the effective electric field strength at the pore base is a key controlling parameter, governing not only the size of pores, but also the detailed geometry of the barrier oxide layer.

  12. Growth of anodic films on niobium

    International Nuclear Information System (INIS)

    Gomes, M.A.B.; Bulhoes, L.O.S.

    1988-01-01

    The analysis of the response of the galvanostatic growth of anodic films on niobium metal in aqueous solutions is shown. The first spark voltage showed a dependence upon value of current density that could be explained as the incorporation of anions into the film. (M.J.C.) [pt

  13. ORDERED POROUS ANODIC ALUMINUM OXIDE FILMS MADE BY TWO-STEP ANODIZATION

    OpenAIRE

    HANSONG XUE; HUAJI LI; YU YI; HUIFANG HU

    2007-01-01

    Porous Anodic Aluminum Oxide (AAO) films were prepared by two-step anodizing in sulfuric and oxalic acid solutions and observed by transmission electron microscope (TEM) and X-ray diffraction. The results show that the form of AAO film is affected by the varieties and concentrations of electrolyte, anodizing voltage, and the anodizing time; the formation and evolution processes of the AAO film are relative with the anodizing voltage severely, and the appropriate voltage is helpful to the orde...

  14. Effect of heat treatment on the structure of incorporated oxalate species and photoluminescent properties of porous alumina films formed in oxalic acid

    Science.gov (United States)

    Vrublevsky, I.; Jagminas, A.; Hemeltjen, S.; Goedel, W. A.

    2008-09-01

    The present work focuses on the use of IR spectroscopy and photoluminescence spectral measurements for studying the treatment temperature effect on the compositional and luminescent properties of oxalic acid alumina films. In line with the recent researches we have also found that heat treatment of porous alumina films formed in oxalic acid leads to considerable changes in their photoluminescence properties: upon annealing the intensity of photoluminescence (PL) increases reaching a maximum at the temperature of around 500 °C and then decreases. IR spectra of as-grown and heat-treated films have proved that PL emission in the anodic alumina films is related with the state of 'structural' oxalate species incorporated in the oxide lattice. These results allowed us to conclude that PL behavior of oxalic acid alumina films can be explained through the concept of variations in the bonding molecular orbitals of incorporated oxalate species including σ- and π-bonds.

  15. Vertically aligned nanowires on flexible silicone using a supported alumina template prepared by pulsed anodization

    DEFF Research Database (Denmark)

    Mátéfi-Tempfli, Stefan; Mátéfi-Tempfli, M.

    2009-01-01

    Carpets of vertically aligned nanowires on flexible substrates are successfully realized by a template method. Applying special pulsed anodization conditions, defect-free nanoporous alumina structures supported on polydimethylsiloxane (PDMS), a flexible silicone elastomer, are created. By using...... this template with nanopores ending on a conducting underlayer, a high-density nanowire array can be simply grown by direct DCelectrodeposition on the top of the silicone rubber....

  16. Plasmonic properties of gold-coated nanoporous anodic alumina ...

    Indian Academy of Sciences (India)

    gold-coated NAA is strongly quenched due to the strong plasmonic coupling. Keywords. Plasmon ... When coated by a thin film of gold, these templates can support surface plasmon resonance. ... 2.2 Equipment for characterization. Surface ...

  17. Fabrication and Characterization of Magnetic Nanowires in Anodic Alumina

    Science.gov (United States)

    Xiao, Z. L.; Han, Y. R.; Wang, H. H.; Welp, U.; Kwok, W. K.; Crabtree, G. W.

    2002-03-01

    Magnetic nanowires (cobalt, iron and nickel) with diameters down to 20 nm have been fabricated by electrodeposition. Both commercial and home-made anodized aluminum oxide (AAO) membranes with nanochannel arrays were used as templates. The structure and magnetization hysteresis of the specimens with nanowires were investigated with scanning electron microscope (SEM) and superconducting quantum interference device (SQUID), respectively. Growth of nanowires with both aqueous and dimethylsulfoxide (DMSO) solutions was conducted and better quality nanowires were obtained with the organic DMSO solution. The influence of the diameter, the length and the separation of the nanochannels on the magnetization orientation was investigated in detail. Work supported by the US Department of Energy (DOE), BES-Materials Science, Contract No. W-31-109-ENG-38.

  18. Luminescence characteristics of nanoporous anodic alumina annealed at different temperatures

    Science.gov (United States)

    Ilin, D. O.; Vokhmintsev, A. S.; Weinstein, I. A.

    2016-09-01

    Anodic aluminum oxide (AAO) membranes with 100 µm thickness were synthesized in oxalic acid solution under constant current density. Grown samples were annealed in 500-1250 °C range for 5 h in air. Average pore diameter was evaluated using quantitative analysis of SEM images and appeared to be within 78-86 nm diapason. It was found there was a broad emission band in the 350-620 nm region of photoluminescence (PL) spectra in amorphous membranes which is attributed to F-type oxygen deficient centers or oxalic ions. It was shown that intensive red emission caused by Cr3+ (696 nm) and Mn4+ (680 nm) impurities dominates in PL of AAO samples with crystalline α- and δ-phases after annealing at 1100-1250 °C temperatures.

  19. Morphological evolution of porous nanostructures grown from a single isolated anodic alumina nanochannel

    Science.gov (United States)

    Chen, Shih-Yung; Chang, Hsuan-Hao; Lai, Ming-Yu; Liu, Chih-Yi; Wang, Yuh-Lin

    2011-09-01

    Porous anodic aluminum oxide (AAO) membranes have been widely used as templates for growing nanomaterials because of their ordered nanochannel arrays with high aspect ratio and uniform pore diameter. However, the intrinsic growth behavior of an individual AAO nanochannel has never been carefully studied for the lack of a means to fabricate a single isolated anodic alumina nanochannel (SIAAN). In this study, we develop a lithographic method for fabricating a SIAAN, which grows into a porous hemispherical structure with its pores exhibiting fascinating morphological evolution during anodization. We also discover that the mechanical stress affects the growth rate and pore morphology of AAO porous structures. This study helps reveal the growth mechanism of arrayed AAO nanochannels grown on a flat aluminum surface and provides insights to help pave the way to altering the geometry of nanochannels on AAO templates for the fabrication of advanced nanocomposite materials.

  20. Morphological evolution of porous nanostructures grown from a single isolated anodic alumina nanochannel

    International Nuclear Information System (INIS)

    Chen, Shih-Yung; Wang, Yuh-Lin; Chang, Hsuan-Hao; Lai, Ming-Yu; Liu, Chih-Yi

    2011-01-01

    Porous anodic aluminum oxide (AAO) membranes have been widely used as templates for growing nanomaterials because of their ordered nanochannel arrays with high aspect ratio and uniform pore diameter. However, the intrinsic growth behavior of an individual AAO nanochannel has never been carefully studied for the lack of a means to fabricate a single isolated anodic alumina nanochannel (SIAAN). In this study, we develop a lithographic method for fabricating a SIAAN, which grows into a porous hemispherical structure with its pores exhibiting fascinating morphological evolution during anodization. We also discover that the mechanical stress affects the growth rate and pore morphology of AAO porous structures. This study helps reveal the growth mechanism of arrayed AAO nanochannels grown on a flat aluminum surface and provides insights to help pave the way to altering the geometry of nanochannels on AAO templates for the fabrication of advanced nanocomposite materials.

  1. Morphology and transmittance of porous alumina on glass substrate

    Energy Technology Data Exchange (ETDEWEB)

    Guo Peitao, E-mail: guopeitao@hotmail.com [Wuhan University of Technology. Wuhan (China); Xia Zhilin [Wuhan University of Technology. Wuhan (China); Key Laboratory of Low Dimensional Materials and Application Technology, Xiangtan University, Ministry of Education, Xiangtan (China); Xue Yiyu [Wuhan University of Technology. Wuhan (China); Huang Caihua [China Three Gorges University, Yichang (China); Zhao Lixin [Wuhan University of Technology. Wuhan (China)

    2011-02-01

    The porous optical film has higher threshold of laser-induced damage than densified films, for the study of mechanism of laser-induced damage of porous optical film with ordered pore structure. Porous anodic alumina (PAA) film with high transmittance on glass substrate has been prepared. Aluminum film was deposited on glass substrate by means of resistance and electron beam heat (EBH) evaporation. Porous alumina was prepared in oxalic acid solution under different anodizing conditions. At normal incidence, the optical transmittance spectrum over 300-1000 nm spectra region was obtained by spectrophotometer. SEM was introduced to analysis the morphology of the porous alumina film. The pore aperture increased with the increase of anodizing voltage, which resulted in a rapid decrease of the pore concentration and the optical thickness of porous alumina film. Damage morphology of porous alumina film is found to be typically defects initiated, and the defect is the pore presented on the film.

  2. Liquid-film assisted formation of alumina/niobium interfaces

    OpenAIRE

    Sugar, Joshua D.; McKeown, Joseph T.; Marks, Robert A.; Glaeser, Andreas M.

    2002-01-01

    Alumina has been joined at 1400 degrees C using niobium-based interlayers. Two different joining approaches were compared: solid-state diffusion bonding using a niobium foil as an interlayer, and liquid-film assisted bonding using a multilayer copper/niobium/copper interlayer. In both cases, a 127-(mu)m thick niobium foil was used; =1.4-(mu)m or =3-(mu)m thick copper films flanked the niobium. Room-temperature four-point bend tests showed that the introduction of a copper film had a significa...

  3. Synthesis and photocatalytic properties of graphitic carbon nitride nanofibers using porous anodic alumina templates

    Science.gov (United States)

    Suchitra, S. M.; Udayashankar, N. K.

    2017-12-01

    In the present study, we describe an effective method for the synthesis of Graphitic carbon nitride (GCN) nanostructures using porous anodic alumina (AAO) membrane as template by simple thermal condensation of cyanamide. Synthesized nanostructure was fully analysed by various techniques to detect its crystalline nature, morphology, luminescent properties followed by the evaluation of its photocatalytic activity in the degradation of Methylene blue dye. Structural analysis of synthesized GCNNF was systematically carried out using x-ray powder diffraction (XRD) and scanning electron microscope (SEM), and. The results confirmed the growth of GCN inside the nanochannels of anodic alumina templates. Luminescent properties of GCNNF were studied using photoluminescence (PL) spectroscopy. PL analysis showed the presence of a strong emission peak in the wavelength range of 350-600 nm in blue region. GCNNF displays higher photocatalytic performance in the photodegradation of methylene blue compare to the bulk GCN. Highlights 1. In the present paper, we report the synthesis of graphitic carbon nitride nanofibers (GCNNF) using porous anodic aluminium oxide membranes as templates through thermal condensation of cyanamide at 500 °C. 2. The synthesis of Graphitic carbon nitride nanofibers using porous andic alumina template is the efficient approach for increasing crystallinity and surface area. 3. The high surface area of graphitic carbon nitride nanofibers has a good impact on novel optical and photocatalytic properties of the bulkGCN. 4. AAO templating of GCN is one of the versatile method to produce tailorable GCN nanostructures with higher surface area and less number of structural defects. 5. Towards photocatalytic degradation of dyes, the tuning of physical properties is very essential thing hence we are succeeded in achieving better catalytic performance of GCN nanostructures by making use of AAO templates.

  4. Fabrication of CdSe nanocrystals using porous anodic alumina and their optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Laatar, Fakher, E-mail: fakher8laatar@gmail.com [Laboratory of Semiconductors, Nanostructures and Advanced Technology (LSNTA), Center for Research and Technology Energy, Tourist Route Soliman, BP 95, 2050 Hammam-Lif (Tunisia); Science faculty of Bizerte–Carthage University (Tunisia); Hassen, Mohamed [Laboratory of Semiconductors, Nanostructures and Advanced Technology (LSNTA), Center for Research and Technology Energy, Tourist Route Soliman, BP 95, 2050 Hammam-Lif (Tunisia); Higher Institute of Applied Science and Technology of Sousse, City Taffala (Ibn Khaldun), 4003 Sousse (Tunisia); Amri, Chohdi [Laboratory of Semiconductors, Nanostructures and Advanced Technology (LSNTA), Center for Research and Technology Energy, Tourist Route Soliman, BP 95, 2050 Hammam-Lif (Tunisia); Laatar, Fekri [Laboratory of Physical Chemistry of Minerals and Materials Applications, National Research Center for Materials Science, Technopole Borj Cedria (Tunisia); Smida, Alia; Ezzaouia, Hatem [Laboratory of Semiconductors, Nanostructures and Advanced Technology (LSNTA), Center for Research and Technology Energy, Tourist Route Soliman, BP 95, 2050 Hammam-Lif (Tunisia)

    2016-10-15

    In this paper, Porous anodic alumina (PAA) template with highly ordered nanopores structure was synthesized on aluminum foils by two step anodization process. PAA template has hexagonal pores with average size between 30 and 180 nm. L-cysteine (L-Cys) functionalized cadmium selenide nanocrystals (CdSe NCs) were successfully embedded inside PAA layers by simple immersion in aqueous solution. The effect of pore diameter enlargement on the microstructure of CdSe NCs/PAA films was systematically studied by FE-SEM, XRD, EDX, Raman, UV–VIS absorbance and PL analysis. FE-SEM microscopy was used to investigate the surface morphology of PAA templates before and after CdSe NCs deposition. XRD investigation demonstrates that CdSe NCs into PAA templates were cubic in nature with zinc-blende structure. Raman measurements exhibit the characteristic modes of CdSe on the PAA layers as well as the films crystallinity as function of widening pores diameter. Optical properties of deposited CdSe NCs on PAA templates have been investigated using optical absorption and PL techniques. Photoluminescence spectroscopy has been used to determine the bandgap energy and the average size of CdSe NCs deposited on PAA layer. This method involves fitting the experimental spectra, using a model based on quantum confinement of electrons in CdSe nanocrystals having spherical and cylindrical forms (Quantum Dots (QDs) and Quantum Wires (QWs)). This model allows correlation between the PL spectra and the microstructure of the CdSe/PAA. Both photoluminescence and optical absorption show that the PL peak energy and the optical absorption edge of CdSe NCs/PAA exhibit similar behavior with changes in nanostructure size. The spectral behaviors of optical absorption and PL are consistent with a quantum confinement model throughout the sizes and shapes of the CdSe nanocrystals of the luminescent films. The effective bandgap energies determined from the PL peaks position are in good agreement with those

  5. Fabrication of CdSe nanocrystals using porous anodic alumina and their optical properties

    International Nuclear Information System (INIS)

    Laatar, Fakher; Hassen, Mohamed; Amri, Chohdi; Laatar, Fekri; Smida, Alia; Ezzaouia, Hatem

    2016-01-01

    In this paper, Porous anodic alumina (PAA) template with highly ordered nanopores structure was synthesized on aluminum foils by two step anodization process. PAA template has hexagonal pores with average size between 30 and 180 nm. L-cysteine (L-Cys) functionalized cadmium selenide nanocrystals (CdSe NCs) were successfully embedded inside PAA layers by simple immersion in aqueous solution. The effect of pore diameter enlargement on the microstructure of CdSe NCs/PAA films was systematically studied by FE-SEM, XRD, EDX, Raman, UV–VIS absorbance and PL analysis. FE-SEM microscopy was used to investigate the surface morphology of PAA templates before and after CdSe NCs deposition. XRD investigation demonstrates that CdSe NCs into PAA templates were cubic in nature with zinc-blende structure. Raman measurements exhibit the characteristic modes of CdSe on the PAA layers as well as the films crystallinity as function of widening pores diameter. Optical properties of deposited CdSe NCs on PAA templates have been investigated using optical absorption and PL techniques. Photoluminescence spectroscopy has been used to determine the bandgap energy and the average size of CdSe NCs deposited on PAA layer. This method involves fitting the experimental spectra, using a model based on quantum confinement of electrons in CdSe nanocrystals having spherical and cylindrical forms (Quantum Dots (QDs) and Quantum Wires (QWs)). This model allows correlation between the PL spectra and the microstructure of the CdSe/PAA. Both photoluminescence and optical absorption show that the PL peak energy and the optical absorption edge of CdSe NCs/PAA exhibit similar behavior with changes in nanostructure size. The spectral behaviors of optical absorption and PL are consistent with a quantum confinement model throughout the sizes and shapes of the CdSe nanocrystals of the luminescent films. The effective bandgap energies determined from the PL peaks position are in good agreement with those

  6. The effect of sulfuric acid on pore initiation in anodic alumina formed in oxalic acid

    Directory of Open Access Journals (Sweden)

    Behnam Hafezi

    2014-07-01

    Full Text Available In this work, a tracer study on pore initiation in anodic alumina in oxalic acid was performed. Effects of some experimental parameters such as applied electrical potential, electrolyte composition and heat pretreatment were evaluated. Electrochemical and morphological experiments were performed using potentiostatic anodizing and scanning electron microscopy (SEM techniques, respectively. Effect of electrolyte composition on current density was discussed. In various electrical potentials, electrolyte composition had different effects on current density. Addition of sulfuric acid into oxalic acid increased porosity. Also, distribution of pore size and pore diameter were influenced by presence of sulfuric acid. Effect of electrolyte composition on the morphology of aluminum surface layer depended on the electric potential. Current density and porosity of aluminum surface layer was decreased by heat pretreatment.

  7. Formation of self-ordered porous anodized alumina template for growing tungsten trioxide nanowires

    Science.gov (United States)

    Hussain, Tajamal; Shah, Asma Tufail; Shehzad, Khurram; Mujahid, Adnan; Farooqi, Zahoor Hussain; Raza, Muhammad Hamid; Ahmed, Mirza Nadeem; Nisa, Zaib Un

    2015-12-01

    Uniform porous anodized aluminum oxide (AAO) membrane has been synthesized by two-step anodization for fabricating tungsten trioxide (WO3) nanowires. Under assayed conditions, uniform porous structure of alumina (Al2O3) membrane with long range ordered hexagonal arrangements of nanopores was achieved. The self-assembled template possesses pores of internal diameter of 50 nm and interpore distance ( d int) of 80 nm with a thickness of about 80 µm, i.e., used for fabrication of nanostructures. WO3 nanowires have been fabricated by simple electroless deposition method inside Al2O3 nanopores. SEM images show tungsten trioxide nanowire with internal diameter of about 50 nm, similar to porous diameter of AAO template. XRD results showed that nanowires exist in cubic crystalline state with minor proportion of monoclinic phase.

  8. Effect of the local electric field on the formation of an ordered structure in porous anodic alumina

    Science.gov (United States)

    Lazarouk, S. K.; Katsuba, P. S.; Leshok, A. A.; Vysotskii, V. B.

    2015-09-01

    Experimental data and a model are presented, and the electric field that appears in porous alumina during electrochemical anodic oxidation of aluminum in electrolytes based on an aqueous solution of oxalic acid at a voltage of 90-250 V is calculated. It is found that the electric field in the layers with a porosity of 1-10% in growing alumina reaches 109-1010 V/m, which exceeds the electric strength of the material and causes microplasma patterns emitting visible light at the pore bottom, the self-organization of the structure of porous alumina, and the anisotropy of local porous anodizing. Moreover, other new effects are to be expected during aluminum anodizing under the conditions that ensure a high electric field inside the barrier layer of porous oxide.

  9. A novel vertical fan-out platform based on an array of curved anodic alumina nanochannels

    International Nuclear Information System (INIS)

    Liu, Chih-Yi; Lai, Ming-Yu; Tsai, Kun-Tong; Chang, Hsuan-Hao; Wang, Yuh-Lin; He, Jr-Hau; Shiue, Jessie

    2013-01-01

    Focused ion beam lithography and a two-step anodization have been combined to fabricate a vertical fan-out platform containing an array of unique probes. Each probe comprises three anodic alumina nanochannels with a fan-out arrangement. The lithography is used to pattern an aluminum sheet with a custom-designed array of triangular ‘cells’ whose apexes are composed of nanoholes. The nanoholes grow into straight nanochannels under proper voltage in the first-step anodization. The second step uses a doubled voltage to induce lateral repulsion among the nanochannels’ growth fronts originating in the same cell. Therefore, the fronts fan out. The repulsion roots in the inter-front distance being shorter than the naturally favoured length, which increases with anodization voltage. The fan-out evolution continues until the growth fronts originating in all the cells evolve into a close-packed two-dimensional hexagonal lattice whose spacing is identical to the favoured one. The chemical and physical mechanisms behind the fan-out fabrication are discussed. This novel fan-out platform facilitates probing and handling of many signals from different areas on a sample’s surface and is therefore promising for applications in detection and manipulation at the nanoscale level. (paper)

  10. EFFECT OF PHOSPHORIC ACID CONCENTRATION AND ANODIZING TIME ON THE PROPERTIES OF ANODIC FILMS ON TITANIUM

    Directory of Open Access Journals (Sweden)

    DIMAS L. TORRES

    2015-07-01

    Full Text Available In this study, it was investigated the influence of electrolyte concentration and anodizing time on the electrochemical behaviour and morphology of anodic films formed on commercially pure Ti. Electrochemical methods and surface analyses were used to characterize the films. It was found that the electrolyte concentration and anodizing time affect the growth and protective characteristics of films in a physiologic medium. It was possible to observe their non-uniformity on Ti substrates under the tested conditions. In potentiodynamic profiles, it was observed that passivation current values are affected by an anodizing time increase. Variations in impedance spectra were associated with an increase of defects within the film.

  11. An electrochemical investigation on the dissolution of bilayered porous anodic alumina

    International Nuclear Information System (INIS)

    Liao, Jinfu; Ling, Zhiyuan; Li, Yi; Hu, Xing

    2015-01-01

    Highlights: • Pulse polarization was introduced to investigate the dissolution of PAA. • Electric field within the bilayers was estimated. • The formation of the barrier layer involves mainly solid-state processes. • The structure should be the determining factor in the dissolution of the bilayers. - Abstract: Anodic alumina attracts much research interest in many disciplines for its versatility. Meanwhile, some aspects regarding its growth are still not well-understood, such as the formation and properties of its bilayer structure. In this paper, along with capacitance measurement, pulse polarization is introduced to study the dissolution of bilayered porous anodic alumina (PAA). Combined with electron microscope observation, the electric field in the outer layer is estimated to be slightly higher than that in the inner layer. By comparing with (oxy-)hydroxide layers, the electric field distribution within barrier layer of PAA confirms that the bilayers are compact and are formed mainly by solid-state ionic migration. The changes of dissolution rates after annealing and application of electric pulses suggest that structure may be a determining factor for the dissolution behaviors of the bilayers.

  12. Ion Transport in Organic Electrolyte Solution through the Pore Channels of Anodic Nanoporous Alumina Membranes

    International Nuclear Information System (INIS)

    Fukutsuka, Tomokazu; Koyamada, Kohei; Maruyama, Shohei; Miyazaki, Kohei; Abe, Takeshi

    2016-01-01

    Highlights: • Ion transport in organic electrolyte solution in macro- and meso-pores was focused. • Anodic nanoporous alumina membrane was used as a porous material. • The specific ion conductivities drastically decreased in macro- and meso-pores. - Abstract: For the development of high energy density lithium-ion batteries with the high rate performance, the enhancement of the ion transport in the electrolyte solutions impregnated in the porous electrodes is a key. To study the ion transport in porous electrodes, anodic nanoporous alumina (APA) self-standing membranes with macro- or meso-pores were used as model porous materials. These membranes had nearly spherical pore channels of discrete 20–68 nm in diameters. By using the geometric shape of the pores, we attempted to evaluate the specific ion conductivities of the organic electrolyte solution dissolving lithium salt simply. AC impedance spectroscopy measurement of a four-electrode cell with membranes showed one depressed semi-circle in the Nyquist plots and this semi-circle can be assigned as the ion transport resistance in the pores. The specific ion conductivities evaluated from the ion transport resistances and the geometric parameters showed very small values, even in the macro-pores, as compared with that of the bulk electrolyte solution.

  13. Fine tuning of optical signals in nanoporous anodic alumina photonic crystals by apodized sinusoidal pulse anodisation.

    Science.gov (United States)

    Santos, Abel; Law, Cheryl Suwen; Chin Lei, Dominique Wong; Pereira, Taj; Losic, Dusan

    2016-11-03

    In this study, we present an advanced nanofabrication approach to produce gradient-index photonic crystal structures based on nanoporous anodic alumina. An apodization strategy is for the first time applied to a sinusoidal pulse anodisation process in order to engineer the photonic stop band of nanoporous anodic alumina (NAA) in depth. Four apodization functions are explored, including linear positive, linear negative, logarithmic positive and logarithmic negative, with the aim of finely tuning the characteristic photonic stop band of these photonic crystal structures. We systematically analyse the effect of the amplitude difference (from 0.105 to 0.840 mA cm -2 ), the pore widening time (from 0 to 6 min), the anodisation period (from 650 to 950 s) and the anodisation time (from 15 to 30 h) on the quality and the position of the characteristic photonic stop band and the interferometric colour of these photonic crystal structures using the aforementioned apodization functions. Our results reveal that a logarithmic negative apodisation function is the most optimal approach to obtain unprecedented well-resolved and narrow photonic stop bands across the UV-visible-NIR spectrum of NAA-based gradient-index photonic crystals. Our study establishes a fully comprehensive rationale towards the development of unique NAA-based photonic crystal structures with finely engineered optical properties for advanced photonic devices such as ultra-sensitive optical sensors, selective optical filters and all-optical platforms for quantum computing.

  14. Investigating the effect of sputtering conditions on the physical properties of aluminum thin film and the resulting alumina template

    Science.gov (United States)

    Taheriniya, Shabnam; Parhizgar, Sara Sadat; Sari, Amir Hossein

    2018-06-01

    To study the alumina template pore size distribution as a function of Al thin film grain size distribution, porous alumina templates were prepared by anodizing sputtered aluminum thin films. To control the grain size the aluminum samples were sputtered with the rate of 0.5, 1 and 2 Å/s and the substrate temperature was either 25, 75 or 125 °C. All samples were anodized for 120 s in 1 M sulfuric acid solution kept at 1 °C while a 15 V potential was being applied. The standard deviation value for samples deposited at room temperature but with different rates is roughly 2 nm in both thin film and porous template form but it rises to approximately 4 nm with substrate temperature. Samples with the average grain size of 13, 14, 18.5 and 21 nm respectively produce alumina templates with an average pore size of 8.5, 10, 15 and 16 nm in that order which shows the average grain size limits the average pore diameter in the resulting template. Lateral correlation length and grain boundary effect are other factors that affect the pore formation process and pore size distribution by limiting the initial current density.

  15. Structural study of anodic films formed on aluminum in nitric acid electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Yakovleva, N.M.; Anicai, L.; Yakovlev, A.N.; Dima, L.; Khanina, E.Ya.; Buda, M.; Chupakhina, E.A

    2002-09-02

    The paper presents the results of investigations of porous Al anodic films formed in HNO{sub 3} electrolytes carried out by means of electrochemical techniques and X-ray diffraction as well as scanning electron microscopy (SEM). It was assumed that both electrochemical formation of a porous oxide and anodic dissolution of metal take place at Al/oxide interface at the same time. The analysis of short-range order (SRO) parameters for relatively high current density, 1x10{sup 3} A/m{sup 2}, and anodizing time, 10 min, leads to the conclusion that films mainly consist of amorphous alumina with {gamma}'-Al{sub 2}O{sub 3}-like SRO and a small amount ({approx}10%) of amorphous aluminum oxyhydroxide. SEM investigation of the films revealed strong dependence of the surface relief on different applied forming conditions. This marked change in the surface relief is discussed taking into account the relatively complex behavior of Al during anodization in HNO{sub 3} electrolytes, that involves both electrochemical growth and dissolution processes of anodic film associated with an electrochemical dissolution of aluminum substrate.

  16. Structural study of anodic films formed on aluminum in nitric acid electrolyte

    International Nuclear Information System (INIS)

    Yakovleva, N.M.; Anicai, L.; Yakovlev, A.N.; Dima, L.; Khanina, E.Ya.; Buda, M.; Chupakhina, E.A.

    2002-01-01

    The paper presents the results of investigations of porous Al anodic films formed in HNO 3 electrolytes carried out by means of electrochemical techniques and X-ray diffraction as well as scanning electron microscopy (SEM). It was assumed that both electrochemical formation of a porous oxide and anodic dissolution of metal take place at Al/oxide interface at the same time. The analysis of short-range order (SRO) parameters for relatively high current density, 1x10 3 A/m 2 , and anodizing time, 10 min, leads to the conclusion that films mainly consist of amorphous alumina with γ'-Al 2 O 3 -like SRO and a small amount (∼10%) of amorphous aluminum oxyhydroxide. SEM investigation of the films revealed strong dependence of the surface relief on different applied forming conditions. This marked change in the surface relief is discussed taking into account the relatively complex behavior of Al during anodization in HNO 3 electrolytes, that involves both electrochemical growth and dissolution processes of anodic film associated with an electrochemical dissolution of aluminum substrate

  17. Nanoporous alumina formed by self-organized two-step anodization of Ni3Al intermetallic alloy in citric acid

    International Nuclear Information System (INIS)

    Stępniowski, Wojciech J.; Cieślak, Grzegorz; Norek, Małgorzata; Karczewski, Krzysztof; Michalska-Domańska, Marta; Zasada, Dariusz; Polkowski, Wojciech; Jóźwik, Paweł; Bojar, Zbigniew

    2013-01-01

    Highlights: ► Anodic porous alumina was formed by Ni 3 Al intermetallic alloy anodization. ► The anodizations were conducted in 0.3 M citric acid. ► Nanopores geometry depends on anodizing voltage. ► No barrier layer was formed during anodization. - Abstract: Formation of the nanoporous alumina on the surface of Ni 3 Al intermetallic alloy has been studied in details and compared with anodization of aluminum. Successful self-organized anodization of this alloy was performed in 0.3 M citric acid at voltages ranging from 2.0 to 12.0 V using a typical two-electrode cell. Current density records revealed different mechanism of the porous oxide growth when compared to the mechanism pertinent for the anodization of aluminum. Electrochemical impedance spectroscopy experiments confirmed the differences in anodic oxide growth. Surface and cross-sections of the Ni 3 Al intermetallic alloy with anodic oxide were observed with field-emission scanning electron microscope and characterized with appropriate software. Nanoporous oxide growth rate was estimated from cross-sectional FE-SEM images. The lowest growth rate of 0.14 μm/h was found for the anodization at 0 °C and 2.0 V. The highest one – 2.29 μm/h – was noticed for 10.0 V and 30 °C. Pore diameter was ranging from 18.9 nm (2.0 V, 0 °C) to 32.0 nm (12.0 V, 0 °C). Interpore distance of the nanoporous alumina was ranging from 56.6 nm (2.0 V, 0 °C) to 177.9 nm (12.0 V, 30 °C). Pore density (number of pore occupying given area) was decreasing with anodizing voltage increase from 394.5 pores/μm 2 (2.0 V, 0 °C) to 94.9 pores/μm 2 (12.0 V, 0 °C). All the geometrical features of the anodic alumina formed by two-step self-organized anodization of Ni 3 Al intermetallic alloy are depending on the operating conditions.

  18. Two-Step Cycle for Producing Multiple Anodic Aluminum Oxide (AAO) Films with Increasing Long-Range Order.

    Science.gov (United States)

    Choudhary, Eric; Szalai, Veronika

    2016-01-01

    Nanoporous anodic aluminum oxide (AAO) membranes are being used for an increasing number of applications. However, the original two-step anodization method in which the first anodization is sacrificial to pre-pattern the second is still widely used to produce them. This method provides relatively low throughput and material utilization as half of the films are discarded. An alternative scheme that relies on alternating anodization and cathodic delamination is demonstrated that allows for the fabrication of several AAO films with only one sacrificial layer thus greatly improving total aluminum to alumina yield. The thickness for which the cathodic delamination performs best to yield full, unbroken AAO sheets is around 85 μm. Additionally, an image analysis method is used to quantify the degree of long-range ordering of the unit cells in the AAO films which was found to increase with each successive iteration of the fabrication cycle.

  19. Effects of Processing Temperatures of Nickel Plating on Capacitance Density of Alumina Film Capacitor.

    Science.gov (United States)

    Jeong, Myung-Sun; Ju, Byeong-Kwon; Lee, Jeon-Kook

    2015-06-01

    We observed the effects of nickel plating temperatures for controlling the surface morphologies of the deposited nickel layers on the alumina nano-pores. The alumina nano-channels were filled with nickel at various processing temperatures of 60-90 degrees C. The electrical properties of the alumina film capacitors were changed with processing temperatures. The electroless nickel plating (ENP) at 60 degrees C improved the nickel penetration into the alumina nano-channels due to the reduced reaction rate. Nickel layers are uniformly formed on the high aspect ratio alumina pores. Due to the uniform nickel electrode, the capacitance density of the alumina film capacitors is improved by the low leakage current, dissipation factor and equivalent series resistance. Alumina film capacitors made by ENP at 60 degrees C had a high capacitance density of 160 nF/cm2.

  20. Physical-mechanical and electrical properties of aluminium anodic films

    Energy Technology Data Exchange (ETDEWEB)

    Dima, L. [Research and Design Inst. for Electr. Eng., Bucharest (Romania); Anicai, L. [Research and Design Inst. for Electr. Eng., Bucharest (Romania)

    1995-11-01

    Mechanical, thermal and electrical properties of aluminium anodic films obtained by continuously anodization of Al wires of 4.5 mm diameter and Al sheets of 40 x 0.2 mm (Al min.99.5% purity), using an electrolyte based on oxalic acid, citric acid, boric acid, isopropilic alcohol, were investigated. The thickness of Al anodic oxide layers was 5 {+-} 1{mu}, 10 {+-} 1{mu}, for Al sheet, respectively 5 {+-} 1{mu}, 10 {+-} 1{mu}, 15 {+-} 1{mu}, for Al wire. To establish the influence of anodic film formation on mechanical parameters, measurements of breaking strength and relative elongation at break for anodized and non-anodized Al conductors, were made. In order to electrically characterize the anodic films, the breakdown voltage for different curvature radii of the conductor, between 50 - 12.5 mm, were measured. The influence of the layer thickness, as well as of the cracking during its bending, was established, too. To test the thermal resistance of the insulating anodic films, the Al conductors were subjected to 1 - 5 cyclic thermal shocks at 500 C. After the experimentals were done, it was found that Al anodic films of 5 {+-} 1{mu} may assure a breakdown voltage of minimum 200 V, for coils having a curvature radius greater than 12.5 mm and operating temperatures up to 500 C. From mechanical point of view, anodic oxide film determines a relatively reinforcing of Al conductor, but it doesn`t influence its functional properties. (orig.)

  1. Growth of anodic oxide films on oxygen-containing niobium

    Energy Technology Data Exchange (ETDEWEB)

    Habazaki, H. [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan)]. E-mail: habazaki@eng.hokudai.ac.jp; Ogasawara, T. [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Konno, H. [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Shimizu, K. [University Chemical Laboratory, Keio University, Yokohama 223-8522 (Japan); Asami, K. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Saito, K. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Nagata, S. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Skeldon, P. [Corrosion and Protection Centre, School of Materials, The University of Manchester, P.O. Box 88, Manchester M60 1QD (United Kingdom); Thompson, G.E. [Corrosion and Protection Centre, School of Materials, The University of Manchester, P.O. Box 88, Manchester M60 1QD (United Kingdom)

    2005-09-20

    The present study is directed at understanding of the influence of oxygen in the metal on anodic film growth on niobium, using sputter-deposited niobium containing from about 0-52 at.% oxygen, with anodizing carried out at high efficiency in phosphoric acid electrolyte. The findings reveal amorphous anodic niobia films, with no significant effect of oxygen on the field strength, transport numbers, mobility of impurity species and capacitance. However, since niobium is partially oxidized due to presence of oxygen in the substrate, less charge is required to form the films, hence reducing the time to reach a particular film thickness and anodizing voltage. Further, the relative thickness of film material formed at the metal/film interface is increased by the incorporation of oxygen species into the films from the substrate, with an associated altered depth of incorporation of phosphorus species into the films.

  2. Adhesion of silver films to ion-bombarded alumina

    International Nuclear Information System (INIS)

    Erck, R.A.; Fenske, G.R.

    1990-01-01

    This paper reports on silver films deposited on alumina substrates using ion bombardment. Adhesion strength was measured as a function of deposition conditions, sputter-cleaning time, and bombarding ion species, using a pull-type adhesion tester. Argon- and argon/oxygen-ion sputtering produced large increases in adhesion strength, with the greatest increases occurring for oxygen-ion bombardment. Adhesion strength increased monotonically as a function of ion sputtering time. At a given deposition rate, further enhancement of adhesion is seen with concurrent ion bombardment

  3. Formation and Entrapment of Tris(8-hydroxyquinolinealuminum from 8-Hydroxyquinoline in Anodic Porous Alumina

    Directory of Open Access Journals (Sweden)

    Shohei Yamaguchi

    2016-08-01

    Full Text Available The formation and entrapment of tris(8-hydroxyquinolinealuminum (Alq3 molecules on the surface of anodic porous alumina (APA immersed in an ethanol solution of 8-hydroxyquinoline (HQ were investigated by absorption, fluorescence, and Raman spectroscopies. The effects of the selected APA preparation conditions (galvanostatic or potentiostatic anodization method, anodizing current and voltage values, one- or two-step anodizing process, and sulfuric acid electrolyte concentration on the adsorption and desorption of Alq3 species were examined. Among the listed parameters, sulfuric acid concentration was the most important factor in determining the Alq3 adsorption characteristics. The Alq3 content measured after desorption under galvanostatic conditions was 2.5 times larger than that obtained under potentiostatic ones, regardless of the adsorbed quantities. The obtained results suggest the existence of at least two types of adsorption sites on the APA surface characterized by different magnitudes of the Alq3 bonding strength. The related fluorescence spectra contained two peaks at wavelengths of 480 and 505 nm, which could be attributed to isolated Alq3 species inside nanovoids and aggregated Alq3 clusters in the pores of APA, respectively. The former species were attached to the adsorption sites with higher binding energies, whereas the latter ones were bound to the APA surface more weakly. Similar results were obtained for the Alq3 species formed from the HQ solution, which quantitatively exceeded the number of the Alq3 species adsorbed from the Alq3 solution. Alq3 molecules were formed in the HQ solution during the reaction of HQ molecules with the Al3+ ions in the oxide dissolution zone near the oxide/electrolyte interface through the cracks and the Al3+ ions adsorbed on surface of pore and cracks. In addition, it was suggested that HQ molecules could penetrate the nanovoids more easily than Alq3 species because of their smaller sizes, which

  4. Formation and Entrapment of Tris(8-hydroxyquinoline)aluminum from 8-Hydroxyquinoline in Anodic Porous Alumina

    Science.gov (United States)

    Yamaguchi, Shohei; Matsui, Kazunori

    2016-01-01

    The formation and entrapment of tris(8-hydroxyquinoline)aluminum (Alq3) molecules on the surface of anodic porous alumina (APA) immersed in an ethanol solution of 8-hydroxyquinoline (HQ) were investigated by absorption, fluorescence, and Raman spectroscopies. The effects of the selected APA preparation conditions (galvanostatic or potentiostatic anodization method, anodizing current and voltage values, one- or two-step anodizing process, and sulfuric acid electrolyte concentration) on the adsorption and desorption of Alq3 species were examined. Among the listed parameters, sulfuric acid concentration was the most important factor in determining the Alq3 adsorption characteristics. The Alq3 content measured after desorption under galvanostatic conditions was 2.5 times larger than that obtained under potentiostatic ones, regardless of the adsorbed quantities. The obtained results suggest the existence of at least two types of adsorption sites on the APA surface characterized by different magnitudes of the Alq3 bonding strength. The related fluorescence spectra contained two peaks at wavelengths of 480 and 505 nm, which could be attributed to isolated Alq3 species inside nanovoids and aggregated Alq3 clusters in the pores of APA, respectively. The former species were attached to the adsorption sites with higher binding energies, whereas the latter ones were bound to the APA surface more weakly. Similar results were obtained for the Alq3 species formed from the HQ solution, which quantitatively exceeded the number of the Alq3 species adsorbed from the Alq3 solution. Alq3 molecules were formed in the HQ solution during the reaction of HQ molecules with the Al3+ ions in the oxide dissolution zone near the oxide/electrolyte interface through the cracks and the Al3+ ions adsorbed on surface of pore and cracks. In addition, it was suggested that HQ molecules could penetrate the nanovoids more easily than Alq3 species because of their smaller sizes, which resulted in higher

  5. Enhancing the platinum atomic layer deposition infiltration depth inside anodic alumina nanoporous membrane

    Energy Technology Data Exchange (ETDEWEB)

    Vaish, Amit, E-mail: anv@udel.edu; Krueger, Susan; Dimitriou, Michael; Majkrzak, Charles [National Institute of Standards and Technology (NIST) Center for Neutron Research, Gaithersburg, MD 20899-8313 (United States); Vanderah, David J. [Institute for Bioscience and Biotechnology Research, NIST, Rockville, Maryland 20850 (United States); Chen, Lei, E-mail: lei.chen@nist.gov [NIST Center for Nanoscale Science and Technology, Gaithersburg, Maryland 20899-8313 (United States); Gawrisch, Klaus [Laboratory of Membrane Biochemistry and Biophysics, National Institute on Alcohol Abuse and Alcoholism, National Institutes of Health, Bethesda, Maryland 20892 (United States)

    2015-01-15

    Nanoporous platinum membranes can be straightforwardly fabricated by forming a Pt coating inside the nanopores of anodic alumina membranes (AAO) using atomic layer deposition (ALD). However, the high-aspect-ratio of AAO makes Pt ALD very challenging. By tuning the process deposition temperature and precursor exposure time, enhanced infiltration depth along with conformal coating was achieved for Pt ALD inside the AAO templates. Cross-sectional scanning electron microscopy/energy dispersive x-ray spectroscopy and small angle neutron scattering were employed to analyze the Pt coverage and thickness inside the AAO nanopores. Additionally, one application of platinum-coated membrane was demonstrated by creating a high-density protein-functionalized interface.

  6. Effects of Alclad Layer and Anodizing Time on Sulfuric Acid Anodizing and Film Properties of 2E12 Aluminum Alloy

    OpenAIRE

    CHEN Gao-hong; HU Yuan-sen; YU Mei; LIU Jian-hua; LI Guo-ai

    2017-01-01

    Alclad and unclad 2E12 aerospace aluminum alloy were treated by sulfuric acid anodic oxidation. The effects of alclad layer and anodizing time on the anodization behaviour and corrosion resistance of anodic oxide layer on 2E12 aluminum alloy were studied. Surface and cross-section morphology of anodic oxide films were observed by scanning electron microscopy. The electrochemical properties of anodic oxide films were analyzed by potentiodynamic polarization curve and electrochemical impedance ...

  7. Structural, optical and mechanical properties of amorphous and crystalline alumina thin films

    Energy Technology Data Exchange (ETDEWEB)

    Nayar, Priyanka [Department of Physics, Guru Nanak Dev University, Amritsar 143005 (India); Khanna, Atul, E-mail: akphysics@yahoo.com [Department of Physics, Guru Nanak Dev University, Amritsar 143005 (India); Kabiraj, D.; Abhilash, S.R. [Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110067 (India); Beake, Ben D.; Losset, Yannick [Micro Materials Limited, Unit 3, Wrexham Technology Park, Wrexham LL13 7YP (United Kingdom); Chen, Banghao [Chemistry and Biochemistry Department, Florida State University, Tallahassee 32306 (United States)

    2014-10-01

    Thin films of amorphous alumina of thickness 350 nm were deposited on fused silica substrates by electron beam evaporation. Amorphous films were annealed at several temperatures in the range: 400–1130 °C and changes in film crystallinity, short-range structure, optical and mechanical properties were studied. X-ray diffraction studies found that crystallization starts at 800 °C and produces γ and δ-alumina, the latter phase grows with heat treatment and the sample was mostly δ and θ-alumina after annealing at 1130 °C. The as-deposited amorphous alumina films have low hardness of 5 to 8 GPa, which increases to 11 to 12 GPa in crystalline sample. {sup 27}Al Magic Angle Spinning Nuclear Magnetic Resonance was used to study the short-range order of amorphous and crystalline alumina films and it was found that amorphous alumina film contains AlO{sub 5} and AlO{sub 4} structural units in the ratio of 1:2. The concentration of AlO{sub 5} was significantly suppressed in crystalline film, which contains 48% of Al{sup 3+} ions in AlO{sub 6}, 7% in AlO{sub 5} and 45% in AlO{sub 4} units. - Highlights: • Structure–property correlations in alumina films grown by electron-beam evaporation • Amorphous films crystallize into γ and δ-alumina on annealing in air at 800 °C. • δ and θ-alumina films are stable up to 1130 °C and do not transform to α-phase. • Amorphous alumina films contain {sup [5]}Al and {sup [4]}Al structural units in the ratio of 1:2. • {sup [5]}Al decreases whereas {sup [6]}Al concentration increases on crystallization.

  8. Surface-enhanced Raman scattering of self-assembled thiol monolayers and supported lipid membranes on thin anodic porous alumina

    Directory of Open Access Journals (Sweden)

    Marco Salerno

    2017-01-01

    Full Text Available Thin anodic porous alumina (tAPA was fabricated from a 500 nm thick aluminum (Al layer coated on silicon wafers, through single-step anodization performed in a Teflon electrochemical cell in 0.4 M aqueous phosphoric acid at 110 V. Post-fabrication etching in the same acid allowed obtaining tAPA surfaces with ≈160 nm pore diameter and ≈80 nm corresponding wall thickness to be prepared. The tAPA surfaces were made SERS-active by coating with a thin (≈25 nm gold (Au layer. The as obtained tAPA–Au substrates were incubated first with different thiols, namely mercaptobenzoic acid (MbA and aminothiol (AT, and then with phospholipid vesicles of different composition to form a supported lipid bilayer (SLB. At each step, the SERS substrate functionality was assessed, demonstrating acceptable enhancement (≥100×. The chemisorption of thiols during the first step and the formation of SLB from the vesicles during the second step, were independently monitored by using a quartz crystal microbalance with dissipation monitoring (QCM-D technique. The SLB membranes represent a simplified model system of the living cells membranes, which makes the successful observation of SERS on these films promising in view of the use of tAPA–Au substrates as a platform for the development of surface-enhanced Raman spectroscopy (SERS biosensors on living cells. In the future, these tAPA–Au-SLB substrates will be investigated also for drug delivery of bioactive agents from the APA pores.

  9. Through-mask anodization of titania dot- and pillar-like nanostructures on bulk Ti substrates using a nanoporous anodic alumina mask

    International Nuclear Information System (INIS)

    Sjoestroem, Terje; Su Bo; Fox, Neil

    2009-01-01

    Nanosized surface topography on an implant material has the capability of stimulating the acceptance of the material in its host surrounding. Fine-tuning of nanotopography feature size has been shown to trigger differentiation of mesenchymal stem cells into bone cells in vitro. For this purpose we have created well defined nanosized titania dot- and pillar-like structures on mechanically polished Ti substrates using a through-mask anodization technique with an anodic porous alumina template. The anodization technique allowed the titania structure dimensions to be precisely tuned in the range 15-140 nm in a single electrolyte system. The fabricated surfaces serve as good model surfaces for precise studies of in vitro cell behaviour. The through-mask anodization technique was used directly on bulk Ti surfaces, thus demonstrating a potential application for patterning of actual Ti implant surfaces.

  10. On the variation in the electrical properties and ac conductivity of through-thickness nano-porous anodic alumina with temperature

    International Nuclear Information System (INIS)

    Tahir, Mahmood; Mehmood, Mazhar; Nadeem, Muhammad; Waheed, Abdul; Tanvir, Muhammad Tauseef

    2013-01-01

    The electrical response of self-organized through-thickness anodic alumina with hexagonal arrangement of cylindrical pores has been studied as a function of temperature. Mechanically stable thick porous anodic alumina was prepared, by through-thickness anodic oxidation of aluminum sheet in sulfuric acid, with extremely high aspect ratio pores exhibiting fairly uniform diameter and interpore distance. It was observed that the electrical properties of through-thickness anodic alumina are very sensitive to minute changes in temperature and the role of surface conductivity in governing its electrical response cannot be overlooked. At high frequencies, intrinsic dielectric response of anodic alumina was dominant. The frequency-dependent conductivity behavior at low and intermediate frequencies was explained on the basis of correlated barrier hopping (CBH) and quantum mechanical tunneling (QMT) models, respectively. Experimental data was modeled using an equivalent circuit consisting of Debye circuit, for bulk alumina, parallel to surface conduction path. The surface conduction was primarily based on two circuits in series, each with a parallel arrangement of a resistor and a constant phase element. This suggested heterogeneity in alumina pore surface, possibly related with islands of physisorbed water separated by the regions of chemisorbed water. Temperature dependence of some circuit elements has been analyzed to express different charge migration phenomena occurring in nano-porous anodic alumina

  11. The role and effect of residual stress on pore generation during anodization of aluminium thin films

    International Nuclear Information System (INIS)

    Liao, M.W.; Chung, C.K.

    2013-01-01

    Highlights: •Al films of varying residual stress were prepared by sputtering. •Variation of the residual stress in the Al films influences pore growth during anodization. •The change in average pore size with residual stress is fairly small. •Interaction of residual stress with oxide growth stress leads to change in structure. •Residual tensile stress increases the pore density of porous alumina. -- Abstract: The role and effect of residual stress on pore generation of anodized aluminium oxide (AAO) have been investigated into anodizing the various-residual-stresses aluminium films. The plane stresses were characterised by X-ray diffraction with sin 2 ψ method. The pore density roughly linearly increased with residual stress from 64.6 (−132.5 MPa) to 90.5 pores/μm 2 (135.9 MPa). However, the average pore size around 40 nm was not changed significantly except for the rougher film. The tensile residual stress lessened the compressive oxide growth stress to reduce AAO plastic deformation for higher pore density. The findings provide new foundations for realizing AAO films on silicon

  12. The characterization of thin platinum films on alumina

    International Nuclear Information System (INIS)

    Altman, E.I.; Gorte, R.J.

    1987-01-01

    Industrial metal catalysts are usually in the form of small metal particles supported on a porous oxide. The typical size of these metal particles ranges between 1.0 and 10.0 nm and it is well known that the particle size and the oxide substrate can affect the catalytic properties of the metal for some important reactions. Previous work with adsorption on small particles has indicated that desorption temperatures and the ability to dissociate CO can also be affected by the particle size. To further investigate these size and substrate effects, the authors have examined the adsorption properties of several simple gases on small Pt particles supported on alumina using temperature programmed desorption (TPD). The author show that the desorption curves for CO, H/sub 2/, and NO on these particles are very similar to curves measured on single crystals. The details of sample preparation and characterization have been described previously. Samples were prepared by vapor depositing Pt onto an alumina substrate which was formed by exposing an Al film to O/sub 2/. Auger electron spectroscopy was used to monitor surface cleanliness and to characterize the growth of the Pt on the substrate. As reported previously, the Pt grew in a layer-by-layer manner at both 90K and 300K. This film aggregated into clusters when the sample was heated above 650K and the average size of these particles could be determined from the saturation coverage of CO and from the quantity of metal deposited, as measured using a film thickness monitor. All adsorption measurements reported in this paper were made on samples heated above 650K

  13. Fabrication of optical chemical ammonia sensors using anodized alumina supports and sol-gel method.

    Science.gov (United States)

    Markovics, Akos; Kovács, Barna

    2013-05-15

    In this comparative study, the fabrication and the sensing properties of various reflectometric optical ammonia gas sensors are described. In the first set of experiments the role of the support material was investigated on four different sensor membranes. Two of them were prepared by the adsorption of bromocresol green indicator on anodized aluminum plates. The applied anodizing voltages were 12 V and 24 V, which resulted in different dynamic ranges and response times for gaseous ammonia. The sol-gel method was used for the preparation of the other batch of sensors. These layers were coated on anodized aluminum plates (24 V) and on standard microscope cover glasses. In spite of the identical sensing chemistry, slightly different response times were measured merely because of the aluminum surface porosity. Gas molecules can remain entrapped in the pores, which results in delayed recovery time. On the other hand, the porous oxide film provides excellent adhesion, making the anodized aluminum an attractive support for the sol-gel layer. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Sustained, Controlled and Stimuli-Responsive Drug Release Systems Based on Nanoporous Anodic Alumina with Layer-by-Layer Polyelectrolyte

    Science.gov (United States)

    Porta-i-Batalla, Maria; Eckstein, Chris; Xifré-Pérez, Elisabet; Formentín, Pilar; Ferré-Borrull, J.; Marsal, Lluis F.

    2016-08-01

    Controlled drug delivery systems are an encouraging solution to some drug disadvantages such as reduced solubility, deprived biodistribution, tissue damage, fast breakdown of the drug, cytotoxicity, or side effects. Self-ordered nanoporous anodic alumina is an auspicious material for drug delivery due to its biocompatibility, stability, and controllable pore geometry. Its use in drug delivery applications has been explored in several fields, including therapeutic devices for bone and dental tissue engineering, coronary stent implants, and carriers for transplanted cells. In this work, we have created and analyzed a stimuli-responsive drug delivery system based on layer-by-layer pH-responsive polyelectrolyte and nanoporous anodic alumina. The results demonstrate that it is possible to control the drug release using a polyelectrolyte multilayer coating that will act as a gate.

  15. Protein adsorption on low temperature alpha alumina films for surgical instruments

    Energy Technology Data Exchange (ETDEWEB)

    Cloud, A.N., E-mail: acloud@uark.ed [University of Arkansas, Fayetteville, AR 72701 (United States); Kumar, S. [Ian Wark Research Institute, University of South Australia, Mawson Lakes, Adelaide, SA 5095 (Australia); Kavdia, M.; Abu-Safe, H.H.; Gordon, M.H. [University of Arkansas, Fayetteville, AR 72701 (United States)

    2009-08-31

    Bulk alumina has been shown to exhibit reduced protein adsorption, a property that can be exploited for developing alumina-coated surgical instruments and devices. Alpha alumina thin films were deposited on surgical stainless steel substrates to investigate the adsorption of a model protein (BSA, bovine serum albumin). The films were deposited at 480 {sup o}C by AC inverted cylindrical magnetron sputtering. Films were obtained at 6 kW and 50% oxygen partial pressure by volume. The presence of alpha-phase alumina has been shown by transmission electron microscopy. Results indicate that there was a 50% reduction in protein adsorption for samples with the alumina coating compared to those with no coating.

  16. Dielectric breakdown and healing of anodic oxide films on aluminium under single pulse anodizing

    International Nuclear Information System (INIS)

    Sah, Santosh Prasad; Tatsuno, Yasuhiro; Aoki, Yoshitaka; Habazaki, Hiroki

    2011-01-01

    Research highlights: → We examined dielectric breakdown of anodic alumina by single pulse anodizing. → Current transients and morphology of discharge channels are dependent upon electrolyte and voltage. → There is a good correlation between current transient and morphology of discharge channel. → Healing of open discharge pores occurs in alkaline silicate, but not in pentaborate electrolyte. - Abstract: Single pulse anodizing of aluminium micro-electrode has been employed to study the behaviour of dielectric breakdown and subsequent oxide formation on aluminium in alkaline silicate and pentaborate electrolytes. Current transients during applying pulse voltage have been measured, and surface has been observed by scanning electron microscopy. Two types of current transients are observed, depending on the electrolyte and applied voltage. There is a good correlation between the current transient behaviour and the shape of discharge channels. In alkaline silicate electrolyte, circular open pores are healed by increasing the pulse width, but such healing is not obvious in pentaborate electrolyte.

  17. Realisation and optical engineering of linear variable bandpass filters in nanoporous anodic alumina photonic crystals.

    Science.gov (United States)

    Sukarno; Law, Cheryl Suwen; Santos, Abel

    2017-06-08

    We present the first realisation of linear variable bandpass filters in nanoporous anodic alumina (NAA-LVBPFs) photonic crystal structures. NAA gradient-index filters (NAA-GIFs) are produced by sinusoidal pulse anodisation and used as photonic crystal platforms to generate NAA-LVBPFs. The anodisation period of NAA-GIFs is modified from 650 to 850 s to systematically tune the characteristic photonic stopband of these photonic crystals across the UV-visible-NIR spectrum. Then, the nanoporous structure of NAA-GIFs is gradually widened along the surface under controlled conditions by wet chemical etching using a dip coating approach aiming to create NAA-LVBPFs with finely engineered optical properties. We demonstrate that the characteristic photonic stopband and the iridescent interferometric colour displayed by these photonic crystals can be tuned with precision across the surface of NAA-LVBPFs by adjusting the fabrication and etching conditions. Here, we envisage for the first time the combination of the anodisation period and etching conditions as a cost-competitive, facile, and versatile nanofabrication approach that enables the generation of a broad range of unique LVBPFs covering the spectral regions. These photonic crystal structures open new opportunities for multiple applications, including adaptive optics, hyperspectral imaging, fluorescence diagnostics, spectroscopy, and sensing.

  18. Fine tuning of transmission features in nanoporous anodic alumina distributed Bragg reflectors

    Science.gov (United States)

    Lim, Siew Yee; Law, Cheryl Suwen; Santos, Abel

    2018-01-01

    This study introduces an innovative apodisation strategy to tune the filtering features of distributed Bragg reflectors based on nanoporous anodic alumina (NAA-DBRs). The effective medium of NAA-DBRs, which is modulated in a stepwise fashion by a pulse-like anodisation approach, is apodised following a logarithmic negative function to engineer the transmission features of NAA-DBRs. We investigate the effect of various apodisation parameters such as apodisation amplitude difference, anodisation period, current density offset and pore widening time, to tune and optimise the optical properties of NAA-DBRs in terms of central wavelength position, full width at half maximum and quality of photonic stop band. The transmission features of NAA-DBRs are shown to be fully controllable with precision across the spectral regions by means of the apodisation parameters. Our study demonstrates that an apodisation strategy can significantly narrow the width and enhance the quality of the characteristic photonic stop band of NAA-DBRs. This rationally designed anodisation approach based on the combination of apodisation and stepwise pulse anodisation enables the development of optical filters with tuneable filtering features to be integrated into optical technologies acting as essential photonic elements in devices such as optical sensors and biosensors.

  19. Fabrication and Optimization of Bilayered Nanoporous Anodic Alumina Structures as Multi-Point Interferometric Sensing Platform

    Science.gov (United States)

    Nemati, Mahdieh; Santos, Abel

    2018-01-01

    Herein, we present an innovative strategy for optimizing hierarchical structures of nanoporous anodic alumina (NAA) to advance their optical sensing performance toward multi-analyte biosensing. This approach is based on the fabrication of multilayered NAA and the formation of differential effective medium of their structure by controlling three fabrication parameters (i.e., anodization steps, anodization time, and pore widening time). The rationale of the proposed concept is that interferometric bilayered NAA (BL-NAA), which features two layers of different pore diameters, can provide distinct reflectometric interference spectroscopy (RIfS) signatures for each layer within the NAA structure and can therefore potentially be used for multi-point biosensing. This paper presents the structural fabrication of layered NAA structures, and the optimization and evaluation of their RIfS optical sensing performance through changes in the effective optical thickness (EOT) using quercetin as a model molecule. The bilayered or funnel-like NAA structures were designed with the aim of characterizing the sensitivity of both layers of quercetin molecules using RIfS and exploring the potential of these photonic structures, featuring different pore diameters, for simultaneous size-exclusion and multi-analyte optical biosensing. The sensing performance of the prepared NAA platforms was examined by real-time screening of binding reactions between human serum albumin (HSA)-modified NAA (i.e., sensing element) and quercetin (i.e., analyte). BL-NAAs display a complex optical interference spectrum, which can be resolved by fast Fourier transform (FFT) to monitor the EOT changes, where three distinctive peaks were revealed corresponding to the top, bottom, and total layer within the BL-NAA structures. The spectral shifts of these three characteristic peaks were used as sensing signals to monitor the binding events in each NAA pore in real-time upon exposure to different concentrations of

  20. Fabrication and Optimization of Bilayered Nanoporous Anodic Alumina Structures as Multi-Point Interferometric Sensing Platform

    Directory of Open Access Journals (Sweden)

    Mahdieh Nemati

    2018-02-01

    Full Text Available Herein, we present an innovative strategy for optimizing hierarchical structures of nanoporous anodic alumina (NAA to advance their optical sensing performance toward multi-analyte biosensing. This approach is based on the fabrication of multilayered NAA and the formation of differential effective medium of their structure by controlling three fabrication parameters (i.e., anodization steps, anodization time, and pore widening time. The rationale of the proposed concept is that interferometric bilayered NAA (BL-NAA, which features two layers of different pore diameters, can provide distinct reflectometric interference spectroscopy (RIfS signatures for each layer within the NAA structure and can therefore potentially be used for multi-point biosensing. This paper presents the structural fabrication of layered NAA structures, and the optimization and evaluation of their RIfS optical sensing performance through changes in the effective optical thickness (EOT using quercetin as a model molecule. The bilayered or funnel-like NAA structures were designed with the aim of characterizing the sensitivity of both layers of quercetin molecules using RIfS and exploring the potential of these photonic structures, featuring different pore diameters, for simultaneous size-exclusion and multi-analyte optical biosensing. The sensing performance of the prepared NAA platforms was examined by real-time screening of binding reactions between human serum albumin (HSA-modified NAA (i.e., sensing element and quercetin (i.e., analyte. BL-NAAs display a complex optical interference spectrum, which can be resolved by fast Fourier transform (FFT to monitor the EOT changes, where three distinctive peaks were revealed corresponding to the top, bottom, and total layer within the BL-NAA structures. The spectral shifts of these three characteristic peaks were used as sensing signals to monitor the binding events in each NAA pore in real-time upon exposure to different

  1. Topotactic preparation of textured alumina ceramics from dehydroxylation of gibbsite films

    Energy Technology Data Exchange (ETDEWEB)

    Louaer, Seif-Eddine; Wang, Yao, E-mail: yao@buaa.edu.cn; Guo, Lin, E-mail: guolin@buaa.edu.cn

    2014-11-14

    In this paper, textured alumina ceramics were prepared from dehydroxylation of gibbsite films and the pseudomorphic and topotactic nature of the dehydroxylation of textured gibbsite films has been investigated. First, the precursor film with a (001)-textured structure was obtained via vacuum filtration deposition of diluted aqueous suspensions of gibbsite nanoplatelets. Subsequently, (001)-textured α-alumina ceramics were successfully achieved by sintering of the deposited gibbsite films without addition of α-alumina seeds. The Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD) results show that, during the phase transition from gibbsite to α-alumina, both layered morphology and crystal's axis orientation have been retained to a considerable extent. For the first time, a direct XRD evidence of gibbsite topotactic dehydroxylation to the α-alumina phase is presented. It is believed that the method described here exploits gibbsite's pseudomorphic and topotactic dehydroxylation, not on individual particles scale but on a bulk form. The resulting structure can be considered as inorganic scaffolds which can have applications for fabrication of dense, textured alumina-based ceramics and other layered/textured nanocomposites. - Highlights: • Gibbsite nanoplatelets were assembled on their basal plane to form (001)-textured films. • Textured alumina ceramics were prepared by sintering textured gibbsite films without addition of α-alumina seeds. • Both pseudomorphic and topotactic aspects were exploited in bulk form instead of individual nanoparticulate size. • Direct XRD evidence of the topotactic dehydroxylation from gibbsite to α-alumina is presented in this work.

  2. Topotactic preparation of textured alumina ceramics from dehydroxylation of gibbsite films

    International Nuclear Information System (INIS)

    Louaer, Seif-Eddine; Wang, Yao; Guo, Lin

    2014-01-01

    In this paper, textured alumina ceramics were prepared from dehydroxylation of gibbsite films and the pseudomorphic and topotactic nature of the dehydroxylation of textured gibbsite films has been investigated. First, the precursor film with a (001)-textured structure was obtained via vacuum filtration deposition of diluted aqueous suspensions of gibbsite nanoplatelets. Subsequently, (001)-textured α-alumina ceramics were successfully achieved by sintering of the deposited gibbsite films without addition of α-alumina seeds. The Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD) results show that, during the phase transition from gibbsite to α-alumina, both layered morphology and crystal's axis orientation have been retained to a considerable extent. For the first time, a direct XRD evidence of gibbsite topotactic dehydroxylation to the α-alumina phase is presented. It is believed that the method described here exploits gibbsite's pseudomorphic and topotactic dehydroxylation, not on individual particles scale but on a bulk form. The resulting structure can be considered as inorganic scaffolds which can have applications for fabrication of dense, textured alumina-based ceramics and other layered/textured nanocomposites. - Highlights: • Gibbsite nanoplatelets were assembled on their basal plane to form (001)-textured films. • Textured alumina ceramics were prepared by sintering textured gibbsite films without addition of α-alumina seeds. • Both pseudomorphic and topotactic aspects were exploited in bulk form instead of individual nanoparticulate size. • Direct XRD evidence of the topotactic dehydroxylation from gibbsite to α-alumina is presented in this work

  3. A Study on Sealing Process of Anodized Al Alloy Film

    Science.gov (United States)

    Tsujita, Takeshi; Sato, Hiroshi; Tsukahara, Sonoko; Ishikawa, Yuuichi

    Since sealing is an important process to improve the corrosion resistance in practical application of anodized aluminum, we prepared anodic oxide films on A5052 alloy in an oxalic acid bath and a sulfuric acid bath, sealed them at various conditions, and analyzed them by scanning electron microscopy, acid-dissolution examination, admittance measurements and infrared spectroscopy. The pore radius of the oxalic acid anodized film was about 5 times larger than that of sulfuric acid anodized film, while the corrosion resistance of the former showed about 2 times higher value than the latter with the same sealed state and amount of hydroxide formed by sealing process of the former was 6 times larger than the latter, respectively. Steam sealing formed dense hydroxide and boiling water sealing formed big coral-like hydroxide, whereas the corrosion resistance of the film sealed by the former showed about 1.5 times higher value than that sealed by the latter, respectively. Thus microstructure of anodic oxide films and their surface morphology after sealing process clearly depended on their anodizing solution and the sealing condition and showed obvious relation to electric and corrosive properties.

  4. The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films

    Science.gov (United States)

    Ren, Jianjun; Zuo, Yu

    2012-11-01

    The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films were studied. The voltage-time response for galvanostatic anodization of aluminum in malonic acid solution exhibits a conventional three-stage feature but the formation voltage is much higher. With the increase of electrolyte concentration, the electrolyte viscosity increases simultaneously and the high viscosity decreases the film growth rate. With the concentration increase of the malonic acid electrolyte, the critical current density that initiates local "burning" on the sample surface decreases. For malonic acid anodization, the field-assisted dissolution on the oxide surface is relatively weak and the nucleation of pores is more difficult, which results in greater barrier layer thickness and larger cell dimension. The embryo of the porous structure of anodic film has been created within the linear region of the first transient stage, and the definite porous structure has been established before the end of the first transient stage. The self-ordering behavior of the porous film is influenced by the electrolyte concentration, film thickness and the applied current density. Great current density not only improves the cell arrangement order but also brings about larger cell dimension.

  5. Reaction products between Bi-Sr-Ca-Cu-oxide thick films and alumina substrates

    International Nuclear Information System (INIS)

    Alarco, J.A.; Ilushechkin, A.; Yamashita, T.; Bhargava, A.; Barry, J.; Mackinnon, I.D.R.

    1997-01-01

    The structure and composition of reaction products between Bi-Sr-Ca-Cu-oxide (BSCCO) thick films and alumina substrates have been characterized using a combination of electron diffraction, scanning electron microscopy and energy dispersive X-ray spectrometry (EDX). Sr and Ca are found to be the most reactive cations with alumina. Sr 4 Al 6 O 12 SO 4 is formed between the alumina substrates and BSCCO thick films prepared from paste with composition close to Bi-2212 (and Bi-2212+10 wt.% Ag). For paste with composition close to Bi(Pb)-2223 +20 wt.% Ag, a new phase with f.c.c. structure, lattice parameter about a=24.5 A and approximate composition Al 3 Sr 2 CaBi 2 CuO x has been identified in the interface region. Understanding and control of these reactions is essential for growth of high quality BSCCO thick films on alumina. (orig.)

  6. Effects of Alclad Layer and Anodizing Time on Sulfuric Acid Anodizing and Film Properties of 2E12 Aluminum Alloy

    Directory of Open Access Journals (Sweden)

    CHEN Gao-hong

    2017-07-01

    Full Text Available Alclad and unclad 2E12 aerospace aluminum alloy were treated by sulfuric acid anodic oxidation. The effects of alclad layer and anodizing time on the anodization behaviour and corrosion resistance of anodic oxide layer on 2E12 aluminum alloy were studied. Surface and cross-section morphology of anodic oxide films were observed by scanning electron microscopy. The electrochemical properties of anodic oxide films were analyzed by potentiodynamic polarization curve and electrochemical impedance spectroscopy. The results show that the protective anodic oxide layers are formed on alclad and unclad 2E12 aluminum alloy. The film thickness increases with anodizing time extending. The copper rich second phase particles lead to more cavity defects and even micro cracks on anodic oxide films of unclad 2E12 aluminum alloy. The anodic oxide films on alclad 2E12 aluminum alloy are thicker and have fewer cavity defects, resulting in better corrosion resistance. The films obtained after 30min and 45min anodic oxidation treatment exhibit lower corrosion current and higher impedance of the porous layer than other anodizing time.

  7. Surface modification of nanoporous anodic alumina photonic crystals for photocatalytic applications

    Science.gov (United States)

    Lim, Siew Yee; Law, Cheryl Suwen; Santos, Abel

    2018-01-01

    Herein, we report on the development of a rationally designed composite photocatalyst material by combining nanoporous anodic alumina-rugate filters (NAA-RFs) with photo-active layers of titanium dioxide (TiO2). NAA-RFs are synthesised by sinusoidal pulse anodisation and subsequently functionalised with TiO2 by sol-gel method to provide the photonic structures with photocatalytic properties. We demonstrate that the characteristic photonic stopband (PSB) of the surface-modified NAA-RFs can be precisely tuned across the UV-visible-NIR spectrum to enhance the photon-toelectron conversion of TiO2 by `slow photon effect'. We systematically investigate the effect of the anodisation parameters (i.e. anodisation period and pore widening time) on the position of the PSB of NAA-RFs as well as the photocatalytic performances displayed by these photonic crystal structures. When the edges of the PSB of surfacemodified NAA-RFs are positioned closely to the absorption peak of the model organic dye (i.e. methyl orange - MO), the photocatalytic performance of the system to degrade these molecules is enhanced under simulated solar light irradiation due to slow photon effect. Our investigation also reveals that the photocatalytic activity of surface-modified NAA-RFs is independent of slow photon effect and enhances with increasing period length (i.e. increasing anodisation period) of the photonic structures when there is no overlap between the PSB and the absorption peak of MO. This study therefore provides a rationale towards the photocatalytic enhancement of photonic crystals by a rational design of the PSB, creating new opportunities for the future development of high-performance photocatalysts.

  8. Fabrication of Acrylonitrile-Butadiene-Styrene Nanostructures with Anodic Alumina Oxide Templates, Characterization and Biofilm Development Test for Staphylococcus epidermidis.

    Directory of Open Access Journals (Sweden)

    Camille Desrousseaux

    Full Text Available Medical devices can be contaminated by microbial biofilm which causes nosocomial infections. One of the strategies for the prevention of such microbial adhesion is to modify the biomaterials by creating micro or nanofeatures on their surface. This study aimed (1 to nanostructure acrylonitrile-butadiene-styrene (ABS, a polymer composing connectors in perfusion devices, using Anodic Alumina Oxide templates, and to control the reproducibility of this process; (2 to characterize the physico-chemical properties of the nanostructured surfaces such as wettability using captive-bubble contact angle measurement technique; (3 to test the impact of nanostructures on Staphylococcus epidermidis biofilm development. Fabrication of Anodic Alumina Oxide molds was realized by double anodization in oxalic acid. This process was reproducible. The obtained molds present hexagonally arranged 50 nm diameter pores, with a 100 nm interpore distance and a length of 100 nm. Acrylonitrile-butadiene-styrene nanostructures were successfully prepared using a polymer solution and two melt wetting methods. For all methods, the nanopicots were obtained but inside each sample their length was different. One method was selected essentially for industrial purposes and for better reproducibility results. The flat ABS surface presents a slightly hydrophilic character, which remains roughly unchanged after nanostructuration, the increasing apparent wettability observed in that case being explained by roughness effects. Also, the nanostructuration of the polymer surface does not induce any significant effect on Staphylococcus epidermidis adhesion.

  9. Preparing magnetic yttrium iron garnet nanodot arrays by ultrathin anodic alumina template on silicon substrate

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Hui; Han, Mangui, E-mail: han-mangui@yahoo.com; Deng, Longjiang [National Engineering Research Center of Electromagnetic Radiation Control Materials, University of Electronic Science and Technology of China, Chengdu 610054 (China); Zheng, Liang; Zheng, Peng; Qin, Huibin [Institute of Electron Device and Application, Hangzhou Dianzi University, Hangzhou 310008 (China); Wu, Qiong [Magnetism Key Laboratory of Zhejiang Province, China Jiliang University, Hangzhou 310018 (China)

    2015-08-10

    Ultrahigh density periodically ordered magnetic yttrium iron garnet (Y{sub 3}Fe{sub 5}O{sub 12}, YIG) nanodot arrays have been prepared by pulsed laser deposition through an ultrathin alumina mask (UTAM). UTAM having periodically ordered circularly shaped holes with 350 nm in diameter, 450 nm in inter-pore distance, and 700 nm in height has been prepared on silicon substrate. Furthermore, the microstructure and magnetic properties of YIG nanodot arrays have been characterized. Nanodot arrays with a sharp distribution in diameter centered at 340 nm with standard deviation of 10 nm have been fabricated. Moreover, typical hysteresis loops and ferromagnetic resonance spectra in in-plane and out-of-plane revealed that this unique structure greatly influences the magnetics properties of YIG. First, coercivity of YIG nanodot arrays in in-plane was increased about from 15 Oe of YIG films to 500 Oe. Then, the degree of uniformity about nanodot height decided that two or more resonance peaks in out-of-plane were detected in the spectra. The peak-to-peak linewidth values were about 94 Oe and 40 Oe in the parallel and perpendicular directions, respectively, which indicated that the values were larger by the two-magnon scattering. Consequently, this pattering method creates opportunities for studying physics in oxide nanomagnets and may be applied in spin-wave devices.

  10. Preparation and properties of antimony thin film anode materials

    Institute of Scientific and Technical Information of China (English)

    SU Shufa; CAO Gaoshao; ZHAO Xinbing

    2004-01-01

    Metallic antimony thin films were deposited by magnetron sputtering and electrodeposition. Electrochemical properties of the thin film as anode materials for lithium-ion batteries were investigated and compared with those of antimony powder. It was found that both magnetron sputtering and electrodeposition are easily controllable processes to deposit antimony films with fiat charge/discharge potential plateaus. The electrochemical performances of antimony thin films, especially those prepared with magnetron sputtering, are better than those of antimony powder. The reversible capacities of the magnetron sputtered antimony thin film are above 400 mA h g-1 in the first 15 cycles.

  11. Photophysics and energy transfer studies of Alq3 confined in the voids of nanoporous anodic alumina.

    Science.gov (United States)

    Mohammadpour, Arash; Utkin, Ilya; Bodepudi, Srikrishna Chanakya; Kar, Piyush; Fedosejevs, Robert; Pramanik, Sandipan; Shankar, Karthik

    2013-04-01

    We report on a hierarchical nanoarchitecture wherein distinct chromophores are deterministically placed at two different types of sites in a nanoporous metal oxide framework. One chromophore, namely Tris(8-hydroxyquinoline)aluminium(III) (Alq3), is embedded in the 1-2 nm sized nanovoids of anodic aluminum oxide (AAO) and another chromophore (carboxyfluorescein or pyrenebutyric acid) is anchored in the form of a monolayer to the surface of the walls of the cylindrical nanopores (- 20 nm in diameter) of AAO. We found the luminescence maximum to occur at 492 nm, blueshifted by at least 18 nm from the value in solutions and thin films. The excited state decay of Alq3 molecules in nanovoids was found to be biexponential with a fast component of 338 ps and a slower component of 2.26 ns, different from Alq3 thin films and solutions. Using a combination of steady state and time-resolved luminescence studies, we found that efficient Forster-type resonance energy transfer (FRET) from Alq3 in the nanovoids to the carboxyfluorescein monolayer could be used to pump the emission of surface-bound chromophores. Conversely, the emission of nanovoid-confined Alq3 could be pumped by energy transfer from a pyrenebutyric acid monolayer. Such intra-nanoarchitecture interactions between chromophores deterministically placed in different spatial locations are important in applications such as organic light emitting diodes, chemical sensors, energy transfer fluorescent labels, light harvesting antennas and organic spintronics.

  12. Growth behavior of anodic oxide formed by aluminum anodizing in glutaric and its derivative acid electrolytes

    Science.gov (United States)

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2014-12-01

    The growth behavior of anodic oxide films formed via anodizing in glutaric and its derivative acid solutions was investigated based on the acid dissociation constants of electrolytes. High-purity aluminum foils were anodized in glutaric, ketoglutaric, and acetonedicarboxylic acid solutions under various electrochemical conditions. A thin barrier anodic oxide film grew uniformly on the aluminum substrate by glutaric acid anodizing, and further anodizing caused the film to breakdown due to a high electric field. In contrast, an anodic porous alumina film with a submicrometer-scale cell diameter was successfully formed by ketoglutaric acid anodizing at 293 K. However, the increase and decrease in the temperature of the ketoglutaric acid resulted in non-uniform oxide growth and localized pitting corrosion of the aluminum substrate. An anodic porous alumina film could also be fabricated by acetonedicarboxylic acid anodizing due to the relatively low dissociation constants associated with the acid. Acid dissociation constants are an important factor for the fabrication of anodic porous alumina films.

  13. A Novel Method for Fabricating Double Layers Porous Anodic Alumina in Phosphoric/Oxalic Acid Solution and Oxalic Acid Solution

    Directory of Open Access Journals (Sweden)

    Yanfang Xu

    2016-01-01

    Full Text Available A novel method for fabricating ordered double layers porous anodic alumina (DL-PAA with controllable nanopore size was presented. Highly ordered large pore layer with interpore distance of 480 nm was fabricated in phosphoric acid solution with oxalic acid addition at the potential of 195 V and the small pore layer was fabricated in oxalic acid solution at the potential from 60 to 100 V. Experimental results show that the thickness of large pore layer is linearly correlative with anodizing time, and pore diameter is linearly correlative with pore widening time. When the anodizing potential in oxalic acid solution was adjusted from 60 to 100 V, the small pore layers with continuously tunable interpore distance from 142 to 241 nm and pore density from 1.94×109 to 4.89×109 cm−2 were obtained. And the interpore distance and the pore density of small pore layers are closely correlative with the anodizing potential. The fabricated DL-PAA templates can be widely utilized for fabrication of ordered nanomaterials, such as superhydrophobic or gecko-inspired adhesive materials and metal or semiconductor nanowires.

  14. Digital simulation of anodic stripping voltammetry from thin film electrodes

    International Nuclear Information System (INIS)

    Magallanes, J.F.

    1984-01-01

    The anodic stripping voltammetry (ASV) is routinely applied to control of Cu(II) in heavy water in the primary cooling loop of the Nuclear Power Reactor. The anodic stripping voltammetry (ASV) is a very well-known technique in electroanalytical chemistry. However, due to the complexity of the phenomena, it is practised with the fundamentals of empiric considerations. A geometric model for the anodic stripping voltammetry (ASV) from thin film electrodes which can be calculated by explicit digital simulation method is proposed as a possibility of solving the electrochemically reversible, cuasi-reversible and irreversible reactions under linear potential scan and multiple potential scans. (Until now the analytical mathematical method was applied to reversible reactions). All the results are compared with analytical solutions and experimental results and it permits to conclude that the anodic stripping voltammetry (ASV) can be studied with the simplicity and potentialities of explicit digital simulation methods. (M.E.L.) [es

  15. Research of the photovoltaic properties of anodized films of Sn

    Science.gov (United States)

    Afanasyev, D. A.; Ibrayev, N. Kh; Omarova, G. S.; Smagulov, Zh K.

    2015-04-01

    The results of studies of photovoltaic properties of solar cells based on porous tin oxide films, sensitized with an organic dye are presented. Porous films were prepared by electrochemical anodization of tin in alkaline electrolytes based on aqueous solution of NaOH and aqueous ammonia NH4OH. It was found that the time of anodizing of the Sn films affects on conversion efficiency of light energy into electrical energy. Increasing of the sorption time leads to an increase of the number of molecules on the surface of the porous film. For the solar cell based on tin oxide there is a strong dark current, which significantly reduces the efficiency of conversion of light energy into electrical energy.

  16. Spectroscopic and nonlinear photophysical characterization of organic octupolar-compounds supported by anodic-alumina nanotube-arrays

    International Nuclear Information System (INIS)

    Morales-Saavedra, O.G.; Ontiveros-Barrera, F.G.; Hennrich, G.; Mata-Zamora, M.E.; Rodriguez-Rosales, A.A.; Banuelos, J.G.

    2011-01-01

    Highlights: → Preparation of organic-inorganic nanostructured hybrid materials. → Insertion of octupolar compounds in alumina nanotube arrays. → Linear and nonlinear photophysical characterization of solid-state hybrid structures. → Fabrication of photonic materials. - Abstract: Amorphous anodic alumina membranes (AAM) comprising highly ordered nanometric porous arrays (porous anodic aluminas: PAA) with 1D-nanotube dimensions of ∼75 nm in diameter and 45 microns in depth were successfully prepared and used as nanostructured host networks for different functionalized octupolar chromophores (named here Oct-(n)). Atomic force microscopy (AFM) studies performed on the developed hybrid systems confirmed a homogeneous insertion of these organic molecules into the PAA nanotube-arrays. Samples with high structural quality were selected for several photophysical characterizations: Comprehensive X-ray diffraction (XRD) and optical spectroscopic characterizations performed according to UV-vis absorption, photoluminescent (PL) and Raman measurements revealed the structural and optical performance of these molecules within the PAA-confinement. Since the implemented optical chromophores were specifically functionalized for nonlinear optical (NLO) applications, the obtained Oct-(n)/PAA-based amorphous hybrids were also characterized according to cubic NLO-techniques such as third harmonic generation (THG) and the Z-Scan method. PAA-confined octupolar chromophores have shown interesting linear and NLO optical properties which have not yet been intensively investigated in bulk hybrid systems; hence, the obtained hybrid nanostructures represent a promising field of investigation in the route to functional octupolar-based materials, where different self-assembled molecular structures may be formed, giving rise to enhanced linear and NLO-properties.

  17. Role of Annealing Temperature on Morphology of Alumina Thin Film Prepared by Wet-Chemical Method

    Directory of Open Access Journals (Sweden)

    Manju Pandey

    2015-03-01

    Full Text Available In this paper, we reported the compositional, morphological and structural properties of the alumina(Al2O3 thin films prepared by sol-gel technique and annealed between 800 0C to 1200 0C for 1-hour in an air atmosphere. The deposited films were polycrystalline in nature. Thin films were found uniform and adherent to the alumina substrate. Effect of annealing temperature on structural parameters such as pore size and surface area were calculated. The result indicates that pore size and surface area was decreased by increasing annealing temperature. The material characterization was done by field emission scanning electron microscope (SEM, atomic force microscopy (AFM and Brunaur, Emmet and Teller (BET.

  18. Nanoporous alumina formed by self-organized two-step anodization of Ni{sub 3}Al intermetallic alloy in citric acid

    Energy Technology Data Exchange (ETDEWEB)

    Stepniowski, Wojciech J., E-mail: wstepniowski@wat.edu.pl [Department of Advanced Materials and Technology, Faculty of New Technologies and Chemistry, Military University of Technology, Kaliskiego 2 Str., 00-908 Warszawa (Poland); Cieslak, Grzegorz; Norek, Malgorzata; Karczewski, Krzysztof; Michalska-Domanska, Marta; Zasada, Dariusz; Polkowski, Wojciech; Jozwik, Pawel; Bojar, Zbigniew [Department of Advanced Materials and Technology, Faculty of New Technologies and Chemistry, Military University of Technology, Kaliskiego 2 Str., 00-908 Warszawa (Poland)

    2013-01-01

    Highlights: Black-Right-Pointing-Pointer Anodic porous alumina was formed by Ni{sub 3}Al intermetallic alloy anodization. Black-Right-Pointing-Pointer The anodizations were conducted in 0.3 M citric acid. Black-Right-Pointing-Pointer Nanopores geometry depends on anodizing voltage. Black-Right-Pointing-Pointer No barrier layer was formed during anodization. - Abstract: Formation of the nanoporous alumina on the surface of Ni{sub 3}Al intermetallic alloy has been studied in details and compared with anodization of aluminum. Successful self-organized anodization of this alloy was performed in 0.3 M citric acid at voltages ranging from 2.0 to 12.0 V using a typical two-electrode cell. Current density records revealed different mechanism of the porous oxide growth when compared to the mechanism pertinent for the anodization of aluminum. Electrochemical impedance spectroscopy experiments confirmed the differences in anodic oxide growth. Surface and cross-sections of the Ni{sub 3}Al intermetallic alloy with anodic oxide were observed with field-emission scanning electron microscope and characterized with appropriate software. Nanoporous oxide growth rate was estimated from cross-sectional FE-SEM images. The lowest growth rate of 0.14 {mu}m/h was found for the anodization at 0 Degree-Sign C and 2.0 V. The highest one - 2.29 {mu}m/h - was noticed for 10.0 V and 30 Degree-Sign C. Pore diameter was ranging from 18.9 nm (2.0 V, 0 Degree-Sign C) to 32.0 nm (12.0 V, 0 Degree-Sign C). Interpore distance of the nanoporous alumina was ranging from 56.6 nm (2.0 V, 0 Degree-Sign C) to 177.9 nm (12.0 V, 30 Degree-Sign C). Pore density (number of pore occupying given area) was decreasing with anodizing voltage increase from 394.5 pores/{mu}m{sup 2} (2.0 V, 0 Degree-Sign C) to 94.9 pores/{mu}m{sup 2} (12.0 V, 0 Degree-Sign C). All the geometrical features of the anodic alumina formed by two-step self-organized anodization of Ni{sub 3}Al intermetallic alloy are depending on the

  19. Dispersion tailoring of a silicon strip waveguide employing Titania-Alumina thin-film coating

    DEFF Research Database (Denmark)

    Guo, Kai; Christensen, Jesper B.; Christensen, Erik N.

    2017-01-01

    We numerically demonstrate dispersion tailoring of a silicon strip waveguide employing Titania-Alumina thin-film coating using a finite-difference mode solver. The proposed structure exhibits spectrally-flattened near-zero anomalous dispersion within the telecom wavelength range. We also numerica......We numerically demonstrate dispersion tailoring of a silicon strip waveguide employing Titania-Alumina thin-film coating using a finite-difference mode solver. The proposed structure exhibits spectrally-flattened near-zero anomalous dispersion within the telecom wavelength range. We also...

  20. Hydrogen uptake in alumina thin films synthesized from an aluminum plasma stream in an oxygen ambient

    International Nuclear Information System (INIS)

    Schneider, J.M.; Anders, A.; Hjoervarsson, B.; Petrov, I.; Macak, K.; Helmersson, U.; Sundgren, J.

    1999-01-01

    We describe the hydrogen uptake during the synthesis of alumina films from H 2 O present in the high vacuum gas background. The hydrogen concentration in the films was determined by the 1 H( 15 N,αγ) 12 C nuclear resonance reaction. Furthermore, we show the presence of hydrogen ions in the plasma stream by time-of-flight mass spectrometry. The hydrogen content increased in both the film and the plasma stream, as the oxygen partial pressure was increased. On the basis of these measurements and thermodynamic considerations, we suggest that an aluminum oxide hydroxide compound is formed, both on the cathode surface as well as in the film. The large scatter in the data reported in the literature for refractive index and chemical stability of alumina thin films can be explained on the basis of the suggested aluminum oxide hydroxide formation. copyright 1999 American Institute of Physics

  1. Simulator of Non-homogenous Alumina and Current Distribution in an Aluminum Electrolysis Cell to Predict Low-Voltage Anode Effects

    Science.gov (United States)

    Dion, Lukas; Kiss, László I.; Poncsák, Sándor; Lagacé, Charles-Luc

    2018-04-01

    Perfluorocarbons are important contributors to aluminum production greenhouse gas inventories. Tetrafluoromethane and hexafluoroethane are produced in the electrolysis process when a harmful event called anode effect occurs in the cell. This incident is strongly related to the lack of alumina and the current distribution in the cell and can be classified into two categories: high-voltage and low-voltage anode effects. The latter is hard to detect during the normal electrolysis process and, therefore, new tools are necessary to predict this event and minimize its occurrence. This paper discusses a new approach to model the alumina distribution behavior in an electrolysis cell by dividing the electrolytic bath into non-homogenous concentration zones using discrete elements. The different mechanisms related to the alumina distribution are discussed in detail. Moreover, with a detailed electrical model, it is possible to calculate the current distribution among the different anodic assemblies. With this information, the model can evaluate if low-voltage emissions are likely to be present under the simulated conditions. Using the simulator will help the understanding of the role of the alumina distribution which, in turn, will improve the cell energy consumption and stability while reducing the occurrence of high- and low-voltage anode effects.

  2. Structured Ni catalysts on porous anodic alumina membranes for methane dry reforming: NiAl 2 O 4 formation and characterization

    KAUST Repository

    Zhou, Lu

    2015-06-29

    This communication presents the successful design of a structured catalyst based on porous anodic alumina membranes for methane dry reforming. The catalyst with a strong Ni-NiAl2O4 interaction shows both excellent activity and stability. This journal is © The Royal Society of Chemistry.

  3. Structured Ni catalysts on porous anodic alumina membranes for methane dry reforming: NiAl 2 O 4 formation and characterization

    KAUST Repository

    Zhou, Lu; Guo, Y.; Basset, Jean-Marie; Kameyama, H.

    2015-01-01

    This communication presents the successful design of a structured catalyst based on porous anodic alumina membranes for methane dry reforming. The catalyst with a strong Ni-NiAl2O4 interaction shows both excellent activity and stability. This journal is © The Royal Society of Chemistry.

  4. FIB-SEM investigation of trapped intermetallic particles in anodic oxide films on AA1050 aluminium

    DEFF Research Database (Denmark)

    Jariyaboon, Manthana; Møller, Per; Dunin-Borkowski, Rafal E.

    2011-01-01

    -containing intermetallic particles incorporated into the anodic oxide films on industrially pure aluminium (AA1050, 99.5 per cent) has been investigated. AA1050 aluminium was anodized in a 100?ml/l sulphuric acid bath with an applied voltage of 14?V at 20°C ±2°C for 10 or 120?min. The anodic film subsequently was analyzed......Purpose - The purpose of this investigation is to understand the structure of trapped intermetallics particles and localized composition changes in the anodized anodic oxide film on AA1050 aluminium substrates. Design/methodology/approach - The morphology and composition of Fe......-shaped particles were embedded in the anodic oxide film as a thin strip structure and located near the top surface of the film, whereas the round-shaped particles were trapped in the film with a spherical structure, but partially dissolved and were located throughout the thickness of the anodic film. The Fe...

  5. Experimentally validated dispersion tailoring in a silicon strip waveguide with alumina thin-film coating

    DEFF Research Database (Denmark)

    Guo, Kai; Christensen, Jesper Bjerge; Shi, Xiaodong

    2018-01-01

    We propose a silicon strip waveguide structure with alumina thin-film coating in-between the core and the cladding for group-velocity dispersion tailoring. By carefully designing the core dimension and the coating thickness, a spectrally-flattened near-zero anomalous group-velocity dispersion...

  6. Formation of Flower-Like Crystals of Tris(8-hydroxyquinolinealuminum from 8-Hydroxyquinoline on Anodic Porous Alumina

    Directory of Open Access Journals (Sweden)

    Shohei Yamaguchi

    2017-01-01

    Full Text Available The treatment of anodic porous alumina (APA plates in heated water containing 8-hydroxyquinoline (HQ produces crystalline tris(8-hydroxyquinolinealuminum (Alq3 microbelts about 5–10 μm wide and 5–20 μm long. These microbelts were found to aggregate to form flower-like structures on the surface. X-ray diffraction studies indicated that the Alq3 microbelts are composed of an α-phase having a meridional structure. The Alq3 microbelts exhibited green photoluminescence with a peak at around 520 nm. Scanning electron microscope images and energy dispersive X-ray spectra showed that this reaction is induced at the APA surface by the reaction between the HQ and amorphous Al2O3 species.

  7. The simulation of the temperature effects on the microhardness of anodic alumina oxide layers

    Directory of Open Access Journals (Sweden)

    M. Gombár

    2014-01-01

    Full Text Available In order to improve the mechanical properties of the layer deposited by anodic oxidation of aluminum on the material EN AW-1050 H24, in the contribution was investigated the microhardness of the deposited layer as a function of the physic-chemical factors affecting in the process of anodic oxidation at the constant anodic current density J = 3 A.dm-2 in electrolyte formed by sulfuric acid and oxalic acid, with the emphasis on the influence of electrolyte temperature in the range – 1,78 °C to 45,78 °C. The model of the studied dependence was compiled based on mathematical and statistical analysis of matrix from experimental obtained data from composite rotation plan of experiment with five independent variable factors (amount of sulfuric acid in the electrolyte, the amount of oxalic acid in the electrolyte, electrolyte, anodizing time and applied voltage.

  8. Self-Ordered Nanoporous Alumina Templates Formed by Anodization of Aluminum in Oxalic Acid

    Science.gov (United States)

    Vida-Simiti, Ioan; Nemes, Dorel; Jumate, Nicolaie; Thalmaier, Gyorgy; Sechel, Niculina

    2012-10-01

    Anodic aluminum oxide (AAO) membranes with highly ordered nanopores serve as ideal templates for the formation of various nanostructured materials. The procedure of the template preparation is based on a two-step self-organized anodization of aluminum. In the current study, AAO templates were fabricated in 0.3 M oxalic acid under the anodizing potential range of 30-60 V at an electrolyte temperature of ~5°C. The AAO templates were analyzed using scanning electron microscopy, x-ray diffraction, Fourier-transform infrared spectroscopy, and differential thermal analysis. The as obtained layers are amorphous; the mean pore size is between 40 nm and 75 nm and increases with the increase of the anodization potential. Well-defined pores across the whole aluminum template, a pore density of ~1010 pores/cm2, and a tendency to form a porous structure with hexagonal symmetry were observed.

  9. Effect of various de-anodizing techniques on the surface stability of non-colored and colored nanoporous AAO films in acidic solution

    Energy Technology Data Exchange (ETDEWEB)

    Awad, Ahmed M. [Chemical Engineering & Pilot Plant Department, National Research Centre, Dokki, Giza (Egypt); Shehata, Omnia S. [Physical Chemistry Department, National Research Centre, Dokki, Giza (Egypt); Heakal, Fakiha El-Taib, E-mail: fakihaheakal@yahoo.com [Chemistry Department, Faculty of Science, Cairo University, Giza 12613 (Egypt)

    2015-12-30

    Highlights: • Three de-anodization methods were used during two-step fabrication of nanoporous AAO. • Electrolytic etching (EE), chemical etching with H{sub 3}PO{sub 4} (PE) or NaOH (HE) were adopted. • After the second anodizing step, HE film was the thinnest as compared to EE and HE. • Stability order of nanoporous AAO films in 0.5 M HCl solution was: PE > EE > HE. • For the colored films by electrodeposited Cu atoms, the order was: HE > EE > PE. - Abstract: Anodic aluminum oxide (AAO) is well known as an important nanostructured material, and a useful template in the fabrication of nanostructures. Nanoporous anodic alumina (PAA) with high open porosity was prepared by adopting three de-anodizing regimes following the first anodizing step and preceding the second one. The de-anodizing methods include electrolytic etching (EE) and chemical etching using either phosphoric acid (PE) or sodium hydroxide (HE) solutions. Three of the obtained AAO samples were black colored by electrodeposition of copper nanoparticles in their pores. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to characterize the electrochemical performance of the two sets of the prepared samples. In general, the data obtained in aggressive aerated 0.5 M HCl solution demonstrated dissimilar behavior for the three prepared samples despite that the second anodizing step was the same for all of them. The data indicated that the resistance and thickness of the inner barrier part of nano-PAA film, are the main controlling factors determining its stability. On the other hand, coloring the film decreased its stability due to the galvanic effect. The difference in the electrochemical behavior of the three colored samples was discussed based on the difference in both the pore size and thickness of the outer porous part of PAA film as supported by SEM, TEM and cross-sectional micrographs. These results can thus contribute for better engineering

  10. Interface termination and band alignment of epitaxially grown alumina films on Cu-Al alloy

    Science.gov (United States)

    Yoshitake, Michiko; Song, Weijie; Libra, Jiří; Mašek, Karel; Šutara, František; Matolín, Vladimír; Prince, Kevin C.

    2008-02-01

    Epitaxial ultrathin alumina films were grown on a Cu-9 at. % Al(111) substrate by selective oxidation of Al in the alloy in ultrahigh vacuum. The photoelectron spectra of Al 2p and valence band were measured in situ during oxidation. By analyzing multiple peaks of Al 2p, the interface atomic structure was discussed. The energy difference between the Fermi level of the substrate and the valence band maximum of alumina (band offset) was obtained. The relation between the interface atomic structure and the band offset was compared with the reported first-principles calculations. A novel method for controlling the band offset was proposed.

  11. Non-isothermal kinetics of phase transformations in magnetron sputtered alumina films with metastable structure

    International Nuclear Information System (INIS)

    Zuzjaková, Š.; Zeman, P.; Kos, Š.

    2013-01-01

    Highlights: • Non-isothermal kinetics of phase transformations in alumina films was investigated. • The structure of alumina films affects kinetics of the transformation processes. • Kinetic triplets of all transformation processes were determined. • The KAS, FWO, FR and IKP methods for determination of E a and A were used. • The Málek method for determination of the kinetic model was used. - Abstract: The paper reports on non-isothermal kinetics of transformation processes in magnetron sputtered alumina thin films with an amorphous and γ-phase structure leading ultimately to the formation of the thermodynamically stable α-Al 2 O 3 phase. Phase transformation sequences in the alumina films were investigated using differential scanning calorimetry (DSC) at four different heating rates (10, 20, 30, 40 °C/min). Three isoconversional methods (Kissinger–Akahira–Sunose (KAS), Flynn–Wall–Ozawa (FWO) and Friedman (FR) method) as well as the invariant kinetic parameters (IKP) method were used to determine the activation energies for transformation processes. Moreover, the pre-exponential factors were determined using the IKP method. The kinetic models of the transformation processes were determined using the Málek method. It was found that the as-deposited structure of alumina films affects kinetics of the transformation processes. The film with the amorphous as-deposited structure heated at 40 °C/min transforms to the crystalline γ phase at a temperature of ∼930 °C (E a,IKP = 463 ± 10 kJ/mol) and subsequently to the crystalline α phase at a temperature of ∼1200 °C (E a,IKP = 589 ± 10 kJ/mol). The film with the crystalline γ-phase structure heated at 40 °C/min is thermally stable up to ∼1100 °C and transforms to the crystalline α phase (E a,IKP = 511 ± 16 kJ/mol) at a temperature of ∼1195 °C. The empirical two-parameter Šesták–Berggren kinetic model was found to be the most adequate one to describe all transformation processes

  12. Systematic in vitro nanotoxicity study on anodic alumina nanotubes with engineered aspect ratio: understanding nanotoxicity by a nanomaterial model.

    Science.gov (United States)

    Wang, Ye; Kaur, Gagandeep; Zysk, Aneta; Liapis, Vasilios; Hay, Shelley; Santos, Abel; Losic, Dusan; Evdokiou, Andreas

    2015-04-01

    Here, we report a detailed and systematic approach for studying the in vitro nanotoxicity study of high aspect ratio (HAR) nanomaterials using anodic alumina nanotubes (AANTs) as a nanomaterial model. AANTs with bio-inert properties and tailored aspect ratios ranging from 7.8 to 63.3 were synthesized by an electrochemical pulse anodization process. Cytotoxicity studies were conducted with RAW 264.7 mouse macrophage cells and MDA-MB 231-TXSA human breast cancer cells through several toxicity parameters, including cell viability and morphology, pro-inflammatory response, mitochondrial depolarization, lysosomal membrane permeabilization (LMP), induction of autophagy and endoplasmic reticulum (ER) stress. The resulting toxicity patterns were cell-type dependent and strongly related with AANTs dose, length of time, and importantly the AR of AANTs. Long AANTs triggered enhanced cell death, morphological changes, tumor necrosis factor α (TNF-α) release, LMP and ER stress than short AANTs. The toxic AR window of AANTs was determined to be 7.8, which is shorter than that of other previously reported HAR nanomaterials. This toxic AR window provides a promising opportunity to control the nanotoxicity of HAR nanomaterials for their advanced drug delivery application. Copyright © 2014 Elsevier Ltd. All rights reserved.

  13. Effect of various de-anodizing techniques on the surface stability of non-colored and colored nanoporous AAO films in acidic solution

    Science.gov (United States)

    Awad, Ahmed M.; Shehata, Omnia S.; Heakal, Fakiha El-Taib

    2015-12-01

    Anodic aluminum oxide (AAO) is well known as an important nanostructured material, and a useful template in the fabrication of nanostructures. Nanoporous anodic alumina (PAA) with high open porosity was prepared by adopting three de-anodizing regimes following the first anodizing step and preceding the second one. The de-anodizing methods include electrolytic etching (EE) and chemical etching using either phosphoric acid (PE) or sodium hydroxide (HE) solutions. Three of the obtained AAO samples were black colored by electrodeposition of copper nanoparticles in their pores. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to characterize the electrochemical performance of the two sets of the prepared samples. In general, the data obtained in aggressive aerated 0.5 M HCl solution demonstrated dissimilar behavior for the three prepared samples despite that the second anodizing step was the same for all of them. The data indicated that the resistance and thickness of the inner barrier part of nano-PAA film, are the main controlling factors determining its stability. On the other hand, coloring the film decreased its stability due to the galvanic effect. The difference in the electrochemical behavior of the three colored samples was discussed based on the difference in both the pore size and thickness of the outer porous part of PAA film as supported by SEM, TEM and cross-sectional micrographs. These results can thus contribute for better engineering applications of nanoporous AAO.

  14. Analysis of physical factors on chosen properties of anodic alumina oxide (AAO layers and environment

    Directory of Open Access Journals (Sweden)

    M. Gombár

    2016-10-01

    Full Text Available In the contribution is evaluated an impact of physical factors of anodizing process, namely the temperature of an electrolyte, anodizing time and voltage, on the change of values of Vickers microhardness and thickness of formed layer of experimental materials Al99∙5. By increasing of electrolyte temperature, the values of layer microhardness and thickness layer increase, namely about 0.78 % at the increasing of electrolyte temperature by 1 °C. By lengthening of anodizing time grows the value of layer thickness, but only to the value of the critical deposition time, when chemical dissolution of the layer start to be more prominent. By voltage increasing, values of layer thickness and micro-hardness are increased in the range of the used experimental values.

  15. Structural transformation of nickel hydroxide films during anodic oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Crocker, Robert W. [Univ. of California, Berkeley, CA (United States); Muller, Rolf H. [Univ. of California, Berkeley, CA (United States)

    1992-05-01

    The transformation of anodically formed nickel hydroxide/oxy-hydroxide electrodes has been investigated. A mechanism is proposed for the anodic oxidation reaction, in which the reaction interface between the reduced and oxidized phases of the electrode evolves in a nodular topography that leads to inefficient utilization of the active electrode material. In the proposed nodular transformation model for the anodic oxidation reaction, nickel hydroxide is oxidized to nickel oxy-hydroxide in the region near the metal substrate. Since the nickel oxy-hydroxide is considerably more conductive than the surrounding nickel hydroxide, as further oxidation occurs, nodular features grow rapidly to the film/electrolyte interface. Upon emerging at the electrolyte interface, the reaction boundary between the nickel hydroxide and oxy-hydroxide phases spreads laterally across the film/electrolyte interface, creating an overlayer of nickel oxy-hydroxide and trapping uncharged regions of nickel hydroxide within the film. The nickel oxy-hydroxide overlayer surface facilitates the oxygen evolution side reaction. Scanning tunneling microscopy of the electrode in its charged state revealed evidence of 80 - 100 Angstrom nickel oxy-hydroxide nodules in the nickel hydroxide film. In situ spectroscopic ellipsometer measurements of films held at various constant potentials agree quantitatively with optical models appropriate to the nodular growth and subsequent overgrowth of the nickel oxy-hydroxide phase. A two-dimensional, numerical finite difference model was developed to simulate the current distribution along the phase boundary between the charged and uncharged material. The model was used to explore the effects of the physical parameters that govern the electrode behavior. The ratio of the conductivities of the nickel hydroxide and oxy-hydroxide phases was found to be the dominant parameter in the system.

  16. Structural transformation of nickel hydroxide films during anodic oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Crocker, R.W.; Muller, R.H.

    1992-05-01

    The transformation of anodically formed nickel hydroxide/oxy-hydroxide electrodes has been investigated. A mechanism is proposed for the anodic oxidation reaction, in which the reaction interface between the reduced and oxidized phases of the electrode evolves in a nodular topography that leads to inefficient utilization of the active electrode material. In the proposed nodular transformation model for the anodic oxidation reaction, nickel hydroxide is oxidized to nickel oxy-hydroxide in the region near the metal substrate. Since the nickel oxy-hydroxide is considerably more conductive than the surrounding nickel hydroxide, as further oxidation occurs, nodular features grow rapidly to the film/electrolyte interface. Upon emerging at the electrolyte interface, the reaction boundary between the nickel hydroxide and oxy-hydroxide phases spreads laterally across the film/electrolyte interface, creating an overlayer of nickel oxy-hydroxide and trapping uncharged regions of nickel hydroxide within the film. The nickel oxy-hydroxide overlayer surface facilitates the oxygen evolution side reaction. Scanning tunneling microscopy of the electrode in its charged state revealed evidence of 80 {endash} 100 Angstrom nickel oxy-hydroxide nodules in the nickel hydroxide film. In situ spectroscopic ellipsometer measurements of films held at various constant potentials agree quantitatively with optical models appropriate to the nodular growth and subsequent overgrowth of the nickel oxy-hydroxide phase. A two-dimensional, numerical finite difference model was developed to simulate the current distribution along the phase boundary between the charged and uncharged material. The model was used to explore the effects of the physical parameters that govern the electrode behavior. The ratio of the conductivities of the nickel hydroxide and oxy-hydroxide phases was found to be the dominant parameter in the system.

  17. Anodic luminescence, structural, photoluminescent, and photocatalytic properties of anodic oxide films grown on niobium in phosphoric acid

    Energy Technology Data Exchange (ETDEWEB)

    Stojadinović, Stevan, E-mail: sstevan@ff.bg.ac.rs [University of Belgrade, Faculty of Physics, Studentski trg 12-16, 11000 Belgrade (Serbia); Tadić, Nenad [University of Belgrade, Faculty of Physics, Studentski trg 12-16, 11000 Belgrade (Serbia); Radić, Nenad [University of Belgrade, Institute of Chemistry, Technology and Metallurgy, Department of Catalysis and Chemical Engineering, Njegoševa 12, 11000 Belgrade (Serbia); Stefanov, Plamen [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Block 11, 1113 Sofia (Bulgaria); Grbić, Boško [University of Belgrade, Institute of Chemistry, Technology and Metallurgy, Department of Catalysis and Chemical Engineering, Njegoševa 12, 11000 Belgrade (Serbia); Vasilić, Rastko [University of Belgrade, Faculty of Physics, Studentski trg 12-16, 11000 Belgrade (Serbia)

    2015-11-15

    Graphical abstract: - Highlights: • Anodic luminescence is correlated to the existence of morphological defects in the oxide. • Spectrum under spark discharging reveals only oxygen and hydrogen lines. • Oxide films formed under spark discharging are crystallized and composed of Nb{sub 2}O{sub 5}. • Photocatalytic activity and photoluminescence of Nb{sub 2}O{sub 5} films increase with time. - Abstract: This article reports on properties of oxide films obtained by anodization of niobium in phosphoric acid before and after the dielectric breakdown. Weak anodic luminescence of barrier oxide films formed during the anodization of niobium is correlated to the existence of morphological defects in the oxide layer. Small sized sparks generated by dielectric breakdown of formed oxide film cause rapid increase of luminescence intensity. The luminescence spectrum of obtained films on niobium under spark discharging is composed of continuum radiation and spectral lines caused by electronic spark discharging transitions in oxygen and hydrogen atoms. Oxide films formed before the breakdown are amorphous, while after the breakdown oxide films are partly crystalline and mainly composed of Nb{sub 2}O{sub 5} hexagonal phase. The photocatalytic activity of obtained oxide films after the breakdown was investigated by monitoring the degradation of methyl orange. Increase of the photocatalytic activity with time is related to an increase of oxygen vacancy defects in oxide films formed during the process. Also, higher concentration of oxygen vacancy defects in oxide films results in higher photoluminescence intensity.

  18. Study on Pt-structured anodic alumina catalysts for catalytic combustion of toluene: Effects of competitive adsorbents and competitive impregnation methods

    Science.gov (United States)

    Zhang, Qi; Luan, Hongjuan; Li, Tao; Wu, Yongqiang; Ni, Yanhui

    2016-01-01

    Novel competitive impregnation methods were used to prepare high dispersion Pt-structured anodic alumina catalysts. It is found that competitive adsorbents owning different acidity result in different Pt loading amount and also exert great effects on Pt distribution, particle size and redox ability. The suitable adsorption ability of lactic acid led to its best activity for catalytic combustion of toluene. Co-competitive and pre-competitive impregnation methods were also compared and the mechanisms of two competitive methods were proposed. Co-competitive impregnation made Pt distribute more uniformly through pore channels and resulted in better catalytic activity, because of the weaker spatial constraint effect of lactic acid. Furthermore, the optimized Pt-structured anodic alumina catalyst also showed a good chlorine-resistance under moisture atmosphere, because water could promote the reaction of dichloromethane (DCM) transformation and clean chloride by-products to release more active sites.

  19. Fabrication and characterisation of embedded metal nanostructures by ion implantation with nanoporous anodic alumina masks

    Energy Technology Data Exchange (ETDEWEB)

    Guan, Wei [NanoLAB, Department of Materials Science and Engineering, University of Sheffield, Sheffield S1 3JD (United Kingdom); School of Physics and Astronomy, University of Edinburgh, Mayfield Road, Edinburgh EH9 3JZ (United Kingdom); Peng, Nianhua, E-mail: n.peng@surrey.ac.uk [Surrey Ion Beam Centre, Surrey University, Guildford GU2 7XH (United Kingdom); Jeynes, Christopher [Surrey Ion Beam Centre, Surrey University, Guildford GU2 7XH (United Kingdom); Ghatak, Jay [NanoLAB, Department of Materials Science and Engineering, University of Sheffield, Sheffield S1 3JD (United Kingdom); Peng, Yong [NanoLAB, Department of Materials Science and Engineering, University of Sheffield, Sheffield S1 3JD (United Kingdom); School of Physical Science and Technology, Lanzhou University, 222 Tianshui Road, Lanzhou 730000 (China); Ross, Ian M. [Department of Electronic and Electric Engineering, University of Sheffield, Sheffield S1 3JD (United Kingdom); Bhatta, Umananda M.; Inkson, Beverley J.; Möbus, Günter [NanoLAB, Department of Materials Science and Engineering, University of Sheffield, Sheffield S1 3JD (United Kingdom)

    2013-07-15

    Lateral ordered Co, Pt and Co/Pt nanostructures were fabricated in SiO{sub 2} and Si{sub 3}N{sub 4} substrates by high fluence metal ion implantation through periodic nanochannel membrane masks based on anodic aluminium oxides (AAO). The quality of nanopatterning transfer defined by various AAO masks in different substrates was examined by transmission electron microscopy (TEM) in both imaging and spectroscopy modes.

  20. Mechanical constraint and release generates long, ordered horizontal pores in anodic alumina templates

    International Nuclear Information System (INIS)

    Bolger, Ciara T; Petkov, Nikolay; Holmes, Justin D; Fois, Giovanni; Cross, Graham L W; Sassiat, Nicolas; Burke, Micheál; Quinn, Aidan J

    2012-01-01

    We describe the formation of long, highly ordered arrays of planar oriented anodic aluminum oxide (AAO) pores during plane parallel anodization of thin aluminum ‘finger’ microstructures fabricated on thermally oxidized silicon substrates and capped with a silicon oxide layer. The pore morphology was found to be strongly influenced by mechanical constraint imposed by the oxide layers surrounding the Al fingers. Tractions induced by the SiO 2 substrate and capping layer led to frustrated volume expansion and restricted oxide flow along the interface, with extrusion of oxide into the primary pore volume, leading to the formation of dendritic pore structures and meandering pore growth. However, partial relief of the constraint by a delaminating interfacial fracture, with its tip closely following the anodization front, led to pore growth that was highly ordered with regular, hexagonally packed arrays of straight horizontal pores up to 3 µm long. Detailed characterization of both straight and dendritic planar pores over a range of formation conditions using advanced microscopy techniques is reported, including volume reconstruction, enabling high quality 3D visualization of pore formation. (paper)

  1. Dissolution of anodic zirconium dioxide films in aqueous media

    International Nuclear Information System (INIS)

    Merati, A.; Cox, B.

    1999-01-01

    Zirconium with a low thermal neutron cross section, good corrosion resistance in high-temperature water, and high thermal conductivity is an ideal material for nuclear reactors. Its good resistance to water and steam at reactor temperatures is of the greatest interest to nuclear fuel designers. Dissolution of zirconium dioxide (ZrO 2 ) films in aggressive media was investigated. The extent of uniform and localized dissolution was measured by ultraviolet-visible (UV-VIS) spectrometry and an alternating current (AC) impedance test, respectively. Scanning electron microscopy (SEM) showed the extent of dissolution of ZrO 2 was a function only of the fluoride ion content and pH of the medium. Cathodic polarization was used to identify the preferred sites for localized dissolution of the oxide film. In 0.1 M potassium bifluoride (KHF 2 ), both uniform thinning and local breakdown of the oxide were observed. Within the limits of the investigating techniques, no evidence of dissolution was observed in the other solutions tested: 0.5 M sulfuric acid (H 2 SO 4 ). 1.0 M nitric acid (HNO 3 ), 5 M hydrochloric acid (HCl), or 0.1 M potassium fluoride (KF). In areas around iron-containing particles, fine cracks in the anodic oxide at prior metal grain boundaries and arrays of cracks in the oxide associated with residual scratches from the initial specimen preparation were the preferred spots for localized dissolution of the oxide film. Iron precipitates immediately below the surface of the oxide layer increased the local electrical conductivity. Enrichment of iron in the oxide matrix around these precipitates during the anodization process appeared to cause prospective spots, acting as anodic sites for pH formation

  2. Room temperature H{sub 2}S gas sensing characteristics of platinum (Pt) coated porous alumina (PoAl) thick films

    Energy Technology Data Exchange (ETDEWEB)

    More, P.S., E-mail: p_smore@yahoo.co.in [Department of Physics, Institute of Science, Mumbai 400 032 (India); Raut, R.W. [Department of Botany, Institute of Science, Mumbai 400 032 (India); Ghuge, C.S. [Department of Physics, Institute of Science, Mumbai 400 032 (India)

    2014-02-14

    The study reports H{sub 2}S gas sensing characteristics of platinum (Pt) coated porous alumina (PoAl) films. The porous alumina (PoAl) thick layers were formed in the dark on aluminum substrates using an electrochemical anodization method. Thin semitransparent platinum (Pt) films were deposited on PoAl samples using chemical bath deposition (CBD) method. The films were characterized using energy dispersive X-ray analysis (EDAX) and scanning electron microscopy (SEM). The thicknesses of coated and bare films were measured using ellipsometry. The sensing properties such as sensitivity factor (S.F.), response time, recovery time and repeatability were measured using a static gas sensing system for H{sub 2}S gas. The EDAX studies confirmed the purity of Pt–PoAl film and indicated the formation of pure platinum (Pt) phase. The ellipsometry studies revealed the thickness of PoAl layer of about 15–17 μm on aluminum substrates. The SEM studies demonstrated uniform distribution of spherical pores with a size between 0.250 and 0.500 μm for PoAl film and nearly spherical platinum particles with average particle size ∼100 nm for Pt–PoAl film. The gas-sensing properties of these samples were studied in a home-built static gas characterization system. The H{sub 2}S gas sensing properties of Pt–PoAl at 1000 ppm of H{sub 2}S gave maximum sensitivity factor (S.F.) = 1200. The response time and recovery time were found to be 2–3 min and ∼1 min respectively. Further, the measurement of H{sub 2}S gas sensing properties clearly indicated the repeatability of gas sensing response of Pt–PoAl film. The present study indicated the significant potential of Pt coated PoAl films for H{sub 2}S gas sensing applications in diverse areas. - Highlights: • Electrochemical anodization, cheap and effective method for fabrication of PoAl. • Chemical bath deposition, a simple and effective method for deposition of Pt on PoAl. • A nano-composite film sensor with high sensitivity

  3. Structural features of anodic oxide films formed on aluminum substrate coated with self-assembled microspheres

    International Nuclear Information System (INIS)

    Asoh, Hidetaka; Uchibori, Kota; Ono, Sachiko

    2009-01-01

    The structural features of anodic oxide films formed on an aluminum substrate coated with self-assembled microspheres were investigated by scanning electron microscopy and atomic force microscopy. In the first anodization in neutral solution, the growth of a barrier-type film was partially suppressed in the contact area between the spheres and the underlying aluminum substrate, resulting in the formation of ordered dimple arrays in an anodic oxide film. After the subsequent second anodization in acid solution at a voltage lower than that of the first anodization, nanopores were generated only within each dimple. The nanoporous region could be removed selectively by post-chemical etching using the difference in structural dimensions between the porous region and the surrounding barrier region. The mechanism of anodic oxide growth on the aluminum substrate coated with microspheres through multistep anodization is discussed.

  4. Structural features of anodic oxide films formed on aluminum substrate coated with self-assembled microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Asoh, Hidetaka [Department of Applied Chemistry, Faculty of Engineering, Kogakuin University, 2665-1 Nakano, Hachioji, Tokyo 192-0015 (Japan)], E-mail: asoh@cc.kogakuin.ac.jp; Uchibori, Kota; Ono, Sachiko [Department of Applied Chemistry, Faculty of Engineering, Kogakuin University, 2665-1 Nakano, Hachioji, Tokyo 192-0015 (Japan)

    2009-07-15

    The structural features of anodic oxide films formed on an aluminum substrate coated with self-assembled microspheres were investigated by scanning electron microscopy and atomic force microscopy. In the first anodization in neutral solution, the growth of a barrier-type film was partially suppressed in the contact area between the spheres and the underlying aluminum substrate, resulting in the formation of ordered dimple arrays in an anodic oxide film. After the subsequent second anodization in acid solution at a voltage lower than that of the first anodization, nanopores were generated only within each dimple. The nanoporous region could be removed selectively by post-chemical etching using the difference in structural dimensions between the porous region and the surrounding barrier region. The mechanism of anodic oxide growth on the aluminum substrate coated with microspheres through multistep anodization is discussed.

  5. Friction behaviour of anodic oxide film on aluminum impregnated with molybdenum sulfide compounds

    Energy Technology Data Exchange (ETDEWEB)

    Maejima, M.; Saruwatari, K. [Fujikura Ltd., Tokyo (Japan); Takaya, M. [Faculty of Engineering, Chiba Institute of Technology 17-1, Tsudanuma 2-Chome, 275-0016, Narasino-shi Chiba (Japan)

    2000-10-23

    In order to improve the lubricity and wear resistance of aluminum anodic oxide films, it is necessary to ensure the film layers are dense to prevent cracking, and to harden the films as well as reduce the shear stress of the film surfaces. From this view point, lubricious, hard anodic oxide films have been studied in the past, but fully satisfactory results have yet to be realized. In this paper, we report on our study of the re-anodizing of anodic oxide film in an aqueous solution of (NH)MoS. Molybdenum sulfide and compounds filled the 20-nm diameter pores of the film, creating internal stress which compressed the film, suppressing the occurrence of cracks and reducing the friction coefficient. (orig.)

  6. The preparation and corrosion resistance of Ce and Nd modified anodic films on aluminum

    International Nuclear Information System (INIS)

    Li Qizheng; Tang Yuming; Zuo Yu

    2010-01-01

    Rare earth element Ce and Nd modified anodic films were prepared on aluminum surface by a relatively simple method: the aluminum samples were first immersed in Ni(NO 3 ) 2 solutions containing Ce or Nd salts at 90 deg. C, then were dried and anodized. The contents of Ce or Nd in the anodic films were from 0.5% to 0.9%, and about 4-5% Ni was also introduced in the films. The modified anodic films were more compact with much smaller pores and increased hardness. In neutral, acidic and basic NaCl solutions, the rare earth modified films showed obviously improved corrosion resistance. The Ce modified films showed better corrosion resistance than Nd modified films. The cracking resistance of the films under heating was also improved.

  7. Nanostructured thin films of indium oxide nanocrystals confined in alumina matrixes

    International Nuclear Information System (INIS)

    Bouifoulen, A.; Edely, M.; Errien, N.; Kassiba, A.; Outzourhit, A.; Makowska-Janusik, M.; Gautier, N.; Lajaunie, L.; Oueriagli, A.

    2011-01-01

    Nanocrystals of indium oxide (In 2 O 3 ) with sizes below 10 nm were prepared in alumina matrixes by using a co-pulverization method. The used substrates such as borosilicate glasses or (100) silicon as well as the substrate temperatures during the deposition process were modified and their effects characterized on the structural and physical properties of alumina-In 2 O 3 films. Complementary investigation methods including X-ray diffraction, optical transmittance in the range 250-1100 nm and transmission electron microscopy were used to analyze the nanostructured films. The crystalline order, morphology and optical responses were monitored as function of the deposition parameters and the post-synthesis annealing. The optimal conditions were found and allow realizing suitable nanostructured films with a major crystalline order of cubic phase for the In 2 O 3 nanocrystals. The optical properties of the films were analyzed and the key parameters such as direct and indirect band gaps were evaluated as function of the synthesis conditions and the crystalline quality of the films.

  8. X-ray photoelectron spectroscopy study of excimer laser treated alumina films

    Science.gov (United States)

    Georgiev, D. G.; Kolev, K.; Laude, L. D.; Mednikarov, B.; Starbov, N.

    1998-01-01

    Amorphous alumina layers are deposited on a single crystal Si substrate by a e-gun evaporation technique. These films are then thermally annealed in oxygen to be crystallized and, further, irradiated with an excimer laser beam. At each stage of the film preparation, an x-ray photoelectron spectroscopy analysis is performed at the film surface and in depth, upon ion beam grinding. Results give evidence for the formation of an aluminosilicate upon thermal annealing of the film in oxygen. At the surface itself, this compound is observed to decompose upon excimer laser irradiation at energy densities exceeding 1.75 J/cm2, giving rise to free Si atoms and SiO2, however with complete disappearance of Al atoms. Model photochemical reactions are proposed to explain such transformations.

  9. Fabrication of superhydrophobic niobium pentoxide thin films by anodization

    Energy Technology Data Exchange (ETDEWEB)

    Jeong, Bong-Yong [Future Convergence Ceramic Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of); Jung, Eun-Hye [Future Convergence Ceramic Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of); Department of Chemical Engineering, Inha University, Incheon 402-024 (Korea, Republic of); Kim, Jin-Ho, E-mail: jhkim@kicet.re.kr [Electronic and Optic Materials Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of)

    2014-07-01

    We report a simple method to fabricate a niobium oxide film with a lotus-like micro–nano surface structure. Self-assembled niobium pentoxide (Nb{sub 2}O{sub 5}) films with superhydrophobic property were fabricated by an anodization and a hydrophobic treatment. This process has several advantages such as low cost, simplicity and easy coverage of a large area. The surface of fabricated Nb{sub 2}O{sub 5} film was changed from hydrophilic to superhydrophobic surface by a treatment using fluoroaldyltrimethoxysilane (FAS) solution. This value is considered to be the lowest surface free energy of any solid, based on the alignment of -CF{sub 3} groups on the surface. In particular, among FAS coated surfaces, the micro–nano complex cone structured Nb{sub 2}O{sub 5} film showed the highest water-repellent property with a static contact angle of ca. 162°. This study gives promising routes from biomimetic superhydrophobic surfaces.

  10. Luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid

    International Nuclear Information System (INIS)

    Stojadinovic, S.; Vasilic, R.; Petkovic, M.; Nedic, Z.; Kasalica, B.; Belca, I.; Zekovic, Lj.

    2010-01-01

    In this paper, we have investigated luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid. For the first time we have measured weak luminescence during anodization of aluminum in this electrolyte (so-called galvanoluminescence GL) and showed that there are wide GL bands in the visible region of the spectrum and observed two dominant spectral peaks. The first one is at about 425 nm, and the second one shifts with anodization voltage. As the anodization voltage approaches the breakdown voltage, a large number of sparks appear superimposed on the anodic GL. Several intensive band peaks were observed under breakdown caused by electron transitions in W, P, Al, O, H atoms. Furthermore, photoluminescence (PL) of anodic oxide films and anodic-spark formed oxide coatings were performed. In both cases wide PL bands in the range from 320 nm to 600 nm were observed.

  11. Optical properties of InP/ZnS quantum dots deposited into nanoporous anodic alumina

    International Nuclear Information System (INIS)

    Savchenko, S S; Vokhmintsev, A S; Weinstein, I A

    2016-01-01

    Spectral characteristics of InP/ZnS core/shell colloidal quantum dots of two different sizes (QD-1 and QD-2) were investigated. Absorption and luminescence spectra were analyzed for a series of solutions with a concentration range from 0.04 to 40 g/l. Energies of the optical transitions are evaluated. The obtained values of 2.60 eV (QD-1) and 2.38 eV (QD-2) correspond to the InP first excitonic transitions while 4.06 (QD-2) and 4.70 eV (QD-1, QD-2) are assumed to be caused by the ZnS shell absorption. Structures based on nanoporous anodic aluminum oxide (AAO) with the QDs were synthesized via an electrochemical oxidation and ultrasonic-assisted deposition. Chromaticity coordinates and correlated color temperatures for all phosphors under study were calculated. The fabrication possibilities of InP/ZnS@AAO nanostructures with tunable emission color (including the border of white region) were shown. (paper)

  12. Optical properties of InP/ZnS quantum dots deposited into nanoporous anodic alumina

    Science.gov (United States)

    Savchenko, S. S.; Vokhmintsev, A. S.; Weinstein, I. A.

    2016-08-01

    Spectral characteristics of InP/ZnS core/shell colloidal quantum dots of two different sizes (QD-1 and QD-2) were investigated. Absorption and luminescence spectra were analyzed for a series of solutions with a concentration range from 0.04 to 40 g/l. Energies of the optical transitions are evaluated. The obtained values of 2.60 eV (QD-1) and 2.38 eV (QD-2) correspond to the InP first excitonic transitions while 4.06 (QD-2) and 4.70 eV (QD-1, QD-2) are assumed to be caused by the ZnS shell absorption. Structures based on nanoporous anodic aluminum oxide (AAO) with the QDs were synthesized via an electrochemical oxidation and ultrasonic-assisted deposition. Chromaticity coordinates and correlated color temperatures for all phosphors under study were calculated. The fabrication possibilities of InP/ZnS@AAO nanostructures with tunable emission color (including the border of white region) were shown.

  13. Optimization of Aluminum Anodization Conditions for the Fabrication of Nanowires by Electrodeposition

    Science.gov (United States)

    Fucsko, Viola

    2005-01-01

    Anodized alumina nanotemplates have a variety of potential applications in the development of nanotechnology. Alumina nanotemplates are formed by oxidizing aluminum film in an electrolyte solution.During anodization, aluminum oxidizes, and, under the proper conditions, nanometer-sized pores develop. A series of experiments was conducted to determine the optimal conditions for anodization. Three-micrometer thick aluminum films on silicon and silicon oxide substrates were anodized using constant voltages of 13-25 V. 0.1-0.3M oxalic acid was used as the electrolyte. The anodization time was found to increase and the overshooting current decreased as both the voltage and the electrolyte concentrations were decreased. The samples were observed under a scanning electron microscope. Anodizing with 25V in 0.3M oxalic acid appears to be the best process conditions. The alumina nanotemplates are being used to fabricate nanowires by electrodeposition. The current-voltage characteristics of copper nanowires have also been studied.

  14. Realisation and advanced engineering of true optical rugate filters based on nanoporous anodic alumina by sinusoidal pulse anodisation

    Science.gov (United States)

    Santos, Abel; Yoo, Jeong Ha; Rohatgi, Charu Vashisth; Kumeria, Tushar; Wang, Ye; Losic, Dusan

    2016-01-01

    This study is the first realisation of true optical rugate filters (RFs) based on nanoporous anodic alumina (NAA) by sinusoidal waves. An innovative and rationally designed sinusoidal pulse anodisation (SPA) approach in galvanostatic mode is used with the aim of engineering the effective medium of NAA in a sinusoidal fashion. A precise control over the different anodisation parameters (i.e. anodisation period, anodisation amplitude, anodisation offset, number of pulses, anodisation temperature and pore widening time) makes it possible to engineer the characteristic reflection peaks and interferometric colours of NAA-RFs, which can be finely tuned across the UV-visible-NIR spectrum. The effect of the aforementioned anodisation parameters on the photonic properties of NAA-RFs (i.e. characteristic reflection peaks and interferometric colours) is systematically assessed in order to establish for the first time a comprehensive rationale towards NAA-RFs with fully controllable photonic properties. The experimental results are correlated with a theoretical model (Looyenga-Landau-Lifshitz - LLL), demonstrating that the effective medium of these photonic nanostructures can be precisely described by the effective medium approximation. NAA-RFs are also demonstrated as chemically selective photonic platforms combined with reflectometric interference spectroscopy (RIfS). The resulting optical sensing system is used to assess the reversible binding affinity between a model drug (i.e. indomethacin) and human serum albumin (HSA) in real-time. Our results demonstrate that this system can be used to determine the overall pharmacokinetic profile of drugs, which is a critical aspect to be considered for the implementation of efficient medical therapies.This study is the first realisation of true optical rugate filters (RFs) based on nanoporous anodic alumina (NAA) by sinusoidal waves. An innovative and rationally designed sinusoidal pulse anodisation (SPA) approach in galvanostatic

  15. Photoluminescence emission of nanoporous anodic aluminum oxide films prepared in phosphoric acid

    Science.gov (United States)

    2012-01-01

    The photoluminescence emission of nanoporous anodic aluminum oxide films formed in phosphoric acid is studied in order to explore their defect-based subband electronic structure. Different excitation wavelengths are used to identify most of the details of the subband states. The films are produced under different anodizing conditions to optimize their emission in the visible range. Scanning electron microscopy investigations confirm pore formation in the produced layers. Gaussian analysis of the emission data indicates that subband states change with anodizing parameters, and various point defects can be formed both in the bulk and on the surface of these nanoporous layers during anodizing. PMID:23272786

  16. Preparation of Aluminum Nanomesh Thin Films from an Anodic Aluminum Oxide Template as Transparent Conductive Electrodes

    Science.gov (United States)

    Li, Yiwen; Chen, Yulong; Qiu, Mingxia; Yu, Hongyu; Zhang, Xinhai; Sun, Xiao Wei; Chen, Rui

    2016-02-01

    We have employed anodic aluminum oxide as a template to prepare ultrathin, transparent, and conducting Al films with a unique nanomesh structure for transparent conductive electrodes. The anodic aluminum oxide template is obtained through direct anodization of a sputtered Al layer on a glass substrate, and subsequent wet etching creates the nanomesh metallic film. The optical and conductive properties are greatly influenced by experimental conditions. By tuning the anodizing time, transparent electrodes with appropriate optical transmittance and sheet resistance have been obtained. The results demonstrate that our proposed strategy can serve as a potential method to fabricate low-cost TCEs to replace conventional indium tin oxide materials.

  17. Exploding metal film active anode source experiments on the LION extractor ion diode

    International Nuclear Information System (INIS)

    Rondeau, G.D.; Bordonaro, G.J.; Greenly, J.B.; Hammer, D.A.

    1989-01-01

    In this paper the authors report results using an extractor geometry magnetically insulated ion diode on the 0.5 TW LION accelerator. Experiments with an exploding metal film active anode plasma source (EMFAAPS) have shown that intense beams with significantly improved turn-on time compared to epoxy-filled-groove anodes can be produced. A new geometry, in which a plasma switch is used to provide the current path that explodes the thin film anode, has improved the ion efficiency (to typically 70%) compared with the previous scheme in which an electron collector on the anode provided this current. Leakage electron current is reduced when no collector is used

  18. DC magnetron sputtering prepared Ag-C thin film anode for thin film lithium ion microbatteries

    International Nuclear Information System (INIS)

    Li, Y.; Tu, J.P.; Shi, D.Q.; Huang, X.H.; Wu, H.M.; Yuan, Y.F.; Zhao, X.B.

    2007-01-01

    An Ag-C thin film was prepared by DC magnetron co-sputtering, using pure silver and graphite as the targets. The microstructure and morphology of the deposited thin film were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Electrochemical performances of the Ag-C thin film anode were investigated by means of discharge/charge and cyclic voltammogram (CV) tests in model cells. The electrochemical impedance spectrum (EIS) characteristics and the chemical diffusion coefficient, D Li of the Ag-C thin film electrode at different discharging states were discussed. It was believed that the excellent cycling performance of the Ag-C electrode was ascribed to the good conductivity of silver and the volume stability of the thin film

  19. The application of the barrier-type anodic oxidation method to thickness testing of aluminum films

    Science.gov (United States)

    Chen, Jianwen; Yao, Manwen; Xiao, Ruihua; Yang, Pengfei; Hu, Baofu; Yao, Xi

    2014-09-01

    The thickness of the active metal oxide film formed from a barrier-type anodizing process is directly proportional to its formation voltage. The thickness of the consumed portion of the metal film is also corresponding to the formation voltage. This principle can be applied to the thickness test of the metal films. If the metal film is growing on a dielectric substrate, when the metal film is exhausted in an anodizing process, because of the high electrical resistance of the formed oxide film, a sudden increase of the recorded voltage during the anodizing process would occur. Then, the thickness of the metal film can be determined from this voltage. As an example, aluminum films are tested and discussed in this work. This method is quite simple and is easy to perform with high precision.

  20. Influence of titanium and vanadium on the hydrogen transport through amorphous alumina films

    Energy Technology Data Exchange (ETDEWEB)

    Palsson, G.K. [Department of Physics, Uppsala University, Box 530, S-751 21 Uppsala (Sweden); Wang, Y.T. [Department of Physics, Uppsala University, Box 530, S-751 21 Uppsala (Sweden); Azofeifa, D. [Centro de Investigacion en Ciencia e Ingenieria de Materiales and Escuela de Fisica, Universidad de Costa Rica, San Jose (Costa Rica); Raanaei, H. [Department of Physics, Uppsala University, Box 530, S-751 21 Uppsala (Sweden); Department of Physics, Persian Gulf University, Bushehr 75168 (Iran, Islamic Republic of); Sahlberg, M. [Department of Materials Chemistry, Uppsala University, Box 538, S-751 21 Uppsala (Sweden); Hjoervarsson, B. [Department of Physics, Uppsala University, Box 530, S-751 21 Uppsala (Sweden)

    2010-04-02

    The influence of titanium and vanadium on the hydrogen transport rate through thin amorphous alumina films is addressed. Only small changes in the transport rate are observed when the Al{sub 2}O{sub 3} are covered with titanium or vanadium. This is in stark contrast to results with a Pd overlayer, which enhances the transport by an order of magnitude. Similarly, when titanium is embedded into the alumina the transport rate is faster than for the covered case but still slower than the undoped reference. Embedding vanadium in the alumina does not yield an increase in uptake rate compared to the vanadium covered oxide layers. These results add to the understanding of the hydrogen uptake of oxidized metals, especially the alanates, where the addition of titanium has been found to significantly enhance the rate of hydrogen uptake. The current findings eliminate two possible routes for the catalysis of alanates by Ti, namely dissociation and effective diffusion short-cuts formed by Ti. Finally, no photocatalytic enhancement was noticed on the titanium covered samples.

  1. An anodic alumina supported Ni-Pt bimetallic plate-type catalysts for multi-reforming of methane, kerosene and ethanol

    KAUST Repository

    Zhou, Lu

    2014-05-01

    An anodic alumina supported Ni-Pt bimetallic plate-type catalyst was prepared by a two-step impregnation method. The trace amount 0.08 wt% of Pt doping efficiently suppressed the nickel particle sintering and improved the nickel oxides reducibility. The prepared Ni-Pt catalyst showed excellent performance during steam reforming of methane, kerosene and ethanol under both 3000 h stationary and 500-time daily start-up and shut-down operation modes. Self-activation ability of this catalyst was evidenced, which was considered to be resulted from the hydrogen spillover effect over Ni-Pt alloy. In addition, an integrated combustion-reforming reactor was proposed in this study. However, the sintering of the alumina support is still a critical issue for the industrialization of Ni-Pt catalyst. Copyright © 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

  2. The electrochemical properties and mechanism of formation of anodic oxide films on Mg-Al alloys

    International Nuclear Information System (INIS)

    Kim, Seong Jong; Okido, Masazumi

    2003-01-01

    The electronchemical properties and the mechanism of formation of anodic oxide films on Mg alloys containing 0-15 mass% Al, when anodized in NaOH solution, were investigated by focusing on the effects of anodizing potential, Al content, and anodizing time. The intensity ratio of Mg(OH) 2 in the XRD analysis decreased with increasing applied potential, while that of MgO increased. Mg(OH) 2 was barely detected at 80 V, while MgO was readily detected. The anti-corrosion properties of anodized specimens at each constant potential were better than those of non-anodized specimens. The specimen anodized at an applied potential of 3 V had the best anti-corrosion property. The intensity ratio of the β phase increased with aluminum content in Mg-Al alloys. During anodizing, the active dissolution reaction occurred preferentially in β phase until about 4 min, and then the current density increased gradually until 7 min. The dissolution reaction progressed in α phase, which had a lower Al content. In the anodic polarization test in 0.017 mol·dm -3 NaCl and 0.1 mol·dm -3 Na 2 SO 4 at 298 K, the current density of Mg-15 mass% Al alloy anodized for 10 min increased, since the anodic film that forms on the α phase is a non-compacted film. The anodic film on the α phase at 30 min was a compact film as compared with that at 10 min

  3. The electrochemical properties and mechanism of formation of anodic oxide films on Mg-Al alloys

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seong Jong; Okido, Masazumi [Nagoya Univ., Nagoya (Japan)

    2003-07-01

    The electronchemical properties and the mechanism of formation of anodic oxide films on Mg alloys containing 0-15 mass% Al, when anodized in NaOH solution, were investigated by focusing on the effects of anodizing potential, Al content, and anodizing time. The intensity ratio of Mg(OH){sub 2} in the XRD analysis decreased with increasing applied potential, while that of MgO increased. Mg(OH){sub 2} was barely detected at 80 V, while MgO was readily detected. The anti-corrosion properties of anodized specimens at each constant potential were better than those of non-anodized specimens. The specimen anodized at an applied potential of 3 V had the best anti-corrosion property. The intensity ratio of the {beta} phase increased with aluminum content in Mg-Al alloys. During anodizing, the active dissolution reaction occurred preferentially in {beta} phase until about 4 min, and then the current density increased gradually until 7 min. The dissolution reaction progressed in {alpha} phase, which had a lower Al content. In the anodic polarization test in 0.017 mol{center_dot}dm{sup -3} NaCl and 0.1 mol{center_dot}dm{sup -3} Na{sub 2}SO{sub 4} at 298 K, the current density of Mg-15 mass% Al alloy anodized for 10 min increased, since the anodic film that forms on the {alpha} phase is a non-compacted film. The anodic film on the {alpha} phase at 30 min was a compact film as compared with that at 10 min.

  4. Structural study on Ni nanowires in an anodic alumina membrane by using in situ heating extended x-ray absorption fine structure and x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Cai Quan; Chen Xing; Chen Zhongjun; Wang Wei; Mo Guang; Wu Zhonghua; Zhang Junxi; Zhang Lide; Pan Wei

    2008-01-01

    Polycrystalline Ni nanowires have been prepared by electrochemical deposition in an anodic alumina membrane template with a nanopore size of about 60 nm. In situ heating extended x-ray absorption fine structure and x-ray diffraction techniques are used to probe the atomic structures. The nanowires are identified as being mixtures of nanocrystallites and amorphous phase. The nanocrystallites have the same thermal expansion coefficient, of 1.7 x 10 -5 K -1 , as Ni bulk; however, the amorphous phase has a much larger thermal expansion coefficient of 3.5 x 10 -5 K -1 . Details of the Ni nanowire structures are discussed in this paper

  5. Effect of ageing in the electrolyte and water on porous anodic films on zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Muratore, F.; Hashimoto, T.; Skeldon, P., E-mail: peter.skeldon@manchester.ac.uk; Thompson, G.E.

    2011-06-15

    Highlights: Porous anodic films are formed on zirconium consisting of nanotubes embedded in a fluoride-rich matrix. {yields}Ageing in the formation electrolyte transforms the films from porous to nanotubular. Ageing causes losses of zirconium and fluorine, due to dissolution of the matrix. Ageing in water has negligible influence on the film composition and the film morphology. - Abstract: The present study demonstrates the significant influence of ageing in the formation electrolyte on the morphology and composition of anodic films grown on zirconium in 0.35 M ammonium fluoride in glycerol. Ageing after anodizing, by immersion in the electrolyte for 1 h, is shown to promote a transition from a porous to a nanotubular morphology, due to the dissolution of the fluoride-rich intratubular material in which the nanotubes are embedded. The morphological change is accompanied by a significant loss of zirconium and fluorine from the film. In contrast, ageing in deionized water has little influence on the films.

  6. Electrophoretic deposition of PTFE particles on porous anodic aluminum oxide film and its tribological properties

    International Nuclear Information System (INIS)

    Zhang, Dongya; Dong, Guangneng; Chen, Yinjuan; Zeng, Qunfeng

    2014-01-01

    Polytetrafluoroethylene (PTFE) composite film was successfully fabricated by depositing PTFE particles into porous anodic aluminum oxide film using electrophoretic deposition (EPD) process. Firstly, porous anodic aluminum oxide film was synthesized by anodic oxidation process in sulphuric acid electrolyte. Then, PTFE particles in suspension were directionally deposited into the porous substrate. Finally, a heat treatment at 300 °C for 1 h was utilized to enhance PTFE particles adhesion to the substrate. The influence of anodic oxidation parameters on the morphology and micro-hardness of the porous anodic aluminum oxide film was studied and the PTFE particles deposited into the pores were authenticated using energy-dispersive spectrometer (EDS) and scanning electron microscopy (SEM). Tribological properties of the PTFE composite film were investigated under dry sliding. The experimental results showed that the composite film exhibit remarkable low friction. The composite film had friction coefficient of 0.20 which deposited in 15% PTFE emulsion at temperature of 15 °C and current density of 3 A/dm 2 for 35 min. In addition, a control specimen of porous anodic aluminum oxide film and the PTFE composite film were carried out under the same test condition, friction coefficient of the PTFE composite film was reduced by 60% comparing with the control specimen at 380 MPa and 100 mm/s. The lubricating mechanism was that PTFE particles embedded in porous anodic aluminum oxide film smeared a transfer film on the sliding path and the micro-pores could support the supplement of solid lubricant during the sliding, which prolonged the lubrication life of the aluminum alloys.

  7. Hydrogenated amorphous silicon thin film anode for proton conducting batteries

    Science.gov (United States)

    Meng, Tiejun; Young, Kwo; Beglau, David; Yan, Shuli; Zeng, Peng; Cheng, Mark Ming-Cheng

    2016-01-01

    Hydrogenated amorphous Si (a-Si:H) thin films deposited by chemical vapor deposition were used as anode in a non-conventional nickel metal hydride battery using a proton-conducting ionic liquid based non-aqueous electrolyte instead of alkaline solution for the first time, which showed a high specific discharge capacity of 1418 mAh g-1 for the 38th cycle and retained 707 mAh g-1 after 500 cycles. A maximum discharge capacity of 3635 mAh g-1 was obtained at a lower discharge rate, 510 mA g-1. This electrochemical discharge capacity is equivalent to about 3.8 hydrogen atoms stored in each silicon atom. Cyclic voltammogram showed an improved stability 300 mV below the hydrogen evolution potential. Both Raman spectroscopy and Fourier transform infrared spectroscopy studies showed no difference to the pre-existing covalent Si-H bond after electrochemical cycling and charging, indicating a non-covalent nature of the Si-H bonding contributing to the reversible hydrogen storage of the current material. Another a-Si:H thin film was prepared by an rf-sputtering deposition followed by an ex-situ hydrogenation, which showed a discharge capacity of 2377 mAh g-1.

  8. N-type polycrystalline silicon films formed on alumina by aluminium induced crystallization and overdoping

    Energy Technology Data Exchange (ETDEWEB)

    Tuezuen, O. [InESS, UMR 7163 CNRS-ULP, 23 rue du Loess, F-67037 Strasbourg (France)], E-mail: Ozge.Tuzun@iness.c-strasbourg.fr; Slaoui, A. [InESS, UMR 7163 CNRS-ULP, 23 rue du Loess, F-67037 Strasbourg (France); Gordon, I. [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Focsa, A. [InESS, UMR 7163 CNRS-ULP, 23 rue du Loess, F-67037 Strasbourg (France); Ballutaud, D. [GEMaC-UMR 8635 CNRS, 1 place Aristide Briand, F-92195 Meudon (France); Beaucarne, G.; Poortmans, J. [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium)

    2008-08-30

    In this work, we investigated the formation of n-type polysilicon films on alumina substrates by overdoping a p-type silicon layer obtained by aluminium induced crystallization of amorphous silicon (AIC), and subsequent epitaxy. The phosphorus doping of the AIC was carried out by thermal diffusion from a solid source. The structural quality of the n-type Si film was monitored by optical microscope and scanning electron microscope (SEM). The doping efficiency was determined by resistivity measurements and secondary ion mass spectroscopy (SIMS). The sheet resitivity changed from 2700{omega}/sq to 19.6{omega}/sq after thermal diffusion at 950 deg. C for 1h, indicating the overdoping effect. The SIMS profile carried out after the high temperature epitaxy exhibits a two steps phosphorus distribution, indicating the formation of an n{sup +}n structure.

  9. Porous anodic film formation on an Al-3.5 wt% Cu alloy

    Energy Technology Data Exchange (ETDEWEB)

    Paez, M.A.; Bustos, O.; Thompson, G.E.; Skeldon, P.; Shimizu, K.; Wood, G.C.

    2000-03-01

    Anodic film growth has been undertaken on an electropolished Al-3.5 wt % Cu alloy to determine the influence of copper in solid solution on the anodizing behavior. At the commencement of anodizing of the electropolished alloy, in the presence of interfacial enrichment of copper, Al{sup 3+} and Cu{sup 2+} ions egress and O{sup 2{minus}} ion ingress proceed; film growth occurs at the alloy/film interface though O{sup 2{minus}} ion ingress, with outwardly mobile Al{sup 3+} and Cu{sup 2+} ions ejected at the film/electrolyte interface, and field-assisted dissolution proceeding at the bases of pores. Oxidation of copper, in the presence of the enriched layer, is also associated with O{sub 2} gas generation, leading to development of oxygen-filled voids. As a result of significant pressures in the voids, film rupture proceeds, with electrolyte access to the alloy, dissolution of the enriched interfacial layer and re-anodizing. The consequence of such processes in the development of anodic films of increased porosity and reduced efficiency of film formation compared with anodizing of superpure aluminum under similar conditions.

  10. Features of film growth during plasma anodizing of Al 2024/SiC metal matrix composite

    Energy Technology Data Exchange (ETDEWEB)

    Xue Wenbin [Key Laboratory for Radiation Beam Technology and Materials Modification, Institute of Low Energy Nuclear Physics, Beijing Normal University, Beijing 100875 (China)]. E-mail: xuewb@bnu.edu.cn

    2006-07-15

    Plasma anodizing is a novel promising process to fabricate corrosion-resistant protective films on metal matrix composites. The corrosion-resistant films were prepared by plasma anodizing on SiC reinforced aluminum matrix composite. The morphology and microstructure of films were analyzed by scanning electron microscopy. Specifically, the morphology of residual SiC reinforcement particles in the film was observed. It is found that the most SiC reinforcement particles have been molten to become silicon oxide, but a few tiny SiC particles still remain in the film close to the composite/film interface. This interface is irregular due to the hindering effect of SiC particles on the film growth. Morphology and distribution of residual SiC particles in film provide direct evidence to identify the local melt occurs in the interior of plasma anodizing film even near the composite/film interface. A model of film growth by plasma anodizing on metal matrix composites was proposed.

  11. Features of film growth during plasma anodizing of Al 2024/SiC metal matrix composite

    International Nuclear Information System (INIS)

    Xue Wenbin

    2006-01-01

    Plasma anodizing is a novel promising process to fabricate corrosion-resistant protective films on metal matrix composites. The corrosion-resistant films were prepared by plasma anodizing on SiC reinforced aluminum matrix composite. The morphology and microstructure of films were analyzed by scanning electron microscopy. Specifically, the morphology of residual SiC reinforcement particles in the film was observed. It is found that the most SiC reinforcement particles have been molten to become silicon oxide, but a few tiny SiC particles still remain in the film close to the composite/film interface. This interface is irregular due to the hindering effect of SiC particles on the film growth. Morphology and distribution of residual SiC particles in film provide direct evidence to identify the local melt occurs in the interior of plasma anodizing film even near the composite/film interface. A model of film growth by plasma anodizing on metal matrix composites was proposed

  12. Mechanism of formation and growth of sunflower-shaped imperfections in anodic oxide films on niobium

    Energy Technology Data Exchange (ETDEWEB)

    Nagahara, K. [Graduate School of Engineering, Hokkaido University, N13 W8 Kita-ku, Sapporo 060-8628 (Japan); Sakairi, M. [Graduate School of Engineering, Hokkaido University, N13 W8 Kita-ku, Sapporo 060-8628 (Japan); Takahashi, H. [Graduate School of Engineering, Hokkaido University, N13 W8 Kita-ku, Sapporo 060-8628 (Japan)]. E-mail: Takahasi@elechem1-mc.eng.hokudai.ac.jp; Matsumoto, K. [Cabot Supermetals K.K., Higashinagahara Works, 111 Nagayachi, Kawahigashi-machi, Kawanuma-gun, Fukushima-ken 969-3431 (Japan); Takayama, K. [Cabot Supermetals K.K., Higashinagahara Works, 111 Nagayachi, Kawahigashi-machi, Kawanuma-gun, Fukushima-ken 969-3431 (Japan); Oda, Y. [Cabot Supermetals K.K., Higashinagahara Works, 111 Nagayachi, Kawahigashi-machi, Kawanuma-gun, Fukushima-ken 969-3431 (Japan)

    2007-01-01

    Anodizing of niobium has been investigated to develop niobium solid electrolytic capacitors. Chemically polished niobium specimens were anodized in a diluted phosphoric acid solution, initially galvanostatically at i {sub a} = 4 A m{sup -2} up to E {sub a} = 100 V, and then potentiostatically at E {sub a} = 100 V for t {sub pa} = 43.2 ks. During the galvanostatic anodizing, the anode potential increased almost linearly with time, while, during potentiostatic anodizing, the anodic current decreased up to t {sub pa} = 3.6 ks, and then increased slowly before decreasing again after t {sub pa} = 30.0 ks. Images of FE-SEM and in situ AFM showed that nuclei of imperfections were formed at the ridge of cell structures before t {sub pa} = 3.6 ks. After formation, the imperfection nuclei grew, showing cracking and rolling-up of the anodic oxide film, and crystalline oxide was formed at the center of imperfections after t {sub pa} = 3.6 ks. The growth of imperfections caused increases in the anodic current between t {sub pa} = 3.6 and 30.0 ks. Long-term anodizing caused a coalescence of the imperfections, leading to decreases in the anodic current after t {sub pa} = 30.0 ks. As the imperfections grew, the dielectric dispersion of the anodic oxide films became serious, showing a bias voltage dependence of the parallel equivalent capacitance, C {sub p}, and a dielectric dissipation factor, tan {delta}. The mechanism of formation and growth of the imperfections, and the correlation between the structure and dielectric properties of anodic oxide films is discussed.

  13. Effect of hydrogen on stresses in anodic oxide film on titanium

    International Nuclear Information System (INIS)

    Kim, Joong-Do; Pyun, Su-Il; Seo, Masahiro

    2003-01-01

    Stresses in anodic oxide film on titanium thin film/glass electrode in pH 8.4 borate solution were investigated by a bending beam method. The increases in compressive stress observed with cathodic potential sweeps after formation of anodic oxide film were attributed to the volume expansion due to the compositional change of anodic oxide film from TiO 2 to TiO 2-x (OH) x . The instantaneous responses of changes in stress, Δσ, in the anodic oxide film to potential steps demonstrated the reversible characteristic of the TiO 2-x (OH) x formation reaction. In contrast, the transient feature of Δσ for the titanium without anodic oxide film represented the irreversible formation of TiH x at the metal/oxide interphase. The large difference in stress between with and without the oxide film, has suggested that most of stresses generated during the hydrogen absorption/desorption reside in the anodic oxide film. A linear relationship between changes in stress, Δ(Δσ) des , and electric charge, ΔQ des , during hydrogen desorption was found from the current and stress transients, manifesting that the stress changes were crucially determined by the amount of hydrogen desorbed from the oxide film. The increasing tendency of -Δ(Δσ) des with increasing number of potential steps and film formation potential were discussed in connection with the increase in desorption amount of hydrogen in the oxide film with increasing absorption/desorption cycles and oxide film thickness

  14. Nitrogen and europium doped TiO2 anodized films with applications in photocatalysis

    International Nuclear Information System (INIS)

    Chi, Choong-Soo; Choi, Jinwook; Jeong, Yongsoo; Lee, Oh Yeon; Oh, Han-Jun

    2011-01-01

    Micro-arc oxidation method is a useful process for mesoporous titanium dioxide films. In order to improve the photocatalytic activity of the TiO 2 film, N-Eu co-doped titania catalyst was synthesized by micro-arc oxidation in the H 2 SO 4 /Eu(NO 3 ) 3 mixture solution. The specific surface area and the roughness of the anodic titania film fabricated in the H 2 SO 4 /Eu(NO 3 ) 3 electrolyte, were increased compared to that of the anodic TiO 2 film prepared in H 2 SO 4 solution. The absorbance response of N-Eu titania film shows a higher adsorption onset toward visible light region, and the incorporated N and Eu ions during anodization as a dopant in the anodic TiO 2 film significantly enhanced the photocatalytic activity for dye degradation. After dye decomposition test for 3 h, dye removal rates for the anodic TiO 2 film were 60.7% and 90.1% for the N-Eu doped titania film. The improvement of the photocatalytic activity was ascribed to the synergistic effects of the surface enlargement and the new electronic state of the TiO 2 band gap by N and Eu co-doping.

  15. Microstructural and Optical Properties of Porous Alumina Elaborated on Glass Substrate

    Science.gov (United States)

    Zaghdoudi, W.; Gaidi, M.; Chtourou, R.

    2013-03-01

    A transparent porous anodized aluminum oxide (AAO) nanostructure was formed on a glass substrate using the anodization of a highly pure evaporated aluminum layer. A parametric study was carried out in order to achieve a fine control of the microstructural and optical properties of the elaborated films. The microstructural and surface morphologies of the porous alumina films were characterized by x-ray diffraction and atomic force microscopy. Pore diameter, inter-pore separation, and the porous structure as a function of anodization conditions were investigated. It was then found that the pores density decreases with increasing the anodization time. Regular cylindrical porous AAO films with a flat bottom structure were formed by chemical etching and anodization. A high transmittance in the 300-900 nm range is reported, indicating a fulfilled growth of the transparent sample (alumina) from the aluminum metal. The data showed typical interference oscillations as a result of the transparent characteristics of the film throughout the visible spectral range. The thickness and the optical constants ( n and k) of the porous anodic alumina films, as a function of anodizing time, were obtained using spectroscopic ellipsometry in the ultraviolet-visible-near infrared (UV-vis-NIR) regions.

  16. Understanding anodic wear at boron doped diamond film electrodes

    International Nuclear Information System (INIS)

    Chaplin, Brian P.; Hubler, David K.; Farrell, James

    2013-01-01

    This research investigated the mechanisms associated with anodic wear of boron-doped diamond (BDD) film electrodes. Cyclic voltammetry (CV), x-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS) were used to measure changes in electrode response and surface chemistry as a function of the charge passed and applied current density. Density functional theory (DFT) modeling was used to evaluate possible reaction mechanisms. The initial hydrogen-terminated surface was electrochemically oxidized at lower potentials than water oxidation (≤ 1.83 V/SHE), and was not catalyzed by the hydrogen-terminated surface. In the region where water oxidation produces hydroxyl radicals (OH·), the hydrogen-terminated surface may also be oxidized by chemical reaction with OH·. Oxygen atoms became incorporated into the surface via reaction of carbon atoms with OH·, forming both C = O and C-OH functional groups, that were also detected by XPS measurements. Experimental and DFT modeling results indicate that the oxygenated diamond surface lowers the potential for activationless water oxidation from 2.74 V/SHE for the hydrogen terminated surface to 2.29 V/SHE for the oxygenated surface. Electrode wear was accelerated at high current densities (i.e., 500 mA cm −2 ), where SEM results indicated oxidation of the BDD film resulted in significant surface roughening. These results are supported by EIS measurements that document an increase in the double-layer capacitance as a function of the charge passed. DFT simulations provide a possible mechanism that explains the observed diamond oxidation. DFT simulation results indicate that BDD edge sites (=CH 2 ) can be converted to COOH functional groups, which are further oxidized via reactions with OH· to form H 2 CO 3(aq.) with an activation energy of 58.9 kJ mol −1

  17. An Analysis of Mechanical Properties of Anodized Aluminum Film at High Stress

    Science.gov (United States)

    Zhao, Xixi; Wei, Guoying; Yu, Yundan; Guo, Yuemei; Zhang, Ao

    2015-10-01

    In this paper, a new environmental-friendly electrolyte containing sulfuric acid and tartaric acid has been used as the substitute of chromic acid for anodization. The work discussed the influence of anodizing voltages on the fatigue life of anodized Al 2024-T3 by performing fatigue tests with 0.1 stress ratio (R) at 320 MPa. Meanwhile the fatigue cycles to failure, yield strength, tensile strength and fracture surface of anodic films at different conditions were investigated. The results showed that the fatigue life of anodized and sealed specimens reduced a lot compared to aluminum alloy, which can be attributed to the crack sites initiated at the oxide layer. The fracture surface analyses also revealed that the number of crack initiation sites enlarged with the increase of anodizing voltage.

  18. Characterization of anodic barrier films on tantalum and 1100 aluminum by ISS/SIMS

    International Nuclear Information System (INIS)

    McCune, R.C.

    1978-01-01

    Ion scattering spectrometry (ISS) and concurrent secondary ion mass spectrometry (SIMS) were used to determine the depth profiles of anodic barrier oxide films grown on tantalum and type 1100 aluminum. The sputter rate in each case was determined from the film thickness measured by the anodic overvoltage, and the penetration time determined by the decrease in intensity of the metal oxide fragment observed using SIMS. A mixture of helium and neon ions was used to sputter aluminum oxide films in order to observe ion scattering of helium by oxygen, while taking advantage of the higher sputtering rate available with neon. A comparison of sputter rates for helium and neon on tantalum oxide indicated that neon sputtered the film at a rate eight times that of helium. SIMS depth profiling of the residual boron in the anodic aluminum oxide indicated a mixing effect which did not permit adequate resolution of the interface between the oxide film and the underlying metal

  19. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

    Highlights: ► Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. ► NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. ► NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7–4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography–mass spectrometry (GC–MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient analytical method for the potential study of trace and small molecular

  20. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. Black-Right-Pointing-Pointer NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. Black-Right-Pointing-Pointer NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7-4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography-mass spectrometry (GC-MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient

  1. Growth of porous type anodic oxide films at micro-areas on aluminum exposed by laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Kikuchi, Tatsuya [Graduate School of Engineering, Hokkaido University, N13-W8, Kita-Ku, Sapporo 060-8628 (Japan)], E-mail: kiku@eng.hokudai.ac.jp; Sakairi, Masatoshi [Graduate School of Engineering, Hokkaido University, N13-W8, Kita-Ku, Sapporo 060-8628 (Japan); Takahashi, Hideaki [Asahikawa National College of Technology, Syunkohdai, 2-2, 1-6, Asahikawa 071-8142 (Japan)

    2009-11-30

    Aluminum covered with pore-sealed anodic oxide films was irradiated with a pulsed Nd-YAG laser to remove the oxide film at micro-areas. The specimen was re-anodized for long periods to examine the growth of porous anodic oxide films at the area where substrate had been exposed by measuring current variations and morphological changes in the oxide during the re-anodizing. The chemical dissolution resistance of the pore-sealed anodic oxide films in an oxalic acid solution was also examined by measuring time-variations in rest potentials during immersion. The resistance to chemical dissolution of the oxide film became higher with increasing pore-sealing time and showed higher values at lower solution temperatures. During potentiostatic re-anodizing at five 35-{mu}m wide and 4-mm long lines for 72 h after the film was removed the measured current was found to increase linearly with time. Semicircular columnar-shaped porous type anodic oxide was found to form during the re-anodizing at the laser-irradiated area, and was found to grow radially, thus resulting in an increase in the diameter. After long re-anodizing, the central and top parts of the oxide protruded along the longitudinal direction of the laser-irradiated area. The volume expansion during re-anodizing resulted in the formation of cracks, parallel to the lines, in the oxide film formed during the first anodizing.

  2. Analysis of nanopore arrangement of porous alumina layers formed by anodizing in oxalic acid at relatively high temperatures

    Science.gov (United States)

    Zaraska, Leszek; Stępniowski, Wojciech J.; Jaskuła, Marian; Sulka, Grzegorz D.

    2014-06-01

    Anodic aluminum oxide (AAO) layers were formed by a simple two-step anodization in 0.3 M oxalic acid at relatively high temperatures (20-30 °C) and various anodizing potentials (30-65 V). The effect of anodizing conditions on structural features of as-obtained oxides was carefully investigated. A linear and exponential relationships between cell diameter, pore density and anodizing potential were confirmed, respectively. On the other hand, no effect of temperature and duration of anodization on pore spacing and pore density was found. Detailed quantitative and qualitative analyses of hexagonal arrangement of nanopore arrays were performed for all studied samples. The nanopore arrangement was evaluated using various methods based on the fast Fourier transform (FFT) images, Delaunay triangulations (defect maps), pair distribution functions (PDF), and angular distribution functions (ADF). It was found that for short anodizations performed at relatively high temperatures, the optimal anodizing potential that results in formation of nanostructures with the highest degree of pore order is 45 V. No direct effect of temperature and time of anodization on the nanopore arrangement was observed.

  3. Ultrathin alumina film on Cu 9at%Al(1 1 1)

    Science.gov (United States)

    Napetschnig, E.; Schmid, M.; Varga, P.

    2008-05-01

    We have investigated the structure of the clean and the oxidized (1 1 1) surface of a Cu-Al alloy with 9 at% Al by scanning tunneling microscopy (STM), Auger electron spectroscopy (AES), low energy ion scattering (LEIS) and low energy electron diffraction (LEED). Annealing of the clean crystal at 680 °C leads to segregation of Al to the surface. The Al concentration at the annealed surface is 23 ± 2% and domains with a (√3 × √3)R30° superstructure are visible, as well as small Cu(1 1 1) areas and disordered patches. Oxidation at 680 °C leads to the formation of a well-ordered flat alumina film with two very similar oxide structures. One oxide structure has a nearly commensurate rectangular cell rotated by 30° with respect to a close-packed row of the substrate and grows in three different domains. The second structure has a commensurate cell consisting of four equivalent building blocks and has a rectangular centered symmetry. This structure is rotated by 18° with respect to a close-packed row of the substrate and grows in six different domains. The rectangular building blocks of these two oxide structures have a similar thickness, the same surface termination and the same number and arrangement of the atoms as the oxide film on NiAl(1 1 0) [G. Kresse, M. Schmid, E. Napetschnig, M. Shishkin, L. Köhler, P. Varga, Science 308 (2005) 1448]. In contrast to the oxide on NiAl(1 1 0), alumina on the Cu-Al alloy crystal does not show stress-induced domain boundaries and grows in large defect-free domains. Thus, Pd deposited on this oxide nucleates not only on domain boundaries and steps but also on the unperturbed oxide, forming (1 1 1)-oriented clusters.

  4. Effect of Pore Thickness and the State of Polarization on the Optical Properties of Hexagonal Nanoarray of Au/Nanoporous Anodic Alumina Membrane

    Directory of Open Access Journals (Sweden)

    Mohamed Shaban

    2015-01-01

    Full Text Available Hexagonal nanoarrays of Au particles were deposited on nanoporous anodic alumina membrane (NAAM utilizing r.f. magnetron sputtering. The thickness of the NAAMs is adjusted by changing the second anodization time from 5 min to 20 min. The surface morphology, composition, and optical properties are characterized by using SEM, EDX, and spectrophotometer, respectively. The effects of the NAAM thickness and state of polarization on the morphological changes and on the optical properties of the fabricated nanoarrays were addressed. According to the measured optical spectra, the rate of decrease of NAAMs refractive index was found to be 3.825 × 10−4 nm−1. Using the modified Kubelka-Munk radiative transfer model, the energy gap of NAAMs was calculated from diffused reflectance and was decreased from 1.682 to 1.376 as the anodization time increased from 5 to 20 min. Also, the saturation of interference fringes is substantially enhanced, and field enhancement can be achieved due to the excitation and constructive interference of surface plasmon waves by coating NAAMs with the hexagonal nanoarrays of Au. Based on the advantages of the fabrication approach and the enhanced and controlled properties, this new generation of samples can be used as promising building blocks for nanophotonic and nanoelectronics devices.

  5. L2O3 NANOSTRUCTURED FILMS CREATION BY METHOD OF ELECTROCHEMICAL ANODIZING

    Directory of Open Access Journals (Sweden)

    M. V. Zhukov

    2013-05-01

    Full Text Available Thin oxide films of aluminum were investigated by method of scanning probe microscopy. Electrical parameters of anodizing process were studied on different samples of aluminum to get the most structured oxide. The comparison of surface structure topography was held on oxide films by NTegra scanning probe microscope

  6. Incorporation of transition metal ions and oxygen generation during anodizing of aluminium alloys

    International Nuclear Information System (INIS)

    Habazaki, H.; Konno, H.; Shimizu, K.; Nagata, S.; Skeldon, P.; Thompson, G.E.

    2004-01-01

    Enrichment of nickel at the alloy/film interface and incorporation of nickel species into the anodic film have been examined for a sputtering-deposited Al-1.2at.%Ni alloy in order to assist understanding of oxygen generation in barrier anodic alumina films. Anodizing of the alloy proceeds in two stages similarly to other dilute aluminium alloys, for example Al-Cr and Al-Cu alloys, where the Gibbs free energies per equivalent for formation of alloying element oxide exceeds the value for alumina. In the first stage, a nickel-free alumina film is formed, with nickel enriching in an alloy layer, 2 nm thick, immediately beneath the anodic oxide film. In the second stage, nickel atoms are oxidized together with aluminium, with oxygen generation forming gas bubbles within the anodic oxide film. This stage commences after accumulation of about 5.4 x 10 15 nickel atoms cm -2 in the enriched alloy layer. Oxygen generation also occurs when a thin layer of the alloy, containing about 2.0 x 10 19 nickel atoms m -2 , on electropolished aluminium, is completely anodized, contrasting with thin Al-Cr and Al-Cu alloy layers on electropolished aluminium, for which oxygen generation is essentially absent. A mechanism of oxygen generation, based on electron impurity levels of amorphous alumina and local oxide compositions, is discussed in order to explain the observations

  7. Process of film formation by anodizing AZ91D magnesium alloy

    Energy Technology Data Exchange (ETDEWEB)

    Qian Jiangang; Li Di; Zhang Feng [School of Materials Science and Engineering, Beijing Univ. of Aeronautics and Astronautics (China)

    2005-07-01

    The kinetics of film-forming process by anodizing AZ91D Mg alloy has been studied by ways of voltage-time and thickness-time curve, and the surface morphology, structure, composition and valence of element, phase constituent of anodic films have been analyzed by SEM, EDS, XPS and XRD respectively. The results show that the film-forming course can be divided into four stages. Formation of dense layer before sparking is the first stage. Formation of porous layer accompanied with a bit of small sparking is the second stage. Porous layer fast growth along with middle sparking is the third stage. Porous layer slowly-growth along with bigger sparking is the fourth stage. The anodic films contains approximately Mg,O,Si and B, which is composed mainly of MgO, MgSiO{sub 3} and Mg{sub 3}B{sub 2}O{sub 6}. (orig.)

  8. Formation and dissolution of the anodic oxide film on zirconium in alcoholic aqueous solutions

    International Nuclear Information System (INIS)

    Mogoda, A.S.

    1995-01-01

    The dissolution behavior of the anodic oxide film formed in alcoholic aqueous solutions was studied. Results indicated the dissolution mechanism of the duplex oxide film followed a zero-order rate equation. The increase in methanol concentration in the formation medium (phosphoric acid [H 3 PO 4 ]) resulted in formation of an oxide film that incorporated little phosphate ion and that dissolved at a low rate. The dissolution rate of the oxide film decreased with increasing methanol concentration in the dissolution medium. This was attributed to the increase in the viscosity of the medium, which led to a decrease in the diffusion coefficient of the dissolution product of the zirconium oxide film. Dissolution of the anodic oxide film also was investigated as a function of the chain length of alcohols

  9. Li+-Permeable Film on Lithium Anode for Lithium Sulfur Battery.

    Science.gov (United States)

    Yang, Yan-Bo; Liu, Yun-Xia; Song, Zhiping; Zhou, Yun-Hong; Zhan, Hui

    2017-11-08

    Lithium-sulfur (Li-S) battery is an important candidate for next-generation energy storage. However, the reaction between polysulfide and lithium (Li) anode brings poor cycling stability, low Coulombic efficiency, and Li corrosion. Herein, we report a Li protection technology. Li metal was treated in crown ether containing electrolyte, and thus, treated Li was further used as the anode in Li-S cell. Due to the coordination between Li + and crown ether, a Li + -permeable film can be formed on Li, and the film is proved to be able to block the detrimental reaction between Li anode and polysulfide. By using the Li anode pretreated in 2 wt % B15C5-containing electrolyte, Li-S cell exhibits significantly improved cycling stability, such as∼900 mAh g -1 after 100 cycles, and high Coulombic efficiency of>93%. In addition, such effect is also notable when high S loading condition is applied.

  10. Investigation of CuInSe2 nanowire arrays with core-shell structure electrodeposited at various duty cycles into anodic alumina templates

    Science.gov (United States)

    Cheng, Yu-Song; Wang, Na-Fu; Tsai, Yu-Zen; Lin, Jia-Jun; Houng, Mau-Phon

    2017-02-01

    Copper indium selenide (CuInSe2) nanowire (NW) arrays were prepared at various electrolyte duty cycles by filling anodic alumina templates through the pulsed electrodeposition technique. X-ray diffraction and scanning electron microscopy (SEM) images showed that the nucleation mechanism of CuInSe2 NW arrays was affected by the electrodeposition duty cycle. Moreover, SEM images showed that the diameter and length of the NWs were 80 nm and 2 μm, respectively. Furthermore, PEDOT/CuInSe2 NW core-shell arrays were fabricated using surfactant-modified CuInSe2 NW surfaces showing the lotus effect. Transmission electron microscopy images confirmed that a core-shell structure was achieved. Current-voltage plots revealed that the CuInSe2 NW arrays were p-type semiconductors; moreover, the core-shell structure improved the diode ideality factor from 3.91 to 2.63.

  11. Fabrication and optical properties of TiO sub 2 nanowire arrays made by sol-gel electrophoresis deposition into anodic alumina membranes

    CERN Document Server

    Lin, Y; Yuan, X Y; Xie, T; Zhang, L D

    2003-01-01

    Ordered TiO sub 2 nanowire arrays have been successfully fabricated into the nanochannels of a porous anodic alumina membrane by sol-gel electrophoretic deposition. After annealing at 500 deg. C, the TiO sub 2 nanowire arrays and the individual nanowires were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and x-ray diffraction (XRD). SEM and TEM images show that these nanowires are dense and continuous with a uniform diameter throughout their entire length. XRD and SAED analysis together indicate that these TiO sub 2 nanowires crystallize in the anatase polycrystalline structure. The optical absorption band edge of TiO sub 2 nanowire arrays exhibits a blue shift with respect of that of the bulk TiO sub 2 owing to the quantum size effect.

  12. In situ detection of porosity initiation during aluminum thin film anodizing

    Science.gov (United States)

    Van Overmeere, Quentin; Nysten, Bernard; Proost, Joris

    2009-02-01

    High-resolution curvature measurements have been performed in situ during aluminum thin film anodizing in sulfuric acid. A well-defined transition in the rate of internal stress-induced curvature change is shown to allow for the accurate, real-time detection of porosity initiation. The validity of this in situ diagnostic tool was confirmed by a quantitative analysis of the spectral density distributions of the anodized surfaces. These were obtained by analyzing ex situ atomic force microscopy images of surfaces anodized for different times, and allowed to correlate the in situ detected transition in the rate of curvature change with the appearance of porosity.

  13. Optical constants of anodic aluminum oxide films formed in oxalic acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Wang Jian [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); Wang Chengwei [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)], E-mail: cwwang@nwnu.edu.cn; Li Yan [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); Liu Weimin [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)

    2008-09-01

    The anodic aluminum oxide (AAO) films with highly ordered nanopore arrays were prepared in oxalic acid solution under different anodizing voltage and time, its surface and cross section appearances were characterized by using field emission scanning electron microscopy, the transmission spectra with the interference fringes were measured at normal incidence over the wavelength range 200 to 2500 nm. Then the modified Swanepoel method was used for the determination of the optical constants and thickness of the free standing AAO films. The results indicate that the refractive index increases with the increase of anodizing voltage and the decrease of anodizing time, which is mainly due to the content of Al{sub 2}O{sub 3} with octahedron increases in the AAO films. The dispersion of the refractive index is discussed in terms of the single-oscillator Wemple-DiDomenico model, and the energy dependence of the absorption coefficient can be described using the direct transition model proposed by Tauc. Likewise, the optical energy gap E{sub g} is derived from Tauc's extrapolation, and E{sub g} increases from 4.178 to 4.256 eV with the anodizing voltage, but is weakly dependent on anodizing time. All the results are self-consistent in the paper.

  14. XPS characterization of the anodic oxide film formed on uranium metal in sodium hydroxide solution

    International Nuclear Information System (INIS)

    Fu Xiaoguo; Wang Xiaolin; Guo Huanjun; Wang Qingfu; Zhao Zhengping; Zhong Yongqiang

    2002-01-01

    X-ray photoelectron spectroscopy (XPS) is used to examine the anodic oxide film formed on uranium metal in 0.8 mol/L NaOH solution. The U4f 7/2 fitting spectra suggests that the anodic oxide film is composed of uranium trioxide and a small amount of UO 2+x . Under UHV condition, the U4f peak shifts to the lower binding energy, while a gradual increase in the intensity of U5f peak and the broad of U4f peak are also observed. All of these changes are due to reduction of uranium trioxide in the anodic oxide film. XPS quantitative analysis confirms the occurrence of reduction reaction

  15. Effects of the voltage and time of anodization on modulation of the pore dimensions of AAO films for nanomaterials synthesis

    Science.gov (United States)

    Chahrour, Khaled M.; Ahmed, Naser M.; Hashim, M. R.; Elfadill, Nezar G.; Maryam, W.; Ahmad, M. A.; Bououdina, M.

    2015-12-01

    Highly-ordered and hexagonal-shaped nanoporous anodic aluminum oxide (AAO) of 1 μm thickness of Al pre-deposited onto Si substrate using two-step anodization was successfully fabricated. The growth mechanism of the porous AAO film was investigated by anodization current-time behavior for different anodizing voltages and by visualizing the microstructural procedure of the fabrication of AAO film by two-step anodization using cross-sectional and top view of FESEM imaging. Optimum conditions of the process variables such as annealing time of the as-deposited Al thin film and pore widening time of porous AAO film were experimentally determined to obtain AAO films with uniformly distributed and vertically aligned porous microstructure. Pores with diameter ranging from 50 nm to 110 nm and thicknesses between 250 nm and 1400 nm, were obtained by controlling two main influential anodization parameters: the anodizing voltage and time of the second-step anodization. X-ray diffraction analysis reveals amorphous-to-crystalline phase transformation after annealing at temperatures above 800 °C. AFM images show optimum ordering of the porous AAO film anodized under low voltage condition. AAO films may be exploited as templates with desired size distribution for the fabrication of CuO nanorod arrays. Such nanostructured materials exhibit unique properties and hold high potential for nanotechnology devices.

  16. Low-density silicon thin films for lithium-ion battery anodes

    Energy Technology Data Exchange (ETDEWEB)

    Demirkan, M.T., E-mail: tmdemirkan@ualr.edu [Department of Physics and Astronomy, University of Arkansas at Little Rock, Little Rock, AR 72204 (United States); Department of Materials Science and Engineering, Gebze Technical University, Kocaeli (Turkey); Trahey, L. [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Karabacak, T. [Department of Physics and Astronomy, University of Arkansas at Little Rock, Little Rock, AR 72204 (United States)

    2016-02-01

    Density of sputter deposited silicon (Si) thin films was changed by a simple working gas pressure control process, and its effects on the cycling performance of Si films in Li-ion batteries as anodes was investigated. Higher gas pressure results in reduced film densities due to a shadowing effect originating from lower mean free path of sputter atoms, which leads to a wider angular distribution of the incoming flux and formation of a porous film microstructure. Si thin film anodes of different densities ranging from 2.27 g/cm{sup 3} (film porosity ~ 3%) down to 1.64 g/cm{sup 3} (~ 30% porosity) were fabricated by magnetron sputtering at argon pressures varying from 0.2 Pa to 2.6 Pa, respectively. High density Si thin film anodes of 2.27 g/cm{sup 3} suffered from an unstable cycling behavior during charging/discharging depicted by a continuous reduction in specific down to ~ 830 mAh/g at the 100th cycle. Electrochemical properties of lower density films with 1.99 g/cm{sup 3} (~ 15% porosity) and 1.77 g/cm{sup 3} (~ 24% porosity) got worse resulting in only ~ 100 mAh/g capacity at 100th cycle. On the other hand, as the density of anode was further reduced down to about 1.64 g/cm{sup 3} (~ 30% porosity), cycling stability and capacity retention significantly improved resulting in specific capacity values ~ 650 mAh/g at 100th cycle with coulombic efficiencies of > 98%. Enhancement in our low density Si film anodes are believed to mainly originate from the availability of voids for volumetric expansion during lithiation and resulting compliant behavior that provides superior mechanical and electrochemical stability. - Highlights: • Low density Si thin films were studied as Li-ion battery anodes. • Low density Si films were fabricated by magnetron sputter deposition. • Density of Si films reduced down to as low as ~ 1.64 g/cm{sup 3} with a porosity of ~ 30% • Low density Si films presented superior mechanical properties during cycling.

  17. Analysis of chemical dissolution of the barrier layer of porous oxide on aluminum thin films using a re-anodizing technique

    Energy Technology Data Exchange (ETDEWEB)

    Vrublevsky, I. [Department of Microelectronics, Belarusian State University of Informatics and Radioelectronics, 6 Brovka street, Minsk 220013 (Belarus)]. E-mail: nil-4-2@bsuir.edu.by; Parkoun, V. [Department of Microelectronics, Belarusian State University of Informatics and Radioelectronics, 6 Brovka street, Minsk 220013 (Belarus); Sokol, V. [Department of Microelectronics, Belarusian State University of Informatics and Radioelectronics, 6 Brovka street, Minsk 220013 (Belarus); Schreckenbach, J. [Institut fuer Chemie, Technische Universitaet Chemnitz, Chemnitz D-09107 (Germany)

    2005-09-30

    Chemical dissolution of the barrier layer of porous oxide formed on thin aluminum films (99.9% purity) in the 4% oxalic acid after immersion in 2 mol dm{sup -3} sulphuric acid at 50 deg. C has been studied. The barrier layer thickness before and after dissolution was calculated using a re-anodizing technique. It has been shown that above 57 V the change in the growth mechanism of porous alumina films takes place. As a result, the change in the amount of regions in the barrier oxide with different dissolution rates is observed. The barrier oxide contains two layers at 50 V: the outer layer with the highest dissolution rate and the inner layer with a low dissolution rate. Above 60 V the barrier oxide contains three layers: the outer layer with a high dissolution rate, the middle layer with the highest dissolution rate and the inner layer with a low dissolution rate. We suggest that the formation of the outer layer of barrier oxide with a high dissolution rate is linked with the injection of protons or H{sub 3}O{sup +} ions from the electrolyte into the oxide film at the anodizing voltages above 57 V.

  18. Evolution of insoluble eutectic Si particles in anodic oxidation films during adipic-sulfuric acid anodizing processes of ZL114A aluminum alloys

    Science.gov (United States)

    Hua, Lei; Liu, Jian-hua; Li, Song-mei; Yu, Mei; Wang, Lei; Cui, Yong-xin

    2015-03-01

    The effects of insoluble eutectic Si particles on the growth of anodic oxide films on ZL114A aluminum alloy substrates were investigated by optical microscopy (OM) and scanning electron microscopy (SEM). The anodic oxidation was performed at 25°C and a constant voltage of 15 V in a solution containing 50 g/L sulfuric acid and 10 g/L adipic acid. The thickness of the formed anodic oxidation film was approximately 7.13 μm. The interpore distance and the diameters of the major pores in the porous layer of the film were within the approximate ranges of 10-20 nm and 5-10 nm, respectively. Insoluble eutectic Si particles strongly influenced the morphology of the anodic oxidation films. The anodic oxidation films exhibited minimal defects and a uniform thickness on the ZL114A substrates; in contrast, when the front of the oxide oxidation films encountered eutectic Si particles, defects such as pits and non-uniform thickness were observed, and pits were observed in the films.

  19. Application of anodizing as a pre-treatment for nickel plating on aluminum

    International Nuclear Information System (INIS)

    Mehmood, M.; Ahmad, J.; Aslam, M.; Iqbal, M.; Akhtar, J.I.

    2003-01-01

    Effect of anodizing on subsequent electroplating of nickel on aluminum was investigated. Electroplated nickel did not exhibit any adhesion with un-anodized aluminum. Formation of a very thin anodized alumina film prior to nickel plating led to an excellent adhesion between the nickel film and the substrate. If the thickness of the alumina film increased, adhesion of electroplated nickel was significantly deteriorated and became similar to that of un-anodized bare aluminum. The study revealed that deposition proceeded through pores and defects in the insulator alumina film. These pores and defects also acted as nucleation and anchor points for nickel deposit. There was larger number of nucleation/ anchor points on thin alumina films. This provided better adhesion of nickel with the substrate as well as excellent coverage in relatively shorter times. On the other hand, very rough and poorly adherent nickel deposits formed on thick anodized films. Therefore, it may be used as precursor for producing nickel powder with controlled particle size as well as a catalyst with high specific surface area for hydrogenation and dehydrogenation reactions. (author)

  20. Cobalt nanosheet arrays supported silicon film as anode materials for lithium ion batteries

    International Nuclear Information System (INIS)

    Huang, X.H.; Wu, J.B.; Cao, Y.Q.; Zhang, P.; Lin, Y.; Guo, R.Q.

    2016-01-01

    Cobalt nanosheet arrays supported silicon film is prepared and used as anode materials for lithium ion batteries. The film is fabricated using chemical bath deposition, hydrogen reduction and radio-frequency magnetron sputtering techniques. The microstructure and morphology are characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS). In this composite film, the silicon layer is supported by interconnected aligned cobalt nanosheet arrays that act as the three-dimensional current collector and buffering network. The electrochemical performance as anode materials for lithium ion batteries is investigated by cyclic voltammetry (CV) and galvanostatic charge-discharge tests. The results show that the film prepared by sputtering for 1500 s exhibits high capacity, good rate capability and stable cycle ability. It is believed that the cobalt nanosheet arrays play important roles in the electrochemical performance of the silicon layer.

  1. Organic photovoltaics using thin gold film as an alternative anode to indium tin oxide

    International Nuclear Information System (INIS)

    Haldar, Amrita; Yambem, Soniya D.; Liao, Kang-Shyang; Alley, Nigel J.; Dillon, Eoghan P.; Barron, Andrew R.; Curran, Seamus A.

    2011-01-01

    Indium Tin Oxide (ITO) is the most commonly used anode as a transparent electrode and more recently as an anode for organic photovoltaics (OPVs). However, there are significant drawbacks in using ITO which include high material costs, mechanical instability including brittleness and poor electrical properties which limit its use in low-cost flexible devices. We present initial results of poly(3-hexylthiophene): phenyl-C 61 -butyric acid methyl ester OPVs showing that an efficiency of 1.9% (short-circuit current 7.01 mA/cm 2 , open-circuit voltage 0.55 V, fill factor 0.49) can be attained using an ultra thin film of gold coated glass as the device anode. The initial I-V characteristics demonstrate that using high work function metals when the thin film is kept ultra thin can be used as a replacement to ITO due to their greater stability and better morphological control.

  2. Cauliflower hillock formation through crystallite migration of SnO2 thin films prepared on alumina substrates by using MOCVD

    International Nuclear Information System (INIS)

    Choi, Gwangpyo; Ryu, Hyunwook; Lee, Woosun; Hong, Kwangjun; Shin, Dongcharn; Park, Jinseong; Seo, Yongjin; Akbar, Sheikh A.

    2003-01-01

    Tin-oxide thin films were deposited at 375 .deg. C on α-alumina substrates by using metalorganic chemical vapor deposition (MOCVD) process. A number of hillocks were formed on the film after annealing in air at 500 .deg. C for 30 min, but fewer hillocks were formed for annealing in N 2 . The hillocks on the film and the grains on the alumina substrate were composed of crystallites. The oxygen content and the binding energy after annealing in air came to close to values for the stoichiometric SnO 2 . There was no relationship between the film thickness and the binding energy shift, but the binding energy did change with the annealing atmosphere and the oxygen content. The cauliflower hillocks on the film seem to be formed by the continuous migration of crystallites from cauliflower grains on the substrate to release the stress due to the increased oxygen content and volume. A cauliflower hillock can be grown by continuous migration of crystallites from nearby grains to the hillock.

  3. Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy

    OpenAIRE

    Ferreira, Sonia C.; Conde, Ana; Arenas, Mar?a A.; Rocha, Luis A.; Velhinho, Alexandre

    2014-01-01

    Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiCnp) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiCnp on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodi...

  4. Growth and Etch Rate Study of Low Temperature Anodic Silicon Dioxide Thin Films

    Directory of Open Access Journals (Sweden)

    Akarapu Ashok

    2014-01-01

    Full Text Available Silicon dioxide (SiO2 thin films are most commonly used insulating films in the fabrication of silicon-based integrated circuits (ICs and microelectromechanical systems (MEMS. Several techniques with different processing environments have been investigated to deposit silicon dioxide films at temperatures down to room temperature. Anodic oxidation of silicon is one of the low temperature processes to grow oxide films even below room temperature. In the present work, uniform silicon dioxide thin films are grown at room temperature by using anodic oxidation technique. Oxide films are synthesized in potentiostatic and potentiodynamic regimes at large applied voltages in order to investigate the effect of voltage, mechanical stirring of electrolyte, current density and the water percentage on growth rate, and the different properties of as-grown oxide films. Ellipsometry, FTIR, and SEM are employed to investigate various properties of the oxide films. A 5.25 Å/V growth rate is achieved in potentiostatic mode. In the case of potentiodynamic mode, 160 nm thickness is attained at 300 V. The oxide films developed in both modes are slightly silicon rich, uniform, and less porous. The present study is intended to inspect various properties which are considered for applications in MEMS and Microelectronics.

  5. Structural and morphological changes in pseudobarrier films of anodic aluminum oxide caused by irradiation with high-energy particles

    International Nuclear Information System (INIS)

    Chernykh, M.A.; Belov, V.T.

    1988-01-01

    We have studied the structural and morphological changes, occurring under the electron beam in pseudobarrier films of anodic aluminum oxide, prepared in seven different solutions and irradiated beforehand by protons of x-rays, with the aim of elucidating the structure of anodic aluminum oxides. An increased stability of the pseudobarrier films of anodic aluminum oxide has been observed towards the action of the electron beam of an UEMV-100K microscope at standard working regimes (75 keV) as a result of irradiation with protons or x-rays. A difference has been found to exist between structural and morphological changes of anodic aluminum oxide films, prepared in different solutions, when irradiated with high-energy particles. A structural and phase inhomogeneity of amorphous pseudobarrier films of anodic aluminum oxide has been detected and its influence on the character of solid-phase transformations under the maximum-intensity electron beam

  6. Kramers-Kronig method for determination of optical properties of PZT nanotubes fabricated by sol-gel method and porous anodic alumina with high aspect ratio

    Science.gov (United States)

    Pakizeh, Esmaeil; Moradi, Mahmood

    2018-03-01

    Ferroelectric Pb(ZrTi)O3 (PZT) nanotubes were prepared by sol-gel method and porous anodic alumina (PAA) membrane using spin-coating technique. This method is based on filling-pyrolysis-filling process and the use of one-stage alumina membranes. One of the advantages of this method is its rapidity, which takes only 1 h time before the calcination step. The effect of repeated pores filling was investigated to get the required size of nanotubes. The field emission scanning electron microscope (FE-SEM) images were shown that the PZT nanotubes have inner diameters in the range of 65-90 nm and length of about 50-60 μm. This means that the samples have a significant aspect ratio (700-800). Also the FE-SEM image confirmed that the highly ordered, hexagonally distributed PAA membranes with the pore diameter about 140-150 nm were formed. The X-ray diffraction (XRD) results showed that the PZT nanotubes have a tetragonal structure. The metal oxide bands like ZrO6 and TiO6 of the final PZT nanotubes were detected by Fourier transform infrared (FT-IR) analysis and confirmed the formation of perovskite structure. By using FT-IR spectroscopy and Kramers-Kronig transformation method, the optical constants like real 𝜀1(ω) and imaginary 𝜀2(ω) parts of dielectric function, extinction coefficient k(ω) and refractive index n(ω) were determined. It was shown that the optical constants of PZT nanotubes are different from PZT nanoparticles.

  7. Micro-length anodic porous niobium oxide for lithium-ion thin film battery applications

    International Nuclear Information System (INIS)

    Yoo, Jeong Eun; Park, Jiyoung; Cha, Gihoon; Choi, Jinsub

    2013-01-01

    The anodization of niobium in an aqueous mixture of H 3 PO 4 and HF in the potential range from 2.5 to 30 V for 2 h at 5 °C was performed, demonstrating that anodic porous niobium oxide film with a thickness of up to 2000 nm, including a surface dissolution layer, can be obtained by controlling the applied potential and composition of the electrolytes. Specifically, surface dissolution-free porous niobium oxide film with a thickness of 800 nm can be prepared in a low electrolyte concentration. The surface dissolution is observed when the concentration ratio of HF (wt.%):H 3 PO 4 (M) was more than 2:1. The discontinuous layers in the niobium oxide film were observed when the thickness was higher than 500 nm, which was ascribed to the large volume expansion of the niobium oxide grown from the niobium metal. The anodic porous niobium oxide film was used as the cathode for lithium-ion batteries in the potential range from 1.2 to 3.0 V at a current density of 7.28 × 10 − 6 A cm −2 . The first discharge capacity of ca. 53 μA h cm − 2 was obtained in 800 nm thick niobium oxide without a surface dissolution layer. - Highlights: ► Anodic porous niobium oxide film with a thickness of 2000 nm was obtained. ► Surface dissolution-free porous niobium oxide film was prepared. ► The niobium oxide film was used as the cathode for lithium-ion batteries

  8. Boric/sulfuric acid anodizing of aluminum alloys 2024 and 7075: Film growth and corrosion resistance

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, G.E.; Zhang, L.; Smith, C.J.E.; Skeldon, P.

    1999-11-01

    The influence of boric acid (H{sub 3}BO{sub 3}) additions to sulfuric acid (H{sub 2}SO{sub 4}) were examined for the anodizing of Al 2024-T3 (UNS A92024) and Al 7075-T6 (UNS A97075) alloys at constant voltage. Alloys were pretreated by electropolishing, by sodium dichromate (Na{sub 2}Cr{sub 2}O{sub 7})/H{sub 2}SO{sub 4} (CSA) etching, or by alkaline etching. Current-time responses revealed insignificant dependence on the concentration of H{sub 3}BO{sub 3} to 50 g/L. Pretreatments affected the initial film development prior to the establishment of the steady-state morphology of the porous film, which was related to the different compositions and morphologies of pretreated surfaces. More detailed studies of the Al 7075-T6 alloy indicated negligible effects of H{sub 3}BO{sub 3} on the coating weight, morphology of the anodic film, and thickening rate of the film, or corrosion resistance provided by the film. In salt spray tests, unsealed films formed in H{sub 2}SO{sub 4} or mixed acid yielded similar poor corrosion resistances, which were inferior to that provided by anodizing in chromic acid (H{sub 2}CrO{sub 4}). Sealing of films in deionized water, or preferably in chromate solution, improved corrosion resistance, although not matching the far superior performance provided by H{sub 2}CrO{sub 4} anodizing and sealing.

  9. Monodispersed macroporous architecture of nickel-oxide film as an anode material for thin-film lithium-ion batteries

    International Nuclear Information System (INIS)

    Wu, Mao-Sung; Lin, Ya-Ping

    2011-01-01

    A nickel-oxide film with monodispersed open macropores was prepared on a stainless-steel substrate by electrophoretic deposition of a polystyrene-sphere monolayer followed by anodic electrodeposition of nickel oxy-hydroxide. The deposited films convert to cubic nickel oxide after annealing at 400 o C for 1 h. Galvanostatic charge and discharge results indicate that the nickel-oxide film with monodispersed open macropores is capable of delivering a higher capacity than the bare nickel-oxide film, especially in high-rate charge and discharge processes. The lithiation capacity of macroporous nickel oxide reaches 1620 mA h g -1 at 1 C current discharge and decreases to 990 mA h g -1 at 15 C current discharge. The presence of monodispersed open macropores in the nickel-oxide film might facilitate the electrolyte penetration, diffusion, and migration. Electrochemical reactions between nickel oxide and lithium ions are therefore markedly improved by this tailored film architecture.

  10. Anodic films grown on magnesium and magnesium alloys in fluoride solutions

    Energy Technology Data Exchange (ETDEWEB)

    Ono, S. [Dept. of Applied Chemistry, Kogakuin Univ., Tokyo (Japan); Masuko, N. [Dept. of Metallurgical Engineering, Chiba Inst. of Tech., Narashino, Chiba (Japan)

    2003-07-01

    Formation behavior of anodic oxide films on magnesium in fluoride electrolytes was investigated with attention to the effects of anodizing voltage and aluminum content. In the range of voltage between 2 V and 100 V, porous film was formed in alkaline fluoride solution associated with high current density at around 5 V and at breakdown voltage. The critical voltage of breakdown to allow maximum current flow was approximately 60 V and relatively independent on substrate purity. The films formed at breakdown voltage showed a lava-like porous structure similar to those obtained on aluminum and other valve metals. Barrier films or semi-barrier films, which were composed of hydrated outer layer and relatively dense inner layer, were formed at the other voltages. In the case of AZ91D, the critical voltage increased to 70 V and peculiar phenomenon at 5 V was not observed, so that only barrier films were formed at less than the breakdown voltage. These phenomena can be explained by the effects of aluminum incorporation into the film to prevent dissolution and to promote passivation of magnesium. The depth profiles of constituent elements showed that aluminum distributed in whole depth of the film. (orig.)

  11. The effect of different aluminum alloy surface compositions on barrier anodic film formation

    International Nuclear Information System (INIS)

    Panitz, J.K.G.; Sharp, D.J.

    1984-01-01

    The authors have grown barrier anodic coatings on samples of aluminum alloy with different elemental surface compositions. In one series of experiments, they characterized the surface composition present on 6061 aluminum alloy samples after different chemical treatments including a detergent-water and methyl-ethyl ketone solvent clean, a 50% nitric acid-water etch, and a concentrated nitric acid-ammonium bifluoride etch. They anodized samples which were prepared similarly to those analyzed to evaluate the practical effects of the three different surface compositions. The anodization voltage rise time to 950V at constant current was used as a figure of merit. The solvent cleaned and the 50% nitric acid etched samples required, respectively, 113% and 41% more time to reach 950V than the concentrated nitric acidammonium bifloride etched samples. In a second series of experiments, they alternately anodized groups of either 6061 or 1100 (commercially pure) aluminum alloy, observed rise times to 950V, and measured chloride ion concentrations in the electrolyte. Longer rise times and higher chloride ion concentrations were observed for the 1100 samples. It was observed that the chloride ion concentration fell from initially high levels when 6061 samples were anodized. The results of both series of experiments augment the results of other investigators, who report that the surface species initially present on aluminum have a significant effect on anodic film formation

  12. High performance sandwich structured Si thin film anodes with LiPON coating

    Science.gov (United States)

    Luo, Xinyi; Lang, Jialiang; Lv, Shasha; Li, Zhengcao

    2018-04-01

    The sandwich structured silicon thin film anodes with lithium phosphorus oxynitride (LiPON) coating are synthesized via the radio frequency magnetron sputtering method, whereas the thicknesses of both layers are in the nanometer range, i.e. between 50 and 200 nm. In this sandwich structure, the separator simultaneously functions as a flexible substrate, while the LiPON layer is regarded as a protective layer. This sandwich structure combines the advantages of flexible substrate, which can help silicon release the compressive stress, and the LiPON coating, which can provide a stable artificial solidelectrolyte interphase (SEI) film on the electrode. As a result, the silicon anodes are protected well, and the cells exhibit high reversible capacity, excellent cycling stability and good rate capability. All the results demonstrate that this sandwich structure can be a promising option for high performance Si thin film lithium ion batteries.

  13. High-Temperature Electrical Insulation Behavior of Alumina Films Prepared at Room Temperature by Aerosol Deposition and Influence of Annealing Process and Powder Impurities

    Science.gov (United States)

    Schubert, Michael; Leupold, Nico; Exner, Jörg; Kita, Jaroslaw; Moos, Ralf

    2018-04-01

    Alumina (Al2O3) is a widely used material for highly insulating films due to its very low electrical conductivity, even at high temperatures. Typically, alumina films have to be sintered far above 1200 °C, which precludes the coating of lower melting substrates. The aerosol deposition method (ADM), however, is a promising method to manufacture ceramic films at room temperature directly from the ceramic raw powder. In this work, alumina films were deposited by ADM on a three-electrode setup with guard ring and the electrical conductivity was measured between 400 and 900 °C by direct current measurements according to ASTM D257 or IEC 60093. The effects of film annealing and of zirconia impurities in the powder on the electrical conductivity were investigated. The conductivity values of the ADM films correlate well with literature data and can even be improved by annealing at 900 °C from 4.5 × 10-12 S/cm before annealing up to 5.6 × 10-13 S/cm after annealing (measured at 400 °C). The influence of zirconia impurities is very low as the conductivity is only slightly elevated. The ADM-processed films show a very good insulation behavior represented by an even lower electrical conductivity than conventional alumina substrates as they are commercially available for thick-film technology.

  14. X-ray spectral determination of chemical state of phosphorus and sulfur in anodic oxide films on niobium

    International Nuclear Information System (INIS)

    Bokij, L.P.; Kostikov, Yu.P.

    1989-01-01

    Chemical forms of phosphorus and sulfur in niobium oxide anodic film, obtained by electrochemical technique using niobium in H 2 SO 4 and H 3 PO 4 aqueous solutions, are determined using data on chemical shifts of X-ray emission lines. Films represent Nb 2 O 5(1-γ) (SO 4 ) 5γ and Nb 2 O 5(1-γ) (PO 4 ) 10γ/3 (γ -share of oxygen substituted by acid anion) composition oxosalts. Electrolyte role in formation of niobium anodic oxide structure and effect of phosphorus and sulfur compounds on anodic film conductivity are determined

  15. 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.

  16. Fabrication of Mesoporous Silica/Alumina Hybrid Membrane Film Nanocomposites using Template Sol-Gel Synthesis of Amphiphilic Triphenylene

    Science.gov (United States)

    Lintang, H. O.; Jalani, M. A.; Yuliati, L.; Salleh, M. M.

    2017-05-01

    Herein we reported that by introducing a one-dimensional (1D) substrate with a porous structure such as anodic aluminum oxide (AAO) membrane, mesoporous silica/alumina hybrid nanocomposites were successfully fabricated by using amphiphilic triphenylene (TPC10TEG) as a template in sol-gel synthesis (TPC10TEG/silicahex). For the optical study of the nanocomposites, TPC10TEG/silicahex showed absorption peak at 264 nm due to the ordered and long-range π-π stacking of the disc-like aromatic triphenylene core. Moreover, the hexagonal arrangement of TPC10TEG/silicahex was proven based on their diffraction peaks of d 100 and d 200 at 2θ = 2.52° and 5.04° and images of transmission electron microscopy (TEM), respectively. For fabrication of mesoporous silica/alumina hybrid membrane, TPC10TEG/silicahex was drop-casted onto AAO membrane for penetration into the porous structure via gravity. X-ray diffraction (XRD) analysis on the resulted hybrid nanocomposites showed that the diffraction peaks of d 100 and d 200 of TPC10TEG/silicahex were still preserved, indicating that the hexagonal arrangements of mesoporous silica were maintained even on AAO substrate. The morphology study on the hybrid nanocomposites using TEM, scanning electron microscope (SEM) and field emission scanning electron microscope (FE-SEM) showed the successful filling of most AAO channels with the TPC10TEG/silicahex nanocomposites.

  17. Effect of Si additions on thermal stability and the phase transition sequence of sputtered amorphous alumina thin films

    Energy Technology Data Exchange (ETDEWEB)

    Bolvardi, H.; Baben, M. to; Nahif, F.; Music, D., E-mail: music@mch.rwth-aachen.de; Schnabel, V.; Shaha, K. P.; Mráz, S.; Schneider, J. M. [Materials Chemistry, RWTH Aachen University, Kopernikusstr. 10, D-52074 Aachen (Germany); Bednarcik, J.; Michalikova, J. [Deutsches Elektronen Synchrotron DESY, FS-PE group, Notkestrasse 85, D-22607 Hamburg (Germany)

    2015-01-14

    Si-alloyed amorphous alumina coatings having a silicon concentration of 0 to 2.7 at. % were deposited by combinatorial reactive pulsed DC magnetron sputtering of Al and Al-Si (90-10 at. %) split segments in Ar/O{sub 2} atmosphere. The effect of Si alloying on thermal stability of the as-deposited amorphous alumina thin films and the phase formation sequence was evaluated by using differential scanning calorimetry and X-ray diffraction. The thermal stability window of the amorphous phase containing 2.7 at. % of Si was increased by more than 100 °C compared to that of the unalloyed phase. A similar retarding effect of Si alloying was also observed for the α-Al{sub 2}O{sub 3} formation temperature, which increased by more than 120 °C. While for the latter retardation, the evidence for the presence of SiO{sub 2} at the grain boundaries was presented previously, this obviously cannot explain the stability enhancement reported here for the amorphous phase. Based on density functional theory molecular dynamics simulations and synchrotron X-ray diffraction experiments for amorphous Al{sub 2}O{sub 3} with and without Si incorporation, we suggest that the experimentally identified enhanced thermal stability of amorphous alumina with addition of Si is due to the formation of shorter and stronger Si–O bonds as compared to Al–O bonds.

  18. Effect of Si additions on thermal stability and the phase transition sequence of sputtered amorphous alumina thin films

    International Nuclear Information System (INIS)

    Bolvardi, H.; Baben, M. to; Nahif, F.; Music, D.; Schnabel, V.; Shaha, K. P.; Mráz, S.; Schneider, J. M.; Bednarcik, J.; Michalikova, J.

    2015-01-01

    Si-alloyed amorphous alumina coatings having a silicon concentration of 0 to 2.7 at. % were deposited by combinatorial reactive pulsed DC magnetron sputtering of Al and Al-Si (90-10 at. %) split segments in Ar/O 2 atmosphere. The effect of Si alloying on thermal stability of the as-deposited amorphous alumina thin films and the phase formation sequence was evaluated by using differential scanning calorimetry and X-ray diffraction. The thermal stability window of the amorphous phase containing 2.7 at. % of Si was increased by more than 100 °C compared to that of the unalloyed phase. A similar retarding effect of Si alloying was also observed for the α-Al 2 O 3 formation temperature, which increased by more than 120 °C. While for the latter retardation, the evidence for the presence of SiO 2 at the grain boundaries was presented previously, this obviously cannot explain the stability enhancement reported here for the amorphous phase. Based on density functional theory molecular dynamics simulations and synchrotron X-ray diffraction experiments for amorphous Al 2 O 3 with and without Si incorporation, we suggest that the experimentally identified enhanced thermal stability of amorphous alumina with addition of Si is due to the formation of shorter and stronger Si–O bonds as compared to Al–O bonds

  19. Low-temperature α-alumina thin film growth: ab initio studies of Al adatom surface migration

    International Nuclear Information System (INIS)

    Wallin, E; Helmersson, U; Muenger, E P; Chirita, V

    2009-01-01

    Investigations of activation energy barriers for Al surface hopping on α-Al 2 O 3 (0 0 0 1) surfaces have been carried out by means of first-principles density functional theory calculations and the nudged elastic band method. Results show that surface diffusion on the (most stable) Al-terminated surface is relatively fast with an energy barrier of 0.75 eV, whereas Al hopping on the O-terminated surface is slower, with barriers for jumps from the two metastable positions existing on this surface to the stable site of 0.31 and 0.99 eV. Based on this study and on the literature, the governing mechanisms during low-temperature α-alumina thin film growth are summarized and discussed. Our results support suggestions made in some previous experimental studies, pointing out that limited surface diffusivity is not the main obstacle for α-alumina growth at low-to-moderate temperatures, and that other effects should primarily be considered when designing novel processes for low-temperature α-alumina deposition.

  20. Preparation of titanium dioxide films on etched aluminum foil by vacuum infiltration and anodizing

    Science.gov (United States)

    Xiang, Lian; Park, Sang-Shik

    2016-12-01

    Al2O3-TiO2 (Al-Ti) composite oxide films are a promising dielectric material for future use in capacitors. In this study, TiO2 films were prepared on etched Al foils by vacuum infiltration. TiO2 films prepared using a sol-gel process were annealed at various temperatures (450, 500, and 550 °C) for different time durations (10, 30, and 60 min) for 4 cycles, and then anodized at 100 V. The specimens were characterized using X-ray diffraction, field emission scanning electron microscopy, and field emission transmission electron microscopy. The results show that the tunnels of the specimens feature a multi-layer structure consisting of an Al2O3 outer layer, an Al-Ti composite oxide middle layer, and an aluminum hydrate inner layer. The electrical properties of the specimens, such as the withstanding voltage and specific capacitance, were also measured. Compared to specimens without TiO2 coating, the specific capacitances of the TiO2-coated specimens are increased. The specific capacitance of the anode Al foil with TiO2 coating increased by 42% compared to that of a specimen without TiO2 coating when annealed at 550 °C for 10 min. These composite oxide films could enhance the specific capacitance of anode Al foils used in dielectric materials.

  1. Preparation of titanium dioxide films on etched aluminum foil by vacuum infiltration and anodizing

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, Lian, E-mail: xianglian93@163.com; Park, Sang-Shik, E-mail: parkss@knu.ac.kr

    2016-12-01

    Highlights: • Al{sub 2}O{sub 3}–TiO{sub 2} composite films were prepared onto high voltage Al etching foil. • The coated and anodized samples showed multi-layer structures. • The capacitances of TiO{sub 2} coated samples showed an increase of 42%. • The increase in capacitance was mainly due to the Al–Ti composite layer. - Abstract: Al{sub 2}O{sub 3}–TiO{sub 2} (Al–Ti) composite oxide films are a promising dielectric material for future use in capacitors. In this study, TiO{sub 2} films were prepared on etched Al foils by vacuum infiltration. TiO{sub 2} films prepared using a sol–gel process were annealed at various temperatures (450, 500, and 550 °C) for different time durations (10, 30, and 60 min) for 4 cycles, and then anodized at 100 V. The specimens were characterized using X-ray diffraction, field emission scanning electron microscopy, and field emission transmission electron microscopy. The results show that the tunnels of the specimens feature a multi-layer structure consisting of an Al{sub 2}O{sub 3} outer layer, an Al–Ti composite oxide middle layer, and an aluminum hydrate inner layer. The electrical properties of the specimens, such as the withstanding voltage and specific capacitance, were also measured. Compared to specimens without TiO{sub 2} coating, the specific capacitances of the TiO{sub 2}-coated specimens are increased. The specific capacitance of the anode Al foil with TiO{sub 2} coating increased by 42% compared to that of a specimen without TiO{sub 2} coating when annealed at 550 °C for 10 min. These composite oxide films could enhance the specific capacitance of anode Al foils used in dielectric materials.

  2. Indium-Doped Zinc Oxide Thin Films as Effective Anodes of Organic Photovoltaic Devices

    Directory of Open Access Journals (Sweden)

    Ziyang Hu

    2011-01-01

    Full Text Available Indium-doped zinc oxide (IZO thin films were prepared by low-cost ultrasonic spray pyrolysis (USP. Both a low resistivity (3.13×10−3 Ω cm and an average direct transmittance (400∼1500 nm about 80% of the IZO films were achieved. The IZO films were investigated as anodes in bulk-heterojunction organic photovoltaic (OPV devices based on poly(3-hexylthiophene and [6,6]-phenyl C61-butyric acid methyl ester. The device fabricated on IZO film-coated glass substrate showed an open circuit voltage of 0.56 V, a short circuit current of 8.49 mA cm-2, a fill factor of 0.40, and a power conversion efficiency of 1.91%, demonstrating that the IZO films prepared by USP technique are promising low In content and transparent electrode candidates of low-cost OPV devices.

  3. Metal-insulator transition in nanocomposite VO{sub x} films formed by anodic electrodeposition

    Energy Technology Data Exchange (ETDEWEB)

    Tsui, Lok-kun; Lu, Jiwei; Zangari, Giovanni, E-mail: gz3e@virginia.edu [Department of Materials Science and Engineering, University of Virginia, 395 McCormick Rd., Charlottesville, Virginia 22904 (United States); Hildebrand, Helga; Schmuki, Patrik [Department for Materials Science LKO, University of Erlangen-Nuremberg, Martensstr. 7, D-91058 Erlangen (Germany)

    2013-11-11

    The ability to grow VO{sub 2} films by electrochemical methods would open a low-cost, easily scalable production route to a number of electronic devices. We have synthesized VO{sub x} films by anodic electrodeposition of V{sub 2}O{sub 5}, followed by partial reduction by annealing in Ar. The resulting films are heterogeneous, consisting of various metallic/oxide phases and including regions with VO{sub 2} stoichiometry. A gradual metal insulator transition with a nearly two order of magnitude change in film resistance is observed between room temperature and 140 °C. In addition, the films exhibit a temperature coefficient of resistance of ∼ −2.4%/ °C from 20 to 140 °C.

  4. Low-cost shape-control synthesis of porous carbon film on β″-alumina ceramics for Na-based battery application

    Science.gov (United States)

    Hu, Yingying; Wen, Zhaoyin; Wu, Xiangwei; Jin, Jun

    2012-12-01

    Porous carbon films with tunable pore structure to modify the β″-alumina electrolyte surface are fabricated through a low-cost and direct wet chemistry method with glucose and poly(methyl-methacrylate) (PMMA) as precursors. FTIR analysis confirms the effective connection between the carbohydrate and the pore-forming agent PMMA through hydrogen bonds. The experimental results indicate that the structural parameters of the porous carbon films, including mean pore size and film thickness, can be tuned simply by adjusting the amount of PMMA in the glucose/PMMA composite. This soft-template-assisted method could be readily extended to modify any other ceramic surfaces. The porous carbon films are demonstrated to greatly improve the wettability of the β″-alumina ceramics by molten sodium. Na/β″-alumina/Na cells are used to investigate the interfacial properties between sodium and the β″-alumina electrolyte. The results obtained at 350 °C reveal that the polarization behavior of the cell is alleviated by the porous coating. This work represents a successful method to coat ceramics with porous carbon and offers a promising solution to overcome the polarization problems of the sodium/β″-alumina interface in Na-based batteries.

  5. Influences of the main anodic electroplating parameters on cerium oxide films

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Yang; Yang, Yumeng; Du, Xiaoqing; Chen, Yu [Department of Chemistry, Zhejiang University, Hangzhou 310027, Zhejiang (China); Zhang, Zhao, E-mail: eaglezzy@zjuem.zju.edu.cn [Department of Chemistry, Zhejiang University, Hangzhou 310027, Zhejiang (China); Zhang, Jianqing [Department of Chemistry, Zhejiang University, Hangzhou 310027, Zhejiang (China); State Key Laboratory for Corrosion and Protection of Metals, Shenyang 110016 (China)

    2014-06-01

    Cerium oxide thin films were fabricated onto 316 L stainless steel via a potentiostatically anodic electrodeposition approach in the solutions containing cerium(III) nitrate (0.05 M), ammonia acetate (0.1 M) and ethanol (10% V/V). The electrochemical behaviors and deposition parameters (applied potential, bath temperature, dissolving O{sub 2} and bath pH) have been investigated. Results show that, the electrochemical oxidation of Ce{sup 3+} goes through one electrochemical step, which is under charge transfer control. The optimum applied potential for film deposition is 0.8 V. Bath temperature plays a significant effect on the deposition rate, composition (different colors of the film) and surface morphology of the deposits. Due to the hydrolysis of Ce{sup 3+}, cerous hydroxide is facility to form when the bath temperature is higher than 60 °C. The electroplating bath pH is another key role for the anodic deposition of cerium oxide thin films, and the best bath pH is around 6.20. N{sub 2} or O{sub 2} purged into the bath will result in film porosities and O{sub 2} favors cerium oxide particles and film generation.

  6. Effects of thermal treatment on the anodic growth of tungsten oxide films

    Energy Technology Data Exchange (ETDEWEB)

    Chai, Y., E-mail: yqchai85@gmail.com; Tam, C.W.; Beh, K.P.; Yam, F.K.; Hassan, Z.

    2015-08-03

    This work reports the investigation of the effects of thermal treatment on anodic growth tungsten oxide (WO{sub 3}). The increase of the thermal treatment temperature above 400 °C significantly influences WO{sub 3} film where high porosity structure reduces to more compact film. As-grown film is amorphous, which transforms to monoclinic/orthorhombic phase upon annealing at 300–600 °C. With the reducing of porous structure, preferential growth of (002) plane shifts to (020) plane at 600 °C with more than twentyfold increase of peak's intensity compared to the film annealed at 500 °C. Films annealed at low thermal treatment show better ion intercalation and reversibility during electrochemical measurements; however, it has larger optical band gap. Photoelectrochemical measurement reveals that film annealed at 400 °C exhibits the best photocatalytic performance among the films annealed at 300–600 °C. - Highlights: • Porosity of the WO{sub 3} reduces as annealing temperature increases above 400 °C. • As-grown film is amorphous which transforms to monoclinic/orthorhombic upon annealing. • As-grown film shows better ion intercalation in electrochemical process. • Optical band gap of WO{sub 3} reduces as the annealing temperature increases. • Film annealed at 400 °C exhibits best photocatalytic performance.

  7. Electrical Properties of a Thin Anodized Capacitor Made of Y-Doped Al Alloy Film

    Science.gov (United States)

    Onozuka, Tomotake; Sasaki, Hayato; Mikuni, Naohiro; Shinkai, Satoko; Sasaki, Katsutaka; Yamane, Misao; Abe, Yoshio

    2005-09-01

    We have prepared an Al-Y anodized capacitor using sputter-deposited Al-Y alloy film with 5 at. % Y atoms, and evaluated the capacitor properties and the leakage current properties before and after heat treatment. In addition, the characterization of Al-Y anodized films was examined by X-ray diffraction, Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy analyses. As a result, it is revealed that the thermal stability of an Al-Y anodized capacitor is superior to that of a pure Al anodized capacitor because of its excellent passive nature, and the loss properties can be improved by increasing the heat treatment temperature in air because of the reduction of the equivalent series resistance. Furthermore, it is clarified that the cause of the short-circuited state observed at 550°C is the formation of a narrow capillary-like conduction path of metallic Al atoms as a result of the interdiffusion of Al.

  8. An Auger electron spectroscopy study on the anodization process of high-quality thin-film capacitors made of hafnium

    International Nuclear Information System (INIS)

    Noya, Atsushi; Sasaki, Katsutaka; Umezawa, Toshiji

    1989-01-01

    Formation process of the anodic oxide film of hafnium for use as a thin-film capacitor has been examined by the current-voltage characteristics of the anodization and the in-depth analysis of formed oxide using Auger electron spectroscopy. It is found that the oxide growth obeys three different rate laws such as the linear rate law at first and next the parabolic rate law during the constant current anodization, and then the reciprocal logarithmic rate law during the constant voltage anodization following after the constant current process. From the Auger electron spectroscopy analysis, it is found that the shape of the compositional depth profile of the grown oxide film varies associating with the rate law of oxidation obeyed. The variation of depth profile correlating with the rate law is discussed with respect to each elementary process such as the transport and/or the reaction of chemical species interpreted from the over-all behavior of anodization process. It is revealed that the stoichiometric film having an interface with sharp transition, which is favorable for obtaining excellent electrical properties of the capacitor, can be obtained under the condition that the phase-boundary reaction is the rate-determining step of the anodization. The constant voltage anodization process also satisfies such circumstances and therefore can be favorable method for preparing highquality thin-film capacitors. (author)

  9. Preparation and analysis of anodic aluminum oxide films with continuously tunable interpore distances

    Science.gov (United States)

    Qin, Xiufang; Zhang, Jinqiong; Meng, Xiaojuan; Deng, Chenhua; Zhang, Lifang; Ding, Guqiao; Zeng, Hao; Xu, Xiaohong

    2015-02-01

    Nanoporous anodic aluminum oxides are often used as templates for preparation of nanostructures such as nanodot, nanowire and nanotube arrays. The interpore distance of anodic aluminum oxide is the most important parameter in controlling the periodicity of these nanostructures. Herein we demonstrate a simple and yet powerful method to fabricate ordered anodic aluminum oxides with continuously tunable interpore distances. By using mixed solution of citric and oxalic acids with different molar ratio, the range of anodizing voltages within which self-ordered films can be formed were extended to between 40 and 300 V, resulting in the interpore distances change from 100 to 750 nm. Our work realized very broad range of interpore distances in a continuously tunable fashion and the experiment processes are easily controllable and reproducible. The dependence of the interpore distances on acid ratios in mixed solutions was discussed through analysis of anodizing current and it was found that the effective dissociation constant of the mixed acids is of great importance. The interpore distances achieved are comparable to wavelengths ranging from UV to near IR, and may have potential applications in optical meta-materials for photovoltaics and optical sensing.

  10. Growth of anodic films on compound semiconductor electrodes: InP in aqueous (NH sub 4) sub 2 S

    CERN Document Server

    Buckley, D N

    2002-01-01

    Film formation on compound semiconductors under anodic conditions is discussed. The surface properties of InP electrodes were examined following anodization in a (NH sub 4) sub 2 S electrolyte. The observation of a current peak in the cyclic voltammetric curve was attributed to selective etching of the substrate and a film formation process. AFM images of samples anodized in the sulfide solution revealed surface pitting. Thicker films formed at higher potentials exhibited extensive cracking as observed by optical and electron microscopy, and this was explicitly demonstrated to occur ex situ rather than during the electrochemical treatment. The composition of the thick film was identified as In sub 2 S sub 3 by EDX and XPS. The measured film thickness varies linearly with the charge passed, and comparison between experimental thickness measurements and theoretical estimates for the thickness indicate a porosity of over 70 %. Cracking is attributed to shrinkage during drying of the highly porous film and does n...

  11. ATOMIC LAYER DEPOSITION OF TITANIUM OXIDE THIN FILMS ONNANOPOROUS ALUMINA TEMPLATES FOR MEDICAL APPLICATIONS

    Energy Technology Data Exchange (ETDEWEB)

    Brigmon, R.

    2009-05-05

    Nanostructured materials may play a significant role in controlled release of pharmacologic agents for treatment of cancer. Many nanoporous polymer materials are inadequate for use in drug delivery. Nanoporous alumina provides several advantages over other materials for use in controlled drug delivery and other medical applications. Atomic layer deposition was used to coat all the surfaces of the nanoporous alumina membrane in order to reduce the pore size in a controlled manner. Both the 20 nm and 100 nm titanium oxide-coated nanoporous alumina membranes did not exhibit statistically lower viability compared to the uncoated nanoporous alumina membrane control materials. In addition, 20 nm pore size titanium oxide-coated nanoporous alumina membranes exposed to ultraviolet light demonstrated activity against Escherichia coli and Staphylococcus aureus bacteria. Nanostructured materials prepared using atomic layer deposition may be useful for delivering a pharmacologic agent at a precise rate to a specific location in the body. These materials may serve as the basis for 'smart' drug delivery devices, orthopedic implants, or self-sterilizing medical devices.

  12. Method for nanomodulation of metallic thin films following the replica-antireplica process based on porous alumina membranes

    Energy Technology Data Exchange (ETDEWEB)

    Palma, J.L. [Departamento de Ciencias Básicas, Facultad de Ingeniería, Universidad Central de Chile, Santa Isabel 1186, 8330601 Santiago (Chile); Center for the Development of Nanoscience and Nanotechnology (CEDENNA), 9170124 Santiago (Chile); Denardin, J.C.; Escrig, J. [Departamento de Física, Universidad de Santiago de Chile (USACH), Avda. Ecuador 3493, 9170124 Santiago (Chile); Center for the Development of Nanoscience and Nanotechnology (CEDENNA), 9170124 Santiago (Chile)

    2017-03-15

    In this paper we have introduced a method for modulation of metallic thin films by sputtering of metals on anodized aluminum templates. Using a high deposition rate during deposition of the non-magnetic metal on the Al pattern, we have separated the two metallic surfaces and, thus, imprinted a pattern of nanohills on a non-magnetic metallic film, such as Au, Ag or Cu. The morphology of the nanostructured metallic films was determined by scanning electron microscopy. Thus, we have confirmed that the ordering degree of the Al template remained after the replication process. Additionally, and as an example of use of these films, we have prepared Supermalloy thin films deposited by sputtering onto these nanostructured non-magnetic metals. The room temperature magnetic behavior of these thin films is also studied. Interestingly, we have found that when the external magnetic field is applied out of plane of the substrate, the coercivity increases linearly as we increase the radius of the nanohills. These soft magnetic films can open new opportunities for magnetic field sensor applications. - Highlights: • A very soft magnetic film is investigated on ordered nanohills. • It is possible to imprint a metallic pattern directly from the etched aluminum foil. • These nanopatterned substrates add an additional degree of freedom. • A method for modulation of metallic thin films.

  13. Superhydrophilicity of anodic aluminum oxide films: From 'honeycomb' to 'bird's nest'

    International Nuclear Information System (INIS)

    Ye Jiaming; Yin Qiming; Zhou Yongliang

    2009-01-01

    An electrochemical method has been used to prepare different kinds of surfaces including 'honeycomb'-like and 'bird's nest'-like surfaces on anodic aluminum oxide (AAO) films. The relationship between the morphology and wettability of the AAO films was investigated by scanning electron microscopy and the measurement of water contact angles. The results show that the 'bird's nest'-like structure is necessary for superhydrophilic property, which provide direct experimental evidences for the 3D capillary theory concerning superhydrophilicity. It is expected that this investigation will be devoted to guiding the fabrication of superhydrophilic and superhydrophobic surfaces.

  14. Formation of barrier-type anodic films on ZE41 magnesium alloy in a fluoride/glycerol electrolyte

    International Nuclear Information System (INIS)

    Hernández-López, J.M.; Němcová, A.; Zhong, X.L.; Liu, H.; Arenas, M.A.; Haigh, S.J.; Burke, M.G.; Skeldon, P.; Thompson, G.E.

    2014-01-01

    Highlights: • Barrier anodic films formed on ZE41 Mg alloy in glycerol/fluoride electrolyte. • Films contain oxygen and fluorine species; formation ratio ∼1.3 nm V −1 . • Nanocrystalline film structure, with MgO and MgF 2. • Zinc enrichment in alloy beneath anodic film. • Modified film formed above Mg-Zn-RE second phase. - Abstract: Barrier-type, nanocrystalline anodic films have been formed on a ZE41 magnesium alloy under a constant current density of 5 mA cm −2 in a glycerol/fluoride electrolyte, containing 5 vol.% of added water, at 293 K. The films contain magnesium, fluorine and oxygen as the major species, and lower amounts of alloying element species. The films grow at an efficiency of ∼0.8 to 0.9, with a formation ratio in the range of ∼1.2 to 1.4 nm V −1 at the matrix regions and with a ratio of ∼1.8 nm V −1 at Mg-Zn-RE second phase. At the former regions, rare earth species are enriched at the film surface and zinc is enriched in the alloy. A carbon- and oxygen-rich band within the film suggests that the films grow at the metal/film and film/electrolyte interfaces

  15. Fabrication and characterization of nanostructured anatase TiO{sub 2} films prepared by electrochemical anodization and their photocatalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Yurddaskal, Metin [Dokuz Eylul University, The Graduate School of Natural and Applied Sciences, Buca 35390, Izmir (Turkey); Dokuz Eylul University, Center for Fabrication and Applications of Electronic Materials (EMUM), Buca, 35390, Izmir (Turkey); Dikici, Tuncay, E-mail: tuncay.dikici@ikc.edu.tr [Dokuz Eylul University, The Graduate School of Natural and Applied Sciences, Buca 35390, Izmir (Turkey); Izmir Katip Celebi University, Department of Materials Science and Engineering, Cigli 35620, Izmir (Turkey); Yildirim, Serdar [Dokuz Eylul University, The Graduate School of Natural and Applied Sciences, Buca 35390, Izmir (Turkey); Dokuz Eylul University, Center for Fabrication and Applications of Electronic Materials (EMUM), Buca, 35390, Izmir (Turkey); Yurddaskal, Melis [Celal Bayar University, Department of Mechanical Engineering, Muradiye, 45140 Manisa (Turkey); Toparli, Mustafa; Celik, Erdal [Dokuz Eylul University, Center for Fabrication and Applications of Electronic Materials (EMUM), Buca, 35390, Izmir (Turkey); Dokuz Eylul University, Department of Metallurgical and Materials Engineering, Buca 35390, Izmir (Turkey)

    2015-12-05

    In this study, nanostructured anatase titanium dioxide (TiO{sub 2}) films were fabricated by electrochemical anodization of titanium first, and then annealed at 500 °C for 2 h. Effect of electrolyte concentration, anodization time and electrolyte temperature on the surface morphology of the resulting TiO{sub 2} thin films were investigated. The phase structures, surface morphology and chemical composition were analyzed using X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity tests of the samples were evaluated by the degradation of aqueous methylene blue (MB) solutions under UV light illumination for different periods of time. The results showed that the structure of nanostructured TiO{sub 2} films depended strongly on the anodization parameters. It was found that there were micro-scale pores (<10 μm) and nano-scale pores (diameter in the range from 40 to 70 nm) on the anodized titanium surfaces. This study indicated that structures, surface morphology, and surface area of the nanostructured anatase TiO{sub 2} films played an important role on their photocatalytic performance. The results clearly proved that nanostructured anatase TiO{sub 2} film prepared with optimum process parameters resulted in enhancement of the photocatalytic activity. - Highlights: • TiO{sub 2} thin films were prepared on titanium substrates by electrochemical anodization at 30 V. • Effect of various anodization parameters on the photocatalytic activity of titanium was investigated. • Micro- and nanoscale TiO{sub 2} pores formed on the titanium by anodizing. • Surface morphology of the TiO{sub 2} films plays an important role on the photocatalytic performance. • The sample anodized for 240 min showed the highest photocatalytic activity.

  16. Spectroscopic ellipsometry analysis of a thin film composite membrane consisting of polysulfone on a porous α-alumina support.

    Science.gov (United States)

    Ogieglo, Wojciech; Wormeester, Herbert; Wessling, Matthias; Benes, Nieck E

    2012-02-01

    Exposure of a thin polymer film to a fluid can affect properties of the film such as the density and thickness. In particular in membrane technology, these changes can have important implications for membrane performance. Spectroscopic ellipsometry is a convenient technique for in situ studies of thin films, because of its noninvasive character and very high precision. The applicability of spectroscopic ellipsometry is usually limited to samples with well-defined interfacial regions, whereas in typical composite membranes, often substantial and irregular intrusion of the thin film into the pores of a support exists. In this work, we provide a detailed characterization of a polished porous alumina membrane support, using variable-angle spectroscopic ellipsometry in combination with atomic force microscopy and mercury porosimetry. Two Spectroscopic ellipsometry optical models are presented that can adequately describe the surface roughness of the support. These models consider the surface roughness as a distinct layer in which the porosity gradually increases toward the outer ambient interface. The first model considers the porosity profile to be linear; the second model assumes an exponential profile. It is shown that the models can be extended to account for a composite membrane geometry, by deposition of a thin polysulfone film onto the support. The developed method facilitates practicability for in situ spectroscopic ellipsometry studies of nonequilibrium systems, i.e., membranes under actual permeation conditions.

  17. Investigation of CuInSe{sub 2} nanowire arrays with core–shell structure electrodeposited at various duty cycles into anodic alumina templates

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Yu-Song [Institute of Microelectronics, Department of Electrical Engineering, National Cheng-Kung University, Tainan 701, Taiwan (China); Wang, Na-Fu; Tsai, Yu-Zen [Department of Electronic Engineering, Cheng Shiu University, 840 Chengcing Rd., Niaosong District, Kaohsiung City 833, Taiwan (China); Lin, Jia-Jun [Institute of Microelectronics, Department of Electrical Engineering, National Cheng-Kung University, Tainan 701, Taiwan (China); Houng, Mau-Phon, E-mail: mphoung@eembox.ncku.edu.tw [Institute of Microelectronics, Department of Electrical Engineering, National Cheng-Kung University, Tainan 701, Taiwan (China)

    2017-02-28

    Highlights: • The present paper reports that CuInSe2 NW arrays were fabricated through pulsed electrode position onto an AAO template with various duty cycles, and a pore-filling ratio of approximately 92% was achieved. • GIXRD patterns showed that all CuInSe2 NW arrays were chalcopyrite and SAED images confirmed that the CuInSe2 NWs were polycrystalline. • PEDOT/CuInSe2 NW core–shell arrays were fabricated using surfactant-modified CuInSe2 NW surfaces showing the lotus effect. • Current–voltage plots revealed that the CuInSe2 NW arrays were p-type semiconductors; moreover, the core–shell structure improved the diode ideality factor from 3.91 to 2.63. - Abstract: Copper indium selenide (CuInSe{sub 2}) nanowire (NW) arrays were prepared at various electrolyte duty cycles by filling anodic alumina templates through the pulsed electrodeposition technique. X-ray diffraction and scanning electron microscopy (SEM) images showed that the nucleation mechanism of CuInSe{sub 2} NW arrays was affected by the electrodeposition duty cycle. Moreover, SEM images showed that the diameter and length of the NWs were 80 nm and 2 μm, respectively. Furthermore, PEDOT/CuInSe{sub 2} NW core–shell arrays were fabricated using surfactant-modified CuInSe{sub 2} NW surfaces showing the lotus effect. Transmission electron microscopy images confirmed that a core–shell structure was achieved. Current–voltage plots revealed that the CuInSe{sub 2} NW arrays were p-type semiconductors; moreover, the core–shell structure improved the diode ideality factor from 3.91 to 2.63.

  18. Enhanced apatite-forming ability and antibacterial activity of porous anodic alumina embedded with CaO-SiO2-Ag2O bioactive materials.

    Science.gov (United States)

    Ni, Siyu; Li, Xiaohong; Yang, Pengan; Ni, Shirong; Hong, Feng; Webster, Thomas J

    2016-01-01

    In this study, to provide porous anodic alumina (PAA) with bioactivity and anti-bacterial properties, sol-gel derived bioactive CaO-SiO2-Ag2O materials were loaded onto and into PAA nano-pores (termed CaO-SiO2-Ag2O/PAA) by a sol-dipping method and subsequent calcination of the gel-glasses. The in vitro apatite-forming ability of the CaO-SiO2-Ag2O/PAA specimens was evaluated by soaking them in simulated body fluid (SBF). The surface microstructure and chemical property before and after soaking in SBF were characterized. Release of ions into the SBF was also measured. In addition, the antibacterial properties of the samples were tested against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). The results showed that CaO-SiO2-Ag2O bioactive materials were successfully decorated onto and into PAA nano-pores. In vitro SBF experiments revealed that the CaO-SiO2-Ag2O/PAA specimens dramatically enhanced the apatite-forming ability of PAA in SBF and Ca, Si and Ag ions were released from the samples in a sustained and slow manner. Importantly, E. coli and S. aureus were both killed on the CaO-SiO2-Ag2O/PAA (by 100%) samples compared to PAA controls after 3 days of culture. In summary, this study demonstrated that the CaO-SiO2-Ag2O/PAA samples possess good apatite-forming ability and high antibacterial activity causing it to be a promising bioactive coating candidate for implant materials for orthopedic applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Investigation of CuInSe2 nanowire arrays with core–shell structure electrodeposited at various duty cycles into anodic alumina templates

    International Nuclear Information System (INIS)

    Cheng, Yu-Song; Wang, Na-Fu; Tsai, Yu-Zen; Lin, Jia-Jun; Houng, Mau-Phon

    2017-01-01

    Highlights: • The present paper reports that CuInSe2 NW arrays were fabricated through pulsed electrode position onto an AAO template with various duty cycles, and a pore-filling ratio of approximately 92% was achieved. • GIXRD patterns showed that all CuInSe2 NW arrays were chalcopyrite and SAED images confirmed that the CuInSe2 NWs were polycrystalline. • PEDOT/CuInSe2 NW core–shell arrays were fabricated using surfactant-modified CuInSe2 NW surfaces showing the lotus effect. • Current–voltage plots revealed that the CuInSe2 NW arrays were p-type semiconductors; moreover, the core–shell structure improved the diode ideality factor from 3.91 to 2.63. - Abstract: Copper indium selenide (CuInSe 2 ) nanowire (NW) arrays were prepared at various electrolyte duty cycles by filling anodic alumina templates through the pulsed electrodeposition technique. X-ray diffraction and scanning electron microscopy (SEM) images showed that the nucleation mechanism of CuInSe 2 NW arrays was affected by the electrodeposition duty cycle. Moreover, SEM images showed that the diameter and length of the NWs were 80 nm and 2 μm, respectively. Furthermore, PEDOT/CuInSe 2 NW core–shell arrays were fabricated using surfactant-modified CuInSe 2 NW surfaces showing the lotus effect. Transmission electron microscopy images confirmed that a core–shell structure was achieved. Current–voltage plots revealed that the CuInSe 2 NW arrays were p-type semiconductors; moreover, the core–shell structure improved the diode ideality factor from 3.91 to 2.63.

  20. Compositionally graded SiCu thin film anode by magnetron sputtering for lithium ion battery

    Energy Technology Data Exchange (ETDEWEB)

    Polat, B.D., E-mail: bpolat@itu.edu.tr [Department of Metallurgical and Materials Engineering, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey); Eryilmaz, O.L. [Energy Systems Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Keleş, O., E-mail: ozgulkeles@itu.edu.tr [Department of Metallurgical and Materials Engineering, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey); Erdemir, A. [Energy Systems Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Amine, K. [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2015-12-01

    Compositionally graded and non-graded composite SiCu thin films were deposited by magnetron sputtering technique on Cu disks for investigation of their potentials in lithium ion battery applications. The compositionally graded thin film electrodes with 30 at.% Cu delivered a 1400 mAh g{sup −1} capacity with 80% Coulombic efficiency in the first cycle and still retained its capacity at around 600 mAh g{sup −1} (with 99.9% Coulombic efficiency) even after 100 cycles. On the other hand, the non-graded thin film electrodes with 30 at.% Cu exhibited 1100 mAh g{sup −1} as the first discharge capacity with 78% Coulombic efficiency but the cycle life of this film degraded very quickly, delivering only 250 mAh g{sup −1} capacity after 100th cycles. Not only the Cu content but also the graded film thickness were believed to be the main contributors to the much superior performance of the compositionally graded SiCu films. We also believe that the Cu-rich region of the graded film helped reduce internal stress build-up and thus prevented film delamination during cycling. In particular, the decrease of Cu content from interface region to the top of the coating reduced the possibility of stress build-up across the film during cycling, thus leading to a high electrochemical performance.b - Highlights: • Highly adherent SiCu films are deposited by magnetron sputtering. • Compositionally graded SiCu film is produced and characterized. • Decrease of Cu content diverted the propagation of stress in the anode. • Cu rich layer at the bottom improves the adherence of the film.

  1. Structural-morphological variations in pseudo-barrier films of anode aluminium oxide under irradiation with high-energy particles

    International Nuclear Information System (INIS)

    Chernykh, M.A.; Belov, V.T.

    1988-01-01

    Comparative study of structural-morphological variations under electron beam effect in pseudo-barrier films of anode aluminium oxide, obtained in seven different solutions and proton or X-rays pre-irradiated to determine structure peculiarities of anode aluminium oxides, is presented. Such study is a matter of interest from the solid-phase transformation theory point of view and for anode aluminium films application under radiation. Stability increase of pseudo-barrier films of anode aluminium oxide to the effect of UEhMV-100 K microscope electron beam at standard modes of operation (75 kV) due to proton or X-rays irradiation is found. Difference in structural-monorphological variations obtained in different solutions of anode aluminium films under high-energy particles irradiation is determined. Strucural-phase microinhomogeneity of amorphous pseudo-barrier films of anode aluminium oxide and its influence on solid-phase transformations character under electron bean of maximal intensity are detected

  2. Electrochemical performance of Sn-Sb-Cu film anodes prepared by layer-by-layer electrodeposition

    International Nuclear Information System (INIS)

    Jiang Qianlei; Xue Ruisheng; Jia Mengqiu

    2012-01-01

    A novel layer-by-layer electrodeposition and heat-treatment approach was attempted to obtain Sn-Sb-Cu film anode for lithium ion batteries. The preparation of Sn-Sb-Cu anodes started with galvanostatic electrochemically depositing antimony and tin sequentially on the substrate of copper foil collector. Sn-Sb and Cu-Sb alloys were formed when heated. The SEM analysis showed that the crystalline grains become bigger and the surface of the Sn-Sb-Cu anode becomes more denser after annealing. The energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analysis showed the antimony, tin and copper were alloyed to form SnSb and Cu 2 Sb after heat treatment. The X-ray photoelectron spectroscopy (XPS) analysis showed the surface of the Sn-Sb-Cu electrode was covered by a thin oxide layer. Electrochemical measurements showed that the annealed Sn-Sb-Cu anode has high reversible capacity and good capacity retention. It exhibited a reversible capacity of about 962 mAh/g in the initial cycle, which still remained 715 mAh/g after 30 cycles.

  3. Ultrasonic Welding of Thin Alumina and Aluminum Using Inserts

    Science.gov (United States)

    Ishikuro, Tomoaki; Matsuoka, Shin-Ichi

    This paper describes an experimental study of ultrasonic welding of thin ceramics and metals using inserts. Ultrasonic welding has enable the joining of various thick ceramics, such as Al2O3 and ZrO2, to aluminum at room temperature quickly and easily as compared to other welding methods. However, for thin ceramics, which are brittle, welding is difficult to perform without causing damage. In this study, aluminum anodized oxide with different anodizing time was used as thin alumina ceramic. Vapor deposition of aluminum alloys was used to create an effective binder layer for welding at a low pressure and within a short duration in order to prevent damage to the anodic oxide film formed with a short anodizing time. For example, ultrasonic welding of thin Al2O3/Al was accomplished under the following conditions: ultrasonic horn tip amplitude of 30µm, welding pressure of 5MPa, and required duration of 0.1s. However, since the vapor deposition film tends to exfoliate as observed in the anodic oxide film formed with a long anodizing time, welding was difficult.

  4. Effect of postreatment on the corrosion behaviour of tartaric-sulphuric anodic films

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Rubio, M. [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049 Madrid (Spain); Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906 Getafe (Spain); Lara, M.P. de [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049 Madrid (Spain); Ocon, P. [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049 Madrid (Spain)], E-mail: pilar.ocon@uam.es; Diekhoff, S. [Fraunhofer-IFAM, Lesumer Heerstrasse 36, 28717 Bremen (Germany); Beneke, M. [Department of Surface Technologies, Engineering of Materials and Processes, Airbus Deutschland, GmbH Hunefeldstr. 1-5, 28199 Bremen (Germany); Lavia, A.; Garcia, I. [Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906 Getafe (Spain)

    2009-08-30

    Unclad and clad AA2024 T3 specimens were anodised in a chromium-free tartaric-sulphuric acid bath (TSA) and subsequently postreated by different processes including impregnation in a cold, concentrated chromate solution, Cr-free hot-water sealing, and dichromate hot-water sealing. The purpose of this work is to evaluate the effectiveness of the classical postreatments used in the aircraft industry on the TSA-anodic films and their corrosion resistance behaviour. TSA-anodic films were characterised by scanning electron microscopy (SEM) and their thicknesses were measured by SEM and the eddy current method. Electrochemical impedance spectroscopy (EIS) was used to characterise the barrier and porous layers, and jointly with potentiodynamic polarisation allowed the evaluation of corrosion resistance parameters with immersion time in NaCl solution for anodised and postreated specimens. In all cases the postreatments increased the resistance of the barrier layer against degradation. However, the NaCl electrolyte easily penetrated TSA-anodised porous layers when they were not postreated, while penetration was slightly more difficult in cold-postreated specimens. The effective pore plugging was observed in the sealed TSA specimens resulting in an improved corrosion resistance. On the other hand, unsealed clad AA2024 specimens showed a self-sealing process of the TSA-anodic layer, which was slower for the cold chromate solution-postreated specimens.

  5. Effect of postreatment on the corrosion behaviour of tartaric-sulphuric anodic films

    International Nuclear Information System (INIS)

    Garcia-Rubio, M.; Lara, M.P. de; Ocon, P.; Diekhoff, S.; Beneke, M.; Lavia, A.; Garcia, I.

    2009-01-01

    Unclad and clad AA2024 T3 specimens were anodised in a chromium-free tartaric-sulphuric acid bath (TSA) and subsequently postreated by different processes including impregnation in a cold, concentrated chromate solution, Cr-free hot-water sealing, and dichromate hot-water sealing. The purpose of this work is to evaluate the effectiveness of the classical postreatments used in the aircraft industry on the TSA-anodic films and their corrosion resistance behaviour. TSA-anodic films were characterised by scanning electron microscopy (SEM) and their thicknesses were measured by SEM and the eddy current method. Electrochemical impedance spectroscopy (EIS) was used to characterise the barrier and porous layers, and jointly with potentiodynamic polarisation allowed the evaluation of corrosion resistance parameters with immersion time in NaCl solution for anodised and postreated specimens. In all cases the postreatments increased the resistance of the barrier layer against degradation. However, the NaCl electrolyte easily penetrated TSA-anodised porous layers when they were not postreated, while penetration was slightly more difficult in cold-postreated specimens. The effective pore plugging was observed in the sealed TSA specimens resulting in an improved corrosion resistance. On the other hand, unsealed clad AA2024 specimens showed a self-sealing process of the TSA-anodic layer, which was slower for the cold chromate solution-postreated specimens.

  6. Properties of alumina films prepared by metal-organic chemical vapour deposition at atmospheric pressure in hte presence of small amounts of water

    NARCIS (Netherlands)

    Haanappel, V.A.C.; Haanappel, V.A.C.; van Corbach, H.D.; Rem, J.B.; Fransen, T.; Gellings, P.J.

    1995-01-01

    Thin alumina films were deposited on stainless steel, type AISI 304. The deposition process was carried out in nitrogen with low partial pressures of water (0–2.6 × 10−2 kPa (0−0.20 mmHg)) by metal-organic chemical vapour deposition (MOCVD) with aluminium-tri-sec-butoxide (ATSB) as the precursor.

  7. Deposition of fluorocarbon films by Pulsed Plasma Thruster on the anode side

    International Nuclear Information System (INIS)

    Zhang, Rui; Zhang, Daixian; Zhang, Fan; He, Zhen; Wu, Jianjun

    2013-01-01

    Fluorocarbon thin films were deposited by Pulsed Plasma Thruster at different angles on the anode side of the thruster. Density and velocity of the plasma in the plume of the Pulsed Plasma Thruster were determined using double and triple Langmuir probe apparatus respectively. The deposited films were characterized by X-ray photoelectron spectroscopy (XPS), scanning probe microscope (SPM) and UV–vis spectrometer. Low F/C ratio (0.64–0.86) fluorocarbon films are deposited. The F/C ratio decreases with angle increasing from 0 degree to 30 degree; however it turns to increase with angle increasing from 45 degree to 90 degree. The films deposited at center angles appear rougher compared with that prepared at angles beyond 45 degree. These films basically show having strong absorption properties for wavelength below 600 nm and having enhanced reflective characteristics. Due to the influence of the chemical composition and the surface morphology of the films, the optical properties of these films also show significant angular dependence.

  8. Effect of crystallographic orientation on the anodic formation of nanoscale pores/tubes in TiO 2 films

    Science.gov (United States)

    Kalantar-zadeh, K.; Sadek, A. Z.; Zheng, H.; Partridge, J. G.; McCulloch, D. G.; Li, Y. X.; Yu, X. F.; Wlodarski, W.

    2009-10-01

    Self-organized nanopores and nanotubes have been produced in thin films of titanium (Ti) prepared using filtered cathodic vacuum arc (FCVA), DC- and RF-sputter deposition systems. The anodization process was performed using a neutral electrolyte containing fluoride ions with an applied potential between 2 and 20 V (for clarity the results are only presented for 5 V). Scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD) techniques were used to characterise the films. It was found that the crystallographic orientation of the Ti films played a significant role in determining whether pores or tubes were formed during the anodic etching process.

  9. The effects of anode material type on the optoelectronic properties of electroplated CdTe thin films and the implications for photovoltaic application

    Science.gov (United States)

    Echendu, O. K.; Dejene, B. F.; Dharmadasa, I. M.

    2018-03-01

    The effects of the type of anode material on the properties of electrodeposited CdTe thin films for photovoltaic application have been studied. Cathodic electrodeposition of two sets of CdTe thin films on glass/fluorine-doped tin oxide (FTO) was carried out in two-electrode configuration using graphite and platinum anodes. Optical absorption spectra of films grown with graphite anode displayed significant spread across the deposition potentials compared to those grown with platinum anode. Photoelectrochemical cell result shows that the CdTe grown with graphite anode became p-type after post-deposition annealing with prior CdCl2 treatment, as a result of carbon incorporation into the films, while those grown with platinum anode remained n-type after annealing. A review of recent photoluminescence characterization of some of these CdTe films reveals the persistence of a defect level at (0.97-0.99) eV below the conduction band in the bandgap of CdTe grown with graphite anode after annealing while films grown with platinum anode showed the absence of this defect level. This confirms the impact of carbon incorporation into CdTe. Solar cell made with CdTe grown with platinum anode produced better conversion efficiency compared to that made with CdTe grown using graphite anode, underlining the impact of anode type in electrodeposition.

  10. Low hydrogen containing amorphous carbon films - Growth and electrochemical properties as lithium battery anodes

    Energy Technology Data Exchange (ETDEWEB)

    Subramanian, V.; Masarapu, Charan; Wei, Bingqing [Department of Mechanical Engineering, University of Delaware, 130 Academy Street, Newark, DE 19716 (United States); Karabacak, Tansel [Department of Applied Science, University of Arkansas at Little Rock, 2801 South University Avenue, Little Rock, AR 72204 (United States); Teki, Ranganath [Department of Chemical and Biological Engineering, Rensselaer Polytechnic Institute, Troy, NY 12180 (United States); Lu, Toh-Ming [Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, Troy, NY 12180 (United States)

    2010-04-02

    Amorphous carbon films were deposited successfully on Cu foils by DC magnetron sputtering technique. Electrochemical performance of the film as lithium battery anode was evaluated across Li metal at 0.2 C rate in a non-aqueous electrolyte. The discharge curves showed unusually low irreversible capacity in the first cycle with a reversible capacity of {proportional_to}810 mAh g{sup -1}, which is at least 2 times higher than that of graphitic carbon. For the first time we report here an amorphous carbon showing such a high reversibility in the first cycle, which is very much limited to the graphitic carbon. The deposited films were extensively characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and step profilometer for the structural and surface properties. The hydrogen content of the synthesized films was studied using residual gas analysis (RGA). The low hydrogen content and the low specific surface area of the synthesized amorphous carbon film are considered responsible for such a high first cycle columbic efficiency. The growth mechanism and the reasons for enhanced electrochemical performance of the carbon films are discussed. (author)

  11. Low hydrogen containing amorphous carbon films-Growth and electrochemical properties as lithium battery anodes

    Science.gov (United States)

    Subramanian, V.; Karabacak, Tansel; Masarapu, Charan; Teki, Ranganath; Lu, Toh-Ming; Wei, Bingqing

    Amorphous carbon films were deposited successfully on Cu foils by DC magnetron sputtering technique. Electrochemical performance of the film as lithium battery anode was evaluated across Li metal at 0.2 C rate in a non-aqueous electrolyte. The discharge curves showed unusually low irreversible capacity in the first cycle with a reversible capacity of ∼810 mAh g -1, which is at least 2 times higher than that of graphitic carbon. For the first time we report here an amorphous carbon showing such a high reversibility in the first cycle, which is very much limited to the graphitic carbon. The deposited films were extensively characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and step profilometer for the structural and surface properties. The hydrogen content of the synthesized films was studied using residual gas analysis (RGA). The low hydrogen content and the low specific surface area of the synthesized amorphous carbon film are considered responsible for such a high first cycle columbic efficiency. The growth mechanism and the reasons for enhanced electrochemical performance of the carbon films are discussed.

  12. The effect of different thickness alumina capping layers on the final morphology of dewet thin Ni films

    Science.gov (United States)

    White, Benjamin C.; Behbahanian, Amir; Stoker, T. McKay; Fowlkes, Jason D.; Hartnett, Chris; Rack, Phillip D.; Roberts, Nicholas A.

    2018-03-01

    Nanoparticles on a substrate have numerous applications in nanotechnology, from enhancements to solar cell efficiency to improvements in carbon nanotube growth. Producing nanoparticles in a cost effective fashion with control over size and spacing is desired, but difficult to do. This work presents a scalable method for altering the radius and pitch distributions of nickel nanoparticles. The introduction of alumina capping layers to thin nickel films during a pulsed laser-induced dewetting process has yielded reductions in the mean and standard deviation of radii and pitch for dewet nanoparticles with no noticeable difference in final morphology with increased capping layer thickness. The differences in carbon nanotube mats grown, on the uncapped sample and one of the capped samples, is also presented here, with a more dense mat being present for the capped case.

  13. Solid-state electrochromic cell with anodic iridium oxide film electrodes

    International Nuclear Information System (INIS)

    Dautremont-Smith, W.C.; Beni, G.; Schiavone, L.M.; Shay, J.L.

    1979-01-01

    A new solid-state electrochromic cell has been fabricated using an anodic iridium oxide film (AIROF) display electrode. The cell has the symmetric sandwich structure AIROFvertical-barNafionvertical-barAIROF, with the Nafion solid electrolyte opacified by an in situ precipitation technique. A symmetric square-wave voltage of 1.5 V amplitude produces clearly perceivable color changes from pale to dark blue-gray in approx. =1 sec when viewed in diffuse reflection. Good open-circuit optical memory is exhibited:

  14. Lasing of a Solid-State Active Element Based on Anodized Aluminum Oxide Film Doped with Rhodamine 6G

    Science.gov (United States)

    Shelkovnikov, V. V.; Lyubas, G. A.; Korotaev, S. V.; Kopylova, T. N.; Tel'minov, E. N.; Gadirov, R. M.; Nikonova, E. N.; Nikonov, S. Yu.; Solodova, T. A.; Novikov, V. A.

    2017-04-01

    Spectral-luminescent and lasing characteristics of rhodamine 6G in porous aluminum oxide films anodized under various conditions are investigated. Lasing is obtained without external resonator in the longitudinal scheme under excitation by the second harmonic of Nd3+:YAG-laser radiation. The threshold pump power densities are in the range 3.5-15 MW/cm2 depending on the anodizing conditions. Wherein, the lasing line narrows down from 12 to 5 nm.

  15. Composition, structure and electrical properties of alumina barrier layers grown in fluoride-containing oxalic acid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Jagminas, A. [Institute of Chemistry, A. Gostauto 9, LT-01108 Vilnius (Lithuania)], E-mail: jagmin@ktl.mii.lt; Vrublevsky, I. [Department of Microelectricals, Belarusian State University of Informatics and Radioelectricals, 6 Brovka Street, Minsk 220013 (Belarus); Kuzmarskyte, J.; Jasulaitiene, V. [Institute of Chemistry, A. Gostauto 9, LT-01108 Vilnius (Lithuania)

    2008-04-15

    The composition, structure and electrical properties of alumina barrier layers grown by anodic oxidation in F{sup -}-containing (FC) and F{sup -}-free (FF) oxalic acid solutions were studied using the re-anodizing/dissolution technique, Fourier-transformed infrared and X-ray photoelectron spectroscopy. These results confirmed formation in FC anodizing solutions of films structurally different from ones grown in FF oxalic acid baths. It was found that the barrier layer of FC alumina films is composed of two layers differing in the dissolution rate. These differences are related to the formation in the FC electrolyte of a barrier layer composed of a more microporous outer part and a thin, non-porous and non-scalloped inner part consisting of aluminum oxide and aluminum fluoride.

  16. Preparation of CaO-SiO2-CuO bioactive glasses-embedded anodic alumina with improved biological activities

    Directory of Open Access Journals (Sweden)

    Ni Siyu

    2017-10-01

    Full Text Available To improve bone cell cytocompatibility properties of porous anodic alumina (PAA and implement anti-bacterial properties, amorphous CaO-SiO2-CuO materials were loaded into PAA nano-pores (termed CaO-SiO2- CuO/PAA by a facile ultrasonic-assisted sol-dipping strategy. The surface features and chemistry of the obtained CaO-SiO2-CuO/PAA were investigated by a field emission scanning microscope (FESEM, an energy-dispersive Xray spectrometer (EDS and an X-ray photoelectron spectroscopy (XPS. The ability of the CaO-SiO2-CuO/PAA specimens to form apatite via a bio-mineralization processwas evaluated by soaking them in simulated body fluid (SBF in vitro. The surface microstructure and chemical properties after soaking in SBFwere characterized. The release of ions into the SBF was also measured. In addition, rat osteoblasts and two types of bacterial were cultured on the samples to determine their cytocompatibility and antibacterial properties. The results showed that the amorphous CaO-SiO2-CuO materials were successfully decorated into PAA nano-pores and at the same time maintained their nano-featured surfaces. The CaO-SiO2-CuO/PAA samples induced apatite-mineralization in SBF. Meanwhile, the CaO-SiO2-CuO/PAA samples demonstrated great potential for promoting the proliferation of osteoblasts and inhibiting Escherichia coli (E. coli as well as Staphylococcus. aureus (S. aureus growth. Specifically, there was an 86.5±4.1% reduction in E. coli, an 88.0 ± 2.2% reduction in S. aureus for the CaO-SiO2-CuO/PAA surfaces compared to PAA controls. The capability to promote osteoblast proliferation and better antibacterial activity of CaO-SiO2- CuO/PAA may be attributed to the fact that Cu ions can be slowly and constantly released from the samples. Importantly, this was achieved without the use of antibiotics or any pharmaceutical agent. Ultimately, these results suggest that the CaO-SiO2-CuO/PAA substrates possessed improved bone cell cytocompatibility and high

  17. Karakteristik Tcr Dan Vcr Resistor Pasta Resistor Pada Substrat Alumina Dengan Teknologi Film Tebal

    OpenAIRE

    Raden Arief Setyawan, ST., MT., Rhezananta Arya H., Ir. M. Julius St., MS

    2014-01-01

    Resistor merupakan komponen yang sangat berperan dalam rangkaian film tebal. Resistor berteknologi film tebal mempunyai karakteristik yang terdiri dari TCR (Temperature Coefficient of Resistance) dan VCR (Voltage Coefficient of Resistance). Dari alasan di atas maka perlu untuk mengetahui bagaimana pembuatan resistor film tebal dan mengetahui karakteristiknya.Penelitian ini menggunakan proses screen printing dalam pembuatan resistor yang kemudian melalui proses pengendapan (15 menit), drying (...

  18. Tube Inner Coating of Non-Conductive Films by Pulsed Reactive Coaxial Magnetron Plasma with Outer Anode

    Directory of Open Access Journals (Sweden)

    Musab Timan Idriss Gasab

    2018-03-01

    Full Text Available The double-ended coaxial magnetron pulsed plasma (DCMPP method with auxiliary outer anode was introduced in order to achieve the uniform coating of non-conductive thin films on the inner walls of insulator tubes. In this study, titanium (Ti was employed as a cathode (sputtering target, and a glass tube was used as a substrate. In an argon (Ar and oxygen (O2 gas mixture, magnetron plasma was generated. Oxygen gas was introduced to deposit a titanium oxide (TiO2 film. A comparison between films coated with and without an auxiliary outer anode was made. As a result, it was clearly shown that the DCMPP method using an auxiliary outer anode enhanced the uniformity of the deposited non-conductive film compared to the conventional DCMPP method. Moreover, the optimum conditions under which the thin TiO2 film was deposited on the inner wall of the glass tube were revealed. From the results, it was supposed that the auxiliary outer anode contributed to the uniformity of the distributions of deposited negative charge on the non-conductive film and consequently the electric field and the plasma density uniform.

  19. Designing robust alumina nanowires-on-nanopores structures: superhydrophobic surfaces with slippery or sticky water adhesion.

    Science.gov (United States)

    Peng, Shan; Tian, Dong; Miao, Xinrui; Yang, Xiaojun; Deng, Wenli

    2013-11-01

    Hierarchical alumina surfaces with different morphologies were fabricated by a simple one-step anodization method. These alumina films were fabricated by a new raw material: silica gel plate (aluminum foil with a low purity of 97.17%). The modulation of anodizing time enabled the formation of nanowires-on-nanopores hybrid nanostructures having controllable nanowires topographies through a self-assembly process. The resultant structures were demonstrated to be able to achieve superhydrophobicity without any hydrophobic coating layer. More interestingly, it is found that the as-prepared superhydrophobic alumina surfaces exhibited high contrast water adhesion. Hierarchical alumina film with nanowire bunches-on-nanopores (WBOP) morphology presents extremely slippery property which can obtain a sliding angle (SA) as low as 1°, nanowire pyramids-on-nanopores (WPOP) structure shows strongly sticky water adhesion with the adhesive ability to support 15 μL inverted water droplet at most. The obtained superhydrophobic alumina surfaces show remarkable mechanical durability even treated by crimping or pressing without impact on the water-repellent performance. Moreover, the created surfaces also show excellent resistivity to ice water, boiling water, high temperature, organic solvent and oil contamination, which could expand their usefulness and efficacy in harsh conditions. Copyright © 2013 Elsevier Inc. All rights reserved.

  20. An anode with aluminum doped on zinc oxide thin films for organic light emitting devices

    International Nuclear Information System (INIS)

    Xu Denghui; Deng Zhenbo; Xu Ying; Xiao Jing; Liang Chunjun; Pei Zhiliang; Sun Chao

    2005-01-01

    Doped zinc oxides are attractive alternative materials as transparent conducting electrode because they are nontoxic and inexpensive compared with indium tin oxide (ITO). Transparent conducting aluminum-doped zinc oxide (AZO) thin films have been deposited on glass substrates by DC reactive magnetron sputtering method. Films were deposited at a substrate temperature of 150-bar o C in 0.03 Pa of oxygen pressure. The electrical and optical properties of the film with the Al-doping amount of 2 wt% in the target were investigated. For the 300-nm thick AZO film deposited using a ZnO target with an Al content of 2 wt%, the lowest electrical resistivity was 4x10 -4 Ωcm and the average transmission in the visible range 400-700 nm was more than 90%. The AZO film was used as an anode contact to fabricate organic light-emitting diodes. The device performance was measured and the current efficiency of 2.9 cd/A was measured at a current density of 100 mA/cm 2

  1. Enhanced tribological behavior of anodic films containing SiC and PTFE nanoparticles on Ti6Al4V alloy

    International Nuclear Information System (INIS)

    Li, Songmei; Zhu, Mengqi; Liu, Jianhua; Yu, Mei; Wu, Liang; Zhang, Jindan; Liang, Hongxing

    2014-01-01

    Highlights: • An environmental friendly sodium tartrate (C 4 O 6 H 4 Na 2 ) electrolyte is used. • SiC and PTFE nanoparticles reduce friction coefficient of composite films. • SiC and PTFE nanoparticles demonstrate a favorable synergistic effect on improving tribological properties of composite films. • Lubricating mechanisms of SiC and PTFE nanoparticles are discussed. - Abstract: Anodic films containing SiC and polytetrafluoroethylene (PTFE) nanoparticles were successfully fabricated on Ti6Al4V alloy by using anodic oxidation method in an environmental friendly electrolyte. The morphology, structure and composition of the films were studied with the scanning electron microscope (SEM) and energy dispersive spectrometer (EDS). The results showed that the film contained a layered structure and have a surface full of petaloid bulges, which was totally different from the common anodic oxide film of the porous kind. The tribological properties of the films were investigated with dry friction tests in terms of the friction coefficient, wear rate and the morphology of worn surfaces. The results indicated that the SiC/PTFE composite film exhibited much better anti-wear and anti-friction performances than that of the SiC composite film, the PTFE composite film and the ordinary film without nanoparticles. The SiC/PTFE composite film has friction coefficient of 0.1 and wear rate of 20.133 mg/m, which was decreased respectively by 80% and 44.5% compared with that of the ordinary film. The lubricating mechanisms of the composite film containing SiC and PTFE nanoparticles were discussed. PTFE nanoparticles could lead to the formation of lubricating layer while SiC nanoparticles inside the lubricating layer turned sliding friction to rolling friction

  2. Effects of benzotriazole on anodized film formed on AZ31B magnesium alloy in environmental-friendly electrolyte

    International Nuclear Information System (INIS)

    Guo Xinghua; An Maozhong; Yang Peixia; Li Haixian; Su Caina

    2009-01-01

    An environmental-friendly electrolyte of silicate and borate, which contained an addition agent of 1H-benzotriazole (BTA) with low toxicity (LD50 of 965 mg/kg), was used to prepare an anodized film on AZ31B magnesium alloy under the constant current density of 1.5 A/dm 2 at room temperature. Effects of BTA on the properties of the anodized film were studied by scanning electron microscopy (SEM), energy dispersion spectrometry (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), loss weight measurement, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS), respectively. The results demonstrated that anodized growth process, surface morphology, thickness, phase structure and corrosion resistance of the anodized film were strongly dependant on the BTA concentration, which might be attributed to the formation of an BTA adsorption layer on magnesium substrate surface. When the BTA concentration was 5 g/L in the electrolyte, a compact and thick anodized film could provide excellent corrosion resistance for AZ31B magnesium alloy.

  3. Relationship between microstructure and optical properties of a novel perovskite C12PbI4 embedded in matrix of porous alumina

    Science.gov (United States)

    Zaghdoudi, W.; Bardaoui, A.; Khalifa, N.; Chtourou, R.

    2013-01-01

    In this study, organic-inorganic hybrid perovskite multiple quantum wells (PbI QWs) embedded in porous anodic alumina (PAA) thin films on glass and aluminum substrates are investigated in detail. The pore height and diameter of the nanoscale structure of porous anodic alumina (PAA) film produced by the anodization technique are controllable. The synthesized films are characterized morphologically using the atomic force microscopy (AFM). Scanning electron microscopy (SEM) study showed granular surface. The structural and optical properties were investigated by X-ray diffraction (XRD), photoluminescence (PL) and UV-Vis-NIR spectrophotometer. The effect of the two different substrates on the impregnation of the PbI QW in the PAA is presented. Both PL and AFM studies show a better penetration of the PbI QW in the case of the Al substrate providing a wider pore diameter. Remarkable enhancement of quantum confinement is demonstrated.

  4. Light-Weight Free-Standing Carbon Nanotube-Silicon Films for Anodes of Lithium Ion Batteries

    KAUST Repository

    Cui, Li-Feng

    2010-07-27

    Silicon is an attractive alloy-type anode material because of its highest known capacity (4200 mAh/g). However, lithium insertion into and extraction from silicon are accompanied by a huge volume change, up to 300%, which induces a strong strain on silicon and causes pulverization and rapid capacity fading due to the loss of the electrical contact between part of silicon and current collector. Si nanostructures such as nanowires, which are chemically and electrically bonded to the current collector, can overcome the pulverization problem, however, the heavy metal current collectors in these systems are larger in weight than Si active material. Herein we report a novel anode structure free of heavy metal current collectors by integrating a flexible, conductive carbon nanotube (CNT) network into a Si anode. The composite film is free-standing and has a structure similar to the steel bar reinforced concrete, where the infiltrated CNT network functions as both mechanical support and electrical conductor and Si as a high capacity anode material for Li-ion battery. Such free-standing film has a low sheet resistance of ∼30 Ohm/sq. It shows a high specific charge storage capacity (∼2000 mAh/g) and a good cycling life, superior to pure sputtered-on silicon films with similar thicknesses. Scanning electron micrographs show that Si is still connected by the CNT network even when small breaking or cracks appear in the film after cycling. The film can also "ripple up" to release the strain of a large volume change during lithium intercalation. The conductive composite film can function as both anode active material and current collector. It offers ∼10 times improvement in specific capacity compared with widely used graphite/copper anode sheets. © 2010 American Chemical Society.

  5. Mathematical modeling of sustainability of porous Al2O3 growth during two-stage anodization process

    Science.gov (United States)

    Aryslanova, Elizaveta M.; Alfimov, Anton V.; Chivilikhin, Sergey A.

    2015-06-01

    Currently, due to the development of nanotechnology and metamaterials, it has become important to obtain regular nanoporous structures with different parameters, such as porous anodic alumina films that are used for synthesis of various nanocomposites. In this work we consider the motion of the interfaces between electrolyte and alumina layers, and between alumina and aluminum layers. We also took into account the dynamics of moving boundaries and the change of small perturbations of these boundaries. Each area under Laplace's equation is solved for the potential of the electric field. The growth of porous alumina is described with the theory of small perturbations. Small perturbations of the interface are considered, which lead to small changes in potential and current in the boundaries. As a result of the developed model we obtained the minimum distance between centers of aluminum oxide pores in the beginning of anodizing process and the wavelength of porous structure irregularities.

  6. Thermally Annealed Iron (Oxide) Thin Film on an Alumina Barrier Layer, by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Madaan, Nitesh; Kanyal, Supriya S.; Jensen, David S.; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Linford, Matthew R.

    2013-09-06

    Herein we show characterization of an Fe thin film on Al_2O_3 after thermal annealing under H_2 using Al Ka X-rays. The XPS survey spectrum, narrow Fe 2p scan, and valence band regions are presented. The survey spectrum shows aluminum signals due to exposure of the underlying Al_2O_3 film during Fe nanoparticle formation.

  7. In vitro biocompatibility and electrical stability of thick-film platinum/gold alloy electrodes printed on alumina

    Science.gov (United States)

    Carnicer-Lombarte, Alejandro; Lancashire, Henry T.; Vanhoestenberghe, Anne

    2017-06-01

    Objective. High-density electrode arrays are a powerful tool in both clinical neuroscience and basic research. However, current manufacturing techniques require the use of specialised techniques and equipment, which are available to few labs. We have developed a high-density electrode array with customisable design, manufactured using simple printing techniques and with commercially available materials. Approach. Electrode arrays were manufactured by thick-film printing a platinum-gold alloy (Pt/Au) and an insulating dielectric on 96% alumina ceramic plates. Arrays were conditioned in serum and serum-free conditions, with and without 1 kHz, 200 µA, charge balanced stimulation for up to 21 d. Array biocompatibility was assessed using an extract assay and a PC-12 cell contact assay. Electrode impedance, charge storage capacity and charge injection capacity were before and after array conditioning. Main results. The manufactured Pt/Au electrodes have a highly porous surface and exhibit electrical properties comparable to arrays manufactured using alternative techniques. Materials used in array manufacture were found to be non-toxic to L929 fibroblasts by extract assay, and neuronal-like PC-12 cells adhered and extended neurites on the array surfaces. Arrays remained functional after long-term delivery of electrical pulses while exposed to protein-rich environments. Charge storage capacities and charge injection capacities increased following stimulation accounted for by an increase in surface index (real surface area) observed by vertical scanning interferometry. Further, we observed accumulation of proteins at the electrode sites following conditioning in the presence of serum. Significance. This study demonstrates the in vitro biocompatibility of commercially available thick-film printing materials. The printing technique is both simple and versatile, with layouts readily modified to produce customized electrode arrays. Thick-film electrode arrays are an

  8. TiO2 nanotube formation by Ti film anodization and their transport properties for dye-sensitized solar cells

    NARCIS (Netherlands)

    Iraj, M.; Kolahdouz, M.; Asl-Soleimani, E.; Esmaeili, E.; Kolahdouz Esfahani, Z.

    2016-01-01

    In this paper, we present the synthesis of TiO2 nanotube (NT) arrays formed by anodization of Ti film deposited on a fluorine-doped tin oxide-coated glass substrate by direct current magnetron sputtering. NH4F/ethylene glycol electrolyte was used to demonstrate the growth of stable nanotubes at room

  9. Nickel oxide film with open macropores fabricated by surfactant-assisted anodic deposition for high capacitance supercapacitors.

    Science.gov (United States)

    Wu, Mao-Sung; Wang, Min-Jyle

    2010-10-07

    Nickel oxide film with open macropores prepared by anodic deposition in the presence of surfactant shows a very high capacitance of 1110 F g(-1) at a scan rate of 10 mV s(-1), and the capacitance value reduces to 950 F g(-1) at a high scan rate of 200 mV s(-1).

  10. Light-Weight Free-Standing Carbon Nanotube-Silicon Films for Anodes of Lithium Ion Batteries

    KAUST Repository

    Cui, Li-Feng; Hu, Liangbing; Choi, Jang Wook; Cui, Yi

    2010-01-01

    and Si as a high capacity anode material for Li-ion battery. Such free-standing film has a low sheet resistance of ∼30 Ohm/sq. It shows a high specific charge storage capacity (∼2000 mAh/g) and a good cycling life, superior to pure sputtered-on silicon

  11. Correlation of electrolyte-derived inclusions to crystallization in the early stage of anodic oxide film growth on titanium

    Energy Technology Data Exchange (ETDEWEB)

    Jaeggi, C., E-mail: christian.jaeggi@empa.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Advanced Materials Processing Laboratory, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Parlinska-Wojtan, M., E-mail: magdalena.parlinska@empa.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Center for Electron Microscopy, Ueberlandstrasse 129, CH-8600 Duebendorf (Switzerland); Kern, P., E-mail: Philippe.Kern@neopac.ch [Empa, Swiss Federal Laboratories for Materials Testing and Research, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland)

    2012-01-01

    Pure titanium has been subjected to anodization in sulfuric and phosphoric acid. For a better understanding of the oxide growth and properties of the final film, with a particular interest focused on the solution anions in the early stage of crystallization, microstructural analyses (Raman, Transmission Electron Microscopy [TEM]) of the oxide films were correlated to chemical depth profiling by glow discharge optical emission spectroscopy (GDOES). Raman spectroscopy shows that crystallization of the oxide films starts at potentials as low as 10-20 V. The onset of crystallization and the ongoing increase in crystallinity with increasing anodization potentials had already earlier been correlated to ac-impedance measurements [Jaeggi et al., Surf. Interface Anal. 38 (2006) 182]. TEM observations show a clear difference in the early phase of crystallization between oxides grown in 1 M sulfuric acid compared to 1 M phosphoric acid. Moreover, independent of electrolyte type, nano-sized pores from oxygen bubbles formation were revealed in the central part of the films. Until now, oxygen bubbles inside an anodically grown oxide have not been observed before without the presence of crystalline regions nearby. A growth model is proposed, in which the different starting locations of crystallization inside the films are correlated to the presence of the acid anions as residues in the film, as found by GDOES chemical depth-profiling.

  12. Red Phosphorus-Embedded Cross-Link-Structural Carbon Films as Flexible Anodes for Highly Reversible Li-Ion Storage

    Energy Technology Data Exchange (ETDEWEB)

    Ruan, Jiafeng [School of Materials; Yuan, Tao [School of Materials; Pang, Yuepeng [School of Materials; Xu, Xinbo [School of Materials; Yang, Junhe [School of Materials; Hu, Wenbin; Zhong, Cheng; Ma, Zi-Feng [Shanghai Electrochemical Energy Devices Research Center,; Bi, Xuanxuan [Chemical; Zheng, Shiyou [School of Materials

    2017-10-06

    Red phosphorus (P) is considered to be one of the most attractive anodic materials for lithium-ion batteries (LIBs) due to its high theoretical capacity of 2596 mAh g–1. However, intrinsic characteristics such as the poor electronic conductivity and large volume expansion at lithiation impede the development of red P. Here, we design a new strategy to embed red P particles into a cross-link-structural carbon film (P–C film), in order to improve the electronic conductivity and accommodate the volume expansion. The red P/carbon film is synthesized via vapor phase polymerization (VPP) followed by the pyrolysis process, working as a flexible binder-free anode for LIBs. High cycle stability and good rate capability are achieved by the P–C film anode. With 21% P content in the film, it displays a capacity of 903 mAh g–1 after 640 cycles at a current density of 100 mA g–1 and a capacity of 460 mAh g–1 after 1000 cycles at 2.0 A g–1. Additionally, the Coulombic efficiency reaches almost 100% for each cycle. The superior properties of the P–C films together with their facile fabrication make this material attractive for further flexible and high energy density LIB applications.

  13. Flexible Overoxidized Polypyrrole Films with Orderly Structure as High-Performance Anodes for Li- and Na-Ion Batteries.

    Science.gov (United States)

    Yuan, Tao; Ruan, Jiafeng; Zhang, Weimin; Tan, Zhuopeng; Yang, Junhe; Ma, Zi-Feng; Zheng, Shiyou

    2016-12-28

    Flexible polypyrrole (PPy) films with highly ordered structures were fabricated by a novel vapor phase polymerization (VPP) process and used as the anode material in lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs). The PPy films demonstrate excellent rate performance and cycling stability. At a charge/discharge rate of 1 C, the reversible capacities of the PPy film anode reach 284.9 and 177.4 mAh g -1 in LIBs and SIBs, respectively. Even at a charge/discharge rate of 20 C, the reversible capacity of the PPy film anode retains 54.0% and 52.9% of the capacity of 1 C in LIBs and SIBs, respectively. After 1000 electrochemical cycles at a rate of 10 C, there is no obvious capacity fading. The molecular structure and electrochemical behaviors of Li- and Na-ion doping and dedoping in the PPy films are investigated by XPS and ex situ XRD. It is believed that the PPy film electrodes in the overoxidized state can be reversibly charged and discharged through the doping and dedoping of lithium or sodium ions. Because of the self-adaptation of the doped ions, the ordered pyrrolic chain structure can realize a fast charge/discharge process. This result may substantially contribute to the progress of research into flexible polymer electrodes in various types of batteries.

  14. Role of oxygen vacancies in anodic TiO2 thin films

    International Nuclear Information System (INIS)

    Tit, N.; Halley, J.W.

    1992-05-01

    Defects play an important role in the electronic and optical properties of amorphous solids in general. Here we present both experimental and theoretical investigations on the nature and origin of defect states in anodic rutile TiO 2 thin films (of thickness 5nm to 20nm). There is experimental evidence that the observed gap state at 0.7eV below the edge of conduction-band is due to an oxygen vacancy. For this reason, oxygen vacancies are used in our model. A comparison of the calculated bulk-photoconductivity to photospectroscopy experiment reveals that the films have bulk-like transport properties. On the other hand a fit of the surface density of states to the scanning tunneling microscopy (STM) on the (001) surfaces has suggested a surface defect density of 5% of oxygen vacancies. To resolve this discrepancy, we calculated the dc-conductivity where localization effects are included. Our results show an impurity band formation at about p c =9% of oxygen vacancies. We concluded that the gap states seen in STM are localized and the oxygen vacancies are playing the role of trapping centers (deep levels) in the studied films. (author). 15 refs, 5 figs

  15. New roots to formation of nanostructures on glass surface through anodic oxidation of sputtered aluminum

    Directory of Open Access Journals (Sweden)

    Satoru Inoue, Song-Zhu Chu, Kenji Wada, Di Li and Hajime Haneda

    2003-01-01

    Full Text Available New processes for the preparation of nanostructure on glass surfaces have been developed through anodic oxidation of sputtered aluminum. Aluminum thin film sputtered on a tin doped indium oxide (ITO thin film on a glass surface was converted into alumina by anodic oxidation. The anodic alumina gave nanometer size pore array standing vertically on the glass surface. Kinds of acids used in the anodic oxidation changed the pore size drastically. The employment of phosphoric acid solution gave several tens nanometer size pores. Oxalic acid cases produced a few tens nanometer size pores and sulfuric acid solution provided a few nanometer size pores. The number of pores in a unit area could be changed with varying the applied voltage in the anodization and the pore sizes could be increased by phosphoric acid etching. The specimen consisting of a glass substrate with the alumina nanostructures on the surface could transmit UV and visible light. An etched specimen was dipped in a TiO2 sol solution, resulting in the impregnation of TiO2 sol into the pores of alumina layer. The TiO2 sol was heated at ~400 °C for 2 h, converting into anatase phase TiO2. The specimens possessing TiO2 film on the pore wall were transparent to the light in UV–Visible region. The electro deposition technique was applied to the introduction of Ni metal into pores, giving Ni nanorod array on the glass surface. The removal of the barrier layer alumina at the bottom of the pores was necessary to attain smooth electro deposition of Ni. The photo catalytic function of the specimens possessing TiO2 nanotube array was investigated in the decomposition of acetaldehyde gas under the irradiation of UV light, showing that the rate of the decomposition was quite large.

  16. Lead migration from toys by anodic stripping voltammetry using a bismuth film electrode.

    Science.gov (United States)

    Leal, M Fernanda C; Catarino, Rita I L; Pimenta, Adriana M; Souto, M Renata S; Afonso, Christelle S; Fernandes, Ana F Q

    2016-09-02

    Metals may be released from toys via saliva during mouthing, via sweat during dermal contact, or via gastric and intestinal fluids after partial or whole ingestion. In this study, we determined the lead migration from toys bought on the Portuguese market for children below 3 years of age. The lead migration was performed according to the European Committee for Standardization EN 71-3, which proposes a 2-hour migration test that simulates human gastric conditions. The voltammetric determination of migrated lead was performed by anodic stripping voltammetry (ASV) at a bismuth film electrode (BiFE). For all the analyzed toys, the values of migrated lead did not exceed the limits imposed by the European Committee for Standardization EN 71-3 (90 mg kg -1 ) and by the EU Directive 2009/48/EC (13.5 mg kg -1 ) on the safety of toys.

  17. Electrostatic spray deposition of porous SnO₂/graphene anode films and their enhanced lithium-storage properties.

    Science.gov (United States)

    Jiang, Yinzhu; Yuan, Tianzhi; Sun, Wenping; Yan, Mi

    2012-11-01

    Porous SnO₂/graphene composite thin films are prepared as anodes for lithium ion batteries by the electrostatic spray deposition technique. Reticular-structured SnO₂ is formed on both the nickel foam substrate and the surface of graphene sheets according to the scanning electron microscopy (SEM) results. Such an assembly mode of graphene and SnO₂ is highly beneficial to the electrochemical performance improvement by increasing the electrical conductivity and releasing the volume change of the anode. The novel engineered anode possesses 2134.3 mA h g⁻¹ of initial discharge capacity and good capacity retention of 551.0 mA h g⁻¹ up to the 100th cycle at a current density of 200 mA g⁻¹. This anode also exhibits excellent rate capability, with a reversible capacity of 507.7 mA h g⁻¹ after 100 cycles at a current density of 800 mA g⁻¹. The results demonstrate that such a film-type hybrid anode shows great potential for application in high-energy lithium-ion batteries.

  18. Phase transition and thermal expansion studies of alumina thin films prepared by reactive pulsed laser deposition.

    Science.gov (United States)

    Balakrishnan, G; Thirumurugesan, R; Mohandas, E; Sastikumar, D; Kuppusami, P; Songl, J I

    2014-10-01

    Aluminium oxide (Al2O3) thin films were deposited on Si (100) substrates at an optimized oxygen partial pressure of 3 x 10(-3) mbar at room temperature by pulsed laser deposition (PLD). The films were characterized by high temperature X-ray diffraction (HTXRD), field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). The HTXRD pattern showed the cubic y-Al2O3 phase in the temperature range 300-973 K. At temperatures ≥ 1073 K, the δ and θ-phases of Al2O3 were observed. The mean linear thermal expansion coefficient and volume thermal expansion coefficient of γ-Al2O3 was found to be 12.66 x 10(-6) K(-1) and 38.87 x 10(-6) K(-1) in the temperature range 300 K-1073 K. The field emission scanning electron microscopy revealed a smooth and structureless morphology of the films deposited on Si (100). The atomic force microscopy study indicated the increased crystallinity and surface roughness of the films after annealing at high temperature.

  19. Vortex pinning in superconducting Nb thin films deposited on nanoporous alumina templates

    DEFF Research Database (Denmark)

    Vinckx, W.; Vanacken, J.; Moshchalkov, V.V.

    2006-01-01

    We present a study of magnetization and transport properties of superconducting Nb thin films deposited on nanoporous aluminium oxide templates. Periodic oscillations in the critical temperature vs. field, matching effects in fields up to 700 mT and strongly enhanced critical currents were observed...

  20. Analysis on porous aluminum anodic oxide film formed in Re-OA-H{sub 3}PO{sub 4} solution

    Energy Technology Data Exchange (ETDEWEB)

    Wang, H. [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 1954 Huashan Road, Shanghai 200030 (China); Wang, H.W. [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 1954 Huashan Road, Shanghai 200030 (China)]. E-mail: hwwang@sjtu.edu.cn

    2006-06-10

    An anodic porous film on aluminum was prepared in a mixed electrolyte of phosphoric acid and organic acid and cerium salt. The growth, morphology and chemical composition of the film were investigated. The results indicate that the growth of porous layers in this solution undergo three stages during anodizing, as in other conventional solution, while the whole growth rate is nonlinear. This electrolyte is sensitive to anodizing temperature, which affects current density in great degree. SEM indicates the surface morphology of film is strongly dependent on temperature and current density and its cross-section has two distinct oxide layers. Al, O and P are found in the film with different distribution in the two layers with EPMA. However, Ce has been detected on the outer surface with EDAX. XPS analysis on the electron binding energy of the component elements show the chemical composition of oxide film surface are Al{sub 2}O{sub 3}, Ce(OH) and some phosphates. The formation mechanics of Ce compound is also deduced.

  1. Simultaneous Formation of Artificial SEI Film and 3D Host for Stable Metallic Sodium Anodes.

    Science.gov (United States)

    Zhang, Di; Li, Bin; Wang, Shuai; Yang, Shubin

    2017-11-22

    Metallic sodium is a promising anode for sodium-based batteries, owing to its high theoretical capacity (1165 mAh g -1 ) and low potential (-2.714 V vs standard hydrogen electrode). However, the growth of sodium dendrites and the infinite volume change of metallic sodium during sodium striping/plating result in a low Coulombic efficiency and poor cycling stability, generating a safety hazard of sodium-based batteries. Here, an efficient approach was proposed to simultaneously generate an artificial SEI film and 3D host for metallic sodium based on a conversion reaction (CR) between sodium and MoS 2 (4Na + MoS 2 = 2Na 2 S + Mo) at room temperature. In the resultant sodium-MoS 2 hybrid after the conversion reaction (Na-MoS 2 (CR)), the production Na 2 S is homogeneously dispersed on the surface of metallic sodium, which can act as an artificial SEI film, efficiently preventing the growth of sodium dendrites; the residual MoS 2 nanosheets can construct a 3D host to confine metallic sodium, accommodating largely the volume change of sodium. Consequently, the Na-MoS 2 (CR) hybrid exhibits very low overpotential of 25 mV and a very long cycle stability more than 1000 cycles. This novel strategy is promising to promote the development of metal (lithium, sodium, zinc)-based electrodes.

  2. Sandwiched Thin-Film Anode of Chemically Bonded Black Phosphorus/Graphene Hybrid for Lithium-Ion Battery.

    Science.gov (United States)

    Liu, Hanwen; Zou, Yuqin; Tao, Li; Ma, Zhaoling; Liu, Dongdong; Zhou, Peng; Liu, Hongbo; Wang, Shuangyin

    2017-09-01

    A facile vacuum filtration method is applied for the first time to construct sandwich-structure anode. Two layers of graphene stacks sandwich a composite of black phosphorus (BP), which not only protect BP from quickly degenerating but also serve as current collector instead of copper foil. The BP composite, reduced graphene oxide coated on BP via chemical bonding, is simply synthesized by solvothermal reaction at 140 °C. The sandwiched film anode used for lithium-ion battery exhibits reversible capacities of 1401 mAh g -1 during the 200th cycle at current density of 100 mA g -1 indicating superior cycle performance. Besides, this facile vacuum filtration method may also be available for other anode material with well dispersion in N-methyl pyrrolidone (NMP). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Experiments in anodic film effects during electrorefining of scrap U-10Mo fuels in support of modeling efforts

    Energy Technology Data Exchange (ETDEWEB)

    Van Kleeck, M. [School of Nuclear Engineering, Purdue University, West Lafayette, IN 47907 (United States); Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Willit, J.; Williamson, M.A. [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Fentiman, A.W. [School of Nuclear Engineering, Purdue University, West Lafayette, IN 47907 (United States)

    2013-07-01

    A monolithic uranium molybdenum alloy clad in zirconium has been proposed as a low enriched uranium (LEU) fuel option for research and test reactors, as part of the Reduced Enrichment for Research and Test Reactors program. Scrap from the fuel's manufacture will contain a significant portion of recoverable LEU. Pyroprocessing has been identified as an option to perform this recovery. A model of a pyroprocessing recovery procedure has been developed to assist in refining the LEU recovery process and designing the facility. Corrosion theory and a two mechanism transport model were implemented on a Mat-Lab platform to perform the modeling. In developing this model, improved anodic behavior prediction became necessary since a dense uranium-rich salt film was observed at the anode surface during electrorefining experiments. Experiments were conducted on uranium metal to determine the film's character and the conditions under which it forms. The electro-refiner salt used in all the experiments was eutectic LiCl/KCl containing UCl{sub 3}. The anodic film material was analyzed with ICP-OES to determine its composition. Both cyclic voltammetry and potentiodynamic scans were conducted at operating temperatures between 475 and 575 C. degrees to interrogate the electrochemical behavior of the uranium. The results show that an anodic film was produced on the uranium electrode. The film initially passivated the surface of the uranium on the working electrode. At high over potentials after a trans-passive region, the current observed was nearly equal to the current observed at the initial active level. Analytical results support the presence of K{sub 2}UCl{sub 6} at the uranium surface, within the error of the analytical method.

  4. Multifunctional substrates of thin porous alumina for cell biosensors

    KAUST Repository

    Toccafondi, Chiara; Thorat, Sanjay B.; La Rocca, Rosanna; Scarpellini, Alice; Salerno, Marco; Dante, Silvia; Das, Gobind

    2014-01-01

    We have fabricated anodic porous alumina from thin films (100/500 nm) of aluminium deposited on technological substrates of silicon/glass, and investigated the feasibility of this material as a surface for the development of analytical biosensors aiming to assess the status of living cells. To this goal, porous alumina surfaces with fixed pitch and variable pore size were analyzed for various functionalities. Gold coated (about 25 nm) alumina revealed surface enhanced Raman scattering increasing with the decrease in wall thickness, with factor up to values of approximately 104 with respect to the flat gold surface. Bare porous alumina was employed for micro-patterning and observation via fluorescence images of dye molecules, which demonstrated the surface capability for a drug-loading device. NIH-3T3 fibroblast cells were cultured in vitro and examined after 2 days since seeding, and no significant (P > 0.05) differences in their proliferation were observed on porous and non-porous materials. The effect on cell cultures of pore size in the range of 50–130 nm—with pore pitch of about 250 nm—showed no significant differences in cell viability and similar levels in all cases as on a control substrate. Future work will address combination of all above capabilities into a single device.

  5. Multifunctional substrates of thin porous alumina for cell biosensors

    KAUST Repository

    Toccafondi, Chiara

    2014-02-27

    We have fabricated anodic porous alumina from thin films (100/500 nm) of aluminium deposited on technological substrates of silicon/glass, and investigated the feasibility of this material as a surface for the development of analytical biosensors aiming to assess the status of living cells. To this goal, porous alumina surfaces with fixed pitch and variable pore size were analyzed for various functionalities. Gold coated (about 25 nm) alumina revealed surface enhanced Raman scattering increasing with the decrease in wall thickness, with factor up to values of approximately 104 with respect to the flat gold surface. Bare porous alumina was employed for micro-patterning and observation via fluorescence images of dye molecules, which demonstrated the surface capability for a drug-loading device. NIH-3T3 fibroblast cells were cultured in vitro and examined after 2 days since seeding, and no significant (P > 0.05) differences in their proliferation were observed on porous and non-porous materials. The effect on cell cultures of pore size in the range of 50–130 nm—with pore pitch of about 250 nm—showed no significant differences in cell viability and similar levels in all cases as on a control substrate. Future work will address combination of all above capabilities into a single device.

  6. Nafion/2,2'-bipyridyl-modified bismuth film electrode for anodic stripping voltammetry

    International Nuclear Information System (INIS)

    Torma, Ferenc; Kadar, Mihaly; Toth, Klara; Tatar, Eniko

    2008-01-01

    This paper describes the fabrication, characterisation and the application of a Nafion/2,2'-bipyridyl/bismuth composite film-coated glassy carbon electrode (NC(Bpy)BiFE) for the anodic stripping voltammetric determination of trace metal ions (Zn 2+ , Cd 2+ and Pb 2+ ). The NC(Bpy)BiFE electrode is prepared by first applying a 2.5 mm 3 drop of a coating solution containing 0.5 wt% Nafion and 0.1% (w/v) 2,2'-bipyridil (Bpy) onto the surface of a glassy carbon electrode, while the Bi film was plated in situ simultaneously with the target metal ions at -1.4 V. The main advantage of the polymer coated bismuth film electrode is that the sensitivity of the stripping responses is increased considerably due to the incorporation of the neutral chelating agent of 2,2'-bipyridyl (Bpy) in the Nafion film, while the Nafion coating improved the mechanical stability of the bismuth film and its resistance to the interference of surfactants. The key experimental parameters relevant to both the electrode fabrication and the voltammetric measurement were optimized on the basis of the stripping signals. With a 2 min deposition time in the presence of oxygen, linear calibration curves were obtained in a wide concentration range (about 2-0.001 μM) with detection limits of 8.6 nM (0.56 μg dm -3 ) for Zn 2+ , 1.1 nM (0.12 μg dm -3 ) for Cd 2+ and 0.37 nM (0.077 μg dm -3 ) for Pb 2+ . For nine successive preconcentration/determination/electrode renewal experiments the standard deviations were between 3 and 5% at 1.2 μM for zinc and 0.3-0.3 μM concentration level for lead and cadmium, respectively, and the method exhibited excellent selectivity in the presence of the excess of several potential interfering metal ions. The analytical utility of the stripping voltammetric method elaborated was tested in the assay of heavy metals in some real samples and the method was validated by ICP-MS technique

  7. Fabrication of amorphous Si and C anode films via co-sputtering for an all-solid-state battery

    Energy Technology Data Exchange (ETDEWEB)

    Lee, K.S. [Department of Materials Science and Engineering, Yonsei University Shinchondong, 262 Seongsanno, Seodaemoongu, Seoul 120-749 (Korea, Republic of); Department of Environment and Energy Engineering, Gachon University, Seongnamdaero 1342, 461-710 Gyeonggi-do (Korea, Republic of); Lee, S.H. [Department of Environment and Energy Engineering, Gachon University, Seongnamdaero 1342, 461-710 Gyeonggi-do (Korea, Republic of); Woo, S.P. [Department of Materials Science and Engineering, Yonsei University Shinchondong, 262 Seongsanno, Seodaemoongu, Seoul 120-749 (Korea, Republic of); Department of Environment and Energy Engineering, Gachon University, Seongnamdaero 1342, 461-710 Gyeonggi-do (Korea, Republic of); Kim, H.S. [Department of Mechanical Engineering, Gachon University, Seongnamdaero 1342, 461-710 Gyeonggi-do (Korea, Republic of); Yoon, Y.S., E-mail: benedicto@gachon.ac.kr [Department of Environment and Energy Engineering, Gachon University, Seongnamdaero 1342, 461-710 Gyeonggi-do (Korea, Republic of)

    2014-08-01

    In this study, a combination of silicon and carbon as the anode material for an all-solid-state battery has been investigated to overcome their individual deficiencies. The capacity of silicon thin films with an input power of 60 W shows dramatic failure after 38 cycles due to serious volume expansion. In contrast, C thin films at 60 W show high stability of cyclic performance and capacity retention. The amorphous silicon and carbon composite reduced the volume expansion of silicon during long term cycles and enhanced the low specific capacity of the carbon. This resistance of the volume expansion might be expected from the cushion effect caused by the carbon, which was confirmed by scanning electron microscope images after a 100 cycle test. These results indicate that amorphous silicon and carbon composite thin films have a high possibility as the stable anode material for an all-solid-state battery. - Highlights: • Amorphous Si/C nanocomposite thin films have been prepared by co-sputtering. • Carbon can act as a cushion effect to prevent volume expansion of Si. • Amorphous Si/C nanocomposite thin films show structure stability at 100 cycles. • Capacity of the amorphous Si/C nanocomposite thin films was enhanced considerably.

  8. Structural, optical and electrical properties of CeO2 thin films simultaneously prepared by anodic and cathodic electrodeposition

    Science.gov (United States)

    Yang, Yumeng; Du, Xiaoqing; Yi, Chenxi; Liu, Jiao; Zhu, Benfeng; Zhang, Zhao

    2018-05-01

    CeO2 thin films were deposited on stainless steel (SS) and indium tin oxide (ITO)-coated glass by simultaneous anodic and cathodic electrodeposition, and the influence of negative potential on the formation of ceria films was studied with scanning electron microscopy, X-ray diffraction, Raman spectroscopy, van der Pauw measurements, UV-visible spectroscopy and X-ray photoelectron spectroscopy. The results show that CeO2 films on the anode are slightly affected by the potential, but the particle size, crystal orientation, strain, film thickness, resistivity and Ce(III) content of the films on the cathode increases with increasing potential on the SS substrate. Contradictory to the results of the SS cathode, redshift (Ed changed from 3.95 eV to 3.56 eV and Ei changed from 3.42 eV to 3.04 eV) occurring in the absorption spectrum of CeO2 deposited on the ITO-coated glass cathode indicates that the content of Ce3+ in the cathodic films is dependent on the adopted substrates and decreases as the applied potential is increased.

  9. Film growth and alloy enrichment during anodizing AZ31 magnesium alloy in fluoride/glycerol electrolytes of a range of water contents

    Czech Academy of Sciences Publication Activity Database

    Němcová, A.; Galal, O.; Skeldon, P.; Kuběna, Ivo; Šmíd, Miroslav; Briand, E.; Vickridge, I.; Ganem, J.-J.; Habazaki, H.

    2016-01-01

    Roč. 219, NOV (2016), s. 28-37 ISSN 0013-4686 Institutional support: RVO:68081723 Keywords : magnesium * anodic film * enrichment Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 4.798, year: 2016

  10. Anodic polarization behavior and film breakdown potential of pure copper in the simulated geological environment containing carbonate

    International Nuclear Information System (INIS)

    Kawasaki, Manabu; Taniguchi, Naoki; Naito, Morimasa

    2009-01-01

    In order to clarify the influence of environmental factors on the corrosion behavior of copper overpacks in oxidizing environment, potentiodynamic and potentiostatic anodic polarization tests were performed in carbonate aqueous solutions at 80degC. As the results, the passivation was promoted and film breakdown was suppressed in higher carbonate concentrations, in lower chloride ion concentrations, and in higher pH conditions. The sulfate ion tended to promote the film breakdown of copper. The effects of the composition of the test solutions on the anodic polarization curve of copper in bentonite/sand mixture were quite smaller than those in simple aqueous solution. By comparison with previous data for lower temperature condition, it was clarified that passivation of copper was promoted in higher temperature condition, but breakdown potential, Eb was independent of temperature. The Eb, was expressed as a function of the ratio of aggressive ion and inhibiting ion such as [Cl - ]/[HCO 3 - ] and [SO 4 2- ]/[HCO 3 - ], and it was confirmed that the Eb was lowered with increasing the ratio. When the ratio exceeds a certain value, the Eb was no longer able to be determined since the anodic polarization curve becomes active dissolution type. The lower limit of Eb in passive type region was estimated to be about -200 mV vs. SCE. The results of potentiostatic tests showed that pitting corrosion or non-uniform corrosion was observed at the potentials over Eb or second current peak potentials in anodic polarization curve. (author)

  11. Preparation of sodium beta″-alumina electrolyte thin film by electrophoretic deposition using Taguchi experimental design approach

    International Nuclear Information System (INIS)

    Wei, Xiao-ling; Xia, Yi; Liu, Xiao-min; Yang, Hui; Shen, Xiao-dong

    2014-01-01

    Highlights: • Sodium beta″ alumina electrolyte thin film is successfully prepared via electrophoretic deposition. • The ionic conductivity of the optimized electrolyte disk is 0.138 S cm -1 . • A Daniell-typed cell is built which approves the reversible Na + conduction at only 100 °C. - Abstract: With the desire to lowering the working temperature of Na-β″-Al 2 O 3 solid electrolyte (BASE) based batteries, electrophoretic deposition process is employed to fabricate 300 μm thick Na-β″-Al 2 O 3 sheet with densification microstructure and high ionic conductivity. Taguchi design of experiment approach with signal to noise ratio analysis is utilized to optimize the operation parameters. The results show that the TiO 2 content in the precursor powders is critical to determine the ionic conductivity of the resulting electrolyte. X-Ray diffraction analysis and X-ray photoelectron spectroscopy examination point out that Ti 4+ can enter the crystal lattice of Na-β″-Al 2 O 3 , which results in the variation of lattice parameters, densifies the microstructure and improves both β″ phase content and ionic conductivity of the resulting sample. The thin Na-β″-Al 2 O 3 disk obtained under the optimized conditions Exhibit 97% β″ phase content and relatively high ionic conductivity. Moreover, a Daniell-typed cell built with this optimized sample disk, using copper/zinc redox couples as electrodes and 1 M NaBF 4 in DMSO as the secondary electrolyte, shows reversible charge and discharge behaviors at relatively low temperature, 100 °C

  12. Polyethylene oxide film coating enhances lithium cycling efficiency of an anode-free lithium-metal battery.

    Science.gov (United States)

    Assegie, Addisu Alemayehu; Cheng, Ju-Hsiang; Kuo, Li-Ming; Su, Wei-Nien; Hwang, Bing-Joe

    2018-03-29

    The practical implementation of an anode-free lithium-metal battery with promising high capacity is hampered by dendrite formation and low coulombic efficiency. Most notably, these challenges stem from non-uniform lithium plating and unstable SEI layer formation on the bare copper electrode. Herein, we revealed the homogeneous deposition of lithium and effective suppression of dendrite formation using a copper electrode coated with a polyethylene oxide (PEO) film in an electrolyte comprising 1 M LiTFSI, DME/DOL (1/1, v/v) and 2 wt% LiNO3. More importantly, the PEO film coating promoted the formation of a thin and robust SEI layer film by hosting lithium and regulating the inevitable reaction of lithium with the electrolyte. The modified electrode exhibited stable cycling of lithium with an average coulombic efficiency of ∼100% over 200 cycles and low voltage hysteresis (∼30 mV) at a current density of 0.5 mA cm-2. Moreover, we tested the anode-free battery experimentally by integrating it with an LiFePO4 cathode into a full-cell configuration (Cu@PEO/LiFePO4). The new cell demonstrated stable cycling with an average coulombic efficiency of 98.6% and capacity retention of 30% in the 200th cycle at a rate of 0.2C. These impressive enhancements in cycle life and capacity retention result from the synergy of the PEO film coating, high electrode-electrolyte interface compatibility, stable polar oligomer formation from the reduction of 1,3-dioxolane and the generation of SEI-stabilizing nitrite and nitride upon lithium nitrate reduction. Our result opens up a new route to realize anode-free batteries by modifying the copper anode with PEO to achieve ever more demanding yet safe interfacial chemistry and control of dendrite formation.

  13. Self-sealing of unsealed aluminium anodic oxide films in very different atmospheres

    Directory of Open Access Journals (Sweden)

    González, J. A.

    2003-12-01

    Full Text Available It is widely believed that the corrosion resistance behaviour of bare aluminium in natural environments is superior to that of unsealed anodised aluminium. However, results obtained in the exposure of unsealed anodised aluminium specimens with three different film thicknesses, in 9 atmospheres of Ibero-America with salinity levels between 3.9 and 517 mg.m-2.d-1 chloride, clearly shows the reverse to be true. After a sufficient time, which is shorter the higher the precipitation rate and the environmental relative humidity, a self-sealing process takes place, leading to coatings that surpass the quality standards demanded in industrial practice. Anodic films, sealed and unsealed, are protective coatings whose quality improves with ageing in most natural environments.

    Está muy difundida la idea de que el comportamiento del aluminio es superior al del aluminio anodizado y sin sellar, desde el punto de vista de la resistencia a la corrosión, en los ambientes naturales. Sin embargo, los resultados obtenidos en la exposición de anodizados sin sellar, de tres espesores diferentes, a 9 atmósferas de Iberoamérica, con salinidades comprendidas entre 3,9 y 517 mg.m-2.d-1 de cloruros, muestran, sin lugar a dudas, lo contrario. Con tiempo suficiente, tanto más rápidamente cuanto mayor sean las precipitaciones y la humedad relativa ambiental, tiene lugar un proceso de autosellado que conduce a recubrimientos que superan las normas de calidad exigidas en la práctica industrial. Los anodizados, sellados y sin sellar, son recubrimientos protectores que mejoran su calidad, en la mayoría de los ambientes naturales, con el envejecimiento.

  14. Titanium oxynitride thin films as high-capacity and high-rate anode materials for lithium-ion batteries

    International Nuclear Information System (INIS)

    Chiu, Kuo-Feng; Su, Shih-Hsuan; Leu, Hoang-Jyh; Hsia, Chen-Hsien

    2015-01-01

    Titanium oxynitride (TiO_xN_y) was synthesized by reactive magnetron sputtering in a mixed N_2/O_2/Ar gas at ambient temperature. TiO_xN_y thin films with various amounts of nitrogen contents were deposited by varying the N_2/O_2 ratios in the background gas. The synthesized TiO_xN_y films with different compositions (TiO_1_._8_3_7N_0_._0_6_0_, TiO_1_._8_9_0N_0_._0_6_8_, TiO_1_._8_6_5N_0_._0_7_3, and TiO_1_._8_8_2N_0_._1_6_3) all displayed anatase phase, except TiO_1_._8_8_2N_0_._1_6_3. The impedances and grain sizes showed obvious variations with the nitrogen contents. A wide potential window from 3.0 V to 0.05 V, high-rate charge–discharge testing, and long cycle testing were applied to investigate the performances of synthesized TiO_xN_y and pure TiO_2 as anodes for lithium-ion batteries. These TiO_xN_y anodes can be cycled under high rates of 125 μA/cm"2 (10 °C) because of the lower charge–transfer resistance compared with the TiO_2 anode. At 10 °C the discharge capacity of the optimal TiO_xN_y composition is 1.5 times higher than that of pure TiO_2. An unexpectedly large reversible capacity of ~ 300 μAh/cm"2 μm (~ 800 mAh/g) between 1.0 V and 0.05 V was recorded for the TiO_xN_y anodes. The TiO_xN_y anode was cycled (3.0 V to 0.05 V) at 10 °C over 300 times without capacity fading while delivering a capacity of ~ 150 μAh/cm"2 μm (~ 400 mAh/g). - Highlights: • Titanium oxynitride (TiO_xN_y) thin films as anode materials were studied. • TiO_xN_y thin films with various amounts of nitrogen contents were studied_. • High rate capability of TiO_xN_y was studied.

  15. Study of the phase composition of nanostructures produced by the local anodic oxidation of titanium films

    International Nuclear Information System (INIS)

    Avilov, V. I.; Ageev, O. A.; Konoplev, B. G.; Smirnov, V. A.; Solodovnik, M. S.; Tsukanova, O. G.

    2016-01-01

    The results of experimental studies of the phase composition of oxide nanostructures formed by the local anodic oxidation of a titanium thin film are reported. The data of the phase analysis of titanium-oxide nanostructures are obtained by X-ray photoelectron spectroscopy in the ion profiling mode of measurements. It is established that the surface of titanium-oxide nanostructures 4.5 ± 0.2 nm in height possesses a binding energy of core levels characteristic of TiO_2 (458.4 eV). By analyzing the titanium-oxide nanostructures in depth by X-ray photoelectron spectroscopy, the formation of phases with binding energies of core levels characteristic of Ti_2O_3 (456.6 eV) and TiO (454.8 eV) is established. The results can be used in developing the technological processes of the formation of a future electronic-component base for nanoelectronics on the basis of titanium-oxide nanostructures and probe nanotechnologies.

  16. Effects of substrate heating and vacuum annealing on optical and electrical properties of alumina-doped ZnO films deposited by DC magnetron sputtering

    Science.gov (United States)

    Tang, Chien-Jen; Wang, Chun-Yuan; Jaing, Cheng-Chung

    2011-10-01

    Alumina-doped zinc oxide (AZO) films have wide range of applications in optical and optoelectronic devices. AZO films have advantage in high transparency, high stability to hydrogen plasma and low cost to alternative ITO film. AZO film was prepared by direct-current (DC) magnetron sputtering from ceramic ZnO:Al2O3 target. The AZO films were compared in two different conditions. The first is substrate heating process, in which AZO film was deposited by different substrate temperature, room temperature, 150 °C and 250 °C. The second is vacuum annealing process, in which AZO film with deposited at room temperature have been annealed at 250 °C and 450 °C in vacuum. The optical properties, electrical properties, grain size and surface structure properties of the films were studied by UV-VIS-NIR spectrophotometer, Hall effect measurement equipment, x-ray diffraction, and scanning electron microscopy. The resistivity, carrier mobility, carrier concentration, and grain size of AZO films were 1.92×10-3 Ω-cm, 6.38 cm2/Vs, 5.08×1020 #/cm3, and 31.48 nm respectively, in vacuum annealing of 450 °C. The resistivity, carrier mobility, carrier concentration, and grain size of AZO films were 8.72×10-4 Ω-cm, 6.32 cm2/Vs, 1.13×1021 #/cm3, and 31.56 nm, respectively, when substrate temperature was at 250 °C. Substrate heating process is better than vacuum annealed process for AZO film deposited by DC Magnetron Sputtering.

  17. Study of passive films formed on mild steel in alkaline media by the application of anodic potentials

    Energy Technology Data Exchange (ETDEWEB)

    Freire, L. [Universidade de Vigo, E.T.S.E.I., Campus Universitario, 36310 Vigo (Spain)], E-mail: lorenafp@uvigo.es; Novoa, X.R. [Universidade de Vigo, E.T.S.E.I., Campus Universitario, 36310 Vigo (Spain); Montemor, M.F. [ICEMS - Instituto Superior Tecnico, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049 - 001 Lisboa (Portugal); Carmezim, M.J. [ICEMS - Instituto Superior Tecnico, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049 - 001 Lisboa (Portugal); EST Setubal, DEM, Instituto Politecnico de Setubal, Campus IPS, 2910 Setubal (Portugal)

    2009-04-15

    In this paper, iron oxide thin layers formed on mild steel substrates in alkaline media by the application of different anodic potentials were studied in order to characterize their morphology, composition and electrochemical behaviour, in particular under conditions of cathodic protection. The surface composition was evaluated by X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). The morphology of the surface oxides was studied via Atomic Force Microscopy (AFM). The electrochemical behaviour of the surface oxides was studied using Electrochemical Impedance Spectroscopy (EIS). The results showed that the surface film is composed by Fe{sup 2+}oxides and Fe{sup 3+} oxides and/or hydroxides. The contribution of Fe{sup 2+} species vanishes when the potential of film formation increases in the passive domain. Two distinct phases were differentiated in the outer layers of the surface film, which proves that film growing is topotactic in nature.

  18. Study of passive films formed on mild steel in alkaline media by the application of anodic potentials

    International Nuclear Information System (INIS)

    Freire, L.; Novoa, X.R.; Montemor, M.F.; Carmezim, M.J.

    2009-01-01

    In this paper, iron oxide thin layers formed on mild steel substrates in alkaline media by the application of different anodic potentials were studied in order to characterize their morphology, composition and electrochemical behaviour, in particular under conditions of cathodic protection. The surface composition was evaluated by X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). The morphology of the surface oxides was studied via Atomic Force Microscopy (AFM). The electrochemical behaviour of the surface oxides was studied using Electrochemical Impedance Spectroscopy (EIS). The results showed that the surface film is composed by Fe 2+ oxides and Fe 3+ oxides and/or hydroxides. The contribution of Fe 2+ species vanishes when the potential of film formation increases in the passive domain. Two distinct phases were differentiated in the outer layers of the surface film, which proves that film growing is topotactic in nature

  19. Study on the influences of reduction temperature on nickel-yttria-stabilized zirconia solid oxide fuel cell anode using nickel oxide-film electrode

    Science.gov (United States)

    Jiao, Zhenjun; Ueno, Ai; Suzuki, Yuji; Shikazono, Naoki

    2016-10-01

    In this study, the reduction processes of nickel oxide at different temperatures were investigated using nickel-film anode to study the influences of reduction temperature on the initial performances and stability of nickel-yttria-stabilized zirconia anode. Compared to conventional nickel-yttria-stabilized zirconia composite cermet anode, nickel-film anode has the advantage of direct observation at nickel-yttria-stabilized zirconia interface. The microstructural changes were characterized by scanning electron microscopy. The reduction process of nickel oxide is considered to be determined by the competition between the mechanisms of volume reduction in nickel oxide-nickel reaction and nickel sintering. Electrochemical impedance spectroscopy was applied to analyze the time variation of the nickel-film anode electrochemical characteristics. The anode performances and microstructural changes before and after 100 hours discharging and open circuit operations were analyzed. The degradation of nickel-film anode is considered to be determined by the co-effect between the nickel sintering and the change of nickel-yttria-stabilized zirconia interface bonding condition.

  20. Structure, Morphology and Optical Properties of TiO2 Films Formed by Anodizing in a Mixed Solution of Citric Acid and Sulfamic Acid

    Science.gov (United States)

    Choudhary, R. K.; Sarkar, P.; Biswas, A.; Mishra, P.; Abraham, G. J.; Sastry, P. U.; Kain, V.

    2017-08-01

    TiO2 films of 50-180 nm thickness were formed at room temperature by anodization of titanium metal in a mixture of citric acid and sulfamic acid in the potential range of 5-30 V. The films so obtained were characterized for their crystal structure, surface morphology, chemical composition and optical properties. Grazing incidence x-ray diffraction and micro-laser Raman spectroscopy measurements of the anodic films confirmed the formation of brookite phase of TiO2 at anodizing potentials of 15, 20, 25 and 30 V and amorphous structure at 5 and 10 V. Field emission scanning electron microscopy revealed non-porous microstructure of the films. Spectroscopic ellipsometry measurements evaluated the band gap of TiO2 at around 3.3 eV, whereas the refractive index of the films was found to be in the range of 2-2.35, in the visible range of spectrum.

  1. Fabrication of Meso-Porous Gamma-Alumina Films by Sol-Gel and Gel Casting Processes for Making Moisture Sensors

    Directory of Open Access Journals (Sweden)

    Kalyan Kumar Mistry

    2007-04-01

    Full Text Available Meso-porous g-Al2O3 film may be used as a highly sensitive trace moisture sensor. The crack-free alumina film was developed using a combination of sol-gel and tape casting processes, which produce high porosity, high surface area and small pore dimensions in the range of few nano-meter at uniform distribution. Sol-gel processes are well known in nano-technology and nano-material preparation, but it is difficult to make crack-free thick or thin films using this method. Tape cast methods are used for the fabrication of flexible crack-free thick ceramic sheets. Our objective was to develop nano-structured, crack-free, transparent Al2O3 film a few microns thick, has a highly porous and stable crystallographic nature. A metallic paste was printed by screen printing on both side of the film surface for electrodes to form a sensitive element. A silver wire (dia j=0.1mm lead was connected to a grid structure electrode using a silver paste spot for fine joining. Alumina is absorbs moisture molecules into its meso-porous layer and changes its electrical characteristics according to the moisture content, its dielectric constant increase as moisture increase. Moisture molecules can be conceived of as dipoles in random state before the application of an electric field. When the dipole orientation was changed from random to an equilibrium state under the application of external field, a large change in dielectric constant was observed. The number of water molecules absorbed determines the electrical impedance of the capacitor, which in turn is proportional to water vapor pressure.

  2. Study of preparation and surface morphology of self-ordered nanoporous alumina; Estudo da preparacao e da morfologia de superficie de alumina nanoporosa auto-organizada

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, Elisa Marchezini; Martins, Maximiliano Delany, E-mail: elisamarch@gmail.com, E-mail: MG.mdm@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG. (Brazil); Silva, Ronald Arreguy, E-mail: arregsilva@yahoo.com.br [Centro Universitario de Belo Horizonte (UniBH), Belo Horizonte, MG (Brazil)

    2013-07-01

    Nanoporous alumina is a typical material that exhibits self-ordered nanochannels spontaneously organized in hexagonal shape. Produced by anodizing of metallic aluminum, it has been used as a template for production of materials at the nanoscale. This work aimed to study the preparation of nanoporous alumina by anodic anodizing of metallic aluminum substrates. The nanoporous alumina was prepared following the methodology proposed by Masuda and Fukuda (1995), a two-step method consisting of anodizing the aluminum sample in the potentiostatic mode, removing the layer of aluminum oxide (alumina) formed and then repeat the anodization process under the same conditions as the first anodization. This method produces nanoporous alumina with narrow pore diameter distribution and well-ordered structure. (author)

  3. Triethyl orthoformate as a new film-forming electrolytes solvent for lithium-ion batteries with graphite anodes

    International Nuclear Information System (INIS)

    Wang Lishi; Huang Yudai; Jia Dianzeng

    2006-01-01

    Triethyl orthoformate (TEOF) as a new solvent used in propylene carbonate (PC)-based electrolytes together with graphitic anodes in lithium-ion batteries has been investigated. It can be observed that TEOF was capable of suppressing the co-intercalation of PC solvated lithium-ions into the graphite layer during the first lithiation process and the irreversible discharge capacity of the first cycle is the smallest when using 1.0 M LiPF 6 in PC and TEOF at solvent ratio of 1:1 as the electrolytes. The CV, FTIR, EIS, SEM results show that the PC-based electrolytes containing the solvent TEOF can generate an effective solid electrolytes interphase (SEI) film during the first cycling process, and the film is probably mainly composed of ROCO 2 Li, ROLi, Li 2 CO 3 , etc. The formation of a stable passivating film on the graphite surface is believed to be the reason for the improved cell performance. All these results show that TEOF possesses a promising performance for use as an effective film-forming electrolytes solvent in lithium-ion batteries with graphitic anodes

  4. Capacitor Property and Leakage Current Mechanism of ZrO2 Thin Dielectric Films Prepared by Anodic Oxidation

    Science.gov (United States)

    Kamijyo, Masahiro; Onozuka, Tomotake; Shinkai, Satoko; Sasaki, Katsutaka; Yamane, Misao; Abe, Yoshio

    2003-07-01

    Polycrystalline ZrO2 thin film capacitors were prepared by anodizing sputter-deposited Zr films. Electrical measurements are performed for the parallel-plate anodized capacitors with an Al-ZrO2-Zr (metal-insulator-metal) structure, and a high capacitance density (0.6 μF/cm2) and a low dielectric loss of nearly 1% are obtained for a very thin-oxide capacitor anodized at 10 V. In addition, the leakage current density of this capacitor is about 1.8 × 10-8 A/cm2 at an applied voltage of 5 V. However, the leakage current is somewhat larger than that of a low-loss HfO2 capacitor. The leakage current density (J) of ZrO2 capacitors as a function of applied electric field (E) was investigated for several capacitors with different oxide thicknesses, by plotting \\ln(J) vs E1/2 curves. As a result, it is revealed that the conduction mechanism is due to the Poole-Frenkel effect, irrespective of the oxide thickness.

  5. Production of lithium positive ions from LiF thin films on the anode in PBFA II

    International Nuclear Information System (INIS)

    Green, T.A.; Stinnett, R.W.; Gerber, R.A.

    1995-09-01

    The production of positive lithium ions using a lithium-fluoride-coated stainless steel anode in the particle beam fusion accelerator PBFA II is considered from both the experimental and theoretical points of view. It is concluded that the mechanism of Li + ion production is electric field desorption from the tenth-micron-scale crystallites which compose the columnar growth of the LiF thin film. The required electric field is estimated to be of the order of 5 MV/cm. An essential feature of the mechanism is that the crystallites are rendered electronically conducting through electron-hole pair generation by MeV electron bombardment of the thin film during the operation of the diode. It is proposed that the ion emission mechanism is an electronic conductivity analogue to that discovered by Rollgen for lithium halide crystallites which were rendered ionically conducting by heating to several hundred degrees Celsius. Since an electric field desorption mechanism cannot operate if a surface flashover plasma has formed and reduced the anode electric field to low values, the possibility of flashover on the lithium fluoride coated anode of the PBFA II Li + ion source is studied theoretically. It is concluded with near certainty that flashover does not occur

  6. Influence of molybdate species on the tartaric acid/sulphuric acid anodic films grown on AA2024 T3 aerospace alloy

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Rubio, M. [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049 Madrid (Spain); Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906 Getafe (Spain); Ocon, P. [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049 Madrid (Spain)], E-mail: pilar.ocon@uam.es; Climent-Font, A. [Departamento de Fisica Aplicada, Universidad Autonoma de Madrid (UAM), 28049 Madrid (Spain); Centro de Micro-Analisis de Materiales (CMAM), Universidad Autonoma de Madrid (UAM), 28049 Madrid (Spain); Smith, R.W. [Unidad de Microanalisis de Materiales, Parque Cientifico de Madrid (PCM), Campus de Cantoblanco, 28049 Madrid (Spain); Curioni, M.; Thompson, G.E.; Skeldon, P. [Corrosion and Protection Centre, School of Materials, University of Manchester, M60 1QD England (United Kingdom); Lavia, A.; Garcia, I. [Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906 Getafe (Spain)

    2009-09-15

    AA2024 T3 alloy specimens have been anodised in tartaric acid/sulphuric media and tartaric acid/sulphuric media containing sodium molybdate; molybdate species were added to the anodising bath to enhance further the protection provided by the porous anodic film developed over the macroscopic alloy surface. Morphological characterisation of the anodic films formed in both electrolytes was undertaken using scanning electron and transmission electron microscopies; the chemical compositions of the films were determined by Rutherford backscattering spectroscopy that was complemented by elemental depth profiling using rf-glow discharge optical emission spectrometry. The electrochemical behaviour was evaluated using potentiodynamic polarisations and electrochemical impedance spectroscopy; the corrosion performance was examined after salt spray testing. The porous anodic film morphology was little influenced by the addition of molybdate salt, although thinner films were generated in its presence. Chemical composition of the anodic film was roughly similar; however, addition of sodium molybdate in the anodizing bath resulted in residues of molybdate species in the porous skeleton and improved corrosion resistance measured by electrochemical techniques that was confirmed by salt spray testing.

  7. Influence of molybdate species on the tartaric acid/sulphuric acid anodic films grown on AA2024 T3 aerospace alloy

    International Nuclear Information System (INIS)

    Garcia-Rubio, M.; Ocon, P.; Climent-Font, A.; Smith, R.W.; Curioni, M.; Thompson, G.E.; Skeldon, P.; Lavia, A.; Garcia, I.

    2009-01-01

    AA2024 T3 alloy specimens have been anodised in tartaric acid/sulphuric media and tartaric acid/sulphuric media containing sodium molybdate; molybdate species were added to the anodising bath to enhance further the protection provided by the porous anodic film developed over the macroscopic alloy surface. Morphological characterisation of the anodic films formed in both electrolytes was undertaken using scanning electron and transmission electron microscopies; the chemical compositions of the films were determined by Rutherford backscattering spectroscopy that was complemented by elemental depth profiling using rf-glow discharge optical emission spectrometry. The electrochemical behaviour was evaluated using potentiodynamic polarisations and electrochemical impedance spectroscopy; the corrosion performance was examined after salt spray testing. The porous anodic film morphology was little influenced by the addition of molybdate salt, although thinner films were generated in its presence. Chemical composition of the anodic film was roughly similar; however, addition of sodium molybdate in the anodizing bath resulted in residues of molybdate species in the porous skeleton and improved corrosion resistance measured by electrochemical techniques that was confirmed by salt spray testing.

  8. Characterization of anodic SiO2 films on P-type 4H-SiC

    International Nuclear Information System (INIS)

    Woon, W.S.; Hutagalung, S.D.; Cheong, K.Y.

    2009-01-01

    The physical and electronic properties of 100-120-nm thick anodic silicon dioxide film grown on p-type 4H-SiC wafer and annealed at different temperatures (500, 600, 700, and 800 deg. C ) have been investigated and reported. Chemical bonding of the films has been analyzed by Fourier transform infra red spectroscopy. Smooth and defect-free film surface has been revealed under field emission scanning electron microscope. Atomic force microscope has been used to study topography and surface roughness of the films. Electronic properties of the film have been investigated by high frequency capacitance-voltage and current-voltage measurements. As the annealing temperature increased, refractive index, dielectric constant, film density, SiC surface roughness, effective oxide charge, and leakage current density have been reduced until 700 deg. C . An increment of these parameters has been observed after this temperature. However, a reversed trend has been demonstrated in porosity of the film and barrier height between conduction band edge of SiO 2 and SiC

  9. Enhanced Absorption in Organic Thin-Films from Imprinted Concave Nanostructures

    DEFF Research Database (Denmark)

    Goszczak, Arkadiusz Jaroslaw; Rubahn, Horst-Günter; Madsen, Morten

    2017-01-01

    In this work, a rapid, replicable method for imprinting concave nanostructures to be used as functional light-trapping nanostructures in organic thin-films is presented. Porous anodic alumina templates were fabricated both by anodization of thick Al foils and by anodization of submicrometer thin Al...... patterns and used for imprinting of spin coated photoresist on glass substrates. We have investigated semi-periodic and aperiodic imprinted large concave patterns fabricated from rigid masters after anodization of Al in H3PO4. We show that metal covered imprinted concaves show enhancement in absorption...

  10. Ultrafiltro de alumina Alumina ultrafilter

    Directory of Open Access Journals (Sweden)

    M. F. de Souza

    1999-06-01

    Full Text Available Membranas de alumina AKP-50 foram preparadas sobre um substrato de alumina APC-SG de alta resistência mecânica. As membranas foram sinterizadas a 1000 °C e possuem uma distribuição estreita de poros de 40 a 90 nm, espessura média de 57 mm e taxa de fluxo de 0,4 m3/m2h. O filtro assim obtido é classificado como ultrafiltro sendo capaz de reter bactérias e alguns vírus. São quimicamente inertes e resistem a temperaturas inferiores a 1000 °C. A aderência entre as camadas permite a limpeza por contra-fluxo.Alumina ceramic membranes with unimodal pore size distribution in the 40 to 90 nm range were prepared on alumina porous substrates. The 57mm thickness membrane made from AKP-50 alumina shows 0,4 m3/m2h flow rate. The two layer substrate, prepared to have high mechanical strength, was made from commercially available APC-SG alumina. The filter made of three layers, membrane, intermediate layer and substrate, is classified as ultra-filter being able to retain bacteria and some viruses. Adherence between the three layers allows reverse washing. Filters are chemically inert and resistant to temperatures below 1000oC.

  11. Alumina-coated and manganese monoxide embedded 3D carbon derived from avocado as high-performance anode for lithium-ion batteries

    Science.gov (United States)

    rehman, Wasif ur; Xu, Youlong; Du, Xianfeng; Sun, Xiaofei; Ullah, Inam; Zhang, Yuan; Jin, Yanling; Zhang, Baofeng; Li, Xifei

    2018-07-01

    Derived from avocado fruit, a three dimension (3D) carbon is prepared via a hydrothermal/pyrolysis process followed by embedding with MnO nanoparticles by a wet chemical method and coating with Al2O3 through an atomic layer deposition technique. The obtained material presents a hierarchical structure that MnO nanocrystals wrapped in 3D carbon and then encapsulated in a uniform Al2O3 layer with a thickness of about 5 nm. Benefiting from this hierarchical structure in which 3D carbon offers numerous electronic pathways to enhance the conductivity and Al2O3 nanolayer provide a shelter to keep away from dissolution of Mn4+ and volume changes during charge/discharge process. This material (marked as C/MnO@Al2O3) has exhibited high rate performance and excellent cyclability as an anode for lithium ion batteries. A high specific capacity of about 600 mA h g-1 is achieved at a current density of 1000 mA g-1 and the electrode can still deliver a high specific capacity of about 1165 mA h g-1 at 150 mA g-1 after 100 cycles. These results facilitate a green and high potential of anode materials towards promising devices for advance performance of lithium-ion batteries.

  12. In situ fabrication of electrochemically grown mesoporous metallic thin films by anodic dissolution in deep eutectic solvents.

    Science.gov (United States)

    Renjith, Anu; Roy, Arun; Lakshminarayanan, V

    2014-07-15

    We describe here a simple electrodeposition process of forming thin films of noble metallic nanoparticles such as Au, Ag and Pd in deep eutectic solvents (DES). The method consists of anodic dissolution of the corresponding metal in DES followed by the deposition on the cathodic surface. The anodic dissolution process in DES overcomes the problems associated with copious hydrogen and oxygen evolution on the electrode surface when carried out in aqueous medium. The proposed method utilizes the inherent abilities of DES to act as a reducing medium while simultaneously stabilizing the nanoparticles that are formed. The mesoporous metal films were characterized by SEM, XRD and electrochemical techniques. Potential applications of these substrates in surface enhanced Raman spectroscopy and electrocatalysis have been investigated. A large enhancement of Raman signal of analyte was achieved on the mesoporous silver substrate after removing all the stabilizer molecules from the surface by calcination. The highly porous texture of the electrodeposited film provides superior electro catalytic performance for hydrogen evolution reaction (HER). The mechanisms of HER on the fabricated substrates were studied by Tafel analysis and electrochemical impedance spectroscopy (EIS). Copyright © 2014 Elsevier Inc. All rights reserved.

  13. Influence of desiccation procedures on the surface wettability and corrosion resistance of porous aluminium anodic oxide films

    Energy Technology Data Exchange (ETDEWEB)

    Zheng Meng, E-mail: ZhengMeng@eng.hokudai.ac.jp [Graduate School of Engineering, Hokkaido University, Kita-13, Nishi-8, Kita-Ku, Sapporo 060-8628 (Japan); Sakairi, Masatoshi [Faculty of Engineering, Hokkaido University, Kita-13, Nishi-8, Kita-Ku, Sapporo 060-8628 (Japan); Jha, Himendra [Technische Universitaet Muenchen, Lichtenbergstrasse 4, D-85748 Garching (Germany)

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer Simple desiccation treatment without coating or etching produces hydrophobicity of porous anodic oxide film. Black-Right-Pointing-Pointer Treatment time can be shortened by controlling desiccation condition. Black-Right-Pointing-Pointer Surface microstructure is the key point to determine the wettability. Black-Right-Pointing-Pointer The hydrophobic surfaces show better corrosion resistance than oxide aluminium. - Abstract: A hydrophobic oxide film was formed on aluminium by anodizing followed by desiccation treatment. Films subjected to gradual heating and cooling exhibit larger water contact angles than samples exposed to fast heating and cooling at the same temperature. From SEM and Auger Electron Spectroscopic observations, the low wettability surface shows a regular porous morphology with no significant chemical composition differences due to the different treatments. The desiccation process improves the corrosion resistance, shown by immersion in NaCl. The change in morphology by the desiccation processes is considered a main reason to lower the wettability, which further affects the corrosion properties.

  14. Study of preparation and surface morphology of self-ordered nanoporous alumina

    International Nuclear Information System (INIS)

    Rodrigues, Elisa Marchezini; Martins, Maximiliano Delany; Silva, Ronald Arreguy

    2013-01-01

    Nanoporous alumina is a typical material that exhibits self-ordered nanochannels spontaneously organized in hexagonal shape. Produced by anodizing of metallic aluminum, it has been used as a template for production of materials at the nanoscale. This work aimed to study the preparation of nanoporous alumina by anodic anodizing of metallic aluminum substrates. The nanoporous alumina was prepared following the methodology proposed by Masuda and Fukuda (1995), a two-step method consisting of anodizing the aluminum sample in the potentiostatic mode, removing the layer of aluminum oxide (alumina) formed and then repeat the anodization process under the same conditions as the first anodization. This method produces nanoporous alumina with narrow pore diameter distribution and well-ordered structure. (author)

  15. Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy

    Directory of Open Access Journals (Sweden)

    Sonia C. Ferreira

    2014-12-01

    Full Text Available Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiCnp produced by powder metallurgy (PM were anodized under voltage control in tartaric-sulfuric acid (TSA. In this work, the influence of the amount of SiCnp on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050 anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiCnp. The current peaks and the steady-state current density recorded at each voltage step increases with the SiCnp volume fraction due to the oxidation of the SiCnp. The formation mechanism of the anodic film on Al/SiCnp composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiCnp in the anodic film.

  16. Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy

    Science.gov (United States)

    Ferreira, Sonia C.; Conde, Ana; Arenas, María A.; Rocha, Luis A.; Velhinho, Alexandre

    2014-01-01

    Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiCnp) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiCnp on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiCnp. The current peaks and the steady-state current density recorded at each voltage step increases with the SiCnp volume fraction due to the oxidation of the SiCnp. The formation mechanism of the anodic film on Al/SiCnp composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiCnp in the anodic film. PMID:28788295

  17. Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy.

    Science.gov (United States)

    Ferreira, Sonia C; Conde, Ana; Arenas, María A; Rocha, Luis A; Velhinho, Alexandre

    2014-12-19

    Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiC np ) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiC np on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiC np . The current peaks and the steady-state current density recorded at each voltage step increases with the SiC np volume fraction due to the oxidation of the SiC np . The formation mechanism of the anodic film on Al/SiC np composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiC np in the anodic film.

  18. Band gap structure modification of amorphous anodic Al oxide film by Ti-alloying

    DEFF Research Database (Denmark)

    Canulescu, Stela; Rechendorff, K.; Borca, C. N.

    2014-01-01

    The band structure of pure and Ti-alloyed anodic aluminum oxide has been examined as a function of Ti concentration varying from 2 to 20 at. %. The band gap energy of Ti-alloyed anodic Al oxide decreases with increasing Ti concentration. X-ray absorption spectroscopy reveals that Ti atoms...... are not located in a TiO2 unit in the oxide layer, but rather in a mixed Ti-Al oxide layer. The optical band gap energy of the anodic oxide layers was determined by vacuum ultraviolet spectroscopy in the energy range from 4.1 to 9.2 eV (300–135 nm). The results indicate that amorphous anodic Al2O3 has a direct...

  19. Preparation of mesoporous titanium dioxide anode by a film- and pore-forming agent for the dye-sensitized solar cell

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Wenjing; Xiao, Yaoming, E-mail: ymxiao@sxu.edu.cn; Han, Gaoyi, E-mail: han_gaoyis@sxu.edu.cn; Zhou, Haihan; Chang, Yunzhen; Zhang, Ying

    2016-04-15

    Highlights: • PVP is used as a film- and pore-forming agent to prepare the mesoporous TiO{sub 2} anode. • The TiO{sub 2} anode supplies high surface area for the dye adsorption. • The DSSC efficiency is strongly dependent on the pore properties of the TiO{sub 2} anode. • The DSSC efficiency with the TiO{sub 2} anode prepared by 20 wt% PVP reaches 8.39%. - Abstract: A novel mean of generating mesoporous titanium dioxide (TiO{sub 2}) anodes by employing polyvinylpyrrolidone (PVP) as the film- and pore-forming agent are proposed for dye-sensitized solar cells (DSSCs). The influences on the morphology and photovoltaic performances of the TiO{sub 2} anodes are investigated by adjusting the PVP content in synthesizing the mesoporous TiO{sub 2} anodes. The photovoltaic conversion efficiency of the DSSC is found to be strongly dependent on the pore properties of the TiO{sub 2} anode. After the sintering process, the removal of the PVP leaves porously interconnected channel structures inside the TiO{sub 2} anode, supplying enhanced specific surface area for the dye adsorption as well as the efficient electron transmission. As a result, the TiO{sub 2} anode prepared by 20 wt% PVP presents the highest performances, based on which the DSSC achieves the highest conversion efficiency of 8.39%, approximately increased by 56.53% than that of the DSSC fabricated without PVP (5.36%).

  20. Photocatalytic Activity of Nanotubular TiO2 Films Obtained by Anodic Oxidation: A Comparison in Gas and Liquid Phase

    Directory of Open Access Journals (Sweden)

    Beatriz Eugenia Sanabria Arenas

    2018-03-01

    Full Text Available The availability of immobilized nanostructured photocatalysts is of great importance in the purification of both polluted air and liquids (e.g., industrial wastewaters. Metal-supported titanium dioxide films with nanotubular morphology and good photocatalytic efficiency in both environments can be produced by anodic oxidation, which avoids release of nanoscale materials in the environment. Here we evaluate the effect of different anodizing procedures on the photocatalytic activity of TiO2 nanostructures in gas and liquid phases, in order to identify the most efficient and robust technique for the production of TiO2 layers with different morphologies and high photocatalytic activity in both phases. Rhodamine B and toluene were used as model pollutants in the two media, respectively. It was found that the role of the anodizing electrolyte is particularly crucial, as it provides substantial differences in the oxide specific surface area: nanotubular structures show remarkably different activities, especially in gas phase degradation reactions, and within nanotubular structures, those produced by organic electrolytes lead to better photocatalytic activity in both conditions tested.

  1. Role of aluminum doping on phase transformations in nanoporous titania anodic oxides

    Energy Technology Data Exchange (ETDEWEB)

    Bayata, Fatma [Istanbul Bilgi University, Department of Mechanical Engineering, 34060, Eyup, Istanbul (Turkey); Ürgen, Mustafa, E-mail: urgen@itu.edu.tr [Istanbul Technical University, Department of Metallurgical and Materials Engineering, 34469, Maslak, Istanbul (Turkey)

    2015-10-15

    The role of aluminium doping on anatase to rutile phase transformation of nanoporous titanium oxide films were investigated. For this purpose pure and aluminum doped metal films were deposited on alumina substrates by cathodic arc physical deposition. The nanoporous anodic oxides were prepared by porous anodizing of pure and aluminum doped titanium metallic films in an ethylene glycol + NH{sub 4}F based electrolyte. Nanoporous amorphous structures with 60–80 nm diameter and 2–4 μm length were formed on the surfaces of alumina substrates. The amorphous undoped and Al-doped TiO{sub 2} anodic oxides were heat-treated at different temperatures in the range of 280–720 °C for the investigation of their crystallization behavior. The combined effects of nanoporous structure and Al doping on crystallization behavior of titania were investigated using X-ray diffraction (XRD) and micro Raman analysis. The results indicated that both Al ions incorporated into the TiO{sub 2} structure and the nanoporous structure retarded the rutile formation. It was also revealed that presence or absence of metallic film underneath the nanopores has a major contribution to anatase-rutile transformation. - Highlights: • Al-doped TiO{sub 2} nanopores were grown on alumina substrates using anodization method. • The crystallization behavior of nanoporous Al-doped TiO{sub 2} were investigated. • Al doping into nanoporous TiO{sub 2} retarded the anatase-rutile transformation. • Nanostructuring has significant role in controlling rutile formation temperature. • The absence of the metallic film under the nanopores delayed the rutile formation.

  2. Cycling behaviour of sponge-like nanostructured ZnO as thin-film Li-ion battery anodes

    International Nuclear Information System (INIS)

    Garino, Nadia; Lamberti, Andrea; Gazia, Rossana; Chiodoni, Angelica; Gerbaldi, Claudio

    2014-01-01

    Highlights: • Zn is thermally oxidized in ambient air to obtain sponge-like ZnO film. • Polycrystalline, transparent, porous thin film is obtained. • Film exhibits stabile specific capacity (∼300 mAh g −1 ) after prolonged cycling. • Sponge-like ZnO film shows promising prospects as Li-ion battery anode. - Abstract: Single phase wurtzitic porous ZnO thin films are obtained by a simple two-step method, involving the sputtering deposition of a sponge-like metallic Zn layer, followed by a moderately low temperature treatment for the complete zinc oxidation. Thanks to its 3D nanostructuration, the superimposition of small branches able to grow in length almost isotropically and forming a complex topography, sponge-like ZnO can combine the fast transport properties of one dimensional material and the high surface area usually provided by nanocrystalline electrodes. When galvanostatically tested in lithium cell, after the initial decay, it can provide an almost stable specific capacity higher than 50 μAh cm −2 after prolonged cycling at estimated 0.7 C, with very high Coulombic efficiency

  3. Cycling behaviour of sponge-like nanostructured ZnO as thin-film Li-ion battery anodes

    Energy Technology Data Exchange (ETDEWEB)

    Garino, Nadia, E-mail: nadia.garino@iit.it [Center for Space Human Robotics @Polito, Istituto Italiano di Tecnologia, Corso Trento, 21, 10129 Turin (Italy); Lamberti, Andrea; Gazia, Rossana; Chiodoni, Angelica [Center for Space Human Robotics @Polito, Istituto Italiano di Tecnologia, Corso Trento, 21, 10129 Turin (Italy); Gerbaldi, Claudio, E-mail: claudio.gerbaldi@polito.it [Center for Space Human Robotics @Polito, Istituto Italiano di Tecnologia, Corso Trento, 21, 10129 Turin (Italy); GAME Lab, Department of Applied Science and Technology – DISAT, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Turin (Italy)

    2014-12-05

    Highlights: • Zn is thermally oxidized in ambient air to obtain sponge-like ZnO film. • Polycrystalline, transparent, porous thin film is obtained. • Film exhibits stabile specific capacity (∼300 mAh g{sup −1}) after prolonged cycling. • Sponge-like ZnO film shows promising prospects as Li-ion battery anode. - Abstract: Single phase wurtzitic porous ZnO thin films are obtained by a simple two-step method, involving the sputtering deposition of a sponge-like metallic Zn layer, followed by a moderately low temperature treatment for the complete zinc oxidation. Thanks to its 3D nanostructuration, the superimposition of small branches able to grow in length almost isotropically and forming a complex topography, sponge-like ZnO can combine the fast transport properties of one dimensional material and the high surface area usually provided by nanocrystalline electrodes. When galvanostatically tested in lithium cell, after the initial decay, it can provide an almost stable specific capacity higher than 50 μAh cm{sup −2} after prolonged cycling at estimated 0.7 C, with very high Coulombic efficiency.

  4. Highly transparent and conductive double-layer oxide thin films as anodes for organic light-emitting diodes

    International Nuclear Information System (INIS)

    Yang Yu; Wang Lian; Yan He; Jin Shu; Marks, Tobin J.; Li Shuyou

    2006-01-01

    Double-layer transparent conducting oxide thin film structures containing In-doped CdO (CIO) and Sn-doped In 2 O 3 (ITO) layers were grown on glass by metal-organic chemical vapor deposition and ion-assisted deposition (IAD), respectively, and used as anodes for polymer light-emitting diodes (PLEDs). These films have a very low overall In content of 16 at. %. For 180-nm-thick CIO/ITO films, the sheet resistance is 5.6 Ω/□, and the average optical transmittance is 87.1% in the 400-700 nm region. The overall figure of merit (Φ=T 10 /R sheet ) of the double-layer CIO/ITO films is significantly greater than that of single-layer CIO, IAD-ITO, and commercial ITO films. CIO/ITO-based PLEDs exhibit comparable or superior device performance versus ITO-based control devices. CIO/ITO materials have a much lower sheet resistance than ITO, rendering them promising low In content electrode materials for large-area optoelectronic devices

  5. Titanium oxynitride thin films as high-capacity and high-rate anode materials for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Chiu, Kuo-Feng [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Su, Shih-Hsuan, E-mail: minimono42@gmail.com [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Leu, Hoang-Jyh [Master' s Program of Green Energy Science and Technology, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China); Hsia, Chen-Hsien [Department of Materials Science and Engineering, Feng Chia University, 100 Wenhwa Rd., Taichung 40724, Taiwan (China)

    2015-12-01

    Titanium oxynitride (TiO{sub x}N{sub y}) was synthesized by reactive magnetron sputtering in a mixed N{sub 2}/O{sub 2}/Ar gas at ambient temperature. TiO{sub x}N{sub y} thin films with various amounts of nitrogen contents were deposited by varying the N{sub 2}/O{sub 2} ratios in the background gas. The synthesized TiO{sub x}N{sub y} films with different compositions (TiO{sub 1.837}N{sub 0.060,} TiO{sub 1.890}N{sub 0.068,} TiO{sub 1.865}N{sub 0.073}, and TiO{sub 1.882}N{sub 0.163}) all displayed anatase phase, except TiO{sub 1.882}N{sub 0.163}. The impedances and grain sizes showed obvious variations with the nitrogen contents. A wide potential window from 3.0 V to 0.05 V, high-rate charge–discharge testing, and long cycle testing were applied to investigate the performances of synthesized TiO{sub x}N{sub y} and pure TiO{sub 2} as anodes for lithium-ion batteries. These TiO{sub x}N{sub y} anodes can be cycled under high rates of 125 μA/cm{sup 2} (10 °C) because of the lower charge–transfer resistance compared with the TiO{sub 2} anode. At 10 °C the discharge capacity of the optimal TiO{sub x}N{sub y} composition is 1.5 times higher than that of pure TiO{sub 2}. An unexpectedly large reversible capacity of ~ 300 μAh/cm{sup 2} μm (~ 800 mAh/g) between 1.0 V and 0.05 V was recorded for the TiO{sub x}N{sub y} anodes. The TiO{sub x}N{sub y} anode was cycled (3.0 V to 0.05 V) at 10 °C over 300 times without capacity fading while delivering a capacity of ~ 150 μAh/cm{sup 2} μm (~ 400 mAh/g). - Highlights: • Titanium oxynitride (TiO{sub x}N{sub y}) thin films as anode materials were studied. • TiO{sub x}N{sub y} thin films with various amounts of nitrogen contents were studied{sub .} • High rate capability of TiO{sub x}N{sub y} was studied.

  6. Sequential Vapor Infiltration Treatment Enhances the Ionic Current Rectification Performance of Composite Membranes Based on Mesoporous Silica Confined in Anodic Alumina.

    Science.gov (United States)

    Liang, Yanyan; Liu, Zhengping

    2016-12-20

    Ionic current rectification of nanofluidic diode membranes has been studied widely in recent years because it is analogous to the functionality of biological ion channels in principle. We report a new method to fabricate ionic current rectification membranes based on mesoporous silica confined in anodic aluminum oxide (AAO) membranes. Two types of mesostructured silica nanocomposites, hexagonal structure and nanoparticle stacked structure, were used to asymmetrically fill nanochannels of AAO membranes by a vapor-phase synthesis (VPS) method with aspiration approach and were further modified via sequence vapor infiltration (SVI) treatment. The ionic current measurements indicated that SVI treatment can modulate the asymmetric ionic transport in prepared membranes, which exhibited clear ionic current rectification phenomenon under optimal conditions. The ionic current rectifying behavior is derived from the asymmetry of surface conformations, silica species components, and hydrophobic wettability, which are created by the asymmetrical filling type, silica depositions on the heterogeneous membranes, and the condensation of silanol groups. This article provides a considerable strategy to fabricate composite membranes with obvious ionic current rectification performance via the cooperation of the VPS method and SVI treatment and opens up the potential of mesoporous silica confined in AAO membranes to mimic fluid transport in biological processes.

  7. Multi-band emission in a wide wavelength range from tin oxide/Au nanocomposites grown on porous anodic alumina substrate (AAO)

    International Nuclear Information System (INIS)

    Norek, Małgorzata; Michalska-Domańska, Marta; Stępniowski, Wojciech J.; Ayala, Israel; Bombalska, Aneta; Budner, Bogusław

    2013-01-01

    The photoluminescence (PL) properties of tin oxide nanostructures are investigated. Three samples of different morphology, induced by deposition process and various geometrical features of nanoporous anodic aluminum oxide (AAO) substrate, are analyzed. X-ray photoelectronic spectroscopy (XPS) analysis reveals the presence of two forms of tin oxide on the surface of all studied samples: SnO and SnO 2 . The former form is typical for reduced surface with bridging oxygen atoms and every other row of in-plane oxygen atoms removed. The oxygen defects give rise to a strong emission in visible region. Two intense PL peaks are observed centered at about 540 (band I) and 620 (band II) nm. The origin of these bands was ascribed to the recombination of electrons from the conduction band (band I) and shallow traps levels (band II) to the surface oxygen vacancy levels. Upon deposition of Au nanoparticles on the top of tin oxide nanostructures the emission at 540 and 620 nm disappears and a new band (band III) occurs in the range >760 nm. The PL mechanism operating in the studied systems is discussed. The tin oxide/Au nanocomposites can be used as efficient multi-band light emitters in a wide (from visible to near infrared) wavelength range.

  8. Deposition of MgB2 Thin Films on Alumina-Buffered Si Substrates by using Hybrid Physical-Chemical Vapor Deposition Method

    International Nuclear Information System (INIS)

    Lee, T. G.; Park, S. W.; Seong, W. K.; Huh, J. Y.; Jung, S. G.; Kang, W. N.; Lee, B. K.; An, K. S.

    2008-01-01

    [ MgB 2 ] thin films were fabricated using hybrid physical-chemical vapor deposition (HPCVD) method on silicon substrates with buffers of alumina grown by using atomic layer deposition method. The growth war in a range of temperatures 500 - 600 degrees C and under the reactor pressures of 25 - 50 degrees C. There are some interfacial reactions in the as-grown films with impurities of mostly Mg 2 Si, MgAl 2 O 4 , and other phases. The T c 's of MgB 2 films were observed to be as high as 39 K, but the transition widths were increased with growth temperatures. The magnetization was measured as a function of temperature down to the temperature of 5 K, but the complete Meissner effect was not observed, which shows that the granular nature of weak links is prevailing. The formation of mostly Mg 2 Si impurity in HPCVD process is discussed, considering the diffusion and reaction of Mg vapor with silicon substrates.

  9. Fabrication of Polymeric Antireflection Film Manufactured by Anodic Aluminum Oxide Template on Dye-Sensitized Solar Cells

    Directory of Open Access Journals (Sweden)

    Jenn-Kai Tsai

    2017-03-01

    Full Text Available In this study, high energy conversion efficient dye-sensitized solar cells (DSSCs were successfully fabricated by attaching a double anti-reflection (AR layer, which is composed of a subwavelength moth-eye structured polymethyl methacrylate (PMMA film and a polydimethylsiloxane (PDMS film. An efficiency of up to 6.79% was achieved. The moth-eye structured PMMA film was fabricated by using an anodic aluminum oxide (AAO template which is simple, low-cost and scalable. The nano-pattern of the AAO template was precisely reproduced onto the PMMA film. The photoanode was composed of Titanium dioxide (TiO2 nanoparticles (NPs with a diameter of 25 nm deposited on the fluorine-doped tin oxide (FTO glass substrate and the sensitizer N3. The double AR layer was proved to effectively improve the short-circuit current density (JSC and conversion efficiency from 14.77 to 15.79 mA/cm2 and from 6.26% to 6.79%, respectively.

  10. Nanoporous anodic aluminum oxide as a promising material for the electrostatically-controlled thin film interference filter

    International Nuclear Information System (INIS)

    Lo, Pei-Hsuan; Lee, Chih-Chun; Fang, Weileun; Luo, Guo-Lun

    2015-01-01

    This study presents the approach to implement the electrostatically-controlled thin film optical filter by using a nanoporous anodic aluminum oxide (np-AAO) layer as the key suspended micro structure. The bi-stable optical filter operates in the visible spectral range. In this work, the presented bi-stable optical filter has averaged reflectivity of 60%, and the central wavelengths are 580 and 690 nm respectively for on and off states. The presented np-AAO layer offers the following merits for the thin film optical filter: (1) material properties of np-AAO film, such as refractive index, elastic modulus and dielectric constant, can be easily changed by a low temperature pore-widening process, (2) in-use stiction of the suspended np-AAO structure can be reduced by the small contact area of nanoporous textures, (3) driving (pull-in) voltage can be reduced due to a large dielectric constant (ε AAO is 7.05) and small stiffness of np-AAO film and (4) dielectric charging can be reduced by the np-AAO material; thus the offset voltage is small. The study reports the design, fabrication and experimental results of the bi-stable optical filter to demonstrate the advantages of the presented device. The np-AAO material also has the potential for applications of other electrostatic drive micro devices. (paper)

  11. Properties and Structure of the LiCl-films on Lithium Anodes in Liquid Cathodes

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg; Hennesø, Erik

    2016-01-01

    Lithium anodes passivated by LiCl layers in different types of liquid cathodes (catholytes) based on LiAlCl4 in SOCl2 or SO2 have been studied by means of impedance spectroscopy. The impedance spectra have been fitted with two equivalent circuits using a nonlinear least squares fit program...

  12. Preparation and Characterization of Anode-Supported YSZ Thin Film Electrolyte by Co-Tape Casting and Co-Sintering Process

    International Nuclear Information System (INIS)

    Liu, Q L; Fu, C J; Chan, S H; Pasciak, G

    2011-01-01

    In this study, a co-tape casting and co-sintering process has been developed to prepare yttria-stabilized zirconia (YSZ) electrolyte films supported on Ni-YSZ anode substrates in order to substantially reduce the fabrication cost of solid oxide fuel cells (SOFC). Through proper control of the process, the anode/electrolyte bilayer structures with a size of 7.8cm x 7.8cm were achieved with good flatness. Scanning electron microscopy (SEM) observation indicated that the YSZ electrolyte film was about 16 μm in thickness, highly dense, crack free and well-bonded to the anode support. The electrochemical properties of the prepared anode-supported electrolyte film was evaluated in a button cell mode incorporating a (LaSr)MnO 3 -YSZ composite cathode. With humidified hydrogen as the fuel and stationary air as the oxidant, the cell demonstrated an open-circuit voltage of 1.081 V and a maximum power density of 1.01 W/cm 2 at 800 deg. C. The obtained results represent the important progress in the development of anode-supported intermediate temperature SOFC with reduced fabrication cost.

  13. Preparation and Characterization of Anode-Supported YSZ Thin Film Electrolyte by Co-Tape Casting and Co-Sintering Process

    Science.gov (United States)

    Liu, Q. L.; Fu, C. J.; Chan, S. H.; Pasciak, G.

    2011-06-01

    In this study, a co-tape casting and co-sintering process has been developed to prepare yttria-stabilized zirconia (YSZ) electrolyte films supported on Ni-YSZ anode substrates in order to substantially reduce the fabrication cost of solid oxide fuel cells (SOFC). Through proper control of the process, the anode/electrolyte bilayer structures with a size of 7.8cm × 7.8cm were achieved with good flatness. Scanning electron microscopy (SEM) observation indicated that the YSZ electrolyte film was about 16 μm in thickness, highly dense, crack free and well-bonded to the anode support. The electrochemical properties of the prepared anode-supported electrolyte film was evaluated in a button cell mode incorporating a (LaSr)MnO3-YSZ composite cathode. With humidified hydrogen as the fuel and stationary air as the oxidant, the cell demonstrated an open-circuit voltage of 1.081 V and a maximum power density of 1.01 W/cm2 at 800°C. The obtained results represent the important progress in the development of anode-supported intermediate temperature SOFC with reduced fabrication cost.

  14. Superhydrophilicity of a nanofiber-covered aluminum surface fabricated via pyrophosphoric acid anodizing

    Science.gov (United States)

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2016-12-01

    A superhydrophilic aluminum surface covered by numerous alumina nanofibers was fabricated via pyrophosphoric acid anodizing. High-density anodic alumina nanofibers grow on the bottom of a honeycomb oxide via anodizing in concentrated pyrophosphoric acid. The water contact angle on the nanofiber-covered aluminum surface decreased with time after a 4 μL droplet was placed on the surface, and a superhydrophilic behavior with a contact angle measuring 2.2° was observed within 2 s; this contact angle is considerably lower than those observed for electropolished and porous alumina-covered aluminum surfaces. There was no dependence of the superhydrophilicity on the density of alumina nanofibers fabricated via different constant voltage anodizing conditions. The superhydrophilic property of the surface covered by anodic alumina nanofibers was maintained during an exposure test for 359 h. The quick-drying and snow-sliding behaviors of the superhydrophilic aluminum covered with anodic alumina nanofibers were demonstrated.

  15. Semiconducting behavior of the anodically passive films formed on AZ31B alloy

    Directory of Open Access Journals (Sweden)

    A. Fattah-alhosseini

    2014-12-01

    Full Text Available This work includes determination of the semiconductor character and estimation of the dopant levels in the passive film formed on AZ31B alloy in 0.01 M NaOH, as well as the estimation of the passive film thickness as a function of the film formation potential. Mott–Schottky analysis revealed that the passive films displayed n-type semiconductive characteristics, where the oxygen vacancies and interstitials preponderated. Based on the Mott–Schottky analysis, it was shown that the calculated donor density increases linearly with increasing the formation potential. Also, the electrochemical impedance spectroscopy (EIS results indicated that the thickness of the passive film was decreased linearly with increasing the formation potential. The results showed that decreasing the formation potential offer better conditions for forming the passive films with higher protection behavior, due to the growth of a much thicker and less defective films.

  16. Morphology and performances of the anodic oxide films on Ti6Al4V alloy formed in alkaline-silicate electrolyte with aminopropyl silane addition under low potential

    International Nuclear Information System (INIS)

    Chen, Jiali; Wang, Jinwei; Yuan, Hongye

    2013-01-01

    Oxide films on Ti6Al4V alloy are prepared using sodium hydroxide–sodium silicate as the base electrolyte with addition of aminopropyl trimethoxysilane (APS) as additive by potentiostatic anodizing under 10 V. APS is incorporated into the films during anodizing and the surface morphology of the oxide films is changed from particle stacked to honeycomb-like porous surfaces as shown by scanning electron microscopy (SEM) with Energy Disperse Spectroscopy (EDX). The surface roughness and aminopropyl existence on the oxide films result in their differences in wettability as tested by the surface profile topography and contact angle measurements. The anti-abrasive ability of the anodic films is improved with the addition of APS due to its toughening effects and serving as lubricants in the ceramic oxide films as measured by ball-on-disk friction test. Also, potentiodynamic corrosion test proves that their anticorrosive ability in 3.5 wt.% NaCl is greatly improved as reflected by their much lower corrosion current (I corr ) and higher corrosion potential (E corr ) than those of the substrate.

  17. Morphology and performances of the anodic oxide films on Ti6Al4V alloy formed in alkaline-silicate electrolyte with aminopropyl silane addition under low potential

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Jiali; Wang, Jinwei, E-mail: wangjw@ustb.edu.cn; Yuan, Hongye

    2013-11-01

    Oxide films on Ti6Al4V alloy are prepared using sodium hydroxide–sodium silicate as the base electrolyte with addition of aminopropyl trimethoxysilane (APS) as additive by potentiostatic anodizing under 10 V. APS is incorporated into the films during anodizing and the surface morphology of the oxide films is changed from particle stacked to honeycomb-like porous surfaces as shown by scanning electron microscopy (SEM) with Energy Disperse Spectroscopy (EDX). The surface roughness and aminopropyl existence on the oxide films result in their differences in wettability as tested by the surface profile topography and contact angle measurements. The anti-abrasive ability of the anodic films is improved with the addition of APS due to its toughening effects and serving as lubricants in the ceramic oxide films as measured by ball-on-disk friction test. Also, potentiodynamic corrosion test proves that their anticorrosive ability in 3.5 wt.% NaCl is greatly improved as reflected by their much lower corrosion current (I{sub corr}) and higher corrosion potential (E{sub corr}) than those of the substrate.

  18. Highly efficient and large-scale fabrication of superhydrophobic alumina surface with strong stability based on self-congregated alumina nanowires.

    Science.gov (United States)

    Peng, Shan; Tian, Dong; Yang, Xiaojun; Deng, Wenli

    2014-04-09

    In this study, a large-area superhydrophobic alumina surface with a series of superior properties was fabricated via an economical, simple, and highly effective one-step anodization process, and subsequently modified with low-surface-energy film. The effects of the anodization parameters including electrochemical anodization time, current density, and electrolyte temperature on surface morphology and surface wettability were investigated in detail. The hierarchical alumina pyramids-on-pores (HAPOP) rough structure which was produced quickly through the one-step anodization process together with a low-surface-energy film deposition [1H,1H,2H,2H-perfluorodecyltriethoxysilane (PDES) and stearic acid (STA)] confer excellent superhydrophobicity and an extremely low sliding angle. Both the PDES-modified superhydrophobic (PDES-MS) and the STA-modified superhydrophobic (STA-MS) surfaces present fascinating nonwetting and extremely slippery behaviors. The chemical stability and mechanical durability of the PDES-MS and STA-MS surfaces were evaluated and discussed. Compared with the STA-MS surface, the as-prepared PDES-MS surface possesses an amazing chemical stability which not only can repel cool liquids (water, HCl/NaOH solutions, around 25 °C), but also can show excellent resistance to a series of hot liquids (water, HCl/NaOH solutions, 30-100 °C) and hot beverages (coffee, milk, tea, 80 °C). Moreover, the PDES-MS surface also presents excellent stability toward immersion in various organic solvents, high temperature, and long time period. In particular, the PDES-MS surface achieves good mechanical durability which can withstand ultrasonication treatment, finger-touch, multiple fold, peeling by adhesive tape, and even abrasion test treatments without losing superhydrophobicity. The corrosion resistance and durability of the diverse-modified superhydrophobic surfaces were also examined. These fascinating performances makes the present method suitable for large

  19. Anodic stripping voltammetric determination of mercury using multi-walled carbon nanotubes film coated glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Yi, Hongchao [Department of Environmental Engineering, Hubei Agriculture College, 434103, Jingzhou (China)

    2003-10-01

    An electrochemical method for the determination of trace levels of mercury based on a multi-walled carbon nanotubes (MWNT) film coated glassy carbon electrode (GCE) is described. In 0.1 mol L{sup -1} HCl solution containing 0.02 mol L{sup -1} KI, Hg{sup 2+} was firstly preconcentrated at the MWNT film and then reduced at -0.60 V. During the anodic potential sweep, reduced mercury was oxidized, and then a sensitive and well-defined stripping peak at about -0.20 V appeared. Under identical conditions, a MWNT film coated GCE greatly enhances the stripping peak current of mercury in contrast to a bare GCE. Low concentrations of I{sup -} remarkably improve the determining sensitivity, since this increases the accumulation efficiency of Hg{sup 2+} at the MWNT film coated GCE. The stripping peak current is proportional to the concentration of Hg{sup 2+} over the range 8 x 10{sup -10}-5 x 10{sup -7} mol L{sup -1}. The lowest detectable concentration of Hg{sup 2+} is 2 x 10{sup -10} mol L{sup -1} at 5 min accumulation. The relative standard deviation (RSD) at 1 x 10{sup -8} mol L{sup -1} Hg{sup 2+} was about 6% (n=10). By using this proposed method, Hg{sup 2+} in some water samples was determined, and the results were compared with those obtained by atomic absorption spectrometry (AAS). The two results are similar, suggesting that the MWNT-film coated GCE has great potential in practical analysis. (orig.)

  20. Microstructural study by XPS and GISAXS of surface layers formed via phase separation and percolation in polystyren/tetrabutyl titanate/alumina composite films

    International Nuclear Information System (INIS)

    Zeng Yanwei; Tian Changan; Liu Junliang

    2006-01-01

    The XPS and GISAXS have been employed as useful tools to probe the chemical compositional and microstructural evolutions in the surface layers formed via phase separation and percolation in polystyren/Ti(OBut) 4 /alumina composite thick films. The surface enrichment of Ti species due to the migration of Ti(OBut) 4 molecules in the films was found to show an incubation period of ∼15 h while the samples were treated at 100 deg. C before a remarkable progress can be identified. According to the XPS and GISAXS data, Key mechanism to govern this surface process is phenomenologically considered to be the specific phase separation behavior in Ti(OBut) 4 /PS blend and the subsequent percolating process. The extended thermal treatment was found to make the surface layer microstructure evolve from local phase separation featured with an increasing population of individual microbeads of Ti(OBut) 4 (∼1.5 nm in radius) to the formation of large size clusters of microbeads due to their interconnections, accompanied by the growth of every microbead itself to ∼10 nm on the average, which provokes and then enhances the surface enrichment of Ti(OBut) 4 since these clusters act as a fast diffusion network due to percolation effect

  1. MoOx thin films deposited by magnetron sputtering as an anode for aqueous micro-supercapacitors

    Science.gov (United States)

    Liu, Can; Li, Zhengcao; Zhang, Zhengjun

    2013-12-01

    In order to examine the potential application of non-stoichiometric molybdenum oxide as anode materials for aqueous micro-supercapacitors, conductive MoOx films (2 ⩽ x ⩽ 2.3) deposited via RF magnetron sputtering at different temperatures were systematically studied for composition, structure and electrochemical properties in an aqueous solution of Li2SO4. The MoOx (x ≈ 2.3) film deposited at 150 °C exhibited a higher areal capacitance (31 mF cm-2 measured at 5 mV s-1), best rate capability and excellent stability at potentials below -0.1 V versus saturated calomel electrode, compared to the films deposited at room temperature and at higher temperatures. These superior properties were attributed to the multi-valence composition and mixed-phase microstructure, i.e., the coexistence of MoO2 nanocrystals and amorphous MoOx (2.3 < x ⩽ 3). A mechanism combining Mo(IV) oxidation/reduction on the hydrated MoO2 grain surfaces and cation intercalation/extrusion is proposed to illustrate the pseudo-capacitive process.

  2. MoOx thin films deposited by magnetron sputtering as an anode for aqueous micro-supercapacitors

    Directory of Open Access Journals (Sweden)

    Can Liu

    2013-11-01

    Full Text Available In order to examine the potential application of non-stoichiometric molybdenum oxide as anode materials for aqueous micro-supercapacitors, conductive MoOx films (2 ≤ x ≤ 2.3 deposited via RF magnetron sputtering at different temperatures were systematically studied for composition, structure and electrochemical properties in an aqueous solution of Li2SO4. The MoOx (x ≈ 2.3 film deposited at 150 °C exhibited a higher areal capacitance (31 mF cm−2 measured at 5 mV s−1, best rate capability and excellent stability at potentials below −0.1 V versus saturated calomel electrode, compared to the films deposited at room temperature and at higher temperatures. These superior properties were attributed to the multi-valence composition and mixed-phase microstructure, i.e., the coexistence of MoO2 nanocrystals and amorphous MoOx (2.3 < x ≤ 3. A mechanism combining Mo(IV oxidation/reduction on the hydrated MoO2 grain surfaces and cation intercalation/extrusion is proposed to illustrate the pseudo-capacitive process.

  3. Photocatalytic activity of ferric oxide/titanium dioxide nanocomposite films on stainless steel fabricated by anodization and ion implantation

    Science.gov (United States)

    Zhan, Wei-ting; Ni, Hong-wei; Chen, Rong-sheng; Yue, Gao; Tai, Jun-kai; Wang, Zi-yang

    2013-08-01

    A simple surface treatment was used to develop photocatalytic activity for stainless steel. AISI 304 stainless steel specimens after anodization were implanted by Ti ions at an extracting voltage of 50 kV with an implantation dose of 3 × 1015 atoms·cm-2 and then annealed in air at 450°C for 2 h. The morphology was observed by scanning electron microscopy. The microstructure was characterized by X-ray diffraction and X-ray photoelectron spectroscopy. The photocatalytic degradation of methylene blue solution was carried out under ultraviolet light. The corrosion resistance of the stainless steel was evaluated in NaCl solution (3.5 wt%) by electrochemical polarization curves. It is found that the Ti ions depth profile resembles a Gaussian distribution in the implanted layer. The nanostructured Fe2O3/TiO2 composite film exhibits a remarkable enhancement in photocatalytic activity referenced to the mechanically polished specimen and anodized specimen. Meanwhile, the annealed Ti-implanted specimen remains good corrosion resistance.

  4. Investigations of Si Thin Films as Anode of Lithium-Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Qingliu [Department of Chemical; Shi, Bing; Bareño, Javier; Liu, Yuzi; Maroni, Victor A.; Zhai, Dengyun; Dees, Dennis W.; Lu, Wenquan

    2018-01-22

    Amorphous silicon thin films having various thicknesses were investigated as a negative electrode material for lithium-ion batteries. Electrochemical characterization of the 20 nm thick thin silicon film revealed a very low first cycle Coulombic efficiency, which can be attributed to the silicon oxide layer formed on both the surface of the as-deposited Si thin film and the interface between the Si and the substrate. Among the investigated films, the 100 nm Si thin film demonstrated the best performance in terms of first cycle efficiency and cycle life. Observations from scanning electron microscopy demonstrated that the generation of cracks was inevitable in the cycled Si thin films, even as the thickness of the film was as little as 20 nm, which was not predicted by previous modeling work. However, the cycling performance of the 20 and 100 nm silicon thin films was not detrimentally affected by these cracks. The poor capacity retention of the 1 mu m silicon thin film was attributed to the delamination.

  5. Electrochemical behavior of thin anodic oxide films on Zircaloy-4: Role of the mobile defects

    International Nuclear Information System (INIS)

    Salot, R.; Lefebvre-Joud, F.; Baroux, B.

    1996-01-01

    The first stages of the electrochemical oxidation of Zircaloy-4 are investigated using simple electrochemical tests and modeling the passive film modifications occurring as a result of contact with the electrolyte. Variations in electrode potential (open-circuit conditions) or current density (potentiodynamic scans) can be simply explained by a high field (F ∼ 10 6 V/cm) assisted passive film growth. Under open-circuit conditions, this field does not vary with exposure time (in the 2 h to 48 h range). The minimum electric field for the onset of high-field behavior is also evaluated and found smaller than the theoretical value which can be explained by a variation in the concentration of mobile defects throughout the film. Measurements of the electrode potential decay after a potentiodynamic scan confirm this model, allowing interpretation of the film modification as a combination of two separate phenomena: film growth under a high electric field and point defect annihilation

  6. Gold-coated silicon nanowire-graphene core-shell composite film as a polymer binder-free anode for rechargeable lithium-ion batteries

    Science.gov (United States)

    Kim, Han-Jung; Lee, Sang Eon; Lee, Jihye; Jung, Joo-Yun; Lee, Eung-Sug; Choi, Jun-Hyuk; Jung, Jun-Ho; Oh, Minsub; Hyun, Seungmin; Choi, Dae-Geun

    2014-07-01

    We designed and fabricated a gold (Au)-coated silicon nanowires/graphene (Au-SiNWs/G) hybrid composite as a polymer binder-free anode for rechargeable lithium-ion batteries (LIBs). A large amount of SiNWs for LIB anode materials can be prepared by metal-assisted chemical etching (MaCE) process. The Au-SiNWs/G composite film on current collector was obtained by vacuum filtration using an anodic aluminum oxide (AAO) membrane and hot pressing method. Our experimental results show that the Au-SiNWs/G composite has a stable reversible capacity of about 1520 mA h/g which was maintained for 20 cycles. The Au-SiNWs/G composite anode showed much better cycling performance than SiNWs/polyvinylidene fluoride (PVDF)/Super-P, SiNWs/G composite, and pure SiNWs anodes. The improved electrochemical properties of the Au-SiNWs/G composite anode material is mainly ascribed to the composite's porous network structure.

  7. Electrostatic layer-by-layer a of platinum-loaded multiwall carbon nanotube multilayer: A tunable catalyst film for anodic methanol oxidation

    International Nuclear Information System (INIS)

    Yuan Junhua; Wang Zhijuan; Zhang Yuanjian; Shen Yanfei; Han Dongxue; Zhang Qixian; Xu Xiaoyu; Niu Li

    2008-01-01

    A simple layer-by-layer (LBL) electrostatic adsorption technique was developed for deposition of films composed of alternating layers of positively charged poly(diallyldimethylammonium chloride) (PDDA) and negatively charged multiwall carbon nanotubes bearing platinum nanoparticles (Pt-CNTs). PDDA/Pt-CNT film structure and morphology up to six layers were characterized by scanning electron microscopy and ultraviolet-visible spectroscopy, showing the Pt-CNT layers to be porous and uniformly deposited within the multilayer films. Electrochemical properties of the PDDA/Pt-CNT films, as well as electrocatalytic activity toward methanol oxidation, were investigated with cyclic voltammetry. Significant activity toward anodic methanol oxidation was observed and is readily tunable through changing film thickness and/or platinum-nanoparticle loading. Overall, the observed properties of these PDDA/Pt-CNT multilayer films indicated unique potential for application in direct methanol fuel cell

  8. Enhanced performance of organic light-emitting devices by using electropolymerized poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) film as the anode modification layer

    Energy Technology Data Exchange (ETDEWEB)

    Liu Xiaona [Graduate University of Chinese Academy of Sciences, Beijing 100049 (China); Key Laboratory of Photochemical Conversion and Optoelectronic Materials, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Yan Jun [Key Laboratory of Photochemical Conversion and Optoelectronic Materials, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Meng Lingchuan [Key Laboratory of Luminescence and Optical Information, Ministry of Education, Institute of Optoelectronic Technology, Beijing Jiaotong University, Beijing 100044 (China); Sun Chenghua; Hu Xiujie; Chen Ping [Key Laboratory of Photochemical Conversion and Optoelectronic Materials, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Zhou Shuyun, E-mail: zhou_shuyun@mail.ipc.ac.cn [Key Laboratory of Photochemical Conversion and Optoelectronic Materials, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Teng Feng [Key Laboratory of Luminescence and Optical Information, Ministry of Education, Institute of Optoelectronic Technology, Beijing Jiaotong University, Beijing 100044 (China)

    2012-01-31

    Poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) films were prepared by electropolymerization on patterned indium tin oxide substrates in isopropanol solution. The thickness and doping level of the PEDOT:PSS films were controlled by adjusting the electropolymerization time and the concentration of poly(styrene sulfonate) acid, respectively. Organic light-emitting diodes were fabricated using the electropolymerized PEDOT:PSS film as the anode modification layer. The dependence of the performance on thickness of PEDOT:PSS films was investigated. It is shown that the performance of the device can be further enhanced when the thickness of PEDOT:PSS films reached an optimum condition. This method facilitates manufacturing procedures of conducting polymers films and may offer an economical route for producing organic electroluminescent devices.

  9. Luminescence enhancement of a self-organised Y.sub.2./sub.O.sub.3./sub.:Eu.sup.3+./sup. thin film-coated porous alumina membrane

    Czech Academy of Sciences Publication Activity Database

    Abdellaoui, N.; Pereira, A.; Kandri, T.; Drouard, E.; Novotný, Michal; Moine, B.; Pillonnet, A.

    2016-01-01

    Roč. 4, č. 39 (2016), s. 9212-9218 ISSN 2050-7526 R&D Projects: GA MŠk LO1409; GA ČR GA16-22092S Institutional support: RVO:68378271 Keywords : pulsed laser deposition * thin film * self- organisation * alumina membrane * luminescence * photonic structure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 5.256, year: 2016

  10. Inkjet-printed thin film radio-frequency capacitors based on sol-gel derived alumina dielectric ink

    KAUST Repository

    McKerricher, Garret; Maller, Robert; Vaseem, Mohammad; McLachlan, Martyn A.; Shamim, Atif

    2017-01-01

    passive electronics. The ability to spatially pattern high quality Al2O3 thin films using, for example, inkjet printing would tremendously simplify the incumbent fabrication processes – significantly reducing cost and allowing for the development of large

  11. Investigating the property profile of polyamide-alumina nanocomposite materials

    International Nuclear Information System (INIS)

    Sarwar, Muhammad Ilyas; Zulfiqar, Sonia; Ahmad, Zahoor

    2009-01-01

    Transparent sol-gel-derived nanocomposites were prepared by incorporating an alumina network into a polyamide matrix. Different amounts of aluminum butoxide were hydrolyzed and condensed to produce the alumina network. Thin composite films were characterized in terms of their optical, morphological, mechanical and thermomechanical properties. Tensile modulus, stress at both yield and break points, improved for alumina loadings of 5-10 wt.%. The glass transition temperature increased to 140 o C for nanocomposites containing 15 wt.% alumina. Scanning electron microscopy investigations indicated a uniform distribution of alumina in the polyamide matrix.

  12. Effects of anodic passivation on the constitution, stability and resistance to corrosion of passive film formed on an Fe-24Mn-4Al-5Cr alloy

    International Nuclear Information System (INIS)

    Zhang, Y.S.; Zhu, X.M.; Liu, M.; Che, R.X.

    2004-01-01

    The effects of anodic aging time and potential on the corrosion resistance, stability and constitution of the passive film formed on an Fe-24Mn-4Al-5Cr alloy in 50% HNO 3 solution were studied by using combined electrochemical measurements and Auger electron spectroscopic (AES)/X-ray photoelectron spectroscopic (XPS) analysis. In the anodic passive region, prolonged anodic aging time or increased passivating potential can induce better protective and stable properties of the passive film and better resistance to corrosion. With increasing aging time from 15 min to 5 h, the time required for the potential decay from the passive to active state increases from about 300 up to above 12,000 s, and the corrosion resistance in 1 mol l -1 Na 2 SO 4 solution of Fe-24Mn-4Al-5Cr alloy, characterized by polarization curves, is superior to that of Fe-13% Cr-0.1% C stainless steel. AES and XPS analyses of the aging passive film show that these improvements of properties are related to modifications of the passive layer with time. The increase of resistance to corrosion is attributed to Al 2 O 3 and Cr 2 O 3 enrichment and oxides of Fe and Mn depletion in the passive film and a thickening of the effective barrier layer of oxides

  13. Electron transfer across anodic films formed on tin in carbonate-bicarbonate buffer solution

    International Nuclear Information System (INIS)

    Gervasi, C.A.; Folquer, M.E.; Vallejo, A.E.; Alvarez, P.E.

    2005-01-01

    Impedance and steady-state data were recorded in order to study the kinetics of electron transfer between passive tin electrodes and an electrolytic solution containing the K 3 Fe(CN) 6 -K 4 Fe(CN) 6 redox couple. Film thickness plays a key role in determining the type of electronic conduction of these oxide covered electrodes. Electron exchange with the oxide takes place with participation of the conduction band in the semiconducting film. A mechanism involving direct electron tunneling through the space charge barrier is the most suitable to interpret the experimental evidence

  14. Electron transfer across anodic films formed on tin in carbonate-bicarbonate buffer solution

    Energy Technology Data Exchange (ETDEWEB)

    Gervasi, C.A. [Universidad Nacional de La Plata (Argentina). Facultad de Ciencias Exactas; Universidad Nacional de La Plata (Argentina). Facultad de Ingenieria; Folquer, M.E. [Universidad Nacional de Tucaman (Argentina). Inst. de Quimica Fisica; Vallejo, A.E. [Universidad Nacional de La Plata (Argentina). Facultad de Ingenieria; Alvarez, P.E. [Universidad Nacional de Tucaman (Argentina). Inst. de Fisica

    2005-01-15

    Impedance and steady-state data were recorded in order to study the kinetics of electron transfer between passive tin electrodes and an electrolytic solution containing the K{sub 3}Fe(CN){sub 6}-K{sub 4}Fe(CN){sub 6} redox couple. Film thickness plays a key role in determining the type of electronic conduction of these oxide covered electrodes. Electron exchange with the oxide takes place with participation of the conduction band in the semiconducting film. A mechanism involving direct electron tunneling through the space charge barrier is the most suitable to interpret the experimental evidence. (Author)

  15. Sodium beta-alumina thin films as gate dielectrics for AlGaN/GaN metal—insulator—semiconductor high-electron-mobility transistors

    International Nuclear Information System (INIS)

    Tian Ben-Lang; Chen Chao; Li Yan-Rong; Zhang Wan-Li; Liu Xing-Zhao

    2012-01-01

    Sodium beta-alumina (SBA) is deposited on AlGaN/GaN by using a co-deposition process with sodium and Al 2 O 3 as the precursors. The X-ray diffraction (XRD) spectrum reveals that the deposited thin film is amorphous. The binding energy and composition of the deposited thin film, obtained from the X-ray photoelectron spectroscopy (XPS) measurement, are consistent with those of SBA. The dielectric constant of the SBA thin film is about 50. Each of the capacitance—voltage characteristics obtained at five different frequencies shows a high-quality interface between SBA and AlGaN. The interface trap density of metal—insulator—semiconductor high-electron-mobility transistor (MISHEMT) is measured to be (3.5∼9.5)×10 10 cm −2 ·eV −1 by the conductance method. The fixed charge density of SBA dielectric is on the order of 2.7×10 12 cm −2 . Compared with the AlGaN/GaN metal—semiconductor heterostructure high-electron-mobility transistor (MESHEMT), the AlGaN/GaN MISHEMT usually has a threshold voltage that shifts negatively. However, the threshold voltage of the AlGaN/GaN MISHEMT using SBA as the gate dielectric shifts positively from −5.5 V to −3.5 V. From XPS results, the surface valence-band maximum (VBM-EF) of AlGaN is found to decrease from 2.56 eV to 2.25 eV after the SBA thin film deposition. The possible reasons why the threshold voltage of AlGaN/GaN MISHEMT with the SBA gate dielectric shifts positively are the influence of SBA on surface valence-band maximum (VBM-EF), the reduction of interface traps and the effects of sodium ions, and/or the fixed charges in SBA on the two-dimensional electron gas (2DEG). (condensed matter: structural, mechanical, and thermal properties)

  16. Plasma-Enhanced Chemical Vapor Deposition (PE-CVD) yields better Hydrolytical Stability of Biocompatible SiOx Thin Films on Implant Alumina Ceramics compared to Rapid Thermal Evaporation Physical Vapor Deposition (PVD).

    Science.gov (United States)

    Böke, Frederik; Giner, Ignacio; Keller, Adrian; Grundmeier, Guido; Fischer, Horst

    2016-07-20

    Densely sintered aluminum oxide (α-Al2O3) is chemically and biologically inert. To improve the interaction with biomolecules and cells, its surface has to be modified prior to use in biomedical applications. In this study, we compared two deposition techniques for adhesion promoting SiOx films to facilitate the coupling of stable organosilane monolayers on monolithic α-alumina; physical vapor deposition (PVD) by thermal evaporation and plasma enhanced chemical vapor deposition (PE-CVD). We also investigated the influence of etching on the formation of silanol surface groups using hydrogen peroxide and sulfuric acid solutions. The film characteristics, that is, surface morphology and surface chemistry, as well as the film stability and its adhesion properties under accelerated aging conditions were characterized by means of X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), inductively coupled plasma-optical emission spectroscopy (ICP-OES), and tensile strength tests. Differences in surface functionalization were investigated via two model organosilanes as well as the cell-cytotoxicity and viability on murine fibroblasts and human mesenchymal stromal cells (hMSC). We found that both SiOx interfaces did not affect the cell viability of both cell types. No significant differences between both films with regard to their interfacial tensile strength were detected, although failure mode analyses revealed a higher interfacial stability of the PE-CVD films compared to the PVD films. Twenty-eight day exposure to simulated body fluid (SBF) at 37 °C revealed a partial delamination of the thermally deposited PVD films whereas the PE-CVD films stayed largely intact. SiOx layers deposited by both PVD and PE-CVD may thus serve as viable adhesion-promoters for subsequent organosilane coupling agent binding to α-alumina. However, PE-CVD appears to be favorable for long-term direct film exposure to aqueous

  17. A self-supported metal-organic framework derived Co3O4 film prepared by an in-situ electrochemically assistant process as Li ion battery anodes

    Science.gov (United States)

    Zhao, Guangyu; Sun, Xin; Zhang, Li; Chen, Xuan; Mao, Yachun; Sun, Kening

    2018-06-01

    Derivates of metal-organic frameworks are promising materials of self-supported Li ion battery anodes due to the good dispersion of active materials, conductive scaffold, and mass transport channels in them. However, the discontinuous growth and poor adherence of metal-organic framework films on substrates hamper their development in self-supported electrodes. In the present study, cobalt-based metal-organic frameworks are anchored on Ti nanowire arrays through an electrochemically assistant method, and then the metal-organic framework films are pyrolyzed to carbon-containing, porous, self-supported anodes of Li ion battery anodes. Scanning electron microscope images indicate that, a layer cobaltosic oxide polyhedrons inserted by the nanowires are obtained with the controllable in-situ synthesis. Thanks to the good dispersion and adherence of cobaltosic oxide polyhedrons on Ti substrates, the self-supported anodes exhibit remarkable rate capability and durability. They possess a capacity of 300 mAh g-1 at a rate current of 20 A g-1, and maintain 2000 charge/discharge cycles without obvious decay.

  18. Microwave Plasma Chemical Vapor Deposition of Nano-Structured Sn/C Composite Thin-Film Anodes for Li-ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Stevenson, Cynthia; Marcinek, M.; Hardwick, L.J.; Richardson, T.J.; Song, X.; Kostecki, R.

    2008-02-01

    In this paper we report results of a novel synthesis method of thin-film composite Sn/C anodes for lithium batteries. Thin layers of graphitic carbon decorated with uniformly distributed Sn nanoparticles were synthesized from a solid organic precursor Sn(IV) tert-butoxide by a one step microwave plasma chemical vapor deposition (MPCVD). The thin-film Sn/C electrodes were electrochemically tested in lithium half cells and produced a reversible capacity of 440 and 297 mAhg{sup -1} at C/25 and 5C discharge rates, respectively. A long term cycling of the Sn/C nanocomposite anodes showed 40% capacity loss after 500 cycles at 1C rate.

  19. Self-assembly silicon/porous reduced graphene oxide composite film as a binder-free and flexible anode for lithium-ion batteries

    International Nuclear Information System (INIS)

    Tang, H.; Zhang, Y.J.; Xiong, Q.Q.; Cheng, J.D.; Zhang, Q.; Wang, X.L.; Gu, C.D.; Tu, J.P.

    2015-01-01

    A Si/porous reduced graphene oxide (rGO) composite film synthesized by evaporation and leavening method are developed as a high-performance anode material for lithium ion batteries. The porous structure as buffer base can effectively release the volume expansion of the silicon particles, increase the electrical conductivity and reduce the transfer resistance of Li ions. The Si/porous rGO composite film presents high specific capacity and good cycling stability (1261 mA h g −1 at 50 mA g −1 up to 70 cycles), as well as enhanced rate capability. This approach to prepare such a unique structure is a low-cost and facile route for the silicon-based anode materials

  20. Inkjet-printed thin film radio-frequency capacitors based on sol-gel derived alumina dielectric ink

    KAUST Repository

    McKerricher, Garret

    2017-05-03

    There has been significant interest in printing radio frequency passives, however the dissipation factor of printed dielectric materials has limited the quality factor achievable. Al2O3 is one of the best and widely implemented dielectrics for RF passive electronics. The ability to spatially pattern high quality Al2O3 thin films using, for example, inkjet printing would tremendously simplify the incumbent fabrication processes – significantly reducing cost and allowing for the development of large area electronics. To-date, particle based Al2O3 inks have been explored as dielectrics, although several drawbacks including nozzle clogging and grain boundary formation in the films hinder progress. In this work, a particle free Al2O3 ink is developed and demonstrated in RF capacitors. Fluid and jetting properties are explored, along with control of ink spreading and coffee ring suppression. The liquid ink is heated to 400 °C decomposing to smooth Al2O3 films ~120 nm thick, with roughness of <2 nm. Metal-insulator-metal capacitors, show high capacitance density >450 pF/mm2, and quality factors of ~200. The devices have high break down voltages, >25 V, with extremely low leakage currents, <2×10−9 A/cm2 at 1 MV/cm. The capacitors compare well with similar Al2O3 devices fabricated by atomic layer deposition.

  1. Layered double hydroxide films on nanoporous anodic aluminum oxide/aluminum wire: a new fiber for rapid analysis of Origanum vulgare essential oils.

    Science.gov (United States)

    Piryaei, Marzieh

    2018-01-01

    Zn/Al layered double hydroxide (LDH) films were fabricated in situ with anodic aluminium oxide aluminium as both the substrate and the sole aluminium source by means of urea hydrolysis. Headspace solid phase microextraction using LDH fibre in combination with capillary GC-MS was utilised as a monitoring technique for the collection and detection of the volatile compounds of Origanum vulgare. Experimental parameters, including the sample weight, microwave power, extraction time and humidity effect, were examined and optimised.

  2. Vanadium nitride as a novel thin film anode material for rechargeable lithium batteries

    International Nuclear Information System (INIS)

    Sun Qian; Fu Zhengwen

    2008-01-01

    Vanadium mononitride (VN) thin films have been successfully fabricated by magnetron sputtering. Its electrochemical behaviour with lithium was examined by galvanostatic cell cycling and cyclic voltammetry. The capacity of VN was found to be stable above 800 mAh g -1 after 50 cycles. By using ex situ X-ray diffraction, high-resolution transmission electron microscopy and selected area electron diffraction as well as in situ spectroelectrochemical measurements, the electrochemical reaction mechanism of VN with lithium was investigated. The reversible conversion reaction of VN into metal V and Li 3 N was revealed. The high reversible capacity and good stable cycle of VN thin film electrode made it a new promising lithium-ion storage material for future rechargeable lithium batteries

  3. Failure Analysis of Alumina Reinforced Aluminum Microtruss and Tube Composites

    Science.gov (United States)

    Chien, Hsueh Fen (Karen)

    The energy absorption capacity of cellular materials can be dramatically increased by applying a structural coating. This thesis examined the failure mechanisms of alumina reinforced 3003 aluminum alloy microtrusses and tubes. Alumina coatings were produced by hard anodizing and by plasma electrolytic oxidation (PEO). The relatively thin and discontinuous oxide coating at the hinge acted as a localized weak spot which triggered a chain reaction of failure, including oxide fracture, oxide spallation, oxide penetration to the aluminum core and severe local plastic deformation of the core. For the PEO microtrusses, delamination occurred within the oxide coating resulting in a global strut buckling failure mode. A new failure mode for the anodized tubes was observed: (i) axisymmetric folding of the aluminum core, (ii) longitudinal fracture, and (iii) alumina pulverization. Overall, the alumina coating enhanced the buckling resistance of the composites, while the aluminum core supported the oxide during the damage propagation.

  4. A Dew Point Meter Comprising a Nanoporous Thin Film Alumina Humidity Sensor with a Linearizing Capacitance Measuring Electronics

    Directory of Open Access Journals (Sweden)

    Dilip Kumar Ghara

    2008-02-01

    Full Text Available A novel trace moisture analyzer is presented comprising a capacitive nanoporous film of metal oxide sensor and electronics. The change in capacity of the sensor is due to absorption of water vapor by the pores. A simple capacitance measuring electronics is developed which can detect any change in capacitance and correlates to ambient humidity. The circuit can minimize the parasitic earth capacitance. The non linear response of the sensor is linearized with a micro-controller linearizing circuit. The experimental result shows a resolution of -4°C DP and accuracy within 2%.

  5. Li4SiO4-Based Artificial Passivation Thin Film for Improving Interfacial Stability of Li Metal Anodes.

    Science.gov (United States)

    Kim, Ji Young; Kim, A-Young; Liu, Guicheng; Woo, Jae-Young; Kim, Hansung; Lee, Joong Kee

    2018-03-14

    An amorphous SiO 2 (a-SiO 2 ) thin film was developed as an artificial passivation layer to stabilize Li metal anodes during electrochemical reactions. The thin film was prepared using an electron cyclotron resonance-chemical vapor deposition apparatus. The obtained passivation layer has a hierarchical structure, which is composed of lithium silicide, lithiated silicon oxide, and a-SiO 2 . The thickness of the a-SiO 2 passivation layer could be varied by changing the processing time, whereas that of the lithium silicide and lithiated silicon oxide layers was almost constant. During cycling, the surface of the a-SiO 2 passivation layer is converted into lithium silicate (Li 4 SiO 4 ), and the portion of Li 4 SiO 4 depends on the thickness of a-SiO 2 . A minimum overpotential of 21.7 mV was observed at the Li metal electrode at a current density of 3 mA cm -2 with flat voltage profiles, when an a-SiO 2 passivation layer of 92.5 nm was used. The Li metal with this optimized thin passivation layer also showed the lowest charge-transfer resistance (3.948 Ω cm) and the highest Li ion diffusivity (7.06 × 10 -14 cm 2 s -1 ) after cycling in a Li-S battery. The existence of the Li 4 SiO 4 artificial passivation layer prevents the corrosion of Li metal by suppressing Li dendritic growth and improving the ionic conductivity, which contribute to the low charge-transfer resistance and high Li ion diffusivity of the electrode.

  6. Metal ion analysis in contaminated water samples using anodic stripping voltammetry and a nanocrystalline diamond thin-film electrode

    International Nuclear Information System (INIS)

    Sonthalia, Prerna; McGaw, Elizabeth; Show, Yoshiyuki; Swain, Greg M.

    2004-01-01

    Boron-doped nanocrystalline diamond thin-film electrodes were employed for the detection and quantification of Ag (I), Cu (II), Pb (II), Cd (II), and Zn (II) in several contaminated water samples using anodic stripping voltammetric (ASV). Diamond is an alternate electrode that possesses many of the same attributes as Hg and, therefore, appears to be a viable material for this electroanalytical measurement. The nanocrystalline form has been found to perform slightly better than the more conventional microcrystalline form of diamond in this application. Differential pulse voltammetry (DPASV) was used to detect these metal ions in lake water, well water, tap water, wastewater treatment sludge, and soil. The electrochemical results were compared with data from inductively coupled plasma mass spectrometric (ICP-MS) and or atomic absorption spectrometric (AAS) measurements of the same samples. Diamond is shown to function well in this electroanalytical application, providing a wide linear dynamic range, a low limit of quantitation, excellent response precision, and good response accuracy. For the analysis of Pb (II), bare diamond provided a response nearly identical to that obtained with a Hg-coated glassy carbon electrode

  7. Degradation of the corrosion resistance of anodic oxide films through immersion in the anodising electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Rubio, M. [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049-Madrid (Spain); Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906-Getafe (Spain); Ocon, P., E-mail: pilar.ocon@uam.e [Departamento de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, 28049-Madrid (Spain); Curioni, M.; Thompson, G.E.; Skeldon, P. [Corrosion and Protection Center, School of Materials, The University of Manchester, M60 1QD England (United Kingdom); Lavia, A. [Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906-Getafe (Spain); Garcia, I. [Department of Surface Technologies, Engineering of Materials and Processes, Airbus Spain, Av. John Lennon s/n 28906-Getafe (Spain); Department of Corrosion and Protection, National Center for Metallurgical Research CENIM-CSIC, Av. Gregorio del Amo 8, 28040-Madrid (Spain)

    2010-07-15

    The deterioration of AA2024, AA6061 and AA7475 anodised in an environmentally-compliant tartaric acid/sulphuric acid electrolyte has been examined as a function of the immersion time in the electrolyte after termination of anodising. By transmission electron microscopy and scanning electron microscopy, degradation of the porous oxide film was qualitatively observed on AA2024. Electrochemical impedance spectroscopy revealed that AA2024 and AA7075 were more sensitive to prolonged immersion in the anodising electrolyte compared with AA6061, due to increased barrier layer thinning rates and increased susceptibility to localized corrosion. Salt spray tests confirmed the previous, indicating decay of anticorrosion performance for AA2024 and AA7075.

  8. Degradation of the corrosion resistance of anodic oxide films through immersion in the anodising electrolyte

    International Nuclear Information System (INIS)

    Garcia-Rubio, M.; Ocon, P.; Curioni, M.; Thompson, G.E.; Skeldon, P.; Lavia, A.; Garcia, I.

    2010-01-01

    The deterioration of AA2024, AA6061 and AA7475 anodised in an environmentally-compliant tartaric acid/sulphuric acid electrolyte has been examined as a function of the immersion time in the electrolyte after termination of anodising. By transmission electron microscopy and scanning electron microscopy, degradation of the porous oxide film was qualitatively observed on AA2024. Electrochemical impedance spectroscopy revealed that AA2024 and AA7075 were more sensitive to prolonged immersion in the anodising electrolyte compared with AA6061, due to increased barrier layer thinning rates and increased susceptibility to localized corrosion. Salt spray tests confirmed the previous, indicating decay of anticorrosion performance for AA2024 and AA7075.

  9. Semi-transparent ordered TiO{sub 2} nanostructures prepared by anodization of titanium thin films deposited onto the FTO substrate

    Energy Technology Data Exchange (ETDEWEB)

    Szkoda, Mariusz, E-mail: mariusz-szkoda@wp.pl [Department of Chemistry and Technology of Functional Materials, Faculty of Chemistry, Gdańsk University of Technology, Narutowicza 11/12, Gdańsk 80-233 (Poland); Lisowska-Oleksiak, Anna [Department of Chemistry and Technology of Functional Materials, Faculty of Chemistry, Gdańsk University of Technology, Narutowicza 11/12, Gdańsk 80-233 (Poland); Grochowska, Katarzyna [Centre for Plasma and Laser Engineering, Szewalski Institute of Fluid-Flow Machinery, Polish Academy of Science, Fiszera 14, 80-231 Gdańsk (Poland); Skowroński, Łukasz [Institute of Mathematics and Physics, UTP University of Science and Technology, Kaliskiego 7, 85-796 Bydgoszcz (Poland); Karczewski, Jakub [Faculty of Applied Physics and Mathematics, Gdańsk University of Technology, Narutowicza 11/12, 80-233 Gdańsk (Poland); Siuzdak, Katarzyna [Centre for Plasma and Laser Engineering, Szewalski Institute of Fluid-Flow Machinery, Polish Academy of Science, Fiszera 14, 80-231 Gdańsk (Poland)

    2016-09-15

    Highlights: • High quality titanium coatings were doposited using industrial magnetron sputtering equipment. • Semi-transparent TiO{sub 2} were prepared via anodization realized in various conditions. • Depending on electrolyte type, ordered tubular or porous TiO{sub 2} layers were obtained. • Prepared material can act as semiconducting layer in photovoltaic cells. - Abstract: In a significant amount of cases, the highly ordered TiO{sub 2} nanotube arrays grow through anodic oxidation of a titanium metal plate immersed in electrolyte containing fluoride ions. However, for some practical applications, e.g. solar cells or electrochromic windows, the semi-transparent TiO{sub 2} formed directly on the transparent, conductive substrate is very much desired. This work shows that high-quality Ti coating could be formed at room temperature using an industrial magnetron sputtering system within 50 min. Under optimized conditions, the anodization process was performed on 2 μm titanium films deposited onto the FTO (fluorine-tin-oxide) support. Depending on the electrolyte type, highly ordered tubular or porous titania layers were obtained. The fabricated samples, after their thermal annealing, were investigated using scanning electron microscopy, Raman spectroscopy and UV–vis spectroscopy in order to investigate their morphology, crystallinity and absorbance ability. The photocurrent response curves indicate that materials are resistant to the photocorrosion process and their activity is strongly connected to optical properties. The most transparent TiO{sub 2} films were fabricated when Ti was anodized in water electrolyte, whereas the highest photocurrent densities (12 μA cm{sup −2}) were registered for titania received after Ti anodization in ethylene glycol solution. The obtained results are of significant importance in the production of thin, semi-transparent titania nanostructures on a commercial scale.

  10. Semi-transparent ordered TiO_2 nanostructures prepared by anodization of titanium thin films deposited onto the FTO substrate

    International Nuclear Information System (INIS)

    Szkoda, Mariusz; Lisowska-Oleksiak, Anna; Grochowska, Katarzyna; Skowroński, Łukasz; Karczewski, Jakub; Siuzdak, Katarzyna

    2016-01-01

    Highlights: • High quality titanium coatings were doposited using industrial magnetron sputtering equipment. • Semi-transparent TiO_2 were prepared via anodization realized in various conditions. • Depending on electrolyte type, ordered tubular or porous TiO_2 layers were obtained. • Prepared material can act as semiconducting layer in photovoltaic cells. - Abstract: In a significant amount of cases, the highly ordered TiO_2 nanotube arrays grow through anodic oxidation of a titanium metal plate immersed in electrolyte containing fluoride ions. However, for some practical applications, e.g. solar cells or electrochromic windows, the semi-transparent TiO_2 formed directly on the transparent, conductive substrate is very much desired. This work shows that high-quality Ti coating could be formed at room temperature using an industrial magnetron sputtering system within 50 min. Under optimized conditions, the anodization process was performed on 2 μm titanium films deposited onto the FTO (fluorine-tin-oxide) support. Depending on the electrolyte type, highly ordered tubular or porous titania layers were obtained. The fabricated samples, after their thermal annealing, were investigated using scanning electron microscopy, Raman spectroscopy and UV–vis spectroscopy in order to investigate their morphology, crystallinity and absorbance ability. The photocurrent response curves indicate that materials are resistant to the photocorrosion process and their activity is strongly connected to optical properties. The most transparent TiO_2 films were fabricated when Ti was anodized in water electrolyte, whereas the highest photocurrent densities (12 μA cm"−"2) were registered for titania received after Ti anodization in ethylene glycol solution. The obtained results are of significant importance in the production of thin, semi-transparent titania nanostructures on a commercial scale.

  11. alumina solid electrolyte

    Indian Academy of Sciences (India)

    -β/β -alumina ceramics come from two parent phases designated as β-alumina and β ..... Acknowledgements. This work was supported by the Energy Efficiency & ... of Trade, Industry & Energy, Republic of Korea (No. 20142010102460).

  12. One-step synthesis of continuous free-standing Carbon Nanotubes-Titanium oxide composite films as anodes for lithium-ion batteries

    International Nuclear Information System (INIS)

    Gao, Hongxu; Hou, Feng; Wan, Zhipeng; Zhao, Sha; Yang, Deming; Liu, Jiachen; Guo, Anran; Gong, Yuxuan

    2015-01-01

    Highlights: • CNTs/TiO 2 compoiste films synthesized are continuous and free-standing. • The film can be directly used as flexible, binder-free Lithium-Ion Battery electrode. • The CNTs/TiO 2 electrodes exhibit excellent rate capacity and cyclic stability. • Our strategy is readily applicable to fabricate other CNTs-based composite films. - Abstract: Continuous free-standing Carbon Nanotubes (CNTs)/Titanium oxide (TiO 2 ) composite films were fabricated in a vertical CVD gas flow reactor with water sealing by the One-Step Chemical Vapor Deposition (CVD) approach. The composite films consist of multiple layers of conductive carbon nanotube networks with titanium oxide nanoparticles decorating on carbon nanotube surface. The as-synthesized flexible and transferrable composite films show excellent electrochemical properties, when the content of tetrabutyl titanate is 19.0 wt.%, which can be promising as binder-free anodes for Lithium-Ion Battery (LIB) applications. It demonstrates remarkably high rate capacity of 150 mAh g −1 , as well as excellent high rate cyclic stability over 500 cycles (current density of 3000 mA g −1 ). Such observations can be attributed to the relatively larger surface area and pore volume comparing with pristine CNT films. Great potentials of CNTs/TiO 2 composite films for large-scale production and application in energy devices were shown

  13. Formation of self-assembled stripes on the anodic aluminum oxide

    International Nuclear Information System (INIS)

    Liu Hongwen; Guo Haiming; Wang Yeliang; Shen Chengmin; Yang Haitao; Wang Yutian; Wei Long

    2004-01-01

    Non-polished aluminum sheets were anodized and the coexistence of self-assembled stripes and porous arrays on the Al surface was observed. The nanostructures were investigated in details using an atomic force microscope. And the formation mechanism of the stripes was discussed and simulated using Brusselator model in this work. The authors demonstrated that the self-assembled patterns on the Al surface were governed by the competition of formation and dissolution of alumina film during the reaction process. Moreover, this type of ordered structure could only form in certain conditions

  14. Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Mubarak Ali, M., E-mail: masterscience2003@yahoo.co.in [Advanced Materials Research Laboratory, Department of Chemistry, Periyar University, Omalur Main Road, Salem 636 011, Tamil Nadu (India); Raj, V., E-mail: alaguraj2@rediffmail.com [Advanced Materials Research Laboratory, Department of Chemistry, Periyar University, Omalur Main Road, Salem 636 011, Tamil Nadu (India)

    2010-04-01

    Alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres were synthesized by conventional anodization route. Scanning Electron Microscopy (SEM), Atomic Force microscopy (AFM), X-Ray Diffraction (XRD) and Energy Dispersive X-Ray spectroscopy (EDAX) were used to characterize the morphology and crystalloid structure of ASZNC fibres. Current density (DC) is one of the important parameters to get the alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres by this route. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity. The root mean square roughness of the sample observed from atomic force microscopic analysis is about 71.5 nm which is comparable to the average grain size of the coatings which is about 72 nm obtained from X-Ray diffraction. The results indicate that, the ASZNC fibres are arranged well in the nanostructure. The thickness of the coating increased with the anodizing time, but the coatings turned rougher and more porous. At the initial stage the growth of ceramic coating increases inwards to the metal substrate and outwards to the coating surface simultaneously. Subsequently, it mainly grows towards the metal substrate and the density of the ceramic coating increases gradually, which results in the decrease of the total thickness as anodizing time increases. This new approach of preparing ASZNC ceramic fibres may be important in applications ranging from gas sensors to various engineering materials.

  15. Mirror-backed Dark Alumina: A Nearly Perfect Absorber for Thermoelectronics and Thermophotovotaics

    KAUST Repository

    Farhat, Mohamed; Cheng, Tsung-Chieh; Le, Khai. Q.; Cheng, Mark Ming-Cheng; Bagci, Hakan; Chen, Pai-Yen

    2016-01-01

    We present here a broadband, wide-angle, and polarization-independent nearly perfect absorber consisting of mirror-backed nanoporous alumina. By electrochemically anodizing the disordered multicomponent aluminum and properly tailoring the thickness

  16. Probing anodic oxidation kinetics and nanoscale heterogeneity within TiO2 films by Conductive Atomic Force Microscopy and combined techniques

    International Nuclear Information System (INIS)

    Diamanti, M.V.; Souier, T.; Stefancich, M.; Chiesa, M.; Pedeferri, M.P.

    2014-01-01

    Graphical abstract: - Highlights: • Nanoscale anodic titanium oxides were investigated with multidisciplinary approach. • Oxide thickness was estimated via spectrophotometry and coulometry. • C-AFM identified nanometric conductivity heterogeneities, ascribed to oxide structure. • High conductivity areas exhibited local memristive behavior. - Abstract: Anodic oxidation of titanium in acid electrolytes allows to obtain a thin, compact oxide layer with thickness, structure, color, and electrical properties that vary with process parameters imposed, among which cell voltage has a key effect. Although oxidation kinetics have been investigated in several research works, a broader vision of oxide properties–including thickness and structure–still has to be achieved, especially in the case of very thin oxide films, few tens of nanometers thick. This is vital for engineered applications of nanostructured TiO 2 films, as in the field of memristive devices, where a precise control of oxide thickness, composition and structure is required to tune its electrical response. In this work, oxide films were produced on titanium with thickness ranging from few nanometers to 200 nm. Oxide thickness was estimated by coulometry and spectrophotometry. These techniques were then combined with C-AFM, which provided a deeper understanding of oxide thickness and uniformity of the metal surface and probed the presence of crystalline nano-domains within the amorphous oxide phase affecting the overall film electrical and optical properties

  17. Effect of hydrothermal process for inorganic alumina sol on crystal structure of alumina gel

    Directory of Open Access Journals (Sweden)

    K. Yamamura

    2016-09-01

    Full Text Available This paper reports the effect of a hydrothermal process for alumina sol on the crystal structure of alumina gel derived from hydrothermally treated alumina sol to help push forward the development of low temperature synthesis of α-Al2O3. White precipitate of aluminum hydroxide was prepared with a homogeneous precipitation method using aluminum nitrate and urea in aqueous solution. The obtained aluminum hydroxide precipitate was peptized by using acetic acid at room temperature, which resulted in the production of a transparent alumina sol. The alumina sol was treated with a hydrothermal process and transformed into an alumina gel film by drying at room temperature. Crystallization of the alumina gel to α-Al2O3 with 900 °C annealing was dominant for a hydrothermal temperature of 100 °C and a hydrothermal time of 60 min, as production of diaspore-like species was promoted with the hydrothermal temperature and time. Excess treatments with hydrothermal processes at higher hydrothermal temperature for longer hydrothermal time prevented the alumina gel from being crystallized to α-Al2O3 because the excess hydrothermal treatments promoted production of boehmite.

  18. Properties of Sn-doped TiO2 nanotubes fabricated by anodization of co-sputtered Ti–Sn thin films

    International Nuclear Information System (INIS)

    Kyeremateng, Nana Amponsah; Hornebecq, Virginie; Knauth, Philippe; Djenizian, Thierry

    2012-01-01

    Self-organized Sn-doped TiO 2 nanotubes (nts) were fabricated for the first time, by anodization of co-sputtered Ti and Sn thin films. This nanostructured material was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, UV–vis spectroscopy and transmission electron microscopy. Due to their remarkable properties, Sn-doped TiO 2 nts can find potential applications in Li-ion microbatteries, photovoltaics, and catalysis. Particularly, the electrochemical performance as an anode material for Li-ion microbatteries was evaluated in Li test cells. With current density of 70 μA cm −2 (1 C) and cut-off potential of 1 V, Sn-doped TiO 2 nts showed improved performance compared to simple TiO 2 nts, and differential capacity plots revealed that the material undergoes full electrochemical reaction as a Rutile-type TiO 2 .

  19. Electrochemical behavior of anodized AA6063-T6 alloys affected by matrix structures

    International Nuclear Information System (INIS)

    Huang, Yung-Sen; Shih, Teng-Shih; Wu, Chen-En

    2013-01-01

    Highlights: ► Deformation after solution treatment introduced Al matrix to have deformation bands and few Si particles. ► Dislocations remained in the matrix lift up field potential and produce AlOOH oxide in the AAO film. ► The silicon-containing particles were found to trap in the AAO film. ► The silicon particles and the Al(OOH) oxide is significantly to influence the electrochemical behavior of AAO films. - Abstract: AA 6063 alloys were cold-rolled (CR) either before or after solution treatment (S) and then different samples were artificially aged (T6) to obtain different samples (CRST6 and SCRT6). The highest dislocation density was observed in the SCRT6 sample which also showed the lowest particle count among the three samples; ST6, CRST6 and SCRT6. Subsequently, all samples were anodized in a 15 wt% sulfuric acid solution for different time spans to obtain anodic aluminum oxide (AAO) films. The anodized samples were further analyzed with X-ray Photoelectron Spectroscopy (XPS) analysis. We determined that the constituent phases in the AAO film were composed of hydrated amorphous alumina, hydrated oxide (Al(OH) 3 ) and oxyhydroxide (AlOOH) phases together with some silicon-containing particles trapped in the films on all samples. In the electrochemical test, the silicon-containing particles and hydrated Al(OH) 3 oxide that existed at the electrolyte/film (e/f) interface were found to inversely influence the corrosion resistance of the anodized samples.

  20. Growth of superconducting Bi/sub 2/Sr/sub 2/CaCu/sub 2/O/sub 8+//sub x/ films on alumina, silicon, and fused quartz

    International Nuclear Information System (INIS)

    Hung, L.S.; Agostinelli, J.A.; Paz-Pujalt, G.R.; Mir, J.M.

    1988-01-01

    Interactions between superconducting Bi/sub 2/Sr/sub 2/CaCu/sub 2/O/sub 8+//sub x/ films and substrates were investigated by ion backscattering, x-ray diffraction, and four-point probe resistivity measurements. During annealing at temperatures above- 800 /sup 0/C, Bi/sub 2/Sr/sub 2/CaCu/sub 2/ oxide films rapidly reacted with alumina, Si, Si covered with SiO/sub 2/, and quartz, resulting in catastrophic failure. Zr-based barrier layers were used to minimize film-substrate interactions. When a single ZrO/sub 2/ layer was interposed between the superconducting oxide film and the underlying substrate, the Bi/sub 2/Sr/sub 2/CaCu/sub 2/ oxide films showed a large-grained polycrystalline microstructure and exhibited the orthorhombic structure. Films on sapphire showed transitions to the superconducting state beginning near 100 K with zero resistance achieved at 70 K. Films on Si and thermally grown SiO/sub 2/ showed a similar drop in resistance around 95 K, whereas the transition was broad and the zero resistance state was not reached. For films on quartz, high thermal stress caused cracking of the superconducting oxide film. Best results were achieved using a barrier composed of a Zr-Si-O mixed layer underneath ZrO/sub 2/. In this case, the films grown on Si and quartz were uniform and showed the onset to superconductivity at 95 K, attaining zero resistance at 70 K

  1. Study on the fabrication of back surface reflectors in nano-crystalline silicon thin-film solar cells by using random texturing aluminum anodization

    Science.gov (United States)

    Shin, Kang Sik; Jang, Eunseok; Cho, Jun-Sik; Yoo, Jinsu; Park, Joo Hyung; Byungsung, O.

    2015-09-01

    In recent decades, researchers have improved the efficiency of amorphous silicon solar cells in many ways. One of the easiest and most practical methods to improve solar-cell efficiency is adopting a back surface reflector (BSR) as the bottom layer or as the substrate. The BSR reflects the incident light back to the absorber layer in a solar cell, thus elongating the light path and causing the so-called "light trapping effect". The elongation of the light path in certain wavelength ranges can be enhanced with the proper scale of BSR surface structure or morphology. An aluminum substrate with a surface modified by aluminum anodizing is used to improve the optical properties for applications in amorphous silicon solar cells as a BSR in this research due to the high reflectivity and the low material cost. The solar cells with a BSR were formed and analyzed by using the following procedures: First, the surface of the aluminum substrate was degreased by using acetone, ethanol and distilled water, and it was chemically polished in a dilute alkali solution. After the cleaning process, the aluminum surface's morphology was modified by using a controlled anodization in a dilute acid solution to form oxide on the surface. The oxidized film was etched off by using an alkali solution to leave an aluminum surface with randomly-ordered dimple-patterns of approximately one micrometer in size. The anodizing conditions and the anodized aluminum surfaces after the oxide layer had been removed were systematically investigated according to the applied voltage. Finally, amorphous silicon solar cells were deposited on a modified aluminum plate by using dc magnetron sputtering. The surfaces of the anodized aluminum were observed by using field-emission scanning electron microscopy. The total and the diffuse reflectances of the surface-modified aluminum sheets were measured by using UV spectroscopy. We observed that the diffuse reflectances increased with increasing anodizing voltage. The

  2. Hydrothermal fabrication of Ni{sub 3}S{sub 2}/TiO{sub 2} nanotube composite films on Ni anode and application in photoassisted water electrolysis

    Energy Technology Data Exchange (ETDEWEB)

    He, Hongbo; Chen, Aiping, E-mail: apchen@ecust.edu.cn; Lv, Hui; Dong, Haijun; Chang, Ming; Li, Chunzhong

    2013-10-15

    Highlights: •Ni{sub 3}S{sub 2}/TiO{sub 2} nanotube photocatalysts were synthesized on Ni by hydrothermal method. •Structure of Ni{sub 3}S{sub 2} wrapped by TiO{sub 2} nanotubes improves remarkably stability of Ni{sub 3}S{sub 2}. •Ni{sub 3}S{sub 2}/TiO{sub 2} film on Ni has better H{sub 2} production performance than TiO{sub 2}-modified anode. -- Abstract: Nanostructured films of rhombohedral Ni{sub 3}S{sub 2} were hydrothermally synthesized on Ni and TiO{sub 2} nanotube layer, as substrates. A possible mechanism is proposed to explain the formation of rhombohedral Ni{sub 3}S{sub 2} nanostructures. The results of UV–vis spectrophotometric studies indicate that optical absorption spectrum of Ni{sub 3}S{sub 2}/TiO{sub 2} nanotube composites could be extended to the visible region. As-synthesized Ni{sub 3}S{sub 2}/TiO{sub 2} nanotube composite films on Ni substrate had better (by about 40%) hydrogen production performance under the visible light irradiation, in comparison with the Ni anode modified by TiO{sub 2} nanotubes.

  3. Hierarchical porous Co3O4 films with size-adjustable pores as Li ion battery anodes with excellent rate performances

    International Nuclear Information System (INIS)

    Zhao, Guangyu; Xu, Zhanming; Zhang, Li; Sun, Kening

    2013-01-01

    Highlights: •Template-free synthesis of hierarchical porous Co 3 O 4 films on Ni foams. •Hierarchical porous Co 3 O 4 films with size-adjustable pores. •Excellent rate performances (650 mAh g −1 at 30 C) as Li ion battery anodes. -- Abstract: Constructing hierarchical porous structures on the current collectors is an attractive strategy for improving the rate performance of the Li ion battery electrodes. However, preparing hierarchical porous structures normally requires hard or soft templates to create hollows or pores in different sizes. Rigorous preparation conditions are needed to control the size (especially nanosize) and size distribution of the pores obtained by conventional methods. Herein, we describe a template-free two-step synthesis process to prepare hierarchical porous Co 3 O 4 films on Ni foam substrates. In this synthesis process, free-standing mesoporous precursor flakes are deposited on Ni foams by an electrochemical method. Subsequently, the meosporous precursor flake arrays are calcined to obtain hierarchical porous Co 3 O 4 films. More strikingly, the size of the mesopores in the flakes can be adjusted by altering the calcination temperature. The structure and morphology of the samples are characterized by scanning electron microscopy, transmission electron microscopy and Brunauer–Emmett–Teller measurements. The relationship of the in-flake-pore size and the calcinations temperature is proposed here. Electrochemical tests have revealed that the hierarchical porous Co 3 O 4 films demonstrate excellent rate performances (650 mAh g −1 at 30 C) as Li ion battery anodes due to the hierarchical porous structure, which endows fast ion transmission

  4. Synthesis by anodic-spark deposition of Ca- and P-containing films on pure titanium and their biological response

    Energy Technology Data Exchange (ETDEWEB)

    Banakh, Oksana, E-mail: oksana.banakh@he-arc.ch [Haute Ecole Arc Ingénierie (HES-SO), Eplatures-Grise 17, CH-2300 La Chaux-de-Fonds (Switzerland); Journot, Tony; Gay, Pierre-Antoine; Matthey, Joël; Csefalvay, Catherine [Haute Ecole Arc Ingénierie (HES-SO), Eplatures-Grise 17, CH-2300 La Chaux-de-Fonds (Switzerland); Kalinichenko, Oleg [Ukrainian State University of Chemical Technology (SHEI), Gagarin av. 8, Dnepropetrovsk, UA-49005 (Ukraine); Sereda, Olha [Centre Suisse d’Electronique et de Microtechnique (CSEM), Rue Jaquet-Droz 1, CH-2000 Neuchâtel (Switzerland); Moussa, Mira; Durual, Stéphane [Laboratory of Biomaterials, University of Geneva, rue Barthelemy Menn 19, CH-1205 Geneva (Switzerland); Snizhko, Lyubov [Ukrainian State University of Chemical Technology (SHEI), Gagarin av. 8, Dnepropetrovsk, UA-49005 (Ukraine)

    2016-08-15

    Highlights: • ​CP-4 Ti was treated by anodic spark oxidation in the electrolyte containing Ca and P ions by varying process time and electrolyte concentration. • Ca/P ratio in layers is 0.23–0.47, much lower than in hydroxyapatites (1.67). It means coatings should be resorbable in a biological medium • After immersion in SBF, Ca and P content in layers decrease. Ca and P loss occurs faster in thin layers than in thicker coatings. • The biological response of the samples suggests their excellent biocompatibility and even stimulating effects on osteoblasts proliferation. - Abstract: The purpose of this work is to characterize the anodized layers formed on titanium by anodic-spark deposition in an electrolyte containing Ca and P ions, Ca{sub 3}(PO{sub 4}){sub 2}, studied for the first time. The oxidation experiments were performed at different periods of time and using different concentrations of electrolyte. The influence of the process parameters (time of electrolysis and electrolyte concentration) on the surface morphology and chemical composition of the anodized layers was studied. It has been found that it is possible to incorporate Ca and P into the growing layer. A response of the anodized layers in a biological medium was evaluated by their immersion in a simulated body fluid. An enrichment of titanium and a simultaneous loss of calcium and phosphorus in the layer after immersion tests indicate that these coatings should be bioresorbable in a biological medium. Preliminary biological assays were performed on some anodized layers in order to assess their biocompatibility with osteoblast cells. The cell proliferation on one selected anodized sample was assessed up to 21 days after seeding. The preliminary results suggest excellent biocompatibility properties of anodized coatings.

  5. Synthesis by anodic-spark deposition of Ca- and P-containing films on pure titanium and their biological response

    International Nuclear Information System (INIS)

    Banakh, Oksana; Journot, Tony; Gay, Pierre-Antoine; Matthey, Joël; Csefalvay, Catherine; Kalinichenko, Oleg; Sereda, Olha; Moussa, Mira; Durual, Stéphane; Snizhko, Lyubov

    2016-01-01

    Highlights: • ​CP-4 Ti was treated by anodic spark oxidation in the electrolyte containing Ca and P ions by varying process time and electrolyte concentration. • Ca/P ratio in layers is 0.23–0.47, much lower than in hydroxyapatites (1.67). It means coatings should be resorbable in a biological medium • After immersion in SBF, Ca and P content in layers decrease. Ca and P loss occurs faster in thin layers than in thicker coatings. • The biological response of the samples suggests their excellent biocompatibility and even stimulating effects on osteoblasts proliferation. - Abstract: The purpose of this work is to characterize the anodized layers formed on titanium by anodic-spark deposition in an electrolyte containing Ca and P ions, Ca_3(PO_4)_2, studied for the first time. The oxidation experiments were performed at different periods of time and using different concentrations of electrolyte. The influence of the process parameters (time of electrolysis and electrolyte concentration) on the surface morphology and chemical composition of the anodized layers was studied. It has been found that it is possible to incorporate Ca and P into the growing layer. A response of the anodized layers in a biological medium was evaluated by their immersion in a simulated body fluid. An enrichment of titanium and a simultaneous loss of calcium and phosphorus in the layer after immersion tests indicate that these coatings should be bioresorbable in a biological medium. Preliminary biological assays were performed on some anodized layers in order to assess their biocompatibility with osteoblast cells. The cell proliferation on one selected anodized sample was assessed up to 21 days after seeding. The preliminary results suggest excellent biocompatibility properties of anodized coatings.

  6. Thermal stability of alumina thin films containing γ-Al.sub.2./sub.O.sub.3./sub. phase prepared by reactive magnetron sputtering

    Czech Academy of Sciences Publication Activity Database

    Musil, Jindřich; Blažek, J.; Zeman, P.; Prokšová, Š.; Šašek, M.; Čerstvý, R.

    2010-01-01

    Roč. 257, č. 3 (2010), s. 1058-1062 ISSN 0169-4332 Institutional research plan: CEZ:AV0Z10100520 Keywords : Al 2 O 3 (alumina) * annealing * thermal stability * nanocrystalline material * sputtering Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.795, year: 2010

  7. A novel technique for synthesizing dense alumina nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Pancholi, A [Department of Materials Science and Engineering, University of Delaware, Newark, DE 19716 (United States); Stoleru, V G [Department of Materials Science and Engineering, University of Delaware, Newark, DE 19716 (United States); Kell, C D [Department of Chemical Engineering, University of Delaware, Newark, DE 19716 (United States)

    2007-05-30

    The formation of highly ordered nanoporous alumina membranes by anodizing high-purity aluminium under optimum conditions (i.e., anodization time, electrolyte temperature, and cell voltage) in various electrolyte solutions is a well established process. In this paper we report on the formation of a wide range of alumina nanostructures, including nanotubes/nanochannels, nanoplates, and nanofibres, by using a technique that involves anodization and etching processing steps similar to the ones that yield nanopores, under slightly modified experimental conditions. The effects of the anodization voltage, time, and temperature, as well as the effects of the etching time, on the formation and the properties of the alumina nanostructures are analysed. We propose a simple analytical model to describe the formation of different types of alumina nanostructures, as a result of irreversible breakage of the pore walls for long etching times. The geometry of the nanostructures and their dimensions, ranging between 10 and 100 nm, were found to be dependent on the pore dimensions and on the location of the cleavage/breakage of the pore walls.

  8. Dewetting of polymer thin films on modified curved surfaces: preparation of polymer nanoparticles with asymmetric shapes by anodic aluminum oxide templates.

    Science.gov (United States)

    Liu, Chih-Ting; Tsai, Chia-Chan; Chu, Chien-Wei; Chi, Mu-Huan; Chung, Pei-Yun; Chen, Jiun-Tai

    2018-04-18

    We study the dewetting behaviors of poly(methyl methacrylate) (PMMA) thin films coated in the cylindrical nanopores of anodic aluminum oxide (AAO) templates by thermal annealing. Self-assembled monolayers (SAMs) of n-octadecyltrichlorosilane (ODTS) are introduced to modify the pore surfaces of the AAO templates to induce the dewetting process. By using scanning electron microscopy (SEM), the dewetting-induced morphology transformation from the PMMA thin films to PMMA nanoparticles with asymmetric shapes can be observed. The sizes of the PMMA nanoparticles can be controlled by the original PMMA solution concentrations. The dewetting phenomena on the modified nanopores are explained by taking into account the excess intermolecular interaction free energy (ΔG). This work opens a new possibility for creating polymer nanoparticles with asymmetric shapes in confined geometries.

  9. Enhanced Absorption in Organic Thin-Films from Imprinted Concave Nanostructures

    Directory of Open Access Journals (Sweden)

    Arkadiusz Jarosław GOSZCZAK

    2017-02-01

    Full Text Available In this work, a rapid, replicable method for imprinting concave nanostructures to be used as functional light-trapping nanostructures in organic thin-films is presented. Porous anodic alumina templates were fabricated both by anodization of thick Al foils and by anodization of submicrometer thin Al films evaporated via e-beam evaporation on Si substrates. The template formation leads to natural patterning of the underlying Al layers that are used as rigid masters for stamp fabrication, after selective etching of the porous anodic alumina. PDMS stamps were made after replicating the Al concave patterns and used for imprinting of spin coated photoresist on glass substrates. We have investigated semi-periodic and aperiodic imprinted large concave patterns fabricated from rigid masters after anodization of Al in H3PO4. We show that metal covered imprinted concaves show enhancement in absorption that is attributed to field enhancement and diffuse scattering, leading to efficient light trapping for a selected active layer material (P3HT:PCBM.DOI: http://dx.doi.org/10.5755/j01.ms.23.1.14188

  10. Significant room-temperature ferromagnetism in porous ZnO films: The role of oxygen vacancies

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Xue; Liu, Huiyuan [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China); Sun, Huiyuan, E-mail: huiyuansun@126.com [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China); Liu, Lihu; Jia, Xiaoxuan [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China)

    2015-10-15

    Graphical abstract: - Highlights: • Porous ZnO films were deposited on porous anodic alumina substrates. • Significant ferromagnetism (FM) has been observed in porous ZnO films (110 emu/cm{sup 3}). • The strong magnetic anisotropy was observed in the porous ZnO films. • The origin of FM is attributed to the oxygen vacancy with a local magnetic moment. - Abstract: Pure porous ZnO films were prepared by direct current reactive magnetron sputtering on porous anodic alumina substrates. Remarkably large room-temperature ferromagnetism was observed in the films. The highest saturation moment along the out-of-plane direction was about 110 emu/cm{sup 3}. Experimental and theoretical results suggested that the oxygen vacancies and the unique porous structure of the films are responsible for the large ferromagnetism. There are two modes of coupling between oxygen vacancies in the porous ZnO films: (i) exchange interactions directly between the oxygen vacancies and (ii) with the mediation of conduction electrons. In addition, it was found that the magnetic moment of ZnO films can be changed by tuning the concentration of oxygen vacancies. These observations may be useful in the development of ZnO-based spintronics devices.

  11. Honeycomb-inspired design of ultrafine SnO2@C nanospheres embedded in carbon film as anode materials for high performance lithium- and sodium-ion battery

    Science.gov (United States)

    Ao, Xiang; Jiang, Jianjun; Ruan, Yunjun; Li, Zhishan; Zhang, Yi; Sun, Jianwu; Wang, Chundong

    2017-08-01

    Tin oxide (SnO2) has been considered as one of the most promising anodes for advanced rechargeable batteries due to its advantages such as high energy density, earth abundance and environmental friendly. However, its large volume change during the Li-Sn/Na-Sn alloying and de-alloying processes will result in a fast capacity degradation over a long term cycling. To solve this issue, in this work we design and synthesize a novel honeycomb-like composite composing of carbon encapsulated SnO2 nanospheres embedded in carbon film by using dual templates of SiO2 and NaCl. Using these composites as anodes both in lithium ion batteries and sodium-ion batteries, no discernable capacity degradation is observed over hundreds of long term cycles at both low current density (100 mA g-1) and high current density (500 mA g-1). Such a good cyclic stability and high delivered capacity have been attributed to the high conductivity of the supported carbon film and hollow encapsulated carbon shells, which not only provide enough space to accommodate the volume expansion but also prevent further aggregation of SnO2 nanoparticles upon cycling. By engineering electrodes of accommodating high volume expansion, we demonstrate a prototype to achieve high performance batteries, especially high-power batteries.

  12. Core-shell Si/C nanospheres embedded in bubble sheet-like carbon film with enhanced performance as lithium ion battery anodes.

    Science.gov (United States)

    Li, Wenyue; Tang, Yongbing; Kang, Wenpei; Zhang, Zhenyu; Yang, Xia; Zhu, Yu; Zhang, Wenjun; Lee, Chun-Sing

    2015-03-18

    Due to its high theoretical capacity and low lithium insertion voltage plateau, silicon has been considered one of the most promising anodes for high energy and high power density lithium ion batteries (LIBs). However, its rapid capacity degradation, mainly caused by huge volume changes during lithium insertion/extraction processes, remains a significant challenge to its practical application. Engineering Si anodes with abundant free spaces and stabilizing them by incorporating carbon materials has been found to be effective to address the above problems. Using sodium chloride (NaCl) as a template, bubble sheet-like carbon film supported core-shell Si/C composites are prepared for the first time by a facile magnesium thermal reduction/glucose carbonization process. The capacity retention achieves up to 93.6% (about 1018 mAh g(-1)) after 200 cycles at 1 A g(-1). The good performance is attributed to synergistic effects of the conductive carbon film and the hollow structure of the core-shell nanospheres, which provide an ideal conductive matrix and buffer spaces for respectively electron transfer and Si expansion during lithiation process. This unique structure decreases the charge transfer resistance and suppresses the cracking/pulverization of Si, leading to the enhanced cycling performance of bubble sheet-like composite. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Tribological and stability investigations of alkylphosphonic acids on alumina surface

    International Nuclear Information System (INIS)

    Cichomski, M.; Kośla, K.; Grobelny, J.; Kozłowski, W.; Szmaja, W.

    2013-01-01

    Alumina substrates are commonly used for various micro-/nanoelectromechanical systems (MEMS/NEMS). For efficient and lifetime longevity of these devices, lubricant films of self-assembled monolayers (SAMs) with nanometer thickness are increasingly being employed. In the present paper, we report preparation, tribological and stability investigations of alkylphosphonic acids on the alumina surface. The alkylphosphonic acids were prepared on the alumina surface using the liquid phase deposition method. The effectiveness of modification of the alumina surface by alkylphosphonic acids was investigated using water contact angle measurements, secondary ion mass spectrometry, X-ray photoelectron and infrared spectroscopy. Frictional behavior in milinewton load range was studied by microtribometry. It is shown that surface modification of the alumina surface by alkylphosphonic acids reduces the coefficient of friction values compared to the unmodified alumina. In comparison to the non-modified alumina surface, all tested alkylphosphonic acids cause a decrease in the friction coefficients in friction tests for counterparts made from different materials, such as steel, zirconia and silicon nitride. It is also found that the alumina surface modified by alkylphosphonic acids with longer chain has a higher degree of hydrophobicity and lower coefficient of friction. The best frictional properties are obtained for the system consisting of the alumina surface modified by n-octadecylphosphonic acid and silicon nitride counterpart. Stability tests in different environmental conditions: laboratory, acidic and alkaline solutions were also monitored.

  14. A transmission electron microscopy and X-ray photoelectron spectroscopy study of annealing induced γ-phase nucleation, clustering, and interfacial dynamics in reactively sputtered amorphous alumina thin films

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, A. K. Nanda, E-mail: aknk27@yahoo.com; Subramanian, B. [ECMS Division, Central Electro Chemical Research Institute, Karaikudi (India); Prasanna, S. [Department of Physics, PSG College of Technology, Coimbatore (India); Jayakumar, S. [Department of Physics, PSG Institute of Technology and Applied Research, Coimbatore (India); Rao, G. Mohan [Department of Instrumentation, Indian Institute of Science, Bangalore (India)

    2015-03-28

    Pure α-Al{sub 2}O{sub 3} exhibits a very high degree of thermodynamical stability among all metal oxides and forms an inert oxide scale in a range of structural alloys at high temperatures. We report that amorphous Al{sub 2}O{sub 3} thin films sputter deposited over crystalline Si instead show a surprisingly active interface. On annealing, crystallization begins with nuclei of a phase closely resembling γ-Alumina forming almost randomly in an amorphous matrix, and with increasing frequency near the substrate/film interface. This nucleation is marked by the signature appearance of sharp (400) and (440) reflections and the formation of a diffuse diffraction halo with an outer maximal radius of ≈0.23 nm enveloping the direct beam. The microstructure then evolves by a cluster-coalescence growth mechanism suggestive of swift nucleation and sluggish diffusional kinetics, while locally the Al ions redistribute slowly from chemisorbed and tetrahedral sites to higher anion coordinated sites. Chemical state plots constructed from XPS data and simple calculations of the diffraction patterns from hypothetically distorted lattices suggest that the true origins of the diffuse diffraction halo are probably related to a complex change in the electronic structure spurred by the a-γ transformation rather than pure structural disorder. Concurrent to crystallization within the film, a substantially thick interfacial reaction zone also builds up at the film/substrate interface with the excess Al acting as a cationic source.

  15. A transmission electron microscopy and X-ray photoelectron spectroscopy study of annealing induced γ-phase nucleation, clustering, and interfacial dynamics in reactively sputtered amorphous alumina thin films

    Science.gov (United States)

    Kumar, A. K. Nanda; Prasanna, S.; Subramanian, B.; Jayakumar, S.; Rao, G. Mohan

    2015-03-01

    Pure α-Al2O3 exhibits a very high degree of thermodynamical stability among all metal oxides and forms an inert oxide scale in a range of structural alloys at high temperatures. We report that amorphous Al2O3 thin films sputter deposited over crystalline Si instead show a surprisingly active interface. On annealing, crystallization begins with nuclei of a phase closely resembling γ-Alumina forming almost randomly in an amorphous matrix, and with increasing frequency near the substrate/film interface. This nucleation is marked by the signature appearance of sharp (400) and (440) reflections and the formation of a diffuse diffraction halo with an outer maximal radius of ≈0.23 nm enveloping the direct beam. The microstructure then evolves by a cluster-coalescence growth mechanism suggestive of swift nucleation and sluggish diffusional kinetics, while locally the Al ions redistribute slowly from chemisorbed and tetrahedral sites to higher anion coordinated sites. Chemical state plots constructed from XPS data and simple calculations of the diffraction patterns from hypothetically distorted lattices suggest that the true origins of the diffuse diffraction halo are probably related to a complex change in the electronic structure spurred by the a-γ transformation rather than pure structural disorder. Concurrent to crystallization within the film, a substantially thick interfacial reaction zone also builds up at the film/substrate interface with the excess Al acting as a cationic source.

  16. A transmission electron microscopy and X-ray photoelectron spectroscopy study of annealing induced γ-phase nucleation, clustering, and interfacial dynamics in reactively sputtered amorphous alumina thin films

    International Nuclear Information System (INIS)

    Kumar, A. K. Nanda; Subramanian, B.; Prasanna, S.; Jayakumar, S.; Rao, G. Mohan

    2015-01-01

    Pure α-Al 2 O 3 exhibits a very high degree of thermodynamical stability among all metal oxides and forms an inert oxide scale in a range of structural alloys at high temperatures. We report that amorphous Al 2 O 3 thin films sputter deposited over crystalline Si instead show a surprisingly active interface. On annealing, crystallization begins with nuclei of a phase closely resembling γ-Alumina forming almost randomly in an amorphous matrix, and with increasing frequency near the substrate/film interface. This nucleation is marked by the signature appearance of sharp (400) and (440) reflections and the formation of a diffuse diffraction halo with an outer maximal radius of ≈0.23 nm enveloping the direct beam. The microstructure then evolves by a cluster-coalescence growth mechanism suggestive of swift nucleation and sluggish diffusional kinetics, while locally the Al ions redistribute slowly from chemisorbed and tetrahedral sites to higher anion coordinated sites. Chemical state plots constructed from XPS data and simple calculations of the diffraction patterns from hypothetically distorted lattices suggest that the true origins of the diffuse diffraction halo are probably related to a complex change in the electronic structure spurred by the a-γ transformation rather than pure structural disorder. Concurrent to crystallization within the film, a substantially thick interfacial reaction zone also builds up at the film/substrate interface with the excess Al acting as a cationic source

  17. Thin Film Microbatteries

    International Nuclear Information System (INIS)

    Dudney, Nancy J.

    2008-01-01

    aerosol spray coating, for one or more components of the battery. The active materials used for the thin film cathodes and anodes are familiar intercalation compounds, but the microstructures and often the cycling properties of the thin films may be quite distinct from those of battery electrodes formed from powders. The thin film cathodes are dense and homogeneous with no added phases such as binders or electrolytes. When deposited at ambient temperatures, the films of cathodes, such as LiCoO 2 , V 2 O 5 , LiMn 2 O4 , LiFePO 4 are amorphous or nanocrystalline. But even in this form, they often act as excellent cathodes with large specific capacities and good stability for hundreds to thousands of cycles. Annealing the cathode films at temperatures of 300 to 800 C may be used to induce crystallization and grain growth of the desired intercalation compound. Crystallizing the cathode film generally improves the Li chemical diffusivity in the electrode material, and hence the power delivered by the battery, by 1-2 orders of magnitude. The microstructure is also tailored by the deposition and heat treatment. Figure 3 shows a fracture edge of an annealed LiCoO 2 cathode film on an alumina substrate. The columnar microstructure, which is typical of a vapor deposited film, sinters at high temperatures leaving small fissures between the dense columns. Such crystalline films also may have a preferred crystallographic orientation. For LiCoO 2 films the crystallographic texture differs for films deposited by sputtering versus pulse laser ablation processes. To improve the manufacturability of the thin film batteries, it would be beneficial to eliminate or minimize the temperature or duration of the annealing step. Several efforts have lead to low temperature fabrication of thin film batteries on polyimide substrates, but the battery capacity and rate are lower than those treated at high temperatures. For the battery anode, many designs use a vapor-deposited metallic lithium film as

  18. Characterization and corrosion resistance of anodic electrodeposited titanium oxide/phosphate films on Ti-20Nb-10Zr-5Ta bioalloy

    Energy Technology Data Exchange (ETDEWEB)

    Popa, Monica; Vasilescu, Cora; Drob, Silviu I.; Osiceanu, Petre; Anastasescu, Mihai; Calderon-Moreno, Jose M., E-mail: josecalderonmoreno@yahoo.com [Institute of Physical Chemistry ' Ilie Murgulescu' of the Romanian Academy, Bucharest (Romania)

    2013-07-15

    In this work, the anodic galvanostatic electrodeposition of an oxidation film containing phosphates on Ti-20Nb-10Zr-5Ta alloy from orthophosphoric acid solution is presented. Its composition was determined by X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman micro-spectroscopy, and its topography by atomic force microscopy (AFM). The corrosion resistance of the coated alloy in simulated human fluid (by linear polarization method and monitoring of open circuit potentials, corresponding open circuit potential gradients) as well as the characterization of the coating (by Raman spectroscopy and depth profile X-ray photoelectron spectroscopy (XPS)) deposited in a period of 300 h soaking in simulated human body fluid were studied. The electrodeposited film was composed of amorphous titanium dioxide and contained phosphate groups. The corrosion resistance of the coated Ti-20Nb-10Zr-5Ta alloy in neutral and alkaline Ringer's solutions was higher than that of the bare alloy due to the protective properties of the electrodeposited film. The corrosion parameters improved over time as result of the thickening of the surface film by the deposition from the physiological solution. The deposited coating presented a variable composition in depth: at the deeper layer nucleated nanocrystalline hydroxyapatite and at the outer layer amorphous calcium phosphate. (author)

  19. Characterization and corrosion resistance of anodic electrodeposited titanium oxide/phosphate films on Ti-20Nb-10Zr-5Ta bioalloy

    International Nuclear Information System (INIS)

    Popa, Monica; Vasilescu, Cora; Drob, Silviu I.; Osiceanu, Petre; Anastasescu, Mihai; Calderon-Moreno, Jose M.

    2013-01-01

    In this work, the anodic galvanostatic electrodeposition of an oxidation film containing phosphates on Ti-20Nb-10Zr-5Ta alloy from orthophosphoric acid solution is presented. Its composition was determined by X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman micro-spectroscopy, and its topography by atomic force microscopy (AFM). The corrosion resistance of the coated alloy in simulated human fluid (by linear polarization method and monitoring of open circuit potentials, corresponding open circuit potential gradients) as well as the characterization of the coating (by Raman spectroscopy and depth profile X-ray photoelectron spectroscopy (XPS)) deposited in a period of 300 h soaking in simulated human body fluid were studied. The electrodeposited film was composed of amorphous titanium dioxide and contained phosphate groups. The corrosion resistance of the coated Ti-20Nb-10Zr-5Ta alloy in neutral and alkaline Ringer's solutions was higher than that of the bare alloy due to the protective properties of the electrodeposited film. The corrosion parameters improved over time as result of the thickening of the surface film by the deposition from the physiological solution. The deposited coating presented a variable composition in depth: at the deeper layer nucleated nanocrystalline hydroxyapatite and at the outer layer amorphous calcium phosphate. (author)

  20. Flexible free-standing TiO2/graphene/PVdF films as anode materials for lithium-ion batteries

    International Nuclear Information System (INIS)

    Ren, H.M.; Ding, Y.H.; Chang, F.H.; He, X.; Feng, J.Q.; Wang, C.F.; Jiang, Y.; Zhang, P.

    2012-01-01

    Highlights: ► Flexible TiO 2 /graphene electrode was prepared by a solvent evaporation technique. ► PVdF was used as substance to support the TiO 2 /graphene active materials. ► The flexible films can be employed as anode materials for Li-ion battery. - Abstract: Graphene composites were prepared by hydrothermal method using titanium dioxide (TiO 2 ) adsorbed graphene oxide (GO) sheets as precursors. Free-standing hybrid films for lithium-ion batteries were prepared by adding TiO 2 /graphene composites to the polyvinylidene fluoride (PVdF)/N-methyl-2-pyrrolidone (NMP) solution, followed by a solvent evaporation technique. These films were characterized by atomic force microscopy (AFM), X-ray diffraction (XRD), scanning electron microscopy (SEM) and various electrochemical techniques. Flexible films show an excellent cycling performance, which was attributed to the interconnected graphene conducting network, which depressed the increasing of electric resistance during the cycling.

  1. Reuse of activated alumina

    Energy Technology Data Exchange (ETDEWEB)

    Hobensack, J.E. [Martin Marietta Energy Systems, Inc., Piketon, OH (United States)

    1991-12-31

    Activated alumina is used as a trapping media to remove trace quantities of UF{sub 6} from process vent streams. The current uranium recovery method employs concentrated nitric acid which destroys the alumina pellets and forms a sludge which is a storage and disposal problem. A recently developed technique using a distilled water rinse followed by three dilute acid rinses removes on average 97% of the uranium, and leaves the pellets intact with crush strength and surface area values comparable with new material. Trapping tests confirm the effectiveness of the recycled alumina as UF{sub 6} trapping media.

  2. Anodic self-organized transparent nanotubular/porous hematite films from Fe thin-films sputtered on FTO and photoelectrochemical water splitting

    Czech Academy of Sciences Publication Activity Database

    Wang, L.; Lee, C.-Y.; Kirchgeorg, R.; Liu, N.; Lee, K.; Kment, Š.; Hubička, Zdeněk; Krýsa, J.; Olejníček, J.; Čada, M.; Zbořil, R.; Schmuki, P.

    2015-01-01

    Roč. 41, č. 12 (2015), s. 9333-9341 ISSN 0922-6168. [Pannonian Symposium on Catalysis /12./. Třešť, 16.09.2014-20.09.2014] Institutional support: RVO:68378271 Keywords : hematite * nanotubular * anodization * magnetron * sputtering * water splitting Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 1.833, year: 2015

  3. Investigation of in-pile formed corrosion films on zircaloy fuel-rod claddings by impedance spectroscopy and galvanostatic anodization

    International Nuclear Information System (INIS)

    Gebhardt, O.

    1993-01-01

    Hot-cell investigations have been executed to study the corrosion behaviour of irradiated Zircaloy fuel-rod claddings by impedance spectroscopy and galvanostatic anodization. The thickness of the compact oxide at the metal/oxide interface and the thickness of the minimum barrier oxide have been determined at different positions along the claddings. As shown by analysis, both quantities first increase and then decrease with increasing thickness of the total oxide. (author) 6 figs., 33 refs

  4. Electrochemical heterogeneity and chemical stability of anodic oxide films of barrier type on certain valve metals and alloys

    International Nuclear Information System (INIS)

    Isaev, N.I.; Yakovlev, V.B.

    1986-01-01

    Direct current and alternating current electrochemical methods are used to study kinetic regularities and mechanism of titanium films dissolution in NaOH and H 2 SO 4 concentrated solutions. Piece-line dependence of oxidized electrode specific reverse capacitance on the time of C c -1 =α i -β i τ type is stated. Effective activation energy and dissolution reaction apparent order are determined by agressive ions. For amorphous alloys films interrelation of structure heterogeneity, film composition and resistance to pitting corrosion is shown. Decrease of oxide protecting properties is due to crystallization of originally amorphous films

  5. Combined micro-droplet and thin-film-assisted pre-concentration of lead traces for on-line monitoring using anodic stripping voltammetry.

    Science.gov (United States)

    Belostotsky, Inessa; Gridin, Vladimir V; Schechter, Israel; Yarnitzky, Chaim N

    2003-02-01

    An improved analytical method for airborne lead traces is reported. It is based on using a Venturi scrubber sampling device for simultaneous thin-film stripping and droplet entrapment of aerosol influxes. At least threefold enhancement of the lead-trace pre-concentration is achieved. The sampled traces are analyzed by square-wave anodic stripping voltammetry. The method was tested by a series of pilot experiments. These were performed using contaminant-controlled air intakes. Reproducible calibration plots were obtained. The data were validated by traditional analysis using filter sampling. LODs are comparable with the conventional techniques. The method was successfully applied to on-line and in situ environmental monitoring of lead.

  6. Combined micro-droplet and thin-film-assisted pre-concentration of lead traces for on-line monitoring using anodic stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Belostotsky, Inessa; Gridin, Vladimir V.; Schechter, Israel; Yarnitzky, Chaim N. [Department of Chemistry, Technion Israel Institute of Technology, 32000, Haifa (Israel)

    2003-02-01

    An improved analytical method for airborne lead traces is reported. It is based on using a Venturi scrubber sampling device for simultaneous thin-film stripping and droplet entrapment of aerosol influxes. At least threefold enhancement of the lead-trace pre-concentration is achieved. The sampled traces are analyzed by square-wave anodic stripping voltammetry. The method was tested by a series of pilot experiments. These were performed using contaminant-controlled air intakes. Reproducible calibration plots were obtained. The data were validated by traditional analysis using filter sampling. LODs are comparable with the conventional techniques. The method was successfully applied to on-line and in situ environmental monitoring of lead. (orig.)

  7. To the problem on formation kinetics of absorption and polylayer films in anodic oxidation of cadmium in alkali hydroxides. Kinetics of irreversible absorption of oxide

    International Nuclear Information System (INIS)

    Grachev, D.K.

    1978-01-01

    An attempt is made to substantiate the formation of adsorption and polylayer films on cadmium electrode during its oxidation in KOH diluted solutions based on the interpretation of data from methods of the potential control. Using relaxation methods (voltammetry and chronoammetry) the conditions were determined at which irreversible abd sorption kinetics of the passivating oxide turns out to dominate the anodic dissolution process in the KOH 1-0.1 N solutions. Parts of monolayer and polylayer surface filling are shown. Kinetics of monolayer oxide growth is interpreted based on the Temkin-Zeldovich type equation for irreversible adsorption process. Ways of the kinetic equation precision are discussed for its full correspondence with the experiment obtained

  8. Low-temperature preparation of crystalline nanoporous TiO2 films by surfactant-assisted anodic electrodeposition

    Czech Academy of Sciences Publication Activity Database

    Wessels, K.; Feldhoff, A.; Wark, M.; Rathouský, Jiří; Oekermann, T.

    2006-01-01

    Roč. 9, č. 6 (2006), C93-C96 ISSN 1099-0062 Institutional research plan: CEZ:AV0Z40400503 Keywords : thin films * cathodic electrodeposition * phase-stability * ZnO films Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.009, year: 2006

  9. Unexpected large room-temperature ferromagnetism in porous Cu{sub 2}O thin films

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Xue [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China); Sun, Huiyuan, E-mail: huiyuansun@126.com [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China); Liu, Lihu; Jia, Xiaoxuan; Liu, Huiyuan [College of Physics Science & Information Engineering, Hebei Normal University, Shijiazhuang 050024 (China); Key Laboratory of Advanced Films of Hebei Province, Shijiazhuang 050024 (China)

    2015-05-15

    Porous Cu{sub 2}O films have been fabricated on porous anodic alumina substrates using DC-reactive magnetron sputtering with pure Cu targets, and unexpectedly large room temperature ferromagnetism has been observed in the films. The maximum saturation magnetic moment along the out-of-plane direction was as high as 94 emu/cm{sup 3}. Photoluminescence spectra show that the ferromagnetism originates with oxygen vacancies. The ferromagnetism could be adjusted by changing the concentration of oxygen vacancies through annealing in an oxygen atmosphere. These observations suggest that the origin of the ferromagnetism is due to coupling between oxygen vacancies with local magnetic moments in the porous Cu{sub 2}O films, which can occur either directly through exchange interactions between oxygen vacancies, or through the mediation of conduction electrons. Such a ferromagnet without the presence of any ferromagnetic dopant may find applications in spintronic devices. - Highlights: • Porous Cu{sub 2}O films were deposited on porous anodic alumina (PAA) substrates. • Significant room-temperature ferromagnetism has been observed in porous Cu{sub 2}O films. • Ferromagnetism of Cu{sub 2}O films exhibited different magnetic signals with the field. • The saturation magnetization is 94 emu/cm{sup 3} with an out-of-plane.

  10. Gradient and alternating diameter nanopore templates by focused ion beam guided anodization

    International Nuclear Information System (INIS)

    Chen Bo; Lu, Kathy; Tian Zhipeng

    2010-01-01

    Ordered arrays of anodic alumina nanopores with uniform pore diameters have been fabricated by self-organized anodization of aluminum. However, gradient or alternating diameter nanopore arrays with designed interpore distances have not been possible. In this study, focused ion beam lithography is used to fabricate hexagonally arranged concaves with different diameters in designed arrangements on aluminum surfaces. The patterns are then used to guide the further growth of alumina nanopores in the subsequent oxalic acid anodization. Gradient and alternating nanopore arrangements have been attained by FIB patterning guided oxalic acid anodization. The fundamental understanding of the process is discussed.

  11. Alumina Concentration Detection Based on the Kernel Extreme Learning Machine.

    Science.gov (United States)

    Zhang, Sen; Zhang, Tao; Yin, Yixin; Xiao, Wendong

    2017-09-01

    The concentration of alumina in the electrolyte is of great significance during the production of aluminum. The amount of the alumina concentration may lead to unbalanced material distribution and low production efficiency and affect the stability of the aluminum reduction cell and current efficiency. The existing methods cannot meet the needs for online measurement because industrial aluminum electrolysis has the characteristics of high temperature, strong magnetic field, coupled parameters, and high nonlinearity. Currently, there are no sensors or equipment that can detect the alumina concentration on line. Most companies acquire the alumina concentration from the electrolyte samples which are analyzed through an X-ray fluorescence spectrometer. To solve the problem, the paper proposes a soft sensing model based on a kernel extreme learning machine algorithm that takes the kernel function into the extreme learning machine. K-fold cross validation is used to estimate the generalization error. The proposed soft sensing algorithm can detect alumina concentration by the electrical signals such as voltages and currents of the anode rods. The predicted results show that the proposed approach can give more accurate estimations of alumina concentration with faster learning speed compared with the other methods such as the basic ELM, BP, and SVM.

  12. Antibacterial activity of zinc oxide-coated nanoporous alumina

    Energy Technology Data Exchange (ETDEWEB)

    Skoog, S.A. [Joint Department of Biomedical Engineering, University of North Carolina and North Carolina State University, Box 7115, Raleigh, NC 27695-7115 (United States); Bayati, M.R. [Department of Materials Science and Engineering, North Carolina State University, Box 7907, Raleigh, NC 27695-7907 (United States); Petrochenko, P.E. [Joint Department of Biomedical Engineering, University of North Carolina and North Carolina State University, Box 7115, Raleigh, NC 27695-7115 (United States); Division of Biology, Office of Science and Engineering Laboratories, Center for Devices and Radiological Health, U.S. Food and Drug Administration, Silver Spring, MD 20993 (United States); Stafslien, S.; Daniels, J.; Cilz, N. [Center for Nanoscale Science and Engineering, North Dakota State University, 1805 Research Park Drive, Fargo, ND 58102 (United States); Comstock, D.J.; Elam, J.W. [Energy Systems Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Narayan, R.J., E-mail: roger_narayan@msn.com [Joint Department of Biomedical Engineering, University of North Carolina and North Carolina State University, Box 7115, Raleigh, NC 27695-7115 (United States); Department of Materials Science and Engineering, North Carolina State University, Box 7907, Raleigh, NC 27695-7907 (United States)

    2012-07-25

    Highlights: Black-Right-Pointing-Pointer Atomic layer deposition was used to deposit ZnO on nanoporous alumina membranes. Black-Right-Pointing-Pointer Scanning electron microscopy showed continuous coatings of zinc oxide nanocrystals. Black-Right-Pointing-Pointer Activity against B. subtilis, E. coli, S. aureus, and S. epidermidis was shown. - Abstract: Nanoporous alumina membranes, also known as anodized aluminum oxide membranes, are being investigated for use in treatment of burn injuries and other skin wounds. In this study, atomic layer deposition was used for coating the surfaces of nanoporous alumina membranes with zinc oxide. Agar diffusion assays were used to show activity of zinc oxide-coated nanoporous alumina membranes against several bacteria found on the skin surface, including Bacillus subtilis, Escherichia coli, Staphylococcus aureus, and Staphylococcus epidermidis. On the other hand, zinc oxide-coated nanoporous alumina membranes did not show activity against Pseudomonas aeruginosa, Enterococcus faecalis, and Candida albicans. These results suggest that zinc oxide-coated nanoporous alumina membranes have activity against some Gram-positive and Gram-negative bacteria that are associated with skin colonization and skin infection.

  13. Preparation of Ni-Fe bimetallic porous anode support for solid oxide fuel cells using LaGaO{sub 3} based electrolyte film with high power density

    Energy Technology Data Exchange (ETDEWEB)

    Ju, Young-Wan; Ida, Shintaro; Ishihara, Tatsumi [Department of Applied Chemistry, Faculty of Engineering, Kyushu University, Motooka 744, Nishi-Ku, Fukuoka 819-0395 (Japan); Eto, Hiroyuki [Mitsubishi Materials Corporation, Central Research Institute, 1002-14 Mukohyama, Naka-Shi, Ibaraki 311-0102 (Japan); Inagaki, Toru [The Kansai Electric Power Co., Inc., 11-20 Nakoji 3-Chome, Amagasaki, Hyogo 661-0974 (Japan)

    2010-10-01

    Optimization of sintering temperature for NiO-Fe{sub 2}O{sub 3} composite oxide substrate was studied in order to obtain a dense substrate with smooth surface. By in situ reduction, the substrate was changed to a porous Ni-Fe alloy metal. The volumetric shrinkage and porosity of the substrate were also studied systematically with the Ni-Fe substrate reduced at different temperatures. A Sr and Mg-doped LaGaO{sub 3} (LSGM) thin film was prepared on dense substrate by the pulsed laser deposition (PLD) method. The LSGM film with stoichiometric composition was successfully prepared under optimal deposition parameters and a target composition. Sm{sub 0.5}Sr{sub 0.5}CoO{sub 3} (SSC55) cathode was prepared by the slurry coating method on the deposited film. Prepared SOFC single cell shows high power density and the maximum power density (MPD) achieved was 1.79, 0.82 and 0.29 W cm{sup -2} at 973, 873 and 773 K, respectively. After thermal cycle from 973 to 298 K, the cell shows almost theoretical open circuit potential (1.1 V) and the power density of 1.62 W cm{sup -2}, which is almost the same as that at first cycles. Therefore, the Ni-Fe porous metal support made by the selective reduction is highly promising as a metal anode substrate for SOFC using LaGaO{sub 3} thin film. (author)

  14. Anodization of aluminium thin films on p{sup ++}Si and annihilation of strong luminescence from Al{sub 2}O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Efeoglu, Hasan, E-mail: hefeoglu@atauni.edu.t [Atatuerk University, Faculty of Engineering, Department of Electrical and Electronics Engineering, 25240 Erzurum (Turkey); Karacali, Tevhit [Atatuerk University, Faculty of Engineering, Department of Electrical and Electronics Engineering, 25240 Erzurum (Turkey); Meral, Kadem; Erdogan, Ibrahim Y.; Onganer, Yavuz [Atatuerk University, Faculty of Sciences, Department of Chemistry, 25240 Erzurum (Turkey)

    2010-01-15

    Photoluminescence (PL) of Al{sub 2}O{sub 3} films obtained by anodization of thermally evaporated and annealed thin Al films on p{sup ++}Si in 0.3 M oxalic acid has been investigated. Thermal annealing at 200-950 deg. C under the dry nitrogen atmosphere was used for deactivation of luminescence centres. Luminescence from as grown films was broad and located at 425 nm. This luminescence reached to highest level after annealing at 600 deg. C. Maximum 10 min was required for full optical activation and prolonged annealing up to 4 h did not change the luminescence intensity. Because of deep levels, absorption band edge of as grown films was shifted to the lower energy which is 3.25 eV. Annealing above 800 deg. C reduced the PL intensity and this observation was correlated with the blue shift of band edge as the defects annealed out. Disappearing PL intensity and blue shift of band edge absorption after annealing at 950 deg. C was mainly attributed to the oxygen-related defects and partly to impurities that may be originated from oxalic acid. AFM results did not show any hexagonally ordered holes but uniformly distributed nanosized Al{sub 2}O{sub 3} clusters that were clearly seen. XRD measurements on as grown Al{sub 2}O{sub 3} showed only [1 1 0] direction of alpha phase. Debye-Scherer calculation for this line indicates that cluster size is 35.7 nm. XRD and AFM pictures suggest that nanocrystalline Al{sub 2}O{sub 3} are embedded in amorphous Al{sub 2}O{sub 3}.

  15. Controlling the anodizing conditions in preparation of an nanoporous anodic aluminium oxide template

    Science.gov (United States)

    Nazemi, Azadeh; Abolfazl, Seyed; Sadjadi, Seyed

    2014-12-01

    Porous anodic aluminium oxide (AAO) template is commonly used in the synthesis of one-dimensional nanostructures, such as nanowires and nanorods, due to its simple fabrication process. Controlling the anodizing conditions is important because of their direct influence on the size of AAO template pores; it affects the size of nanostructures that are fabricated in AAO template. In present study, several alumina templates were fabricated by a two-step electrochemical anodization in different conditions, such as the time of first process, its voltage, and electrolyte concentration. The effect of these factors on pore diameters of AAO templates was investigated using scanning electron microscopy (SEM).

  16. Role of the tip induced local anodic oxidation in the conductive atomic force microscopy of mixed phase silicon thin films

    Czech Academy of Sciences Publication Activity Database

    Vetushka, Aliaksi; Fejfar, Antonín; Ledinský, Martin; Rezek, Bohuslav; Stuchlík, Jiří; Kočka, Jan

    2010-01-01

    Roč. 7, 3-4 (2010), s. 728-731 ISSN 1862-6351 R&D Projects: GA MŠk(CZ) LC06040; GA AV ČR KAN400100701; GA MŠk LC510; GA AV ČR(CZ) IAA100100902 Institutional research plan: CEZ:AV0Z10100521 Keywords : local anodic oxidation (LAO) * conductive atomic force microscopy (C-AFM) Subject RIV: BM - Solid Matter Physics ; Magnetism http://www3.interscience.wiley.com/journal/123289759/abstract

  17. Magnetic and electronic studies in the granular (Ni{sub 0.84}Fe{sub 0.16}){sub 54}(alumina){sub 46} sputtered thin films

    Energy Technology Data Exchange (ETDEWEB)

    Omari, N., E-mail: nabila_omari@yahoo.fr [PTA, Universite Hassan II-Casablanca, Faculte des Sciences, B.P. 5366 Maarif, Maroc (Morocco); Institut Neel CNRS, Departement MCMF, B.P. 166, 38042 Grenoble Cedex 9 (France); Lassri, H. [LPMMAT, Universite Hassan II-Casablanca, Faculte des Sciences, B.P. 5366 Maarif, Maroc (Morocco); Fnidiki, A. [Groupe de Physique des Materiaux, UMR CNRS 6634, Faculte des Sciences de Rouen, Site Universitaire du Madrillet, Avenue de l' Universite, B.P. 12, 76801 Saint-Etienne du Rouvray Cedex (France); Abid, M. [PTA, Universite Hassan II-Casablanca, Faculte des Sciences, B.P. 5366 Maarif, Maroc (Morocco); Hlil, E.K. [Institut Neel CNRS, Departement MCMF, B.P. 166, 38042 Grenoble Cedex 9 (France)

    2012-06-15

    We have studied the magnetization in the granular (Ni{sub 0.84}Fe{sub 0.16}){sub 54}(alumina){sub 46} alloy. The thermomagnetization curve is found to obey the Bloch law. Spin wave stiffness constant D and the exchange constant A were calculated from the experimental results. The magnetic experimental measurements have been interpreted in the framework of random magnetic anisotropy (RMA) model. The results have shown that it is possible to extend the application of RMA to the granular alloy. From an analysis of the approach to saturation magnetization some fundamental parameters have been extracted. In addition, self-consistent ab initio calculations, based on Korringa-Kohn-Rostocker (KKR), are performed to investigate magnetic and electronic properties of the granular alloy. Spin polarization within the framework of the coherent potential approximation (CPA) is considered.

  18. Magnetic and electronic studies in the granular (Ni0.84Fe0.16)54(alumina)46 sputtered thin films

    International Nuclear Information System (INIS)

    Omari, N.; Lassri, H.; Fnidiki, A.; Abid, M.; Hlil, E.K.

    2012-01-01

    We have studied the magnetization in the granular (Ni 0.84 Fe 0.16 ) 54 (alumina) 46 alloy. The thermomagnetization curve is found to obey the Bloch law. Spin wave stiffness constant D and the exchange constant A were calculated from the experimental results. The magnetic experimental measurements have been interpreted in the framework of random magnetic anisotropy (RMA) model. The results have shown that it is possible to extend the application of RMA to the granular alloy. From an analysis of the approach to saturation magnetization some fundamental parameters have been extracted. In addition, self-consistent ab initio calculations, based on Korringa-Kohn-Rostocker (KKR), are performed to investigate magnetic and electronic properties of the granular alloy. Spin polarization within the framework of the coherent potential approximation (CPA) is considered.

  19. GeO2 Thin Film Deposition on Graphene Oxide by the Hydrogen Peroxide Route: Evaluation for Lithium-Ion Battery Anode.

    Science.gov (United States)

    Medvedev, Alexander G; Mikhaylov, Alexey A; Grishanov, Dmitry A; Yu, Denis Y W; Gun, Jenny; Sladkevich, Sergey; Lev, Ovadia; Prikhodchenko, Petr V

    2017-03-15

    A peroxogermanate thin film was deposited in high yield at room temperature on graphene oxide (GO) from peroxogermanate sols. The deposition of the peroxo-precursor onto GO and the transformations to amorphous GeO 2 , crystalline tetragonal GeO 2 , and then to cubic elemental germanium were followed by electron microscopy, XRD, and XPS. All of these transformations are influenced by the GO support. The initial deposition is explained in view of the sol composition and the presence of GO, and the different thermal transformations are explained by reactions with the graphene support acting as a reducing agent. As a test case, the evaluation of the different materials as lithium ion battery anodes was carried out revealing that the best performance is obtained by amorphous germanium oxide@GO with >1000 mAh g -1 at 250 mA g -1 (between 0 and 2.5 V vs Li/Li + cathode), despite the fact that the material contained only 51 wt % germanium. This is the first demonstration of the peroxide route to produce peroxogermanate thin films and thereby supported germanium and germanium oxide coatings. The advantages of the process over alternative methodologies are discussed.

  20. Superior thermal conductivity of transparent polymer nanocomposites with a crystallized alumina membrane

    OpenAIRE

    Md. Poostforush; H. Azizi

    2014-01-01

    The properties of novel thermoconductive and optically transparent nanocomposites have been reported. The composites were prepared by the impregnation of thermoset resin into crystallized anodic aluminum oxide (AAO). Crystallized AAO synthesized by annealing amorphous AAO membrane at 1200°C. Although through-plane thermal conductivity of nanocomposites improved up to 1.13 W•m–1•K–1 (39 vol% alumina) but their transparency was preserved (Tλ550 nm ~ 72%). Integrated annealed alumina phase, low ...

  1. Photoluminescence properties of the composite of porous alumina and poly (2,5-dibutoxy-1,4 phenylenevinylene)

    International Nuclear Information System (INIS)

    Zhao Yi; Yang Deren; Zhou Chengyao; Yang Qing; Que Duanlin

    2003-01-01

    The spin coating method was used to assemble polymer (Poly (2,5-dibutoxy-1,4-phenylenevinylene)) (DBO-PPV) into the pores of porous alumina which was prepared by anodization. Four peaks in the photoluminescence (PL) spectra of the composite, with contributions from the DBO-PPV and porous alumina, were found. It was also found that the light emitting from the porous alumina could excite the photoluminescence of DBO-PPV. The nanometer effect of the porous alumina can lead to a blue shift of 90 nm of the PL peaks of DBO-PPV

  2. Properties of nanostructures obtained by anodization of aluminum in phosphoric acid at moderate potentials

    Science.gov (United States)

    Zaraska, L.; Sulka, G. D.; Jaskuła, M.

    2009-01-01

    The influence of the process duration, anodizing potential and methanol addition on the structural features of porous anodic alumina formed in a 0.3 M H3PO4 solutions by twostep self-organized anodizing was investigated for potentials ranging from 100 to 170 V. The structural features of porous structures including pore diameter and interpore distance were evaluated from FE-SEM top-view images for samples anodized in the presence and absence of methanol. For the highest studied anodizing time and methanol volume fraction, an excellent agreement between experimental values of the interpore distance and theoretical predictions was observed. The pore arrangement regularity was analyzed for various electrolyte compositions and anodizing potentials. It was found that the regularity ratio of porous alumina increases linearly with increasing anodizing potential and time. The addition of methanol improves the quality of nanostructures and especially better uniformity of pore sizes is observed in the presence of the highest studied methanol content.

  3. Anodic oxidation

    CERN Document Server

    Ross, Sidney D; Rudd, Eric J; Blomquist, Alfred T; Wasserman, Harry H

    2013-01-01

    Anodic Oxidation covers the application of the concept, principles, and methods of electrochemistry to organic reactions. This book is composed of two parts encompassing 12 chapters that consider the mechanism of anodic oxidation. Part I surveys the theory and methods of electrochemistry as applied to organic reactions. These parts also present the mathematical equations to describe the kinetics of electrode reactions using both polarographic and steady-state conditions. Part II examines the anodic oxidation of organic substrates by the functional group initially attacked. This part particular

  4. Antibacterial Activity of Zinc Oxide-Coated Nanoporous Alumina

    Science.gov (United States)

    2012-05-17

    made nanoporous alumina membranes, which were created by means of anodic oxidation of aluminum in an oxalic acid electrolyte, for treatment of skin...this study. All of the solutions were prepared using 18 M de-ionized water (lab supply) and trace metal grade nitric acid (Thermo Fisher Scientific...low production cost, repro- ducible reproduction, and facile reproduction approach for these materials. Using in vitro studies, keratinocytes (HaCaT

  5. High alumina refractories

    International Nuclear Information System (INIS)

    Simao, L.C.; Lopes, A.B.; Galvao Filho, N.B.; Souza, R.B. de

    1989-01-01

    High alumina refractories with 92 to 96.5% Al 2 O 3 were produced using brown and white fused as aggregate. Those refractories present only alumina-α and mullite as crystalline mineralogical phase. Other physical and chemical characteristics are similar to the ones found in refractories produced in Brazil, Japan and U.S.A. The most important physical and chemical tests used for the characterization of the raw materials and refractories, complemented by those realized at high temperatures, plus X-ray Difractometry and optical microscopy are presented, besides the refractory formulation and main parameters of production [pt

  6. Comparison of analytical possibilities of inversion voltammetry of tellurium with cathodic and anodic potential scanning taking layer-by-layer analysis of GaAs-Te films as example

    International Nuclear Information System (INIS)

    Kaplin, A.A.; Portnyagina, Eh.O.; Gridaev, V.F.

    1979-01-01

    Possibility of application in analytical purposes of the process of tellurium precipitation electrosolution from the surfaces of graphite and mercury-graphite electrodes at the cathode scanning of the potential is shown. As a result of comparison of direct and inversion scanning with cathodic and anodic scanning of the potential, variants of voltammetric method of tellurium determination in artificial solutions and, taking the developed method of layer-by-layer analysis of the GaAsTe films as an example, advantage of mercury-graphite electrode with cathodic scanning as compared to graphite electrode with cathode scanning of the potential is shown. Reproducibility of the GaAs film analysis results according to anodic and cathodic tellurium peaks is satisfactory. Maximum deviation from the results of analysis of oxidation peaks and tellurium peduction does not exceed 15 rel. %. Thus, for tellurium concentrations, exceeding 5x10 -6 g-ion/l, both anodic and cathodic scanning of the potential can be used, though error in tellurium determination according to cathodic peaks is 1.5-2.0 times higher. At tellurium amounts lower 5x10 -6 g-ion/l the determination should be carried out according to the peaks of tellurium anodic oxidation from the surface of graphite electrode or according to the peaks of tellurium cathodic reduction from the surface of mercury-graphite electrode

  7. Infrared radiation properties of anodized aluminum

    Energy Technology Data Exchange (ETDEWEB)

    Kohara, S. [Science Univ. of Tokyo, Noda, Chiba (Japan). Dept. of Materials Science and Technology; Niimi, Y. [Science Univ. of Tokyo, Noda, Chiba (Japan). Dept. of Materials Science and Technology

    1996-12-31

    The infrared radiation heating is an efficient and energy saving heating method. Ceramics have been used as an infrared radiant material, because the emissivity of metals is lower than that of ceramics. However, anodized aluminum could be used as the infrared radiant material since an aluminum oxide film is formed on the surface. In the present study, the infrared radiation properties of anodized aluminum have been investigated by determining the spectral emissivity curve. The spectral emissivity curve of anodized aluminum changed with the anodizing time. The spectral emissivity curve shifted to the higher level after anodizing for 10 min, but little changed afterwards. The infrared radiant material with high level spectral emissivity curve can be achieved by making an oxide film thicker than about 15 {mu}m on the surface of aluminum. Thus, anodized aluminum is applicable for the infrared radiation heating. (orig.)

  8. Alumina Technology Roadmap

    Energy Technology Data Exchange (ETDEWEB)

    none,

    2002-02-01

    The Alumina Technology Roadmap outlines a comprehensive long-term research and development plan that defines the industry's collective future and establishes a clear pathway forward. It emphasizes twelve high-priority R&D areas deemed most significant in addressing the strategic goals.

  9. YSZ thin films deposited on NiO-CSZ anodes by pulsed injection MOCVD for intermediate temperature-SOFC applications

    International Nuclear Information System (INIS)

    Garcia, G.; Pardo, J.A.; Santiso, J.; Merino, R.I.; Orera, V.M.; Larrea, A.; Pena, J.I.; Laguna-Bercero, M.A.; Figueras, A.

    2004-01-01

    Yttria-stabilized zirconia (YSZ) films are prepared on NiO-CaSZ by PIMOCVD (pulsed injection metal organic chemical vapor deposition). High quality, 5 to 10 μm thick, totally dense YSZ layers are prepared by controlling the oxygen partial pressure during the deposition. YSZ solid electrolyte deposition onto Ni-YSZ eutectic substrate is found to be a promising combination with regard to intermediate-temperature solid-oxide fuel cell applications. (Abstract Copyright [2004], Wiley Periodicals, Inc.)

  10. Preparation of thin hexagonal highly-ordered anodic aluminum oxide (AAO) template onto silicon substrate and growth ZnO nanorod arrays by electrodeposition

    Science.gov (United States)

    Chahrour, Khaled M.; Ahmed, Naser M.; Hashim, M. R.; Elfadill, Nezar G.; Qaeed, M. A.; Bououdina, M.

    2014-12-01

    In this study, anodic aluminum oxide (AAO) templates of Aluminum thin films onto Ti-coated silicon substrates were prepared for growth of nanostructure materials. Hexagonally highly ordered thin AAO templates were fabricated under controllable conditions by using a two-step anodization. The obtained thin AAO templates were approximately 70 nm in pore diameter and 250 nm in length with 110 nm interpore distances within an area of 3 cm2. The difference between first and second anodization was investigated in details by in situ monitoring of current-time curve. A bottom barrier layer of the AAO templates was removed during dropping the voltage in the last period of the anodization process followed by a wet etching using phosphoric acid (5 wt%) for several minutes at ambient temperature. As an application, Zn nanorod arrays embedded in anodic alumina (AAO) template were fabricated by electrodeposition. Oxygen was used to oxidize the electrodeposited Zn nanorods in the AAO template at 700 °C. The morphology, structure and photoluminescence properties of ZnO/AAO assembly were analyzed using Field-emission scanning electron microscope (FESEM), Energy dispersive X-ray spectroscopy (EDX), Atomic force microscope (AFM), X-ray diffraction (XRD) and photoluminescence (PL).

  11. Electrochemical generation of oxygen. 1: The effects of anions and cations on hydrogen chemisorption and anodic oxide film formation on platinum electrode. 2: The effects of anions and cations on oxygen generation on platinum electrode

    Science.gov (United States)

    Huang, C. J.; Yeager, E.; Ogrady, W. E.

    1975-01-01

    The effects were studied of anions and cations on hydrogen chemisorption and anodic oxide film formation on Pt by linear sweep voltammetry, and on oxygen generation on Pt by potentiostatic overpotential measurement. The hydrogen chemisorption and anodic oxide film formation regions are greatly influenced by anion adsorption. In acids, the strongly bound hydrogen occurs at more cathodic potential when chloride and sulfate are present. Sulfate affects the initial phase of oxide film formation by produced fine structure while chloride retards the oxide-film formation. In alkaline solutions, both strongly and weakly bound hydrogen are influenced by iodide, cyanide, and barium and calcium cations. These ions also influence the oxide film formation. Factors considered to explain these effects are discussed. The Tafel slope for oxygen generation was found to be independent on the oxide thickness and the presence of cations or anions. The catalytic activity indicated by the exchange current density was observed decreasing with increasing oxide layer thickness, only a minor dependence on the addition of certain cations and anions was found.

  12. Electrochemical and morphological analyses on the titanium surface modified by shot blasting and anodic oxidation processes

    Energy Technology Data Exchange (ETDEWEB)

    Szesz, Eduardo M., E-mail: eszesz@neoortho.com.br [Neoortho Research Institute, Rua Ângelo Domingos Durigan, 607-Cascatinha, CEP 82025-100 Curitiba, PR (Brazil); Pereira, Bruno L., E-mail: brnl7@hotmail.com [Physics Department, Universidade Federal do Paraná, 81531-980 Curitiba, PR (Brazil); Kuromoto, Neide K., E-mail: kuromoto@fisica.ufpr.br [Physics Department, Universidade Federal do Paraná, 81531-980 Curitiba, PR (Brazil); Marino, Claudia E.B., E-mail: claudiamarino@yahoo.com [Mechanical Engineering Department, Universidade Federal do Paraná, 81531-980 Curitiba, PR (Brazil); Souza, Gelson B. de, E-mail: gelsonbs@uepg.br [Physics Department, Universidade Estadual de Ponta Grossa, 84051-510 Ponta Grossa, PR (Brazil); Soares, Paulo, E-mail: pa.soares@pucpr.br [Mechanical Engineering Department, Pontifícia Universidade Católica do Paraná, 80215-901 Curitiba, PR (Brazil)

    2013-01-01

    In recent years, many surface modification processes have been developed in order to induce the osseointegration on titanium surface and thus to improve the implants' biocompatibility. In this work, Ti surface has been modified by shot blasting followed by anodic oxidation process in order to associate the good surface characteristics of both processes to obtain a rough and porous surface able to promote the titanium surface bioactivity. Commercially pure titanium (grade 2) plates were used on the surface treatments that were as follows: Shot blasting (SB) performed using alumina (Al{sub 2}O{sub 3}) particles, and anodic oxidation (AO) using NaOH electrolyte. The morphology, structural changes and the open-circuit potentials (OCP) of the surfaces were analyzed. It can be observed that an increase on the roughness of the blasted surface and a rough and porous surface happens after the AO process. The anodic film produced is thin and followed the blasted surface topography. It can be observed that there are small pores with regular shape covering the entire surface. X-ray diffraction results showed the presence of the anatase and rutile phases on the blasted and anodized surface after heat treatment at 600 °C/1 h. Concerning electrochemical measurements, when the different samples were submitted to open-circuit conditions in a physiological electrolyte, the protective effect increases with the oxidation process due to the oxide layer. When the surface was blasted, the OCP was more negative when compared with the Ti surface without surface treatments. - Highlights: ► A combination of shot blasting and anodic oxidation surface treatments is proposed. ► Both processes produced an increase in roughness compared to the polished surface. ► The combination of processes produced a rough and porous surface. ► Open circuit results show that the protective effect increases with oxidation process. ► The combination of processes presents the better results in this

  13. Improvement of pentathiophene/fullerene planar heterojunction photovoltaic cells by improving the organic films morphology through the anode buffer bilayer

    Science.gov (United States)

    El Jouad, Zouhair; Cattin, Linda; Martinez, Francisco; Neculqueo, Gloria; Louarn, Guy; Addou, Mohammed; Predeep, Padmanabhan; Manuvel, Jayan; Bernède, Jean-Christian

    2016-05-01

    Organic photovoltaic cells (OPVCs) are based on a heterojunction electron donor (ED)/electron acceptor (EA). In the present work, the electron donor which is also the absorber of light is pentathiophene. The typical cells were ITO/HTL/pentathiophene/fullerene/Alq3/Al with HTL (hole transport layer) = MoO3, CuI, MoO3/CuI. After optimisation of the pentathiophene thickness, 70 nm, the highest efficiency, 0.81%, is obtained with the bilayer MoO3/CuI as HTL. In order to understand these results the pentathiophene films deposited onto the different HTLs were characterized by scanning electron microscopy, atomic force microscopy, X-rays diffraction, optical absorption and electrical characterization. It is shown that CuI improves the conductivity of the pentathiophene layer through the modification of the film structure, while MoO3 decreases the leakage current. Using the bilayer MoO3/CuI allows cumulating the advantages of each layer. Contribution to the topical issue "Materials for Energy Harvesting, Conversion and Storage (ICOME 2015) - Elected submissions", edited by Jean-Michel Nunzi, Rachid Bennacer and Mohammed El Ganaoui

  14. Anodization of cast aluminium alloys produced by different casting methods

    Directory of Open Access Journals (Sweden)

    K. Labisz

    2008-08-01

    Full Text Available In this paper the usability of two casting methods, of sand and high pressure cast for the anodization of AlSi12 and AlSi9Cu3 aluminium cast alloys was investigated. With defined anodization parameters like electrolyte composition and temperature, current type and value a anodic alumina surface layer was produced. The quality, size and properties of the anodic layer was investigated after the anodization of the chosen aluminium cast alloys. The Alumina layer was observed used light microscope, also the mechanical properties were measured as well the abrasive wear test was made with using ABR-8251 equipment. The researches included analyze of the influence of chemical composition, geometry and roughness of anodic layer obtained on aluminum casts. Conducted investigations shows the areas of later researches, especially in the direction of the possible, next optimization anodization process of aluminum casting alloys, for example in the range of raising resistance on corrosion to achieve a suitable anodic surface layer on elements for increasing applications in the aggressive environment for example as materials on working building constructions, elements in electronics and construction parts in air and automotive industry.

  15. Preparation of alumina microspheres

    International Nuclear Information System (INIS)

    Santos, W.R. dos; Abrao, A.

    1980-01-01

    Inorganic exchangers are widely used for adsorption and column partition chromatography. The main difficulty of using commercial alumina (in powder) for column chromatography is related to its packing, and the operations through the column become diffcult and time-consuming; also it turns to be virtually impossible to use large dimension columns. In order to eliminate these problems, a process for the preparation of alumina micro-spheres was developed as an adaptation of a similar process used to prepare nuclear fuel microspheres (UO 2 , ThO 2 ). The flowsheet of this process is presented together with the analytical results of sphericity after calcination, granulometry, density and characterization by X-ray diffractometry. Solubility tests showed that the so-prepared microspheres are well resistant to strong acids and bases; retention tests showed their efficiency, mainly to copper. (C.L.B.) [pt

  16. Uranyl sorption onto alumina

    International Nuclear Information System (INIS)

    Jacobsson, A.M.M.

    1997-01-01

    The mechanism for the adsorption of uranyl onto alumina from aqueous solution was studied experimentally and the data were modeled using a triple layer surface complexation model. The experiments were carried out at low uranium concentrations (9 x 10 -11 --5 x 10 -8 M) in a CO 2 free environment at varying electrolyte concentrations (0.01--1 M) and pH (4.5--12). The first and second acid dissociation constants, pK a1 and pK a2 , of the alumina surface were determined from potentiometric titrations to be 7.2 ± 0.6 and 11.2 ± 0.4, respectively. The adsorption of uranium was found to be independent of the electrolyte concentration. The authors therefore conclude that the uranium binds as an inner sphere complex. The results were modeled using the code FITEQL. Two reactions of uranium with the surface were needed to fit the data, one forming a uranyl complex with a single surface hydroxyl and the other forming a bridged or bidentate complex reacting with two surface hydroxyls of the alumina. There was no evidence from these experiments of site heterogeneity. The constants used for the reactions were based in part on predictions made utilizing the Hard Soft Acid Base, HSAB, theory, relating the surface complexation constants to the hydrolysis of the sorbing metal ion and the acid dissociation constants of the mineral oxide surface

  17. Nanoporous alumina as templates for multifunctional applications

    Science.gov (United States)

    Sousa, C. T.; Leitao, D. C.; Proenca, M. P.; Ventura, J.; Pereira, A. M.; Araujo, J. P.

    2014-09-01

    Due to its manufacturing and size tailoring ease, porous anodic alumina (PAA) templates are an elegant physical-chemical nanopatterning approach and an emergent alternative to more sophisticated and expensive methods currently used in nanofabrication. In this review, we will describe the ground work on the fabrication methods of PAA membranes and PAA-based nanostructures. We will present the specificities of the electrochemical growth processes of multifunctional nanomaterials with diversified shapes (e.g., nanowires and nanotubes), and the fabrication techniques used to grow ordered nanohole arrays. We will then fo