Effects of vanadium ion implantation on microstructure, mechanical and tribological properties of TiN coatings

NASA Astrophysics Data System (ADS)

Deng, Bin; Tao, Ye; Guo, Deliang

2012-09-01

TiN coatings were deposited on the substrates of cemented carbide (WC-TiC-Co) by Magnetic Filter Arc Ion Plating (MFAIP) and then implanted with vanadium through Metal Vacuum Vapor Arc (MEVVA) ion source with the doses of 1 × 1017 and 5 × 1017 ions/cm2 at 40 kV. The microstructures and chemical compositions of the V-implanted TiN coatings were investigated using Glancing Incidence X-ray Diffraction (GIXRD) and X-ray Photoelectron Spectroscopy (XPS), together with the mechanical and tribological properties of coatings were characterized using nano-indentation and ball-on-disk tribometer. It was found that the diffraction peaks of the V-implanted TiN coatings at the doses of 5 × 1017 ions/cm2 shifted to higher angles and became broader. The hardness and elastic modulus of TiN coatings increased after V ion implantation. The wear mechanism for both un-implanted and V-implanted TiN coatings against GCr15 steel ball was adhesive wear, and the V-implanted TiN coatings had a lower friction coefficient as well as a better wear resistance

Investigation on the effect of collagen and vitamins on biomimetic hydroxyapatite coating formation on titanium surfaces.

PubMed

Ciobanu, Gabriela; Ciobanu, Octavian

2013-04-01

This study uses an in vitro experimental approach to investigate the roles of collagen and vitamins in regulating the deposition of hydroxyapatite layer on the pure titanium surface. Titanium implants were coated with a hydroxyapatite layer under biomimetic conditions by using a supersaturated calcification solution (SCS), modified by adding vitamins A and D3, and collagen. The hydroxyapatite deposits on titanium were investigated by means of scanning electron microscopy (SEM) coupled with X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy. The results obtained have shown that hydroxyapatite coatings were produced in vitro under vitamins and collagen influence. Copyright © 2012 Elsevier B.V. All rights reserved.

Deuterium permeation of amorphous alumina coating on 316L prepared by MOCVD

NASA Astrophysics Data System (ADS)

Li, Shuai; He, Di; Liu, Xiaopeng; Wang, Shumao; Jiang, Lijun

2012-01-01

The deuterium permeation behavior of the alumina coating on 316L stainless steel prepared by metal organic chemical vapor deposition (MOCVD) was investigated. The alumina coating was also characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and scanning electron microscope (SEM). It was found that the as-prepared coating consisted of amorphous alumina. This alumina coating had a dense, crack-free and homogeneous morphology. Although the alumina coating was amorphous, effective suppression of deuterium permeation was demonstrated. The deuterium permeability of the alumina coating was 51-60 times less than that of the 316L stainless steel and 153-335 times less than that of the referred low activation martensitic steels at 860-960 K.

Effect of oxygen incorporation on the structure and elasticity of Ti-Al-O-N coatings synthesized by cathodic arc and high power pulsed magnetron sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hans, M., E-mail: hans@mch.rwth-aachen.de; Baben, M. to; Music, D.

2014-09-07

Ti-Al-O-N coatings were synthesized by cathodic arc and high power pulsed magnetron sputtering. The chemical composition of the coatings was determined by means of elastic recoil detection analysis and energy dispersive X-ray spectroscopy. The effect of oxygen incorporation on the stress-free lattice parameters and Young's moduli of Ti-Al-O-N coatings was investigated by X-ray diffraction and nanoindentation, respectively. As nitrogen is substituted by oxygen, implications for the charge balance may be expected. A reduction in equilibrium volume with increasing O concentration is identified by X-ray diffraction and density functional theory calculations of Ti-Al-O-N supercells reveal the concomitant formation of metal vacancies.more » Hence, the oxygen incorporation-induced formation of metal vacancies enables charge balancing. Furthermore, nanoindentation experiments reveal a decrease in elastic modulus with increasing O concentration. Based on ab initio data, two causes can be identified for this: First, the metal vacancy-induced reduction in elasticity; and second, the formation of, compared to the corresponding metal nitride bonds, relatively weak Ti-O and Al-O bonds.« less

Improving the oxidation resistance and stability of Ag nanoparticles by coating with multilayered reduced graphene oxide

NASA Astrophysics Data System (ADS)

Li, Yahui; Zhang, Huayu; Wu, Bowen; Guo, Zhuo

2017-12-01

A kind of coating nanostructure, Ag nanoparticles coated with multilayered reduced graphene oxide (RGO), is fabricated by employing a three-step reduction method in an orderly manner, which is significantly different from the conventional structures that are simply depositing or doping with Ag nanoparticles on RGO via chemical reduction. The as-prepared nanostructure is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SEAD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The results show that the obtained Ag/RGO nanostructure is observed to be a perfect coating structure with well dispersed Ag particles, which is responsible for the remarkable oxidation resistance. The results of XPS spectra indicate the content of metallic Ag is far greater than that of Ag oxides despite of prolonged exposure to the air, which fully demonstrate the excellent stability of thus coating nanostructure.

Effect of intrinsic zinc oxide coating on the properties of Al-doped zinc oxide nanorod arrays

NASA Astrophysics Data System (ADS)

Saidi, S. A.; Mamat, M. H.; Ismail, A. S.; Malek, M. F.; Yusoff, M. M.; Sin, N. D. Md.; Zoolfakar, A. S.; Khusaimi, Z.; Rusop, M.

2018-05-01

The aim of this study was to explore the influence of intrinsic zinc oxide (ZnO) coating fabricated by a simple immersion method. X-ray powder diffraction (XRD) analysis indicated that the Al-doped ZnO nanorod arrays films had a hexagonal wurtzite structure, similar to that of an intrinsic ZnO coating. Structural properties of the samples were characterised using field emission scanning electron microscopy (FESEM; JEOL JSM-7600F) and optical properties using X-ray diffraction (XRD). The XRD results showed that all films were crystallized under hexagonal wurtzite structure and presented a preferential orientation along the c-axis (002) was obtained. The XRD results showed that the intrinsic ZnO coating material had a strong orientation, whereas the ZnO was randomly oriented. Overall these results indicate that intrinsic ZnO coating are pontetial for the creation of functional materials such as barrier protection, optoelectronic devices, humidity sensor and ultraviolet photoconductive sensor.

A synchrotron X-ray diffraction deconvolution method for the measurement of residual stress in thermal barrier coatings as a function of depth.

PubMed

Li, C; Jacques, S D M; Chen, Y; Daisenberger, D; Xiao, P; Markocsan, N; Nylen, P; Cernik, R J

2016-12-01

The average residual stress distribution as a function of depth in an air plasma-sprayed yttria stabilized zirconia top coat used in thermal barrier coating (TBC) systems was measured using synchrotron radiation X-ray diffraction in reflection geometry on station I15 at Diamond Light Source, UK, employing a series of incidence angles. The stress values were calculated from data deconvoluted from diffraction patterns collected at increasing depths. The stress was found to be compressive through the thickness of the TBC and a fluctuation in the trend of the stress profile was indicated in some samples. Typically this fluctuation was observed to increase from the surface to the middle of the coating, decrease a little and then increase again towards the interface. The stress at the interface region was observed to be around 300 MPa, which agrees well with the reported values. The trend of the observed residual stress was found to be related to the crack distribution in the samples, in particular a large crack propagating from the middle of the coating. The method shows promise for the development of a nondestructive test for as-manufactured samples.

Evolution processes of the corrosion behavior and structural characteristics of plasma electrolytic oxidation coatings on AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Chen, Dong; Wang, Ruiqiang; Huang, Zhiquan; Wu, Yekang; Zhang, Yi; Wu, Guorui; Li, Dalong; Guo, Changhong; Jiang, Guirong; Yu, Shengxue; Shen, Dejiu; Nash, Philip

2018-03-01

Evolution processes of the corrosion behavior and structural characteristics of the plasma electrolytic oxidation (PEO) coated AZ31 magnesium alloy were investigated by using scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), potentio-dynamic polarization curves and electrochemical impedance spectroscopy (EIS) measurements. Detached coating samples were fabricated by an electrochemical method and more details of the internal micro-structure of coatings were clearly observed on the fractured cross-section morphologies of the samples compared to general polished cross-section morphologies. Evolution mechanisms of the coating corrosion behavior in relation to the evolution of micro-structural characteristics were discussed in detail.

Comparison study of biomimetic strontium-doped calcium phosphate coatings by electrochemical deposition and air plasma spray: morphology, composition and bioactive performance.

PubMed

Li, Ling; Lu, Xia; Meng, Yizhi; Weyant, Christopher M

2012-10-01

In this study, strontium-doped calcium phosphate coatings were deposited by electrochemical deposition and plasma spray under different process parameters to achieve various coating morphologies. The coating composition was investigated by energy dispersive X-ray spectroscopy and X-ray diffraction. The surface morphologies of the coatings were studied through scanning electron microscopy while the cytocompatibility and bioactivity of the strontium-doped calcium phosphate coatings were evaluated using bone cell culture using MC3T3-E1 osteoblast-like cells. The addition of strontium leads to enhanced proliferation suggesting the possible benefits of strontium incorporation in calcium phosphate coatings. The morphology and composition of deposited coatings showed a strong influence on the growth of cells.

Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

NASA Astrophysics Data System (ADS)

Mubarak Ali, M.; Raj, V.

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.

Effect of Sputtering Current on the Comprehensive Properties of (Ti,Al)N Coating and High-Speed Steel Substrate

NASA Astrophysics Data System (ADS)

Su, Yongyao; Tian, Liangliang; Hu, Rong; Liu, Hongdong; Feng, Tong; Wang, Jinbiao

2018-05-01

To improve the practical property of (Ti,Al)N coating on a high-speed steel (HSS) substrate, a series of sputtering currents were used to obtain several (Ti,Al)N coatings using a magnetron sputtering equipment. The phase structure, morphology, and components of (Ti,Al)N coatings were characterized by x-ray diffraction, scanning electron microscopy, energy-dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy, respectively. The performance of (Ti,Al)N coatings, adhesion, hardness, and wear resistance was tested using a scratch tester, micro/nanohardness tester, and tribometer, respectively. Based on the structure-property relationships of (Ti,Al)N coatings, the results show that both the Al content and deposition temperature of (Ti,Al)N coatings increased with sputtering current. A high Al content helped to improve the performance of (Ti,Al)N coatings. However, the HSS substrate was softened during the high sputtering current treatment. Therefore, the optimum sputtering current was determined as 2.5 A that effectively increased the hardness and wear resistance of (Ti,Al)N coating.

Preparation and characterization of hydroxyapatite-coated iron oxide particles by spray-drying technique.

PubMed

Donadel, Karina; Felisberto, Marcos D V; Laranjeira, Mauro C M

2009-06-01

Magnetic particles of iron oxide have been increasingly used in medical diagnosis by magnetic resonance imaging and in cancer therapies involving targeted drug delivery and magnetic hyperthermia. In this study we report the preparation and characterization of iron oxide particles coated with bioceramic hydroxyapatite by spray-drying. The iron oxide magnetic particles (IOMP) were coated with hydroxyapatite (HAp) by spray-drying using two IOMP/HAp ratios (0.7 and 3.2). The magnetic particles were characterized by way of scanning electronic microscopy, energy dispersive X-ray, X-ray diffraction, Fourier transformed infrared spectroscopy, flame atomic absorption spectrometry,vibrating sample magnetometry and particle size distribution (laser diffraction). The surface morphology of the coated samples is different from that of the iron oxide due to formation of hydroxyapatite coating. From an EDX analysis, it was verified that the surface of the coated magnetic particles is composed only of HAp, while the interior containsiron oxide and a few layers of HAp as expected. The results showed that spray-drying technique is an efficient and relatively inexpensive method for forming spherical particles with a core/shell structure.

Chrome-free Samarium-based Protective Coatings for Magnesium Alloys

NASA Astrophysics Data System (ADS)

Hou, Legan; Cui, Xiufang; Yang, Yuyun; Lin, Lili; Xiao, Qiang; Jin, Guo

The microstructure of chrome-free samarium-based conversion coating on magnesium alloy was investigated and the corrosion resistance was evaluated as well. The micro-morphology, transverse section, crystal structure and composition of the coating were observed by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and X- ray photoelectron spectroscopy (XPS), respectively. The corrosion resistance was evaluated by potentiodynamic polarization curve and electrochemical impedance spectroscopy (EIS). The results reveal that the morphology of samarium conversion coating is of crack-mud structure. Tiny cracks distribute in the compact coating deposited by samarium oxides. XRD, EDS and XPS results characterize that the coating is made of amorphous and trivalent-samarium oxides. The potentiodynamic polarization curve, EIS and OCP indicate that the samarium conversion coating can improve the corrosion resistance of magnesium alloys.

Surface and biological evaluation of hydroxyapatite-based coatings on titanium deposited by different techniques.

PubMed

Massaro, C; Baker, M A; Cosentino, F; Ramires, P A; Klose, S; Milella, E

2001-01-01

Hydroxyapatite coatings have been deposited on titanium cp by plasma spray, sol-gel, and sputtering techniques for dental implant applications. The latter two techniques are of current interest, as they allow coatings of micrometer dimensions to be deposited. Coating morphology, composition, and structure have been investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). All coatings were homogeneous and exhibited a rough morphology suitable for implant applications. The sputtered (after annealing), plasma spray, and sol-gel coatings all showed diffraction peaks corresponding to hydroxyapatite. The surface contaminants were observed to be different for the different coating types. The sputtered coatings were found to have a composition most similar to hydroxyapatite; the sol-gel deposits also showed a high concentration of hydroxyl ions. A discrepancy in the Ca/P ratio was observed for the plasma spray coatings, and a small concentration of carbonate ions was found in the sputter-deposited coatings. The in vitro cell-culture studies using MG63 osteoblast-like cells demonstrated the ability of cells to proliferate on the materials tested. The sol-gel coating promotes higher cell growth, greater alkaline phosphatase activity, and greater osteocalcin production compared to the sputtered and plasma-sprayed coatings. Copyright 2001 John Wiley & Sons, Inc.

Humidity control and hydrophilic glue coating applied to mounted protein crystals improves X-ray diffraction experiments

PubMed Central

Baba, Seiki; Hoshino, Takeshi; Ito, Len; Kumasaka, Takashi

2013-01-01

Protein crystals are fragile, and it is sometimes difficult to find conditions suitable for handling and cryocooling the crystals before conducting X-ray diffraction experiments. To overcome this issue, a protein crystal-mounting method has been developed that involves a water-soluble polymer and controlled humid air that can adjust the moisture content of a mounted crystal. By coating crystals with polymer glue and exposing them to controlled humid air, the crystals were stable at room temperature and were cryocooled under optimized humidity. Moreover, the glue-coated crystals reproducibly showed gradual transformations of their lattice constants in response to a change in humidity; thus, using this method, a series of isomorphous crystals can be prepared. This technique is valuable when working on fragile protein crystals, including membrane proteins, and will also be useful for multi-crystal data collection. PMID:23999307

Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

Production of thick uniform-coating films containing rectorite on nanofibers through the use of an automated coating machine.

PubMed

Wu, Yang; Li, Xueyong; Shi, Xiaowen; Zhan, Yingfei; Tu, Hu; Du, Yumin; Deng, Hongbing; Jiang, Linbin

2017-01-01

When an efficient automated coating machine is used to process layer-by-layer (LBL) deposited nanofibrous mats, it causes an obvious planar effect on the surface of the mats, which can be eliminated through ultimate immersion. During this process, chitosan (CS) - rectorite (REC) intercalated composite films are built on the surface of cellulose acetate (CA) nanofibrous mats by a coating machine. Then, the immersion process is utilized to allow positively charged CS or CS-REC intercalated composites to uniformly assemble on the surface of negatively charged CA nanofibers. An investigation into the morphology of the resultant scaffolds confirms that the uniquely small pore size, high specific surface area and typically three-dimensional (3D) structure of nanofibrous mats remain present. The results of Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS) indicate that it is feasible to assemble nanofibrous mats using a coating machine. The intercalated structure of CS-REC is confirmed by the results of small-angle X-ray diffraction (SAXRD) and wide-angle X-ray diffraction (WAXRD). The results of the cell experiment and antibacterial test demonstrate that the addition of REC not only has little impact on the cytocompatibility of the mats but also enhances their ability to inhibit bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

Design of a multilayer-based collimated plane-grating monochromator for tender X-ray range.

PubMed

Yang, Xiaowei; Wang, Hongchang; Hand, Matthew; Sawhney, Kawal; Kaulich, Burkhard; Kozhevnikov, Igor V; Huang, Qiushi; Wang, Zhanshan

2017-01-01

Collimated plane-grating monochromators (cPGMs), consisting of a plane mirror and plane diffraction grating, are essential optics in synchrotron radiation sources for their remarkable flexibility and good optical characteristics in the soft X-ray region. However, the poor energy transport efficiency of a conventional cPGM (single-layer-coated) degrades the source intensity and leaves reduced flux at the sample, especially for the tender X-ray range (1-4 keV) that covers a large number of K- and L-edges of medium-Z elements, and M-edges of high-Z elements. To overcome this limitation, the use of a multilayer-based cPGM is proposed, combining a multilayer-coated plane mirror with blazed multilayer gratings. With this combination, the effective efficiency of cPGMs can be increased by an order of magnitude compared with the conventional single-layer cPGMs. In addition, higher resolving power can be achieved with improved efficiency by increasing the blaze angle and working at higher diffraction order.

Design of a multilayer-based collimated plane-grating monochromator for tender X-ray range

PubMed Central

Yang, Xiaowei; Wang, Hongchang; Hand, Matthew; Sawhney, Kawal; Kaulich, Burkhard; Kozhevnikov, Igor V.; Huang, Qiushi; Wang, Zhanshan

2017-01-01

Collimated plane-grating monochromators (cPGMs), consisting of a plane mirror and plane diffraction grating, are essential optics in synchrotron radiation sources for their remarkable flexibility and good optical characteristics in the soft X-ray region. However, the poor energy transport efficiency of a conventional cPGM (single-layer-coated) degrades the source intensity and leaves reduced flux at the sample, especially for the tender X-ray range (1–4 keV) that covers a large number of K- and L-edges of medium-Z elements, and M-edges of high-Z elements. To overcome this limitation, the use of a multilayer-based cPGM is proposed, combining a multilayer-coated plane mirror with blazed multilayer gratings. With this combination, the effective efficiency of cPGMs can be increased by an order of magnitude compared with the conventional single-layer cPGMs. In addition, higher resolving power can be achieved with improved efficiency by increasing the blaze angle and working at higher diffraction order. PMID:28009556

Dip-coated ZrO2-Y2O3 coatings tested in molten salts for CSP applications

NASA Astrophysics Data System (ADS)

Pérez, Francisco Javier; Encinas-Sánchez, Víctor; Lasanta, María Isabel; de Miguel, María Teresa; García-Martín, Gustavo

2017-06-01

In the present work, the behaviour of ZrO2 - Y2O3 coatings in contact with molten salts at 500 °C has been studied. The coatings were prepared by sol-gel and deposited by dip-coating on AISI 304 specimens previously prepared by sanding and polishing. The behaviour in contact with molten salt was studied through static corrosion tests by the immersion of the coated samples in an alkali-nitrate mixture with a composition of 60 wt.% NaNO3/40 wt.% KNO3 (commonly known as Solar Salt). Prior to test, the deposited coatings were characterized using Scanning Electron Microscopy and X-Ray Diffraction, showing a compacted, homogeneous and uniform aspect and t-YSZ as main component. After corrosion tests, the samples were characterized via gravimetric, Scanning Electron Microscopy and X-Ray Diffraction. The results show a good behaviour of the coated samples compared with the bare coupon samples. However after 1000 h of testing m-ZrO2 appears in the composition,. At this preliminary study, results confirm the suitability of ZrO2 - Y2O3 coatings in solar applications after those working hours, although it is necessary to optimize the coating and study its behaviour at longer times.

In Vitro Sustained Release Study of Gallic Acid Coated with Magnetite-PEG and Magnetite-PVA for Drug Delivery System

PubMed Central

Kura, Aminu Umar; Hussein-Al-Ali, Samer Hasan; Bin Hussein, Mohd Zobir; Fakurazi, Sharida; Shaari, Abdul Halim; Ahmad, Zalinah

2014-01-01

The efficacy of two nanocarriers polyethylene glycol and polyvinyl alcohol magnetic nanoparticles coated with gallic acid (GA) was accomplished via X-ray diffraction, infrared spectroscopy, magnetic measurements, thermal analysis, and TEM. X-ray diffraction and TEM results showed that Fe3O4 nanoparticles were pure iron oxide having spherical shape with the average diameter of 9 nm, compared with 31 nm and 35 nm after coating with polyethylene glycol-GA (FPEGG) and polyvinyl alcohol-GA (FPVAG), respectively. Thermogravimetric analyses proved that after coating the thermal stability was markedly enhanced. Magnetic measurements and Fourier transform infrared (FTIR) revealed that superparamagnetic iron oxide nanoparticles could be successfully coated with two polymers (PEG and PVA) and gallic acid as an active drug. Release behavior of gallic acid from two nanocomposites showed that FPEGG and FPVAG nanocomposites were found to be sustained and governed by pseudo-second-order kinetics. Anticancer activity of the two nanocomposites shows that the FPEGG demonstrated higher anticancer effect on the breast cancer cell lines in almost all concentrations tested compared to FPVAG. PMID:24737969

Remanufacture of Zirconium-Based Conversion Coatings on the Surface of Magnesium Alloy

NASA Astrophysics Data System (ADS)

Liu, Zhe; Jin, Guo; Song, Jiahui; Cui, Xiufang; Cai, Zhaobing

2017-04-01

Brush plating provides an effective method for creating a coating on substrates of various shapes. A corroded zirconium-based conversion coating was removed from the surface of a magnesium alloy and then replaced with new coatings prepared via brush plating. The structure and composition of the remanufactured coating were determined via x-ray photoelectron spectroscopy, x-ray diffraction, and Fourier transform infrared spectroscopy. The results revealed that the coatings consist of oxide, fluoride, and tannin-related organics. The composition of the coatings varied with the voltage. Furthermore, as revealed via potentiodynamic polarization spectroscopy, these coatings yielded a significant increase in the corrosion resistance of the magnesium alloy. The friction coefficient remained constant for almost 300s during wear resistance measurements performed under a 1-N load and dry sliding conditions, indicating that the remanufactured coatings provide effective inhibition to corrosion.

Refraction effects in soft x-ray multilayer blazed gratings.

PubMed

Voronov, D L; Salmassi, F; Meyer-Ilse, J; Gullikson, E M; Warwick, T; Padmore, H A

2016-05-30

A 2500 lines/mm Multilayer Blazed Grating (MBG) optimized for the soft x-ray wavelength range was fabricated and tested. The grating coated with a W/B₄C multilayer demonstrated a record diffraction efficiency in the 2nd blazed diffraction order in the energy range from 500 to 1200 eV. Detailed investigation of the diffraction properties of the grating demonstrated that the diffraction efficiency of high groove density MBGs is not limited by the normal shadowing effects that limits grazing incidence x-ray grating performance. Refraction effects inherent in asymmetrical Bragg diffraction were experimentally confirmed for MBGs. The refraction affects the blazing properties of the MBGs and results in a shift of the resonance wavelength of the gratings and broadening or narrowing of the grating bandwidth depending on diffraction geometry. The true blaze angle of the MBGs is defined by both the real structure of the multilayer stack and by asymmetrical refraction effects. Refraction effects can be used as a powerful tool in providing highly efficient suppression of high order harmonics.

40 CFR 59.508 - What test methods must I use?

Code of Federal Regulations, 2010 CFR

2010-07-01

... the metal content of metallic aerosol coating products, you must use South Coast Air Quality Management District (SCAQMD) Method 318-95, Determination of Weight Percent Elemental Metal in Coatings by X-ray Diffraction, July, 1996, in 40 CFR part 59 (incorporated by reference in § 59.515). To determine...

40 CFR 59.508 - What test methods must I use?

Code of Federal Regulations, 2011 CFR

2011-07-01

... the metal content of metallic aerosol coating products, you must use South Coast Air Quality Management District (SCAQMD) Method 318-95, Determination of Weight Percent Elemental Metal in Coatings by X-ray Diffraction, July, 1996, in 40 CFR part 59 (incorporated by reference in § 59.515). To determine...

X-ray measurements of the strain and shape of dielectric/metallic wrap-gated InAs nanowires

NASA Astrophysics Data System (ADS)

Eymery, J.; Favre-Nicolin, V.; Fröberg, L.; Samuelson, L.

2009-03-01

Wrap-gate (111) InAs nanowires (NWs) were studied after HfO2 dielectric coating and Cr metallic deposition by a combination of grazing incidence x-ray techniques. In-plane and out-of-plane x-ray diffraction (crystal truncation rod analysis) allow determining the strain tensor. The longitudinal contraction, increasing with HfO2 and Cr deposition, is significantly larger than the radial dilatation. For the Cr coating, the contraction along the growth axis is quite large (-0.95%), and the longitudinal/radial deformation ratio is >10, which may play a role on the NW transport properties. Small angle x-ray scattering shows a smoothening of the initial hexagonal bare InAs NW shape and gives the respective core/shell thicknesses, which are compared to flat surface values.

Micro and Nano Systems for Space Exploration

NASA Technical Reports Server (NTRS)

Manohara, Harish

2007-01-01

This slide presentation reviews the use of micro and nano systems in Space exploration. Included are: an explanation of the rationales behind nano and micro technologies for space exploration, a review of how the devices are fabricated, including details on lithography with more information on Electron Beam (E-Beam) lithography, and X-ray lithography, a review of micro gyroscopes and inchworm Microactuator as examples of the use of MicroElectoMechanical (MEMS) technology. Also included is information on Carbon Nanotubes, including a review of the CVD growth process. These micro-nano systems have given rise to the next generation of miniature X-ray Diffraction, X-ray Fluorescence instruments, mass spectrometers, and terahertz frequency vacuum tube oscillators and amplifiers, scanning electron microscopes and energy dispersive x-ray spectroscope. The nanotechnology has also given rise to coating technology, such as silicon nanotip anti-reflection coating.

Soft X-ray Foucault test: A path to diffraction-limited imaging

NASA Astrophysics Data System (ADS)

Ray-Chaudhuri, A. K.; Ng, W.; Liang, S.; Cerrina, F.

1994-08-01

We present the development of a soft X-ray Foucault test capable of characterizing the imaging properties of a soft X-ray optical system at its operational wavelength and its operational configuration. This optical test enables direct visual inspection of imaging aberrations and provides real-time feedback for the alignment of high resolution soft X-ray optical systems. A first application of this optical test was carried out on a Mo-Si multilayer-coated Schwarzschild objective as part of the MAXIMUM project. Results from the alignment procedure are presented as well as the possibility for testing in the hard X-ray regime.

Morphology, Composition, and Bioactivity of Strontium-Doped Brushite Coatings Deposited on Titanium Implants via Electrochemical Deposition

PubMed Central

Liang, Yongqiang; Li, Haoyan; Xu, Jiang; Li, Xin; Qi, Mengchun; Hu, Min

2014-01-01

Surface modification techniques have been applied to generate titanium implant surfaces that promote osseointegration for use in dental applications. In this study, strontium-doped brushite coatings were deposited on titanium by electrochemical deposition. The phase composition of the coating was investigated by energy dispersive X-ray spectroscopy and X-ray diffraction. The surface morphologies of the coatings were studied through scanning electron microscopy, and the cytocompatibility and bioactivity of the strontium-doped brushite coatings were evaluated using cultured osteoblasts. Osteoblast proliferation was enhanced by the addition of strontium, suggesting a possible mechanism by which strontium incorporation in brushite coatings increased bone formation surrounding the implants. Cell growth was also strongly influenced by the composition of the deposited coatings, with a 10% Sr-doped brushite coating inducing the greatest amount of bone formation among the tested materials. PMID:24901526

Surface modification of tantalum pentoxide coatings deposited by magnetron sputtering and correlation with cell adhesion and proliferation in in vitro tests

NASA Astrophysics Data System (ADS)

Zykova, A.; Safonov, V.; Goltsev, A.; Dubrava, T.; Rossokha, I.; Donkov, N.; Yakovin, S.; Kolesnikov, D.; Goncharov, I.; Georgieva, V.

2016-03-01

The effect was analyzed of surface treatment by argon ions on the surface properties of tantalum pentoxide coatings deposited by reactive magnetron sputtering. The structural parameters of the as-deposited coatings were investigated by means of transmission electron microscopy, atomic force microscopy and scanning electron microscopy. X-ray diffraction profiles and X-ray photoelectron spectra were also acquired. The total surface free energy (SFE), the polar, dispersion parts and fractional polarities, were estimated by the Owens-Wendt-Rabel-Kaeble method. The adhesive and proliferative potentials of bone marrow cells were evaluated for both Ta2O5 coatings and Ta2O5 coatings deposited by simultaneous bombardment by argon ions in in vitro tests.

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation.

PubMed

Huang, Yong; Wang, Yingjun; Ning, Chengyun; Nan, Kaihui; Han, Yong

2007-09-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and beta-glycerol phosphate disodium salt pentahydrate (beta-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 microm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Deposition of Visible Light Active Photocatalytic Bismuth Molybdate Thin Films by Reactive Magnetron Sputtering

PubMed Central

Ratova, Marina; Kelly, Peter J.; West, Glen T.; Xia, Xiaohong; Gao, Yun

2016-01-01

Bismuth molybdate thin films were deposited by reactive magnetron co-sputtering from two metallic targets in an argon/oxygen atmosphere, reportedly for the first time. Energy dispersive X-ray spectroscopy (EDX) analysis showed that the ratio of bismuth to molybdenum in the coatings can be effectively controlled by varying the power applied to each target. Deposited coatings were annealed in air at 673 K for 30 min. The crystalline structure was assessed by means of Raman spectroscopy and X-ray diffraction (XRD). Oxidation state information was obtained by X-ray photoelectron spectroscopy (XPS). Photodegradation of organic dyes methylene blue and rhodamine B was used for evaluation of the photocatalytic properties of the coatings under a visible light source. The photocatalytic properties of the deposited coatings were then compared to a sample of commercial titanium dioxide-based photocatalytic product. The repeatability of the dye degradation reactions and photocatalytic coating reusability are discussed. It was found that coatings with a Bi:Mo ratio of approximately 2:1 exhibited the highest photocatalytic activity of the coatings studied; its efficacy in dye photodegradation significantly outperformed a sample of commercial photocatalytic coating. PMID:28787867

Structure and properties of TiSiCN coatings with different bias voltages by arc ion plating

NASA Astrophysics Data System (ADS)

Xie, Xinming; Li, Jinlong; Dong, Minpeng; Zhang, Henghua; Wang, Liping

2018-03-01

TiSiCN coatings were deposited on 316 L steel using the multi-arc ion plating system. All the coatings had the same total thickness of approximately 1.6 µm. The TiSiCN coatings were deposited under the mixture constant flow of N2 and C2H2 but varying bias. Information about structures, composition and properties were characterized by scanning electron microscope, x-ray diffraction, x-ray photoelectron spectroscopy, nanoindentation and ball-on-plate wear tests. The results show that all of the coatings consist of a TiCN nano-crystal phase and an Si3N4 amorphous phase. With an increase in the bias, the film becomes denser and exhibits better tribological behavior and mechanical properties. Moreover, the bonding strength between the coatings and the substrate increased and the resistance to thermal shock intensified when the coatings were made at a higher bias voltage.

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, Andrew M.; Seppala, Lynn G.

1991-01-01

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm.sup.2. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics.

Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, S.R.; Wilkinson, E.J.

Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on themore » IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.« less

Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Voronov, D.L.; Warwick, T.; Gullikson, E. M.

2016-07-27

High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

CMC-coated Fe3O4 nanoparticles as new MRI probes for hepatocellular carcinoma

NASA Astrophysics Data System (ADS)

Sitthichai, Sudarat; Pilapong, Chalermchai; Thongtem, Titipun; Thongtem, Somchai

2015-11-01

Pure Fe3O4 nanoparticles and Fe3O4 magnetic nanoparticles (MNPs) coated with carboxymethyl cellulose (CMC) were successfully prepared by co-precipitating of FeCl2·4H2O and FeCl3·6H2O in the solutions containing ammonia at 80 °C for 3 h. Phase, morphology, particle-sized distribution, surface chemistry, and weight loss were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) including high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), thermogravimetric analysis (TGA), and Fourier transform infrared (FTIR) spectroscopy. In this research, CMC-coated Fe3O4 MNPs consisting of Fe2+ and Fe3+ ions with 543.3-mM-1 s-1 high relaxivity were detected and were able to be used for magnetic resonance imaging (MRI) application with very good contrast for targeting hepatocellular carcinoma (HCC) without any further vectorization.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jung, Min-Cherl; Zhang, Dongrong; Nikiforov, Gueorgui O.

Ultrathin (<6 nm) polycrystalline films of 6,13-bis(triisopropylsilylethynyl) pentacene (TIPS-P) are deposited with a two-step spin-coating process. The influence of spin-coating conditions on morphology of the resulting film was examined by atomic force microscopy. Film thickness and RMS surface roughness were in the range of 4.0–6.1 and 0.6–1.1 nm, respectively, except for small holes. Polycrystalline structure was confirmed by grazing incidence x-ray diffraction measurements. Near-edge x-ray absorption fine structure measurements suggested that the plane through aromatic rings of TIPS-P molecules was perpendicular to the substrate surface.

Attenuation of encrustation by self-assembled inorganic fullerene-like nanoparticles

NASA Astrophysics Data System (ADS)

Ron, Racheli; Zbaida, David; Kafka, Ilan Z.; Rosentsveig, Rita; Leibovitch, Ilan; Tenne, Reshef

2014-04-01

Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed.Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr06231g

Coating and functionalization of high density ion track structures by atomic layer deposition

NASA Astrophysics Data System (ADS)

Mättö, Laura; Szilágyi, Imre M.; Laitinen, Mikko; Ritala, Mikko; Leskelä, Markku; Sajavaara, Timo

2016-10-01

In this study flexible TiO2 coated porous Kapton membranes are presented having electron multiplication properties. 800 nm crossing pores were fabricated into 50 μm thick Kapton membranes using ion track technology and chemical etching. Consecutively, 50 nm TiO2 films were deposited into the pores of the Kapton membranes by atomic layer deposition using Ti(iOPr)4 and water as precursors at 250 °C. The TiO2 films and coated membranes were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray reflectometry (XRR). Au metal electrode fabrication onto both sides of the coated foils was achieved by electron beam evaporation. The electron multipliers were obtained by joining two coated membranes separated by a conductive spacer. The results show that electron multiplication can be achieved using ALD-coated flexible ion track polymer foils.

Composite Ni-Co-fly ash coatings on 5083 aluminium alloy

NASA Astrophysics Data System (ADS)

Panagopoulos, C. N.; Georgiou, E. P.; Tsopani, A.; Piperi, L.

2011-03-01

Ni-Co-fly ash coatings were deposited on zincate treated 5083 wrought aluminium alloy substrates with the aid of the electrodeposition technique. Structural and chemical characterization of the produced composite coatings was performed with the aid of X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron dispersive X-ray analysis (EDS) techniques. The Ni-Co-fly ash coatings were found to consist of a crystalline Ni-Co solid solution with dispersed fly ash particles. In addition, chemical analysis of the Ni-Co matrix showed that it consisted of 80 wt.% Ni and 20 wt.% Co. The co-deposition of fly ash particles leads to a significant increase of the microhardness of the coating. The corrosion behaviour of the Ni-Co-fly ash/zincate coated aluminium alloy, in a 0.3 M NaCl solution (pH = 3.5), was studied by means of potentiodynamic corrosion experiments.

Calcium phosphate coatings modified with zinc- or copper- incorporation on Ti-40Nb alloy

NASA Astrophysics Data System (ADS)

Komarova, E. G.; Sedelnikova, M. B.; Sharkeev, Yu P.; Kazakbaeva, A. A.; Glukhov, I. A.; Khimich, M. A.

2017-05-01

The influence of the microarc oxidation parameters and electrolyte composition on the structure, properties and composition of CaP coatings modified with Zn- or Cu- incorporation on the Ti-40mas.%Nb (Ti-40Nb) alloy was investigated. The linear growth of thickness, roughness, and size of structural elements with process voltage increasing has been revealed. It was shown that the CaP coatings have the low contact angles with liquids and, consequently, high free surface energy. This indicates a high hydrophilicity of the coatings. X-ray diffraction analysis showed that the coatings have X-ray amorphous structure. The increase of the process voltage leads to the formation of such crystalline phases as CaHPO4 and β-Ca2P2O7 in the coatings. The maximum Ca/P atomic ratio was equal to 0.4, and Zn or Cu contents was equal to 0.3 or 0.2 at.%, respectively.

X-ray analysis of residual stress gradients in TiN coatings by a Laplace space approach and cross-sectional nanodiffraction: a critical comparison.

PubMed

Stefenelli, Mario; Todt, Juraj; Riedl, Angelika; Ecker, Werner; Müller, Thomas; Daniel, Rostislav; Burghammer, Manfred; Keckes, Jozef

2013-10-01

Novel scanning synchrotron cross-sectional nanobeam and conventional laboratory as well as synchrotron Laplace X-ray diffraction methods are used to characterize residual stresses in exemplary 11.5 µm-thick TiN coatings. Both real and Laplace space approaches reveal a homogeneous tensile stress state and a very pronounced compressive stress gradient in as-deposited and blasted coatings, respectively. The unique capabilities of the cross-sectional approach operating with a beam size of 100 nm in diameter allow the analysis of stress variation with sub-micrometre resolution at arbitrary depths and the correlation of the stress evolution with the local coating microstructure. Finally, advantages and disadvantages of both approaches are extensively discussed.

Surface mechanical behaviour of composite Ni-P-fly ash/zincate coated aluminium alloy

NASA Astrophysics Data System (ADS)

Panagopoulos, C. N.; Georgiou, E. P.

2009-04-01

Ni-P-fly ash coatings were produced on zincate coated 5083 wrought aluminium alloy substrates with the aid of an electroless deposition technique. Structural and chemical characterization of the produced coatings was performed with the aid of X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron dispersive X-ray analysis (EDS) techniques. The Ni-P-fly ash coating was found to consist of an amorphous Ni-P matrix with dispersed fly ash particles. The wear resistance of the Ni-P-fly ash coating on zincate treated aluminium alloy was observed to be higher than that of the bare aluminium alloy, when sliding against a stainless steel counterface. In addition, the adhesion between the Ni-P-fly ash/zincate coating and the aluminium alloy substrate was also studied with a scratch testing apparatus. The adhesion strength of Ni-P-fly ash/zincate coating on the aluminium alloy substrate was observed to be higher in comparison to the Ni-P/zincate coating on the same aluminium alloy.

The effect of Al intermediate layer on thermal resistance of EB-PVD yttria-stabilized zirconia coatings on titanium substrate

NASA Astrophysics Data System (ADS)

Panin, Alexey; Panin, Victor; Kazachenok, Marina; Shugurov, Artur; Sinyakova, Elena; Martynov, Sergey; Rusyaev, Andrey; Kasterov, Artur

2017-12-01

The yttria-stabilized zirconia coatings sprayed on titanium substrates by the electron beam physical vapor deposition were subjected to thermal annealing in air at 1000°C for 1, 30 and 60 min. The delamination and fracture of the coatings are studied by the scanning electron microscopy and X-ray diffraction. It is shown that a magnetron sputtered Al interlayer between the coating and the substrate considerably improves the thermal resistance of ceramic coatings.

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, A.M.; Seppala, L.G.

1991-03-26

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm[sup 2]. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics. 9 figures.

In situ X-ray diffraction contribution to the study of reactive element oxide coating effect on the high temperature oxidation behaviour of FeCrAl alloys

NASA Astrophysics Data System (ADS)

Cueff, R.; Buscail, H.; Caudron, E.; Riffard, F.; Issartel, C.; Perrier, S.; El Messki, S.

2004-11-01

The influence of yttrium oxide coating (processed by sol-gel method) on the oxidation behaviour of a commercial FeCrAl alloy (Kanthal A1) has been investigated during isothermal exposures in air at 1373K. The scale growth kinetic of the uncoated alloy obeys a parabolic rate law during the whole oxidation test whereas the kinetic curve of the Y-coated specimen exhibits an initial transient stage during the first hours, followed by a parabolic regime. The yttrium sol-gel coating deposited on the bare alloy does not conduct to the beneficial effect usually ascribed to the reactive elements. No oxidation rate improvement of the coated alloy is observed, the parabolic rate constants values are strictly identical for the both specimens. In situ X-ray diffraction reveals a marked influence of the reactive element on the composition of the oxide scale. The oxide layer formed on the yttrium-coated specimen revealed, in addition to α-alumina which is the main oxide also identified on the bare specimen, the presence of yttrium aluminates (YAlO{3}, Y{3}Al{5}O{12}) located in the outermost part of the layer.

Influence of microstructure on hardness of plasma sprayed Al2O3-TiO2-MgO coatings with interface diffusion by heat treatment

NASA Astrophysics Data System (ADS)

Chen, Kunlun; Song, Peng; Li, Chao; Lu, Jiansheng

2017-12-01

The effect of heat treatment on the microstructure and mechanical properties of Al2O3-TiO2 coatings doped with 5 wt% MgO was investigated in this paper. The composite coatings were prepared by atmospheric plasma spraying (APS) and heat treated at 1000 °C for 24 h in Ar. The coatings were analyzed using scanning electron microscopy with electron probe x-ray microanalysis and x-ray diffraction. The hardness was determined using a Vickers hardness test on the as-sprayed coatings and after heat treatment. The results showed that the interface diffusion between the Al-rich and Ti-rich layers resulted in mutual pinning within the coating during the heat treatment. The newly formed MgAl2O4 phase promoted cracking-healing behavior within the coating. We conclude that increase of the hardness of the coatings was mainly caused by the mutual pinning interface and crack healing.

Cobalt coated substrate for matrix-free analysis of small molecules by laser desorption/ionization mass spectrometry

NASA Astrophysics Data System (ADS)

Yalcin, Talat; Li, Liang

2009-12-01

Small molecule analysis is one of the most challenging issues in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. We have developed a cobalt coated substrate as a target for matrix-free analysis of small molecules in laser desorption/ionization mass spectrometry. Cobalt coating of 60-70 nm thickness has been characterized by scanning electron microscopy, energy dispersive X-ray analysis, X-ray diffraction, and laser induced breakdown spectroscopy. This target facilitates hundreds of samples to be spotted and analyzed without mixing any matrices, in a very short time. This can save a lot of time and money and can be a very practical approach for the analysis of small molecules by laser desorption/ionization mass spectrometry.

Effect of nitrogen-containing plasma on adherence, friction, and wear of radiofrequency-sputtered titanium carbide coatings

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Wheeler, D. R.

1979-01-01

Friction and wear experiments on 440C steel surfaces that were rf sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. Both X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that the small partial pressure of nitrogen (approximately 0.5 percent) markedly improves the adherence, friction, and wear properties when compared with coatings applied to sputter-etched surfaces, oxidized surfaces, or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Investigation of (Ti-Zr-Hf-V-Nb)N Multicomponent Nanostructured Coatings before and after Thermal Annealing by Nuclear Physics Methods of Analysis

NASA Astrophysics Data System (ADS)

Pogrebnjak, A. D.; Beresnev, V. M.; Bondar', A. V.; Kaverin, M. V.; Ponomarev, A. G.

2013-10-01

(Ti-Zr-Hf-V-Nb)N multicomponent nanostructured coatings with thickness of 1.0-1.4 μm synthesized by the method of cathode arc-vapor deposition at temperatures of 250-300°С are investigated by various mutually complementary methods of elemental structural analysis using slow positron beams (SPB), proton microbeam based particle-induced x-ray emission (μ-PIXE), energy-dispersive x-ray spectroscopy (EDS) and scanning electron microscopy (SEM) analyses based on electron micro- and nanobeams, x-ray diffraction (XRD) method of phase structural analysis, and the "a-sin2φ" method of measuring a stressed-strained state (x-ray tensometry). The elemental composition, microstructure, residual stress in nanograins, profiles of defect and atom distributions with depth and over the coating surface in 3D-representation are studied for these coatings, and their phase composition, severely strained state, and composition of coatings before and after annealing at Tann = 600°С for annealing time τ = 30 min are investigated. It is demonstrated that the oxidation resistance of the examined coatings can be significantly increased by high-temperature annealing that leads to the formation of elastic severely strained compression state of the coating. Redistribution of elements and defects, their segregation near the interface boundaries and around grains and subgrains in the process of thermostimulated diffusion, and termination of spinodal segregation without considerable change of the average nanograin size are revealed.

Preparation of an orthodontic bracket coated with an nitrogen-doped TiO(2-x)N(y) thin film and examination of its antimicrobial performance.

PubMed

Cao, Baocheng; Wang, Yuhua; Li, Na; Liu, Bin; Zhang, Yingjie

2013-01-01

A bracket coated with a nitrogen-doped (N-doped) TiO(2-x)N(y) thin film was prepared using the RF magnetron sputtering method. The physicochemical properties of the thin film were measured using X-ray diffraction and energy-dispersive X-ray spectrometry, while the antimicrobial activity of the bracket against common oral pathogenic microbes was assessed on the basis of colony counts. The rate of antimicrobial activity of the bracket coated with nano-TiO(2-x)N(y) thin film against Streptococcus mutans, Lactobacillus acidophilus, Actinomyces viscous, and Candida albicans was 95.19%, 91.00%, 69.44%, and 98.86%, respectively. Scanning electron microscopy showed that fewer microbes adhered to the surface of this newly designed bracket than to the surface of the normal edgewise bracket. The brackets coated with the N-doped TiO(2-x)N(y) thin film showed high antimicrobial and bacterial adhesive properties against normal oral pathogenic bacterial through visible light, which is effective in prevention of enamel demineralization and gingivitis in orthodontic patients.

Design and analysis of a fast, two-mirror soft-x-ray microscope

NASA Technical Reports Server (NTRS)

Shealy, D. L.; Wang, C.; Jiang, W.; Jin, L.; Hoover, R. B.

1992-01-01

During the past several years, a number of investigators have addressed the design, analysis, fabrication, and testing of spherical Schwarzschild microscopes for soft-x-ray applications using multilayer coatings. Some of these systems have demonstrated diffraction limited resolution for small numerical apertures. Rigorously aplanatic, two-aspherical mirror Head microscopes can provide near diffraction limited resolution for very large numerical apertures. The relationships between the numerical aperture, mirror radii and diameters, magnifications, and total system length for Schwarzschild microscope configurations are summarized. Also, an analysis of the characteristics of the Head-Schwarzschild surfaces will be reported. The numerical surface data predicted by the Head equations were fit by a variety of functions and analyzed by conventional optical design codes. Efforts have been made to determine whether current optical substrate and multilayer coating technologies will permit construction of a very fast Head microscope which can provide resolution approaching that of the wavelength of the incident radiation.

Tribocorrosion Failure Mechanism of TiN/SiOx Duplex Coating Deposited on AISI304 Stainless Steel.

PubMed

Chen, Qiang; Xie, Zhiwen; Chen, Tian; Gong, Feng

2016-11-26

TiN/SiO x duplex coatings were synthesized on AISI304 stainless steel by plasma immersion ion implantation and deposition (PIIID) followed by radio frequency magnetron sputtering (RFMS). The microstructure and tribocorrosion failure behaviors of the duplex coatings were investigated by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, atomic force microscopy, reciprocating-sliding tribometer, and electrochemical tests. The as-deposited duplex coating had a two-layered columnar growth structure consisting of face-centered cubic TiN and amorphous SiO x . Sliding tests showed that the TiN interlayer had good adhesion with the substrate, but the SiO x layer suffered from severe delamination failure. Friction force induced a number of micro-cracks in the coating, which provided channels for the diffusion of NaCl solution. The tribocorrosion test showed that the duplex coating exhibited a lower wear-performance in NaCl solution than in ambient atmosphere. Multi-scale chloride ion corrosion occurred simultaneously and substantially degraded the bonding strength of the columnar crystals or neighboring layers. Force-corrosion synergy damage eventually led to multi-degradation failure of the duplex coating. The presented results provide a comprehensive understanding of the tribocorrosion failure mechanism in coatings with duplex architecture.

Corrosion behaviors and effects of corrosion products of plasma electrolytic oxidation coated AZ31 magnesium alloy under the salt spray corrosion test

NASA Astrophysics Data System (ADS)

Wang, Yan; Huang, Zhiquan; Yan, Qin; Liu, Chen; Liu, Peng; Zhang, Yi; Guo, Changhong; Jiang, Guirong; Shen, Dejiu

2016-08-01

The effects of corrosion products on corrosion behaviors of AZ31 magnesium alloy with a plasma electrolytic oxidation (PEO) coating were investigated under the salt spray corrosion test (SSCT). The surface morphology, cross-sectional microstructure, chemical and phase compositions of the PEO coating were determined using scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction analysis (XRD), respectively. Further, the corrosion process of the samples under the SSCT was examined in a non-aqueous electrolyte (methanol) using electrochemical impedance spectroscopy (EIS) coupled with equivalent circuit. The results show that the inner layer of the coating was destroyed firstly and the corrosion products have significant effects on the corrosion behaviors of the coating. The results above are discussed and an electrochemical corrosion model is proposed in the paper.

High Temperature Behavior of Cr3C2-NiCr Coatings in the Actual Coal-Fired Boiler Environment

NASA Astrophysics Data System (ADS)

Bhatia, Rakesh; Sidhu, Hazoor Singh; Sidhu, Buta Singh

2015-03-01

Erosion-corrosion is a serious problem observed in steam-powered electricity generation plants, and industrial waste incinerators. In the present study, four compositions of Cr3C2-(Ni-20Cr) alloy coating powder were deposited by high-velocity oxy-fuel spray technique on T-91 boiler tube steel. The cyclic studies were performed in a coal-fired boiler at 1123 K ± 10 K (850 °C ± 10 °C). X-ray diffraction, scanning electron microscopy/energy dispersive X-ray analysis and elemental mapping analysis techniques were used to analyze the corrosion products. All the coatings deposited on T-91 boiler tube steel imparted hot corrosion resistance. The 65 pctCr3C2 -35 pct (Ni-20Cr)-coated T-91 steel sample performed better than all other coated samples in the given environment.

Effect of Sodium Dodecyl Sulphate and Sodium Bromide Additives on Ni–W Nanocoatings.

PubMed

Das, Malay Kumar; Qin, Jiaqian; Zhang, Xinyu; Li, Rongxia; Thueploy, Adisak; Limpanart, Sarintorn; Boonyongmaneerat, Yuttanat; Ma, Mingzhen; Liu, Riping

2017-02-01

Nickel-tungsten (Ni–W) coatings were fabricated by electrodeposition method with varying quantities of sodium dodecyl sulphate and sodium bromide to examine the effects of the aforesaid additives on the coatings. The obtained nanocoatings were studied by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and hardness tester. The hardness, tungsten content and grain size attained a maximum value at current density of 0.15 A/cm²,0.1 A/cm² and 0.1 A/cm², respectively. There was a pronounced impact of both the additives on the microstructure and morphology of the coatings. According to results, there are considerable difference in terms of the impact caused by the additives to the tungsten content, hardness and grain size of the coatings. The obtained results suggest that hardness of coatings is mainly contributed by W content in the deposits.

Deposition and characterization of TiAlSiN nanocomposite coatings prepared by reactive pulsed direct current unbalanced magnetron sputtering

NASA Astrophysics Data System (ADS)

Barshilia, Harish C.; Ghosh, Moumita; Shashidhara; Ramakrishna, Raja; Rajam, K. S.

2010-08-01

This work reports the performance of high speed steel drill bits coated with TiAlSiN nanocomposite coating at different Si contents (5.5-8.1 at.%) prepared using a four-cathode reactive pulsed direct current unbalanced magnetron sputtering system. The surface morphology of the as-deposited coatings was characterized using field emission scanning electron microscopy. The crystallographic structure, chemical composition and bonding structure were evaluated using X-ray diffraction, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, respectively. The corrosion behavior, mechanical properties and thermal stability of TiAlSiN nanocomposite coatings were also studied using potentiodynamic polarization, nanoindentation and Raman spectroscopy, respectively. The TiAlSiN coating thickness was approximately 2.5-2.9 μm. These coatings exhibited a maximum hardness of 38 GPa at a silicon content of approximately 6.9 at.% and were stable in air up to 850 °C. For the performance evaluation, the TiAlSiN coated drills were tested under accelerated machining conditions by drilling a 12 mm thick 304 stainless steel plate. Under dry conditions the uncoated drill bits failed after drilling 50 holes, whereas, TiAlSiN coated drill bits (Si = 5.5 at.%) drilled 714 holes before failure. Results indicated that for TiAlSiN coated drill bits the tool life increased by a factor of more than 14.

Pulsed electrodeposition for the synthesis of strontium-substituted calcium phosphate coatings with improved dissolution properties.

PubMed

Drevet, Richard; Benhayoune, Hicham

2013-10-01

Strontium-substituted calcium phosphate coatings are synthesized by pulsed electrodeposition on titanium alloy (Ti6Al4V) substrates. Experimental conditions of the process are optimized in order to obtain a coating with a 5% atomic substitution of calcium by strontium which corresponds to the best observations on the osteoblast cells activity and on the osteoclast cells proliferation. The physical and chemical characterizations of the obtained coating are carried out by scanning electron microscopy associated to energy dispersive X-ray spectroscopy (EDXS) for X-ray microanalysis and the structural characterization of the coating is carried out by X-ray diffraction. The in vitro dissolution/precipitation properties of the coated substrates are investigated by immersion into Dulbecco's Modified Eagle Medium (DMEM) from 1h to 14 days. The calcium, phosphorus and strontium concentrations variations in the biological liquid are assessed by Induced Coupled Plasma - Atomic Emission Spectroscopy for each immersion time. The results show that under specific experimental conditions, the electrodeposition process is suitable to synthesize strontium-substituted calcium phosphate coatings. Moreover, the addition of hydrogen peroxide (H2O2) into the electrolytic solution used in the process allows us to observe a control of the strontium release during the immersion of the prosthetic materials into DMEM. © 2013.

Cyclic oxidation behavior of plasma sprayed NiCrAlY/WC-Co/cenosphere coating

NASA Astrophysics Data System (ADS)

Mathapati, Mahantayya; Ramesh M., R.; Doddamani, Mrityunjay

2018-04-01

Components working at elevated temperature like boiler tubes of coal and gas fired power generation plants, blades of gas and steam turbines etc. experience degradation owing to oxidation. Oxidation resistance of such components can be increased by developing protective coatings. In the present investigation NiCrAlY-WC-Co/Cenosphere coating is deposited on MDN 321 steel substrate using plasma spray coating. Thermo cyclic oxidation behavior of coating and substrate is studied in static air at 600 °C for 20 cycles. The thermo gravimetric technique is used to approximate the kinetics of oxidation. X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray mapping techniques are used to characterize the oxidized samples. NiCrAlY-WC-Co/Cenosphere coating exhibited lower oxidation rate in comparison to MDN 321 steel substrate. The lower oxidation rate of coating is attributed to formation of Al2O3, Cr2O3, NiO and CoWO4 oxides on the outermost surface.

Calcium phosphate coatings obtained by Nd:YAG laser cladding: physicochemical and biologic properties.

PubMed

Lusquiños, F; De Carlos, A; Pou, J; Arias, J L; Boutinguiza, M; León, B; Pérez-Amor, M; Driessens, F C M; Hing, K; Gibson, I; Best, S; Bonfield, W

2003-03-15

The plasma spray (PS) technique is the most popular method commercially in use to produce calcium phosphate (CaP) coatings to promote fixation and osteointegration of the cementless prosthesis. Nevertheless, PS has some disadvantages, such as the poor coating-to-substrate adhesion, low mechanical strength, and brittleness of the coating. In order to overcome the drawbacks of plasma spraying, we introduce in this work a new method to apply a CaP coating on a Ti alloy using a well-known technique in the metallurgical field: laser surface cladding. The physicochemical characterization of the coatings has been carried out by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray analysis (EDX). The biologic properties of the coatings have been assessed in vitro with human osteoblast-like MG-63 cells. The overall results of this study affirm that the Nd:YAG laser cladding technique is a promising method in the biomedical field. Copyright 2003 Wiley Periodicals, Inc.

Effect of substrate temperature and gas flow ratio on the nanocomposite TiAlBN coating

NASA Astrophysics Data System (ADS)

Rosli, Z. M.; Kwan, W. L.; Juoi, J. M.

2016-07-01

Nanocomposite TiAlBN (nc-TiAlBN) coatings were successfully deposited via RF magnetron sputtering by varying the nitrogen-to-total gas flow ratio (RN), and substrate temperature (TS). All coatings were deposited on AISI 316 substrates using single Ti-Al-BN hot-pressed disc as a target. The grain size, phases, and chemical composition of the coatings were evaluated using glancing angle X-ray diffraction analysis (GAXRD) and X-ray photoelectron spectroscopy (XPS). Results showed that the grains size of the deposited nc-TiAlBN coatings were in the range of 3.5 to 5.7 nm and reached a nitride saturation state as early as 15 % RN. As the nitrogen concentration decreases, boron concentration increased from 9 at.% to 16.17 at.%. and thus, increase the TiB2 phase within the coatings. The TS, however, showed no significant effect either on the crystallographic structure, grain size, or in the chemical composition of the deposited nc-TiAlBN coating.

Diffraction grating transmission efficiencies for XUV and soft X rays. [for HEAO-B extrasolar astronomy

NASA Technical Reports Server (NTRS)

Schnopper, H. W.; Van Speybroeck, L. P.; Delvaille, J. P.; Epstein, A.; Kaellne, E.; Bachrach, R. Z.; Dijkstra, J.; Lantward, L.

1977-01-01

The manufacture and properties of a grating intended for extrasolar X-ray studies are described. The manufacturing process uses a split laser beam exposing an interference pattern on the photoresist-coated glass plated with a nickel parting layer. The grating, supporting structure, and mounting frame are electrodeposited on the nickel parting layer, and the final product is lifted from the glass substrate by selective etching of the nickel. A model was derived which relates the number of counts received in a given order m as a function of photon wavenumber. A 4-deg beam line was used to measure the efficiencies of gold transmission gratings for diffraction of X-rays in the range of 45 to 275 eV. The experimental results are in good agreement with model calculations.

Synergistic effects of mica and wollastonite fillers on thermal performance of intumescent fire retardant coating

NASA Astrophysics Data System (ADS)

Zia-ul-Mustafa, M.; Ahmad, Faiz; Megat-Yusoff, Puteri S. M.; Aziz, Hammad

2015-07-01

In this study, intumescent fire retardant coatings (IFRC) were developed to investigate the synergistic effects of reinforced mica and wollastonite fillers based IFRC towards heat shielding, char expansion, char composition and char morphology. Ammonium poly-phosphate (APP) was used as acid source, expandable graphite (EG) as carbon source, melamine as blowing agent, boric acid as additive and Hardener H-2310 polyamide amine in bisphenol A epoxy resin BE-188(BPA) was used as curing agent. Bunsen burner fire test was used for thermal performance according to UL-94 for 1 h. Field Emission Scanning Electron Microscopy (FESEM) was used to observe char microstructure. X-Ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to analyse char composition. The results showed that addition of clay filler in IFRC enhanced the fire protection performance of intumescent coating. X-Ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) results showed the presence of boron phosphate, silicon phosphate oxide, aluminium borate in the char that improved the thermal performance of intumescent fire retardant coating (IFRC). Resultantly, the presence of these developed compounds enhanced the Integrity of structural steel upto 500°C.

A study of the physical, chemical and biological properties of TiO2 coatings produced by micro-arc oxidation in a Ca-P-based electrolyte.

PubMed

dos Santos, Amanda; Araujo, Joyce R; Landi, Sandra M; Kuznetsov, Alexei; Granjeiro, José M; de Sena, Lidia Ágata; Achete, Carlos Alberto

2014-07-01

In this work, a porous and homogeneous titanium dioxide layer was grown on commercially pure titanium substrate using a micro-arc oxidation (MAO) process and Ca-P-based electrolyte. The structure and morphology of the TiO2 coatings were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and profilometry. The chemical properties were studied using electron dispersive X-ray spectroscopy (SEM-EDS) and X-ray photoelectron spectroscopy. The wettability of the coating was evaluated using contact angle measurements. During the MAO process, Ca and P ions were incorporated into the oxide layer. The TiO2 coating was composed of a mixture of crystalline and amorphous structures. The crystalline part of the sample consisted of a major anatase phase and a minor rutile phase. A cross-sectional image of the coating-substrate interface reveals the presence of voids elongated along the interface. An osteoblast culture was performed to verify the cytocompatibility of the anodized surface. The results of the cytotoxicity tests show satisfactory cell viability of the titanium dioxide films produced in this study.

Bacteria Adherence Properties of Nitrogen-Doped TiO2 Coatings by Plasma Surface Alloying Technique

NASA Astrophysics Data System (ADS)

Wang, Hefeng; Tang, Bin; Li, Xiuyan; Fan, Ailan

Titanium nitride coatings on 316L stainless steel (S. S) were obtained by plasma surface alloying technique. Nitrogen-doped titanium dioxide (TiO2-xNx) was synthesized by oxidative annealing the resulted TiNx coatings in air. The reference TiO2 samples were also prepared by oxidation of sputtered Ti coatings. The as-prepared coatings were characterized by X-ray diffraction, glow discharge optical emission spectrometer (GDOES), scanning electron microscopy, X-ray hotoelectron spectroscopy and UV-Vis spectrophotometry, respectively. The bacteria adherence property of the TiO2-xNx coatings on stainless steel on the oral bacteria Streptococcus Mutans was investigated and compared with that of stainless steel by fluorescence microscopy. The mechanism of the bacteria adherence was discussed. The results show that the TiO2-xNx coatings are composed of anatase crystalline structure. SEM measurement indicates a rough surface morphology with three-dimensional homogenous protuberances after annealing treatment. Optical properties reveal an extended tailing of the absorption edge toward the visible region due to nitrogen presence. The band gap of the N-doped sample is reduced from 2.29 eV to 1.90 eV compared with the pure TiO2 one. Because of the different roughness and microstructure, the TiO2-xNx coatings inhibit the bacteria adherence.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zia-ul-Mustafa, M., E-mail: engr.ziamustafa@gmail.com; Ahmad, Faiz; Megat-Yusoff, Puteri S. M.

In this study, intumescent fire retardant coatings (IFRC) were developed to investigate the synergistic effects of reinforced mica and wollastonite fillers based IFRC towards heat shielding, char expansion, char composition and char morphology. Ammonium poly-phosphate (APP) was used as acid source, expandable graphite (EG) as carbon source, melamine as blowing agent, boric acid as additive and Hardener H-2310 polyamide amine in bisphenol A epoxy resin BE-188(BPA) was used as curing agent. Bunsen burner fire test was used for thermal performance according to UL-94 for 1 h. Field Emission Scanning Electron Microscopy (FESEM) was used to observe char microstructure. X-Ray Diffraction (XRD)more » and Fourier transform infrared spectroscopy (FTIR) were used to analyse char composition. The results showed that addition of clay filler in IFRC enhanced the fire protection performance of intumescent coating. X-Ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) results showed the presence of boron phosphate, silicon phosphate oxide, aluminium borate in the char that improved the thermal performance of intumescent fire retardant coating (IFRC). Resultantly, the presence of these developed compounds enhanced the Integrity of structural steel upto 500°C.« less

X-ray diffraction diagnostic design for the National Ignition Facility

NASA Astrophysics Data System (ADS)

Ahmed, Maryum F.; House, Allen; Smith, R. F.; Ayers, Jay; Lamb, Zachary S.; Swift, David W.

2013-09-01

This paper describes the design considerations for Target Diffraction In-Situ (TARDIS), an x-ray diffraction diagnostic at the National Ignition Facility. A crystal sample is ramp-compressed to peak pressures between 10 and 30 Mbar and, during a pressure hold period, is probed with quasi-monochromatic x-rays emanating from a backlighter source foil. The crystal spectrography diffraction lines are recorded onto image plates. The crystal sample, filter, and image plates are packaged into one assembly, allowing for accurate and repeatable target to image plate registration. Unconverted laser light impinges upon the device, generating debris, the effects of which have been mitigated. Dimpled blast shields, high strength steel alloy, and high-z tungsten are used to shield and protect the image plates. A tapered opening was designed to provide adequate thickness of shielding materials without blocking the drive beams or x-ray source from reaching the crystal target. The high strength steel unit serves as a mount for the crystal target and x-ray source foil. A tungsten body contains the imaging components. Inside this sub-assembly, there are three image plates: a 160 degree field of view curved plate directly opposite the target opening and two flat plates for the top and bottom. A polycarbonate frame, coated with the appropriate filter material and embedded with registration features for image plate location, is inserted into the diagnostic body. The target assembly is metrologized and then the diagnostic assembly is attached.

Lead foil in dental X-ray film: Backscattering rejection or image intensifier?

NASA Astrophysics Data System (ADS)

Hönnicke, M. G.; Delben, G. J.; Godoi, W. C.; Swinka-Filho, V.

2014-11-01

Dental X-ray films are still largely used due to sterilization issues, simplicity and, mainly, economic reasons. These films almost always are double coated (double emulsion) and have a lead foil in contact with the film for X-ray backscattering rejection. Herein we explore the use of the lead foil as an image intensifier. In these studies, spatial resolution was investigated when images were acquired on the dental X-ray films with and without the lead foil. Also, the lead foil was subjected to atomic analysis (fluorescent measurements) and structure analysis (X-ray diffraction). We determined that the use of the lead foil reduces the exposure time, however, does not affect the spatial resolution on the acquired images. This suggests that the fluorescent radiation spread is smaller than the grain sizes of the dental X-ray films.

A Novel Method for Depositing Precious Metal Films on Difficult Surfaces

NASA Technical Reports Server (NTRS)

Veitch, L. C.; Phillip, W. H.

1994-01-01

A guanidine-based vehicle was developed to deposit precious metal coatings on surfaces known to be difficult to coat. To demonstrate this method, a platinum coating was deposited on alumina fibers using a guanidine-platinum solution. X-ray diffraction confirmed that the only species present in the coating was platinum and that all of the carbon species had been removed upon heat treatment. SEM results showed that some porosity was present but that the coatings uniformly covered the fiber surface and adhered well to the finer.

Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications

NASA Astrophysics Data System (ADS)

Park, Seon-Yeong; Choe, Han-Cheol

2018-02-01

In this study, Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetrons sputtering for dental applications were studied using different experimental techniques. Mn coating films were formed on Ti-29Nb-xHf alloys by a radio frequency magnetron sputtering technique for 0, 1, 3, and 5 min at 45 W. The microstructure, composition, and phase structure of the coated alloys were examined by optical microscopy, field emission scanning electron microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. The microstructure of Ti-29Nb alloy showed α" phase in the needle-like structure and Ti-29Nb-15Hf alloy showed β phase in the equiaxed structure. As the sputtering time increased, the circular particles of Mn coatings on the Ti-29Nb alloy increased at inside and outside surfaces. As the sputtering time increased, [Mn + Ca/P] ratio of the plasma electrolytic oxidized films in Ti- 29Nb-xHf alloys increased. The corrosion potential (Ecorr) of Mn coatings on the Ti-29Nb alloy showed higher than that of Mn coatings on the Ti-29Nb-15Hf alloy. The passive current density (Ipass) of the Mn coating on the Ti-29Nb alloy and Mn coatings on the Ti-29Nb-15Hf alloy was less noble than the non-Mn coated Ti-29Nb and Ti-29Nb-15Hf alloys surface.

Archaeometric study of black-coated pottery from Pompeii by different analytical techniques.

PubMed

Scarpelli, Roberta; Clark, Robin J H; De Francesco, Anna Maria

2014-01-01

Complementary spectroscopic methods were used to characterize ceramic body and black coating of fine pottery found at Pompeii (Italy). This has enabled us to investigate local productions and to clarify the technological changes over the 4th-1st centuries BC. Two different groups of ceramics were originally distinguished on the basis of macroscopic observations. Optical microscopy (OM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) seem to indicate the usage of the same raw materials for the production of black-coated ceramics at Pompeii for about three centuries. Raman microscopy (RM) and micro-analysis (SEM/EDS) suggest different production treatments for both raw material processing and firing practice (duration of the reducing step and the cooling rate). Copyright © 2013 Elsevier B.V. All rights reserved.

REACTIVE SPUTTER DEPOSITION OF CHROMIUM NITRIDE COATINGS

EPA Science Inventory

The effect of substrate temperature and sputtering gas compositon on the structure and properties of chromium-chromium nitride films deposited on C-1040 steel using r.f. magnetron sputter deposition was investigated. X-ray diffraction analysis was used to determine the structure ...

Strain response of thermal barrier coatings captured under extreme engine environments through synchrotron X-ray diffraction

NASA Astrophysics Data System (ADS)

Knipe, Kevin; Manero, Albert; Siddiqui, Sanna F.; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M.; Bartsch, Marion; Raghavan, Seetha

2014-07-01

The mechanical behaviour of thermal barrier coatings in operation holds the key to understanding durability of jet engine turbine blades. Here we report the results from experiments that monitor strains in the layers of a coating subjected to thermal gradients and mechanical loads representing extreme engine environments. Hollow cylindrical specimens, with electron beam physical vapour deposited coatings, were tested with internal cooling and external heating under various controlled conditions. High-energy synchrotron X-ray measurements captured the in situ strain response through the depth of each layer, revealing the link between these conditions and the evolution of local strains. Results of this study demonstrate that variations in these conditions create corresponding trends in depth-resolved strains with the largest effects displayed at or near the interface with the bond coat. With larger temperature drops across the coating, significant strain gradients are seen, which can contribute to failure modes occurring within the layer adjacent to the interface.

Influence of load and temperature on tribological behaviour of electroless Ni-P deposits

NASA Astrophysics Data System (ADS)

Kundu, S.; Das, S. K.; Sahoo, P.

2016-09-01

Electroless Ni-P coatings have shown tremendous potential as tribology material at room temperature. However, the performance of the same in high temperature field needs to be evaluated as investigation reveals the softening of most of the coating materials. In the current study, both as-deposited as well as heat treated samples are developed for the performance evaluation. Coatings are tested under different loads with a constant speed and at temperatures ranging from room temperature (R.T.) to 500°C. Tribological tests are carried out on a pin-on- disc tribotester by selecting a wear track diameter of 60 mm for 5 minutes. Wear is reported in the form of wear rate by following Archard's equation. The microstructure characterization of the coating is performed using SEM (Scanning Electron Microscopy), EDX (Energy Dispersive X-Ray Analysis) and XRD (X-Ray Diffraction Analysis). Coating is developed with phosphorous weight percentages around 9% on cylindrical mild steel samples and the deposition thickness is observed to be around 50 μm. The as-deposited coating is found to be amorphous in nature and hardness of the as-deposited coating is found to be around 585HV01. Friction coefficient increases initially with the increase in temperature from room temperature up to 100°C but thereafter gradually decrease with the increase in temperature. Initial increase in temperature (up to 100°C) provides higher rate of wear compared to room temperature but with further increase it drops in most of the cases. Wear rate increases with the increase in temperature but as it crosses or nears the phase transformation temperature (around 340°C), the scenario gets reversed. From X-ray diffraction analysis, it is found that coating is amorphous in as-deposited condition but transforms into a crystalline structure with heat treatment.

Microstructures and Properties of Laser Cladding Al-TiC-CeO2 Composite Coatings

PubMed Central

Kong, Dejun; Song, Renguo

2018-01-01

Al-TiC-CeO2 composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV0.2. In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance. PMID:29373555

Microstructures and Properties of Laser Cladding Al-TiC-CeO₂ Composite Coatings.

PubMed

He, Xing; Kong, Dejun; Song, Renguo

2018-01-26

Al-TiC-CeO₂ composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV 0.2 . In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance.

Corrosion mechanism and model of pulsed DC microarc oxidation treated AZ31 alloy in simulated body fluid

NASA Astrophysics Data System (ADS)

Gu, Yanhong; Chen, Cheng-fu; Bandopadhyay, Sukumar; Ning, Chengyun; Zhang, Yongjun; Guo, Yuanjun

2012-06-01

This paper addresses the effect of pulse frequency on the corrosion behavior of microarc oxidation (MAO) coatings on AZ31 Mg alloys in simulated body fluid (SBF). The MAO coatings were deposited by a pulsed DC mode at four different pulse frequencies of 300 Hz, 500 Hz, 1000 Hz and 3000 Hz with a constant pulse ratio. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) tests were used for corrosion rate and electrochemical impedance evaluation. The corroded surfaces were examined by X-ray diffraction (XRD), X-ray fluorescence (XRF) and optical microscopy. All the results exhibited that the corrosion resistance of MAO coating produced at 3000 Hz is superior among the four frequencies used. The XRD spectra showed that the corrosion products contain hydroxyapatite, brucite and quintinite. A model for corrosion mechanism and corrosion process of the MAO coating on AZ31 Mg alloy in the SBF is proposed.

Modification of carbon composites by nanoceramic compounds

NASA Astrophysics Data System (ADS)

Stoch, A.; Jastrzebski, W.; Długoń, E.; Stoch, G. J.; Błażewicz, S.; Adamczyk, A.; Tatarzyńska, K.

2005-06-01

Carbon-carbon composites (C/C) exhibit excellent high-temperature mechanical properties but their air oxidation limits their use at temperatures above 500 °C to inert atmosphere. Variety of coatings has been used to protect C/C composites from oxidation. In this work C/C composite substrates were covered with ceramic multilayer coats by electrophoretic deposition from ceramic sols such as silica sol, alumina sol and silica-lumina sol. Sol particles were of nano-sized dimensions. Deposited coats were annealed at 900-1500 °C. Oxidation tests at 600 °C reveal that the best protection of C/C composite against oxidation gives the multilayer coat formed by three or four electrophoretic depositions. The phase composition in the final annealed layers was analyzed by Infrared spectroscopy (FTIR) and by X-ray diffraction analysis (XRD). Morphology and chemical composition was observed using Scanning electron microscopy (SEM) with energy dispersive X-ray microanalysis (EDS).

Mechanical Grinding Preparation and Characterization of TiO2-Coated Wollastonite Composite Pigments

PubMed Central

Chen, Wanting; Liang, Yu; Hou, Xifeng; Zhang, Jing; Ding, Hao; Sun, Sijia; Cao, Hu

2018-01-01

TiO2-coated wollastonite composite pigments were prepared by the mechano-chemical grinding of wollastonite and TiO2 powder together in a wet ultrafine stirred mill. X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy and infrared spectra were used to investigate the microstructures and morphologies of the composite and the reaction mechanism. The results indicate that the TiO2-coated wollastonite composite pigments have similar properties to titanium dioxide pigment, showing much better properties than dry and wet mixing of wollastonite and TiO2. The hiding power of TiO2-coated wollastonite composite pigments (45% TiO2) is 17.97 g/m2, reaching 81.08% of titanium dioxide. A firm combination between wollastonite and TiO2 is obtained through a surface dehydroxylation reaction during the mechano-chemical method. PMID:29649116

Effect of basalt fibres reinforcement and aluminum trihydrate on the thermal properties of intumescent fire retardant coatings

NASA Astrophysics Data System (ADS)

Yasir, Muhammad; Amir, Norlaili Binti; Ahmad, Faiz; Syahirah Rodzhan, N.

2017-08-01

This research is carried out in order to study the synergistic effect of aluminium trihydrate and basalt fibres on the properties of fire resistant intumescent coatings. Intumescent fire retardant coatings were developed using different flame retardants such as ammonium polyphosphate, expandable graphite, melamine and boric acid. These flame retardants were bound together with the help of epoxy binder along with curing agent. Furthermore, individual and combinations of aluminium trihydrate and basalt fibres was incorporated in the formulations to analyse mechanical and chemical properties of the coatings. Char expansion was observed using furnace test, thermogravimetric analysis was used to determine residual weight, X-Ray Diffraction was performed to investigate compounds present in the char, shear test was conducted to determine char strength and scanning electron microscopy analysis was performed to observe morphology of the burnt char. From the microscopic investigation it was concluded that the dense structure of the char increased the char integrity by adding basalt and aluminium trihydrate as fillers. X-Ray Diffraction results shows the presence boron phosphate, and boric acid which enhanced the thermal performance of the coating up to 800°C. From the Thermogravimetric analysis it was concluded that the residual weight of the char was increased up to 34.9 % for IC-B2A4 which enhanced thermal performance of intumescent coating.

Phosphate Remediation and Recovery using Iron Oxide-based Adsorbents

EPA Science Inventory

E33-modified sorbents for the removal of phosphate from lake water was investigated in this study. E33-modified sorbents were synthesized by coating with manganese and nanoparticles. Characterization was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-...

The effect of cerium oxide argon-annealed coatings on the high temperature oxidation of a FeCrAl alloy

NASA Astrophysics Data System (ADS)

Nguyen, C. T.; Buscail, H.; Cueff, R.; Issartel, C.; Riffard, F.; Perrier, S.; Poble, O.

2009-09-01

Ceria coatings were applied in order to improve the adherence of alumina scales developed on a model Fe-20Cr-5Al alloy during oxidation at high temperature. These coatings were performed by argon annealing of a ceria sol-gel coating at temperatures ranging between 600 and 1000 °C. The influence of these coatings on the alloy oxidation behaviour was studied at 1100 °C. In situ X-ray diffraction (XRD) was performed to characterize the coating crystallographic nature after annealing and during the oxidation process. The alumina scale morphologies were studied by means of scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS). The present work shows that the alumina scale morphology observed on cerium sol-gel coated alloy was very convoluted. On the cerium sol-gel coated alloy, argon annealing results in an increase of the oxidation rate in air, at 1100 °C. The 600 °C argon annealing temperature results in a good alumina scale adherence under thermal cycling conditions at 1100 °C.

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

NASA Astrophysics Data System (ADS)

Zhang, Leilei; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-12-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Formation of Ca/P ceramic coatings by Plasma Electrolytic Oxidation (PEO) on Ti6Al4V ELI alloy

NASA Astrophysics Data System (ADS)

Rodriguez-Jaimes, Y.; Naranjo, D. I.; Blanco, S.; García-Vergara, S. J.

2017-12-01

The formation of PEO ceramic coatings on Ti6Al4V ELI alloy was investigated using a phosphate/calcium containing electrolyte at 300 and 400V at 310K for different times. The Plasma Electrolytic Oxidation (PEO) coated specimens were then heat treated at 873 and 1073K for 2 hours. Scanning electron microscopy, Energy Dispersive X-Ray Spectroscopy (EDS) and X-ray diffraction analysis were used to study the composition and the morphology of the ceramic coatings. The corrosion behaviour of the coatings was studied by Electrochemical Impedance Spectroscopy (EIS) in Simulated Body Fluid (SBF). The PEO-treated specimens primarily revealed a porous structure with thickness between 4 and 12μm, according to the voltage and process time used. The coatings are mainly composed of hydroxyapatite; however, as the voltage and anodizing time increase, the Ca/P ratio decreases. Generally, the corrosion resistance of the alloy was improved by the PEO-treated coatings, although the specimens treated at 1073K showed the presence of cracks that reduced the protective effect of the coatings.

SnS thin films deposited by chemical bath deposition, dip coating and SILAR techniques

NASA Astrophysics Data System (ADS)

Chaki, Sunil H.; Chaudhary, Mahesh D.; Deshpande, M. P.

2016-05-01

The SnS thin films were synthesized by chemical bath deposition (CBD), dip coating and successive ionic layer adsorption and reaction (SILAR) techniques. In them, the CBD thin films were deposited at two temperatures: ambient and 70 °C. The energy dispersive analysis of X-rays (EDAX), X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and optical spectroscopy techniques were used to characterize the thin films. The electrical transport properties studies on the as-deposited thin films were done by measuring the I-V characteristics, DC electrical resistivity variation with temperature and the room temperature Hall effect. The obtained results are deliberated in this paper.

Synthesis of galium nitride thin films using sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Hamid, Maizatul Akmam Ab; Ng, Sha Shiong

2017-12-01

In this research, gallium nitride (GaN) thin film were grown on silicon (Si) substrate by a low-cost sol-gel dip coating deposition method. The GaN precursor solution was prepared using gallium (III) nitrate hydrate powder, ethanol and diethanolamine as a starting material, solvent and surfactant respectively. The structural, morphological and optical characteristics of the deposited GaN thin film were investigated. Field-emission scanning electron microscopy observations showed that crack free and dense grains GaN thin films were formed. Energy dispersive X-ray analysis confirmed that the oxygen content in the deposited films was low. X-ray diffraction results revealed that deposited GaN thin films have hexagonal wurtzite structure.

Thallium Bromide Deposited Using Spray Coating

NASA Astrophysics Data System (ADS)

Ferreira, E. S.; Mulato, M.

2012-08-01

Spray coating was used to produce thallium bromide samples on glass substrates. The influence of several fabrication parameters on the final structural properties of the samples was investigated. Substrate position, substrate temperature, solution concentration, carrying gas, and solution flow were varied systematically, the physical deposition mechanism involved in each case being discussed. Total deposition time of about 3.5 h can lead to 62-μm-thick films, comprising completely packed micrometer-sized crystalline grains. X-ray diffraction and scanning electron microscopy were used to characterize the samples. On the basis of the experimental data, the optimum fabrication conditions were identified. The technique offers an alternative method for fast, cheap fabrication of large-area devices for the detection of high-energy radiation, i.e., X-rays and γ-rays, in medical imaging.

Relationship Between pH and Electrochemical Corrosion Behavior of Thermal-Sprayed Ni-Al-Coated Q235 Steel in Simulated Soil Solutions

NASA Astrophysics Data System (ADS)

Wei, Wei; Wu, Xin-qiang; Ke, Wei; Xu, Song; Feng, Bing; Hu, Bo-tao

2017-09-01

Electrochemical corrosion behavior of a thermal-sprayed Ni-Al-coated Q235 steel was investigated in the simulated soil solutions at different pH values using measurements of potentiodynamic polarization curves and electrochemical impedance spectroscopy as well as surface analyses including x-ray diffraction analysis, scanning electron microscope equipped with an energy-dispersive x-ray spectroscopy and x-ray photoelectron spectroscopy. The results showed that the corrosion resistance of the Ni-Al-coated Q235 steel was dependent on the pH of the test solution. From pH = 3.53 to pH = 4.79, the corrosion resistance of the coated steel increased rapidly. In the pH range from 4.79 to 12.26, the corrosion resistance exhibited no significant change. At pH 13.25, the corrosion resistance of the sample was found to decrease. The calculated corrosion rate of Ni-Al-coated Q235 steel was lower than that of the uncoated Q235 steel and galvanized steel in all the test solutions. Over a wide range of pH values, the Ni-Al-coated Q235 steel exhibited extremely good corrosion resistance. The experimental data together with the potential-pH diagrams provided a basis for a detailed discussion of the related corrosion mechanisms of the coated steel.

Restricting the high-temperature growth of nanocrystalline tin oxide

NASA Astrophysics Data System (ADS)

Savin, S.; Chadwick, A. V.

2003-01-01

The sensitivity of tin oxide is dependent on various factors, one of which is the grain size. Three methods have been investigated with the aim of stabilising the grain size in the nanometer range, namely; (i) encapsulation within a silica matrix, (ii) coating the crystallites with hexamethyldisilazane and (iii) pinning the grain boundaries with a second metal oxide nanocrystal. The resulting materials have been characterised by X-ray powder diffraction (XRPD), Extended X-ray absorption fine structure (EXAFS) and conductivity measurements.

Microstructure and corrosion resistance of sputter-deposited titanium-chromium alloy coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Landolt, D.; Robyr, C.; Mettraux, P.

1998-10-01

Titanium, chromium, and titanium-chromium alloy coatings were sputter-deposited to study their corrosion behaviors in relation to microstructure and composition. Silicon substrates were used to study the effect of alloying on intrinsic corrosion resistance of the coating materials, and brass substrates were used to study the effect of alloying on the penetrating porosity of the coatings. Corrosion behavior was characterized using linear sweep voltammetry. The crystal structure of the coatings was examined by x-ray diffraction (XRD) and the microstructure by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) was used to estimate the real surface area of the coatings. Results showedmore » alloying of titanium with chromium greatly influenced microstructure of the coatings. Alloying led to deposits of higher apparent density and, in some cases, to an x-ray amorphous structure. Alloy coatings showed significantly lower corrosion currents than the constituting metals. The effect was attributed to a smoother surface topography. When corrected of differences in real surface area, the intrinsic corrosion rate of the alloy coatings did not differ significantly from that of the constituting metals. Alloy coatings deposited on brass exhibited a lower porosity than titanium or chromium metal coatings produced under identical conditions.« less

Fabrication of Porous Ag/TiO2/Au Coatings with Excellent Multipactor Suppression

PubMed Central

Wu, Duoduo; Ma, Jianzhong; Bao, Yan; Cui, Wanzhao; Hu, Tiancun; Yang, Jing; Bai, Yuanrui

2017-01-01

Porous Ag/TiO2/Au coatings with excellent multipactor suppression were prepared by fabrication of porous Ag surface through two-step wet chemical etching, synthesis of TiO2 coatings by electroless-plating-like solution deposition and deposition of Au coatings via electroless plating. Porous structure of Ag surface, TiO2 coatings on porous Ag surface and Au coatings on porous Ag/TiO2 surface were verified by field-emission scanning electron microscopy, the composition and crystal type of TiO2 coatings was characterized by X-ray photoelectron spectroscopy and X-ray diffraction. Secondary electron yield (SEY) measurement was used to monitor the SEY coefficient of the porous Ag coatings and Ag/TiO2/Au coatings. The as-obtained porous Ag coatings were proved exhibiting low SEY below 1.2, and the process was highly reproducible. In addition, the porous Ag/TiO2/Au coatings showed excellent multipactor suppression with the SEY 1.23 and good environmental stability. It is worth mentioning that the whole preparation process is simple and feasible, which would provide a promising application in RF devices. PMID:28281546

Development of a flexible nanocomposite TiO2 film as a protective coating for bioapplications of superelastic NiTi alloys

NASA Astrophysics Data System (ADS)

Aun, Diego Pinheiro; Houmard, Manuel; Mermoux, Michel; Latu-Romain, Laurence; Joud, Jean-Charles; Berthomé, Gregory; Buono, Vicente Tadeu Lopes

2016-07-01

An experimental procedure to coat superelastic NiTi alloys with flexible TiO2 protective nanocomposite films using sol-gel technology was developed in this work to improve the metal biocompatibility without deteriorating its superelastic mechanical properties. The coatings were characterized by scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, and glazing incidence X-ray diffraction. The elasticity of the film was tested in coated specimens submitted to three-point bending tests. A short densification by thermal treatment at 500 °C for 10 min yielded a bilayer film consisting of a 50 nm-thick crystallized TiO2 at the inner interface with another 50-nm-thick amorphous oxide film at the outer interface. This bilayer could sustain over 6.4% strain without cracking and could thus be used to coat biomedical instruments as well as other devices made with superelastic NiTi alloys.

Comparative characteristic and erosion behavior of NiCr coatings deposited by various high-velocity oxyfuel spray processes

NASA Astrophysics Data System (ADS)

Sidhu, Hazoor Singh; Sidhu, Buta Singh; Prakash, S.

2006-12-01

The purpose of this study is to analyze and compare the mechanical properties and microstructure details at the interface of high-velocity oxyfuel (HVOF)-sprayed NiCr-coated boiler tube steels, namely ASTM-SA-210 grade A1, ASTM-SA213-T-11, and ASTM-SA213-T-22. Coatings were developed by two different techniques, and in these techniques liquefied petroleum gas was used as the fuel gas. First, the coatings were characterized by metallographic, scanning electron microscopy/energy-dispersive x-ray analysis, x-ray diffraction, surface roughness, and microhardness, and then were subjected to erosion testing. An attempt has been made to describe the transformations taking place during thermal spraying. It is concluded that the HVOF wire spraying process offers a technically viable and cost-effective alternative to HVOF powder spraying process for applications in an energy generation power plant with a point view of life enhancement and to minimize the tube failures because it gives a coating having better resistance to erosion.

Investigations on the Behavior of HVOF and Cold Sprayed Ni-20Cr Coating on T22 Boiler Steel in Actual Boiler Environment

NASA Astrophysics Data System (ADS)

Bala, Niraj; Singh, Harpreet; Prakash, Satya; Karthikeyan, J.

2012-01-01

High temperature corrosion accompanied by erosion is a severe problem, which may result in premature failure of the boiler tubes. One countermeasure to overcome this problem is the use of thermal spray protective coatings. In the current investigation high velocity oxy-fuel (HVOF) and cold spray processes have been used to deposit commercial Ni-20Cr powder on T22 boiler steel. To evaluate the performance of the coatings in actual conditions the bare as well as the coated steels were subjected to cyclic exposures, in the superheater zone of a coal fired boiler for 15 cycles. The weight change and thickness loss data were used to establish kinetics of the erosion-corrosion. X-ray diffraction, surface and cross-sectional field emission scanning electron microscope/energy dispersive spectroscopy (FE-SEM/EDS) and x-ray mapping techniques were used to analyse the as-sprayed and corroded specimens. The HVOF sprayed coating performed better than its cold sprayed counterpart in actual boiler environment.

Application of valence-to-core X-ray emission spectroscopy for identification and estimation of amount of carbon covalently bonded to chromium in amorphous Cr-C coatings prepared by magnetron sputtering

NASA Astrophysics Data System (ADS)

Safonov, V. A.; Habazaki, H.; Glatzel, P.; Fishgoit, L. A.; Drozhzhin, O. A.; Lafuerza, S.; Safonova, O. V.

2018-01-01

Cr-C coatings containing different amount of carbon ranging from ∼5 to 50 at.% were prepared by the direct current (DC) magnetron sputtering on a polished substrate of polycrystalline silicon. The thickness of the samples was about 400 nm. We characterized the composition and the structure of the as-received coatings and those annealed at 500 °C by X-ray diffraction (XRD), Energy dispersion X-ray spectroscopy (EDX) and valence-to-core X-ray emission spectroscopy (vtc-XES) methods As follows from XRD measurements, the samples with the carbon content above 35 at.% do not demonstrate any sign of the long-range order and annealing at 500 °C does not change their crystallinity. The vtc-XES curves of the as-prepared and annealed samples can be fitted as a superposition of corresponding spectra of chromium metal and chromium carbide (Cr3C2) phases. After the annealing, the content of carbides in the samples (and, correspondingly, the content of covalently bonded carbon) somewhat increases. This suggests that the as-received coatings contain a certain amount of carbon that is not covalently bonded to chromium (most likely, elemental carbon) and their annealing at 500 °C transforms this carbon into the additional (of the order of 2-5 at.%) amount of chromium carbide compounds. It deserves mentioning that for Cr-C coatings prepared by the electrochemical deposition from Cr(III) electrolytes containing organic compounds we have not observed changes in the vtc-X-ray emission spectra after similar annealing. This suggests that electrochemical deposition method in contrast to magnetron sputtering technique even at low temperatures favors the formation of only covalently bonded carbon.

Phase analysis of plasma-sprayed zirconia-yttria coatings

NASA Technical Reports Server (NTRS)

Shankar, N. R.; Berndt, C. C.; Herman, H.

1983-01-01

Phase analysis of plasma-sprayed 8 wt pct-yttria-stabilized zirconia (YSZ) thermal barrier coatings and powders was carried out by X-ray diffraction. Step scanning was used for increased peak resolution. Plasma spraying of the YSZ powder into water or onto a steel substrate to form a coating reduced the cubic and monoclinic phases with a simultaneous increase in the tetragonal phase. Heat treatment of the coating at 1150 C for 10 h in an Ar atmosphere increased the amount of cubic and monoclinic phases. The implications of these transformations on coating performance and integrity are discussed.

Dose-Dependent Effects of CeO2 on Microstructure and Antibacterial Property of Plasma-Sprayed TiO2 Coatings for Orthopedic Application

NASA Astrophysics Data System (ADS)

Zhao, Xiaobing; Liu, Gaopeng; Zheng, Hai; Cao, Huiliang; Liu, Xuanyong

2015-02-01

Titanium and its alloys have been used extensively for orthopedic and dental implants. Although these devices have achieved high rates of success, two major complications may be encountered: the lack of osseointegration and the biomaterial-related infection. Accordingly, cerium oxide (CeO2)-doped titanium oxide (TiO2) materials were coated on titanium by an atmospheric plasma spraying (APS) technique. The phase structures, morphologies, and surface chemical states of the obtained coatings were characterized by x-ray diffraction, scanning electron microscopy, and x-ray photoelectron spectroscopy techniques. The in vitro antibacterial and cytocompatibility of the materials were studied with Staphylococcus aureus ( S. aureus, ATCC25923) and osteoblast precursor cell line MC3T3-E1. The results indicated that the addition of CeO2 shifts slightly the diffraction peaks of TiO2 matrix to low angles but does not change its rutile phase structure. In addition, the CeO2/TiO2 composite coatings possess dose-dependent corrosion resistance and antimicrobial properties. And doping of 10 wt.% CeO2 exhibits the highest activity against S. aureus, improved corrosion resistance, and competitive cytocompatibility, which argues a promising option for balancing the osteogenetic and antibacterial properties of titanium implants.

Attenuation of encrustation by self-assembled inorganic fullerene-like nanoparticles.

PubMed

Ron, Racheli; Zbaida, David; Kafka, Ilan Z; Rosentsveig, Rita; Leibovitch, Ilan; Tenne, Reshef

2014-05-21

Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed.

Bioactive (Si, O, N)/(Ti, O, N)/Ti composite coating on NiTi shape memory alloy for enhanced wear and corrosion performance

NASA Astrophysics Data System (ADS)

Sun, Tao; Xue, Ning; Liu, Chao; Wang, Chao; He, Jin

2015-11-01

In this investigation, (Si, O, N)/(Ti, O, N)/Ti composite coating was synthesized on a NiTi shape memory alloy (SMA) substrate (50.8 at.% Ni) via plasma immersion ion implantation and deposition (PIIID) followed by magnetron sputtering, with the aim of promoting bioactivity and biocompatibility of NiTi SMAs. Nano featured (Si, O, N)/(Ti, O, N)/Ti coating was approximate 0.84 ± 0.05 μm in thickness, and energy dispersive X-ray (EDX) spectroscopy showed that Ni element was depleted from the surface of coated samples. X-ray diffraction (XRD) did not identify the phase composition of the (Si, O, N)/(Ti, O, N)/Ti coating, probably due to its thin thickness and poor crystalline resulting from low-temperature coating processes (<200 °C). X-ray photoelectron spectroscopy (XPS) analyses confirmed that a Ni-free surface was formed and Si element was incorporated into the composite coating via the magnetron sputtering process. Additionally, phase transformation behaviors of uncoated and coated NiTi SMA samples were characterized using differential scanning calorimetry (DSC). Wear and corrosion resistance of uncoated and coated NiTi SMA samples were evaluated using ball-on-disc tests and potentio-dynamic polarization curves, respectively. The (Si, O, N)/(Ti, O, N)/Ti coated NiTi SMA samples showed enhanced wear and corrosion resistance. Furthermore, the (Si, O, N)/(Ti, O, N)/Ti composite coating facilitated apatite formation in simulated body fluid (SBF) and rendered NiTi SMA bioactivity.

Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients.

PubMed

Siddiqui, Sanna F; Knipe, Kevin; Manero, Albert; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M; Bartsch, Marion; Raghavan, Seetha

2013-08-01

Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients

NASA Astrophysics Data System (ADS)

Siddiqui, Sanna F.; Knipe, Kevin; Manero, Albert; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M.; Bartsch, Marion; Raghavan, Seetha

2013-08-01

Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

Microstructural Analysis of TiAl x N y O z Coatings Fabricated by DC Reactive Sputtering

NASA Astrophysics Data System (ADS)

García-González, L.; Hernández-Torres, J.; Flores-Ramírez, N.; Martínez-Castillo, J.; García-Ramírez, P. J.; Muñoz-Saldaña, J.; Espinoza-Beltrán, F. J.

2009-02-01

TiAl x N y O z coatings were prepared by DC reactive sputtering on AISI D2 tool steel substrates, using a target of Ti-Al-O fabricated from a mixture of powders of Ti (22.60 wt.%), Al (24.77 wt.%), and O (52.63 wt.%). The coatings were deposited on substrates at room temperature in a reactive atmosphere of nitrogen and argon under a pressure of 8.5 × 10-3 mbar. X-ray diffraction, electron dispersive spectroscopy, Raman scattering, and nanoindentation techniques were employed to investigate the coatings. The results show that the increment in the nitrogen flow affects the structure and the mechanical properties of the coatings. The sample with the lowest nitrogen flow presented the highest hardness (10.5 GPa) and the Young’s modulus (179.5 GPa). The hardness of the coatings TiAl x N y O z as a function of crystalline grain size shows a behavior consistent with the Hall-Petch relation.

Cadmium sulphide (CdS) thin films deposited by chemical bath deposition (CBD) and dip coating techniques—a comparative study

NASA Astrophysics Data System (ADS)

Khimani, Ankurkumar J.; Chaki, Sunil H.; Malek, Tasmira J.; Tailor, Jiten P.; Chauhan, Sanjaysinh M.; Deshpande, M. P.

2018-03-01

The CdS thin films were deposited on glass slide substrates by Chemical Bath Deposition and dip coating techniques. The films thickness variation with deposition time showed maximum films deposition at 35 min for both the films. The energy dispersive analysis of x-ray showed both the films to be stoichiometric. The x-ray diffraction analysis confirmed the films possess hexagonal crystal structure. The transmission electron, scanning electron and optical microscopy study showed the films deposition to be uniform. The selected area electron diffraction exhibited ring patterns stating the films to be polycrystalline in nature. The atomic force microscopy images showed surface formed of spherical grains, hills and valleys. The recorded optical absorbance spectra analysis revealed the films possess direct optical bandgap having values of 2.25 eV for CBD and 2.40 eV for dip coating. The refractive index (η), extinction coefficient (k), complex dielectric constant (ε) and optical conductivity (σ 0) variation with wavelength showed maximum photon absorption till the respective wavelengths corresponding to the optical bandgap energy values. The recorded photoluminescence spectra showed two emission peaks. All the obtained results have been discussed in details.

Mineralogical characterization of rendering mortars from decorative details of a baroque building in Kozuchow (SW Poland)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bartz, W., E-mail: wojciech.bartz@ing.uni.wroc.pl; Filar, T.

Optical microscopic observations, scanning electron microscopy and microprobe with energy dispersive X-ray analysis, X-ray diffraction and differential thermal/thermogravimetric analysis allowed detailed characterization of rendering mortars from decorative details (figures of Saints) of a baroque building in Kozuchow (Lubuskie Voivodship, Western Poland). Two separate coats of rendering mortars have been distinguished, differing in composition of their filler. The under coat mortar has filler composed of coarse-grained siliceous sand, whereas the finishing one has much finer grained filler, dominated by a mixture of charcoal and Fe-smelting slag, with minor amounts of quartz grains. Both mortars have air-hardening binder composed of gypsum andmore » micritic calcite, exhibiting microcrystalline structure.« less

Improvement of mechanical and tribological properties in steel surfaces by using titanium-aluminum/titanium-aluminum nitride multilayered system

NASA Astrophysics Data System (ADS)

Ipaz, L.; Caicedo, J. C.; Esteve, J.; Espinoza-Beltran, F. J.; Zambrano, G.

2012-02-01

Improvement of mechanical and tribological properties on AISI D3 steel surfaces coated with [Ti-Al/Ti-Al-N]n multilayer systems deposited in various bilayer periods (Λ) via magnetron co-sputtering pulsed d.c. method, from a metallic binary target; has been studied in this work exhaustively. The multilayer coatings were characterized in terms of structural, chemical, morphological, mechanical and tribological properties by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy, nanoindentation, pin-on-disc and scratch tests, respectively. The failure mode mechanisms were studied by optical microscopy. Results from X-ray diffraction analysis revealed that the crystal structure of TiAl/TiAlN multilayer coatings has a tetragonal and FCC NaCl-type lattice structures for Ti-Al and Ti-Al-N, respectively, i.e., it was found to be non-isostructural multilayers. An enhancement of both hardness and elastic modulus up to 29 GPa and 260 GPa, respectively, was observed as the bilayer periods (Λ) in the coatings were decreased. The sample with a bilayer period (Λ) of 25 nm and bilayer number n = 100 showed the lowest friction coefficient (∼0.28) and the highest critical load (45 N), corresponding to 2.7 and 1.5 times better than those values for the coating deposited with n = 1, respectively. These results indicate an enhancement of mechanical, tribological and adhesion properties, comparing to the [Ti-Al/Ti-Al-N]n multilayer systems with 1 bilayer at 26%, 63% and 33%, respectively. This enhancement in hardness and toughness for multilayer coatings could be attributed to the different mechanisms for layer formation with nanometric thickness such as the novel Ti-Al/Ti-Al-N effect and the number of interfaces that act as obstacles for the crack deflection and dissipation of crack energy.

Tribological properties of epoxy composite coatings reinforced with functionalized C-BN and H-BN nanofillers

NASA Astrophysics Data System (ADS)

Yu, Jingjing; Zhao, Wenjie; Wu, Yinghao; Wang, Deliang; Feng, Ruotao

2018-03-01

A series of epoxy resin (EP) composite coatings reinforced with functionalized cubic boron nitride (FC-BN) and functionalized hexagonal boron nitride (FH-BN) were fabricated successfully on 316L stainless steel by hand lay-up technique. The structure properties were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The morphologies were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Moreover, UMT-3 tribometer and surface profiler were used to investigate tribological behaviors of as-prepared composite coatings under dry friction and seawater conditions respectively. The results demonstrated that the presence of FC-BN or FH-BN fillers could greatly decrease the friction coefficient (COF) and wear rate of epoxy, in addition, composite coatings possess better tribological properties under seawater condition which was attributed to the lubricating effect of seawater. Moreover, FC-BN endows the composite coatings the highest wear resistance, and FH-BN /EP composite coatings exhibited the best friction reduction performance which is attributed to the self-lubricating performance of lamella structure for FH-BN sheet.

Electrochemical Characteristics of Cell Cultured Ti-Nb-Zr Alloys After Nano-Crystallized Si-HA Coating.

PubMed

Jeong, Yong-Hoon; Choe, Han-Cheol

2015-01-01

The aim of this study was to investigate the electrochemical characteristics of nano crystallized Si-HA coating on Ti-Nb-Zr alloy after human osteoblast like (HOB) cell attachment. The Ti-Nb-Zr alloy was manufactured with 35 wt.% of Nb and 10 wt.% of Zr by arc melting furnace to appropriate physical properties as biomaterials. The HA and Si-substituted coatings were prepared by electron-beam physical vapor deposition method with 0.5, 0.8 and 1.2 wt.% of Si contents, and nano aging treatment was performed 500 degrees C for 1 h. The characteristics of coating surface were analyzed by field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction, respectively. To evaluate of cell attachment on cell cultured surface, the potentiodynamic test was performed on the surface using HOB cells. The results showed that the Si-HA coating surface showed higher tendency of cell attachment than that of single HA coating, corrosion resistance value was increased by dense of cell attachment.

Electrodeposition of amorphous Ni P coatings onto Nd Fe B permanent magnet substrates

NASA Astrophysics Data System (ADS)

Ma, C. B.; Cao, F. H.; Zhang, Z.; Zhang, J. Q.

2006-12-01

Decorative and protective Ni-P amorphous coatings were electroplated onto NdFeB permanent magnet from an ortho-phosphorous acid contained bath. The influences of the main electroplating technological parameters including current density, bath pH, bath temperature and H3PO3 on the structure and chemical composition of Ni-P coatings were investigated by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques in conjunction with X-ray diffraction (XRD), scanning transmission electron microscopy (SEM) and X-ray energy-dispersive spectrometry (EDX). The optimized amorphous Ni-P coated NdFeB can stand for ca. 180 h against neutral 3.0 wt.% NaCl salt spray without any pitting corrosion. Meanwhile, the results also showed that large phosphorous content is the precondition for Ni-P coatings to possess the amorphous structure, but too much high phosphorous content can damage the amorphous structure due to the separation of superfluous P from Ni2P/Ni3P and the resultant formation of multi-phase coatings (such as Ni2P-P).

Optical and Structural Characterization of ZnO/TiO2 Bilayer Thin Films Grown by Sol-Gel Spin Coating

NASA Astrophysics Data System (ADS)

Gareso, P. L.; Musfitasari; Juarlin, Eko

2018-03-01

Structural and optical properties of ZnO/TiO2 bilayers thin films have been investigated using x-ray diffraction (X-RD), scanning electron microscopy (SEM), and optical transmittance UV-Vis measurements. ZnO thin films were prepared by dissolving zinc acetate dehydrated into a solvent of ethanol and then added triethanolamin. In the case of TiO2 layers, tetraisoproxide was dissolved into ethanol and then added an acetate acid. The layer of ZnO was deposited first followed by TiO2 layer on a glass substrate using a spin coating technique. The ZnO/TiO2 bilayers were annealed at various temperatures from 300°C until 600°C for 60 minutes. The X-ray diffraction results show that there was an enhancement of the x-ray spectra as annealed temperature increased to 600°C in comparison to the samples that were annealed at 300°C. Based on the optical measurement of UV-Vis, the band gap energy of ZnO/TiO2 bilayer is around 3.2 eV at temperature of 300°C. This value is similar to the band gap energy of ZnO. SEM results show that there is no cluster in the surface of ZnO/TiO2 bilayer.

Surface Diagnostics in Tribology Technology and Advanced Coatings Development

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1999-01-01

This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

PVP-coated silver nanoparticles showing antifungal improved activity against dermatophytes

NASA Astrophysics Data System (ADS)

Silva, Edgar; Saraiva, Sofia M.; Miguel, Sónia P.; Correia, Ilídio J.

2014-11-01

Fungal infections affecting human beings have increased during the last years and the currently available treatments, when administered for long periods, trigger microbial resistance. Such demands the development of new viable therapeutic alternatives. Silver is known since the antiquity by its antimicrobial properties and, herein, it was used to produce two types of nanoparticles (NPs), uncoated and coated with polyvinylpyrrolidone (PVP), which were aimed to be used in fungal infection treatment. NPs properties were characterized by Transmission electron microscopy, X-ray diffraction, UV-Vis, Dynamic light scattering, Fourier transform infrared, and Energy-dispersive X-ray spectroscopy. Furthermore, in vitro studies were also performed to evaluate NPs cytotoxic profile and antifungal activity. The results obtained revealed that the produced nanoparticles are biocompatible and have a good potential for being used in the treatment of common skin infections caused by Trichophyton rubrum and Trichophyton mentagrophytes, being PVP-coated silver NPs the most suitable ones.

Corrosion behavior of plasma-sprayed Al 2O 3-Cr 2O 3 coatings in hot lithium molten salt

NASA Astrophysics Data System (ADS)

Cho, Soo Haeng; Park, Sung Bin; Kang, Dae Seong; Jeong, Myeong Soo; Park, Heong; Hur, Jin Mok; Lee, Han Soo

2010-04-01

In this study, hot corrosion studies were performed on bare as well as coated superalloy specimens after exposure to molten lithium chloride environment at 675 °C for 216 h under an oxidizing atmosphere. The substrates of the IN713LC superalloy specimens were sprayed with an aluminized NiCrAlY bond coat and then with an Al 2O 3-Cr 2O 3 top coat. The as-coated and tested specimens were examined by optical microscopy (OM), scanning electron microscopy (SEM)/X-ray energy dispersive spectrometry (EDS) and X-ray diffraction (XRD), respectively. The bare superalloy reveals an obvious weight loss, and the scale formed on the surface of the bare superalloy was spalled due to the rapid scale growth and thermal stress. The top coatings showed a much better hot corrosion resistance in the presence of LiCl-3 wt.% Li 2O molten salt when compared with those of the uncoated superalloy and the aluminized bond coatings. These coatings have been found to be beneficial for increasing to the hot corrosion resistance of the structural materials for handling high temperature lithium molten salts.

Influence of KMnO4 Concentrationon Infrared Emissivity of Coatings Formed on TC4 Alloys by Micro-Arc Oxidation

PubMed Central

Li, Ying; Li, Chaozhong; Hu, Dan; Li, Zhengxian; Xi, Zhengping

2017-01-01

Ceramic coatings with high emissivity were fabricated on TC4 alloys by micro-arc oxidation technique (MAO) in mixed silicate and phosphate electrolytes with varying KMnO4 addition. The microstructure, phase and chemical composition were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), and the infrared emissivity of the MAO coatings was measured in a waveband of 5–20 μm. The results show that the thickness of the coatings increased with the addition of KMnO4, but the roughness of the coatings first decreased and then increased slightly due to the inhibitory effect of KMnO4 on Na2SiO3 deposition. The main phase composition of the coatings was anatase and rutile TiO2, amorphous form of SiO2 and MnO2. The infrared emissivity value of the coatings strongly depended on KMnO4 concentration, the coating formed at the concentration of 0.8 g/L KMnO4 reached the highest and an average of up to 0.87 was observed. PMID:29137192

Biomimetic novel nanoporous niobium oxide coating for orthopaedic applications

NASA Astrophysics Data System (ADS)

Pauline, S. Anne; Rajendran, N.

2014-01-01

Niobium oxide was synthesized by sol-gel methodology and a crystalline, nanoporous and adherent coating of Nb2O5 was deposited on 316L SS using the spin coating technique and heat treatment. The synthesis conditions were optimized to obtain a nanoporous morphology. The coating was characterized using attenuated total reflectance-Infrared spectroscopy (ATR-IR), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM) and transmission electron microscopy (TEM) and the formation of crystalline Nb2O5 coating with nanoporous morphology was confirmed. Mechanical studies confirmed that the coating has excellent adherence to the substrate and the hardness value of the coating was excellent. Contact angle analysis showed increased hydrophilicity for the coated substrate. In vitro bioactivity test confirmed that the Nb2O5 coating with nanoporous morphology facilitated the growth of hydroxyapatite (HAp). This was further confirmed by the solution analysis test where increased uptake of calcium and phosphorous ions from simulated body fluid (SBF) was observed. Electrochemical evaluation of the coating confirmed that the crystalline coating is insulative and protective in nature and offered excellent corrosion protection to 316L SS. Thus, this study confirmed that the nanoporous crystalline Nb2O5 coating conferred bioactivity and enhanced corrosion resistance on 316L SS.

MgO-Al2O3-ZrO2 Amorphous Ternary Composite: A Dense and Stable Optical Coating

NASA Technical Reports Server (NTRS)

Shaoo, Naba K.; Shapiro, Alan P.

1998-01-01

The process-parameter-dependent optical and structural properties of MgO-Al2O3-ZrO2 ternary mixed-composite material were investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases, and process- dependent material composition of films were investigated through the use of atomic force microscopy, x-ray diffraction analysis, and energy-dispersive x-ray analysis. Energy-dispersive x-ray analysis made evident the correlation between the optical constants and the process-dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

Durable flame retardant and antibacterial finishing on cotton fabrics with cyclotriphosphazene/polydopamine/silver nanoparticles hybrid coatings

NASA Astrophysics Data System (ADS)

Li, Yingzhan; Wang, Bijia; Sui, Xiaofeng; Xie, Ruyi; Xu, Hong; Zhang, Linping; Zhong, Yi; Mao, Zhiping

2018-03-01

Durable flame retardant and antibacterial hybrid coatings were developed for cotton fabrics via simultaneous polymerization of dopamine and hydrolytic condensation of N3P3[NH(CH2)3Si(OC2H5)3]6. Silver nanoparticles were also introduced to the coatings by in situ reaction of AgNO3 with catechol moieties on polydopamine (PDA) in the absence of any external reducing agents. Energy dispersive spectrometer (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) were employed to study the morphology and constitution of the coatings. Thermal stability and combustion behaviors were characterized with thermogravimetric analysis (TGA) and vertical flammability tests. Considerable flame retardancy was obtained for the modified cotton fabrics, which also exhibited decent antibacterial activities (99.99%) against Gram-positive bacteria S. aureus and Gram-negative bacteria E. coli. The modification was durable with largely intact flame retardancy and antimicrobial properties after 30 washing cycles.

Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

NASA Astrophysics Data System (ADS)

Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

2010-03-01

Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

Compressive Properties of Open-Cell Al Hybrid Foams at Different Temperatures

PubMed Central

Liu, Jiaan; Si, Fujian; Zhu, Xianyong; Liu, Yaohui; Zhang, Jiawei; Liu, Yan; Zhang, Chengchun

2017-01-01

Hybrid Ni/Al foams were fabricated by depositing electroless Ni–P (EN) coatings on open-cell Al foam substrate to obtain enhanced mechanical properties. The microstructure, chemical components and phases of the hybrid foams were observed and analyzed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The mechanical properties of the foams were studied by compressive tests at different temperatures. The experiment results show that the coating is mainly composed of Ni and P elements. There was neither defect at the interface nor crack in the coatings, indicating that the EN coatings had fine adhesion to the Al substrate. The compressive strengths and energy absorption capacities of the as-received foam and hybrid foams decrease with the increasing testing temperatures, but the hybrid foams exhibit a lower decrement rate than the as-received foam. This might be attributed to the different failure mechanisms at different testing temperatures, which is conformed by fractography observation. PMID:28772456

Control of p-type and n-type thermoelectric properties of bismuth telluride thin films by combinatorial sputter coating technology

NASA Astrophysics Data System (ADS)

Goto, Masahiro; Sasaki, Michiko; Xu, Yibin; Zhan, Tianzhuo; Isoda, Yukihiro; Shinohara, Yoshikazu

2017-06-01

p- and n-type bismuth telluride thin films have been synthesized by using a combinatorial sputter coating system (COSCOS). The crystal structure and crystal preferred orientation of the thin films were changed by controlling the coating condition of the radio frequency (RF) power during the sputter coating. As a result, the p- and n-type films and their dimensionless figure of merit (ZT) were optimized by the technique. The properties of the thin films such as the crystal structure, crystal preferred orientation, material composition and surface morphology were analyzed by X-ray diffraction, energy-dispersive X-ray spectroscopy and atomic force microscopy. Also, the thermoelectric properties of the Seebeck coefficient, electrical conductivity and thermal conductivity were measured. ZT for n- and p-type bismuth telluride thin films was found to be 0.27 and 0.40 at RF powers of 90 and 120 W, respectively. The proposed technology can be used to fabricate thermoelectric p-n modules of bismuth telluride without any doping process.

Effect of surface coating with magnesium stearate via mechanical dry powder coating approach on the aerosol performance of micronized drug powders from dry powder inhalers.

PubMed

Zhou, Qi Tony; Qu, Li; Gengenbach, Thomas; Larson, Ian; Stewart, Peter J; Morton, David A V

2013-03-01

The objective of this study was to investigate the effect of particle surface coating with magnesium stearate on the aerosolization of dry powder inhaler formulations. Micronized salbutamol sulphate as a model drug was dry coated with magnesium stearate using a mechanofusion technique. The coating quality was characterized by X-ray photoelectron spectroscopy. Powder bulk and flow properties were assessed by bulk densities and shear cell measurements. The aerosol performance was studied by laser diffraction and supported by a twin-stage impinger. High degrees of coating coverage were achieved after mechanofusion, as measured by X-ray photoelectron spectroscopy. Concomitant significant increases occurred in powder bulk densities and in aerosol performance after coating. The apparent optimum performance corresponded with using 2% w/w magnesium stearate. In contrast, traditional blending resulted in no significant changes in either bulk or aerosolization behaviour compared to the untreated sample. It is believed that conventional low-shear blending provides insufficient energy levels to expose host micronized particle surfaces from agglomerates and to distribute guest coating material effectively for coating. A simple ultra-high-shear mechanical dry powder coating step was shown as highly effective in producing ultra-thin coatings on micronized powders and to substantially improve the powder aerosolization efficiency.

Generation of drugs coated iron nanoparticles through high energy ball milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Radhika Devi, A.; Murty, B. S.; Chelvane, J. A.

The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

NASA Astrophysics Data System (ADS)

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying.

PubMed

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Polyethylene glycol coated CoFe{sub 2}O{sub 4} nanoparticles: A potential spinel ferrite for biomedical applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Humbe, Ashok V.; Birajdar, Shankar D.; Jadhav, K. M., E-mail: drjadhavkm@gmail.com

2015-06-24

The structural and magnetic properties of the polyethylene glycol (PEG) coated cobalt spinel ferrite (CoFe{sub 2}O{sub 4}) nanoparticles have been reported in the present study. CoFe{sub 2}O{sub 4} nanoparticles were prepared by sol-gel auto-combustion method using citric acid + ethylene glycol as a fuel. The prepared powder of cobalt ferrite nanoparticles was annealed at 600°C for 6h and used for further study. The structural characterization of CoFe{sub 2}O{sub 4} nanoparticles were carried out by X-ray diffraction technique. The X-ray analysis confirmed the formation of single phase cubic spinel structure. The crystallite size, Lattice constant and X-ray density of the PEGmore » coated CoFe{sub 2}O{sub 4} nanoparticles were calculated by using XRD data. The presence of PEG on CoFe{sub 2}O{sub 4} nanoparticles and reduced agglomeration in the CoFe{sub 2}O{sub 4} nanoparticles were revealed by SEM studies. The magnetic properties were studied by pulse field hysteresis loop tracer technique at a room temperature. The magnetic parameters such as saturation magnetization, remanence magnetization, coercivity etc have been obtained. These magnetic parameters were get decreased by PEG coating.« less

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

The effect of substrate bias voltages on impact resistance of CrAlN coatings deposited by modified ion beam enhanced magnetron sputtering

NASA Astrophysics Data System (ADS)

Chunyan, Yu; Linhai, Tian; Yinghui, Wei; Shebin, Wang; Tianbao, Li; Bingshe, Xu

2009-01-01

CrAlN coatings were deposited on silicon and AISI H13 steel substrates using a modified ion beam enhanced magnetron sputtering system. The effect of substrate negative bias voltages on the impact property of the CrAlN coatings was studied. The X-ray diffraction (XRD) data show that all CrAlN coatings were crystallized in the cubic NaCl B1 structure, with the (1 1 1), (2 0 0) (2 2 0) and (2 2 2) diffraction peaks observed. Two-dimensional surface morphologies of CrAlN coatings were investigated by atomic force microscope (AFM). The results show that with increasing substrate bias voltage the coatings became more compact and denser, and the microhardness and fracture toughness of the coatings increased correspondingly. In the dynamic impact resistance tests, the CrAlN coatings displayed better impact resistance with the increase of bias voltage, due to the reduced emergence and propagation of the cracks in coatings with a very dense structure and the increase of hardness and fracture toughness in coatings.

Structure and Infrared Emissivity Properties of the MAO Coatings Formed on TC4 Alloys in K2ZrF6-Based Solution

PubMed Central

Li, Ying; Hu, Dan; Xi, Zhengping

2018-01-01

Micro-arc oxidation (MAO) ceramic coatings were formed on TC4 alloy surface in silicate and metaphosphate electrolytes based with K2ZrF6 for various concentrations. X-ray diffraction (XRD), Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) were used to characterize the phase composition, microstructure and chemical compositions of the coatings. The infrared emissivity of the coatings was measured at 50 °C in a wavelength range of 8–20 µm. The microstructural observations all revealed the typical porousstructures. Moreover, adecline in roughness and thickness of the prepared coatings can be observed when the concentration of K2ZrF6 increases. Combined with the results of XRD and XPS, it was found that all the oxides existed as the amorphous form in the coatings except the TiO2 phase. The coatings exhibited the highest infrared emissivity value (about 0.89) when the concentration of K2ZrF6 was 6 g/L, which was possibly attributed to the defect microstructure and the optimal role of ZrO2. PMID:29414841

Investigation of the Effect of Residual Stress Gradient on the Wear Behavior of PVD Thin Films

NASA Astrophysics Data System (ADS)

Tlili, B.; Nouveau, C.; Guillemot, G.; Besnard, A.; Barkaoui, A.

2018-02-01

The control of residual stresses has been seldom investigated in multilayer coatings dedicated to improvement of wear behavior. Here, we report the preparation and characterization of superposed structures composed of Cr, CrN and CrAlN layers. Nano-multilayers CrN/CrAlN and Cr/CrN/CrAlN were deposited by Physical Vapor Deposition (PVD) onto Si (100) and AISI4140 steel substrates. The Cr, CrN and CrAlN monolayers were developed with an innovative approach in PVD coatings technologies corresponding to deposition with different residual stresses levels. Composition and wear tracks morphologies of the coatings were characterized by scanning electron microscopy, high-resolution transmission electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, energy-dispersive x-ray spectroscopy, x-ray diffraction and 3D-surface analyzer. The mechanical properties (hardness, residual stresses and wear) were investigated by nanoindentation, interferometry and micro-tribometry (fretting-wear tests). Observations suggest that multilayer coatings are composed mostly of nanocrystalline. The residual stresses level in the films has practically affected all the physicochemical and mechanical properties as well as the wear behavior. Consequently, it is demonstrated that the coating containing moderate stresses has a better wear behavior compared to the coating developed with higher residual stresses. The friction contact between coated samples and alumina balls shows also a large variety of wear mechanisms. In particular, the abrasive wear of the coatings was a combination of plastic deformation, fine microcracking and microspallation. The application of these multilayers will be wood machining of green wood.

Surface properties of AZ91 magnesium alloy after PEO treatment using molybdate salts and low current densities

NASA Astrophysics Data System (ADS)

Pezzato, Luca; Brunelli, Katya; Napolitani, Enrico; Magrini, Maurizio; Dabalà, Manuele

2015-12-01

Plasma electrolytic oxidation (PEO) process is a recently developed electrochemical method used to produce on the surface of various metals oxide ceramic coatings that improve corrosion and wear properties of the substrate. In this work, PEO process was applied on AZ91 magnesium alloy using low current densities (0.05 A/cm2) and an alkaline solution of silicates with different concentrations of sodium molybdate (0.3-3 g/l). The effect of the low current densities of process and of molybdate salts on the corrosion resistance of the coatings was studied with potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS) in chloride and sulfate environment. The morphology, the phases and the chemical composition of the coatings were examined using a scanning electron microscope equipped with EDS, X-ray diffraction, secondary ion mass spectrometry and X-ray photoelectron spectroscopy. The corrosion properties of the PEO coated samples were remarkably improved if compared with the uncoated samples. The addition of sodium molybdate, in determinate conditions, had a positive effect on the characteristics of the coatings in terms of corrosion resistance.

Fabricating Blazed Diffraction Gratings by X-Ray Lithography

NASA Technical Reports Server (NTRS)

Mouroulis, Pantazis; Hartley, Frank; Wilson, Daniel

2004-01-01

Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

Direct morphological comparison of vacuum plasma sprayed and detonation gun sprayed hydroxyapatite coatings for orthopaedic applications.

PubMed

Gledhill, H C; Turner, I G; Doyle, C

1999-02-01

Hydroxyapatite coatings on titanium substrates were produced using two thermal spray techniques vacuum plasma spraying and detonation gun spraying. X-ray diffraction was used to compare crystallinity and residual stresses in the coatings. Porosity was measured using optical microscopy in conjunction with an image analysis system. Scanning electron microscopy and surface roughness measurements were used to characterise the surface morphologies of the coatings. The vacuum plasma sprayed coatings were found to have a lower residual stress, a higher crystallinity and a higher level of porosity than the detonation gun coatings. It is concluded that consideration needs to be given to the significance of such variations within the clinical context.

[Preparation of coated tablets of glycyrrhetic acid-HP-beta-cyclodextrin tablets for colon-specific release].

PubMed

Cui, Qi-Hua; Cui, Jing-Hao; Zhang, Jin-Jin

2008-10-01

To prepare coated tablets of glycyrrhetinic acid and hydroxypropyl-beta-cyclodextrin (GTA-HP-beta-CYD) inclusion complex tablets for colon-specific release. In order to improve the solubility of GTA, the GTA-HP-beta-CYD inclusion complex was prepared by ultrasonic-lyophilization technique and its formation were characterized by X-ray powder diffraction profiles and infrared spectrometry. The effects of inclusion condition on the inclusion efficiency and stability coefficient of inclusion complex were investigated, respectively. After prepared GTA-HP-beta-CYD tablets by powder direct compression, the pH dependant polymer Eudragit III and/or mixed with Eudragit II were used for further coating materials in fluid-bed coater. The influences of coating weight on the GTA release in different pH conditions were evaluated to establish the method for prepering colon specific delivery tablets with pulsed release properties. The formation of inclusion complexes were proved by X-ray powder diffraction profile and phase solubility curve. The effect of pH value of solvent was played critical role on the preparation of GTA- HP-beta-CYD inclusion complex. And the inclusion efficiency of GTA was 9. 3% and the solubility was increased to 54. 6 times at optimized method. The Eudragit III coated GTA- HP-beta-CYD tablets with coating weight 10% and 16% were showed pH dependant colon specific release profiles with slow release rate. The release profile of tablets coated with the mixture of Eudragit II and Eudragit III (1:2) were indicated typical pH dependant colon specific and pulsed release properties while the coating weight was 17%. The preliminary method for preparation of colon specific release tablets containing glycyrrhetinic acid with improved solubility was established for further in vivo therapeutic experiment.

Comparative examination of the microstructure and high temperature oxidation performance of NiCrBSi flame sprayed and pack cementation coatings

NASA Astrophysics Data System (ADS)

Chaliampalias, D.; Vourlias, G.; Pavlidou, E.; Skolianos, S.; Chrissafis, K.; Stergioudis, G.

2009-01-01

Coatings formed from NiCrBSi powder were deposited by thermal spray and pack cementation processes on low carbon steel. The microstructure and morphology of the coatings were studied by scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD). Flame sprayed coatings exhibited high porosity and were mechanically bonded to the substrate while pack cementation coatings were more compact and chemically bonded to the substrate. The microhardness and the high temperature oxidation resistance of the coated samples were evaluated by a Vickers microhardness tester and by thermogravimetric measurements (TG), respectively. Pack cementation coatings showed higher hardness and were more protective to high temperature environments than the flame sprayed coatings.

Phosphate Remediation and Recovery from Lake Water using Modified Iron Oxide-based Adsorbents

EPA Science Inventory

Adsorption behavior of Bayoxide ® E33 (E33) and three E33-modified sorbents for the removal of phosphate from lake water was investigated in this study. E33-modified sorbents were synthesized by coating with manganese and nanoparticles. Characterization was done by X-ray diffract...

Analytical methods to characterize heterogeneous raw material for thermal spray process: cored wire Inconel 625

NASA Astrophysics Data System (ADS)

Lindner, T.; Bonebeau, S.; Drehmann, R.; Grund, T.; Pawlowski, L.; Lampke, T.

2016-03-01

In wire arc spraying, the raw material needs to exhibit sufficient formability and ductility in order to be processed. By using an electrically conductive, metallic sheath, it is also possible to handle non-conductive and/or brittle materials such as ceramics. In comparison to massive wire, a cored wire has a heterogeneous material distribution. Due to this fact and the complex thermodynamic processes during wire arc spraying, it is very difficult to predict the resulting chemical composition in the coating with sufficient accuracy. An Inconel 625 cored wire was used to investigate this issue. In a comparative study, the analytical results of the raw material were compared to arc sprayed coatings and droplets, which were remelted in an arc furnace under argon atmosphere. Energy-dispersive X-ray spectroscopy (EDX) and X-ray fluorescence (XRF) analysis were used to determine the chemical composition. The phase determination was performed by X-ray diffraction (XRD). The results were related to the manufacturer specifications and evaluated in respect to differences in the chemical composition. The comparison between the feedstock powder, the remelted droplets and the thermally sprayed coatings allows to evaluate the influence of the processing methods on the resulting chemical and phase composition.

The effect of heat treatment on structural and electronic properties of niobium nitride prepared by a thermal diffusion method

DOE PAGES

Farha, Ashraf Hassan; Ozkendir, Osman Murat; Elsayed-Ali, Hani E.; ...

2016-11-15

NbN coatings are prepared onto Nb substrate by thermal diffusion at high temperatures. The formation of NbN coating by thermal diffusion was studied in the range of 1250-1500 °C at constant nitrogen background gas pressure (1.3x10 -3 Pa) and processing time (180 min). The electronic and crystal structures of the NbN coatings were investigated. It was found that nitrogen diffuses into Nb forming the Nb-N solid solution (bcc) a-NbN phase that starts to appear above 1250 °C. Increasing the processing temperature gives richer a-phase concentration. Besides, X-ray absorption spectroscopy (XAS) was performed to study the electronic structure of the NbNmore » layer. The results of the electronic structural study corroborate the crystal structural analysis. The Nb M 3,2 edge X-ray absorption spectroscopy (XAS) spectrum shows strong temperature dependence. At the highest processing temperature (1500 °C), the number of d holes increased. Nitrogen diffusion into Nb is resulting to increase electrostatic interaction between d electron and core hole. Lastly, for the studied conditions, only the α-NbN was observed in the X-ray diffraction patterns.« less

The effect of heat treatment on structural and electronic properties of niobium nitride prepared by a thermal diffusion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farha, Ashraf Hassan; Ozkendir, Osman Murat; Elsayed-Ali, Hani E.

NbN coatings are prepared onto Nb substrate by thermal diffusion at high temperatures. The formation of NbN coating by thermal diffusion was studied in the range of 1250-1500 °C at constant nitrogen background gas pressure (1.3x10 -3 Pa) and processing time (180 min). The electronic and crystal structures of the NbN coatings were investigated. It was found that nitrogen diffuses into Nb forming the Nb-N solid solution (bcc) a-NbN phase that starts to appear above 1250 °C. Increasing the processing temperature gives richer a-phase concentration. Besides, X-ray absorption spectroscopy (XAS) was performed to study the electronic structure of the NbNmore » layer. The results of the electronic structural study corroborate the crystal structural analysis. The Nb M 3,2 edge X-ray absorption spectroscopy (XAS) spectrum shows strong temperature dependence. At the highest processing temperature (1500 °C), the number of d holes increased. Nitrogen diffusion into Nb is resulting to increase electrostatic interaction between d electron and core hole. Lastly, for the studied conditions, only the α-NbN was observed in the X-ray diffraction patterns.« less

Structural study of Mg doped cobalt ferrite thin films on ITO coated glass substrate

NASA Astrophysics Data System (ADS)

Suthar, Mahesh; Bapna, Komal; Kumar, Kishor; Ahuja, B. L.

2018-05-01

We have synthesized thin films of Co1-xMgxFe2O4 (x = 0, 0.4, 0.6, 0.8, 1) on transparent conducting indium tin oxide (ITO) coated glass substrate by pulsed laser deposition method. The structural properties of the grown films were analyzed by the X-ray diffraction and Raman spectroscopy, which suggest the single phase growth of these films. Raman spectra revealed the incorporation of Mg ions into CoFe2O4 lattice and suggest that the Mg ions initially go both to the octahedral and tetrahedral sites upto a certain concentration. For higher concentration, Mg ions prefer to occupy the tetrahedral sites.

Achromatic nested Kirkpatrick–Baez mirror optics for hard X-ray nanofocusing

PubMed Central

Liu, Wenjun; Ice, Gene E.; Assoufid, Lahsen; Liu, Chian; Shi, Bing; Khachatryan, Ruben; Qian, Jun; Zschack, Paul; Tischler, Jonathan Z.; Choi, J.-Y.

2011-01-01

The first test of nanoscale-focusing Kirkpatrick–Baez (KB) mirrors in the nested (or Montel) configuration used at a hard X-ray synchrotron beamline is reported. The two mirrors are both 40 mm long and coated with Pt to produce a focal length of 60 mm at 3 mrad incident angle, and collect up to a 120 µm by 120 µm incident X-ray beam with maximum angular acceptance of 2 mrad and a broad bandwidth of energies up to 30 keV. In an initial test a focal spot of about 150 nm in both horizontal and vertical directions was achieved with either polychromatic or monochromatic beam. The nested mirror geometry, with two mirrors mounted side-by-side and perpendicular to each other, is significantly more compact and provides higher demagnification than the traditional sequential KB mirror arrangement. Ultimately, nested mirrors can focus larger divergence to improve the diffraction limit of achromatic optics. A major challenge with the fabrication of the required mirrors is the need for near-perfect mirror surfaces near the edge of at least one of the mirrors. Special polishing procedures and surface profile coating were used to preserve the mirror surface quality at the reflecting edge. Further developments aimed at achieving diffraction-limited focusing below 50 nm are underway. PMID:21685674

Iron-based soft magnetic composites with Mn-Zn ferrite nanoparticles coating obtained by sol-gel method

NASA Astrophysics Data System (ADS)

Wu, Shen; Sun, Aizhi; Xu, Wenhuan; Zhang, Qian; Zhai, Fuqiang; Logan, Philip; Volinsky, Alex A.

2012-11-01

This paper focuses on iron-based soft magnetic composites which were synthesized by utilizing Mn-Zn ferrite nanoparticles to coat iron powder. The nanocrystalline iron powders, with an average particle diameter of 20 nm, were obtained via the sol-gel method. Scanning electron microscopy, energy dispersive X-ray spectroscopy and distribution maps show that the iron particle surface is covered with a thin layer of Mn-Zn ferrites. Mn-Zn ferrite uniformly coated the surface of the powder particles, resulting in a reduced imaginary permeability, increased electrical resistivity and a higher operating frequency of the synthesized magnets. Mn-Zn ferrite coated samples have higher permeability and lower magnetic loss when compared with the non-magnetic epoxy resin coated compacts. The real part of permeability increases by 33.5% when compared with the epoxy resin coated samples at 10 kHz. The effects of heat treatment temperature on crystalline phase formation and on the magnetic properties of the Mn-Zn ferrite were investigated via X-ray diffraction and a vibrating sample magnetometer. Ferrites decomposed to FeO and MnO after annealing above 400 °C in nitrogen; thus it is the optimum annealing temperature to attain the desired permeability.

Gold coated metal nanostructures grown by glancing angle deposition and pulsed electroplating

NASA Astrophysics Data System (ADS)

Grüner, Christoph; Reeck, Pascal; Jacobs, Paul-Philipp; Liedtke, Susann; Lotnyk, Andriy; Rauschenbach, Bernd

2018-05-01

Nickel based nanostructures are grown by glancing angle deposition (GLAD) on flat and pre-patterned substrates. These fabricated porous thin films were subsequently coated by pulsed electroplating with gold. The morphology and conformity of the gold coating were investigated by scanning electron microscopy and X-ray diffraction. Controlled growth of closed gold layers on the nanostructures could be achieved, while the open-pore structure of the nanosculptured thin films was preserved. Such gold coated nanostructures are a candidate for optical sensing and catalysis applications. The demonstrated method can be applied for numerous material combinations, allowing to provide GLAD thin films with new surface properties.

Tribological characterization of TiN coatings prepared by magnetron sputtering

NASA Astrophysics Data System (ADS)

Makwana, Nishant S.; Chauhan, Kamlesh V.; Sonera, Akshay L.; Chauhan, Dharmesh B.; Dave, Divyeshkumar P.; Rawal, Sushant K.

2018-05-01

Titanium nitride (TiN) coating deposited on aluminium and brass pin substrates using RF reactive magnetron sputtering. The structural properties and surface morphology were characterized by X-ray diffraction (XRD), atomic force microscope (AFM) and field emission scanning electron microscope (FE-SEM). There was formation of (101) Ti2N, (110) TiN2 and (102) TiN0.30 peaks at 3.5Pa, 2Pa and 1.25Pa sputtering pressure respectively. The tribological properties of coating were inspected using pin on disc tribometer equipment. It was observed that TiN coated aluminium and brass pins demonstrated improved wear resistance than uncoated aluminium and brass pins.

Investigation of ZrO x /ZrC-ZrN/Zr thin-film structural evolution and their degradation using X-ray diffraction and Raman spectrometry

NASA Astrophysics Data System (ADS)

Usmani, B.; Vijay, V.; Chhibber, R.; Dixit, A.

2016-11-01

The thin-film structures of DC/FR magnetron-sputtered ZrO x /ZrC-ZrN/Zr tandem solar-selective coatings are investigated using X-ray diffraction and room-temperature Raman spectroscopic measurements. These studies suggest that the major contribution is coming from h-ZrN0.28, c-ZrC, h-Zr3C2 crystallographic phases in ZrN-ZrC absorber layer, in conjunction with mixed ZrO x crystallographic phases. The change in structure for thermally annealed samples has been examined and observed that cubic and hexagonal ZrO x phase converted partially into tetragonal and monoclinic ZrO x phases, whereas hexagonal and cubic ZrN phases, from absorber layer, have not been observed for these thermally treated samples in air. These studies suggest that thermal treatment may lead to the loss of ZrN phase in absorber, degrading the thermal response for the desired wavelength range in open ambient conditions in contrast to vacuum conditions.

Improvement of Corrosion Resistance of Binary Mg-Ca Alloys Using Duplex Aluminum-Chromium Coatings

NASA Astrophysics Data System (ADS)

Daroonparvar, Mohammadreza; Yajid, Muhamad Azizi Mat; Yusof, Noordin Mohd; Bakhsheshi-Rad, Hamid Reza; Adabi, Mohsen; Hamzah, Esah; Kamali, Hussein Ali

2015-07-01

Al-AlCr was coated on Mg-Ca and Mg-Zn-Ce-La alloys using physical vapor deposition method. The surface morphology of the specimens was characterized by x-ray diffraction, scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and atomic force microscopy (AFM). The AFM results indicated that the average surface roughness of Al-AlCr coating on the Mg-Ca alloy is much lower than that of Al-AlCr coating on the Mg-Zn-Ce-La alloy. However, Al-AlCr coating on the Mg-Ca alloy presented a more compact structure with fewer pores, pinholes, and cracks than Al-AlCr coating on the Mg-Zn-Ce-La alloy. Electrochemical studies revealed that the novel coating (Al-AlCr) can remarkably reduce the corrosion rate of the Mg-Ca alloy in 3.5 wt.% NaCl solution. It was seen that the anodic current density of the Al-AlCr-coated Mg-Ca alloy was very small when compared to the Al-AlCr-coated Mg-Zn-Ce-La and uncoated alloys. Impedance modulus ( Z) of the Al-AlCr-coated samples was higher than that of the bare Mg alloys. Z of Al-AlCr-coated Mg-Ca alloy was higher than that of the Al-AlCr-coated Mg-Zn-Ce-La alloy at low frequency.

Effects of ultraviolet radiation on lattice imperfections in pyrolytic boron nitride.

NASA Technical Reports Server (NTRS)

Buckley, J. D.; Cooley, J. A.

1971-01-01

Pyrolitic boron nitride was exposed to 310 equivalent sun hours of ultraviolet radiation in a space environment simulator with the objective to evaluate its applicability as a pigment for a thermal control coating and to identify radiation damage using X-ray diffraction techniques. Lattice parameter comparisons show a definite increase in lattice imperfections in the crystal structure resulting from the ultraviolet irradiation. This sensitivity to radiation damage makes pyrolitic boron nitride unsuitable as a pigment for thermal control coating.

Effects of Laser Re-melting on the Corrosion Properties of HVOF Coatings

NASA Astrophysics Data System (ADS)

Yilbas, B. S.; Toor, I. H.; Patel, F.; Baig, M. A.

2013-05-01

HVOF coating of Inconel 625 powder on carbon steel is carried out. Laser melting of the resulting coating is realized to improve coating structural integrity. Morphological and microstructural changes are examined in the coating prior and after laser treatment process using scanning electron microscopy, energy dispersive spectroscopy, and x-ray diffraction (XRD). The residual stress developed is measured on the surface vicinity of the laser-treated coating using the XRD technique. The corrosion resistance of the laser-treated and untreated coating surfaces is measured, incorporating the potentiodynamic tests in 0.5 M NaCl aqueous solution. It is found that laser treatment reduces the pores and produces cellular structures with different sizes and orientations in the coating. Laser-controlled melting improves the corrosion resistance of the coating surface.

Development of new magnetic nanoparticles: Oligochitosan obtained by γ-rays and -coated Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Le Thi, Thao Nguyen; Nguyen, Thi Hiep; Hoang, Dong Quy; Tran, Tuong, Vi; Nguyen, Ngoc Thuy; Nguyen, Dai Hai

2017-11-01

Oligochitosan (OCS) have been utilized as a potential bioactive material for improving food quality and human health. In this study, superparamagnetic iron oxide (Fe3O4) nanoparticles were originally coated with OCS irradiated by gamma rays for their possible biomedical applications. The formation of Fe3O4@OCS was characterized by Fourier transform infrared (FT-IR), X-ray diffraction patterns (XRD), energy dispersive X-ray spectroscopy (EDS) and thermogravimetric analysis (TGA). In addition, the superparamagnetic properties and sizes and morphologies of Fe3O4 and Fe3O4@OCS nanoparticles were demonstrated by vibrating sample magnetometer (VSM) and transmission electron microscopy (TEM), respectively. These results indicated that Fe3O4@OCS nanoparticles still maintained their superparamagnetic properties after polymeric coating, and were nearly spherical in shape with average diameter of 14.4 ± 0.31 nm, compared with 11.8 ± 0.52 nm of bare Fe3O4 nanoparticles, respectively. As a result, Fe3O4@OCS nanoparticles may serve as a promising platform for the development of new magnetic materials, which could be useful for biomedical applications.

Influence of Zeolite Coating on the Corrosion Resistance of AZ91D Magnesium Alloy

PubMed Central

Banerjee, P. Chakraborty; Woo, Ren Ping; Grayson, Sam Matthew; Majumder, Amrita; Raman, R. K. Singh

2014-01-01

The protective performance of zeolite coating on AZ91D magnesium alloy was evaluated using potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) in 0.1 M sodium chloride solution (NaCl). Electrical equivalent circuit (EEC) was developed based upon hypothetical corrosion mechanisms and simulated to correspond to the experimental data. The morphology and the chemical nature of the coating were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. Post corrosion morphologies of the zeolite coated and the uncoated AZ91D alloy were investigated using SEM. The corrosion resistance of the zeolite coated specimen was at least one order of magnitude higher than the uncoated specimen. PMID:28788178

Influence of Zeolite Coating on the Corrosion Resistance of AZ91D Magnesium Alloy.

PubMed

Banerjee, P Chakraborty; Woo, Ren Ping; Grayson, Sam Matthew; Majumder, Amrita; Raman, R K Singh

2014-08-22

The protective performance of zeolite coating on AZ91D magnesium alloy was evaluated using potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) in 0.1 M sodium chloride solution (NaCl). Electrical equivalent circuit (EEC) was developed based upon hypothetical corrosion mechanisms and simulated to correspond to the experimental data. The morphology and the chemical nature of the coating were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. Post corrosion morphologies of the zeolite coated and the uncoated AZ91D alloy were investigated using SEM. The corrosion resistance of the zeolite coated specimen was at least one order of magnitude higher than the uncoated specimen.

Strontium coating by electrochemical deposition improves implant osseointegration in osteopenic models

PubMed Central

LIANG, YONGQIANG; LI, HAOYAN; XU, JIANG; LI, XIN; LI, XINCHANG; YAN, YUTING; QI, MENGCHUN; HU, MIN

2015-01-01

Osteopenia, a preclinical state of osteoporosis, restricts the application of adult orthodontic implant anchorage and tooth implantation. Strontium (Sr) is able to promote bone formation and inhibit bone absorption. The aim of the present study was to evaluate a new method for improving the success rate of dental implantation. In this study, an electrochemical deposition (ECD) method was used to prepare a Sr coating on a titanium implant. The coating composition was investigated by energy dispersive X-ray spectroscopy and X-ray diffraction, and the surface morphology of the coating was studied using scanning electron microscopy. A total of 24 Sprague-Dawley rats received bilateral ovariectomy (OVX) and an additional 12 rats underwent a sham surgery. All rats were then implanted in the bilateral tibiae with titanium mini-implants with or without a Sr coating. The results of histological examination and a fluorescence double labeling assay showed strong new bone formation with a wider zone between the double labels, a higher rate of bone mineralization and better osseointegration in the OVX rats that received Sr-coated implants compared with the OVX rats that received uncoated implants. The study indicates that Sr coatings are easily applied by an ECD method, and that Sr coatings have a promoting effect on implant osseointegration in animals with osteopenia. PMID:25452797

Electrochemical performance of La2O3/Li2O/TiO2 nano-particle coated cathode material LiFePO4.

PubMed

Wang, Hong; Yang, Chi; Liu, Shu-Xin

2014-09-01

Cathode material, LiFePO4 was modified by coating with a thin layer of La2O3/Li2O/TiO2 nano-particles for improving its performance for lithium ion batteries. The morphology and structure of the modified cathode material were characterized by powder X-ray diffraction, scanning electron microcopy and AES. The performance of the battery with the modified cathode material, including cycling stability, C-rate discharge was examined. The results show that the battery composed of the coated cathode materials can discharge at a large current density and show stable cycling performance in the range from 2.5 to 4.0 V. The rate of Li ion diffusion increases in the battery with the La2O3/Li2O/TiO2-coated LiFePO4 as a cathode and the coating layer may acts as a faster ion conductor (La(2/3-x)Li(3x)TiO3).

Electron-Beam Deposition of Superconducting Molybdenum Thin Films for the Development of Mo/Au TES X-Ray Microcalorimeter

NASA Technical Reports Server (NTRS)

Finkbeiner, Fred Michael; Adams, Joseph S.; Bandler, Simon R.; Betancour-Martinez, Gabriele L.; Brown, Ari David; Chang, Meng-Ping; Chervenak, James A.; Chiao, Meng P.; Datesman, Aaron; Eckart, Megan E.;

Enhanced protective properties of epoxy/polyaniline-camphorsulfonate nanocomposite coating on an ultrafine-grained metallic surface

NASA Astrophysics Data System (ADS)

Pour-Ali, Sadegh; Kiani-Rashid, Alireza; Babakhani, Abolfazl; Davoodi, Ali

2016-07-01

An ultrafine-grained surface layer on mild steel substrate with average grain size of 77 nm was produced through wire brushing process. Surface grain size was determined through transmission electron microscopy and X-ray diffraction methods. This substrate was coated with epoxy and an in situ synthesized epoxy/polyaniline-camphorsulfonate (epoxy/PANI-CSA) nanocomposite. The corrosion behavior was studied by open circuit potential, potentiodynamic polarization and impedance measurements. Results of electrochemical tests evidenced the enhanced protective properties of epoxy/PANI-CSA coating on the substrate with ultrafine-grained surface.

Role of Oxides and Porosity on High-Temperature Oxidation of Liquid-Fueled HVOF Thermal-Sprayed Ni50Cr Coatings

NASA Astrophysics Data System (ADS)

Song, B.; Bai, M.; Voisey, K. T.; Hussain, T.

2017-02-01

High chromium content in Ni50Cr thermally sprayed coatings can generate a dense and protective scale at the surface of coating. Thus, the Ni50Cr coating is widely used in high-temperature oxidation and corrosion applications. A commercially available gas atomized Ni50Cr powder was sprayed onto a power plant steel (ASME P92) using a liquid-fueled high velocity oxy-fuel thermal spray with three processing parameters in this study. Microstructure of as-sprayed coatings was examined using oxygen content analysis, mercury intrusion porosimetry, scanning electron microscope (SEM), energy-dispersive x-ray spectroscopy (EDX) and x-ray diffraction (XRD). Short-term air oxidation tests (4 h) of freestanding coatings (without boiler steel substrate) in a thermogravimetric analyzer at 700 °C were performed to obtain the kinetics of oxidation of the as-sprayed coating. Long-term air oxidation tests (100 h) of the coated substrates were performed at same temperature to obtain the oxidation products for further characterization in detail using SEM/EDX and XRD. In all samples, oxides of various morphologies developed on top of the Ni50Cr coatings. Cr2O3 was the main oxidation product on the surface of all three coatings. The coating with medium porosity and medium oxygen content has the best high-temperature oxidation performance in this study.

Effects of laser remelting on microstructures and immersion corrosion performance of arc sprayed Al coating in 3.5% NaCl solution

NASA Astrophysics Data System (ADS)

Sun, Ze; Zhang, Donghui; Yan, Baoxu; Kong, Dejun

2018-02-01

An arc sprayed aluminum (Al) coating on S355 steel was processed using a laser remelting (LR). The microstructures, chemical element composition, and phases of the obtained Al coating were analyzed using a field mission scanning electronic microscope (FESEM), energy dispersive spectrometer (EDS), and X-ray diffractometer (XRD), respectively, and the residual stresses were measured using an X-ray diffraction stress tester. The immersion corrosion tests and potentiodynamic polarization of Al coating in 3.5% NaCl solution were performed to investigate the effects of LR on its immersion corrosion behaviors, and the corrosion mechanism of Al coating was also discussed. The results show that the arc sprayed Al coating is composed of Al phase, while that by LR is composed of Al-Fe and AlO4FeO6 phases, and the porosities and cracks in the arc sprayed Al coating are eliminated by LR, The residual stress of arc sprayed Al coating is -5.6 ± 18 MPa, while that after LR is 137.9 ± 12 MPa, which deduces the immersion corrosion resistance of Al coating. The corrosion mechanism of arc sprayed Al coating is pitting corrosion and crevice corrosion, while that by LR is uniform corrosion and pitting corrosion. The corrosion potential of arc sprayed Al coating by LR shifts positively, which improves its immersion corrosion resistance.

The pyrolysis characteristics of moso bamboo

Treesearch

Zehui Jiang; Zhijia Liu; Benhua Fei; Zhiyong Cai; Yan Yu; Xing’e Liu

2012-01-01

In the research, thermogravimetry (TG), a combination of thermogravimetry and Fourier transform infrared spectrometer (TG–FTIR) and X-ray diffraction (XRD) were used to investigate pyrolysis characteristics of moso bamboo (Phyllostachys pubescens). The Flynn–Wall–Ozawa and Coats–Redfern (modified) methods were used to determine the apparent activation energy (

Study of the recrystallization in coated pellets - effect of coating on API crystallinity.

PubMed

Nikowitz, Krisztina; Pintye-Hódi, Klára; Regdon, Géza

2013-02-14

Coated diltiazem hydrochloride-containing pellets were prepared using the solution layering technique. Unusual thermal behavior was detected with differential scanning calorimetry (DSC) and its source was determined using thermogravimetry (TG), X-ray powder diffraction (XRPD) and hot-stage microscopy. The coated pellets contained diltiazem hydrochloride both in crystalline and amorphous form. Crystallization occurs on heat treatment causing an exothermic peak on the DSC curves that only appears in pellets containing both diltiazem hydrochloride and the coating. Results indicate that the amorphous fraction is situated in the coating layer. The migration of drugs into the coating layer can cause changes in its degree of crystallinity. Polymeric coating materials should therefore be investigated as possible crystallization inhibitors. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS₂ Nanoparticles.

PubMed

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev; Tenne, Reshef

2018-02-26

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS₂ (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

Multivalent Mn-doped TiO2 thin films

NASA Astrophysics Data System (ADS)

Lin, C. Y. W.; Channei, D.; Koshy, P.; Nakaruk, A.; Sorrell, C. C.

2012-07-01

Thin films of TiO2 doped with Mn were deposited on F-doped SnO2-coated glass using spin coating. The concentration of the dopant was in the range 0-7 wt% Mn (metal basis). The films were examined in terms of the structural, chemical, and optical properties. Glancing angle X-ray diffraction data show that the films consisted of the anatase polymorph of TiO2, without any contaminant phases. The X-ray photoelectron spectroscopy data indicate the presence of Mn3+ and Mn4+ in the doped films as well as atomic disorder and associated structural distortion. Ultraviolet-visible spectrophotometry data show that the optical indirect band gap of the films decreased significantly with increasing manganese doping, from 3.32 eV for the undoped composition to 2.90 eV for that doped with 7 wt% Mn.

Preparation of Composite Coating on AZ91D Magnesium Alloy by Silica Sol-Micro Oxidation

NASA Astrophysics Data System (ADS)

Shao, Zhongcai; Zhang, Feifei; Zhao, Ruiqiang; Shen, Xiaoyi

2016-03-01

Composite coating was prepared on AZ91D magnesium alloy with a new method which combined silica sol with micro-arc oxidation (MAO). The MAO coating was prepared on the basis of MAO solution, and then coated by sol-gel process. The composite coating was obtained after second MAO treatment. Scanning electron microscopy coupled with X-ray diffraction (XRD), energy spectrum analysis and electrochemical testing was applied to characterize the properties of MAO coating and composite coating. The experimental test results indicated that the Si element derived from SiO2 gel particle embedded into the MAO coating by second MAO treatment. The surface of composite coating became dense and the holes were smaller with silica sol sealing process. The corrosion resistance of composite coating was improved than the MAO coating.

Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

NASA Astrophysics Data System (ADS)

Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

2006-07-01

The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

Effect of heat input on microstructure, wear and friction behavior of (wt.-%) 50FeCrC-20FeW-30FeB coating on AISI 1020 produced by using PTA welding.

PubMed

Özel, Cihan; Gürgenç, Turan

2018-01-01

In this study, AISI 1020 steel surface was coated in different heat inputs with (wt.-%) 50FeCrC-20FeW-30FeB powder mixture by using plasma transferred arc (PTA) welding method. The microstructure of the coated samples were investigated by using optical microscope (OM), scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDS). The hardness was measured with micro hardness test device. The dry sliding wear and friction coefficient properties were determined using a block-on-disk type wear test device. Wear tests were performed at 19.62 N, 39.24 N, 58.86 N load and the sliding distance of 900 m. The results were shown that different microstructures formed due to the heat input change. The highest average micro hardness value was measured at 1217 HV on sample coated with low heat input. It was determined that the wear resistance decreased with increasing heat input.

Wear behavior of electroless Ni-P-W coating under lubricated condition - a Taguchi based approach

NASA Astrophysics Data System (ADS)

Mukhopadhyay, Arkadeb; Duari, Santanu; Barman, Tapan Kumar; Sahoo, Prasanta

2016-09-01

The present study aims to investigate the tribological behavior of electroless Ni-P-W coating under engine oil lubricated condition to ascertain its suitability in automotive applications. Coating is deposited onto mild steel specimens by the electroless method. The experiments are carried out on a pin - on - disc type tribo tester under lubrication. Three tribotesting parameters namely the applied normal load, sliding speed and sliding duration are varied at their three levels and their effects on the wear depth of the deposits are studied. The experiments are carried out based on the combinations available in Taguchi's L27 orthogonal array (OA). Optimization of the tribo-testing parameters is carried out using Taguchi's S/N ratio method to minimize the wear depth. Analysis of variance carried out at a confidence level of 99% indicates that the sliding speed is the most significant parameter in controlling the wear behavior of the deposits. Coating characterization is done using scanning electron microscope, energy dispersive X-ray analysis and X-ray diffraction techniques. It is seen that the wear mechanism under lubricated condition is abrasive in nature.

Electronic structural studies on the improved thermal stability of Li(Ni0.8Co0.15Al0.05)O2 by ZrO2 coating for lithium ion batteries

DOE PAGES

Kim, Ji-Young; Kim, Sang Hoon; Kim, Dong Hyun; ...

2017-03-21

The electronic structures of bare and ZrO 2-coated Li(Ni 0.8Co 0.15Al 0.05)O 2 electrode systems were investigated using a combination of time-resolved X-ray diffraction and soft X-ray absorption spectroscopy (XAS) techniques. The ZrO 2 coating on the surface of Li(Ni 0.8Co 0.15Al 0.05)O 2 was effective in elevating the onset temperature of the dissociation of charged Li 0.33(Ni 0.8Co 0.15Al 0.05)O 2, which will enhance the safety of Li-ion cells. Lastly, soft XAS spectra of the Ni LII,III-edge in the partial electron yield mode were obtained, which showed that the enhanced electrochemical properties and thermal stability of the cathode materialsmore » by ZrO 2 coating can be attributed to the suppression of unwanted Ni oxidation state changes at the surface.« less

Optimization of rotational speed for growing BaFe12O19 thin films using spin coating

NASA Astrophysics Data System (ADS)

Budiawanti, S.; Soegijono, B.; Mudzakir, I.; Suharno, Fadillah, L.

2017-07-01

Barium ferrite (BaFe12O19, BaM) thin films were fabricated by the spin coating of precursors obtained by using a sol-gel method. The effects of the rotational speed on the spin-coating process for growing a BaM thin film were investigated in this study. Coated films were heat-deposited at different rotational speeds ranging from 2000 to 4000 rpm, while the number of layers was set to nine. Further, the effect of the number of layers on the growth of BaM thin films was discussed. For this purpose, we take the layers number 1 to 12 and take the constant rotational speed of 3000 rpm. All the film were characterized using X-Ray diffraction, Scanning Electron microscope, and Energy-dispersive X-Ray spectroscopy and Vibrating Sample Magnetometer. It was found that by increasing the rotational speed the amount of material deposited on the Si substrate decreased. The measured grain size of the BaM thin film was nearly similar for three three different rotational speeds. However, the grain size was found to increase the number of layers.

Investigation of the nanostructure and wear properties of physical vapor deposited CrCuN nanocomposite coatings

NASA Astrophysics Data System (ADS)

Baker, M. A.; Kench, P. J.; Tsotsos, C.; Gibson, P. N.; Leyland, A.; Matthews, A.

2005-05-01

This article presents results on CrCuN nanocomposite coatings grown by physical vapor deposition. The immiscibility of Cr (containing a supersaturation of nitrogen) and Cu offers the potential of depositing a predominantly metallic (and therefore tough) nanocomposite, composed of small Cr(N) metallic and/or β-Cr2N ceramic grains interdispersed in a (minority) Cu matrix. A range of CrCuN compositions have been deposited using a hot-filament enhanced unbalanced magnetron sputtering system. The stoichiometry and nanostructure have been studied by x-ray photoelectron spectroscopy, transmission electron microscopy, scanning electron microscopy, and x-ray diffraction. Hardness, wear resistance, and impact resistance have been determined by nanoindentation, reciprocating-sliding, and ball-on-plate high-cycle impact. Evolution of the nanostructure as a function of composition and correlations of the nanostructure and mechanical properties of the CrCuN coatings are discussed. A nanostructure comprised of 1-3 nm α-Cr(N) and β-Cr2N grains separated by intergranular regions of Cu gives rise to a coating with significantly enhanced resistance to impact wear.

Effect of heat input on microstructure, wear and friction behavior of (wt.-%) 50FeCrC-20FeW-30FeB coating on AISI 1020 produced by using PTA welding

PubMed Central

Gürgenç, Turan

2018-01-01

In this study, AISI 1020 steel surface was coated in different heat inputs with (wt.-%) 50FeCrC-20FeW-30FeB powder mixture by using plasma transferred arc (PTA) welding method. The microstructure of the coated samples were investigated by using optical microscope (OM), scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDS). The hardness was measured with micro hardness test device. The dry sliding wear and friction coefficient properties were determined using a block-on-disk type wear test device. Wear tests were performed at 19.62 N, 39.24 N, 58.86 N load and the sliding distance of 900 m. The results were shown that different microstructures formed due to the heat input change. The highest average micro hardness value was measured at 1217 HV on sample coated with low heat input. It was determined that the wear resistance decreased with increasing heat input. PMID:29324875

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

Calcium-doped ceria/titanate tabular functional nanocomposite by layer-by-layer coating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Xiang W., E-mail: lxwluck@gmail.co; Devaraju, M.K.; Yin, Shu

2010-07-15

Ca-doped ceria (CDC)/tabular titanate (K{sub 0.8}Li{sub 0.27}Ti{sub 1.73}O{sub 4}, TT) UV-shielding functional nanocomposite with fairly uniform CDC coating layers was prepared through a polyelectrolyte-associated layer-by-layer (LbL) coating method. TT with lepidocrocite-like layered structure was used as the substrate, poly (diallyldimethylammonium chloride) (PDDA) was used as a coupling agent, CDC nanoparticles were used as the main UV-shielding component. CDC/TT nanocomposites with various coating layers of CDC were obtained through a multistep coating process. The phases were studied by X-ray diffraction. The morphology and coating quality were studied by scanning electron microscopy and element mapping of energy dispersive X-ray analysis. The oxidationmore » catalytic activity, UV-shielding ability and using comfort were characterized by Rancimat test, UV-vis spectra and dynamic friction test, respectively. CDC/TT nanocomposites with low oxidation catalytic activity, high UV-shielding ability and good using comfort were finally obtained. - Graphical abstract: Through the control of surface charge of particles calcium-doped ceria/titanate composites with low oxidation catalytic activity, higher UV-shielding ability and excellent comfort was obtained by a facile layer-by-layer coating method.« less

Fabrication of TiO2 Crystalline Coatings by Combining Ti-6Al-4V Anodic Oxidation and Heat Treatments

PubMed Central

Schvezov, Carlos Enrique; Ares, Alicia Esther

2015-01-01

The bio- and hemocompatibility of titanium alloys are due to the formation of a TiO2 layer. This natural oxide may have fissures which are detrimental to its properties. Anodic oxidation is used to obtain thicker films. By means of this technique, at low voltages oxidation, amorphous and low roughness coatings are obtained, while, above a certain voltage, crystalline and porous coatings are obtained. According to the literature, the crystalline phases of TiO2, anatase, and rutile would present greater biocompatibility than the amorphous phase. On the other hand, for hemocompatible applications, smooth and homogeneous surfaces are required. One way to obtain crystalline and homogeneous coatings is by heat treatments after anodic oxidation. The aim of this study is to evaluate the influence of heat treatments on the thickness, morphology, and crystalline structure of the TiO2 anodic coatings. The characterization was performed by optical and scanning electron microscopy, X-ray diffraction, and X-ray reflectometry. Coatings with different colors of interference were obtained. There were no significant changes in the surface morphology and roughness after heat treatment of 500°C. Heat treated coatings have different proportions of the crystalline phases, depending on the voltage of anodic oxidation and the temperature of the heat treatment. PMID:25784939

Microstructure characteristics of Ni/WC composite cladding coatings

NASA Astrophysics Data System (ADS)

Yang, Gui-rong; Huang, Chao-peng; Song, Wen-ming; Li, Jian; Lu, Jin-jun; Ma, Ying; Hao, Yuan

2016-02-01

A multilayer tungsten carbide particle (WCp)-reinforced Ni-based alloy coating was fabricated on a steel substrate using vacuum cladding technology. The morphology, microstructure, and formation mechanism of the coating were studied and discussed in different zones. The microstructure morphology and phase composition were investigated by scanning electron microscopy, optical microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. In the results, the coating presents a dense and homogeneous microstructure with few pores and is free from cracks. The whole coating shows a multilayer structure, including composite, transition, fusion, and diffusion-affected layers. Metallurgical bonding was achieved between the coating and substrate because of the formation of the fusion and diffusion-affected layers. The Ni-based alloy is mainly composed of γ-Ni solid solution with finely dispersed Cr7C3/Cr23C6, CrB, and Ni+Ni3Si. WC particles in the composite layer distribute evenly in areas among initial Ni-based alloying particles, forming a special three-dimensional reticular microstructure. The macrohardness of the coating is HRC 55, which is remarkably improved compared to that of the substrate. The microhardness increases gradually from the substrate to the composite zone, whereas the microhardness remains almost unchanged in the transition and composite zones.

Protective coatings on stainless steel bipolar plates for proton exchange membrane (PEM) electrolysers

NASA Astrophysics Data System (ADS)

Gago, A. S.; Ansar, S. A.; Saruhan, B.; Schulz, U.; Lettenmeier, P.; Cañas, N. A.; Gazdzicki, P.; Morawietz, T.; Hiesgen, R.; Arnold, J.; Friedrich, K. A.

2016-03-01

Proton exchange membrane (PEM) electrolysis is a promising technology for large H2 production from surplus electricity from renewable sources. However, the electrolyser stack is costly due to the manufacture of bipolar plates (BPP). Stainless steel can be used as an alternative, but it must be coated. Herein, dense titanium coatings are produced on stainless steel substrates by vacuum plasma spraying (VPS). Further surface modification of the Ti coating with Pt (8 wt% Pt/Ti) deposited by physical vapour deposition (PVD) magnetron sputtering reduces the interfacial contact resistance (ICR). The Ti and Pt/Ti coatings are characterised by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and X-ray photoelectron microscopy (XPS). Subsequently, the coatings are evaluated in simulated and real PEM electrolyser environments, and they managed to fully protect the stainless steel substrate. In contrast, the absence of the thermally sprayed Ti layer between Pt and stainless steel leads to pitting corrosion. The Pt/Ti coating is tested in a PEM electrolyser cell for almost 200 h, exhibiting an average degradation rate of 26.5 μV h-1. The results reported here demonstrate the possibility of using stainless steel as a base material for the stack of a PEM electrolyser.

Synthesis and application of surfactants coated magnetite nanoparticles for demulsification of crude oil in water emulsion

NASA Astrophysics Data System (ADS)

Yau, Xin Hui; Khe, Cheng Seong; Liu, Wei Wen; Lai, Chin Wei; Oo, Zeya

2017-10-01

Magnetite nanoparticles were synthesized through co-precipitation method, in which surfactant such as polyvinylpyrrolidone (PVP) and sodium dodecyl benzene sulfonate (SDBS) were applied as stabilizing agent. Various techniques were employed to characterize the synthesized magnetite nanoparticles. Magnetite nanoparticles with spinel structure are successfully synthesized and confirmed by X-ray diffraction (XRD). X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) results proved that surface of magnetite nanoparticles were successfully coated with PVP and SDBS. From the transmission electron microscope (TEM), it showed that surfactant coated magnetite nanoparticles possess smaller particle size than that of bare magnetite nanoparticles. In comparison with SDBS, PVP has a better capping efficiency and the PVP coated magnetite nanoparticles have an average particle size of 10.8 nm. In addition, surfactant coated magnetite nanoparticles also exhibited lower value of saturation magnetization (Ms). Lower value of Ms might be attributed to the small sized nanoparticles. All magnetite nanoparticles synthesized with and without surfactant showed superparamagnetic behaviour. Bare and surfactant coated magnetite nanoparticles have been utilized as a demulsifier for crude oil in water emulsion. Those nanoparticles that produced using SDBS (ED= 87%) showed higher efficiency than that of PVP coated (ED=80%) and bare magnetite nanoparticles (ED=85%) in demulsification tests.

Tribological properties of CrN coatings deposited by nitro-chromizing treatment on AISI D2 steel

NASA Astrophysics Data System (ADS)

Durmaz, M.; Kilinc, B.; Abakay, E.; Sen, U.; Sen, S.

2015-03-01

In this work, the wear test of uncoated and chromium nitride coated AISI D2 cold work tool steel against alumina ball realized at 0.1 m/s sliding speeds and under the loads of 2.5N, 5N and 10N. Steel samples were nitrided at 575°C for 8 h in the first step of the coating process, and then chromium nitride coating was performed thermo-reactive deposition technique (TRD) in a powder mixture consisting of ferro-chromium, ammonium chloride and alumina at 1000°C for 2 h. Nitro-chromized samples were characterized by X-Ray diffraction analysis (XRD), scanning electron microscopy (SEM), micro-hardness and ball on disk wear tests. The coating layer formed on the AISI D2 steel was compact and homogeneous. X-ray studies showed that the phase formed in the coated layer is Cr2N. The depth of the layer was 8.15 µm. The average hardness of the layer was 2160±15 HV0.025. For uncoated and chromium nitride materials, wear rate increased with increasing load. The results of friction coefficient and wear rate of the tested materials showed that the CrN coating presents the lowest results.

Tribological properties of CrN coatings deposited by nitro-chromizing treatment on AISI D2 steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Durmaz, M., E-mail: mdurmaz@sakarya.edu.tr; Abakay, E.; Sen, U.

2015-03-30

In this work, the wear test of uncoated and chromium nitride coated AISI D2 cold work tool steel against alumina ball realized at 0.1 m/s sliding speeds and under the loads of 2.5N, 5N and 10N. Steel samples were nitrided at 575°C for 8 h in the first step of the coating process, and then chromium nitride coating was performed thermo-reactive deposition technique (TRD) in a powder mixture consisting of ferro-chromium, ammonium chloride and alumina at 1000°C for 2 h. Nitro-chromized samples were characterized by X-Ray diffraction analysis (XRD), scanning electron microscopy (SEM), micro-hardness and ball on disk wear tests. The coating layermore » formed on the AISI D2 steel was compact and homogeneous. X-ray studies showed that the phase formed in the coated layer is Cr{sub 2}N. The depth of the layer was 8.15 µm. The average hardness of the layer was 2160±15 HV{sub 0.025}. For uncoated and chromium nitride materials, wear rate increased with increasing load. The results of friction coefficient and wear rate of the tested materials showed that the CrN coating presents the lowest results.« less

Comparison of Erosion Behavior and Particle Contamination in Mass-Production CF4/O2 Plasma Chambers Using Y2O3 and YF3 Protective Coatings

PubMed Central

Lin, Tzu-Ken; Wang, Wei-Kai; Huang, Shih-Yung; Tasi, Chi-Tsung

2017-01-01

Yttrium fluoride (YF3) and yttrium oxide (Y2O3) protective coatings prepared using an atmospheric plasma spraying technique were used to investigate the relationship between surface erosion behaviors and their nanoparticle generation under high-density plasma (1012–1013 cm−3) etching. As examined by transmission electron microscopy, the Y2O3 and YF3 coatings become oxyfluorinated after exposure to the plasma, wherein the yttrium oxyfluoride film formation was observed on the surface with a thickness of 5.2 and 6.8 nm, respectively. The difference in the oxyfluorination of Y2O3 and YF3 coatings could be attributed to Y–F and Y–O bonding energies. X-ray photoelectron spectroscopy analyses revealed that a strongly fluorinated bonding (Y–F bond) was obtained on the etched surface of the YF3 coating. Scanning electron microscopy and energy dispersive X-ray diffraction analysis revealed that the nanoparticles on the 12-inch wafer are composed of etchant gases and Y2O3. These results indicate that the YF3 coating is a more erosion-resistant material, resulting in fewer contamination particles compared with the Y2O3 coating. PMID:28708079

Interaction of atomic oxygen with thin film and bulk copper: An XPS, AES, XRD, and profilometer study

NASA Technical Reports Server (NTRS)

Raikar, Genesh N.; Gregory, John C.; Christl, Ligia C.; Peters, Palmer N.

1992-01-01

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed primarily to study degradation of material surfaces due to low earth orbital (LEO) atmospheric oxygen. The experiment contained 128 one inch circular samples: metals, polymers, carbons, and semiconductors. Among metal samples, copper has shown some interesting new results. Two types of copper samples, a film sputter coated on fused silica and a bulk piece of OFHC copper, were characterized employing a variety of techniques such as X-ray and Auger electron spectroscopies, X-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to characterize the presence of Cu2O and CuO in addition to Cu Auger LMM lines. These results are supported by our recent X-ray diffraction studies which clearly establish the presence of Cu oxides which we were unable to prove in our earlier work. Profilometry showed an increase in thickness of the film sample where exposed to 106.7 +/- 0.5 nm from an initial thickness of 74.2 +/- 1.1 nm. Further studies with SEM and ellipsometry are underway.

Nanocomposite tribological coatings with "chameleon" surface adaptation

NASA Astrophysics Data System (ADS)

Voevodin, A. A.; Fitz, T. A.; Hu, J. J.; Zabinski, J. S.

2002-07-01

Nanocomposite tribological coatings were designed to respond to changing environmental conditions by self-adjustment of their surface properties to maintain good tribological performance in any environment. These smart coatings have been dubbed "chameleon" because, analogous to a chameleon changing its skin color to avoid predators, the coating changes its "skin" chemistry and structure to avoid wear. The concept was originally developed using WC, diamondlike carbon, and WS2 material combination for adaptation to a humid/dry environment cycling. In order to address temperature variation, nanocomposite coatings made of yttria-stabilized zirconia (YSZ) in a gold matrix were developed with encapsulated nanosized reservoirs of MoS2 and diamondlike carbon (DLC). Coatings were produced using a combination of laser ablation and magnetron sputtering. They were characterized by x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, x-ray energy dispersive spectroscopy, and micro-Raman spectroscopy. Results were correlated with mechanical and tribological characterization. Coating hardness was evaluated using nanoindentation, while coating adhesion and toughness were estimated using scratch and Vickers indentation tests. Friction and wear endurance measurements of YSZ/Au/MoS2/DLC coatings against steel and Si3N4 balls were performed at room temperature in controlled humidity air, dry nitrogen, and vacuum environments, as well as at 500 degC in air. Depending on the environment, coating friction surface changed its chemistry and structure between (i) graphitic carbon for sliding in humid air [coating friction coefficients (c.o.f. 0.10-0.15)], (ii) hexagonal MoS2 for sliding in dry N2 and vacuum (c.o.f. 0.02-0.05), and (iii) metallic Au for sliding in air at 500 degC (c.o.f. 0.10-0.20). The unique coating skin adaptation realized with YSZ/Au/MoS2/DLC and WC/DLC/WS composites proves a universal applicability of the chameleon design concept. copyright 2002 American Vacuum Society.

Alternate Spray-coating for the Direct Fabrication of Hydroxyapatite Films without Crystal Growth Step in Solution.

PubMed

Watanabe, Satoshi; Kashiwagi, Rei; Matsumoto, Mutsuyoshi

2017-03-01

We discuss an alternate spray-coating technique for the direct fabrication of hydroxyapatite films using metal masks, suction-type spray nozzles and two calcification solutions of calcium hydroxide and phosphoric acid aqueous solutions. Hydroxyapatite films were formed only on the hydrophobic surface of the substrates. Scanning electron microscopy and energy dispersive X-ray spectroscopy showed that the spray-coated films consisted of hydroxyapatite nanoparticles. The Ca/P ratio was estimated to be about 1.26. X-ray diffraction patterns of the spray-coated films almost coincided with those of the hydroxyapatite powders, showing that the spray-coated films consisted of hydroxyapatite nanoparticles. Dot arrays of hydroxyapatite films at a diameter of 100 μm were formed by tuning the concentrations of calcium hydroxide and phosphoric acid aqueous solutions. This technique allows for the direct fabrication of the hydroxyapatite films without crystal growth process in hydroxyapatite precursors, the scaffolds of crystal growth such as biocompatibility SiO 2 -CaO glasses, or electrophoresis processes. By using this technique, large-area ceramic films with biocompatibility will be micropatterned with minimized material consumption, short fabrication time, and reduced equipment investments.

Corrosion behavior of an HVOF-sprayed Fe3Al coating in a high-temperature oxidizing/sulfidizing environment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Covino, Bernard S., Jr.; Bullard, Sophie J.; Cramer, Stephen D.

An iron aluminide (Fe3Al) intermetallic coating was deposited onto a F22 (2.25Cr-1Mo) steel substrate using a JP-5000 high velocity oxy-fuel (HVOF) thermal spray system. The as-sprayed coating was examined by electron microscopy and X-ray diffraction and was characterized in terms of oxidation and adhesion. Fe3Al-coated steel specimens were exposed to a mixed oxidizing/sulfidizing environment at 500, 600, 700, and 800DGC for approximately seven days. The gaseous environment consisted of N2-10%CO-5%CO2-2%H2O-0.12%H2S (by volume). All specimens gained mass after exposure to the environment and the mass gains were found to be inversely proportional to temperature increases. Representative specimens exposed at each temperaturemore » were cross-sectioned and subjected to examination under a scanning electron microscope (SEM) and X-ray mapping. Results are presented in terms of corrosion weight gain and corrosion product formation. The purpose of the research presented here was to evaluate the effectiveness of an HVOF-sprayed Fe3Al coating in protecting a steel substrate exposed to a fossil energy environment.« less

Synthesis of Carbon-Coated ZnO Composite and Varistor Properties Study

NASA Astrophysics Data System (ADS)

Sun, Wei-Jie; Liu, Jin-Ran; Yao, Da-Chuan; Chen, Yong; Wang, Mao-Hua

2017-03-01

In this article, monodisperse ZnO composite nanoparticles were successfully prepared by sol-gel mixed precursor method. Subsequently, carbon as the shell was homogeneously coated on the surface of the ZnO composite nanoparticles via a simple adsorption and calcination process. Microstructural studies of the as-obtained powders were carried out using the techniques of the x-ray powder diffraction, scanning electron microscopy, field emission scanning electron microscopy, transmission electron microscopy with energy dispersive x-ray spectroscopy, and Fourier transform infrared spectroscopy. The results show that the pink ZnO composite powders were fully coated by carbon. Based on the results, the effect of glucose content on the microstructure of the synthesized composites and the electrical properties of the ZnO varistors sintered in air at 1150°C for 2 h were also fully studied. As the amount of glucose increased, the thickness of carbon can be increased from 2.5 nm to 5 nm. In particular, the ZnO varistor fabricated with the appropriate thickness of the carbon coating (5 nm) leads to the superior electrical performance, with present high breakdown voltage ( V b = 420 V/mm) and excellent nonlinear coefficient ( α = 61.7), compared with the varistors obtained without carbon coating.

Development and characterization of laser surface cladding (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper

NASA Astrophysics Data System (ADS)

Yan, Hua; Zhang, Peilei; Yu, Zhishui; Li, Chonggui; Li, Ruidi

2012-07-01

To improve the wear resistance of copper components, laser surface cladding (LSC) was applied to deposit (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper using a cladding interlayer of Ni-30Cu alloy by Nd:YAG laser. The microstructure and phases of the composite coating were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray energy dispersive microanalysis (EDX). Microhardness tester and pin-on-disc wear tester were employed to evaluate the hardness and dry-sliding wear resistance. The results show that crack-free composite coating with metallurgical bonding to the copper substrate is obtained. Phases identified in the (Ti,W)C-reinforced Ni-30Cu alloy composite layer are composed of TiWC2 reinforcements and (Ni,Cu) solid solution. TiWC2 reinforcements are distributed uniformly in the (Ni,Cu) solid solution matrix with dendritic morphology in the upper region and with particles in the mid-lower region. The microhardness and wear properties of the composite coating are improved significantly in comparison to the as-received copper substrate due to the addition of 50 wt% (Ti,W)C multicarbides.

Tribological Testing, Analysis and Characterization of D.C. Magnetron Sputtered Ti-Nb-N Thin Film Coatings on Stainless Steel

NASA Astrophysics Data System (ADS)

Joshi, Prathmesh

To enhance the surface properties of stainless steel, the substrate was coated with a 1μm thick coating of Ti-Nb-N by reactive DC magnetron sputtering at different N2 flow rates, substrate biasing and Nb-Ti ratio. The characterization of the coated samples was performed by the following techniques: hardness by Knoop micro-hardness tester, phase analysis by X-ray Diffraction (XRD), compositional analysis by Energy Dispersive X-ray Spectroscopy (EDS) and adhesion by scratch test. The tribology testing was performed on linearly reciprocating ball-on-plate wear testing machine and wear depth and wear volume were evaluated by white light interferometer. The micro-hardness test yielded appreciable enhancement in the surface hardness with the highest value being 1450 HK. Presence of three prominent phases namely NbN, Nb2N3 and TiN resulted from the XRD analysis. EDS analysis revealed the presence of Ti, Nb and Nitrogen. Adhesion was evaluated on the basis of critical loads for cohesive (Lc1) and adhesive (Lc2) failures with values varying between 7-12 N and 16-25 N respectively, during scratch test for coatings on SS substrates.

Phase evolution and thermal properties of yttria-stabilized hafnia nano-coatings deposited on alumina

NASA Astrophysics Data System (ADS)

Rubio, Ernesto Javier

High-temperature coatings are critical to the future power-generation systems and industries. Thermal barrier coatings (TBCs), which are usually the ceramic materials applied as thin coatings, protect engine components and allow further increase in engine temperatures for higher efficiency. Thus, the durability and reliability of the coating systems have to be more robust compared to current natural gas based engines. While a near and mid-term target is to develop TBC architecture with a 1300 °C surface temperature tolerance, a deeper understanding of the structure evolution and thermal behavior of the TBC-bond coat interface, specifically the thermally grown oxide (TGO), is of primary importance. In the present work, attention is directed towards yttria-stabilized hafnia (YSH) coatings on alumina (α-Al2O 3) to simulate the TBC-TGO interface and understand the phase evolution, microstructure and thermal oxidation of the coatings. YSH coatings were grown on α-Al2O3 substrates by sputter deposition by varying coating thickness in a wide range ˜30-1000 nm. The effect of coating thickness on the structure, morphology and the residual stress has been investigated using X-ray diffraction (XRD) and high resolution scanning electron microscopy (SEM). Thermal oxidation behavior of the coatings has been evaluated using the isothermal oxidation measurements under static conditions. X-ray diffraction analyses revealed the existence of monoclinic hafnia phase for relatively thin coatings indicating that the interfacial phenomena are dominant in phase stabilization. The evolution towards pure stabilized cubic phase of hafnia with the increasing coating thickness is observed. The SEM results indicate the changes in morphology of the coatings; the average grain size increases from 15 to 500 nm with increasing thickness. Residual stress was calculated employing XRD using the variable ψ-angle. Relation between residual stress and structural change is also studied. The results obtained on the thermal oxidation behavior indicate that the YSH coatings exhibit initial mass gain in the first 6 hours and sustained structure for extended hours of thermal treatment.

Effect of perfluorodecyltrichlorosilane on the surface properties and anti-corrosion behavior of poly(dimethylsiloxane)-ZnO coatings

NASA Astrophysics Data System (ADS)

Arukalam, Innocent O.; Meng, Meijiang; Xiao, Haigang; Ma, Yuantai; Oguzie, Emeka E.; Li, Ying

2018-03-01

Poly(dimethylsiloxane)-ZnO coatings modified with different amounts of perfluorodecyltrichlorosilane (FDTS) were prepared using sol-gel technique. The results of field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) examinations showed that the surface structures and roughness of the coatings were respectively influenced by the increasing addition of FDTS. The water contact angle measurements showed maximum value of 130.52° with the 0.10 g FDTS-modified coating sample. The X-ray photoelectron spectroscopy (XPS) results indicated the coatings' hydrophobicity was also influenced by surface chemistry. The FTIR-ATR characterization results showed there was remarkable increase in the crystallinity of 0.10 g FDTS-modified coating after modification, and was confirmed by differential scanning calorimetry (DSC) analysis of crystallization temperature and the X-ray diffraction (XRD) results with an estimation of 71.29% percent crystallinity. The mechanical properties of the coatings were also conducted. The EIS measurements for anti-corrosion behavior showed that 0.10 g FDTS-modified coating had the highest barrier performance and lowest rate of degradation. Indeed, the obtained data have demonstrated that 0.10 g (≈ 0.18%) FDTS produced the most significantly effect on the surface and barrier properties of the coatings and thus, can effectively be used for anti-corrosion application in the marine environments.

Study of PVD AlCrN Coating for Reducing Carbide Cutting Tool Deterioration in the Machining of Titanium Alloys.

PubMed

Cadena, Natalia L; Cue-Sampedro, Rodrigo; Siller, Héctor R; Arizmendi-Morquecho, Ana M; Rivera-Solorio, Carlos I; Di-Nardo, Santiago

2013-05-24

The manufacture of medical and aerospace components made of titanium alloys and other difficult-to-cut materials requires the parallel development of high performance cutting tools coated with materials capable of enhanced tribological and resistance properties. In this matter, a thin nanocomposite film made out of AlCrN (aluminum-chromium-nitride) was studied in this research, showing experimental work in the deposition process and its characterization. A heat-treated monolayer coating, competitive with other coatings in the machining of titanium alloys, was analyzed. Different analysis and characterizations were performed on the manufactured coating by scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDXS), and X-ray diffraction (XRD). Furthermore, the mechanical behavior of the coating was evaluated through hardness test and tribology with pin-on-disk to quantify friction coefficient and wear rate. Finally, machinability tests using coated tungsten carbide cutting tools were executed in order to determine its performance through wear resistance, which is a key issue of cutting tools in high-end cutting at elevated temperatures. It was demonstrated that the specimen (with lower friction coefficient than previous research) is more efficient in machinability tests in Ti6Al4V alloys. Furthermore, the heat-treated monolayer coating presented better performance in comparison with a conventional monolayer of AlCrN coating.

Wear and friction characteristics of electroless Ni-B-W coatings at different operating temperatures

NASA Astrophysics Data System (ADS)

Mukhopadhyay, Arkadeb; Barman, Tapan Kumar; Sahoo, Prasanta

2018-02-01

Sodium borohydride reduced electroless nickel alloy coatings have high wear resistance and low coefficient of friction. The present work investigates the deposition and tribological behavior of a ternary variant of the borohydride reduced coating i.e. Ni-B-W. Electroless Ni-B-W coatings were deposited on AISI 1040 steel substrates. In order to improve the mechanical properties of the deposits, they were heat treated at 350 °C for 1 h. The coatings in their as-deposited and heat treated conditions were characterized by scanning electron microscope, energy dispersive x-ray analysis and x-ray diffraction techniques. Ni-B-W coatings are amorphous in their as-deposited state while they become crystalline on heat treatment. In fact a high microhardness of Ni-B-W coatings is also observed in as-deposited condition. The microhardness further improves on heat treatment. Tribological behavior of the heat treated coatings with varying load (10-50 N), sliding speed (0.25-0.42 m s-1) and operating temperature (25 °C-500 °C) were evaluated on a pin-on-disc type test setup while the wear mechanisms were also studied. Tribological behavior of Ni-B-W coatings is enhanced at 500 °C operating temperature in comparison with 100 or 300 °C due to formation of protective oxide scales and microstructural changes due to in-situ heat treatment effect.

Study of PVD AlCrN Coating for Reducing Carbide Cutting Tool Deterioration in the Machining of Titanium Alloys

PubMed Central

Cadena, Natalia L.; Cue-Sampedro, Rodrigo; Siller, Héctor R.; Arizmendi-Morquecho, Ana M.; Rivera-Solorio, Carlos I.; Di-Nardo, Santiago

2013-01-01

The manufacture of medical and aerospace components made of titanium alloys and other difficult-to-cut materials requires the parallel development of high performance cutting tools coated with materials capable of enhanced tribological and resistance properties. In this matter, a thin nanocomposite film made out of AlCrN (aluminum–chromium–nitride) was studied in this research, showing experimental work in the deposition process and its characterization. A heat-treated monolayer coating, competitive with other coatings in the machining of titanium alloys, was analyzed. Different analysis and characterizations were performed on the manufactured coating by scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDXS), and X-ray diffraction (XRD). Furthermore, the mechanical behavior of the coating was evaluated through hardness test and tribology with pin-on-disk to quantify friction coefficient and wear rate. Finally, machinability tests using coated tungsten carbide cutting tools were executed in order to determine its performance through wear resistance, which is a key issue of cutting tools in high-end cutting at elevated temperatures. It was demonstrated that the specimen (with lower friction coefficient than previous research) is more efficient in machinability tests in Ti6Al4V alloys. Furthermore, the heat-treated monolayer coating presented better performance in comparison with a conventional monolayer of AlCrN coating. PMID:28809266

Cyclic oxidation behavior of some plasma-sprayed coatings in Na2SO4-60%V2O5 environment

NASA Astrophysics Data System (ADS)

Singh, Harpreet; Prakash, Satya; Puri, Devendra; Phase, D. M.

2006-12-01

Cyclic oxidation behavior of plasma-sprayed NiCrAlY, Ni-20Cr, Ni3Al, and Stellite-6 coatings was investigated in an aggressive environment of Na2SO4-60%V2O5 by thermogravimetric techniques for 50 cycles. These coatings were deposited on a Ni-base superalloy, namely Superni 600; 10Fe-15.5Cr-0.5Mn-0.2C-Bal Ni (wt.%). X-ray diffraction, scanning electron microscopy/energy dispersive x-ray (SEM/EDX), and electron probe microanalyzer (EPMA) techniques were used to analyze the oxidation products. The uncoated superalloy suffered accelerated oxidation in the form of intense spallation of its oxide scale. After deposition of the NiCrAlY coating, the superalloy showed a minimum mass gain, whereas after application of the Stellite-6 coating, a maximum mass gain was observed among the coatings studied. All of the coatings were found to be useful in reducing the spallation of the substrate superalloy. Moreover, the coatings were successful in maintaining continuous surface contact with the base superalloy during the cyclic oxidation. The phases revealed for the oxidized coatings were mainly the oxides of chromium and/or aluminum and the spinels containing nickel-chromium/cobalt-chromium/nickel-aluminum mixed oxides, which are reported to be protective against high-temperature oxidation/hot corrosion.

Improvements in Microstructure and Wear Resistance of Plasma-Sprayed Fe-Based Amorphous Coating by Laser-Remelting

NASA Astrophysics Data System (ADS)

Jiang, Chaoping; Chen, Hong; Wang, Gui; Chen, Yongnan; Xing, Yazhe; Zhang, Chunhua; Dargusch, Matthew

2017-04-01

Amorphous coating technology is an attractive way of taking advantage of the superior properties of amorphous alloys for structural applications. However, the limited bonds between splats within the plasma-sprayed coatings result in a typically lamellar and porous coating structure. To overcome these limitations, the as-sprayed coating was treated by a laser-remelting process. The microstructure and phase composition of two coatings were analyzed using scanning electron microscopy with energy-dispersive spectroscopy, transmission electron microscopy, and x-ray diffraction. The wear resistance of the plasma-sprayed coating and laser-remelted coating was studied comparatively using a pin-on-disc wear test under dry friction conditions. It was revealed that the laser-remelted coating exhibited better wear resistance because of its defect-free and amorphous-nanocrystalline composited structure.

Mechanical and tribological property of single layer graphene oxide reinforced titanium matrix composite coating

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Li, Yue; Fan, Xueliang; Chen, Feng; Xu, Jiale

2018-04-01

Single layer grapheme oxide Nano sheets and Nano titanium powder were dispersed in deionized water by ultrasonic dispersion. Then the mixed solution was pre-coating on AISI4140 substrate. Using laser sintering process to fabricated grapheme oxide and Ti composite coating. Microstructures and composition of the composite coating was studied by Scanning Electron Microscopy (SEM), x-ray diffract meter (XRD) and Raman spectroscopy. Raman spectrum, XRD pattern and SEM results proved that grapheme oxide sheets were dispersed in the composite coating. The composite coating had much higher average Vickers hardness values than that of pure Ti coating. The tribological performance of the composite coatings became better while the suitable GO content was selected. For the 2.5wt. % GO content coating, the friction coefficient was reduced to near 0.1.

Osteogenic potential of a novel microarc oxidized coating formed on Ti6Al4V alloys

NASA Astrophysics Data System (ADS)

Wang, Yaping; Lou, Jin; Zeng, Lilan; Xiang, Junhuai; Zhang, Shufang; Wang, Jun; Xiong, Fucheng; Li, Chenglin; Zhao, Ying; Zhang, Rongfa

2017-08-01

In order to improve the biocompatibility, Ti6Al4V alloys are processed by micro arc oxidation (MAO) in a novel electrolyte of phytic acid, a natural organic phosphorus-containing matter. The MAO coatings were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS). The cytocompatibility of Ti6A14V alloys before and after MAO were comprehensively evaluated. The results showed that the fabricated MAO coatings were composed of rutile, anatase, TiP2O7 as well as some OH- groups, exhibiting the excellent hydrophilicity and a porous structure with small micro pores. No cytotoxicity towards MC3T3-E1cells was observed in this study. In particular, MAO treated Ti6Al4V alloys presented comparable cell adhesion and proliferation as well as significantly enhanced alkaline phosphatase activity, extracellular matrix (ECM) mineralization and collagen secretion in comparison with the untreated control. The results suggest that the Ti6Al4V alloys treated by MAO in phytic acid can be used as implants for orthopaedic applications, providing a simple and practical method to widen clinical acceptance of titanium alloys.

Enhanced bone regeneration composite scaffolds of PLLA/β-TCP matrix grafted with gelatin and HAp.

PubMed

Wang, Jie-Lin; Chen, Qian; Du, Bei-Bei; Cao, Lu; Lin, Hong; Fan, Zhong-Yong; Dong, Jian

2018-06-01

The composite polylactide PLLA/β-TCP scaffolds were fabricated by solution casting and were coated with gelatin/hydroxyapatite (Gel/HAp) to improve the biological properties of the composite scaffolds. The Gel/HAp mixture was prepared using an in situ reaction, and a grafting-coating method was used to increase the efficiency of coating the PLLA/β-TCP matrix with Gel/HAp. First, free amino groups were introduced by 1,6-hexanediamine to aminolyze the PLLA/β-TCP matrix surface. Second, glutaraldehyde was coupled to Gel/HAp as a crosslinking agent. The structure and properties of Gel/HAp-modified PLLA/β-TCP films were characterized by Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and water contact angle measurements (WCA). The experimental results show that 23 wt% HAp was uniformly dispersed in the gelatin coating by in situ synthesis. The Gel/HAp composite coating was successfully immobilized on the aminolyzed PLLA/β-TCP surface via a chemical grafting method, which promoted a lower degradation rate and was more hydrophilic than a physical grafting method. The Gel/HAp composite coating adhered tightly and homogeneously to the hydrophobic PLLA/β-TCP surface. Moreover, mouse embryo osteoblast precursor (MC3T3-E1) cells grown on the scaffolds were behaviorally and morphologically characterized. The results indicated that the Gel/HAp composite coating was favorable for the attachment and proliferation of preosteoblasts and that Gel/HAp-NH-PLLA/β-TCP would be a candidate scaffold for bone repair. Copyright © 2018 Elsevier B.V. All rights reserved.

Enhanced corrosion resistance of strontium hydroxyapatite coating on electron beam treated surgical grade stainless steel

NASA Astrophysics Data System (ADS)

Gopi, D.; Rajeswari, D.; Ramya, S.; Sekar, M.; R, Pramod; Dwivedi, Jishnu; Kavitha, L.; Ramaseshan, R.

2013-12-01

The surface of 316L stainless steel (316L SS) is irradiated by high energy low current DC electron beam (HELCDEB) with energy of 500 keV and beam current of 1.5 mA followed by the electrodeposition of strontium hydroxyapatite (Sr-HAp) to enhance its corrosion resistance in physiological fluid. The coatings were characterised by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and High resolution scanning electron microscopy (HRSEM). The Sr-HAp coating on HELCDEB treated 316L SS exhibits micro-flower structure. Electrochemical results show that the Sr-HAp coating on HELCDEB treated 316L SS possesses maximum corrosion resistance in Ringer's solution.

X-ray diffraction from shock-loaded polycrystals.

PubMed

Swift, Damian C

2008-01-01

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.

Deposition of dual-layer coating on Ti6Al4V

NASA Astrophysics Data System (ADS)

Hussain Din, Sajad; Shah, M. A.; Sheikh, N. A.

2017-03-01

Dual-layer diamond coatings were deposited on titanium alloy (Ti6Al4V) using a hot filament chemical vapour deposition technique with the anticipation of studying the structural and morphology properties of the alloy. The coated diamond films were characterized using scanning electron microscope, x-ray diffraction (XRD), and Raman spectroscopy. The XRD studies reveal that the deposited films are highly crystalline in nature, whereas morphological studies show that the films have a cauliflower structure. XRD analysis was used to calculate the structural parameters of the Ti6Al4V and CVD-coated Ti6Al4V. Raman spectroscopy was used to determine the nature and magnitude of the residual stress of the coatings.

Superhydrophobic coatings on wood substrate for self-cleaning and EMI shielding

NASA Astrophysics Data System (ADS)

Xing, Yingjie; Xue, Yaping; Song, Jinlong; Sun, Yankui; Huang, Liu; Liu, Xin; Sun, Jing

2018-04-01

A layer of superhydrophobic coating having good electromagnetic shielding and self-cleaning performance was fabricated on a wood surface through an electroless copper plated process. The superhydrophobic property of the wood surface was measured by contact angle (CA) and roll-off angle (RA) measurements. The microstructure and chemical composition of the superhydrophobic coating were analyzed by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). The analysis revealed that the microscale particles were uniformly distributed on the wood surface and the main component of the coating is metallic copper. The as-prepared Cu coatings on wood substrate exhibit a good superhydrophobicity with water contact angle about 160° and rolling angle less than 5°.

Electrospinning of calcium carbonate fibers and their conversion to nanocrystalline hydroxyapatite.

PubMed

Holopainen, Jani; Santala, Eero; Heikkilä, Mikko; Ritala, Mikko

2014-12-01

Calcium carbonate (CaCO3) fibers were prepared by electrospinning followed by annealing. Solutions consisting of calcium nitrate tetrahydrate (Ca(NO3)2·4H2O) and polyvinylpyrrolidone (PVP) dissolved in ethanol or 2-methoxyethanol were used for the fiber preparation. By varying the precursor concentrations in the electrospinning solutions CaCO3 fibers with average diameters from 140 to 290 nm were obtained. After calcination the fibers were identified as calcite by X-ray diffraction (XRD). The calcination process was studied in detail with high temperature X-ray diffraction (HTXRD) and thermogravimetric analysis (TGA). The initially weak fiber-to-substrate adhesion was improved by adding a strengthening CaCO3 layer by spin or dip coating Ca(NO3)2/PVP precursor solution on the CaCO3 fibers followed by annealing of the gel formed inside the fiber layer. The CaCO3 fibers were converted to nanocrystalline hydroxyapatite (HA) fibers by treatment in a dilute phosphate solution. The resulting hydroxyapatite had a plate-like crystal structure with resemblance to bone mineral. The calcium carbonate and hydroxyapatite fibers are interesting materials for bone scaffolds and bioactive coatings. Copyright © 2014 Elsevier B.V. All rights reserved.

Doped indium nitride thin film by sol-gel spin coating method

NASA Astrophysics Data System (ADS)

Lee, Hui San; Ng, Sha Shiong; Yam, Fong Kwong

2017-12-01

In this study, magnesium doped indium nitride (InN:Mg) thin films grown on silicon (100) substrate were prepared via sol-gel spin coating method followed by nitridation process. A custom-made tube furnace was used to perform the nitridation process. Through this method, the low dissociation temperature issue of InN:Mg thin films can be solved. The deposited InN:Mg thin films were investigated using various techniques. The X-rays diffraction results revealed that two intense diffraction peaks correspond to wurtzite structure InN (100), and InN (101) were observed at 29° and 33.1° respectively. Field emission scanning electron microscopy images showed that the surface of the films exhibits densely packed grains. The elemental composition of the deposited thin films was analyzed using energy dispersive X-rays spectroscopy. The detected atomic percentages for In, N, and Mg were 43.22 %, 3.28 %, and 0.61 % respectively. The Raman spectra showed two Raman- and infrared-active modes of E2 (High) and A1 (LO) of the wurtzite InN. The band gap obtained from the Tauc plot showed around 1.74 eV. Lastly, the average surface roughness measured by AFM was around 0.133 µm.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

In operando X-ray diffraction strain measurement in Ni3Sn2 - Coated inverse opal nanoscaffold anodes for Li-ion batteries

NASA Astrophysics Data System (ADS)

Glazer, Matthew P. B.; Wang, Junjie; Cho, Jiung; Almer, Jonathan D.; Okasinski, John S.; Braun, Paul V.; Dunand, David C.

2017-11-01

Volume changes associated with the (de)lithiation of a nanostructured Ni3Sn2 coated nickel inverse opal scaffold anode create mismatch stresses and strains between the Ni3Sn2 anode material and its mechanically supporting Ni scaffold. Using in operando synchrotron x-ray diffraction measurements, elastic strains in the Ni scaffold are determined during cyclic (dis)charging of the Ni3Sn2 anode. These strains are characterized using both the center position of the Ni diffraction peaks, to quantify the average strain, and the peak breadth, which describes the distribution of strain in the measured volume. Upon lithiation (half-cell discharging) or delithiation (half-cell charging), compressive strains and peak breadth linearly increase or decrease, respectively, with charge. The evolution of the average strains and peak breadths suggests that some irreversible plastic deformation and/or delamination occurs during cycling, which can result in capacity fade in the anode. The strain behavior associated with cycling of the Ni3Sn2 anode is similar to that observed in recent studies on a Ni inverse-opal supported amorphous Si anode and demonstrates that the (de)lithiation-induced deformation and damage mechanisms are likely equivalent in both anodes, even though the magnitude of mismatch strain in the Ni3Sn2 is lower due to the lower (de)lithiation-induced contraction/expansion.

Tribological Behavior and Corrosion Resistance of Electroless Ni-B-W Coatings

NASA Astrophysics Data System (ADS)

Mukhopadhyay, Arkadeb; Barman, Tapan Kumar; Sahoo, Prasanta

The present study considers the tribological behavior and corrosion resistance of electroless Ni-B-W coatings deposited on AISI 1040 steel substrates. Coating is characterized using scanning electron microscopy, energy dispersive X-ray analysis and X-ray diffraction technique. In as-deposited condition, coatings are found to be amorphous. On heat treatment, precipitation of crystalline Ni (1 1 1) and its borides take place. For as-deposited coating, the microhardness is obtained as ˜759HV100 which increases to ˜1181HV100 and ˜1098HV100 when heat treated at 350∘C and 450∘C, respectively. Incorporation of W in Ni-B coating results in an increase of hardness by 89HV100 in as-deposited condition. Heat treatment also results in increase in crystallite size of Ni (1 1 1). Wear rate and coefficient of friction (COF) of the coatings are evaluated on a pin-on-disc setup under both dry and lubricated sliding conditions. Wear resistance is observed to improve on heat treatment with an increase in crystallite size while COF deteriorates. However, in as-deposited condition, wear rate and COF of Ni-B-W coatings improve by ˜5 and ˜3 times, respectively, compared with Ni-B coatings. Wear and friction performance of the coatings are enhanced under lubrication due to the columnar structure of the coatings that retain lubricants. Corrosion resistance of Ni-B-W coating in 3.5% NaCl solution gets improved on heat treatment.

The effect of TiO2 thin film thickness on self-cleaning glass properties

NASA Astrophysics Data System (ADS)

Mufti, Nandang; Laila, Ifa K. R.; Hartatiek; Fuad, Abdulloh

2017-05-01

TiO2 is one of semiconductor materials which are widely used as photocatalyst in the form of a thin film. The TiO2 thin film is prepared by using the spin coating sol-gel method. The researcher prepared TiO2 thin film with 3 coating variations and X-Ray Diffraction characterization, UV-Vis Spectrophotometer, Electron Microscopy Scanning, and examined its hydrophilic and anti-fogging properties. The result of X-Ray Diffraction showed that the phase formed is the anatase on 101crystal field. The Electron Microscopy Scanning images showed that TiO2 thin films had a homogeneous surface with the particle sizes as big as 235 nm, 179 nm, and 137 nm. The thickness of each thin film was 2.06μm, 3.33μm, and 5.20μm. The characterization of UV-Vis Spectrophotometer showed that the greatest absorption to the wavelength of visible light was in the thin film’s thickness of 3 coatings with the band-gap determined by using 3.30 eV, 3.33 eV, and 3.33 eV Plot Tuoc. These results indicated that the rate of absorption would be increased by increasing the thickness of film. The increasing thickness of the thin film makes the film hydrophilic able to be used as an anti-fogging substance.

Friction surfaced Stellite6 coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rao, K. Prasad; Damodaram, R.; Rafi, H. Khalid, E-mail: khalidrafi@gmail.com

2012-08-15

Solid state Stellite6 coatings were deposited on steel substrate by friction surfacing and compared with Stellite6 cast rod and coatings deposited by gas tungsten arc and plasma transferred arc welding processes. Friction surfaced coatings exhibited finer and uniformly distributed carbides and were characterized by the absence of solidification structure and compositional homogeneity compared to cast rod, gas tungsten arc and plasma transferred coatings. Friction surfaced coating showed relatively higher hardness. X-ray diffraction of samples showed only face centered cubic Co peaks while cold worked coating showed hexagonally close packed Co also. - Highlights: Black-Right-Pointing-Pointer Stellite6 used as coating material formore » friction surfacing. Black-Right-Pointing-Pointer Friction surfaced (FS) coatings compared with casting, GTA and PTA processes. Black-Right-Pointing-Pointer Finer and uniformly distributed carbides in friction surfaced coatings. Black-Right-Pointing-Pointer Absence of melting results compositional homogeneity in FS Stellite6 coatings.« less

Spectroscopic and x-ray diffraction analyses of asbestos in the World Trade Center dust:

USGS Publications Warehouse

Swayze, Gregg A.; Clark, Roger N.; Sutley, Stephen J.; Hoefen, Todd M.; Plumlee, Geoffrey S.; Meeker, Gregory P.; Brownfield, Isabelle; Livo, Keith E.; Morath, Laurie C.

2009-01-01

On September 17 and 18, 2001, samples of settled dust and airfall debris were collected from 34 sites within a 1-km radius of the WTC collapse site, including a sample from an indoor location unaffected by rainfall, and samples of insulation from two steel beams at Ground Zero. Laboratory spectral and x-ray diffraction analyses of the field samples detected trace levels of serpentine minerals, including chrysotile asbestos, in about two-thirds of the dust samples at concentrations at or below ~1 wt%. One sample of a beam coating material contained up to 20 wt% chrysotile asbestos. Analyses indicate that trace levels of chrysotile were distributed with the dust radially to distances greater than 0.75 km from Ground Zero. The chrysotile content of the dust is variable and may indicate that chrysotile asbestos was not distributed uniformly during the three collapse events.

Nondestructive evaluation of plasma-sprayed thermal barrier coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andrews, D.J.; Taylor, J.A.T.

Acoustic emission has been used as a nondestructive evaluation technique to examine the thermal shock response of thermal barrier coatings. In this study, samples of partially stabilized zirconia powder were sprayed and acoustic emission (AE) data were taken in a series of thermal shock tests in an effort to correlate AE with a given failure mechanism. Microstructural evidence was examined using parallel beam x-ray diffraction and optical microscopy. The AE data are discussed in terms of cumulative amplitude distributions and the use of this technique to characterize fracture events.

Electrophoretic Deposition of Cu-SiO2 Coatings by DC and Pulsed DC for Enhanced Surface-Mechanical Properties

NASA Astrophysics Data System (ADS)

Maharana, H. S.; Lakra, Suprabha; Pal, S.; Basu, A.

2016-01-01

The present study explored the possibilities of improvement in the surface-mechanical properties of electrodeposited Cu-SiO2 composite coating and its underlying mechanism. Composite coatings were developed using SiO2-dispersed acidic copper sulfate electrolyte by direct current and pulse-current electro-codeposition techniques with variation of pulse frequencies at a fixed duty cycle. X-ray diffraction analysis of the coatings revealed information regarding the presence of various phases and crystallographic orientations of the deposited Cu matrix. Scanning electron microscopy and energy dispersive x-ray spectroscopy techniques were used to investigate the surface morphology and chemical composition of the coatings, respectively, and it was observed that SiO2 particles were uniformly distributed in the composite coatings. Surface roughness was found to be reduced with the increasing pulse frequency. The Vickers microhardness and ball-on-plate wear study showed improvement in surface-mechanical properties due to the formation of fine Cu matrix, dispersion strengthening due to homogeneously distributed SiO2 particles, and the preferred orientation of the Cu matrix. Marginal decrease in electrical conductivity with the increasing SiO2 content and pulse frequency was observed from the four-probe electrical conductivity measurement technique.

Electrodeposition of Zn-Co-Mo Alloy on the Steel Substrate from Citrate Bath and Its Corrosion Behavior in the Chloride Media

NASA Astrophysics Data System (ADS)

Keyvani, A.; Yeganeh, M.; Rezaeyan, H.

2017-04-01

In this study, Zn-Co-Mo coatings were deposited on the steel substrate from a citrate bath after adjusting pH, concentration, and current density. The morphology, the content of alloying elements, and the thickness of deposits were studied. Deposition behavior of these ternary coatings was examined by cathodic polarization and cyclic voltammetry (CV) techniques. The synthesized deposits were investigated by scanning electron microscopy (SEM), energy-dispersive x-ray (EDX) analysis, x-ray diffraction (XRD), electrochemical impedance spectroscopy (EIS), and potentiodynamic polarization methods. The results showed that the deposition potential of Zn-Co-Mo alloy was feasible in negative potentials higher than about -1.25 V versus Ag/AgCl. Moreover, the corrosion behavior of these coatings was found to be related to the extent of Mo as well as the local anodes and cathodes. The amount of molybdenum in the Zn-Co-Mo coating varied from 2.6 to 14 wt.% as a result of changing the pH. Based on the experimental findings, a narrow range of pH values between 5 and 5.5 could contribute to the high quality of coating in conjunction with the corrosion resistant alloy. Besides, the coatings with Mo element could show a passive-like behavior in the anodic region.

Internal stresses in wear and corrosion resistant amorphous metallic coatings of (W/0.6/Re/0.4/)76B24 and (Mo/0.6/Ru/0.4/)82B18

NASA Technical Reports Server (NTRS)

Thakoor, A. P.; Lamb, J. L.; Williams, R. M.; Khanna, S. K.

1985-01-01

Hard protective coatings in the W-Re-B and Mo-Ru-B alloy systems have been deposited by magnetron sputtering onto soda-lime glass and heat-treated AISI 52100 steel substrates. X-ray diffraction has confirmed the amorphous nature of the as-deposited coatings, and their crystallization temperatures were determined by differential thermal analysis to be 1000 and 790 C for W-Re-B and Mo-Ru-B coatings, respectively. Both coatings exhibit high microhardness; Mo-Ru-B, in addition, has excellent corrosion resistance by comparison with pure Mo at high anodic potentials. Attention is given to the influence of internal stresses on the protective properties of the coatings deposited under different conditions.

An Assessment of the Residual Stresses in Low Pressure Plasma Sprayed Coatings on an Advanced Copper Alloy

NASA Technical Reports Server (NTRS)

Raj, S. V.; Ghosn, L. J.; Agarwal, A.; Lachtrupp, T. P.

2002-01-01

Modeling studies were conducted on low pressure plasma sprayed (LPPS) NiAl top coat applied to an advanced Cu-8(at.%)Cr-4%Nb alloy (GRCop-84) substrate using Ni as a bond coat. A thermal analysis suggested that the NiAl and Ni top and bond coats, respectively, would provide adequate thermal protection to the GRCop-84 substrate in a rocket engine operating under high heat flux conditions. Residual stress measurements were conducted at different depths from the free surface on coated and uncoated GRCop-84 specimens by x-ray diffraction. These data are compared with theoretically estimated values assessed by a finite element analysis simulating the development of these stresses as the coated substrate cools down from the plasma spraying temperature to room temperature.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

About structural phase state of coating based on zirconium oxide formed by microplasma oxidation method

NASA Astrophysics Data System (ADS)

Gubaidulina, Tatiana A.; Sergeev, Viktor P.; Kuzmin, Oleg S.; Fedorischeva, Marina V.; Kalashnikov, Mark P.

2017-12-01

The oxide-ceramic coating based of zirconium oxide is formed by the method of microplasma oxidation. The producing modes of the oxide layers on E110 zirconium alloy are under testing. It was found that using microplasma treatment of E110 zirconium in aluminosilicate electrolyte makes possible the formation of porous oxide-ceramic coatings based on zirconium alloyed by aluminum and niobium. The study is focused on the modes how to form heat-shielding coatings with controlled porosity and minimal amount of microcracks. The structural-phase state of the coating is studied by X-ray diffraction analysis and scanning electron microscopy (SEM). It was found that the ratio of the monoclinic and tetragonal phases changes with the change occurring in the coating formation modes.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS2 Nanoparticles

PubMed Central

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev

2018-01-01

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS2 (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end. PMID:29495394

Electrochemical Performance Estimation of Anodized AZ31B Magnesium Alloy as Function of Change in the Current Density

NASA Astrophysics Data System (ADS)

Girón, L.; Aperador, W.; Tirado, L.; Franco, F.; Caicedo, J. C.

2017-08-01

The anodized AZ31B magnesium alloys were synthesized via electrodeposition processes. The aim of this work was to determine the electrochemical behavior of magnesium alloys by using anodized alloys as a protective coating. The anodized alloys were characterized by x-ray diffraction, exhibiting the crystallography orientation for Mg and MgO phases. The x-ray photoelectron spectroscopy was used to determine the chemical composition of anodized magnesium alloys. By using electrochemical impedance spectroscopy and Tafel curves, it was possible to estimate the electrochemical behavior of anodized AZ31B magnesium alloys in Hank's balanced salt solution (HBSS). Scanning electron microscopy was performed to analyze chemical changes and morphological surface changes on anodized Mg alloys due to the reaction in HBSS/anodized magnesium surface interface. Electrochemical behavior in HBSS indicates that the coatings may be a promising material for biomedical industry.

Characterization of LaF 3 coatings prepared at different temperatures and rates

NASA Astrophysics Data System (ADS)

Yu, Hua; Shen, Yanming; Cui, Yun; Qi, Hongji; Shao, JianDa; Fan, ZhengXiu

2008-01-01

LaF 3 thin films were prepared by thermal boat evaporation at different substrate temperatures and various deposition rates. X-ray diffraction (XRD), Lambda 900 spectrophotometer and X-ray photoelectron spectroscopy (XPS) were employed to study crystal structure, transmittance and chemical composition of the coatings, respectively. Laser-induce damage threshold (LIDT) was determined by a tripled Nd:YAG laser system with a pulse width of 8 ns. It is found that the crystal structure became more perfect and the refractive index increased gradually with the temperature rising. The LIDT was comparatively high at high temperature. In the other hand, the crystallization status also became better and the refractive index increased when the deposition rate enhanced at a low level. If the rate was super rapid, the crystallization worsened instead and the refractive index would lessen greatly. On the whole, the LIDT decreased with increasing rate.

Characterization of mineral coatings associated with a Pleistocene-Holocene rock art style: The Northern Running Figures of the East Alligator River region, western Arnhem Land, Australia.

PubMed

King, Penelope L; Troitzsch, Ulrike; Jones, Tristen

2017-02-01

This data article contains mineralogic and chemical data from mineral coatings associated with rock art from the East Alligator River region. The coatings were collected adjacent to a rock art style known as the "Northern Running Figures" for the purposes of radiocarbon dating (doi:10.1016/j.jasrep.2016.11.016; (T. Jones, V. Levchenko, P.L. King, U. Troitzsch, D. Wesley, 2017) [1]). This contribution includes raw and processed powder X-ray Diffraction data, Scanning Electron Microscopy energy dispersive spectroscopy data, and Fourier Transform infrared spectral data.

Study on industrial wastewater treatment using superconducting magnetic separation

NASA Astrophysics Data System (ADS)

Zhang, Hao; Zhao, Zhengquan; Xu, Xiangdong; Li, Laifeng

2011-06-01

The mechanism of industrial wastewater treatment using superconducting magnetic separation is investigated. Fe 3O 4 nanoparticles were prepared by liquid precipitation and characterized by X-ray diffraction (XRD). Polyacrylic acid (PAA) film was coated on the magnetic particles using plasma coating technique. Transmission electron microscope (TEM) observation and infrared spectrum measurement indicate that the particle surface is well coated with PAA, and the film thickness is around 1 nm. Practical paper factory wastewater treatment using the modified magnetic seeds in a superconducting magnet (SCM) was carried out. The results show that the maximum removal rate of chemical oxygen demand (COD) by SCM method can reach 76%.

Control of surface topography in biomimetic calcium phosphate coatings.

PubMed

Costa, Daniel O; Allo, Bedilu A; Klassen, Robert; Hutter, Jeffrey L; Dixon, S Jeffrey; Rizkalla, Amin S

2012-02-28

The behavior of cells responsible for bone formation, osseointegration, and bone bonding in vivo are governed by both the surface chemistry and topography of scaffold matrices. Bone-like apatite coatings represent a promising method to improve the osteoconductivity and bonding of synthetic scaffold materials to mineralized tissues for regenerative procedures in orthopedics and dentistry. Polycaprolactone (PCL) films were coated with calcium phosphates (CaP) by incubation in simulated body fluid (SBF). We investigated the effect of SBF ion concentration and soaking time on the surface properties of the resulting apatite coatings. CaP coatings were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), and energy dispersive X-ray spectrometry (EDX). Young's modulus (E(s)) was determined by nanoindentation, and surface roughness was assessed by atomic force microscopy (AFM) and mechanical stylus profilometry. CaP such as carbonate-substituted apatite were deposited onto PCL films. SEM and AFM images of the apatite coatings revealed an increase in topographical complexity and surface roughness with increasing ion concentration of SBF solutions. Young's moduli (E(s)) of various CaP coatings were not significantly different, regardless of the CaP phase or surface roughness. Thus, SBF with high ion concentrations may be used to coat synthetic polymers with CaP layers of different surface topography and roughness to improve the osteoconductivity and bone-bonding ability of the scaffold. © 2012 American Chemical Society

Influence of Applied Voltage and Film-Formation Time on Microstructure and Corrosion Resistance of Coatings Formed on Mg-Zn-Zr-Ca Bio-magnesium Alloy

NASA Astrophysics Data System (ADS)

Yandong, Yu; Shuzhen, Kuang; Jie, Li

2015-09-01

The influence of applied voltage and film-formation time on the microstructure and corrosion resistance of coatings formed on a Mg-Zn-Zr-Ca novel bio-magnesium alloy has been investigated by micro-arc oxidation (MAO) treatment. Phase composition and microstructure of as-coated samples were analyzed by the x-ray diffraction, energy dispersive x-ray spectroscopy and scanning electron microscopy. And the porosity and average of micro-pore aperture of the surface on ceramic coatings were analyzed by general image software. Corrosion microstructure of as-coated samples was caught by a microscope digital camera. The long-term corrosion resistance of as-coated samples was tested in simulated body fluid for 30 days. The results showed that the milky white smooth ceramic coating formed on the Mg-Zn-Zr-Ca novel bio-magnesium alloy was a compound of MgO, Mg2SiO4 and MgSiO3, and its corrosion resistance was significantly improved compared with that of the magnesium substrate. In addition, when the MAO applied voltage were 450 V and 500 V and film-formation time were 9 min and 11 min, the surface micro-morphology and the corrosion resistance of as-coated samples were relatively improved. The results provided a theoretical foundation for the application of the Mg-Zn-Zr-Ca novel bio-magnesium alloy in biomedicine.

Surface characteristics and electrochemical corrosion behavior of NiTi alloy coated with IrO2.

PubMed

Li, M; Wang, Y B; Zhang, X; Li, Q H; Liu, Q; Cheng, Y; Zheng, Y F; Xi, T F; Wei, S C

2013-01-01

The aim of this work is to investigate the surface characteristics and corrosion behavior of NiTi (50.6 at.% Ni) shape memory alloy coated by a ceramic-like and highly biocompatible material, iridium oxide (IrO2). IrO2 coatings were prepared by thermal decomposition of H2IrCl6 · 6H2O precursor solution at the temperature of 300 °C, 400 °C and 500 °C, respectively. The surface morphology and microstructure of the coatings were investigated by scanning electron microscope (SEM) and glancing angle X-ray diffraction (GAXRD). X-ray photoelectron spectroscopy (XPS) was employed to determine the surface elemental composition. Corrosion resistance property of the coated samples was studied in a simulated body fluid at 37±1 °C by electrochemical method. It was found that the morphology and microstructure of the coatings were closely related to the oxidizing temperatures. A relatively smooth, intact and amorphous coating was obtained when the H2IrCl6·6H2O precursor solution (0.03 mol/L) was thermally decomposed at 300 °C for 0.5 h. Compared with the bare NiTi alloy, IrO2 coated samples exhibited better corrosion resistance behavior to some extent. Copyright © 2012 Elsevier B.V. All rights reserved.

In vitro investigation of biodegradable polymeric coating for corrosion resistance of Mg-6Zn-Ca alloy in simulated body fluid.

PubMed

Gaur, Swati; Singh Raman, R K; Khanna, A S

2014-09-01

A silane-based biodegradable coating was developed and investigated to improve corrosion resistance of an Mg-6Zn-Ca magnesium alloy to delay the biodegradation of the alloy in the physiological environment. Conditions were optimized to develop a stable and uniform hydroxide layer on the alloys surface-known to facilitate silane-substrate adhesion. A composite coating of two silanes, namely, diethylphosphatoethyltriethoxysilane (DEPETES) and bis-[3-(triethoxysilyl) propyl] tetrasulfide (BTESPT), was developed, by the sol-gel route. Corrosion resistance of the coated alloy was characterized in a modified-simulated body fluid (m-SBF), using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The silane coating provided significant and durable corrosion resistance. During the course of this, hydrogen evolution and pH variation, if any, were monitored for both bare and coated alloys. The coating morphology was characterized using scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX) and the cross-linking in the coating was studied using Fourier transform infrared spectroscopy (FTIR). As indicated by X-ray diffraction (XRD) results, an important finding was the presence of hydrated magnesium phosphate on the sample that was subjected to immersion in m-SBF for 216h. Magnesium phosphate is reported to support osteoblast formation and tissue healing. Copyright © 2014 Elsevier B.V. All rights reserved.

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

Effect of Cu content on microstructure, mechanical and anti-fouling properties of TiSiN-Cu coating deposited by multi-arc ion plating

NASA Astrophysics Data System (ADS)

Bai, Xuebing; Li, Jinlong; Zhu, Lihui; Wang, Liping

2018-01-01

The copper-doped TiSiN coatings were deposited on 316L stainless steel by reactive co-sputtering in multi-arc ion plating. The surface morphology and structure of the coating were analyzed by scanning electron microcopies, X-ray diffraction and X-ray photoelectron spectroscopy. The hardness was tested using Nano-indentation. The influence of the copper content in the coatings on the structure and mechanical properties of TiSiN-Cu coatings was investigated. Antifouling behaviors of the coatings were evaluated by analyzing adhesion and propagation of P. tricornutum, N. closterium, and Chlorella sp. The TiSiN-Cu coatings had a unique structure of amorphous Si3N4 and nanocrystalline nc-TiN/nc-Cu. The Cu-TiSiN coatings can inhibit effectively attachment and colonization of the algae on the surface. When the copper content increases from 6.75 at.% to 25.15 at.%, the coatings show an obvious decrease in hardness, significantly increase in the surface roughness and greatly weaken in antifouling properties. When the copper content is 6.75 at.%, the coating has the highest hardness with 30 GPa, and the best reduction ratio with 89%, 93% and 57% attachment of P. triceratium, N. closterium and Chlorella sp., respectively. The TiSiN-Cu coating with a copper dosage of 6.75 at.% has the excellent mechanical properties and capability of killing effectively microalgae.

Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

PubMed

Catauro, M; Papale, F; Bollino, F

2016-01-01

The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Development of Multilayer Coatings for Hard X-Ray Optics at NASA Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Gurgew, Danielle N.; Broadway, David M.; Ramsey, Brian; Gregory, Don

2017-01-01

Broadband X-ray multilayer coatings are under development at NASA MSFC for use on future astronomical X-ray telescopes. Multilayer coatings deposited onto the reflecting surfaces of X-ray optics can provide a large bandpass enabling observations of higher energy astrophysical objects and phenomena.

Characterization of mechanical properties and electrochemical behaviour in a Hank´s solution of 316L/Cr1- xAlxN system

NASA Astrophysics Data System (ADS)

Osorio, D. M.; Caicedo, J. C.; Aperador, W.; Benitez-Castro, A. M.; Giraldo-Betancur, A. L.; Muñoz-Saldaña, J.; Yañez-Limón, J. M.; Sanchez, O.; Zambrano, G.

2017-01-01

Cr1-xAlxN hard coatings were successfully deposited by R.F. reactive magnetron co-sputtering in an Ar/N2 gas mixture using chromium and aluminium targets on 316L stainless steel substrates. Crystallographic orientations associated to the Cr1-xAlxN FCC based in the conjugate complex of CrN and w-AlN phases, with ao=4.18Å lattice parameter for the ternary Cr1-xAlxN compound were identified by X-Ray diffraction. The thickness and roughness of the deposited coatings are 1.00±0.05nm and 2.65±0.6nm, respectively. The mechanical properties were determined by nanoindentation leading to a hardness of 27.8±2.6GPa and elastic modulus of 346GPa. The corrosion resistance of the coated 316L/Cr1-xAlxN system under simulated body fluid (SBF, Hank’s solution) was determined via electrochemical impedance spectroscopy. A reduction in the corrosion rate of 99% in relation to uncoated 316L stainless steel substrate was found by Tafel. Thus, these coatings seem to be excellent candidates to be used in biomedical applications.

On the characterization of ultra-precise X-ray optical components: advances and challenges in ex situ metrology

PubMed Central

Siewert, F.; Buchheim, J.; Zeschke, T.; Störmer, M.; Falkenberg, G.; Sankari, R.

2014-01-01

To fully exploit the ultimate source properties of the next-generation light sources, such as free-electron lasers (FELs) and diffraction-limited storage rings (DLSRs), the quality requirements for gratings and reflective synchrotron optics, especially mirrors, have significantly increased. These coherence-preserving optical components for high-brightness sources will feature nanoscopic shape accuracies over macroscopic length scales up to 1000 mm. To enable high efficiency in terms of photon flux, such optics will be coated with application-tailored single or multilayer coatings. Advanced thin-film fabrication of today enables the synthesis of layers on the sub-nanometre precision level over a deposition length of up to 1500 mm. Specifically dedicated metrology instrumentation of comparable accuracy has been developed to characterize such optical elements. Second-generation slope-measuring profilers like the nanometre optical component measuring machine (NOM) at the BESSY-II Optics laboratory allow the inspection of up to 1500 mm-long reflective optical components with an accuracy better than 50 nrad r.m.s. Besides measuring the shape on top of the coated mirror, it is of particular interest to characterize the internal material properties of the mirror coating, which is the domain of X-rays. Layer thickness, density and interface roughness of single and multilayer coatings are investigated by means of X-ray reflectometry. In this publication recent achievements in the field of slope measuring metrology are shown and the characterization of different types of mirror coating demonstrated. Furthermore, upcoming challenges to the inspection of ultra-precise optical components designed to be used in future FEL and DLSR beamlines are discussed. PMID:25177985

Characterisation, corrosion resistance and in vitro bioactivity of manganese-doped hydroxyapatite films electrodeposited on titanium.

PubMed

Huang, Yong; Ding, Qiongqiong; Han, Shuguang; Yan, Yajing; Pang, Xiaofeng

2013-08-01

This work elucidated the corrosion resistance and in vitro bioactivity of electroplated manganese-doped hydroxyapatite (MnHAp) film on NaOH-treated titanium (Ti). The NaOH treatment process was performed on Ti surface to enhance the adhesion of the MnHAp coating on Ti. Scanning electron microscopy images showed that the MnHAp coating had needle-like apatite crystals, and the approximately 10 μm thick layer was denser than HAp. Energy-dispersive X-ray spectroscopy analysis revealed that the MnHAp crystals were Ca-deficient and the Mn/P molar ratio was 0.048. X-ray diffraction confirmed the presence of single-phase MnHAp, which was aligned vertically to the substrate. Fourier transform infrared spectroscopy indicated the presence of phosphate bands ranging from 500 to 650 and 900 to 1,100 cm(-1), and a hydroxyl band at 3,571 cm(-1), which was characteristic of HAp. Bond strength test revealed that adhesion for the MnHAp coating was more enhanced than that of the HAp coating. Potentiodynamic polarisation test showed that the MnHAp-coated surface exhibited superior corrosion resistance over the HAp single-coated surface. Bioactivity test conducted by immersing the coatings in simulated body fluid showed that MnHAp coating can rapidly induce bone-like apatite nucleation and growth. Osteoblast cellular tests revealed that the MnHAp coating was better at improving the in vitro biocompatibility of Ti than the HAp coating.

Characterisation of the Microstructure of Fe–Al/Cr3C2 Composite Coatings

NASA Astrophysics Data System (ADS)

Liu, Xiaoming; JunhuiDong; Yang, Yuehong; Sun, Changming; Tuo, Ya; Li, Yanwei

2018-03-01

An Fe-Al/Cr3C2 composite coating is investigated to assess its suitability for treating high-temperature components in a power plant. The coating exhibits excellent high- temperature properties including good corrosion, erosion and friction-wear resistance at high temperatures. To deduce the formation of the Fe-Al/Cr3C2 composite coating and to provide an adequate theoretical basis for its extensive application, its structures and microstructures are investigated. Scanning electronic microscopy (SEM)is used along with energy-dispersive X-ray analysis (EDAX) to analyse the surface of the coating. Energy-dispersive spectroscopy (EDS) is used to analyse the cross-section of the coating. Further, X-ray diffraction (XRD) and transmission electron microscopy (TEM) are used to analyse the phases and micro structural features within the coating. The results reveal that the basic phases are two orderly inter metallic compounds (Fe3Al and FeAl) and that the reinforcement includes two oxides (Al2O3 and Cr2O3) as well as substantial quantities of Cr3C2. Al2O3is formed using two mechanisms: oxidation of aluminium in the coating and separation of Al2O3crystals from Fe3Al and FeAl. The grain size of Al2O3 and Cr2O3 in the coatings is nanometric. These two oxides may increase the corrosion-erosion and wear resistances of the coating when they are used as reinforcements.

Effect of laser power on the microstructure and mechanical properties of TiN/Ti3Al composite coatings on Ti6Al4V

NASA Astrophysics Data System (ADS)

Liu, Zhengdao; Zhang, Xiancheng; Xuan, Fuzhen; Wang, Zhengdong; Tu, Shandong

2013-07-01

Laser nitriding is one of the effective techniques to improve the surface properties of titanium alloys and has potential application in the life extension of last-stage steam turbine blades. However, cracking of surface coating is a common problem due to heat concentration in laser nitriding process. Conventionally, the cracks can be avoided through heat treatment, which may have an important influence on the mechanical properties of coating. Crack-free TiN/Ti3Al IMC coatings on Ti6Al4V are prepared by plasma spraying and laser nitriding. The microstructures, phase constitutes and compositions of the coating are observed and analyzed with scanning electron microscopy(SEM), X-ray diffraction(XRD) and X-ray energy-dispersive spectroscopy(EDS). Microhardness, elastic modulus, fracture toughness of the coating are measured. The results show that the crack- and pore-free IMC coatings can be made through the proposed method; with increasing laser power, the amount and density of TiN phase in the coating first increased and then decreased, leading to the similar trend of microhardness and elastic modulus and the reverse trend of fracture toughness of the coating. Both the average microhardness and elastic modulus of the coating increase three times higher than those of the substrate. The volume fraction of the TiN reinforced phase in composite can be controlled by varying the laser power and the cracking problem in laser nitriding process is successfully solved.

Wavefront metrology for coherent hard X-rays by scanning a microsphere.

PubMed

Skjønsfjell, Eirik Torbjørn Bakken; Chushkin, Yuriy; Zontone, Federico; Patil, Nilesh; Gibaud, Alain; Breiby, Dag W

2016-05-16

Characterization of the wavefront of an X-ray beam is of primary importance for all applications where coherence plays a major role. Imaging techniques based on numerically retrieving the phase from interference patterns are often relying on an a-priori assumption of the wavefront shape. In Coherent X-ray Diffraction Imaging (CXDI) a planar incoming wave field is often assumed for the inversion of the measured diffraction pattern, which allows retrieving the real space image via simple Fourier transformation. It is therefore important to know how reliable the plane wave approximation is to describe the real wavefront. Here, we demonstrate that the quantitative wavefront shape and flux distribution of an X-ray beam used for CXDI can be measured by using a micrometer size metal-coated polymer sphere serving in a similar way as the hole array in a Hartmann wavefront sensor. The method relies on monitoring the shape and center of the scattered intensity distribution in the far field using a 2D area detector while raster-scanning the microsphere with respect to the incoming beam. The reconstructed X-ray wavefront was found to have a well-defined central region of approximately 16 µm diameter and a weaker, asymmetric, intensity distribution extending 30 µm from the beam center. The phase front distortion was primarily spherical with an effective radius of 0.55 m which matches the distance to the last upstream beam-defining slit, and could be accurately represented by Zernike polynomials.

Thermally Oxidized C, N Co-Doped ANATASE-TiO2 Coatings on Stainless Steel for Tribological Properties

NASA Astrophysics Data System (ADS)

Wang, Hefeng; Shu, Xuefeng; Li, Xiuyan; Tang, Bin; Lin, Naiming

2013-07-01

Ti(C, N) coatings were prepared on stainless steel (SS) substrates by plasma surface alloying technique. Carbon-nitrogen co-doped titanium dioxide (C-N-TiO2) coatings were fabricated by oxidative of the Ti(C, N) coatings in air. The prepared C-N-TiO2 coatings were characterized by SEM, XPS and XRD. Results reveal that the SS substrates were entirely shielded by the C-N-TiO2 coatings. The C-N-TiO2 coatings are anatase in structure as characterized by X-ray diffraction. The tribological behavior of the coatings was tested with ball-on-disc sliding wear and compared with substrate. Such a C-N-TiO2 coatings showed good adhesion with the substrate and tribological properties of the SS in terms of much reduced friction coefficient and increased wear resistance.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Lateral gradients of phases, residual stress and hardness in a laser heated Ti0.52Al0.48N coating on hard metal

PubMed Central

Bartosik, M.; Daniel, R.; Zhang, Z.; Deluca, M.; Ecker, W.; Stefenelli, M.; Klaus, M.; Genzel, C.; Mitterer, C.; Keckes, J.

2012-01-01

The influence of a local thermal treatment on the properties of Ti–Al–N coatings is not understood. In the present work, a Ti0.52Al0.48N coating on a WC–Co substrate was heated with a diode laser up to 900 °C for 30 s and radially symmetric lateral gradients of phases, residual stress and hardness were characterized ex-situ using position-resolved synchrotron X-ray diffraction, Raman spectroscopy, transmission electron microscopy and nanoindentation. The results reveal (i) a residual stress relaxation at the edge of the irradiated area and (ii) a compressive stress increase of few GPa in the irradiated area center due to the Ti–Al–N decomposition, in particular due to the formation of small wurtzite (w) AlN domains. The coating hardness increased from 35 to 47 GPa towards the center of the heated spot. In the underlying heated substrate, a residual stress change from about − 200 to 500 MPa down to a depth of 6 μm is observed. Complementary, in-situ high-temperature X-ray diffraction analysis of stresses in a homogeneously heated Ti0.52Al0.48N coating on a WC–Co substrate was performed in the range of 25–1003 °C. The in-situ experiment revealed the origin of the observed thermally-activated residual stress oscillation across the laser heated spot. Finally, it is demonstrated that the coupling of laser heating to produce lateral thermal gradients and position-resolved experimental techniques opens the possibility to perform fast screening of structure–property relationships in complex materials. PMID:23471140

Structural Characterization of Sputter-Deposited 304 Stainless Steel+10 wt pct Al Coatings

NASA Astrophysics Data System (ADS)

Seelam, Uma Maheswara Rao; Suryanarayana, C.; Heinrich, Helge; Ohkubo, Tadakatsu; Hono, Kazuhiro; Cheruvu, N. S.

2012-08-01

An SS304 + 10 wt pct Al (with a nominal composition of Fe-18Cr-8Ni-10Al by wt pct and corresponding to Fe-17Cr-6Ni-17Al by at. pct) coating was deposited on a 304-type austenitic stainless steel (Fe-18Cr-8Ni by wt pct) substrate by the magnetron sputter-deposition technique using two targets: 304-type stainless steel (SS304) and Al. The as-deposited coatings were characterized by X-ray diffraction, transmission electron microscopy, and three-dimensional (3-D) atom probe techniques. The coating consists of columnar grains with α ferrite with the body-centered cubic (bcc) (A2) structure and precipitates with a B2 structure. It also has a deposition-induced layered structure with two alternative layers (of 3.2 nm wavelength): one rich in Fe and Cr, and the other enriched with Al and Ni. The layer with high Ni and Al contents has a B2 structure. Direct confirmation of the presence of B2 phase in the coating was obtained by electron diffraction and 3-D atom probe techniques.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

X-ray structural investigation of nonsymmetrically and symmetrically alkylated [1]benzothieno[3,2-b]benzothiophene derivatives in bulk and thin films.

PubMed

Gbabode, Gabin; Dohr, Michael; Niebel, Claude; Balandier, Jean-Yves; Ruzié, Christian; Négrier, Philippe; Mondieig, Denise; Geerts, Yves H; Resel, Roland; Sferrazza, Michele

2014-08-27

A detailed structural study of the bulk and thin film phases observed for two potential high-performance organic semiconductors has been carried out. The molecules are based on [1]benzothieno[3,2-b]benzothiophene (BTBT) as conjugated core and octyl side groups, which are anchored either symmetrically at both sides of the BTBT core (C8-BTBT-C8) or nonsymmetrically at one side only (C8-BTBT). Thin films of different thickness (8-85 nm) have been prepared by spin-coating for both systems and analyzed by combining specular and grazing incidence X-ray diffraction. In the case of C8-BTBT-C8, the known crystal structure obtained from single-crystal investigations is observed within all thin films, down to a film thickness of 9 nm. In the case of C8-BTBT, the crystal structure of the bulk phase has been determined from X-ray powder diffraction data with a consistent matching of experimental and calculated X-ray diffraction patterns (Rwp = 5.8%). The packing arrangement of C8-BTBT is similar to that of C8-BTBT-C8, that is, consisting of a lamellar structure with molecules arranged in a "herringbone" fashion, yet with lamellae composed of two head-to-head (or tail-to-tail as the structure is periodic) superimposed molecules instead of only one molecule for C8-BTBT-C8. As for C8-BTBT-C8, we demonstrate that the same phase is observed in bulk and thin films for C8-BTBT whatever the film thickness investigated.

Investigation of phase transition properties of ZrO2 thin films

NASA Astrophysics Data System (ADS)

Kumar, Davinder; Singh, Avtar; Kaur, Manpreet; Rana, Vikrant Singh; Kaur, Raminder

2018-05-01

This paper presents the synthesis of transparent thin films of zirconium oxide (ZrO2) deposited on glass substrates by sol-gel dip coating technique. Synthesized films were characterized for different annealing time and withdrawal speed. Change in crystallographic properties of thin films was investigated by using X-ray diffraction. Surface morphology of transparent thin films was estimated by using scanning electron microscope.

Effects of Heat Treatment on Tribological Behavior of Electroless Ni-B Coating at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Mukhopadhyay, Arkadeb; Barman, Tapan Kumar; Sahoo, Prasanta

The present work investigates the effects of heat treatment on friction and wear behavior of electroless Ni-B coatings at elevated temperatures. Coating is deposited on AISI 1040 steel specimens and subjected to heat treatments at 350∘C, 400∘C and 450∘C. Coating characterization is done using scanning electron microscope, energy dispersive X-Ray analysis and X-Ray diffraction analysis. Improvement in microhardness is observed for the heat treated deposits. Further, the effect of heat treatment on the tribological behavior of the coatings at room temperature, 100∘C, 300∘C and 500∘C are analyzed on a pin-on-disc setup. Heat treatment at 350∘C causes a significant improvement in the tribological behavior at elevated temperatures. Higher heat treatment temperatures cause deterioration in the wear resistance and coefficient of friction. The wear mechanism at 100∘C is observed to be predominantly adhesive along with abrasion. While at 300∘C, abrasive wear is seen to be the governing wear phenomenon. Formation of mechanically mixed layers is noticed at both the test temperatures of 100∘C and 300∘C for the coatings heat treated at 400∘C and 450∘C test temperature. The predominant wear mechanisms at 500∘C are abrasive and fatigue for as-deposited and heat treated coatings, respectively.

Corrosive sliding wear behavior of laser clad Mo 2Ni 3Si/NiSi intermetallic coating

NASA Astrophysics Data System (ADS)

Lu, X. D.; Wang, H. M.

2005-05-01

Many ternary metal silicides such as W 2Ni 3Si, Ti 2Ni 3Si and Mo 2Ni 3Si with the topologically closed-packed (TCP) hP12 MgZn 2 type Laves phase crystal structure are expected to have outstanding wear and corrosion resistance due to their inherent high hardness and sluggish temperature dependence and strong atomic bonds. In this paper, Mo 2Ni 3Si/NiSi intermetallic coating was fabricated on substrate of an austenitic stainless steel AISI321 by laser cladding using Ni-Mo-Si elemental alloy powders. Microstructure of the coating was characterized by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive X-ray analysis (EDS). Wear resistance of the coating is evaluated under corrosive sliding wear test condition. Influence of corrosion solutions on the wear resistance of the coating was studied and the wear mechanism was discussed based on observations of worn surface morphology. Results showed that the laser clad Mo 2Ni 3Si/NiSi composite coating have a fine microstructure of Mo 2Ni 3Si primary dendrites and the interdendritic Mo 2Ni 3Si/NiSi eutectics. The coating has excellent corrosive wear resistance compared with austenitic stainless steel AISI321 under acid, alkaline and saline corrosive environments.

Structure and high temperature oxidation of mechanical alloyed Fe-Al coating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aryanto, Didik, E-mail: Didik-phys@yahoo.co.id, E-mail: didi027@lipi.go.id; Sudiro, Toto; Wismogroho, Agus S.

2016-04-19

The structure and high temperature oxidation resistance of Fe-Al coating on low carbon steel were investigated. The Fe-Al coating was deposited on the surface of low carbon steel using a mechanical alloying method. The coating was then annealed at 600°C for 2 hour in a vacuum of 5 Pa. The cyclic-oxidation tests of low carbon steel, Fe-Al coatings with and without annealing were performed at 600°C for up to 60h in air. The structure of oxidized samples was studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy X-ray spectroscopy (EDS). The results show that the Fe-Al coatingsmore » exhibit high oxidation resistance compared to the uncoated steel. After 60 h exposure, the uncoated steel formed mainly Fe{sub 3}O{sub 4} and Fe{sub 2}O{sub 3} layers with the total thickness of around 75.93 µm. Fe-Al coating without annealing formed a thin oxide layer, probably (Fe,Al){sub 2}O{sub 3}. Meanwhile, for annealed sample, EDX analysis observed the formation of two Fe-Al layers with difference in elements concentration. The obtained results suggest that the deposition of Fe-Al coating on low carbon steel can improve the oxidation resistance of low carbon steel.« less

Effects of alpha-zirconium phosphate on thermal degradation and flame retardancy of transparent intumescent fire protective coating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xing, Weiyi; Zhang, Ping; Song, Lei

2014-01-01

Graphical abstract: - Highlights: • A transparent intumescent fire protective coating was obtained by UV-cured technology. • OZrP could enhance the thermal stability and anti-oxidation of the coating. • OZrP could reduce the combustion properties of the coatings. - Abstract: Organophilic alpha-zirconium phosphate (OZrP) was used to improve the thermal and fire retardant behaviors of the phenyl di(acryloyloxyethyl)phosphate (PDHA)-triglycidyl isocyanurate acrylate (TGICA)-2-phenoxyethyl acrylate (PHEA) (PDHA-TGICA-PHEA) coating. The morphology of nanocomposite coating was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect of OZrP on the flame retardancy, thermal stability, fireproofing time and char formation of the coatingsmore » was investigated by microscale combustion calorimeter (MCC), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), laser Raman spectroscopy (LRS) and scanning electric microscope (SEM). The results showed that by adding OZrP, the peak heat release rate and total heat of combustion were significantly reduced. The highest improvement was achieved with 0.5 wt% OZrP. XPS analysis indicated that the performance of anti-oxidation of the coating was improved with the addition of OZrP, and SEM images showed that a good synergistic effect was obtained through a ceramic-like layer produced by OZrP covered on the surface of char.« less

An investigation of GaN thin films on AlN on sapphire substrate by sol-gel spin coating method

NASA Astrophysics Data System (ADS)

Amin, Nur Fahana Mohd; Ng, Sha Shiong

2017-12-01

In this research, the gallium nitride (GaN) thin films were deposited on aluminium nitride on sapphire (AlN/Al2O3) substrate by sol-gel spin coating method. Simple ethanol-based precursor with the addition of diethanolamine solution was used. The structural and morphology properties of synthesized GaN thin films were characterized by using X-ray Diffraction, Field-Emission Scanning Electron Microscopy and Atomic Force Microscopy. While the elemental compositions and the lattice vibrational properties of the films were investigated by means of the Energy Dispersive X-ray spectroscopy and Raman spectroscopy. All the results revealed that the wurtzite structure GaN thin films with GaN(002) preferred orientation and smooth surface morphology were successfully grown on AlN/Al2O3 substrate by using inexpensive and simplified sol-gel spin coating technique. The sol-gel spin coated GaN thin film with lowest oxygen content was also achieved.FESEM images show that GaN thin films with uniform and packed grains were formed. Based on the obtained results, it can be concluded that wurtzite structure GaN thin films were successfully deposited on AlN/Al2O3 substrate.

Relationship Between Crystalline Structure and Hardness of Ti-Si-N-O Coatings Fabricated by dc Sputtering

NASA Astrophysics Data System (ADS)

García-González, Leandro; Hernández-Torres, Julián; Mendoza-Barrera, Claudia; Meléndez-Lira, Miguel; García-Ramírez, Pedro J.; Martínez-Castillo, Jaime; Sauceda, Ángel; Herrera-May, Agustin L.; Muñoz Saldaña, Juan; Espinoza-Beltrán, Francisco J.

2008-08-01

Ti-Si-N-O coatings were deposited on AISI D2 tool steel and silicon substrates by dc reactive magnetron co-sputtering using a target of Ti-Si with a constant area ratio of 0.2. The substrate temperature was 400 °C and reactive atmosphere of nitrogen and argon. For all samples, argon flow was maintained constant at 25 sccm, while the flow of the nitrogen was varied to analyze the structural changes related to chemical composition and resistivity. According to results obtained by x-ray diffraction and stoichiometry calculations by x-ray energy dispersive spectroscopy the Ti-Si-N-O coatings contain two solid solutions. The higher crystalline part corresponds to titanium oxynitrure. Hardness tests on the coatings were carried out using the indentation work model and the hardness value was determined. Finally, the values of hardness were corroborated by nanoindentation test, and values of Young’s modulus and elastic recovery were discussed. We concluded that F2TSN sample ( F Ar = 25 sccm, F N = 5 sccm, P = 200 W, and P W = 8.9 × 10-3 mbar) presented the greatest hardness and the lowest resistivity values, due to its preferential crystalline orientation.

Fabrication of ternary Ni-TiO2-TiC composite coatings and their enhanced microhardness for metal finishing application

NASA Astrophysics Data System (ADS)

Kumaraguru, S.; Kumar, Gopika G.; Raghu, S.; Gnanamuthu, RM.

2018-07-01

Nickel (Ni) is extensively used for major engineering application. But nickel exhibits lower mechanical properties such as hardness and wear resistance than Ni-based composite materials. So, in this work, we significantly improve the mechanical properties of Ni by incorporating titanium dioxide (TiO2) and titanium carbide (TiC) particles. Ni-TiO2-TiC composite coatings are successfully prepared on mild steel specimens by means of electrodeposition technique. The prepared coatings are characterized by employing X-ray diffraction (XRD), energy dispersive X-ray fluorescence spectroscopy (EDXRF), scanning electron microscopy (SEM), atomic force microscopy (AFM) and Vicker's hardness tester. The surface morphological analysis points out the growth of cauliflower morphology and pyramid-like structure decorated with spherical particles at room temperature. Likewise, hill-valley like structure has been formed in the electrolyte temperature of 75 °C. The upshot of electrolyte temperature and concentration of TiO2-TiC particles on the microhardness of the composite deposits is investigated. The microhardness value is superior when the higher quantity of TiO2-TiC particles encapsulated in the coatings.

Facile preparation of superhydrophobic surfaces based on metal oxide nanoparticles

NASA Astrophysics Data System (ADS)

Bao, Xue-Mei; Cui, Jin-Feng; Sun, Han-Xue; Liang, Wei-Dong; Zhu, Zhao-Qi; An, Jin; Yang, Bao-Ping; La, Pei-Qing; Li, An

2014-06-01

A novel method for fabrication of superhydrophobic surfaces was developed by facile coating various metal oxide nanoparticles, including ZnO, Al2O3 and Fe3O4, on various substrates followed by treatment with polydimethylsiloxane (PDMS) via chemical vapor deposition (CVD) method. Using ZnO nanoparticles as a model, the changes in the surface chemical composition and crystalline structures of the metal oxide nanoparticles by PDMS treatment were investigated by X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) analysis. The results show that the combination of the improved surface roughness generated from of the nanoparticles aggregation with the low surface-energy of silicon-coating originated from the thermal pyrolysis of PDMS would be responsible for the surface superhydrophobicity. By a simple dip-coating method, we show that the metal oxide nanoparticles can be easily coated onto the surfaces of various textural and dimensional substrates, including glass slide, paper, fabric or sponge, for preparation of superhydrophobic surfaces for different purpose. The present strategy may provide an inexpensive and new route to surperhydrophobic surfaces, which would be of technological significance for various practical applications especially for separation of oils or organic contaminates from water.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Influence of Cu-Ti thin film surface properties on antimicrobial activity and viability of living cells.

PubMed

Wojcieszak, Damian; Kaczmarek, Danuta; Antosiak, Aleksandra; Mazur, Michal; Rybak, Zbigniew; Rusak, Agnieszka; Osekowska, Malgorzata; Poniedzialek, Agata; Gamian, Andrzej; Szponar, Bogumila

2015-11-01

The paper describes properties of thin-film coatings based on copper and titanium. Thin films were prepared by co-sputtering of Cu and Ti targets in argon plasma. Deposited coatings consist of 90at.% of Cu and 10at.% of Ti. Characterization of the film was made on the basis of investigations of microstructure and physicochemical properties of the surface. Methods such as scanning electron microscopy, x-ray microanalysis, x-ray diffraction, x-ray photoelectron spectroscopy, atomic force microscopy, optical profilometry and wettability measurements were used to assess the properties of deposited thin films. An impact of Cu-Ti coating on the growth of selected bacteria and viability of the living cells (line L929, NCTC clone 929) was described in relation to the structure, surface state and wettability of the film. It was found that as-deposited films were amorphous. However, in such surroundings the nanocrystalline grains of 10-15nm and 25-35nm size were present. High surface active area with a roughness of 8.9nm, had an effect on receiving relatively high water contact angle value (74.1°). Such wettability may promote cell adhesion and result in an increase of the probability of copper ion transfer from the film surface into the cell. Thin films revealed bactericidal and fungicidal effects even in short term-contact. High activity of prepared films was directly related to high amount (ca. 51 %) of copper ions at 1+ state as x-ray photoelectron spectroscopy results have shown. Copyright © 2015 Elsevier B.V. All rights reserved.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

CMAS Interactions with Advanced Environmental Barrier Coatings Deposited via Plasma Spray- Physical Vapor Deposition

NASA Technical Reports Server (NTRS)

Harder, B. J.; Wiesner, V. L.; Zhu, D.; Johnson, N. S.

2017-01-01

Materials for advanced turbine engines are expected to have temperature capabilities in the range of 1370-1500C. At these temperatures the ingestion of sand and dust particulate can result in the formation of corrosive glass deposits referred to as CMAS. The presence of this glass can both thermomechanically and thermochemically significantly degrade protective coatings on metallic and ceramic components. Plasma Spray- Physical Vapor Deposition (PS-PVD) was used to deposit advanced environmental barrier coating (EBC) systems for investigation on their interaction with CMAS compositions. Coatings were exposed to CMAS and furnace tested in air from 1 to 50 hours at temperatures ranging from 1200-1500C. Coating composition and crystal structure were tracked with X-ray diffraction and microstructure with electron microscopy.

Factors influencing phase compositions and structure of plasma sprayed hydroxyapatite coatings during heat treatment

NASA Astrophysics Data System (ADS)

Lu, Yu-Peng; Song, Yi-Zhong; Zhu, Rui-Fu; Li, Mu-Sen; Lei, Ting-Quan

2003-02-01

Heat treatment was expected to enhance the long-term reliability of hydroxyapatite (HA) coatings on metal substrates. In this study, factors influencing phase compositions and structure of plasma sprayed hydroxyapatite coatings during heat treatment were carefully analyzed. The phases were characterized by using X-ray diffraction (XRD), the OH - ion contents were determined by Fourier transform infrared (FTIR) spectroscopy. Of the involved factors, heating temperature is of more importance. The appropriate heat treatments is (600- 700 ° C)×2 h for coatings made from fine particles (10-20 μm) and 600 ° C×2 h for coatings made from coarse particles (50-80 μm). The excessive high temperatures and long holding times were unfavorable for the structural integrity of HA.

Flower-like Rh/Cu superhydrophobic coating via electrodeposition and its self-cleaning property

NASA Astrophysics Data System (ADS)

Zhao, N.; Lu, S. X.; Xu, W. G.; Cheng, X. L.

2017-01-01

Rh/Cu superhydrophobic coatings with textured flower-like dual micro-nano structures were fabricated on copper substrates via electrodesposition of Rh followed by annealing treatment. The scanning electron microscopy and X-ray diffraction pattern were conducted to analyse the morphology and chemical composition of the coating surfaces, respectively. The water drops exhibited a water contact angle of 168±1° and a sliding angle of 0±1° on the coating surfaces which were obtained by etching in concentrated hydrochloric acid and nitric acid, electrodeposited at -1.0 V for 30 min and annealing in an oven at 180°C for 60 min. The prepared superhydrophobic coatings showed excellent water repellence and self-cleaning property due to its extremely high water contact angle.

The role of microstructure and phase distribution in the failure mechanisms and life prediction model for PSZ coatings

NASA Technical Reports Server (NTRS)

Sisson, R. D., Jr.; Sone, Ichiro; Biederman, R. R.

1985-01-01

Partially Stabilized Zirconia (PSZ) may become widely used for Thermal Barrier Coatings (TBC). Failure of these coatings can occur due to thermal fatigue in oxidizing atmospheres. The failure is due to the strains that develop due to thermal gradients, differences in thermal expansion coefficients, and oxidation of the bond coating. The role of microstructure and the cubic, tetragonal, and monoclinic phase distribution in the strain development and subsequent failure will be discussed. An X-ray diffraction technique for accurate determination of the fraction of each phase in PSZ will be applied to understanding the phase transformations and strain development. These results will be discussed in terms of developing a model for life prediction in PSZ coatings during thermal cycling.

Structural and Optical Properties of La1−xSrxTiO3+δ

PubMed Central

Gao, Lihong; Ma, Zhuang; Wang, Song; Wang, Fuchi; Yang, Cai

2014-01-01

La1−xSrxTiO3+δ has attracted much attention as an important perovskite oxide. However, there are rare reports on its optical properties, especially reflectivity. In this paper, its structural and optical properties were studied. The X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and spectrophotometer were used to characterize the sample. The results show that with increasing Sr concentration, the number of TiO6 octahedral layers in each “slab” increases and the crystal structure changes from layered to cubic structure. A proper Sr doping (x = 0.1) can increase the reflectivity, reaching 95% in the near infrared range, which is comparable with metal Al measured in the same condition. This indicates its potential applications as optical protective coatings or anti-radiation materials at high temperatures. PMID:28788115

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Fabrication and Anti-Oxidation Ability of SiC-SiO₂ Coated Carbon Fibers Using Sol-Gel Method.

PubMed

Yang, Guangyuan; Huang, Zhixiong; Wang, Xu; Wang, Bo

2018-02-27

The paper proposed a method to improve the anti-oxidation performance of carbon fibers (CF) at high temperature environment by coating silicon dioxide (SiO₂) and silicon carbide (SiC). The modified sol-gel method had been used to ensure the proper interface between fibers and coating. We used polydimethylsiloxane and ethyl orthosilicate to make stable emulsion to uniformly disperse SiC nanoparticles. The modified SiO₂/SiC coating had been coated on CF successfully. Compared with the untreated CF, the coated fibers started to be oxidized around 900 °C and the residual weight was 57% at 1400 °C. The oxidation mechanism had been discussed. The structure of SiC/SiO₂ coated CF had been characterized by scanning electron microscope and X-ray diffraction analysis. Thermal gravimetric analysis was used to test the anti-oxidation ability of CF with different coatings.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Small, Leo J.; Brumbach, Michael T.; Clem, Paul G.

A new multi-step, solution-phase method for the spontaneous deposition of tungsten from a room temperature ethereal solution is reported. This immersion process relies on the deposition of a sacrificial zinc coating which is galvanically displaced by the ether-mediated reduction of oxophilic WCl 6. Subsequent thermal treatment renders a crystalline, metallic tungsten film. The chemical evolution of the surface and formation of a complex intermediate tungsten species is characterized by X-ray diffraction, infrared spectroscopy, and X-ray photoelectron spectroscopy. Efficient metallic tungsten deposition is first characterized on a graphite substrate and then demonstrated on a functional carbon foam electrode. The resulting electrochemicalmore » performance of the modified electrode is interrogated with the canonical aqueous ferricyanide system. A tungsten-coated carbon foam electrode showed that both electrode resistance and overall electrochemical cell resistance were reduced by 50%, resulting in a concomitant decrease in redox peak separation from 1.902 V to 0.783 V. Furthermore, this process promises voltage efficiency gains in electrodes for energy storage technologies and demonstrates the viability of a new route to tungsten coating for technologies and industries where high conductivity and chemical stability are paramount.« less

Simple sol-gel process to obtain silica-coated anatase particles with enhanced TiO2-SiO2 interfacial area.

PubMed

Resende, S F; Nunes, E H M; Houmard, M; Vasconcelos, W L

2014-11-01

In this study we prepared silica-titania composites with a low SiO2:TiO2 molar ratio. These materials were prepared using a simple sol-gel route in which a hydrothermal treatment was used to obtain mesoporous anatase particles. Pure titania was also synthetized for comparison purposes. These materials were examined by scanning and transmission electron microscopy (SEM and TEM, respectively), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and nitrogen sorption tests. A thin silica coating was formed on the anatase particles. It was observed that the presence of this coating led to samples with an enhanced thermal stability. Indeed, the composites prepared in this work showed an anatase structure and a high specific surface area (SSA), even after their calcination at 800°C. Thus, we believe that the synthetized material present an outstanding SiO2-TiO2 interfacial area associated with a high amount of anatase particles which could improve its photoactive properties. Copyright © 2014 Elsevier Inc. All rights reserved.

Electrodeposition and Characterization of Hydroxyapatite on TiN/316LSS.

PubMed

Nam, Pham Thi; Lam, Tran Dai; Huong, Ho Thu; Phuong, Nguyen Thu; Trang, Nguyen Thi Thu; Hoang, Thai; Huong, Nguyen Thi Thanh; Thang, Le Ba; Drouet, Christophe; Grossin, David; Kergourlay, Emmanuelle; Bertrand, Ghislaine; Devilliers, Didier; Thanh, Dinh Thi Mai

2015-12-01

The deposition of TiN on stainless steel substrates may improve the stability and compatibility of this material with bone, which may be advantageously exploited for the elaboration of advanced pros- thetic devices. In this work, TiN-coated 316LSS (by way of DC magnetron sputtering) was used as a starting material for investigating the electrochemical post-deposition of hydroxyapatite (HAp) which has a composition close to that of bone. Electrodeposition was carried out starting from an aqueous medium containing solubilized Ca(NO3)2 and NH4H2PO4 in the presence of H2O2. We report the influence of experimental conditions on the morphology of the obtained HAp coating on TiN/316LSS. The effect of applied potential, temperature, H2O2 concentration, pH and duration of reaction were thoroughly discussed on the basis of X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and Energy Dispersive X-ray Spectroscopy (EDX) results. This method appears advantageous for producing HAp-coated implant materials.

Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

NASA Astrophysics Data System (ADS)

Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

2017-03-01

Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

Surface characteristics and corrosion behaviour of WE43 magnesium alloy coated by SiC film

NASA Astrophysics Data System (ADS)

Li, M.; Cheng, Y.; Zheng, Y. F.; Zhang, X.; Xi, T. F.; Wei, S. C.

2012-01-01

Amorphous SiC film has been successfully fabricated on the surface of WE43 magnesium alloy by plasma enhanced chemical vapour deposition (PECVD) technique. The microstructure and elemental composition were analyzed by transmission electron microscopy (TEM), glancing angle X-ray diffraction (GAXRD) and X-ray photoelectron spectroscopy (XPS), respectively. The immersion test indicated that SiC film could efficiently slow down the degradation rate of WE43 alloy in simulated body fluid (SBF) at 37 ± 1 °C. The indirect toxicity experiment was conducted using L929 cell line and the results showed that the extraction medium of SiC coated WE43 alloys exhibited no inhibitory effect on L929 cell growth. The in vitro hemocompatibility of the samples was investigated by hemolysis test and blood platelets adhesion test, and it was found that the hemolysis rate of the coated WE43 alloy decreased greatly, and the platelets attached on the SiC film were slightly activated with a round shape. It could be concluded that SiC film prepared by PECVD made WE43 alloy more appropriate to biomedical application.

Influence of boron content on the microstructure and tribological properties of Cr-B-N coatings in water lubrication

NASA Astrophysics Data System (ADS)

Ma, Qiang; Zhou, Fei; Gao, Song; Wu, Zhiwei; Wang, Qianzhi; Chen, Kangmin; Zhou, Zhifeng; Li, Lawrence Kwok-Yan

2016-07-01

Cr-B-N coatings with different boron contents were deposited on Si(1 0 0) wafers and 316 L stainless steels using unbalanced magnetron sputtering system by way of adjusting the CrB2 target currents. The microstructure and mechanical properties of Cr-B-N coatings were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), white light interferometric three dimensional profilometer and nano-indentation tester, respectively. The tribological properties of Cr-B-N/SiC tribopairs in water were studied using ball-on-disk tribometer. The results showed that the Cr-B-N coatings showed a fine nanocomposite structure consisted of CrN nanograins and amorphous BN phase regardless of boron contents, and the typical columnar structure became featureless with increasing the CrB2 target current. The hardness and reduced elastic modulus first increased to 28.9 GPa and 330 GPa at the CrB2 target current of 2 A, and then decreased gradually with further increasing the CrB2 target current to 4 A. As compared with the CrN/SiC tribopairs, the lowest friction coefficient of Cr-B-N/SiC ball tribopairs in water was 0.15, and the wear resistance of Cr-B-N coatings was effectively enhanced.

Dye sensitized solar cell applications of CdTiO3-TiO2 composite thin films deposited from single molecular complex

NASA Astrophysics Data System (ADS)

Ehsan, Muhammad Ali; Khaledi, Hamid; Pandikumar, Alagarsamy; Huang, Nay Ming; Arifin, Zainudin; Mazhar, Muhammad

2015-10-01

A heterobimetallic complex [Cd2Ti4(μ-O)6(TFA)8(THF)6]·1.5THF (1) (TFA=trifluoroacetato, THF=tetrahydrofuran) comprising of Cd:Ti (1:2) ratio was synthesized by a chemical reaction of cadmium (II) acetate with titanium (IV) isopropoxide and triflouroacetic acid in THF. The stoichiometry of (1) was recognized by single crystal X-ray diffraction, spectroscopic and elemental analyses. Thermal studies revealed that (1) neatly decomposes at 450 °C to furnish 1:1 ratio of cadmium titanate:titania composite oxides material. The thin films of CdTiO3-TiO2 composite oxides were deposited at 550 °C on fluorine doped tin oxide coated conducting glass substrate in air ambient. The micro-structure, crystallinity, phase identification and chemical composition of microspherical architectured CdTiO3-TiO2 composite thin film have been determined by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analysis. The scope of composite thin film having band gap of 3.1 eV was explored as photoanode for dye-sensitized solar cell application.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

PubMed

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-02-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. © 2013.

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

HVOF coatings of Diamalloy 2002 and Diamalloy 4010 onto steel: Tensile and bending response of coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Al-Shehri, Y. A.; Hashmi, M. S. J.; Yilbas, B. S.

HVOF coating of Diamalloy 2002 powders and Diamalloy 4010 powders as well as two-layered coatings consisting of these powders is carried out. In the two-layered structure, Diamalloy 4010 is sprayed at the substrate surface while Diamalloy 2002 is sprayed on the top of Diamalloy 4010 coating. The mechanical properties of the coatings are examined through tensile and three-point bending tests. The coating microstructure and morphology are examined using the Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray diffraction (XRD). It is found that the coating produced is free from defects including voids and cracks. The failure mechanism ofmore » coating during tensile and three-point bending tests is mainly crack formation and propagation in the coating. The elastic modulus of coating produced from Diamalloy 2002 is higher than that of Diamalloy 4010 coating, which is due to the presence of 12% WC in the coating.« less

Magnesium-Aluminum-Zirconium Oxide Amorphous Ternary Composite: A Dense and Stable Optical Coating

NASA Technical Reports Server (NTRS)

Sahoo, N. K.; Shapiro, A. P.

1998-01-01

In the present work, the process parameter dependent optical and structural properties of MgO-Al(2)O(3)-ZrO(2) ternary mixed-composite material have been investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases and process dependent material composition of films have been investigated through the use of Atomic Force Microscopy (AFM), X-ray diffraction analysis and Energy Dispersive X- ray (EDX) analysis. EDX analysis made evident the correlation between the optical constants and the process dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

Processing-property relations in YBa2Cu3O(6+x) superconductors

NASA Astrophysics Data System (ADS)

Safari, A.; Wachtman, J. B., Jr.; Parkhe, V.; Caracciolo, R.; Jeter, D.

Processing of YBa2Cu3O(6+x) superconducting samples by employing different precursor powder preparation techniques such as ball milling, attrition milling, and narrow particle size distribution powder preparation through coprecipitation by spraying will be discussed. CuO coated with oxalates shows the lowest resistance above Tc up to room temperature. The extent of corrosion by water has been studied by employing magnetic susceptibility, XPS, and X-ray diffraction. Superconducting samples are affected to a considerable extent when treated in water at 60 C and the severity of the attack increases with time.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

In operando X-ray diffraction strain measurement in Ni 3Sn 2 – Coated inverse opal nanoscaffold anodes for Li-ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Glazer, Matthew P. B.; Wang, Junjie; Cho, Jiung

Volume changes associated with the (de)lithiation of a nanostructured Ni 3Sn 2 coated nickel inverse opal scaffold anode create mismatch stresses and strains between the Ni 3Sn 2 anode material and its mechanically supporting Ni scaffold. By using in operando synchrotron x-ray diffraction measurements, elastic strains in the Ni scaffold are determined during cyclic (dis)charging of the Ni 3Sn 2 anode. These strains are characterized using both the center position of the Ni diffraction peaks, to quantify the average strain, and the peak breadth, which describes the distribution of strain in the measured volume. Upon lithiation (half-cell discharging) or delithiationmore » (half-cell charging), compressive strains and peak breadth linearly increase or decrease, respectively, with charge. The evolution of the average strains and peak breadths suggests that some irreversible plastic deformation and/or delamination occurs during cycling, which can result in capacity fade in the anode. The strain behavior associated with cycling of the Ni 3Sn 2 anode is similar to that observed in recent studies on a Ni inverse-opal supported amorphous Si anode and demonstrates that the (de)lithiation-induced deformation and damage mechanisms are likely equivalent in both anodes, even though the magnitude of mismatch strain in the Ni 3Sn 2 is lower due to the lower (de)lithiation-induced contraction/expansion.« less

In operando X-ray diffraction strain measurement in Ni 3Sn 2 – Coated inverse opal nanoscaffold anodes for Li-ion batteries

DOE PAGES

Glazer, Matthew P. B.; Wang, Junjie; Cho, Jiung; ...

2017-11-01

Volume changes associated with the (de)lithiation of a nanostructured Ni 3Sn 2 coated nickel inverse opal scaffold anode create mismatch stresses and strains between the Ni 3Sn 2 anode material and its mechanically supporting Ni scaffold. By using in operando synchrotron x-ray diffraction measurements, elastic strains in the Ni scaffold are determined during cyclic (dis)charging of the Ni 3Sn 2 anode. These strains are characterized using both the center position of the Ni diffraction peaks, to quantify the average strain, and the peak breadth, which describes the distribution of strain in the measured volume. Upon lithiation (half-cell discharging) or delithiationmore » (half-cell charging), compressive strains and peak breadth linearly increase or decrease, respectively, with charge. The evolution of the average strains and peak breadths suggests that some irreversible plastic deformation and/or delamination occurs during cycling, which can result in capacity fade in the anode. The strain behavior associated with cycling of the Ni 3Sn 2 anode is similar to that observed in recent studies on a Ni inverse-opal supported amorphous Si anode and demonstrates that the (de)lithiation-induced deformation and damage mechanisms are likely equivalent in both anodes, even though the magnitude of mismatch strain in the Ni 3Sn 2 is lower due to the lower (de)lithiation-induced contraction/expansion.« less

Potentiodynamic Polarization Studies and Surface Chemical Composition of Bismuth Titanate (Bi x Ti y O z ) Films Produced through Radiofrequency Magnetron Sputtering.

PubMed

Alfonso, José E; Olaya, Jhon J; Pinzón, Manuel J; Marco, José F

2013-10-08

The applications of Bismuth Titanate (Bi x Ti y O z ) materials have been focused on their electronic and optical properties, but with respect to the use of these compounds in applications like corrosion resistance, have been very few or nonexistent. For this reason, in the present investigation Bi x Ti y O z thin films were deposited using RF magnetron sputtering onto silicon wafers, stainless steel 316L, and titanium alloy (Ti₆Al₄V) substrates, in order to carry out a study of the corrosion behavior of this compound. The structural properties of the coatings were studied through X-ray diffraction (XRD), the morphology was determined using Scanning Electron Microscopy (SEM), the corrosion resistance behavior of the coated and uncoated substrates was evaluated via the Potentiodynamic Polarization technique, and surface chemical composition was evaluated through X-ray photoelectron spectroscopy (XPS). The XRD results indicated that the films were amorphous. The SEM micrographs showed that the deposited films were homogeneous, but in some cases there were cracks. The potentiodynamic polarization technique showed that the corrosion current in the coated substrates decreased by an order of two magnitudes with respect to the uncoated substrates, but in both cases the corrosion mechanism was pitting due to the pores in the film. The XPS analysis shows that the deposited films contain both Bi 3+ and Ti 4+ .

Nanostructured Ag+-substituted fluorhydroxyapatite-TiO2 coatings for enhanced bactericidal effects and osteoinductivity of Ti for biomedical applications

PubMed Central

Chang, Xiaotong; Wang, Zhenhui; Zhang, Xuejiao; Han, Shuguang; Su, Zhuobin; Yang, Hejie; Yang, Dongdong; Zhang, Xiaojun

2018-01-01

Background Poor mechanical properties, undesirable fast dissolution rate, and lack of antibacterial activity limit the application of hydroxyapatite (HA) as an implant coating material. To overcome these limitations, a hybrid coating of Ag+-substituted fluorhydroxyapatite and titania nanotube (TNT) was prepared. Methods The incorporation of silver into the HA-TiO2 hybrid coating improves its antimicrobial properties. The addition of F as a second binary element increases the structural stability of the coating. The TNT/F-and-Ag-substituted HA (FAgHA) bilayer coating on the Ti substrate was confirmed by X-ray diffraction, scanning electron microscope, energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). Results The results indicate that the FAgHA/TNT nanocomposite coating has a dense and uniform morphology with a nano-rod-like structure. The solubility measurement result shows that the substitution of F− ions into the AgHA structure has a positive effect on the dissolution resistance of HA. The adhesion strength of FAgHA/TNT has significantly increased because of the interlocking of the roughened surface with nano-rod-like particles that entered into the voids of the TiO2 nanotubes. Compared with that of the bare Ti, the corrosion current density of FAgHA/TNT-coated Ti substrate decreased from 3.71 to 0.18 μA, and its corrosion resistance increased by almost two orders of magnitude. Moreover, despite pure HA, the FAgHA killed all viable Staphylococcus aureus after 24 hours of incubation. Although the fabricated FAgHA/TNT coating is hydrophobic, it induced deposition of the typical spherical apatite when immersed in a simulated body fluid (SBF); the osteoblasts spread very well on the surface of the coating. In addition, in vitro cell culture tests demonstrated cell viability and alkaline phosphatase (ALP) similar to pure HA, which indicated good cytocompatibility. Interestingly, compared with bare Ti, FAgHA/TNT-coated Ti surface was innocent for cell vitality and even more beneficial for cell osteogenesis in vitro. Conclusion Enhancing the osseointegration and preventing infection in implants, the FAgHA/TNT-coated Ti makes implants more successful. PMID:29760549

A study on microstructure and corrosion resistance of ZrO2-containing PEO coatings formed on AZ31 Mg alloy in phosphate-based electrolyte

NASA Astrophysics Data System (ADS)

Zhuang, J. J.; Guo, Y. Q.; Xiang, N.; Xiong, Y.; Hu, Q.; Song, R. G.

2015-12-01

ZrO2-containing ceramic coatings formed on the AZ31 Mg alloy were fabricated in an alkaline electrolyte containing sodium phosphate and potassium fluorozirconate (K2ZrF6) by plasma electrolytic oxidation (PEO). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) techniques were used to study the phase structure and composition of the coatings. It is indicated that the coatings formed in the K2ZrF6-containing electrolyte were composed of MgO, MgF2 and t-ZrO2. Morphological investigation carried out by scanning electron microscopy (SEM) and stereoscopic microscopy, revealed that the uniformity of coatings increased and roughness of coatings decreased after the addition of K2ZrF6. Electrochemical investigation was achieved by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) test. The results showed that the PEO coating formed in K2ZrF6-containing electrolyte exhibited an improved corrosion resistance than that of the coating formed in K2ZrF6-free electrolyte. In addition, the polarization and EIS tests results both showed that the suitable concentration (2.5 g/l) of K2ZrF6 is of significant ability to improve the corrosion resistance of coatings. However, 5 g/l and 10 g/l K2ZrF6 has a negative effect on improving the corrosion resistance of PEO coatings compared with the coating formed in 2.5 g/l K2ZrF6-containing electrolyte.

High-resolution coherent x-ray diffraction imaging of metal-coated polymer microspheres.

PubMed

Skjønsfjell, Eirik T B; Kleiven, David; Patil, Nilesh; Chushkin, Yuriy; Zontone, Federico; Gibaud, Alain; Breiby, Dag W

2018-01-01

Coherent x-ray diffraction imaging (CXDI) is becoming an important 3D quantitative microscopy technique, allowing structural investigation of a wide range of delicate mesoscale samples that cannot be imaged by other techniques like electron microscopy. Here we report high-resolution 3D CXDI performed on spherical microcomposites consisting of a polymer core coated with a triple layer of nickel-gold-silica. These composites are of high interest to the microelectronics industry, where they are applied in conducting adhesives as fine-pitch electrical contacts-which requires an exceptional degree of uniformity and reproducibility. Experimental techniques that can assess the state of the composites non-destructively, preferably also while embedded in electronic chips, are thus in high demand. We demonstrate that using CXDI, all four different material components of the composite could be identified, with radii matching well to the nominal specifications of the manufacturer. Moreover, CXDI provided detailed maps of layer thicknesses, roughnesses, and defects such as holes, thus also facilitating cross-layer correlations. The side length of the voxels in the reconstruction, given by the experimental geometry, was 16 nm. The effective resolution enabled resolving even the thinnest coating layer of ∼20  nm nominal width. We discuss critically the influence of the weak phase approximation and the projection approximation on the reconstructed electron density estimates, demonstrating that the latter has to be employed. We conclude that CXDI has excellent potential as a metrology tool for microscale composites.

Preparation, characterization and antibacterial applications of ZnO-nanoparticles coated polyethylene films for food packaging.

PubMed

Tankhiwale, Rasika; Bajpai, S K

2012-02-01

The present work describes the preparation of ZnO nanoparticles loaded starch-coated polyethylene film. The presence of ZnO nanoparticles was confirmed by surface plasmon resonance (SPR), X-ray diffraction (XRD) studies and transmission electron microscopy (TEM). The ZnO loaded film was tested for its biocidal action against model bacteria Escherichia coli using zone inhibition and killing kinetics of bacterial growth methods. This newly developed material bears potential to be used as food packaging material to prevent food stuff from bacterial contamination. Copyright © 2011 Elsevier B.V. All rights reserved.

IN SITU Deposition of Fe-TiC Nanocomposite on Steel by Laser Cladding

NASA Astrophysics Data System (ADS)

Razavi, Mansour; Rahimipour, Mohammad Reza; Ganji, Mojdeh; Ganjali, Mansoreh; Gangali, Monireh

The possibility of deposition of Fe-TiC nanocomposite on the surface of carbon steel substrate with the laser coating method had been investigated. Mechanical milling was used for the preparation of raw materials. The mixture of milled powders was used as a coating material on the substrate steel surface and a CO2 laser was used in continuous mode for coating. Microstructural studies were performed by scanning electron microscopy. Determinations of produced phases, crystallite size and mean strain have been done by X-ray diffraction. The hardness and wear resistance of coated samples were measured. The results showed that the in situ formation of Fe-TiC nanocomposite coating using laser method is possible. This coating has been successfully used to improve the hardness and wear resistance of the substrate so that the hardness increased by about six times. Coated iron and titanium carbide crystallite sizes were in the nanometer scale.

Resistance to Corrosion of Zirconia Coatings Deposited by Spray Pyrolysis in Nitrided Steel

NASA Astrophysics Data System (ADS)

Cubillos, G. I.; Olaya, J. J.; Bethencourt, M.; Cifredo, G.; Blanco, G.

2013-10-01

Coatings of zirconium oxide were deposited onto three types of stainless steel, AISI 316L, 2205, and tool steel AISI D2, using the ultrasonic spray pyrolysis method. The effect of the flux ratio on the process and its influence on the structure and morphology of the coatings were investigated. The coatings obtained, 600 nm thick, were characterized using x-ray diffraction, scanning electron microscopy, confocal microscopy, and atomic force microscopy. The resistance to corrosion of the coatings deposited over steel (not nitrided) and stainless steel nitrided (for 2 h at 823 K) in an ammonia atmosphere was evaluated. The zirconia coating enhances the stainless steel's resistance to corrosion, with the greatest increase in corrosion resistance being observed for tool steel. When the deposition is performed on previously nitrided stainless steel, the morphology of the surface improves and the coating is more homogeneous, which leads to an improved corrosion resistance.

Sonochemical coating of paper by microbiocidal silver nanoparticles.

PubMed

Gottesman, Ronen; Shukla, Sourabh; Perkas, Nina; Solovyov, Leonid A; Nitzan, Yeshayahu; Gedanken, Aharon

2011-01-18

Colloidal silver has gained wide acceptance as an antimicrobial agent, and various substrates coated with nanosilver such as fabrics, plastics, and metal have been shown to develop antimicrobial properties. Here, a simple method to develop coating of colloidal silver on paper using ultrasonic radiation is presented, and the coatings are characterized using X-ray diffraction (XRD), high resolution scanning electron microscope (HRSEM), and thermogravimetry (TGA) measurements. Depending on the variables such as precursor concentrations and ultrasonication time, uniform coatings ranging from 90 to 150 nm in thickness have been achieved. Focused ion beam (FIB) cross section imaging measurements revealed that silver nanoparticles penetrated the paper surface to a depth of more than 1 μm, resulting in highly stable coatings. The coated paper demonstrated antibacterial activity against E. coli and S. aureus, suggesting its potential application as a food packing material for longer shelf life.

High-temperature frictional wear behavior of MCrAlY-based coatings deposited by atmosphere plasma spraying

NASA Astrophysics Data System (ADS)

Tao, Chong; Wang, Lei; Song, Xiu

2017-02-01

Al2O3-Cr2O3/NiCoCrAlYTa coatings were prepared via atmosphere plasma spraying (APS). The microstructure and phase composition of the coatings were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser confocal scanning microscopy (LSCM), and transmission electron microscopy (TEM). The dry frictional wear behavior of the coatings at 500°C in static air was investigated and compared with that of 0Cr25Ni20 steel. The results show that the coatings comprise the slatted layers of oxide phases, unmelted particles, and pores. The hot abrasive resistance of the coatings is enhanced compared to that of 0Cr25Ni20, and their mass loss is approximately one-fifteenth that of 0Cr25Ni20 steel. The main wear failure mechanisms of the coatings are abrasive wear, fatigue wear, and adhesive wear.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Production of Nanocrystalline Ni-20Cr Coatings for High-Temperature Applications

NASA Astrophysics Data System (ADS)

Kumar, Manoj; Singh, Harpreet; Singh, Narinder

2014-04-01

Presynthesized nanocrystalline Ni-20Cr powder was deposited on SA 516 and T91 boiler steels by a high-velocity oxy-fuel spraying process. Ni-20Cr powder was synthesized by the ball milling approach. The high-temperature oxidation behavior of bare and coated samples was then studied under cyclic isothermal conditions at 900 °C for 50 cycles. The kinetics of oxidation was established using weight change measurements for the bare and coated boiler steels. Uncoated and coated samples of T91 steel were exposed to the superheated zone of a power plant boiler at 750 °C under cyclic conditions for 15 cycles. Each cycle consisted of 100 h of heating followed by 1 h of cooling. Attempts were made to study the kinetics of erosion-corrosion using weight change and thickness loss data for the samples. Different characterization techniques were used to study the oxidized and eroded-corroded samples, including x-ray diffraction, scanning electron microscopy/energy-dispersive spectroscopy, and x-ray mapping analyses. The Ni-20Cr alloy powder coating was found to offer excellent oxidation resistance to the base steels and was successful in reducing the weight gain of SA 516 steel by 98.5 % and that of T91 steel by 65 %. The coating was observed to reduce the erosion-corrosion rate of T91 steel by 86 % in terms of thickness loss. This indicates that the investigated nanostructured coating can be a better choice over conventional coating for erosion-corrosion control of boiler tubes.

Formation process of micro arc oxidation coatings obtained in a sodium phytate containing solution with and without CaCO3 on binary Mg-1.0Ca alloy

NASA Astrophysics Data System (ADS)

Zhang, R. F.; Zhang, Y. Q.; Zhang, S. F.; B. Qu; Guo, S. B.; Xiang, J. H.

2015-01-01

Micro arc oxidation (MAO) is an effective method to improve the corrosion resistance of magnesium alloys. In order to reveal the influence of alloying element Ca and CaCO3 electrolyte on the formation process and chemical compositions of MAO coatings on binary Mg-1.0Ca alloy, anodic coatings after different anodizing times were prepared on binary Mg-1.0Ca alloy in a base solution containing 3 g/L sodium hydroxide and 15 g/L sodium phytate with and without addition of CaCO3. The coating formation was studied by using scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD). The results show that Mg-1.0Ca alloy is composed of two phases, the Mg phase and Mg2Ca phase. After treating for 5 s, the coating began to develop and was preferentially formed on the area nearby Mg2Ca phase, which may be resulted from the intrinsic electronegative potential of the Mg phase than that of Mg2Ca phase. Anodic coatings unevenly covered the total surface after 20 s. After 80 s, the coatings were uniformly developed on Mg-1.0Ca alloy with micro pores. During MAO process, some sodium phytate molecules are hydrolyzed into inorganic phosphate. CaCO3 has minor influence on the calcium content of the obtained MAO coatings.

Influence of trimethylsilane flow on the microstructure, mechanical and tribological properties of CrSiCN coatings in water lubrication

NASA Astrophysics Data System (ADS)

Wu, Zhiwei; Zhou, Fei; Wang, Qianzhi; Zhou, Zhifeng; Yan, Jiwang; Li, Lawrence Kwok-Yan

2015-11-01

CrSiCN coatings with different silicon and carbon contents were deposited on silicon wafers and 316L stainless steels using unbalanced magnetron sputtering via adjusting trimethylsilane (TMS) flow, and their microstructure and mechanical properties were characterized by X-ray diffraction (XRD), scanning electron microscopy(SEM), X-ray photoelectrons spectroscopy(XPS) and nano-indenter, respectively. The tribological properties of CrSiCN coatings sliding against SiC balls in water were investigated using ball-on-disk tribometer. The results showed that the CrSiCN coatings had fine composite microstructure consisting of nanocrystallites of Cr(C, N) crystal and amorphous phases such as a-Si3N4 and a-C(a-CNx). The typical columnar structures changed from fine cluster to coarse ones when the Si content was beyond 3.4 at.%. With an increase in the TMS flow, the hardness and Young's modulus of Corsican coatings all first increased, and then rapidly decreased, but the compressive stress in the coatings varied in the range of 2.8-4.8 GPa. When the TMS flow was 10 sccm, the CrSiCN coatings exhibited the highest hardness of 21.3 GPa and the lowest friction coefficient (0.11) and wear rate (8.4 × 10-8 mm3/N m). But when the TMS flow was beyond 15 sccm, the tribological properties of CrSiCN coatings in water became poor.

Dual-scale rough multifunctional superhydrophobic ITO coatings prepared by air annealing of sputtered indium-tin alloy thin films

NASA Astrophysics Data System (ADS)

Gupta, Nitant; Sasikala, S.; Mahadik, D. B.; Rao, A. V.; Barshilia, Harish C.

2012-10-01

A novel method to fabricate multifunctional indium tin oxide (ITO) coatings is discussed. Superhydrophobic ITO coatings are fabricated by radio frequency balanced magnetron sputter deposition of indium-tin alloy on glass substrates followed by complete oxidation of the samples in air. The chemical nature and structure of the coatings are verified by X-ray diffraction, X-ray photoelectron spectroscopy and micro-Raman spectroscopy. Field emission scanning electron microscopic studies of the coatings display rod-like and blob-like microstructures, together with fractal-like nanostructures infused on top. Microscale roughness of the ITO coatings is measured by three-dimensional profilometry and is found to be in the range of 0.1-3 μm. Thus the presence of micro- and nano- sized structures result in dual-scale roughness. The variation in the contact angle with the deposition time is studied using a contact angle goniometer. High water contact angles (>160°) and low contact angle hysteresis (5°) are obtained at an optimum microscale roughness. The ITO coatings also exhibit other functional properties, such as low sheet resistance and semi-transparent behaviour in the visible region. The loss in the transparency of the ITO coatings is attributed to the presence of higher scale of roughness. The photoluminescence measurements show large photoemission in the visible region. It is expected that further improvements in the multifunctional properties of transparent conducting oxides will open new frontiers in designing novel materials with exotic properties.

Photoelectrochemical Properties of CuS-GeO2-TiO2 Composite Coating Electrode

PubMed Central

Wen, Xinyu; Zhang, Huawei

2016-01-01

The ITO (indium tin oxide) conductive glass-matrix CuS-GeO2-TiO2 composite coating was generated via EPD (electrophoretic deposition) and followed by a sintering treatment at 450°C for 40 minutes. Characterizations of the CuS-GeO2-TiO2 composite coating were taken by SEM (scanning electron microscope), XRD (X-ray diffraction), EDX (energy dispersive X-ray), UV-Vis DRS (ultraviolet-visible diffuse reflection spectrum), and FT-IR (Fourier transform infrared spectroscopy). Results showed that CuS and GeO2 had dispersed in this CuS-GeO2-TiO2 composite coating (mass percentages for CuS and GeO2 were 1.23% and 2.79%, respectively). The electrochemical studies (cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and Tafel polarization) of this CuS-GeO2-TiO2 composite coating electrode were performed in pH = 9.51 Na2CO3-NaHCO3 buffer solution containing 0.50 mol/L CH3OH under the conditions of visible light, ultraviolet light (λ = 365 nm), and dark (without light irradiation as control), respectively. Electrochemical studies indicated that this CuS-GeO2-TiO2 composite coating electrode had better photoelectrocatalytic activity than the pure TiO2 electrode in the electrocatalysis of methanol under visible light. PMID:27055277

Photoelectrochemical Properties of CuS-GeO2-TiO2 Composite Coating Electrode.

PubMed

Wen, Xinyu; Zhang, Huawei

2016-01-01

The ITO (indium tin oxide) conductive glass-matrix CuS-GeO2-TiO2 composite coating was generated via EPD (electrophoretic deposition) and followed by a sintering treatment at 450°C for 40 minutes. Characterizations of the CuS-GeO2-TiO2 composite coating were taken by SEM (scanning electron microscope), XRD (X-ray diffraction), EDX (energy dispersive X-ray), UV-Vis DRS (ultraviolet-visible diffuse reflection spectrum), and FT-IR (Fourier transform infrared spectroscopy). Results showed that CuS and GeO2 had dispersed in this CuS-GeO2-TiO2 composite coating (mass percentages for CuS and GeO2 were 1.23% and 2.79%, respectively). The electrochemical studies (cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and Tafel polarization) of this CuS-GeO2-TiO2 composite coating electrode were performed in pH = 9.51 Na2CO3-NaHCO3 buffer solution containing 0.50 mol/L CH3OH under the conditions of visible light, ultraviolet light (λ = 365 nm), and dark (without light irradiation as control), respectively. Electrochemical studies indicated that this CuS-GeO2-TiO2 composite coating electrode had better photoelectrocatalytic activity than the pure TiO2 electrode in the electrocatalysis of methanol under visible light.

Polypyrrole-coated LiCoO2 nanocomposite with enhanced electrochemical properties at high voltage for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Cao, Jingchao; Hu, Guorong; Peng, Zhongdong; Du, Ke; Cao, Yanbing

2015-05-01

A conducting polypyrrole thin film is successfully coated onto the surface of LiCoO2 by a simple chemical polymerization method. The structure and morphology of pristine LiCoO2 and PPy-coated LiCoO2 are investigated by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Energy dispersive X-ray spectroscopy (EDXS), Fourier transform infrared spectrometry (FTIR) and thermogravimetric analysis (TGA) further demonstrate the existence of PPy. The electrochemical properties of the composites are investigated by galvanostatic charge-discharge test and AC impedance measurements, which show that the conductive PPy film on the surface significantly decrease the charge-transfer resistance of LiCoO2. The PPy-coated LiCoO2 exhibits a good electrochemical performance, showing initial discharge capacity of 182 mAh g-1 and retains 94.3% after 170 cycles. However, the retention of pristine LiCoO2 is only 83.5%. The rate capability results show that the reversible capacity retention (10C/0.2C) of LiCoO2 increases from 52.4% to 80.1% after being coated with PPy. The continuously coated thin PPy film is just like a capsule shell, which can protect the core (LiCoO2) from corrosion causing by the HF attacking and greatly reduce the dissolution of Co into electrolyte.

Al-Mn CVD-FBR coating on P92 steel as protection against steam oxidation at 650 °C: TGA-MS study

NASA Astrophysics Data System (ADS)

Castañeda, S. I.; Pérez, F. J.

2018-02-01

The initial stages oxidation of the P92 ferritic/martensitic steel with and without Al-Mn coating at 650 °C in Ar+40%H2O for 240 h were investigated by mass spectrometry (MS) and thermogravimetric analysis (TGA). TGA-MS measurements were conducted in a closed steam loop. An Al-Mn coating was deposited on P92 steel at 580 °C for 2 h by chemical vapour deposition in a fluidized bed reactor (CVD-FBR). The coating as-deposited was treated in the same reactor at 700 °C in Ar for 2h, in order to produce aluminide phases that form the protective alumina layer (Al2O3) during oxidation. MS measurements at 650 °C of the Al-Mn/P92 sample for 200 h indicated the presence of (Al-Mn-Cr-Fe-O) volatile species of small intensity. Uncoated P92 steel oxidized under the same steam oxidation conditions emitted greater intensities of volatile species of Cr, Fe and Mo in comparison with intensities from coated steel. TGA measurements verified that the mass gained by the coated sample was up to 300 times lower than for uncoated P92 steel. The morphology, composition and structure of samples by Scanning Electron Microscopy SEM, Backscattered Electron (BSE) detection, X-ray Energy Dispersive Spectrometry (EDAX) and X-ray Diffraction (XRD) are described.

Bioinspired synthesis of a soft-nanofilament-based coating consisting of polysilsesquioxanes/polyamine and its divergent surface control.

PubMed

Yuan, Jian-Jun; Kimitsuka, Nobuo; Jin, Ren-Hua

2013-04-24

The synthesis of polysilsesquioxanes coating with controllable one-dimensional nanostructure on substrates remains a major long-term challenge by conventional solution-phase method. The hydrolytic polycondensation of organosilanes in solution normally produces a mixture of incomplete cages, ladderlike, and network structures, resulting in the poor control of the formation of specific nanostructure. This paper describes a simple aqueous process to synthesize nanofilament-based coatings of polysilsesquioxanes possessing various organo-functional groups (for example, thiol, methyl, phenyl, vinyl, and epoxy). We utilized a self-assembled nanostructured polyamine layer as a biomimetically catalytic scaffold/template to direct the formation of one-dimensional nanofilament of polysilsesquioxanes by temporally and spatially controlled hydrolytic polycondensation of organosilane. The surface nanostructure and morphology of polysilsesquioxane coating could be modulated by changing hydrolysis and condensation reaction conditions, and the orientation of nanofilaments of polysilsesquioxanes on substrates could be controlled by simply adjusting the self-assembly conditions of polyamine layer. The nanostructure and polyamine@polysilsesquioxane hybrid composition of nanofilament-based coatings were examined by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The template role of nanostructured polyamine layer for the formation of polysilsesquioxane nanofilament was confirmed by combining thin film X-ray diffraction (XRD) and XPS measurements. Moreover, these nanotextured coatings with various organo-functional groups could be changed into superhydrophobic surfaces after surface modification with fluorocarbon molecule.

Phase transformations and residual stresses in environmental barrier coatings

NASA Astrophysics Data System (ADS)

Harder, Bryan J.

Silicon-based ceramics (SiC, Si3N4) are promising materials for high-temperature structural applications in turbine engines. However, the silica layer that forms on these materials is susceptible to attack from water vapor present in combustion environments. To protect against this degradation, environmental barrier coatings (EBCs) were developed to protect the underlying substrate. In the case of silicon carbide (SiC), multilayer coating systems consist of a Ba1-xSrxAl2Si 2O8 (BSAS) topcoat, a mullite or mullite + SrAl2Si 2O8 (SAS) interlayer, and a silicon bond coat. In this work, biaxial strains were measured on as-sprayed and heat-treated samples to analyze the stress and phase evolution in the coating system as a function of depth and temperature. Models were used to compare the results with an ideal coating system. In the assprayed state, tensile stresses as high as 175 MPa were measured, and cracking was observed. After thermally cycling the samples, stresses were significantly reduced and cracks in the topcoat had closed. The addition of SAS to the interlayer increased the compressive stress in the BSAS topcoat in thermally-cycled samples, which was desirable for EBC applications. The BSAS topcoat transformed from the as-deposited hexacelsian state to the stable celsian above 1200°C. This phase transformation is accompanied by a CTE reduction. The kinetics of the hexacelsian-to-celsian transformation were quantified for freestanding plasma-sprayed BSAS. Activation energies for bulk bars and crushed powder were determined to be ˜340 kJ/mol and ˜500 kJ/mol, respectively. X-ray diffraction and electron backscatter diffraction were used to establish how microstructural constraints reduce the transformation energy. Barrier coating lifetime and stability are also influenced by exposure to reactive, low-melting point calcium-magnesium-aluminosilicate (CMAS) deposits formed from dust and sand. Multilayer doped aluminosilicate coatings and bulk BSAS material were exposed to CMAS glass at 1300°C for up to 48 hours. Stresses were measured as a function of depth in the multilayer coatings, and a compressive stress on the surface increased with exposure time from -50 MPa to a maximum of -160 MPa. Backscatter electron imaging and energy dispersive X-ray techniques demonstrated that infiltration depth of the glass increased with exposure time.

Preparation and Characterization of Plasma Electrolytic Oxidation Coating on 5005 Aluminum Alloy with Red Mud as an Electrolyte Additive

NASA Astrophysics Data System (ADS)

Liu, Shifeng; Zeng, Jianmin; Wang, Youbin

2017-10-01

A coating with red mud as an electrolyte additive was applied to 5005 aluminum alloy using plasma electrolytic oxidation (PEO). The phase composition of the coating was investigated using X-ray diffraction. Scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) was used to determine the microstructure and composition profiles of the coating. The coating/substrate adhesion was determined by scratch testing. The corrosion behaviors of the substrate and coating were evaluated using potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS). The results indicated that the PEO coating with red mud consisted mainly of α-Al2O3 and γ-Al2O3, with small amounts of Fe2O3, CaCO3, and CaTiO3. The surface of the coating was the color of the red mud. The coating had a uniform thickness of about 80 μm and consisted of two main layers: a 6- μm porous outer layer and a 74- μm dense inner layer, which showed typical metallurgical adhesion (coating/substrate adhesion strength of 59 N). The coating hardness was about 1142 HV, much higher than that of the substrate (60 HV). The corrosion potential E corr and corrosion current density i corr of the coating were estimated to be -0.743 V and 3.85 × 10-6 A cm-2 from the PDP curve in 3.5 wt pct NaCl solution, and the maximum impedance and phase angle of the coating were 11 000 Ω and -67 deg, respectively, based on EIS. PEO coating with red mud improved the surface properties and corrosion resistance of 5005 aluminum alloy. This study also shows a potential method for reusing red mud.

High temperature wear performance of HVOF-sprayed Cr3C2-WC-NiCoCrMo and Cr3C2-NiCr hardmetal coatings

NASA Astrophysics Data System (ADS)

Zhou, Wuxi; Zhou, Kesong; Li, Yuxi; Deng, Chunming; Zeng, Keli

2017-09-01

A novel Cr3C2-WC-NiCoCrMo and commercial Cr3C2-NiCr thermal spray-grade powders with particle size of -45 + 15 μm were prepared by an agglomeration and sintering process. Cr3C2-WC-NiCoCrMo and Cr3C2-NiCr coatings were deposited by high velocity oxygen fuel (HVOF) spraying. The fundamental properties of both coatings were evaluated and friction wear test against Al2O3 counterbodies of both coatings at high temperatures (450 °C, 550 °C, 650 °C) were carried out ball-on-disk high temperature tribometer. All specimens were characterized by optical microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy with energy dispersive spectroscopy (SEM/EDS) and 3D non-contact surface mapping profiler. The results have shown that the Cr3C2-WC-NiCoCrMo coating exhibited lower porosity, higher micro-hardness compared to the Cr3C2-NiCr coating. The Cr3C2-WC-NiCoCrMo coating also exhibited better wear resistance and higher friction coefficient compared to the Cr3C2-NiCr coating when sliding against the Al2O3 counterpart. Wear rates of both coatings increased with raising temperature. Both coatings experienced abrasive wear; hard phase particles (WC and Cr3C2) with different sizes, distributed in the matrix phase, will effectively improve the resistance against wear at high temperatures.

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Time-Resolved, High-Resolution, X-Ray Microscopy of In-Vitro Biological and Life Science Specimens with the Aid of Laser Plasmas

DTIC Science & Technology

1994-06-30

transmissive Fresnel lens. We have made considerable effort in the last few years to explore the potential of x-ray multilayer-coated Schwarzschild x-ray...ray mirror fabrication and efficient x-ray mirror design. A 120mm diameter, NA = 0.35, 15X Schwarzschild microscope coated with Ni/C multilayer mios for...et al 2 developed a smaller, 33mm diameter, NA - 0.28, 15X Schwarzschild microscope coated with a W/C multilayer mirror for 4.4nm, in the socalled

Preparation and characterization of SnO2 and Carbon Co-coated LiFePO4 cathode materials.

PubMed

Wang, Haibin; Liu, Shuxin; Huang, Yongmao

2014-04-01

The SnO2 and carbon co-coated LiFePO4 cathode materials were successfully synthesized by solid state method. The microstructure and morphology of LiFePO4 composites were characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy and transmission electron microscope. The results showed that the SnO2 and carbon co-coated LiFePO4 cathode materials exhibited more uniform particle size distribution. Compared with the uncoated LiFePO4/C, the structure of LiFePO4 with SnO2 and carbon coating had no change. The existence of SnO2 and carbon coating layer effectively enhanced the initial discharge capacity. Among the investigated samples, the one with DBTDL:LiFePO4 molar ratios of 7:100 exhibited the best electrochemical performance.

Electrophoretic deposition and electrochemical behavior of novel graphene oxide-hyaluronic acid-hydroxyapatite nanocomposite coatings

NASA Astrophysics Data System (ADS)

Li, Ming; Liu, Qian; Jia, Zhaojun; Xu, Xuchen; Shi, Yuying; Cheng, Yan; Zheng, Yufeng; Xi, Tingfei; Wei, Shicheng

2013-11-01

Novel ternary graphene oxide-hyaluronic acid-hydroxyapatite (GO-HY-HA) nanocomposite coatings were prepared on Ti substrate using anodic electrophoretic deposition (EPD). Hyaluronic acid was employed as charging additive and dispersion agent during EPD. The kinetics and mechanism of the deposition, and the microstructure of the coated samples were investigated using scanning electron microscopy, X-ray diffraction, Raman spectrum, thermo-gravimetric analysis, and microscopic Fourier transform infrared analysis. The results showed that the addition of GO sheets into the HY-HA suspensions could increase the deposition rate and inhibit cracks creation and propagation in the coatings. The corrosion resistant of the resulting samples were evaluated using potentiodynamic polarization method in simulated body fluid, and the GO-HY-HA coatings could effectively improve the anti-corrosion property of the Ti substrate.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Microstructures and Dry Sliding Wear Resistance of the Laser Ceramics Composite Coating on Pure Ti

NASA Astrophysics Data System (ADS)

Liu, Peng; Zhang, Yuanbin; Luo, Hui; Huo, Yushuang

2012-06-01

In this study, Al-Ti-Co was used to improve the surface performance of pure Ti. Laser cladding is an important surface modification technique, which can be used to improve the surface performance of pure Ti. Laser cladding of the Al-Ti-Co + TiB2 pre-placed powders on pure Ti can form ceramics reinforced the composite coating, which improved the wear resistance of the substrate. Characteristics of the composite coating were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and wear tests. And the laser-cladded coating can also have major dilution from the substrate. Due to the action of the fine grain strengthening and the phase constituent, the wear resistance and microhardness of pure Ti surface were greatly improved.

Synthesis of CoOOH nanorods and application as coating materials of nickel hydroxide for high temperature Ni-MH cells.

PubMed

Hu, W K; Gao, X P; Geng, M M; Gong, Z X; Noréus, D

2005-03-31

Studies on nanoscale materials have received great interest in both fundamental and applied aspects in recent years. In this letter, we report the synthesis of CoOOH nanorods and their possible applications as coating materials on nickel hydroxide for high-temperature nickel-metal hydride (Ni-MH) cells. The morphology and structure of CoOOH nanorods and coated nickel hydroxide particles are investigated by transmission electron microscopy, X-ray diffraction, and scanning electron microscopy, respectively. The electrochemical properties in the cylindrical AA size Ni-MH cells are evaluated. Our results show that the Ni-MH cells, where the positive electrodes are composed of such nanometer sized CoOOH coatings, have a higher capacity available and good performance at elevated temperatures of >50 degrees C.

Strong coercivity reduction and high initial permeability in NiCoP coated BaFe12O19-polystyrene bilayer composite

NASA Astrophysics Data System (ADS)

Hamad, Mahmoud A.; El-Sayed, Adly H.; Hemeda, O. M.; Tawfik, A.

2016-03-01

Soft-magnetic NiCoP coated hard-magnetic M-type ferrite BaFe12O19 (BaM)-polystyrene (PS) bilayer composite film was successfully synthesized. X-ray diffraction peaks exhibited no change in the structure of BaM after coating with PS. The NiCoP coated BaM-PS composite exhibited a wasp-waisted magnetic hysteretic loop with remarkable reduction in the coercivity, remanence and squareness with respect to BaM-PS, which is useful for the core of a magnetic switching device to control currents so large that they are unmanageable. Moreover, the initial permeability measurement exhibits initial permeability of around 100 000 and thermal stability up to 558 K, which is good for flux-amplifying components of smaller inductors.

The structural and bio-corrosion barrier performance of Mg-substituted fluorapatite coating on 316L stainless steel human body implant

NASA Astrophysics Data System (ADS)

Sharifnabi, A.; Fathi, M. H.; Eftekhari Yekta, B.; Hossainalipour, M.

2014-01-01

In this study, Mg-substituted fluorapatite coatings were deposited on medical grade AISI 316L stainless steel via sol-gel dip coating method. Phase composition, crystallite size and degree of crystallinity of the obtained coatings were evaluated by X-ray diffraction (XRD) analysis. Fourier transform infrared (FTIR) spectroscopy was also used to evaluate functional groups of the obtained coatings. The surface morphology and cross-section of the final coatings were studied using scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy was used to determine elemental chemical composition of the obtained coatings. In order to determine and compare the corrosion behavior of uncoated and Mg-substituted fluorapatite coated 316L stainless steel, electrochemical potentiodynamic polarization tests were performed in physiological solutions at 37 ± 1 °C. Moreover, the released metallic ions from uncoated and coated substrates were measured by inductively coupled plasma-optical emission spectrometry (ICP-OES) within 2 months of immersing in Ringer's solution at 36.5 ± 1 °C as an indication of biocompatibility. The results showed that fluoride and magnesium were successfully incorporated into apatite lattice structure and the prepared coatings were nanostructured with crystallinity of about 70%. Obtained coatings were totally crack-free and uniform and led to decrease in corrosion current densities of 316L stainless steel in physiological solutions. In addition, coated sample released much less ions such as Fe, Cr and Ni in physiological media. Therefore, it was concluded that Mg-substituted fluorapatite coatings could improve the corrosion resistance and biocompatibility of 316L stainless steel human body implants.

In vivo and in vitro investigations of a nanostructured coating material – a preclinical study

PubMed Central

Adam, Martin; Ganz, Cornelia; Xu, Weiguo; Sarajian, Hamid-Reza; Götz, Werner; Gerber, Thomas

2014-01-01

Immediate loading of dental implants is only possible if a firm bone-implant anchorage at early stages is developed. This implies early and high bone apposition onto the implant surface. A nanostructured coating material based on an osseoinductive bone grafting is investigated in relation to the osseointegration at early stages. The goal is to transmit the structure (silica matrix with embedded hydroxyapatite) and the properties of the bone grafting into a coating material. The bone grafting substitute offers an osseoinductive potential caused by an exchange of the silica matrix in vivo accompanied by vascularization. X-ray diffraction and transmission electron microscopy analysis show that the coating material consists of a high porous silica matrix with embedded nanocrystalline hydroxyapatite with the same morphology as human hydroxyapatite. An in vitro investigation shows the early interaction between coating and human blood. Energy-dispersive X-ray analysis showed that the silica matrix was replaced by an organic matrix within a few minutes. Uncoated and coated titanium implants were inserted into the femora of New Zealand White rabbits. The bone-to-implant contact (BIC) was measured after 2, 4, and 6 weeks. The BIC of the coated implants was increased significantly at 2 and 4 weeks. After 6 weeks, the BIC was decreased to the level of the control group. A histological analysis revealed high bone apposition on the coated implant surface after 2 and 4 weeks. Osteoblastic and osteoclastic activities on the coating material indicated that the coating participates in the bone-remodeling process. The nanostructure of the coating material led to an exchange of the silica matrix by an autologous, organic matrix without delamination of the coating. This is the key issue in understanding initial bone formation on a coated surface. PMID:24627631

Hot corrosion evaluation of aluminide coated superalloys in support of an ASTM Round Robin program

NASA Technical Reports Server (NTRS)

Santoro, G.

1975-01-01

Commercial aluminized coatings on substrates were hot corroded at 900 C in a 0.3 Mach burner rig with 5 ppm synthetic sea salt and at two cycling frequencies. Extensive post-exposure examinations were conducted on the corroded specimens such as metallography, X-ray diffraction, scanning electron microscopy, microprobe raster scans, and spectrographic analyses. Thermodynamic calculations were made of the equilibrium burner flame composition and the calculations were compared to the experimental findings. It was found that localized spalling of the coatings preceded coating failure. It is suggested that the spalling of the coatings is due to the formation of localized stresses caused by the depletion of chromium and aluminum in the coating or the enrichment of the coating with sulfur. For the materials and test conditions investigated, it was found that coating life is dependent only upon the initial coating thickness and not on the type of aluminized coating, the substrate, or the cycle frequency.

Formation of Aluminide Coatings on Fe-Based Alloys by Chemical Vapor Deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Ying; Pint, Bruce A; Cooley, Kevin M

2008-01-01

Aluminide and Al-containing coatings were synthesized on commercial ferritic (P91) and austenitic (304L) alloys via a laboratory chemical vapor deposition (CVD) procedure for rigorous control over coating composition, purity and microstructure. The effect of the CVD aluminizing parameters such as temperature, Al activity, and post-aluminizing anneal on coating growth was investigated. Two procedures involving different Al activities were employed with and without including Cr-Al pellets in the CVD reactor to produce coatings with suitable thickness and composition for coating performance evaluation. The phase constitution of the as-synthesized coatings was assessed with the aid of a combination of X-ray diffraction, electronmore » probe microanalysis, and existing phase diagrams. The mechanisms of formation of these CVD coatings on the Fe-based alloys are discussed, and compared with nickel aluminide coatings on Ni-base superalloys. In addition, Cr-Al pellets were replaced with Fe-Al metals in some aluminizing process runs and similar coatings were achieved.« less

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

[Effect of silicon coating on bonding strength of ceramics and titanium].

PubMed

Zhou, Shu; Wang, Yu; Zhang, Fei-Min; Guang, Han-Bing

2009-06-01

This study investigated the effect of silicon coating (SiO2) by solution-gelatin (Sol-Gel) technology on bonding strength of titanium and ceramics. Sixteen pure titanium specimens with the size of 25 mm x 3 mm x 0.5 mm were divided into two groups (n=8), test group was silicon coated by Sol-Gel technology, the other one was control group. The middle area of the samples were veneered with Vita Titankeramik system, the phase composition of two specimens were characterized by X-ray diffraction (XRD). The bonding strength of titanium/porcelain was evaluated using three-point bending test. The interface of titanium and porcelain and fractured titanium surface were investigated by scanning electron microscope (SEM) with energy depressive spectrum (EDS). Contents of surface silicon increased after modification with silicon coated by Sol-Gel technology. The mean bonding strength of test group and control group were (37.768 +/- 0.777) MPa and (29.483 +/- 1.007) MPa. There was a statistically significant difference (P=0.000) between them. The bonded ceramic boundary of test group was wider than control group. Silicon coating by Sol-Gel technology was significant in improving bonding strength of titanium/Vita Titankeramik system.

Effect of particle in-flight behavior on the composition of thermal barrier coatings

NASA Astrophysics Data System (ADS)

Zhao, L.; Bai, Y.; Tang, J. J.; Liu, K.; Ding, C. H.; Yang, J. F.; Han, Z. H.

2013-12-01

In this work, 6 to 11 mol% YO1.5-stabilized zirconia (YSZ) coatings were deposited by supersonic and conventional atmospheric plasma spraying. During spraying, the surface temperature and velocity of in-flight particles were monitored by Spray Watch 2i on-line system. The phase composition of as-sprayed coatings was analyzed by X-ray diffractometry (XRD). Lattice parameters, tetragonality and the content of YO1.5 (mol%) of as-sprayed coatings were calculated according to the position of (0 0 4) and (4 0 0) diffraction peaks. It was found that the as-sprayed coatings were composed of metastable non-transformable tetragonal phase (t‧). However, the amount of YO1.5 (mol%) in the as-sprayed coatings decreased with the increase of melting index of in-flight particles due to the partial evaporation of YO1.5 during spraying.

Anodic Oxidation of Carbon Steel at High Current Densities and Investigation of Its Corrosion Behavior

NASA Astrophysics Data System (ADS)

Fattah-Alhosseini, Arash; Khan, Hamid Yazdani

2017-06-01

This work aims at studying the influence of high current densities on the anodization of carbon steel. Anodic protective coatings were prepared on carbon steel at current densities of 100, 125, and 150 A/dm2 followed by a final heat treatment. Coatings microstructures and morphologies were analyzed using X-ray diffraction (XRD) and scanning electron microscope (SEM). The corrosion resistance of the uncoated carbon steel substrate and the anodic coatings were evaluated in 3.5 wt pct NaCl solution through electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that the anodic oxide coatings which were prepared at higher current densities had thicker coatings as a result of a higher anodic forming voltage. Therefore, the anodized coatings showed better anti-corrosion properties compared to those obtained at lower current densities and the base metal.

In vitro assessments on bacterial adhesion and corrosion performance of TiN coating on Ti6Al4V titanium alloy synthesized by multi-arc ion plating

NASA Astrophysics Data System (ADS)

Lin, Naiming; Huang, Xiaobo; Zhang, Xiangyu; Fan, Ailan; Qin, Lin; Tang, Bin

2012-07-01

TiN coating was synthesized on Ti6Al4V titanium alloy surface by multi-arc ion plating (MIP) technique. Surface morphology, cross sectional microstructure, elemental distributions and phase compositions of the obtained coating were analyzed by means of scanning electron microscope (SEM), optical microscope (OM), glow discharge optical emission spectroscope (GDOES) and X-ray diffraction (XRD). Bacterial adhesion and corrosion performance of Ti6Al4V and the TiN coating were assessed via in vitro bacterial adhesion tests and corrosion experiments, respectively. The results indicated that continuous and compact coating which was built up by pure TiN with a typical columnar crystal structure has reached a thickness of 1.5 μm. This TiN coating could significantly reduce the bacterial adhesion and enhance the corrosion resistance of Ti6Al4V substrate.

FABRICATION OF IN SITUFe-Ti-B COMPOSITE COATING BY LASER CLADDING

NASA Astrophysics Data System (ADS)

Du, Baoshuai

2013-06-01

Laser cladding was applied to deposit in situFe-Ti-B composite coatings on mild carbon steel with precursor of ferrotitanium, ferroboron and pure Fe alloy powders. The composite coatings were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and electron probe microanalysis (EPMA). Wear resistance of the laser-cladded Fe-Ti-B coatings was evaluated under dry sliding condition at room temperature using block-on-ring wear tester. Results indicate that in situ reinforcements of TiB2 and Fe2B can be synthesized in the Fe-Ti-B coatings. The amount of TiB2 increases with the increase of content of ferrotitanium and ferroboron in the precursor. Reinforcements are formed through the liquid-precipitation route following the solidification path of the Fe-Ti-B system. Hardness and wear properties of the coatings improved significantly in comparison to the as-received substrate due to the presence of hard reinforcements.

Bioactivity of calcium phosphate bioceramic coating fabricated by laser cladding

NASA Astrophysics Data System (ADS)

Zhu, Yizhi; Liu, Qibin; Xu, Peng; Li, Long; Jiang, Haibing; Bai, Yang

2016-05-01

There were always strong expectations for suitable biomaterials used for bone regeneration. In this study, to improve the biocompatiblity of titanium alloy, calcium phosphate bioceramic coating was obtained by laser cladding technology. The microstructure, phases, bioactivity, cell differentiation, morphology and resorption lacunae were investigated by optical microscope (OM), x-ray diffraction (XRD), methyl thiazolyl tetrazolium (MTT) assay, tartrate-resistant acid phosphatase (TRAP) staining and scanning electronic microscope (SEM), respectively. The results show that bioceramic coating consists of three layers, which are a substrate, an alloyed layer and a ceramic layer. Bioactive phases of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) were found in ceramic coating. Osteoclast precursors have excellent proliferation on the bioceramic surface. The bioceramics coating could be digested by osteoclasts, which led to the resorption lacunae formed on its surface. It revealed that the gradient bioceramic coating has an excellent bioactivity.

Glass frits coated with silver nanoparticles for silicon solar cells

NASA Astrophysics Data System (ADS)

Li, Yingfen; Gan, Weiping; Zhou, Jian; Li, Biyuan

2015-06-01

Glass frits coated with silver nanoparticles were prepared by electroless plating. Gum Arabic (GA) was used as the activating agent of glass frits without the assistance of stannous chloride or palladium chloride. The silver-coated glass frits prepared with different GA dosages were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and thermogravimetric analysis (TGA). The characterization results indicated that silver-coated glass frits had the structures of both glass and silver. Spherical silver nanoparticles were distributed on the glass frits evenly. The density and particle size of silver nanoparticles on the glass frits can be controlled by adjusting the GA dosage. The silver-coated glass frits were applied to silver pastes to act as both the densification promoter and silver crystallite formation aid in the silver electrodes. The prepared silver-coated glass frits can improve the photovoltaic performances of solar cells.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Spectroscopic evidence for uranium bearing precipitates in vadose zone sediments at the Hanford 300-area site

USGS Publications Warehouse

Arai, Y.; Marcus, M.A.; Tamura, N.; Davis, J.A.; Zachara, J.M.

2007-01-01

Uranium (U) solid-state speciation in vadose zone sediments collected beneath the former North Process Pond (NPP) in the 300 Area of the Hanford site (Washington) was investigated using multi-scale techniques. In 30 day batch experiments, only a small fraction of total U (???7.4%) was released to artificial groundwater solutions equilibrated with 1% pCO2. Synchrotron-based micro-X-ray fluorescence spectroscopy analyses showed that U was distributed among at least two types of species: (i) U discrete grains associated with Cu and (ii) areas with intermediate U concentrations on grains and grain coatings. Metatorbernite (Cu[UO2]2[PO 4]2??8H2O) and uranophane (Ca[UO 2]2[SiO3(OH)]2?? 5H 2O) at some U discrete grains, and muscovite at U intermediate concentration areas, were identified in synchrotron-based micro-X-ray diffraction. Scanning electron microscopy/energy dispersive X-ray analyses revealed 8-10 ??m size metatorbernite particles that were embedded in C-, Al-, and Si-rich coatings on quartz and albite grains. In ??- and bulk-X-ray absorption structure (??-XAS and XAS) spectroscopy analyses, the structure of metatorbernite with additional U-C and U-U coordination environments was consistently observed at U discrete grains with high U concentrations. The consistency of the ??- and bulk-XAS analyses suggests that metatorbernite may comprise a significant fraction of the total U in the sample. The entrapped, micrometer-sized metatorbernite particles in C-, Al-, and Si-rich coatings, along with the more soluble precipitated uranyl carbonates and uranophane, likely control the long-term release of U to water associated with the vadose zone sediments. ?? 2007 American Chemical Society.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Photoluminescent properties of spider silk coated with Eu-doped nanoceria

NASA Astrophysics Data System (ADS)

Dmitrović, Svetlana; Nikolić, Marko G.; Jelenković, Branislav; Prekajski, Marija; Rabasović, Mihailo; Zarubica, Aleksandra; Branković, Goran; Matović, Branko

2017-02-01

Spider dragline silk was coated with pure as well as Eu-doped ceria nanopowders at the room temperature. The treatment was done by immersion of the spider silk mesh into aqueous solutions of cerium nitrate (Ce(NO3)3) and ammonium hydroxide (NH4OH). Depending on the relationship between Ce3+ ion and ammonium hydroxide concentration, coated fibers exhibited a different thickness. Obtained materials were studied by means of FESEM. It was found that ceria nanoparticles of average size of 3 nm were coated along spider thread. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) confirmed crystal nature of nanoparticle coating of spider silk. By using Williamson-Hall plots, crystallite size and strain were estimated. EDS measurement confirmed the presence of Eu in spider-Eu-doped ceria composite, and according to FTIR analysis, the interaction between CeO2 and spider silk was proposed. The morphology of obtained composite was observed by TEM. The photoluminescence emission spectra of spider silk coated with Eu-doped ceria were measured with two different excitations of 385 and 466 nm. The two-photon excited auto-fluorescence of spider silk coated with Eu-doped ceria was detected using a nonlinear laser scanning microscope. Obtained composite has a potential as a fluorescent labeling material in diverse applications.

In Situ X-ray Diffraction Studies on the Mechanism of Capacity Retention Improvement by Coating at the Surface of Li CoO2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chung,K.; Yoon, W.; McBreen, J.

2007-01-01

Synchrotron based in situ X-ray diffraction technique has been used to study the mechanism of capacity fading of LiCoO2 cycled to a higher voltage above the normal 4.2 V limit and to investigate the mechanism of capacity retention improvement by ZrO2 surface coating on LiCoO2. It was found that the capacity fading of LiCoO2 cycled at higher voltage limit is closely related to the increased polarization rather than the bulk crystal structure damage. The capacity of uncoated LiCoO2 sample dropped to less than 70 mAh g-1 when charged to 4.8 V after high voltage cycling. However, when the voltage limitmore » was further increased to 8.35 V, the capacity was partially restored and the corresponding structural changes were recovered to the similar level as seen in fresh sample. This indicates that the integrity of the bulk crystal structure of LiCoO2 was not seriously damaged during cycling to 4.8 V. The increased polarization seems to be responsible for the fading capacity and the uncompleted phase transformation of LiCoO2. The polarization-induced capacity fading can be significantly improved by ZrO2 surface coating. It was proposed that the effect of ZrO2-coating layer on the capacity retention during high voltage cycling is through the formation of protection layer on the surface of LiCoO2 particles, which can reduce the decomposition of the electrolyte at higher voltages.« less

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Real-time imaging, spectroscopy, and structural investigation of cathodic plasma electrolytic oxidation of molybdenum

NASA Astrophysics Data System (ADS)

Stojadinović, Stevan; Tadić, Nenad; Šišović, Nikola M.; Vasilić, Rastko

2015-06-01

In this paper, the results of the investigation of cathodic plasma electrolytic oxidation (CPEO) of molybdenum at 160 V in a mixed solution of borax, water, and ethylene glycol are presented. Real-time imaging and optical emission spectroscopy were used for the characterization of the CPEO. During the process, vapor envelope is formed around the cathode and strong electric field within the envelope caused the generation of plasma discharges. The spectral line shape analysis of hydrogen Balmer line Hβ (486.13 nm) shows that plasma discharges are characterized by the electron number density of about 1.4 × 1021 m-3. The electron temperature of 15 000 K was estimated by measuring molybdenum atomic lines intensity. Surface morphology, chemical, and phase composition of coatings formed by CPEO were characterized by scanning electron microscopy with energy dispersive x-ray spectroscopy and x-ray diffraction. The elemental components of CPEO coatings are Mo and O and the predominant crystalline form is MoO3.

Antioxidation performance of poly(vinyl alcohol) modified poly(vinylidene fluoride) membranes

NASA Astrophysics Data System (ADS)

Wang, Daohui; Li, Xianfeng; Li, Qing; Liu, Zhen; Li, Nana; Huang, Qinglin; Zhang, Yufeng; Xiao, Changfa

2018-03-01

Commercial poly(vinylidene fluoride) (PVDF) membranes were modified by dip-coating and crosslinking hydrophilic poly(vinyl alcohol) (PVA) on the membrane surface. The antioxidation performance of the modified PVDF membranes was evaluated via exposing the modified membranes to sodium hypochlorite and potassium permanganate solutions for 5-30 days, respectively. The evaluation was based on the influences of the two oxidants on the permeability, rejection, and hydrophility of the modified membranes, which were characterized by water flux, ink rejection, water contact angle, x-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy, and x-ray diffraction (XRD) measurements. The XPS and water contact angle results show that the hydrophilicity of PVDF membranes was significantly improved when PVA was crosslinked on the surface of PVDF membranes. When the modified membranes had been treated with sodium hypochlorite or potassium permanganate for 30 days, the permeability and hydrophilicity were basically maintained and the rejection was slightly decreased. XPS and XRD indicated that some of PVAs coated on the membrane surface could be oxidized and peeled.

Effect of Ar{sup +} ion irradiation on the microstructure of pyrolytic carbon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, Shanglei; Zhang, Dongsheng; Yang, Xinmei

2015-03-21

Pyrolytic carbon (PyC) coatings prepared by chemical vapor deposition were irradiated by 300 keV Ar{sup +} ions. Then, atomic force microscopy, synchrotron-based grazing incidence X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy, and transmission electron microscopy were employed to study how Ar{sup +} irradiation affects the microstructure of PyC, including the microstructural damage mechanisms and physics driving these phenomena. The 300 keV Ar{sup +} ion irradiation deteriorated the structure along the c-axis, which increased the interlayer spacing between graphene layers. With increasing irradiation dose, the density of defect states on the surface of PyC coating increases, and the basal planes gradually loses theirmore » initial ordering resulting in breaks in the lattice and turbulence at the peak damage dose reaches 1.58 displacement per atom (dpa). Surprisingly, the PyC becomes more textured as it becomes richer in structural defects with increasing irradiation dose.« less

Design of Inorganic Water Repellent Coatings for Thermal Protection Insulation on an Aerospace Vehicle

NASA Technical Reports Server (NTRS)

Fuerstenau, D. W.; Ravikumar, R.

1997-01-01

In this report, thin film deposition of one of the model candidate materials for use as water repellent coating on the thermal protection systems (TPS) of an aerospace vehicle was investigated. The material tested was boron nitride (BN), the water-repellent properties of which was detailed in our other investigation. Two different methods, chemical vapor deposition (CVD) and pulsed laser deposition (PLD), were used to prepare the BN films on a fused quartz substrate (one of the components of thermal protection systems on aerospace vehicles). The deposited films were characterized by a variety of techniques including X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The BN films were observed to be amorphous in nature, and a CVD-deposited film yielded a contact angle of 60 degrees with water, similar to the pellet BN samples investigated previously. This demonstrates that it is possible to use the bulk sample wetting properties as a guideline to determine the candidate waterproofing material for the TPS.

Potentiodynamic studies of Ni-P-TiO2 nano-composited coating on the mild steel deposited by electroless plating method

NASA Astrophysics Data System (ADS)

Uttam, Vibha; Duchaniya, R. K.

2016-05-01

Now a days, corrosion studies are important for reducing the wastage of metals. The importance of corrosion studies is two folds i.e. first is economic, including the reduction of material losses resulting from the wasting away or sudden failure of materials and second is conservation Electroless process is an autocatalytic reduction method in which metallic ions are reduced in the solution. Nanocomposite coatings of Ni-P-TiO2 on mild steel are deposited by varying volume of TiO2 nano-powder by electroless method from Ni-P plating bath containing Nickel Sulphate as a source of nickel ions, sodium hypophosphite as the reducing agent, lactic acid as a complexing agents and TiO2 nano powder. Electroless Ni-P-TiO2 coating have been widely used in the chemical process industries, mechanical industries, electronic industries and chloroalkali industries due to their excellent corrosion with mechanical properties. In the present work, deposition of Ni-P alloy coating and Ni-P-TiO2 nanocomposited coatings were done on the mild steel and corrosion properties were studied with Potentio-dynamic polarization measurements method in 3.5 wt% sodium chloride solution. It showed in the experiments that Ni-P-TiO2 nanocomposited coating has better corrosion resistance as comparedthan Ni-P alloy coating. Morphological studies were done by field emission scanning electron microscopy (FESEM), energy-dispersive analysis of X-ray (EDAX) and X-ray diffraction (XRD). These studies confirmed the deposition of Ni-P alloy coating and Ni-P-TiO2 nanocomposited coating.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Bakhshi, Hamed; Shokuhfar, Ali; Vahdati, Nima

2016-09-01

Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C2H2) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C2H2 ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples' magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Fabrication, characterization and gas sensing studies of PPy/MWCNT/SLS nanocomposite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tiwari, D. C., E-mail: dctiwari2001@yahoo.com; Atri, Priyanka, E-mail: dctiwari2001@yahoo.com; Sharma, R.

2014-04-24

Multiwall carbon nanotubes (MWCNT) coated with polypyrrole nanocomposite was prepared by in-situ chemical oxidative polymerization method in the presence of surfactant (SLS). The scanning electron microscope (SEM) pictures indicate the core shell structure of PPy/MWCNT/SLS nanocomposite. Nature of the prepared material was investigated by X-ray diffraction spectroscopy. This nanocomposite shows the excellent gas sensing behaviour for ammonia gas at 150 ppm and 300 ppm levels.

Magnesium Nanoparticles for Hydrogen Storage: Structure, Kinetics and Thermodynamics

NASA Astrophysics Data System (ADS)

Pasquini, L.; Brighi, M.; Montone, A.; Vittori Antisari, M.; Dam, B.; Palmisano, V.; Bonetti, E.

2012-08-01

Magnesium nanoparticles coated by a native oxide shell and decorated by palladium clusters were synthesized by the inert gas condensation technique. The kinetics and thermodynamics of hydrogen sorption were investigated by Sieverts measurements at high temperature and by optical hydrogenography close to ambient temperature. The structure and morphology of the nanoparticles were studied by electron microscopy and X-ray diffraction both in the as-prepared state and after hydrogen sorption cycles.

Plasma Sprayed Hydroxyapatite Coatings: Influence of Spraying Power on Microstructure

NASA Astrophysics Data System (ADS)

Mohd, S. M.; Abd, M. Z.; Abd, A. N.

2010-03-01

The plasma sprayed hydroxyapatite (HA) coatings are used on metallic implants to enhance the bonding between the implant and bone in human body. The coating process was implemented at different spraying power for each spraying condition. The coatings formed from a rapid solidification of molten and partly molten particles that impact on the surface of substrate at high velocity and high temperature. The study was concentrated on different spraying power that is between 23 to 31 kW. The effect of different power on the coatings microstructure was investigated using scanning electron microscope (SEM) and phase composition was evaluated using X-ray diffraction (XRD) analysis. The coatings surface morphology showed distribution of molten, partially melted particles and some micro-cracks. The produced coatings were found to be porous as observed from the cross-sectional morphology. The coatings XRD results indicated the presence of crystalline phase of HA and each of the patterns was similar to the initial powder. Regardless of different spraying power, all the coatings were having similar XRD patterns.

Low Conductive Thermal Barrier Coatings Produced by Ion Beam Assisted EB-PVD with Controlled Porosity, Microstructure Refinement and Alloying Additions for High Temperature Applications

NASA Technical Reports Server (NTRS)

Wolfe, Douglas E.; Singh, Jogender

2005-01-01

Various advanced Hafnia-based thermal barrier coatings (TBC) were applied on nickel-based superalloy coupons by electron beam physical vapor deposition. In addition, microstructural modifications to the coating material were made in an effort to reduce the thermal conductivity of the coating materials. Various processing parameters and coating system modifications were made in order to deposit the alloyed TBC with the desired microstructure and thus coating performance, some of which include applying coatings at substrate temperatures of 1150 C on both PtAl and CoNiCrAlY bond coated samples, as well as using 8YSZ as a bond layer. In addition, various characterization techniques including thermal cyclic tests, scanning electron microscopy, x-ray diffraction, thermal conductivity, and reflectivity measurements were performed. Although the coating microstructure was never fully optimized due to funding being cut short, significant reductions in thermal conductivity were accomplished through both chemistry changes (composition) and microstructural modifications.

X-ray mirror development and testing for the ATHENA mission

NASA Astrophysics Data System (ADS)

Della Monica Ferreira, Desiree; Jakobsen, Anders C.; Massahi, Sonny; Christensen, Finn E.; Shortt, Brian; Garnæs, Jørgen; Torras-Rosell, Antoni; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie

2016-07-01

This study reports development and testing of coatings on silicon pore optics (SPO) substrates including pre and post coating characterisation of the x-ray mirrors using Atomic Force Microscopy (AFM) and X-ray reflectometry (XRR) performed at the 8 keV X-ray facility at DTU Space and with synchrotron radiation in the laboratory of PTB at BESSY II. We report our findings on surface roughness and coating reflectivity of Ir/B4C coatings considering the grazing incidence angles and energies of ATHENA and long term stability of Ir/B4C, Pt/B4C, W/Si and W/B4C coatings.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

The Bioactivity and Photocatalytic Properties of Titania Nanotube Coatings Produced with the Use of the Low-Potential Anodization of Ti6Al4V Alloy Surface

PubMed Central

Radtke, Aleksandra; Kozak, Wiesław; Sadowska, Beata; Więckowska-Szakiel, Marzena; Szubka, Magdalena; Talik, Ewa; Pleth Nielsen, Lars; Piszczek, Piotr

2017-01-01

Titania nanotube (TNT) coatings were produced using low-potential anodic oxidation of Ti6Al4V substrates in the potential range 3–20 V. They were analysed by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The wettability was estimated by measuring the contact angle when applying water droplets. The bioactivity of the TNT coatings was established on the basis of the biointegration assay (L929 murine fibroblasts adhesion and proliferation) and antibacterial tests against Staphylococcus aureus (ATCC 29213). The photocatalytic efficiency of the TNT films was studied by the degradation of methylene blue under UV irradiation. Among the studied coatings, the TiO2 nanotubes obtained with the use of 5 V potential (TNT5) were found to be the most appropriate for medical applications. The TNT5 sample possessed antibiofilm properties without enriching it by additional antimicrobial agent. Furthermore, it was characterized by optimal biocompatibility, performing better than pure Ti6Al4V alloy. Moreover, the same sample was the most photocatalytically active and exhibited the potential for the sterilization of implants with the use of UV light and for other environmental applications. PMID:28933732

Poly(methyl methacrylate) coating of soft magnetic amorphous and crystalline Fe,Co-B nanoparticles by chemical reduction.

PubMed

Fernández Barquín, L; Yedra Martínez, A; Rodríguez Fernández, L; Rojas, D P; Murphy, F J; Alba Venero, D; Ruiz González, L; González-Calbet, J; Fdez-Gubieda, M L; Pankhurst, Q A

2012-03-01

The structural and magnetic properties of a collection of nanoparticles coated by Poly(methyl methacrylate) through a wet chemical synthesis have been investigated. The particles display either an amorphous (M = Fe, Co) M-B arrangement or a mixed structure bcc-Fe and fcc-Co + amorphous M-B. Both show the presence of a metal oxi-hydroxide formed in aqueous reduction. The organic coating facilitates technological handling. The cost-effective synthesis involves a reduction in a Poly(methyl methacrylate) aqueous solution of iron(II) or cobalt(II) sulphates (< 0.5 M) by sodium borohydride (< 0.5 M). The particles present an oxidized component, as deduced from X-ray diffraction, Mössbauer and Fe- and Co K-edge X-ray absorption spectroscopy and electron microscopy. For the ferrous alloys, this Fe-oxide is alpha-goethite, favoured by the aqueous solution. The Poly(methyl methacrylate) coating is confirmed by Fourier transform infrared spectroscopy. In pure amorphous core alloys there is a drastic change of the coercivity from bulk to around 30 Oe in the nanoparticles. The mixed structured alloys also lie in the soft magnetic regime. Magnetisation values at room temperature range around 100 emu/g. The coercivity stems from multidomain particles and their agglomeration, triggering the dipolar interactions.

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

Nanocrystalline ferroelectric BaTiO3/Pt/fused silica for implants synthetized by pulsed laser deposition method

NASA Astrophysics Data System (ADS)

Jelínek, Miroslav; Drahokoupil, Jan; Jurek, Karel; Kocourek, Tomáš; Vaněk, Přemysl

2017-09-01

The thin-films of BaTiO3 (BTO)/Pt were prepared to test their potential as coatings for titanium-alloy implants. The nanocrystalline BTO/Pt bi-layers were successfully synthesized using fused silica as substrates. The bi-layers were prepared using KrF excimer laser ablation at substrate temperatures (Ts) ranging from 650 °C to 750 °C. The microstructure and composition of the deposits were investigated by scanning electron microscope, x-ray diffraction and wavelength dispersive x-ray spectroscopy methods. The electrical characterization of the Pt/BTO/Pt capacitors indicated ferroelectric-type response in BTO films containing (40-140) nm-sized grains. The technology, microstructure, and functional response of the layers are presented in detail.

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates.

PubMed

Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA)(2-) and (NH4)2HPO4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

Crystallographic texture in pulsed laser deposited hydroxyapatite bioceramic coatings

PubMed Central

Kim, Hyunbin; Camata, Renato P.; Lee, Sukbin; Rohrer, Gregory S.; Rollett, Anthony D.; Vohra, Yogesh K.

2008-01-01

The orientation texture of pulsed laser deposited hydroxyapatite coatings was studied by X-ray diffraction techniques. Increasing the laser energy density of the KrF excimer laser used in the deposition process from 5 to 7 J/cm2 increases the tendency for the c-axes of the hydroxyapatite grains to be aligned perpendicular to the substrate. This preferred orientation is most pronounced when the incidence direction of the plume is normal to the substrate. Orientation texture of the hydroxyapatite grains in the coatings is associated with the highly directional and energetic nature of the ablation plume. Anisotropic stresses, transport of hydroxyl groups and dehydroxylation effects during deposition all seem to play important roles in the texture development. PMID:18563207

Improvement of interfacial interactions using natural polyphenol-inspired tannic acid-coated nanoclay enhancement of soy protein isolate biofilms

NASA Astrophysics Data System (ADS)

Wang, Zhong; Kang, Haijiao; Zhang, Wei; Zhang, Shifeng; Li, Jianzhang

2017-04-01

In this study, a novel and economic surface modification technique for montmorillonite (MMT) nanosheets, a biocompatible coupling cross-linking agent, was developed on an attempt at improving the interfacial adhesion with soy protein isolate (SPI) matrix. Inspired by natural polyphenol, the "green dip-coating" method using tannic acid (TA) to surface-modify MMT (TA@MMT). SPI nanocomposite films modified with MMT or TA@MMT, as well as the control ones, were prepared via the casting method. The TA layer was successfully coated on the MMT surface through the (FeIII) ions coordination chemistry and the synthetic samples were characterized by the Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), atomic force microscopy (AFM), and transmission electron microscopy (TEM). The compatibility and interfacial interactions between modified MMT and SPI matrix were greatly enhanced by the TA-FeIII coating on the MMT surface. The mechanical properties, water resistance, and thermal stability of the resultant biofilm were increased accordingly. Compared with that of the unmodified SPI film, the tensile strength of the nanocomposite films modified by the green dip-coating was increased by 113.3%. These SPI-based nanocomposite films showed the favorable potential in terms of food packing applications due to their efficient barriers to water vapor and UV and/or visible light.

Effect of cobalt doping on the phase transformation of TiO2 nanoparticles.

PubMed

Barakat, M A; Hayes, G; Shah, S Ismat

2005-05-01

Co-doped TiO2 nanoparticles containing 0.0085, 0.017, 0.0255, 0.034, and 0.085 mol % Co(III) ion dopant were synthesized via sol-gel and dip-coating techniques. The effects of metal ion doping on the transformation of anatase to the rutile phase have been investigated. Several analytical tools, such as X-ray diffraction (XRD), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), and energy dispersive X-ray analysis (EDAX) were used to investigate the nanoparticle structure, size distribution, and composition. Results obtained revealed that the rutile to anatase concentration ratio increases with increase of the cobalt dopant concentration and annealing temperature. The typical composition of Co-doped TiO2 was Ti(1-x)Co(x)O2, where x values ranged from 0.0085 to 0.085. The activation energy for the phase transformation from anatase to rutile was measured to be 229, 222, 211, and 195 kJ/mole for 0.0085, 0.017, 0.0255, and 0.034 mol % Co in TiO2, respectively.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

A novel ion-exchange strategy for the fabrication of high strong BiOI/BiOBr heterostructure film coated metal wire mesh with tunable visible-light-driven photocatalytic reactivity.

PubMed

Wang, Yi; Long, Yang; Yang, Zhiqing; Zhang, Dun

2018-06-05

Visible-light-driven (VLD) BiOI/BiOBr heterostructure films with hierarchical microstructure have been firstly fabricated on 304 stainless steel wire mesh (304SSWM) substrates through a novel ion-exchange method using the BiOI film as precursor. The concentration of tetrabutylammonium bromide (TBAB) is the key factor to control the composition and microstructure of BiOI/BiOBr films. Physical, chemical, and optical properties of BiOI/BiOBr heterostructure films were characterized by X-ray diffraction, scanning electron microscope, energy-dispersive X-ray spectroscopy, high resolution transmittance electron microscopy, X-ray photoelectron spectroscopy, UV-vis diffuse reflectance absorption, and fluorescence spectrophotometer, respectively. The VLD photocatalytic ability of the BiOI/BiOBr heterostructure film coated 304SSWM was studied by degrading rhodamine B and pIRES2-EGFP plasmid as target water organic pollutants and pathogenic bacteria genetic materials. The BiOI/BiOBr heterostructure film coated 304SSWM fabricated with 50 mM TBAB has excellent photocatalytic activity, stability, and reusability in the cycled experiments. The reasons for these unique features can be ascribed to the formation of heterojuction structure and the open framework structure of the 304SSWM. The current work can provide new strategies to construct novel VLD photoactive functional films for water purification and disinfection. Copyright © 2018 Elsevier B.V. All rights reserved.

The formation of tungsten doped Al2O3/ZnO coatings on aluminum by plasma electrolytic oxidation and their application in photocatalysis

NASA Astrophysics Data System (ADS)

Stojadinović, Stevan; Vasilić, Rastko; Radić, Nenad; Tadić, Nenad; Stefanov, Plamen; Grbić, Boško

2016-07-01

Tungsten doped Al2O3/ZnO coatings are formed by plasma electrolytic oxidation of aluminum substrate in supporting electrolyte (0.1 M boric acid + 0.05 M borax + 2 g/L ZnO) with addition of different concentrations of Na2WO4·2H2O. The morphology, crystal structure, chemical composition, and light absorption characteristics of formed surface coatings are investigated. The X-ray diffraction and X-ray photoelectron spectroscopy results indicate that formed surface coatings consist of alpha and gamma phase of Al2O3, ZnO, metallic tungsten and WO3. Obtained results showed that incorporated tungsten does not have any influence on the absorption spectra of Al2O3/ZnO coatings, which showed invariable band edge at about 385 nm. The photocatalytic activity of undoped and tungsten doped Al2O3/ZnO coatings is estimated by the photodegradation of methyl orange. The photocatalytic activity of tungsten doped Al2O3/ZnO coatings is higher thanof undoped Al2O3/ZnO coatings; the best photocatalytic activity is ascribed to coatings formed in supporting electrolyte with addition of 0.3 g/L Na2WO4·2H2O. Tungsten in Al2O3/ZnO coatings acts as a charge trap, thus reducing the recombination rate of photogenerated electron-hole pairs. The results of PL measurements are in agreement with photocatalytic activity. Declining PL intensity corresponds to increasing photocatalytic activity of the coatings, indicating slower recombination of electron-hole pairs.

The effects of nanostructured hydroxyapatite coating on the biodegradation and cytocompatibility of magnesium implants.

PubMed

Iskandar, Maria Emil; Aslani, Arash; Liu, Huinan

2013-08-01

Magnesium (Mg) alloys, a novel class of degradable, metallic biomaterials, have attracted growing interest as a promising alternative for medical implant and device applications due to their advantageous mechanical and biological properties. Although its biodegradability is an attractive property, rapid degradation of Mg in the physiological environments imposes a major obstacle that limits the translation of Mg-based implants to clinical applications. Therefore, the objective of this study was to develop a nanostructured hydroxyapatite (nHA) coating on polished Mg substrates to mediate the rapid degradation of Mg while improving its integration with bone tissue for orthopedic applications. The nHA coatings were deposited on polished Mg using the patented transonic particle acceleration (Spire Biomedical) process. Surface morphology, elemental compositions, and crystal structures were characterized using scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction (XRD) analysis, respectively. The degradation of nHA-coated and non-coated Mg samples was investigated by incubating the samples in phosphate buffered saline and revised simulated body fluid, under standard cell culture conditions. Rat bone marrow stromal cells (BMSCs) were harvested and cultured with nHA-coated and non-coated Mg samples to determine cytocompatibility. The degradation results suggested that the nHA coatings decreased Mg degradation. Improved BMSC adhesion was observed on the surfaces of the nHA-coated and non-coated Mg samples, in comparison with the cells on the culture plate surrounding the Mg samples. In conclusion, nHA coatings showed promise for improving the biodegradation and cytocompatibility properties of Mg-based orthopedic implants and should be further studied. Copyright © 2013 Wiley Periodicals, Inc.

Sol-gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain.

PubMed

Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

2016-01-01

The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol-gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia-porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and P<0.001, respectively). This study showed that aluminosilicate sol-gel dip coating can be considered as a convenient, less expensive reliable method for improving the bond strength between dental Y-TZP ceramics and veneering porcelain.

Sol–gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain

PubMed Central

Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

2016-01-01

The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol–gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia–porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and P<0.001, respectively). This study showed that aluminosilicate sol–gel dip coating can be considered as a convenient, less expensive reliable method for improving the bond strength between dental Y-TZP ceramics and veneering porcelain. PMID:27478376

Surface mediated assembly of small, metastable gold nanoclusters

NASA Astrophysics Data System (ADS)

Pettibone, John M.; Osborn, William A.; Rykaczewski, Konrad; Talin, A. Alec; Bonevich, John E.; Hudgens, Jeffrey W.; Allendorf, Mark D.

2013-06-01

The unique properties of metallic nanoclusters are attractive for numerous commercial and industrial applications but are generally less stable than nanocrystals. Thus, developing methodologies for stabilizing nanoclusters and retaining their enhanced functionality is of great interest. We report the assembly of PPh3-protected Au9 clusters from a heterogeneous mixture into films consisting of sub 3 nm nanocluster assemblies. The depositing nanoclusters are metastable in solution, but the resulting nanocluster assemblies are stabilized indefinitely in air or fresh solvent. The films exhibit distinct structure from Au nanoparticles observed by X-ray diffraction, and film dissolution data support the preservation of small nanoclusters. UV-Vis spectroscopy, electrospray ionization mass spectrometry, X-ray photoelectron spectroscopy and electron microscopy are used to elucidate information regarding the nanocluster formation and assembly mechanism. Preferential deposition of nanocluster assemblies can be achieved on multiple substrates, including polymer, Cr, Si, SiO2, SiNx, and metal-organic frameworks (MOFs). Unlike other vapor phase coating processes, nanocluster assembly on the MIL-68(In) MOF crystal is capable of preferentially coating the external surface and stabilizing the crystal structure in hydrothermal conditions, which should enhance their storage, separation and delivery capabilities.The unique properties of metallic nanoclusters are attractive for numerous commercial and industrial applications but are generally less stable than nanocrystals. Thus, developing methodologies for stabilizing nanoclusters and retaining their enhanced functionality is of great interest. We report the assembly of PPh3-protected Au9 clusters from a heterogeneous mixture into films consisting of sub 3 nm nanocluster assemblies. The depositing nanoclusters are metastable in solution, but the resulting nanocluster assemblies are stabilized indefinitely in air or fresh solvent. The films exhibit distinct structure from Au nanoparticles observed by X-ray diffraction, and film dissolution data support the preservation of small nanoclusters. UV-Vis spectroscopy, electrospray ionization mass spectrometry, X-ray photoelectron spectroscopy and electron microscopy are used to elucidate information regarding the nanocluster formation and assembly mechanism. Preferential deposition of nanocluster assemblies can be achieved on multiple substrates, including polymer, Cr, Si, SiO2, SiNx, and metal-organic frameworks (MOFs). Unlike other vapor phase coating processes, nanocluster assembly on the MIL-68(In) MOF crystal is capable of preferentially coating the external surface and stabilizing the crystal structure in hydrothermal conditions, which should enhance their storage, separation and delivery capabilities. Electronic supplementary information (ESI) available: Further details on stored plating solution preparation, film characterization, solution processing, MOF crystal FIB reconstruction and stability are available. See DOI: 10.1039/c3nr01708g

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

Investigating the structure and biocompatibility of niobium and titanium oxides as coatings for orthopedic metallic implants.

PubMed

Pradhan, D; Wren, A W; Misture, S T; Mellott, N P

2016-01-01

Applying sol gel based coatings to orthopedic metallic implant materials can significantly improve their properties and lifespan in vivo. For this work, niobium (Nb2O5) and titanium (TiO2) oxides were prepared via solution processing in order to determine the effect of atomic arrangement (amorphous/crystalline) on bioactivity. Thermal evaluation on the synthesized materials identified an endotherm for Nb2O5 at 75 °C with 40% weight loss below 400 °C, and minimal weight loss between 400 and 850 °C. Regarding TiO2 an endotherm was present at 92 °C with 25% weight loss below 400 °C, and 4% between 400 and 850 °C. Phase evolution was determined using High Temperature X-ray Diffraction (HT-XRD) where amorphous-Nb2O5 (450 °C), hexagonal-Nb2O5 (525 °C), orthorhombic-Nb2O5 (650 °C), amorphous-TiO2 (275 °C) and tetragonal TiO2 (500 °C) structures were produced. Simulated body fluid (SBF) testing was conducted over 1, 7 and 30 days and resulted in positive chemical and morphological changes for crystalline Nb2O5 (525 °C) and TiO2 (500 °C) after 30 days of incubation. Rod-like CaP deposits were observed on the surfaces using Scanning Electron Microscopy (FE-SEM) and Grazing Incidence-X-ray Diffraction (GI-XRD) shows that the deposits were X-ray amorphous. Cell viability was higher with the TiO2 (122%) samples when compared to the growing cell population while Nb2O5 samples exhibited a range of viability (64-105%), partially dependent on materials atomic structure. Copyright © 2015 Elsevier B.V. All rights reserved.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Biosensing applications of titanium dioxide coated graphene modified disposable electrodes.

PubMed

Kuralay, Filiz; Tunç, Selma; Bozduman, Ferhat; Oksuz, Lutfi; Oksuz, Aysegul Uygun

2016-11-01

In the present work, preparation of titanium dioxide coated graphene (TiO2/graphene) and the use of this nanocomposite modified electrode for electrochemical biosensing applications were detailed. The nanocomposite was prepared with radio frequency (rf) rotating plasma method which serves homogeneous distribution of TiO2 onto graphene. TiO2/graphene was characterized with scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) analysis. Then, this nanocomposite was dissolved in phosphate buffer solution (pH 7.4) and modified onto disposable pencil graphite electrode (PGE) by dip coating for the investigation of the biosensing properties of the prepared electrode. TiO2/graphene modified PGE was characterized with SEM, EDS and cyclic voltammetry (CV). The sensor properties of the obtained surface were examined for DNA and DNA-drug interaction. The detection limit was calculated as 1.25mgL(-1) (n=3) for double-stranded DNA (dsDNA). RSD% was calculated as 2.4% for three successive determinations at 5mgL(-1) dsDNA concentration. Enhanced results were obtained compared to the ones obtained with graphene and unmodified (bare) electrodes. Copyright © 2016 Elsevier B.V. All rights reserved.

Copper-Zinc-Tin-Sulfur Thin Film Using Spin-Coating Technology

PubMed Central

Yeh, Min-Yen; Lei, Po-Hsun; Lin, Shao-Hsein; Yang, Chyi-Da

2016-01-01

Cu2ZnSnS4 (CZTS) thin films were deposited on glass substrates by using spin-coating and an annealing process, which can improve the crystallinity and morphology of the thin films. The grain size, optical gap, and atomic contents of copper (Cu), zinc (Zn), tin (Sn), and sulfur (S) in a CZTS thin film absorber relate to the concentrations of aqueous precursor solutions containing copper chloride (CuCl2), zinc chloride (ZnCl2), tin chloride (SnCl2), and thiourea (SC(NH2)2), whereas the electrical properties of CZTS thin films depend on the annealing temperature and the atomic content ratios of Cu/(Zn + Sn) and Zn/Sn. All of the CZTS films were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDXS), Raman spectroscopy, and Hall measurements. Furthermore, CZTS thin film was deposited on an n-type silicon substrate by using spin-coating to form an Mo/p-CZTS/n-Si/Al heterostructured solar cell. The p-CZTS/n-Si heterostructured solar cell showed a conversion efficiency of 1.13% with Voc = 520 mV, Jsc = 3.28 mA/cm2, and fill-factor (FF) = 66%. PMID:28773647

Deposition of tungsten metal by an immersion process

DOE PAGES

Small, Leo J.; Brumbach, Michael T.; Clem, Paul G.; ...

2017-03-23

A new multi-step, solution-phase method for the spontaneous deposition of tungsten from a room temperature ethereal solution is reported. This immersion process relies on the deposition of a sacrificial zinc coating which is galvanically displaced by the ether-mediated reduction of oxophilic WCl 6. Subsequent thermal treatment renders a crystalline, metallic tungsten film. The chemical evolution of the surface and formation of a complex intermediate tungsten species is characterized by X-ray diffraction, infrared spectroscopy, and X-ray photoelectron spectroscopy. Efficient metallic tungsten deposition is first characterized on a graphite substrate and then demonstrated on a functional carbon foam electrode. The resulting electrochemicalmore » performance of the modified electrode is interrogated with the canonical aqueous ferricyanide system. A tungsten-coated carbon foam electrode showed that both electrode resistance and overall electrochemical cell resistance were reduced by 50%, resulting in a concomitant decrease in redox peak separation from 1.902 V to 0.783 V. Furthermore, this process promises voltage efficiency gains in electrodes for energy storage technologies and demonstrates the viability of a new route to tungsten coating for technologies and industries where high conductivity and chemical stability are paramount.« less

Green synthesis and characterization of Carica papaya leaf extract coated silver nanoparticles through X-ray diffraction, electron microscopy and evaluation of bactericidal properties

PubMed Central

Banala, Rajkiran Reddy; Nagati, Veera Babu; Karnati, Pratap Reddy

2015-01-01

The evolution of nanotechnology and the production of nanomedicine from various sources had proven to be of intense value in the field of biomedicine. The smaller size of nanoparticles is gaining importance in research for the treatment of various diseases. Moreover the production of nanoparticles is eco-friendly and cost effective. In the present study silver nanoparticles were synthesized from Carica papaya leaf extract (CPL) and characterized for their size and shape using scanning electron microscopy and transmission electron microscopy, respectively. Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray spectroscopy (EDS/EDX) and X-ray diffraction spectroscopy (XRD) were conducted to determine the concentration of metal ions, the shape of molecules. The bactericidal activity was evaluated using Luria Bertani broth cultures and the minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) were estimated using turbidimetry. The data analysis showed size of 50–250 nm spherical shaped nanoparticles. The turbidimetry analysis showed MIC and MBC was >25 μg/mL against both Gram positive and Gram negative bacteria in Luria Bertani broth cultures. In summary the synthesized silver nanoparticles from CPL showed acceptable size and shape of nanoparticles and effective bactericidal activity. PMID:26288570

Green synthesis and characterization of Carica papaya leaf extract coated silver nanoparticles through X-ray diffraction, electron microscopy and evaluation of bactericidal properties.

PubMed

Banala, Rajkiran Reddy; Nagati, Veera Babu; Karnati, Pratap Reddy

2015-09-01

The evolution of nanotechnology and the production of nanomedicine from various sources had proven to be of intense value in the field of biomedicine. The smaller size of nanoparticles is gaining importance in research for the treatment of various diseases. Moreover the production of nanoparticles is eco-friendly and cost effective. In the present study silver nanoparticles were synthesized from Carica papaya leaf extract (CPL) and characterized for their size and shape using scanning electron microscopy and transmission electron microscopy, respectively. Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray spectroscopy (EDS/EDX) and X-ray diffraction spectroscopy (XRD) were conducted to determine the concentration of metal ions, the shape of molecules. The bactericidal activity was evaluated using Luria Bertani broth cultures and the minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) were estimated using turbidimetry. The data analysis showed size of 50-250 nm spherical shaped nanoparticles. The turbidimetry analysis showed MIC and MBC was >25 μg/mL against both Gram positive and Gram negative bacteria in Luria Bertani broth cultures. In summary the synthesized silver nanoparticles from CPL showed acceptable size and shape of nanoparticles and effective bactericidal activity.

An environment-friendly phosphate chemical conversion coating on novel Mg-9Li-7Al-1Sn and Mg-9Li-5Al-3Sn-1Zn alloys with remarkable corrosion protection

NASA Astrophysics Data System (ADS)

Maurya, Rita; Siddiqui, Abdul Rahim; Balani, Kantesh

2018-06-01

An environment-friendly phosphate chemical conversion (PCC) coating has been deposited on novel LAT971 (Mg-9 wt%Li-7 wt%Al-1 wt%Sn) and LATZ9531 (Mg-9 wt%Li-5 wt%Al-3 wt%Sn-1 wt%Zn) alloys for improving their corrosion resistance. A dense and homogeneous flower like morphology (∼30 μm thick) was observed on the PCC coated Mg-Li based alloys. The presence of calcium hydrogen phosphate hydrate, tricalcium phosphate and trimagnesium phosphate were confirmed from the X-ray diffraction and X-ray photoelectron spectroscopy analysis. A lower corrosion current density of 6.74 × 10-7 mA/cm2 and 5.39 × 10-7 mA/cm2 was obtained for PCC coated alloys in 3.5% NaCl aqueous solution than that of uncoated LAT971 (0.82 mA/cm2) and LATZ9531 (0.34 mA/cm2) alloys, respectively, which offers corrosion protection efficiency of >99%. Electrochemical impedance spectroscopy (EIS) has revealed that the inner PCC coating (at coating/substrate interface) delay the direct contact between electrolyte and substrate, which offered higher charge transfer resistance (>4 orders of magnitude) than that of uncoated alloys. Thus, the PCC coating provides an effective corrosion protection to the ultra-lightweight LAT971 and LATZ9531 alloys surface and may be helpful in proving good anchoring with the top organic coatings or paints.

Development of a magnetic system for the treatment of Helicobacter pylori infections

NASA Astrophysics Data System (ADS)

Silva, Érica L.; Carvalho, Juliana F.; Pontes, Thales R. F.; Oliveira, Elquio E.; Francelino, Bárbara L.; Medeiros, Aldo C.; do Egito, E. Sócrates T.; Araujo, José H.; Carriço, Artur S.

2009-05-01

We report a study to develop a magnetic system for local delivery of amoxicillin. Magnetite microparticles produced by coprecipitation were coated with a solution of amoxicillin and Eudragit ®S100 by spray drying. Scanning electron microscopy, optical microscopy, X-ray powder diffraction and vibrating sample magnetometry revealed that the particles were superparamagnetic, with an average diameter of 17.2 μm, and an initial susceptibility controllable by the magnetite content in the suspension feeding the sprayer. Our results suggest a possible way to treat Helicobacter pylori infections, using an oral drug delivery system, and open prospects to coat magnetic microparticles by spray drying for biomedical applications.

Single crystal growth in spin-coated films of polymorphic phthalocyanine derivative under solvent vapor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Higashi, T.; Ohmori, M.; Ramananarivo, M. F.

2015-12-01

The effects of solvent vapor on spin-coated films of a polymorphic phthalocyanine derivative were investigated. Growth of single crystal films via redissolving organic films under solvent vapor was revealed by in situ microscopic observations of the films. X-ray diffraction measurement of the films after exposing to solvent vapor revealed the phase transition of polymorphs under solvent vapor. The direction of crystal growth was clarified by measuring the crystal orientation in a grown monodomain film. The mechanism of crystal growth based on redissolving organic films under solvent vapor was discussed in terms of the different solubilities of the polymorphs.

Nanohardness and Residual Stress in TiN Coatings.

PubMed

Hernández, Luis Carlos; Ponce, Luis; Fundora, Abel; López, Enrique; Pérez, Eduardo

2011-05-17

TiN films were prepared by the Cathodic arc evaporation deposition method under different negative substrate bias. AFM image analyses show that the growth mode of biased coatings changes from 3D island to lateral when the negative bias potential is increased. Nanohardness of the thin films was measured by nanoindentation, and residual stress was determined using Grazing incidence X ray diffraction. The maximum value of residual stress is reached at -100 V substrate bias coinciding with the biggest values of adhesion and nanohardness. Nanoindentation measurement proves that the force-depth curve shifts due to residual stress. The experimental results demonstrate that nanohardness is seriously affected by the residual stress.

Highly dispersible diamond nanoparticles for pretreatment of diamond films on Si substrate

NASA Astrophysics Data System (ADS)

Zhao, Shenjie; Huang, Jian; Zhou, Xinyu; Ren, Bing; Tang, Ke; Xi, Yifan; Wang, Lin; Wang, Linjun; Lu, Yicheng

2018-03-01

High quality diamond film on Si substrate was synthesized by coating diamond nanoparticles prepared by polyglycerol grafting (ND-PG) dispersion as pre-treatment method. Transmission electron microscope indicates that ND-PG is much more dispersible than untreated nanoparticles in organic solvents. The surface morphology was characterized by scanning electron microscope while atomic force microscope was conducted to measure the surface roughness. Microstructure properties were carried out by Raman spectroscopy and X-ray diffraction. The results revealed an increase in nucleation density, an acceleration of growth rate and an improvement of film crystalline quality by using spin-coating ND-PG pretreatment.

Effect of Thickness on the Structure, Composition and Properties of Titanium Nitride Nano-Coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martinez, Gustavo; Shutthanandan, V.; Thevuthasan, Suntharampillai

2014-05-05

Titanium nitride (TiNx) coatings were grown by magnetron sputtering onto Si(1 0 0) substrates by varying time of deposition to produce coatings with variable thickness (dTiN) in the range of 20-120 nm. TiNx coatings were characterized by studying their structure, composition, and mechanical properties. Nuclear reaction analysis (NRA) combined with Rutherford backscattering spectrometry (RBS) analyses indicate that the grown coatings were stoichiometric TiN. Grazing incidence X-ray diffraction (GIXRD) measurements indicate that the texturing of TiN coatings changes as a function of dTiN. The (1 1 1) and (0 0 2) peaks appear initially; (1 1 1) becomes intense while (0more » 0 2) disappears with increasing dTiN. Dense, columnar grain structure was evident for all the coatings in electron microscopy analyses. The residual stress for TiN coatings with dTiN~120 nm was 1.07 GPa in compression while thinner samples exhibit higher values of stress.« less

Fabrication and Anti-Oxidation Ability of SiC-SiO2 Coated Carbon Fibers Using Sol-Gel Method

PubMed Central

Yang, Guangyuan; Huang, Zhixiong; Wang, Xu; Wang, Bo

2018-01-01

The paper proposed a method to improve the anti-oxidation performance of carbon fibers (CF) at high temperature environment by coating silicon dioxide (SiO2) and silicon carbide (SiC). The modified sol-gel method had been used to ensure the proper interface between fibers and coating. We used polydimethylsiloxane and ethyl orthosilicate to make stable emulsion to uniformly disperse SiC nanoparticles. The modified SiO2/SiC coating had been coated on CF successfully. Compared with the untreated CF, the coated fibers started to be oxidized around 900 °C and the residual weight was 57% at 1400 °C. The oxidation mechanism had been discussed. The structure of SiC/SiO2 coated CF had been characterized by scanning electron microscope and X-ray diffraction analysis. Thermal gravimetric analysis was used to test the anti-oxidation ability of CF with different coatings. PMID:29495499

In Situ Synthesis and Characterization of Fe-Based Metallic Glass Coatings by Electrospark Deposition Technique

NASA Astrophysics Data System (ADS)

Burkov, Alexander A.; Pyachin, S. A.; Ermakov, M. A.; Syuy, A. V.

2017-02-01

Crystalline FeWMoCrBC electrode materials were prepared by conventional powder metallurgy. Metallic glass (MG) coatings were produced by electrospark deposition onto AISI 1035 steel in argon atmosphere. X-ray diffraction and scanning electron microscopy verified the amorphous structure of the as-deposited coatings. The coatings have a thickness of about 40 microns and a uniform structure. The results of dry sliding wear tests against high-speed steel demonstrated that Fe-based MG coatings had a lower friction coefficient and more than twice the wear resistance for 20 km sliding distance with respect to AISI 1035 steel. High-temperature oxidation treatment of the metal glass coatings at 1073 K in air for 12 h revealed that the oxidation resistance of the best coating was 36 times higher than that for bare AISI 1035 steel. These findings are expected to broaden the applications of electrospark Fe-based MG as highly protective and anticorrosive coatings for mild steel.

Synthesis and characterization of in situ TiC-TiB2 composite coatings by reactive plasma spraying on a magnesium alloy

NASA Astrophysics Data System (ADS)

Zou, Binglin; Tao, Shunyan; Huang, Wenzhi; Khan, Zuhair S.; Fan, Xizhi; Gu, Lijian; Wang, Ying; Xu, Jiaying; Cai, Xiaolong; Ma, Hongmei; Cao, Xueqiang

2013-01-01

TiC-TiB2 composite coatings were successfully synthesized using the technique of reactive plasma spraying (RPS) on a magnesium alloy. Phase composition, microstructure and wear resistance of the coatings were characterized by using X-ray diffraction, scanning electron microscopy and pin-on-disk wear test, respectively. The results showed that the resultant product in the RPS coatings was composed of TiC and TiB2. Depending on the ignition of self-propagating high-temperature synthesis reaction in the agglomerate particles, the RPS coatings displayed porous and dense microstructures. The porosity of the RPS coatings, to some extent, decreased when the feed powders were plasma sprayed with Ni powders. The RPS coatings provided good wear resistance for the substrate under various loads. For high loads (e.g., ≥15 N), the wear resistance could be significantly improved by the proper addition of Ni into the RPS coatings.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mukhametkaliyev, T., E-mail: mtm91@mail.ru; Surmeneva, M., E-mail: feja-mari@yandex.ru; Surmenev, R., E-mail: rsurmenev@gmail.com

A thin film of hydroxyapatite (HA) was deposited on AZ31 and Mg-Ca alloys by using radio frequency (RF) magnetron sputtering. The thickness of the HA coating was determined to be 750 nm. The phase composition, microstructure, and surface morphology of the HA coatings were investigated using X-ray diffraction and scanning electron microscopy. In vitro degradation behaviour of the HA coated alloys was evaluated in simulated body fluid (SBF) and 3.5wt.% NaCl solution using electrochemical method. The coatings homogeneously covered the entire surface of the substrates. The coating structure corresponded to a nanostructured HA. The ultrathin coating significantly improved the degradationmore » resistance of the alloy. Nanocrystalline HA coating significantly improved the corrosion resistance of the Mg-Ca and AZ31 magnesium alloys. The polarization resistance (Rp) of the coated Mg-Ca alloy was more than two-order of magnitude higher and the corrosion current density I{sub corr} reduced by ∼ 98% as compared to the base alloy.« less

A study of degradation resistance and cytocompatibility of super-hydrophobic coating on magnesium.

PubMed

Zhang, Yufen; Feyerabend, Frank; Tang, Shawei; Hu, Jin; Lu, Xiaopeng; Blawert, Carsten; Lin, Tiegui

2017-09-01

Calcium stearate based super-hydrophobic coating was deposited on plasma electrolytic oxidation (PEO) pre-treated magnesium substrate. The pre-treated magnesium and super-hydrophobic coating covered sample were characterized by scanning electron microscopy, X-ray diffraction and electrochemical corrosion measurements. The cytocompatibility and degradation resistance of magnesium, pre-treated magnesium and super-hydrophobic coating were analysed in terms of cell adhesion and osteoblast differentiation. The results indicate that the calcium stearate top coating shows super-hydrophobicity and that the surface is composed of micro/nanostructure. The super-hydrophobic coating covered sample shows higher barrier properties compared with the PEO pre-treated magnesium and bare magnesium. Human osteoblast proliferation, but not differentiation is enhanced by the PEO coating. Contrary, the super-hydrophobic coating reduces proliferation, but enhances differentiation of osteoblast, observable by the formation of hydroxyapatite. The combination of corrosion protection and cell reaction indicates that this system could be interesting for biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Layer-by-Layer Assembly of a Self-Healing Anticorrosion Coating on Magnesium Alloys.

PubMed

Fan, Fan; Zhou, Chunyu; Wang, Xu; Szpunar, Jerzy

2015-12-16

Fabrication of self-healing anticorrosion coatings has attracted attention as it has the ability to extend the service life and prevent the substrate from corrosive attack. However, a coating system with a rapid self-healing ability and an improved corrosion resistance is rarely reported. In this work, we developed a self-healing anticorrosion coating on a magnesium alloy (AZ31). The coating comprises a cerium-based conversion layer, a graphene oxide layer, and a branched poly(ethylene imine) (PEI)/poly(acrylic acid) (PAA) multilayer. We incorporated the graphene oxide as corrosion inhibitors and used the PEI/PAA multilayers to provide the self-healing ability to the coating systems. X-ray diffraction (XRD) and Raman spectroscopy were used to characterize the composition of the multilayers, and scanning electron microscopy (SEM) was used to analyze the surface morphology. The electrochemical impedance spectroscopy (EIS) results illustrate the improved corrosion resistance of the coating. The proposed coating also has a rapid self-healing ability in the presence of water.

Effects of Voltage on Microstructure and Corrosion Resistance of Micro-arc Oxidation Ceramic Coatings Formed on KBM10 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Lu, J. P.; Cao, G. P.; Quan, G. F.; Wang, C.; Zhuang, J. J.; Song, R. G.

2018-01-01

Micro-arc oxidation (MAO) coatings on KBM10 magnesium alloy were prepared in an electrolyte system with sodium silicate, potassium hydroxide, sodium tungstate, and citric acid. The effects of voltage on the microstructure and corrosion resistance of MAO coatings were studied using stereoscopic microscopy, scanning electron microscopy, x-ray diffraction, scratch tests, potentiodynamic polarization, and electrochemical impedance spectroscopy. The results showed that the roughness of the MAO coatings, diameter, and number of pores increase with the increase in voltage. The coating formed at the voltage of 350 V exhibited the best adhesive strength when evaluated by the automatic scratch tester. The coatings were mainly composed of MgO, MgWO4, and Mg2SiO4, and the content of Mg2SiO4 increased with the increase in voltage. The corrosion resistance of MAO coatings could be improved by changing the applied voltage, and the best corrosion resistance of MAO coating was observed at the voltage of 350 V.

Growth of calcium phosphates on magnesium substrates for corrosion control in biomedical applications via immersion techniques.

PubMed

Shadanbaz, Shaylin; Walker, Jemimah; Staiger, Mark P; Dias, George J; Pietak, Alexis

2013-01-01

Magnesium (Mg) has been suggested as a revolutionary biodegradable replacement for current permanent metals used in orthopedic applications. Current investigations concentrate on the control of the corrosion rate to match bone healing. Calcium phosphate coatings have been a recent focus of these investigations through various coating protocols. Within this investigation, an in situ crystallization technique was utilized as an inexpensive and relatively simple method to produce a brushite and monetite coating on pure Mg. Coatings were characterized using energy dispersive spectroscopy, glancing angle X-ray diffraction and field emission scanning electron microscopy. Corrosion protection properties of the coatings were assessed in physiological buffers, Earles balanced salt solution, minimum essential media, and minimum essential media containing serum albumin, over a 4-week period. Using this novel coating protocol, our findings indicate brushite and monetite coated Mg to have significant corrosive protective effects when compared with its uncoated counterpart whilst maintaining high coating substrate adhesion, homogeneity, and reproducibility. Copyright © 2012 Wiley Periodicals, Inc.

The effects of plasma spray parameters and atmosphere on the properties and microstructure of WC-Co coatings

NASA Astrophysics Data System (ADS)

Ghosh, D.; Lamy, D.; Sopkow, T.; Smuga-Otto, I.

Wear- and corrosion-resistant coatings deposited by plasma spray process are increasingly used in severe environments in resource industries, such as oil and gas, oil sands, mining, pulp and paper, etc. While there is a large volume of literature in the area of plasma spray coatings, comparatively few papers deal with the co-relation between coating properties and microstructure as a function of plasma spray processing parameters. In this study, the effect of some plasma spray processing variables and atmosphere (air or inert gas) on the microstructure and the properties of WC-Co coatings were studied. The properties of the coatings measured include: microhardness, porosity by image analysis, wear resistance by dry sand/rubber wheel abrasion test (ASTM G 65-91) and corrosion properties by AC impedance technique. Phase analyses of the coatings were also performed by X-ray diffraction. From the above, optimized coatings were developed for oil and gas industry applications.

Two temperature approach to femtosecond laser oxidation of molybdenum and morphological study

NASA Astrophysics Data System (ADS)

Kotsedi, L.; Kaviyarasu, K.; Fuku, X. G.; Eaton, S. M.; Amara, E. H.; Bireche, F.; Ramponi, R.; Maaza, M.

2017-11-01

The two-temperature model was used to gain insight into the thermal evolution of the hot electrons and the crystal lattice of the molybdenum thin coating during femtosecond laser treatment. The heat from the laser raised the bulk temperature of the sample through heat transfer from the hot electron to the crystal lattice of the material, which then led to the melting of the top layer of the film. This process resulted in the hot melt reacting ambient oxygen, which in turn oxidized the surface of molybdenum coating. The topological study and morphology of the oxidized film was conducted using high-resolution scanning electron microscope, with micrographs taken in both the cross-sectional geometry and normal incidence to the electron beam. The molybdenum oxide nanorods were clearly observed and the x-ray diffraction patterns showed the diffraction peaks due to molybdenum oxide.

Measurements and Diagnostics of Diamond Films and Coatings

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Wu, Richard L. C.

1999-01-01

The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abd El-Lateef, Hany M., E-mail: Hany_shubra@yahoo.co.uk; Khalaf, Mai M., E-mail: Mai_kha1@yahoo.com

This work reports the achievement of preparing of x% zirconia (ZrO{sub 2})–titania (TiO{sub 2}) composite coatings with different ZrO{sub 2} percent on the carbon steel by dipping substrates in sol–gel solutions. The prepared coated samples were investigated by various surface techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDAX). Open-circuit potential (OCP), potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS) methods were employed to investigate the corrosion resistance of the coated carbon steel substrates in 1.0 M HCl solution at 50 °C. The data showed that, the corrosion protection property ismore » not always proportional to the percent of ZrO{sub 2}. It can be inferred that there is an optimum percent (10%ZrO{sub 2}) for beneficial effects of loading ZrO{sub 2} on the protection efficiency (98.70%), while higher loading percent of ZrO{sub 2} in the sol–gel coating leads to the formation of a fragile film with poor barrier properties. EDAX/SEM suggests that the metal surface was protected through coating with ZrO{sub 2}–TiO{sub 2} composite films. - Highlights: • Sol–gel TiO{sub 2} doped with ZrO{sub 2} films deposited on carbon steel substrate • XRD measurements of x wt.% ZrO{sub 2}–TiO{sub 2} showed the (101) peaks broader than that of TiO{sub 2}. • SEM results proved that, the cracking decreases with the number of layers. • The prepared films can improve the corrosion resistance of the carbon steel substrate. • 10%ZrO{sub 2} loading is the optimal percent for useful effects on the corrosion resistance.« less

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Water-repellent coatings prepared by modification of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Chakradhar, R. P. S.; Dinesh Kumar, V.

Superhydrophobic coatings with a static water contact angle (WCA) > 150° were prepared by modifying ZnO nanoparticles with stearic acid (ZnO@SA). ZnO nanoparticles of size ˜14 nm were prepared by solution combustion method. X-ray diffraction (XRD) studies reveal that as prepared ZnO has hexagonal wurtzite structure whereas the modified coatings convert to zinc stearate. Field emission scanning electron micrographs (FE-SEM) show the dual morphology of the coatings exhibiting both particles and flakes. The flakes are highly fluffy in nature with voids and nanopores. Fourier transformed infrared (FTIR) spectrum shows the stearate ion co-ordinates with Zn2+ in the bidentate form. The surface properties such as surface free energy (γp) and work of adhesion (W) of the unmodified and modified ZnO coatings have been evaluated. The electron paramagnetic resonance (EPR) spectroscopy reveals that surface defects play a major role in the wetting behavior.

In Vitro Analysis of Electrophoretic Deposited Fluoridated Hydroxyapatite Coating on Micro-arc Oxidized AZ91 Magnesium Alloy for Biomaterials Applications

NASA Astrophysics Data System (ADS)

Razavi, Mehdi; Fathi, Mohammadhossein; Savabi, Omid; Vashaee, Daryoosh; Tayebi, Lobat

2015-03-01

Magnesium (Mg) alloys have been recently introduced as a biodegradable implant for orthopedic applications. However, their fast corrosion, low bioactivity, and mechanical integrity have limited their clinical applications. The main aim of this research was to improve such properties of the AZ91 Mg alloy through surface modifications. For this purpose, nanostructured fluoridated hydroxyapatite (FHA) was coated on AZ91 Mg alloy by micro-arc oxidation and electrophoretic deposition method. The coated alloy was characterized through scanning electron microscopy, transmission electron microscopy, X-ray diffraction, in vitro corrosion tests, mechanical tests, and cytocompatibility evaluation. The results confirmed the improvement of the corrosion resistance, in vitro bioactivity, mechanical integrity, and the cytocompatibility of the coated Mg alloy. Therefore, the nanostructured FHA coating can offer a promising way to improve the properties of the Mg alloy for orthopedic applications.

High Corrosion Resistance Offered by Multi-Walled Carbon Nanotubes Directly Grown Over Mild Steel Substrate

NASA Astrophysics Data System (ADS)

Arora, Sweety; Rekha, M. Y.; Gupta, Abhay; Srivastava, Chandan

2018-02-01

The inert and hydrophobic nature of carbon nanotubes (CNTs) makes them a potential material for corrosion protection coatings. In this work, a uniform coating of multi-walled CNTs (MWCNTs) was formed over a mild steel substrate by direct decomposition of a ferrocene-benzene mixture over the substrate which was kept inside a chemical vapor deposition setup at a temperature of 800°C. The MWCNTs formed over the substrate were characterized using x-ray diffraction, Raman spectroscopy and transmission electron microscopy techniques. Corrosion behavior of the bare and MWCNT-coated mild steel substrate was examined through potentiodynamic polarization and electrochemical impedance spectroscopy methods. A significant improvement in the corrosion resistance in terms of the reduction in corrosion current and corrosion rate and increase in polarization resistance was noted in the case of the MWCNT-coated mild steel plate. Corrosion resistance increased due to MWCNT coating.

Antibacterial property of fabrics coated by magnesium-based brucites

NASA Astrophysics Data System (ADS)

Wang, Ying; Sha, Lin; Zhao, Jiao; Li, Qian; Zhu, Yimin; Wang, Ninghui

2017-04-01

A kind of environmental-friendly magnesium-based antibacterial agent was reported for the first time, which was composited by brucites with different particle sizes. The antibacterial fabrics were produced by coating the magnesium-based antibacterial agents on the 260T polyester pongee fabrics with waterborne polyurethane. The coating process was simple, low-cost, and harmless to human health and environment. Characteristics of the antibacterial agents and fabrics were studied by particulate size distribution analyzer (PSDA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The results demonstrated that the coating layer was covered tightly on the fabrics and compositing of different particles by a certain proportion made full filling of the coating layer. Meanwhile, compositing did not change the structure of brucites. The antibacterial fabrics presented strong antibacterial properties against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus), with the reduction percentage of 96.6% and 100%, respectively, and the antibacterial fabrics attained excellent washing durability.

Synthesis and Microstructure Evolution of Nano-Titania Doped Silicon Coatings

NASA Astrophysics Data System (ADS)

Moroz, N. A.; Umapathy, H.; Mohanty, P.

2010-01-01

The Anatase phase of Titania (TiO2) in nanocrystalline form is a well known photocatalyst. Photocatalysts are commercially used to accelerate photoreactions and increase photovoltaic efficiency such as in solar cells. This study investigates the in-flight synthesis of Titania and its doping into a Silicon matrix resulting in a catalyst-dispersed coating. A liquid precursor of Titanium Isopropoxide and ethanol was coaxially fed into the plasma gun to form Titania nanoparticles, while Silicon powder was externally injected downstream. Coatings of 75-150 μm thick were deposited onto flat coupons. Further, Silicon powder was alloyed with aluminum to promote crystallization and reduce the amorphous phase in the Silicon matrix. Dense coatings containing nano-Titania particles were observed under electron microscope. X-ray diffraction showed that both the Rutile and Anatase phases of the Titania exist. The influence of process parameters and aluminum alloying on the microstructure evolution of the doped coatings is analyzed and presented.

In situ synthesis of hydroxyapatite coating by laser cladding.

PubMed

Wang, D G; Chen, C Z; Ma, J; Zhang, G

2008-10-15

HA bioceramic coatings were synthesized on titanium substrate by laser cladding using cheap calcium carbonate and calcium hydrogen phosphate. The thermodynamic condition for synthesizing HA was calculated by software Matlab 5.0, the microstructure and phase analysis of laser clad HA bioceramic coatings were studied by electron probe microanalyser (EPMA), X-ray diffractometer (XRD) and transmission electron microscopy (TEM). The theoretical results show that the Gibbs free enthalpy for the synthesis of HA phase is satisfied, and the presence of HA phase in the clad coatings was then further verified by XRD and the selected area diffraction patterns. When the laser power is 600W and the scanning speed is 3.5mm/s, the compact HA bioceramic coatings were obtained, which have cellular dendritic structure and consist of the phases of HA, alpha-Ca(2)P(2)O(7), CaO and CaTiO(3).

Mechanical and tribological properties of crystalline aluminum nitride coatings deposited on stainless steel by magnetron sputtering

NASA Astrophysics Data System (ADS)

Choudhary, R. K.; Mishra, S. C.; Mishra, P.; Limaye, P. K.; Singh, K.

2015-11-01

Aluminum nitride (AlN) coating is a potential candidate for addressing the problems of MHD pressure drop, tritium permeation and liquid metal corrosion of the test blanket module of fusion reactor. In this work, AlN coatings were grown on stainless steel by magnetron sputtering. Grazing incidence X-ray diffraction measurement revealed that formation of mixed phase (wurtzite and rock salt) AlN was favored at low discharge power and substrate negative biasing. However, at sufficiently high discharge power and substrate bias, (100) oriented wurtzite AlN was obtained. Secondary ion mass spectroscopy showed presence of oxygen in the coatings. The highest value of hardness and Young's modulus were 14.1 GPa and 215 GPa, respectively. Scratch test showed adhesive failure at a load of about 20 N. Wear test showed improved wear resistance of the coatings obtained at higher substrate bias.

Construction of a novel pH-sensitive drug release system from mesoporous silica tablets coated with Eudragit

NASA Astrophysics Data System (ADS)

Xu, Yingpu; Qu, Fengyu; Wang, Yu; Lin, Huiming; Wu, Xiang; Jin, Yingxue

2011-03-01

A novel pH-sensitive drug release system has been established by coating Eudragit (Eud) on drug-loaded mesoporous silica (MS) tablets. The release rate of ibuprofen (IBU) from the MS was retarded by coating with Eudragit S-100, and the higher retardation was due to the increase of coating concentration and the coating layers. The target position of the release depended on the pH of the release medium, which was confirmed by the drug release from IBU/MS/Eud increasing rapidly with the change of medium pH from 1.2 to 7.4. This drug delivery system could prohibit irritant drug from leaking in the stomach and make it only release in the intestine. The loaded and unloaded drug samples were characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), N 2 adsorption/desorption, scanning electron microscopy (SEM), and transmission electron microscopy (TEM).

Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

NASA Astrophysics Data System (ADS)

Li, Qianqian; Yan, Yuheng; Yu, Miao; Song, Botao; Shi, Suqing; Gong, Yongkuan

2016-03-01

A fluorinated polymeric sol-gel precursor (PFT) is synthesized by copolymerization of 2,3,4,5,5,5-hexafluoro-2,4-bis(trifluorinated methyl)pentyl methacrylate (FMA) and 3-methacryloxypropyltrimethoxysilane (TSMA) to replace the expensive long chain fluorinated alkylsilanes. The fluorinated silica sol is prepared by introducing PFT as co-precursor of tetraethyl orthosilicate (TEOS) in the sol-gel process with ammonium hydroxide as catalyst, which is then used to fabricate superhydrophobic coating on glass substrate through a simple dip-coating method. The effects of PFT concentrations on the chemical structure of the formed fluorinated silica, the surface chemical composition, surface morphology, wetting and self-cleaning properties of the resultant fluorinated silica coatings were studied by using X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrophotometer (XPS), scanning electron microscopy (SEM) and water contact angle measurements (WCA). The results show that the fluorinated silica sols are successfully obtained. The size and size distribution of the fluorinated silica particles are found greatly dependent on the concentration of PFT, which play a crucial role in the surface morphology of the corresponding fluorinated silica coatings. The suitable PFT concentration added in the sol-gel stage, i.e. for F-sol-1 and F-sol-2, is helpful to achieve both the low surface energy and multi-scaled microstructures, leading to the formation of the superhydrophobic coatings with bio-mimicking self-cleaning property similar to lotus leaves.

Fabrication and Characterization of Conductive Conjugated Polymer-Coated Antheraea mylitta Silk Fibroin Fibers for Biomedical Applications.

PubMed

Gh, Darshan; Kong, Dexu; Gautrot, Julien; Vootla, Shyam Kumar

2017-07-01

Conductive polymers are interesting materials for a number of biological and medical applications requiring electrical stimulation of cells or tissues. Highly conductive polymers (polypyrrole and polyaniline)/Antheraea mylitta silk fibroin coated fibers are fabricated successfully by in situ polymerization without any modification of the native silk fibroin. Coated fibers characterized by scanning electron microscopy confirm the silk fiber surface is covered by conductive polymers. Thermogravimetric analysis reveals preserved thermal stability of silk fiber after coating process. X-ray diffraction of degummed fiber diffraction peaks at around 2θ = 20.4 and 16.5 confirms the preservation of the β-sheet structure typical of degummed silk II fibers. This phenomenon implies that both polypyrrole and polyaniline chains form interactions with peptide linkages in degummed fiber macromolecules, without significantly disrupting protein assembly. Fourier transform infrared spectroscopy of coated fibers indicates hydrogen bonding and electrostatic interactions exist between silk fibroin macromolecules and conductive polymers. Resulting fibers display good conductive properties compared to corresponding conjugated polymers. In vitro analysis (live/dead assay) of the behavior of human immortalized keratinocytes (HaCaTs) on coated fibers demonstrates improved cell-adhesive properties and viability after polymers coating. Hence, polypyrrole- and polyaniline-coated A. mylitta silk fibers are suitable for application in cell culture and for tissue engineering, where electrical conduction properties are required. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

Antimicrobial and biocorrosion-resistant MoO3-SiO2 nanocomposite coating prepared by double cathode glow discharge technique

NASA Astrophysics Data System (ADS)

Xu, Jiang; Sun, Teng Teng; Jiang, Shuyun; Munroe, Paul; Xie, Zong-Han

2018-07-01

In this investigation, a MoO3-SiO2 nanocomposite coating was developed on a 316L stainless steel (SS) substrate by double-cathode glow discharge deposition. Chemical valence states, phase composition and microstructure features of the nanocomposite coating were studied using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It was found that the nanocomposite coating was composed of a mixture of crystalline MoO3 and amorphous phases, in which amorphous SiO2 phase was embedded between the hexagonal-structured MoO3 grains with an average grain size of ∼8.4 nm. Nanoindentation and scratch tests, together with SEM and TEM observation of locally deformed regions, indicated that the nanocomposite coating exhibited high load-bearing capacity due to a combination of high hardness and good adhesion. Contact angle measurements suggested that the nanocomposite coating was more hydrophobic than uncoated 316L SS. The anti-bacterial activity of the MoO3-SiO2 nanocomposite coating against two bacterial strains (E. coli and S. aureus) was determined by the spread plate method. This showed that both bacterial strains exposed to the coating suffered a significant loss of viability. The influences of sulfate-reducing bacteria (SRB) on the electrochemical behavior of the MoO3-SiO2 nanocomposite coating in modified Postgate's C seawater (PCS) medium were investigated through potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The electrochemical tests revealed that the coating had a greater resistance to microbiologically influenced corrosion induced by SRB than uncoated 316L SS. This was corroborated by electrochemical testing (potentiodynamic polarization and EIS), in conjunction with SEM observations of the corroded surfaces.

Parametric Study of Slurry-Erosion of Hydroturbine Steels with and without Detonation Gun Spray Coatings using Taguchi Technique

NASA Astrophysics Data System (ADS)

Grewal, Harpreet Singh; Bhandari, Sanjeev; Singh, Harpreet

2012-09-01

WC-Co-Cr coatings were deposited on some hydroturbine 13Cr4Ni and 16Cr5Ni steels by the detonation-gun spray process. An in-depth characterization of the as-sprayed coating was done using X-ray diffraction (XRD) and scanning electron microscopy (SEM)/energy-dispersive X-ray spectroscopy (EDS) techniques. Microhardness and porosity measurements were also made. The coating was found to have a typical splat-like morphology with some indications of unmelted carbide particles. The XRD results showed the presence of WC as the primary phase along with W2C and Co6W6C as secondary phases. Furthermore, the slurry erosion behavior of the coatings was investigated to ascertain the usefulness of the coatings to reduce the slurry erosion of the steels. The effect of four operating factors viz. the velocity, impact angle, concentration, and particle size on the slurry erosion of coated and bare steels has been studied using a high-speed jet-type test rig. The sand used as an erodent was collected from a power plant to replicate the actual turbine conditions. It has been observed that the given cermet coating can enhance the erosion resistance of the steel. Velocity was found to be the most significant factor affecting the erosion behavior of the coating, whereas it was the erodent particle size in the case of uncoated steel. As evidenced from the SEM images, the platelet mechanism of erosion seemed to be the prominent one, causing the removal of material from the surface of the steel, whereas for the coating, the formation and interlinking of cracks resulted in the removal of material.

Silica Coating of Nonsilicate Nanoparticles for Resin-Based Composite Materials

PubMed Central

Kaizer, M.R.; Almeida, J.R.; Gonçalves, A.P.R.; Zhang, Y.; Cava, S.S.; Moraes, R.R.

2016-01-01

This study was designed to develop and characterize a silica-coating method for crystalline nonsilicate ceramic nanoparticles (Al2O3, TiO2, and ZrO2). The hypothesis was that the coated nonsilicate nanoparticles would stably reinforce a polymeric matrix due to effective silanation. Silica coating was applied via a sol-gel method, with tetraethyl orthosilicate as a silica precursor, followed by heat treatment. The chemical and microstructural characteristics of the nanopowders were evaluated before and after silica coating through x-ray diffraction, BET (Brunauer-Emmett-Teller), energy-dispersive x-ray spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy analyses. Coated and noncoated nanoparticles were silanated before preparation of hybrid composites, which contained glass microparticles in addition to the nanoparticles. The composites were mechanically tested in 4-point bending mode after aging (10,000 thermal cycles). Results of all chemical and microstructural analyses confirmed the successful obtaining of silica-coated nanoparticles. Two distinct aspects were observed depending on the type of nanoparticle tested: 1) formation of a silica shell on the surface of the particles and 2) nanoparticle clusters embedded into a silica matrix. The aged hybrid composites formulated with the coated nanoparticles showed improved flexural strength (10% to 30% higher) and work of fracture (35% to 40% higher) as compared with composites formulated with noncoated nanoparticles. The tested hypothesis was confirmed: silanated silica-coated nonsilicate nanoparticles yielded stable reinforcement of dimethacrylate polymeric matrix due to effective silanation. The silica-coating method presented here is a versatile and promising novel strategy for the use of crystalline nonsilicate ceramics as a reinforcing phase of polymeric composite biomaterials. PMID:27470069

Correlation between surface properties and wettability of multi-scale structured biocompatible surfaces

NASA Astrophysics Data System (ADS)

Gorodzha, S. N.; Surmeneva, M. A.; Prymak, O.; Wittmar, A.; Ulbricht, M.; Epple, M.; Teresov, A.; Koval, N.; Surmenev, R. A.

2015-11-01

The influence of surface properties of radio-frequency (RF) magnetron deposited hydroxyapatite (HA) and Si-containing HA coatings on wettability was studied. The composition and morphology of the coatings fabricated on titanium (Ti) were characterized using atomic force microscopy (AFM) and X-ray diffraction (XRD). The surface wettability was studied using contact angle analysis. Different geometric parameters of acid-etched (AE) and pulse electron beam (PEB)-treated Ti substrates and silicate content in the HA films resulted in the different morphology of the coatings at micro- and nano- length scales. Water contact angles for the HA coated Ti samples were evaluated as a combined effect of micro roughness of the substrate and nano-roughness of the HA films resulting in higher water contact angles compared with acid-etched (AE) or pulse electron beam (PEB) treated Ti substrates.

Corrosion Behavior of PEO Coatings Formed on AZ31 Alloy in Phosphate-Based Electrolytes with Calcium Acetate Additive

NASA Astrophysics Data System (ADS)

Ziyaei, E.; Atapour, M.; Edris, H.; Hakimizad, A.

2017-07-01

The PEO coating started on magnesium AZ31 using a unipolar DC power source. The coating was generated in the electrolyte based on Na3PO4·12H2O and KOH with calcium acetate as additive. The x-ray diffraction method showed some phases containing calcium and phosphate, which was created in the presence of additive. Also, the EDS tests of the sample's surfaces proved the existence of calcium on the surface. Based on the electrochemical tests results, the most corrosion resistance belongs to the sample with calcium acetate additive. In fact, the results of the EIS tests showed the coating with calcium acetate has the highest resistance but the lowest capacitance. However, this state belongs to the surface morphology, the lower porosity, and surface chemical composition.

Supplementary Microstructural Features Induced During Laser Surface Melting of Thermally Sprayed Inconel 625 Coatings

NASA Astrophysics Data System (ADS)

Ahmed, Nauman; Voisey, K. T.; McCartney, D. G.

2014-02-01

Laser surface melting of thermally sprayed coatings has the potential to enhance their corrosion properties by incorporating favorable microstructural changes. Besides homogenizing the as-sprayed structure, laser melting may induce certain microstructural modifications (i.e., supplementary features) in addition to those that directly improve the corrosion performance. Such features, being a direct result of the laser treatment process, are described in this paper which is part of a broader study in which high velocity oxy-fuel sprayed Inconel 625 coatings on mild-steel substrates were treated with a diode laser and the modified microstructure characterized using optical and scanning electron microscopy and x-ray diffraction. The laser treated coating features several different zones, including a region with a microstructure in which there is a continuous columnar dendritic structure through a network of retained oxide stringers.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Line x-ray source for diffraction enhanced imaging in clinical and industrial applications

NASA Astrophysics Data System (ADS)

Wang, Xiaoqin

Mammography is one type of imaging modalities that uses a low-dose x-ray or other radiation sources for examination of breasts. It plays a central role in early detection of breast cancers. The material similarity of tumor-cell and health cell, breast implants surgery and other factors, make the breast cancers hard to visualize and detect. Diffraction enhanced imaging (DEI), first proposed and investigated by D. Chapman is a new x-ray radiographic imaging modality using monochromatic x-rays from a synchrotron source, which produced images of thick absorbing objects that are almost completely free of scatter. It shows dramatically improved contrast over standard imaging when applied to the same phantom. The contrast is based not only on attenuation but also on the refraction and diffraction properties of the sample. This imaging method may improve image quality of mammography, other medical applications, industrial radiography for non-destructive testing and x-ray computed tomography. However, the size, and cost, of a synchrotron source limits the application of the new modality to be applicable at clinical levels. This research investigates the feasibility of a designed line x-ray source to produce intensity compatible to synchrotron sources. It is composed of a 2-cm in length tungsten filament, installed on a carbon steel filament cup (backing plate), as the cathode and a stationary oxygen-free copper anode with molybdenum coating on the front surface serves as the target. Characteristic properties of the line x-ray source were computationally studied and the prototype was experimentally investigated. SIMIION code was used to computationally study the electron trajectories emanating from the filament towards the molybdenum target. A Faraday cup on the prototype device, proof-of-principle, was used to measure the distribution of electrons on the target, which compares favorably to computational results. The intensities of characteristic x-ray for molybdenum, tungsten and rhodium targets were investigated with different window materials for -30kV to -100kV applied potential. Heat loading and thermal management of the target has been investigated computationally using COMSOL code package, and experimental measurements of target temperature rise was taken via thermocouples attached to the target. Temperature measurements for low voltage, low current regime without active cooling were compared to computational results for code-experiment benchmarking. Two different phantoms were used in the simulation of DEI images, which showed that the designed x-ray source with DEI setup could produce images with significant improved contrast. The computational results, along with experimental measurements on the prototype setup, indicate the possibility of scale up to larger area x-ray source adequate for DEI applications.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

Chitosan reinforced apatite-wollastonite coating by electrophoretic deposition on titanium implants.

PubMed

Sharma, Smriti; Soni, Vivek P; Bellare, Jayesh R

2009-07-01

A novel bioactive porous apatite-wollastonite/chitosan composite coating was prepared by electrophoretic deposition. The influence of synthesis parameters like pH of suspension and current density was studied and optimized. X-ray diffraction confirmed crystalline phase of apatite-wollastonite in powder as well as composite coating with coat crystallinity of 65%. Scanning electron microscope showed that the porosity had interconnections with good homogeneity between the phases. The addition of chitosan increased the adhesive strength of the composite coating. Young's modulus of the coating was found to be 9.23 GPa. One of our key findings was sheet-like apatite growth unlike ball-like growth found in bioceramics. Role of chitosan was studied in apatite growth mechanism in simulated body fluid. In presence of chitosan, dense negatively charged surface with homogenous nucleation was the primary factor for sheet-like evolution of apatite layer. The results suggest that incorporation of chitosan with apatite-wollastonite in composite coating could provide excellent in vitro bioactivity with enhanced mechanical properties.

Dilution effect on the formation of amorphous phase in the laser cladded Ni-Fe-B-Si-Nb coatings after laser remelting process

NASA Astrophysics Data System (ADS)

Li, Ruifeng; Li, Zhuguo; Huang, Jian; Zhu, Yanyan

2012-08-01

Ni-Fe-B-Si-Nb coatings have been deposited on mild steel substrates using high power diode laser cladding. Scanning laser beam at high speeds was followed to remelt the surface of the coatings. Different laser cladding powers in the range of 700-1000 W were used to obtain various dilution ratios in the coating. The dilution effect on the chemical characterization, phase composition and microstructure is analyzed by energy dispersive spectroscopy, X-ray diffraction and scanning-electron microscopy. The microhardness distribution of the coatings after laser processing is also measured. The results reveal that Ni-based amorphous composite coatings have successfully been fabricated on mild steel substrate at low dilution ratio when the cladding power was 700 W, 800 W and 900 W. While at high laser power of 1000 W, no amorphous phase was found. The coatings with low dilution ratio exhibit the highest microhardness of 1200 HV0.5 due to their largest volume fraction of amorphous phase.

Microstructure and properties of ceramic coatings prepared by micro-arc oxidation on 7075 aluminum alloy

NASA Astrophysics Data System (ADS)

Cao, G. P.; Song, R. G.

2018-02-01

Micro-arc oxidation (MAO) ceramic coatings were prepared in silicate-based electrolyte on 7075 aluminum alloy. The effects of current density on microstructure and properties of the MAO coatings were studied by scanning electron microscopy (SEM), stereoscopic microscopy, x-ray diffraction (XRD), electrochemical tests as well as tribological and wear tests. The results showed that the current density plays an important role in affecting the quality of the MAO coatings. XRD results showed that the α-Al2O3 phase first increased then decreased with increasing the current density, which matched well with the micro-hardness test and the wearing test results. On the other hand, the coalescent strength measurements revealed that the coating prepared at the current density of 12 A dm-2 is of the highest adhesion force. The potentiodynamic polarization test proved that the coating obtained under 10 A dm-2 exhibits the best corrosion resistance, which is directly related to the morphology of coating.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

PubMed Central

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stefano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

2010-01-01

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

DOE PAGES

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

2010-04-20

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

High rate reactive sputtering of MoN(x) coatings

NASA Technical Reports Server (NTRS)

Rudnik, Paul J.; Graham, Michael E.; Sproul, William D.

1991-01-01

High rate reactive sputtering of MoN(x) films was performed using feedback control of the nitorgen partial pressure. Coatings were made at four different target powers: 2.5, 5.0, 7.5 and 10 kW. No hysteresis was observed in the nitrogen partial pressure vs. flow plot, as is typically seen for the Ti-N system. Four phases were determined by X-ray diffraction: molybdenum, Mo-N solid solution, Beta-Mo2N and gamma-Mo2N. The hardness of the coatings depended upon composition, substrate bias, and target power. The phases present in the hardest films differed depending upon deposition parameters. For example, the Beta-Mo2N phase was hardest (load 25 gf) at 5.0 kW with a value of 3200 kgf/sq mm, whereas the hardest coatings at 10 kW were the gamma-Mo2N phase (3000 kgf/sq mm). The deposition rate generally decreased with increasing nitrogen partial pressure, but there was a range of partial pressures where the rate was relatively constant. At a target power of 5.0 kW, for example, the deposition rates were 3300 A/min for a N2 partial pressure of 0.05 - 1.0 mTorr.

Lacquer polishing of X-ray optics

NASA Technical Reports Server (NTRS)

Catura, R. C.; Joki, E. G.; Roethig, D. T.; Brookover, W. J.

1987-01-01

Techniques for polishing figured X-ray optics by a lacquer-coating process are described. This acrylic lacquer coating has been applied with an optical quality of an eighth-wave in red light and very effectively covers surface roughness with spatial wavelengths less than about 0.2 mm. Tungsten films have been deposited on the lacquer coatings to provide highly efficient X-ray reflectivity.

Characterization, Corrosion Resistance, and Cell Response of High-Velocity Flame-Sprayed HA and HA/TiO2 Coatings on 316L SS

NASA Astrophysics Data System (ADS)

Singh, Tejinder Pal; Singh, Harpreet; Singh, Hazoor

2012-09-01

The main aim of this study is to evaluate corrosion and biocompatibility behavior of thermal spray hydroxyapatite (HA) and hydroxyapatite/titania bond (HA/TiO2)-coated 316L stainless steel (316L SS). In HA/TiO2 coatings, TiO2 was used as a bond coat between HA top coat and 316L SS substrate. The coatings were characterized by x-ray diffraction and scanning electron microscopy/energy dispersive spectroscopy, and corrosion resistance determined for the uncoated substrate and the two coatings. The biological behavior was investigated by the cell culture studies using osteosarcoma cell line KHOS-NP (R-970-5). The corrosion resistance of the steel was found to increase after the deposition of the HA and HA/TiO2 bond coatings. Both HA, as well as, HA/TiO2 coatings exhibit excellent bond strength of 49 and 47 MPa, respectively. The cell culture studies showed that HA-coated 316L SS specimens appeared more biocompatible than the uncoated and HA/TiO2-coated 316L SS specimens.

Effect of zinc phosphate chemical conversion coating on corrosion behaviour of mild steel in alkaline medium: protection of rebars in reinforced concrete.

PubMed

Simescu, Florica; Idrissi, Hassane

2008-12-01

We outline the ability of zinc phosphate coatings, obtained by chemical conversion, to protect mild steel rebars against localized corrosion, generated by chloride ions in alkaline media. The corrosion resistance of coated steel, in comparison with uncoated rebars and coated and uncoated steel rebars embedded in mortar, were evaluated by open-circuit potential, potentiodynamic polarization, cronoamperometry and electrochemical impedance spectroscopy. The coated surfaces were characterized by x-ray diffraction and scanning electron microscopy. First, coated mild steel rebars were studied in an alkaline solution with and without chloride simulating a concrete pore solution. The results showed that the slow dissolution of the coating generates hydroxyapatite Ca 10 (PO 4 ) 6 (OH) 2 . After a long immersion, the coating became dense and provided an effective corrosion resistance compared with the mild steel rebar. Secondly, the coated and uncoated steel rebars embedded in mortar and immersed in chloride solution showed no corrosion or deterioration of the coated steel. Corrosion rate is considerably lowered by this phosphate coating.

Effect of zinc phosphate chemical conversion coating on corrosion behaviour of mild steel in alkaline medium: protection of rebars in reinforced concrete

NASA Astrophysics Data System (ADS)

Simescu, Florica; Idrissi, Hassane

2008-12-01

We outline the ability of zinc phosphate coatings, obtained by chemical conversion, to protect mild steel rebars against localized corrosion, generated by chloride ions in alkaline media. The corrosion resistance of coated steel, in comparison with uncoated rebars and coated and uncoated steel rebars embedded in mortar, were evaluated by open-circuit potential, potentiodynamic polarization, cronoamperometry and electrochemical impedance spectroscopy. The coated surfaces were characterized by x-ray diffraction and scanning electron microscopy. First, coated mild steel rebars were studied in an alkaline solution with and without chloride simulating a concrete pore solution. The results showed that the slow dissolution of the coating generates hydroxyapatite Ca10(PO4)6(OH)2. After a long immersion, the coating became dense and provided an effective corrosion resistance compared with the mild steel rebar. Secondly, the coated and uncoated steel rebars embedded in mortar and immersed in chloride solution showed no corrosion or deterioration of the coated steel. Corrosion rate is considerably lowered by this phosphate coating.

Effect of zinc phosphate chemical conversion coating on corrosion behaviour of mild steel in alkaline medium: protection of rebars in reinforced concrete

PubMed Central

Simescu, Florica; Idrissi, Hassane

2008-01-01

We outline the ability of zinc phosphate coatings, obtained by chemical conversion, to protect mild steel rebars against localized corrosion, generated by chloride ions in alkaline media. The corrosion resistance of coated steel, in comparison with uncoated rebars and coated and uncoated steel rebars embedded in mortar, were evaluated by open-circuit potential, potentiodynamic polarization, cronoamperometry and electrochemical impedance spectroscopy. The coated surfaces were characterized by x-ray diffraction and scanning electron microscopy. First, coated mild steel rebars were studied in an alkaline solution with and without chloride simulating a concrete pore solution. The results showed that the slow dissolution of the coating generates hydroxyapatite Ca10(PO4)6(OH)2. After a long immersion, the coating became dense and provided an effective corrosion resistance compared with the mild steel rebar. Secondly, the coated and uncoated steel rebars embedded in mortar and immersed in chloride solution showed no corrosion or deterioration of the coated steel. Corrosion rate is considerably lowered by this phosphate coating. PMID:27878037

Morphology and structural development of reduced anatase-TiO{sub 2} by pure Ti powder upon annealing and nitridation: Synthesis of TiO{sub x} and TiO{sub x}N{sub y} powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bolokang, A.S., E-mail: Sylvester.Bolokang@transnet.net; DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria 0001; Transnet Engineering, Product Development, Private Bag X 528, Kilnerpark 0127

2015-02-15

It is well known that nitriding of titanium is suitable for surface coating of biomaterials and in other applications such as anti-reflective coating, while oxygen-rich titanium oxynitride has been applied in thin film resistors and photocatalysis. Thus in this work anatase was reduced with pure titanium powder during annealing in argon. This was done to avoid any metallic contamination and unwanted residual metal doping. As a result, interesting and different types of particle morphology were synthesized when the pre-milled elemental anatase and titanium powders were mixed. The formation of metastable face centred cubic and monoclinic titanium monoxide was detected bymore » the X-ray diffraction technique. The phases were confirmed by energy dispersive X-ray spectroscopy analysis. Raman analysis revealed weak intensity peaks for samples annealed in argon as compared to those annealed under nitrogen. - Graphical abstract: Display Omitted - Highlights: • Reaction of TiO{sub 2} and Ti induced metastable FCC and monoclinic TiO{sub x}. • Compositions of mixed powder were prepared from the unmilled and pre-milled powders. • Nitridation of TiO{sub x} yielded TiO{sub x}N{sub y} phase. • Mixed morphology was observed on all three powder samples.« less

Effects of sintering temperature on the microstructural evolution and wear behavior of WCp reinforced Ni-based coatings

NASA Astrophysics Data System (ADS)

Chen, Chuan-hui; Bai, Yang; Ye, Xu-chu

2014-12-01

This article focuses on the microstructural evolution and wear behavior of 50wt%WC reinforced Ni-based composites prepared onto 304 stainless steel substrates by vacuum sintering at different sintering temperatures. The microstructure and chemical composition of the coatings were investigated by X-ray diffraction (XRD), differential thermal analysis (DTA), scanning and transmission electron microscopy (SEM and TEM) equipped with energy-dispersive X-ray spectroscopy (EDS). The wear resistance of the coatings was tested by thrust washer testing. The mechanisms of the decomposition, dissolution, and precipitation of primary carbides, and their influences on the wear resistance have been discussed. The results indicate that the coating sintered at 1175°C is composed of fine WC particles, coarse M6C (M=Ni, Fe, Co, etc.) carbides, and discrete borides dispersed in solid solution. Upon increasing the sintering temperature to 1225°C, the microstructure reveals few incompletely dissolved WC particles trapped in larger M6C, Cr-rich lamellar M23C6, and M3C2 in the austenite matrix. M23C6 and M3C2 precipitates are formed in both the γ/M6C grain boundary and the matrix. These large-sized and lamellar brittle phases tend to weaken the wear resistance of the composite coatings. The wear behavior is controlled simultaneously by both abrasive wear and adhesive wear. Among them, abrasive wear plays a major role in the wear process of the coating sintered at 1175°C, while the effect of adhesive wear is predominant in the coating sintered at 1225°C.

Coherent x-ray zoom condenser lens for diffractive and scanning microscopy.

PubMed

Kimura, Takashi; Matsuyama, Satoshi; Yamauchi, Kazuto; Nishino, Yoshinori

2013-04-22

We propose a coherent x-ray zoom condenser lens composed of two-stage deformable Kirkpatrick-Baez mirrors. The lens delivers coherent x-rays with a controllable beam size, from one micrometer to a few tens of nanometers, at a fixed focal position. The lens is suitable for diffractive and scanning microscopy. We also propose non-scanning coherent diffraction microscopy for extended objects by using an apodized focused beam produced by the lens with a spatial filter. The proposed apodized-illumination method will be useful in highly efficient imaging with ultimate storage ring sources, and will also open the way to single-shot coherent diffraction microscopy of extended objects with x-ray free-electron lasers.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

Antibacterial characteristics of thermal plasma spray system.

PubMed

Goudarzi, M; Saviz, Sh; Ghoranneviss, M; Salar Elahi, A

2018-03-15

The objective of this study is to investigate antibacterial characteristics of a thermal plasma spray system. For this purpose, copper powder was coated on a handmade atmospheric plasma spraying system made by the stainless steel 316 substrate, which is preheated at different temperatures before spraying. A number of deposition characteristics such as antibacterial characteristics, adhesion strength and hardness of coating, was investigated. All of the spray parameters are fixed except the substrate temperature. The chemical composition was analyzed by X-ray diffraction (XRD). A scanning electron microscopy (SEM) and back scattering electron microscopy (BSE) were used to show the coating microstructure, its thickness and also the powder micrograph. The energy dispersive X-ray spectroscopy (EDX) was used to analyze the coating particles. Hardness of the deposition was examined by Vickers tester (HV0.1). Its adhesion strength was declared by cross cut tester (TQC). In addition, the percentage of bactericidal coating was evidenced with Staphylococcus aurous and Escherichia coli bacteria. Study results show that as the substrates temperature increases, the number of splats in the shape of pancake increases, the greatness and percentage of the deposition porosity both decrease. The increment of the substrate temperature leads to more oxidation and makes thicker dendrites on the splat. The enhancement of the substrate temperature also enlarges thickness and efficiency of coating. The interesting results are that antibacterial properties of coatings against the Escherichia coli are more than Staphylococcus aurous bacteria. However the bactericidal percentage of the coatings against Staphylococcus aurous and Escherichia coli bacteria roughly does not change with increasing the substrate temperature. Furthermore, by increment of the substrate temperature, coatings with both high adhesion and hardness are obtained. Accordingly, the temperature of substrate can be an important parameter for progressing mechanical properties of the antiseptic deposition.

Potentiodynamic studies of Ni-P-TiO{sub 2} nano-composited coating on the mild steel deposited by electroless plating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uttam, Vibha, E-mail: vibhauttam74@gmail.com; Duchaniya, R. K., E-mail: rkduchaniya.meta@mnit.ac.in

2016-05-06

Now a days, corrosion studies are important for reducing the wastage of metals. The importance of corrosion studies is two folds i.e. first is economic, including the reduction of material losses resulting from the wasting away or sudden failure of materials and second is conservation Electroless process is an autocatalytic reduction method in which metallic ions are reduced in the solution. Nanocomposite coatings of Ni-P-TiO{sub 2} on mild steel are deposited by varying volume of TiO{sub 2} nano-powder by electroless method from Ni-P plating bath containing Nickel Sulphate as a source of nickel ions, sodium hypophosphite as the reducing agent,more » lactic acid as a complexing agents and TiO{sub 2} nano powder. Electroless Ni-P-TiO{sub 2} coating have been widely used in the chemical process industries, mechanical industries, electronic industries and chloroalkali industries due to their excellent corrosion with mechanical properties. In the present work, deposition of Ni-P alloy coating and Ni-P-TiO{sub 2} nanocomposited coatings were done on the mild steel and corrosion properties were studied with Potentio-dynamic polarization measurements method in 3.5 wt% sodium chloride solution. It showed in the experiments that Ni-P-TiO{sub 2} nanocomposited coating has better corrosion resistance as comparedthan Ni-P alloy coating. Morphological studies were done by field emission scanning electron microscopy (FESEM), energy–dispersive analysis of X-ray (EDAX) and X-ray diffraction (XRD). These studies confirmed the deposition of Ni-P alloy coating and Ni-P-TiO{sub 2} nanocomposited coating.« less

Characterization of coatings formed on AZX magnesium alloys by plasma electrolytic oxidation

NASA Astrophysics Data System (ADS)

Anawati, Anawati; Gumelar, Muhammad Dikdik

2018-05-01

Plasma Electrolytic Oxidation (PEO) is an electrochemical anodization process which involves the application of a high voltage to create intense plasma on a metal surface to form a ceramic type of oxide. The resulted coating exhibits high wear resistance and good corrosion barrier which are suitable to enhance the performance of biodegradable Mg alloys. In this work, the role of alloying element Ca in modifying the characteristics of PEO layer formed on AZ61 series magnesium alloys was investigated. PEO treatment was conducted on AZ61, AZX611, and AZX612 alloys in 0.5 M Na3PO4 solution at a constant current of 200 A/m2 at 25°C for 8 min. The resulted coatings were characterized by field emission-scanning electron microscope (FESEM), X-ray diffraction spectroscopy (XRD), and X-ray fluorescence spectroscopy (XRF), as well as hardness test. The presence of alloying element Ca in the AZ61 alloys accelerated the PEO coatings formation without altering the coating properties significantly. The coating formed on AZX specimen was slightly thicker ( 14-17 µm) than that of formed onthe AZ specimens ( 13 µm). Longer exposure time to plasma discharge was the reason for faster thickening of the coating layer on AZX specimen. XRD detected a similar crystalline oxide phase of Mg3(PO4)2 in the oxide formed on all of the specimens. Zn was highly incorporated in the coatings with a concentration in the range 24-30 wt%, as analyzed by XRF. Zn compound might exist in amorphous phases. The microhardness test on the coatings revealed similar average hardness 124 HVon all of the specimens.

Study of metallic powder behavior in very low pressure plasma spraying (VLPPS) — Application to the manufacturing of titanium–aluminum coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vautherin, B.; Planche, M.-P.; Montavon, G.

2015-08-28

In this study, metallic materials made of aluminum and titanium were manufactured implementing very low pressure plasma spraying (VLPPS). Aluminum was selected at first as a demonstrative material due to its rather low vaporization enthalpy ( i.e., 381.9 kJ·mol⁻¹). Developments were then carried out with titanium which exhibits a higher vaporization enthalpy ( i.e., 563.6 kJ·mol⁻¹). Optical emission spectroscopy (OES) was implemented to analyze the behavior of each solid precursor (metallic powders) when it is injected into the plasma jet under very low pressure ( i.e., in the 150 Pa range). Besides, aluminum, titanium and titanium–aluminum coatings were deposited inmore » the same conditions implementing a stick-cathode plasma torch operated at 50 kW, maximum power. Coating phase compositions were identified by X-Ray Diffraction (XRD). Coating elementary compositions were quantified by Glow Discharge Optical Emission Spectroscopy (GDOES) and Energy Dispersive Spectroscopy (EDS) analyses. The coating structures were observed by Scanning Electron Microscopy (SEM). The coating void content was determined by Ultra-Small Angle X-ray Scattering (USAXS). The coatings exhibit a two-scale structure corresponding to condensed vapors (smaller scale) and solidified areas (larger scale). Titanium–aluminum sprayed coatings, with various Ti/Al atomic ratios, are constituted of three phases: metastable α-Ti, Al and metastable α₂-Ti₃Al. This latter is formed at elevated temperature in the plasma flow, before being condensed. Its rather small fraction, impeded by the rather small amount of vaporized Ti, does not allow modifying however the coating hardness.« less

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Characterization and Evaluation of Ti-Zr-V Non-evaporable Getter Films Used in Vacuum Systems

NASA Astrophysics Data System (ADS)

Ferreira, M. J.; Seraphim, R. M.; Ramirez, A. J.; Tabacniks, M. H.; Nascente, P. A. P.

Among several methods used to obtain ultra-high vacuum (UHV) for particles accelerators chambers, it stands out the internal coating with metallic films capable of absorbing gases, called NEG (non-evaporable getter). Usually these materials are constituted by elements of great chemical reactivity and solubility (such as Ti, Zr, and V), at room temperature for oxygen and other gases typically found in UHV, such as H2, CO, and CO2. Gold and ternary Ti-Zr-V films were produced by magnetron sputtering, and their composition, structure, morphology, and aging characteristics were characterized by energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), field emission gun sc anning electronmicroscopy (FEG-SEM), atomic force microscopy (AFM), high resolution transmission electron microscopy (HRTEM). The comparison between the produced films and commercial samples indicated that the desirable characteristics depend on the nanometric structure of the films and that this structure is sensitive to the heat treatments.

Studying Ultradisperse Diamond Structure within Explosively Synthesized Samples via X-Ray Techniques

NASA Astrophysics Data System (ADS)

Sharkov, M. D.; Boiko, M. E.; Ivashevskaya, S. N.; Belyakova, N. S.

2013-08-01

XRD (X-Ray Diffraction) and SAXS (Small-Angle X-Ray Scattering) data have been measured for a pair of samples produced with the help of explosives. XRD peaks have shown the both samples to contain crystal diamond components as well as graphite ones. Basing on SAXS analysis, possible presence of grains with radii up to 30-50 nm within all the samples has been shown. Structure components with fractal dimension between 1 and 2 in the sample have been detected, this fact being in agreement with the assumption of diamond grain coating similarity to onion shells. In order to broad rocking curves analysis, the standard SAXS treatment technique has been complemented by a Fourier filtering procedure. For the sample #1, rocking curve components corresponding to individual interplanar distances with magnitudes from 5 nm up to 15 nm have been separated. A hypothesis relating these values to the distances between concentric onion-like shells of diamond grains has been formulated.

Angular rheology study of colloidal nanocrystals using Coherent X-ray Diffraction

NASA Astrophysics Data System (ADS)

Liang, Mengning; Harder, Ross; Robinson, Ian

2007-03-01

A new method using coherent x-ray diffraction provides a way to investigate the rotational motion of a colloidal suspension of crystals in real time. Coherent x-ray diffraction uses the long coherence lengths of synchrotron sources to illuminate a nanoscale particle coherently over its spatial dimensions. The penetration of high energy x-rays into various media allows for in-situ measurements making it ideal for suspensions. This technique has been used to image the structure of nanocrystals for some time but also has the capability of providing information about the orientation and dynamics of crystals. The particles are imaged in a specific diffraction condition allowing us to determine their orientation and observe how they rotate in real time with exceptional resolution. Such sensitivity allows for the study of rotational Brownian motion of nanocrystals in various suspensions and conditions. We present a study of the angular rheology of alumina and TiO2 colloidal nanocrystals in media using coherent x-ray diffraction.

Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

NASA Astrophysics Data System (ADS)

Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffière, J. Y.

2010-12-01

The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

NASA Astrophysics Data System (ADS)

Wang, Mao-Hua; Zhang, Bo; Zhou, Fu

2014-07-01

Silica was homogeneously coated on the surface of CaCu3Ti4O12 (CCTO) particles via the sol-gel method. The obtained powders were characterized by x-ray diffraction analysis, Fourier-transform infrared spectroscopy, transmission electron microscopy (TEM), energy-dispersive spectroscopy, scanning electron microscopy, and zeta potential analysis. The results demonstrate that there were silica layers on the surface of the CCTO particles. Physical and dielectric properties of silica-coated CCTO were also studied. TEM imaging showed that the thickness of the silica layer on the CCTO particles was about 20 nm to 35 nm. The specimen coated with 1.0 wt.% silica showed the maximum relative density of 96.7% with high dielectric constant (12.78 × 104) and low dielectric loss (0.005) at 20°C after sintering at 1000°C for 6 h.

Furnace Cyclic Oxidation Behavior of Multi-Component Low Conductivity Thermal Barrier Coatings

NASA Technical Reports Server (NTRS)

Zhu, Dong-Ming; Nesbitt, James A.; Barrett, Charles A.; McCue, Terry R.; Miller, Robert A.

2004-01-01

Ceramic thermal barrier coatings will play an increasingly important role in advanced gas turbine engines because of their ability to further increase engine operating temperatures and reduce cooling, thus helping achieve future engine low emission, high efficiency and improved reliability goals. Advanced multi-component zirconia-based thermal barrier coatings are being developed using an oxide defect clustering design approach to achieve the required coating low thermal conductivity and high temperature stability. Although the new composition coatings were not yet optimized for cyclic durability, an initial durability screening of the candidate coating materials was conducted using conventional furnace cyclic oxidation tests. In this paper, furnace cyclic oxidation behavior of plasma-sprayed zirconia-based defect cluster thermal barrier coatings was investigated at 1163 C using 45 min hot cycles. The ceramic coating failure mechanisms were studied using scanning electron microscopy (SEM) combined with X-ray diffraction (XRD) phase analysis after the furnace tests. The coating cyclic lifetime is also discussed in relation to coating processing, phase structures, dopant concentration, and other thermo-physical properties.

Incorporation of Fe3O4/CNTs nanocomposite in an epoxy coating for corrosion protection of carbon steel

NASA Astrophysics Data System (ADS)

Pham, Gia Vu; Truc Trinh, Anh; To, Thi Xuan Hang; Duong Nguyen, Thuy; Trang Nguyen, Thu; Hoan Nguyen, Xuan

2014-09-01

In this study Fe3O4/CNTs composite with magnetic property was prepared by attaching magnetic nanoparticles (Fe3O4) to carbon nanotubes (CNTs) by hydrothermal method. The obtained Fe3O4/CNTs composite was characterized by Fourier transform infrared (FTIR) spectroscopy, powder x-ray diffraction and transmission electron microscopy. The Fe3O4/CNTs composite was then incorporated into an epoxy coating at concentration of 3 wt%. Corrosion protection of epoxy coating containing Fe3O4/CNTs composite was evaluated by electrochemical impedance spectroscopy and adhesion measurement. The impedance measurements show that Fe3O4/CNTs composite enhanced the corrosion protection of epoxy coating. The corrosion resistance of the carbon steel coated by epoxy coating containing Fe3O4/CNTs composite was significantly higher than that of carbon steel coated by clear epoxy coating and epoxy coating containing CNTs. FE-SEM photographs of fracture surface of coatings showed good dispersion of Fe3O4/CNTs composite in the epoxy matrix.

Enhancement of photoluminescence intensity of GaAs with cubic GaS chemical vapor deposited using a structurally designed single-source precursor

NASA Technical Reports Server (NTRS)

Macinnes, Andrew N.; Power, Michael B.; Barron, Andrew R.; Jenkins, Phillip P.; Hepp, Aloysius F.

1993-01-01

A two order-of-magnitude enhancement of photoluminescence intensity relative to untreated GaAs has been observed for GaAs surfaces coated with chemical vapor-deposited GaS. The increase in photoluminescence intensity can be viewed as an effective reduction in surface recombination velocity and/or band bending. The gallium cluster /(t-Bu)GaS/4 was used as a single-source precursor for the deposition of GaS thin films. The cubane core of the structurally characterized precursor is retained in the deposited film producing a cubic phase. Furthermore, a near-epitaxial growth is observed for the GaS passivating layer. Films were characterized by transmission electron microscopy, X-ray powder diffraction, and X-ray photoelectron and Rutherford backscattering spectroscopies.

Photoluminescence intensity enhancement of GaAs by vapor-deposited GaS - A rational approach to surface passivation

NASA Technical Reports Server (NTRS)

Jenkins, Phillip P.; Hepp, Aloysius F.; Power, Michael B.; Macinnes, Andrew N.; Barron, Andrew R.

1993-01-01

A two order-of-magnitude enhancement of photoluminescence intensity relative to untreated GaAs has been observed for GaAs surfaces coated with chemical vapor-deposited GaS. The increase in photoluminescence intensity can be viewed as an effective reduction in surface recombination velocity and/or band bending. The gallium cluster (/t-Bu/GaS)4 was used as a single-source precursor for the deposition of GaS thin films. The cubane core of the structurally-characterized precursor is retained in the deposited film producing a cubic phase. Furthermore, a near-epitaxial growth is observed for the GaS passivating layer. Films were characterized by transmission electron microscopy, X-ray powder diffraction, and X-ray photoelectron and Rutherford backscattering spectroscopies.

In situ formation deposited ZnO nanoparticles on silk fabrics under ultrasound irradiation.

PubMed

Khanjani, Somayeh; Morsali, Ali; Joo, Sang W

2013-03-01

Deposition of zinc(II) oxide (ZnO) nanoparticles on the surface of silk fabrics was prepared by sequential dipping steps in alternating bath of potassium hydroxide and zinc nitrate under ultrasound irradiation. This coating involves in situ generation and deposition of ZnO in a one step. The effects of ultrasound irradiation, concentration and sequential dipping steps on growth of the ZnO nanoparticles have been studied. Results show a decrease in the particles size as increasing power of ultrasound irradiation. Also, increasing of the concentration and sequential dipping steps increase particle size. The physicochemical properties of the nanoparticles were determined by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and wavelength dispersive X-ray (WDX). Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation of V-Doped LiFePO4/C as the Optimized Cathode Material for Lithium Ion Batteries.

PubMed

Sun, Pingping; Zhang, Haiyang; Shen, Kai; Fan, Qi; Xu, Qingyu

2015-04-01

LiFe1-x,Vx,PO4/C composites were synthesized by solid state reaction. The effect of carbon coating and V doping on the performance of LiFePO4 has been systematically investigated by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), transmission electron microscope (TEM), charge/discharge and cyclic voltammetry (CV) measurement. The results show that carbon coating and proper amount of V incorporation do not significantly change the host crystal structure of LiFePO4, while the electrochemical performance of LiFePO4 can be significantly improved. Particularly, the LiFe0.96V0.04PO4/C exhibits the best performance with a specific discharge capacity of 105.5 mA h/g at 5.0 C, 90.3 mA h/g at 10 C and 66.7 mA h/g at 30 C with stable cycle performance, which is significantly improved compared with the pure LiFePO4/C. The cyclic voltammograms result reveals that V doping could decrease the resistance of LiFePO4/C composite electrode drastically and improve its reversibility.

Development of enteric-coated fixed dose combinations of amorphous solid dispersions of ezetimibe and lovastatin: Investigation of formulation and process parameters.

PubMed

Riekes, Manoela K; Dereymaker, Aswin; Berben, Philippe; Augustijns, Patrick; Stulzer, Hellen K; Van den Mooter, Guy

2017-03-30

Enteric-coated fixed-dose combinations of ezetimibe and lovastatin were prepared by fluid bed coating aiming to avoid the acidic conversion of lovastatin to its hydroxyacid derivative. In a two-step process, sucrose beads were layered with a glass solution of ezetimibe, lovastatin and Soluplus ® , top-coated with an enteric layer. The impact of different bead size, enteric polymers (Eudragit L100 ® and Eudragit L100-55 ® ) and coating time was investigated. Samples were evaluated by X-ray diffraction, scanning electron microscopy, laser diffraction and in vitro studies in 0.1M HCl and phosphate buffer pH 6.8. Results showed that smaller beads tend to agglomerate and release was jeopardized in acidic conditions, most likely due to irregular coating layer. Eudragit L100-55 ® required longer processing, but thinner coating layers provided lower drug release. Both polymers showed low drug release in acidic environment and fast release at pH 6.8. The off-line measurement of the coating thickness determined the ideal coating time as 15 and 30min for Eudragit L100-55 ® and Eudragit L100 ® -based samples, respectively. Both compounds were molecularly dispersed in Soluplus ® , and Eudragit L100 ® formulations showed concave pores on the surface, presenting higher drug release in acidic conditions. Stability studies after 6 months showed unaltered physical properties and drug release. Copyright © 2017 Elsevier B.V. All rights reserved.

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

Influence of annealing temperature on structural and optical properties of Lu{sub 2}O{sub 3}:Eu{sup 3+}, Tb{sup 3+} transparent films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morales-Ramírez, Ángel de Jesús; García-Murillo, Antonieta, E-mail: angarciam@ipn.mx; Carrillo-Romo, Felipe de Jesús

2015-10-15

Highlights: • Lu{sub 2}O{sub 3}:Eu{sup 3+}, Tb{sup 3+} films were synthesized by sol–gel and by dip-coating technique. • Effects of annealing treatment on structural and optical properties were studied. • Optogeometrical characteristics of synthesized films were analyzed. • X-ray diffraction results showed that Lu{sub 2}O{sub 3}:Eu{sup 3+}, Tb{sup 3+} crystallizes at 700 °C. • High reddish emission on transparent films with at least 1 μm thick was observed. - Abstract: High-optical quality Lu{sub 2}O{sub 3}:Eu{sup 3+} 5 mol%, X Tb{sup 3+} (X = 0–0.04 mol%) thin films were prepared by the sol–gel process and dip-coating technique. The procedure was asmore » follows: lutetium, europium and terbium nitrates were used as precursors, and ethanol as a solvent. Etylenglycol (EG) was added as a sol stabilizer, and the pH was adjusted by acetic acid. After 10 dipping-cycles, followed by an annealing process (600–900 °C) for 1 h, transparent, smooth and crack-free films (ra = 8–9 nm) were formed. The X-ray diffraction (XRD) results showed crystallized films into the cubic structure at 800 °C. The ellipsometry results showed that the thickness of the films varied from 1 to 1.4 μm at 1000 and 600 °C, respectively. Finally, the films presented a typical Eu{sup 3+} red emission at 611 nm ({sup 5}D{sub 0} → {sup 7}F{sub 2}); furthermore, the effect of the Tb{sup 3+} content showed that the highest emission intensity corresponded to the lower Tb{sup 3+} content.« less

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

2016-05-15

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

NASA Astrophysics Data System (ADS)

Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

2004-03-01

We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.