Synthesis of mesoporous cerium compound for CO2 capture

NASA Astrophysics Data System (ADS)

Liu, Guiqing; Tatsuda, Kou; Yoneyama, Yoshiharu; Tsubaki, Noritatsu

2017-11-01

A mesoporous adsorbent was simply synthesized by adding alkaline substances to cerium(III) nitric hydrate. The surface characteristics of the synthesized cerium compound were determined with BET, XRD and TEM analysis. It was found that although the specific surface areas of the synthesized cerium compounds were among about 120-200m2 per gram (BET area) which were smaller than the common used zeolite 13X (BET area 743 m2/g) and activated carbon (BET area 1079 m2/g), but the cerium compounds had excellent performances for CO2 adsorption as well as the CO2 desorption.

Role of Exposed Surfaces on Zinc Oxide Nanostructures in the Catalytic Ethanol Transformation.

PubMed

Morales, María V; Asedegbega-Nieto, Esther; Iglesias-Juez, Ana; Rodríguez-Ramos, Inmaculada; Guerrero-Ruiz, Antonio

2015-07-08

For a series of nanometric ZnO materials, the relationship between their morphological and surface functionalities and their catalytic properties in the selective decomposition of ethanol to yield acetaldehyde was explored. Six ZnO solids were prepared by a microemulsion-precipitation method and the thermal decomposition of different precursors and compared with a commercial sample. All these materials were characterized intensively by XRD and SEM to obtain their morphological specificities. Additionally, surface area determinations and IR spectroscopy were used to detect differences in the surface properties. The density of acid surface sites was determined quantitatively using an isopropanol dehydration test. Based on these characterization studies and on the results of the catalytic tests, it has been established that ZnO basal surfaces seem to be responsible for the production of ethylene as a minor product as well as for secondary reactions that yield acetyl acetate. Furthermore, one specific type of exposed hydroxyl groups appears to govern the surface catalytic properties. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biotemplated synthesis of high specific surface area copper-doped hollow spherical titania and its photocatalytic research for degradating chlorotetracycline

NASA Astrophysics Data System (ADS)

Bu, Dan; Zhuang, Huisheng

2013-01-01

Copper-doped titania (Cu/TiO2) hollow microspheres were fabricated using the rape pollen as biotemplates via an improved sol-gel method and a followed calcinations process. In the fabricated process, a titanium(IV)-isopropoxide-based sol directly coated onto the surface of rape pollen. Subsequently, after calcinations, rape pollen was removed by high temperature and the hollow microsphere structure was retained. The average diameter of as-obtained hollow microspheres is 15-20 μm and the thickness of shell is approximately 0.6 μm. Knowing from XRD results, the main crystal phase of microspheres is anatase, coupled with rutile. The specific surface area varied between 141.80 m2/g and 172.51 m2/g. This hollow sphere photocatalysts with high specific surface area exhibited stronger absorption ability and higher photoactivity, stimulated by visible light. The degradation process of chlortetracycline (CTC) solution had been studied. The degradated results indicate that CTC could be effective degradated by fabricated hollow spherical materials. And the intermediate products formed in the photocatalytic process had been identified.

Investigation of Structure and Property of Indian Cocos nucifera L. Fibre

NASA Astrophysics Data System (ADS)

Basu, Gautam; Mishra, Leena; Samanta, Ashis Kumar

2017-12-01

Structure and physico-mechanical properties of Cocos nucifera L. fibre from a specific agro-climatic region of India, was thoroughly studied. Fine structure of the fibre was examined by Fourier Transform Infra-Red (FTIR) spectroscopy, Thermo-Gravimetric Analysis (TGA), X-Ray Diffraction (XRD), component analysis, Scanning Electron Microscope (SEM) and optical microscope. SEM shows prominent longitudinal cracks and micro-pores on the surface. XRD shows a low degree of crystallinity (45%), bigger crystallite size, and even the presence of appreciable amount of non-cellulose matter. FTIR reveals presence of large quantities of hydroxyl, phenolic and aldehyde groups. Component and thermal analyses indicates presence of cellulose and lignin as major components. Physical parameters reveal that, fibres are highly variable in length (range 44-305 mm), and diameter (range 100-795 µm). Mechanical properties of the fibre viz. breaking tenacity, breaking extensibility, specific work of rupture, and coefficient of friction were measured. Microbial decomposition test under soil reveals excellent durability of coconut fibre which makes it appropriate for the application in geotextiles. Mass specific electrical resistance of 4 Ω-kg/m2 indicates its enhanced insulation as compared to the jute.

Few layered vanadyl phosphate nano sheets-MWCNT hybrid as an electrode material for supercapacitor application

NASA Astrophysics Data System (ADS)

Dutta, Shibsankar; De, Sukanta

2016-05-01

It have been already seen that 2-dimensional nano materials are the suitable choice for the supercapacitor application due to their large specific surface area, electrochemical active sites, micromechanical flexibility, expedite ion migration channel properties. Free standing hybrid films of functionalized MWCNT (- COOH group) and α-Vanadyl phosphates (VOPO42H2O) are prepared by vacuum filtering. The surface morphology and microstructure of the samples are studied by transmission electron microscope, field emission scanning electron microscope, XRD, Electrochemical properties of hybrid films have been investigated systematically in 1M Na2SO4 aqueous electrolyte. The hybrid material exhibits a high specific capacitance 236 F/g with high energy density of 65.6 Wh/Kg and a power density of 1476 W/Kg.

Proxy-based accelerated discovery of Fischer–Tropsch catalysts† †Electronic supplementary information (ESI) available: Details of synthesis, analysis and testing, validation experiments for high-throughput XRD and gas treatment, details of statistical analysis and calculations, tabulation of synthesis parameters and XRD results, alternatives to Fig. 3 highlighting different data points, FTS testing results displayed graphically. See DOI: 10.1039/c4sc02116a Click here for additional data file.

PubMed Central

Boldrin, Paul; Gallagher, James R.; Combes, Gary B.; Enache, Dan I.; James, David; Ellis, Peter R.; Kelly, Gordon; Claridge, John B.

2015-01-01

Development of heterogeneous catalysts for complex reactions such as Fischer–Tropsch synthesis of fuels is hampered by difficult reaction conditions, slow characterisation techniques such as chemisorption and temperature-programmed reduction and the need for long term stability. High-throughput (HT) methods may help, but their use has until now focused on bespoke micro-reactors for direct measurements of activity and selectivity. These are specific to individual reactions and do not provide more fundamental information on the materials. Here we report using simpler HT characterisation techniques (XRD and TGA) along with ageing under Fischer–Tropsch reaction conditions to provide information analogous to metal surface area, degree of reduction and thousands of hours of stability testing time for hundreds of samples per month. The use of this method allowed the identification of a series of highly stable, high surface area catalysts promoted by Mg and Ru. In an advance over traditional multichannel HT reactors, the chemical and structural information we obtain on the materials allows us to identify the structural effects of the promoters and their effects on the modes of deactivation observed. PMID:29560180

Oxidation behavior of a ferritic stainless steel Crofer22 APU with thermal cycling

NASA Astrophysics Data System (ADS)

Song, MyoungYoup; Duong, Anh T.; Mumm, Daniel R.

2013-01-01

Crofer22 APU specimens were prepared by grinding with grit 80 and 120 SiC grinding papers and were thermally cycled. The variation in oxidation behavior with thermal cycling was then investigated. Observation of microstructure, measurement of area specific resistance (ASR), analysis of the atomic percentages of the elements by EDX, and XRD analysis were performed. XRD patterns showed that the (Cr, Mn)3O4 spinel phase grew on the surface of the Crofer22 APU samples ground with grit 120. For the samples ground with grit 80, the ASR increased as the number of thermal cycles increased. Plots of ln (ASR/T) vs. 1/T for the samples ground with grit 80 after n = 4, 20 and 40 exhibited good linearity, and the apparent activation energies were between 63.7 kJ/mole and 76.3 kJ/mole.

Mineralogical In-situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernandez-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

2007-01-01

A field campaign was organized in September 2006 by Centro de Astobiologica (Spain) and Washington University (St Louis, USA) for the geological study of the Rio Tinto river bed sediments using a suite of in-situ instruments comprising an ASD reflectance spectrometer, an emission spectrometer, panoramic and close-up color imaging cameras, a life detection system and NASA's CheMin 4 XRD/XRF prototype. The primary objectives of the field campaign were to study the geology of the site and test the potential of the instrument suite in an astrobiological investigation context for future Mars surface robotic missions. The results of the overall campaign will be presented elsewhere. This paper focuses on the results of the XRD/XRF instrument deployment. The specific objectives of the CheMin 4 prototype in Rio Tinto were to 1) characterize the mineralogy of efflorescent salts in their native environments; 2) analyze the mineralogy of salts and oxides from the modern environment to terraces formed earlier as part of the Rio Tinto evaporative system; and 3) map the transition from hematite-dominated terraces to the mixed goethite/salt-bearing terraces where biosignatures are best preserved.

Few layered vanadyl phosphate nano sheets-MWCNT hybrid as an electrode material for supercapacitor application

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

Dutta, Shibsankar; De, Sukanta, E-mail: sukanta.physics@presiuniv.ac.in

It have been already seen that 2-dimensional nano materials are the suitable choice for the supercapacitor application due to their large specific surface area, electrochemical active sites, micromechanical flexibility, expedite ion migration channel properties. Free standing hybrid films of functionalized MWCNT (– COOH group) and α-Vanadyl phosphates (VOPO{sub 4}2H{sub 2}O) are prepared by vacuum filtering. The surface morphology and microstructure of the samples are studied by transmission electron microscope, field emission scanning electron microscope, XRD, Electrochemical properties of hybrid films have been investigated systematically in 1M Na{sub 2}SO{sub 4} aqueous electrolyte. The hybrid material exhibits a high specific capacitance 236more » F/g with high energy density of 65.6 Wh/Kg and a power density of 1476 W/Kg.« less

Preparation and characterization of pitch-based nanoporous carbons for improving CO{sub 2} capture

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

Lee, Seul-Yi; Yoo, Hye-Min; Park, Sang Wook

2014-07-01

Pitch is considered a promising low-cost carbon precursor. However, when pitch is pyrolyzed, it forms polycrystalline graphite, which is non-porous, and therefore, not useful for CO{sub 2} adsorption. In this work, pitch was chemically activated to obtain a large specific surface area and micropore volume. Varying weight ratios of KOH (i.e., 0, 1, 2, and 3) were used as the activating agent. The characteristics of the samples were investigated using scanning electron microscopy (SEM), N{sub 2}/77 K adsorption isotherms, and X-ray diffraction (XRD). The CO{sub 2} adsorption performance was studied by isothermal adsorption/desorption measurements. The results showed that an increasemore » in specific surface areas and total pore volumes of pitch-based nanoporous carbons, resulted in an enhancement of CO{sub 2} adsorption capacity. - Graphical abstract: This is the surface morphologies of pitch precursor and pitch-derived activated carbon (AC-2). - Highlights: • Pitch is considered a promising low-cost carbon precursor. • Specific surface area: 1442 m{sup 2}/g and micropore volume: 0.504 cm{sup 3}/g. • CO{sub 2} adsorption capacity showed 203 mg/g (@ RT/1 bar)« less

Induced superhydrophobic and antimicrobial character of zinc metal modified ceramic wall tile surfaces

NASA Astrophysics Data System (ADS)

Özcan, Selçuk; Açıkbaş, Gökhan; Çalış Açıkbaş, Nurcan

2018-04-01

Hydrophobic surfaces are also known to have antimicrobial effect by restricting the adherence of microorganisms. However, ceramic products are produced by high temperature processes resulting in a hydrophilic surface. In this study, an industrial ceramic wall tile glaze composition was modified by the inclusion of metallic zinc powder in the glaze suspension applied on the pre-sintered wall tile bodies by spraying. The glazed tiles were gloss fired at industrially applicable peak temperatures ranging from 980 °C to 1100 °C. The fired tile surfaces were coated with a commercial fluoropolymer avoiding water absorption. The surfaces were characterized with SEM, EDS, XRD techniques, roughness, sessile water drop contact angle, surface energy measurements, and standard antimicrobial tests. The surface hydrophobicity and the antimicrobial activity results were compared with that of unmodified, uncoated gloss fired wall tiles. A superhydrophobic contact angle of 150° was achieved at 1000 °C peak temperature due to the formation of micro-structured nanocrystalline zinc oxide granules providing a specific surface topography. At higher peak temperatures the hydrophobicity was lost as the specific granular surface topography deteriorated with the conversion of zinc oxide granules to the ubiquitous willemite crystals embedded in the glassy matrix. The antimicrobial efficacy also correlated with the hydrophobic character.

Regeneration of Waste Edible Oil by the Use of Virgin and Calcined Magnesium Hydroxide as Adsorbents.

PubMed

Ogata, Fumihiko; Kawasaki, Naohito

2016-01-01

In this study, we prepared virgin (S, L) and calcined (S-380, S-1000, L-380, L-1000) magnesium hydroxide for regeneration of waste edible oil. Deterioration of soybean oil, rapeseed oil, and olive oil was achieved by heat and aeration treatment. The properties of the different adsorbents were investigated using specific surface area measurements, scanning electron microscopy, X-ray diffraction analysis, thermogravimetric-differential thermal analysis, and surface pH measurement. Moreover, the relationship between the changes in acid value (AV) and carbonyl value (CV) and the adsorbent properties were evaluated. The specific surface areas of S-380 and L-380 were greater than that of other adsorbents. In addition, the XRD results show that S-380 and L-380 contain both magnesium hydroxide and magnesium oxide structures. The decreases in AV and CV using S-380 and L-380 were greater than achieved using other adsorbents. The correlation coefficients between the decrease in AV and CV and specific surface area were 0.947 for soybean oil, 0.649 for rapeseed oil, and 0.773 for olive oil, respectively. The results obtained in this study suggest that a physical property of the adsorbent, namely specific surface area, was primarily responsible for the observed decreases in AV and CV. Overall, the results suggest that S-380 and L-380 are useful for the regeneration of waste edible oil.

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

Use of glancing angle X-ray powder diffractometry to depth-profile phase transformations during dissolution of indomethacin and theophylline tablets.

PubMed

Debnath, Smita; Predecki, Paul; Suryanarayanan, Raj

2004-01-01

The purpose of this study was (i) to develop glancing angle x-ray powder diffractometry (XRD) as a method for profiling phase transformations as a function of tablet depth; and (ii) to apply this technique to (a) study indomethacin crystallization during dissolution of partially amorphous indomethacin tablets and to (b) profile anhydrate --> hydrate transformations during dissolution of theophylline tablets. The intrinsic dissolution rates of indomethacin and theophylline were determined after different pharmaceutical processing steps. Phase transformations during dissolution were evaluated by various techniques. Transformation in the bulk and on the tablet surface was characterized by conventional XRD and scanning electron microscopy, respectively. Glancing angle XRD enabled us to profile these transformations as a function of depth from the tablet surface. Pharmaceutical processing resulted in a decrease in crystallinity of both indomethacin and theophylline. When placed in contact with the dissolution medium, while indomethacin recrystallized, theophylline anhydrate rapidly converted to theophylline monohydrate. Due to intimate contact with the dissolution medium, drug transformation occurred to a greater extent at or near the tablet surface. Glancing angle XRD enabled us to depth profile the extent of phase transformations as a function of the distance from the tablet surface. The processed sample (both indomethacin and theophylline) transformed more rapidly than did the corresponding unprocessed drug. Several challenges associated with the glancing angle technique, that is, the effects of sorbed water, phase transformations during the experimental timescale, and the influence of phase transformation on penetration depth, were addressed. Increased solubility, and consequently dissolution rate, is one of the potential advantages of metastable phases. This advantage is negated if, during dissolution, the metastable to stable transformation rate > dissolution rate. Glancing angle XRD enabled us to quantify and thereby profile phase transformations as a function of compact depth. The technique has potential utility in monitoring surface reactions, both chemical decomposition and physical transformations, in pharmaceutical systems.

Titania nanotube powders obtained by rapid breakdown anodization in perchloric acid electrolytes

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

Ali, Saima, E-mail: saima.ali@aalto.fi; Hannula, Simo-Pekka

Titania nanotube (TNT) powders are prepared by rapid break down anodization (RBA) in a 0.1 M perchloric acid (HClO{sub 4}) solution (Process 1), and ethylene glycol (EG) mixture with HClO{sub 4} and water (Process 2). A study of the as-prepared and calcined TNT powders obtained by both processes is implemented to evaluate and compare the morphology, crystal structure, specific surface area, and the composition of the nanotubes. Longer TNTs are formed in Process 1, while comparatively larger pore diameter and wall thickness are obtained for the nanotubes prepared by Process 2. The TNTs obtained by Process 1 are converted tomore » nanorods at 350 °C, while nanotubes obtained by Process 2 preserve tubular morphology till 350 °C. In addition, the TNTs prepared by an aqueous electrolyte have a crystalline structure, whereas the TNTs obtained by Process 2 are amorphous. Samples calcined till 450 °C have XRD peaks from the anatase phase, while the rutile phase appears at 550 °C for the TNTs prepared by both processes. The Raman spectra also show clear anatase peaks for all samples except the as-prepared sample obtained by Process 2, thus supporting the XRD findings. FTIR spectra reveal the presence of O-H groups in the structure for the TNTs obtained by both processes. However, the presence is less prominent for annealed samples. Additionally, TNTs obtained by Process 2 have a carbonaceous impurity present in the structure attributed to the electrolyte used in that process. While a negligible weight loss is typical for TNTs prepared from aqueous electrolytes, a weight loss of 38.6% in the temperature range of 25–600 °C is found for TNTs prepared in EG electrolyte (Process 2). A large specific surface area of 179.2 m{sup 2} g{sup −1} is obtained for TNTs prepared by Process 1, whereas Process 2 produces nanotubes with a lower specific surface area. The difference appears to correspond to the dimensions of the nanotubes obtained by the two processes. - Graphical abstract: Titania nanotube powders prepared by Process 1 and Process 2 have different crystal structure and specific surface area. - Highlights: • Titania nanotube (TNT) powder is prepared in low water organic electrolyte. • Characterization of TNT powders prepared from aqueous and organic electrolyte. • TNTs prepared by Process 1 are crystalline with higher specific surface area. • TNTs obtained by Process 2 have carbonaceous impurities in the structure.« less

Synthesis of nanoporous carbohydrate metal-organic framework and encapsulation of acetaldehyde

NASA Astrophysics Data System (ADS)

Al-Ghamdi, Saleh; Kathuria, Ajay; Abiad, Mohamad; Auras, Rafael

2016-10-01

Gamma cyclodextrin (γ-CD) metal organic frameworks (CDMOFs) were synthesized by coordinating γ-CDs with potassium hydroxide (KOH), referred hereafter as CDMOF-a, and potassium benzoate (C7H5KO2), denoted as CDMOF-b. The obtained CDMOF structures were characterized using nitrogen sorption isotherm, thermo-gravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). High surface areas were achieved by the γ-CD based MOF structures where the Langmuir specific surface areas (SSA) of CDMOF-a and CDMOF-b were determined as 1376 m2 g-1 and 607 m2 g-1; respectively. The dehydrated CDMOF structures demonstrated good thermal stability up to 250 °C as observed by the TGA studies. XRD results for CDMOF-a and CDMOF-b reveal a body centered-cubic (BCC) and trigonal crystal system; respectively. Due to its accessible porous structure and high surface area, acetaldehyde was successfully encapsulated in CDMOF-b. During the release kinetic studies, we observed peak release of 53 μg of acetaldehyde per g of CDMOF-b, which was 100 times greater than previously reported encapsulation in β-CD. However, aldol condensation reaction occurred during encapsulation of acetaldehyde into CDMOF-a. This research work demonstrates the potential to encapsulate volatile organic compounds in CDMOF-b, and their associated release for applications including food, pharmaceuticals and packaging.

Surface segregation of additives on SnO 2 based powders and their relationship with macroscopic properties

NASA Astrophysics Data System (ADS)

Pereira, Gilberto J.; Castro, Ricardo H. R.; Hidalgo, Pilar; Gouvêa, Douglas

2002-07-01

Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO 2 containing Fe or Mg ions by organic chemical route derived from Pechini's method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.

Mesoporous CeO2 nanoparticles synthesized by an inverse miniemulsion technique and their catalytic properties in methane oxidation

NASA Astrophysics Data System (ADS)

Nabih, Nermeen; Schiller, Renate; Lieberwirth, Ingo; Kockrick, Emanuel; Frind, Robert; Kaskel, Stefan; Weiss, Clemens K.; Landfester, Katharina

2011-04-01

Cerium(IV) oxide nanoparticles were synthesized using an inverse miniemulsion technique with cerium nitrate hexahydrate as precursor. The resulting nanocrystallites are as small as 5 nm with a specific surface area of 158 m2 g - 1 after calcination at 400 °C. With the addition of cetyltrimethylammonium bromide (CTAB) or (poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide)) triblock copolymers (PEO-PPO-PEO) as template in the miniemulsion droplets, the specific surface area can be increased up to 255 m2 g - 1. The miniemulsions were characterized by dynamic light scattering (DLS) and the obtained oxides were examined by x-ray diffraction (XRD), nitrogen sorption (BET and BJH), and transmission electron microscopy (TEM). The catalytic activity of the resulting ceria was investigated for the temperature-programmed oxidation (TPO) of methane.

Nano-Crystalline Diamond Films with Pineapple-Like Morphology Grown by the DC Arcjet vapor Deposition Method

NASA Astrophysics Data System (ADS)

Li, Bin; Zhang, Qin-Jian; Shi, Yan-Chao; Li, Jia-Jun; Li, Hong; Lu, Fan-Xiu; Chen, Guang-Chao

2014-08-01

A nano-crystlline diamond film is grown by the dc arcjet chemical vapor deposition method. The film is characterized by scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), x-ray diffraction (XRD) and Raman spectra, respectively. The nanocrystalline grains are averagely with 80 nm in the size measured by XRD, and further proven by Raman and HRTEM. The observed novel morphology of the growth surface, pineapple-like morphology, is constructed by cubo-octahedral growth zones with a smooth faceted top surface and coarse side surfaces. The as-grown film possesses (100) dominant surface containing a little amorphous sp2 component, which is far different from the nano-crystalline film with the usual cauliflower-like morphology.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

X-Ray Diffraction for In-Situ Mineralogical Analysis of Planetesimals.

NASA Astrophysics Data System (ADS)

Sarrazin, P.; Blake, D. F.; Dera, P.; Downs, R. T.; Taylor, J.

2017-12-01

X-ray diffraction (XRD) is a general purpose technique for definitive, quantitative mineralogical analysis. When combined with XRF data for sample chemistry, XRD analyses yield as complete a characterization as is possible by any spacecraft-capable techniques. The MSL CheMin instrument, the first XRD instrument flown in space, has been used to establish the quantitative mineralogy of the Mars global soil, to discover the first habitable environment on another planet, and to provide the first in-situ evidence of silicic volcanism on Mars. CheMin is now used to characterize the depositional and diagenetic environments associated with the mudstone sediments of lower strata of Mt. Sharp. Conventional powder XRD requires samples comprised of small grains presented in random orientations. In CheMin, sample cells are vibrated to cause loose powder to flow within the cell, driven by granular convection, which relaxes the requirement for fine grained samples. Nevertheless, CheMin still requires mechanisms to collect, crush, sieve and deliver samples before analysis. XTRA (Extraterrestrial Regolith Analyzer) is an evolution of CheMin intended to analyze fines in as-delivered surface regolith, without sample preparation. Fine-grained regolith coats the surfaces of most airless bodies in the solar system, and because this fraction is typically comminuted from the rocky regolith, it can often be used as a proxy for the surface as a whole. HXRD (Hybrid-XRD) is concept under development to analyze rocks or soils without sample preparation. Like in CheMin, the diffracted signal is collected with direct illumination CCD's. If the material is sufficiently fine-grained, a powder XRD pattern of the characteristic X-ray tube emission is obtained, similar to CheMin or XTRA. With coarse grained crystals, the white bremsstrahlung radiation of the tube is diffracted into Laue patterns. Unlike typical Laue applications, HXRD uses the CCD's capability to distinguish energy and analyze the "colors" of each Laue spot, which enable phase identification. The concept was demonstrated with prototypes and dedicated crystallographic software was developed for identification the minerals responsible for the Laue patterns. High TRL subsystems are under development for future deployment opportunities of these new XRD instruments.

Study the oxidation kinetics of uranium using XRD and Rietveld method

NASA Astrophysics Data System (ADS)

Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

2010-03-01

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

Polythiophene nanocomposites as high performance electrode material for supercapacitor application

NASA Astrophysics Data System (ADS)

Vijeth, H.; Niranjana, M.; Yesappa, L.; Ashokkumar, S. P.; Devendrappa, H.

2018-04-01

A polythiophene-aluminium oxide nanocomposite is prepared by in situ chemical polymerisation in presence of anionic surfactant camphor sulfonic acid (CSA). The characterisation of nano composite was done by X-ray Diffraction (XRD), surface morphology was studied using Atomic Force Microscopy (AFM). The electrochemical performance is evaluated using cyclic voltammetry in 1M H2SO4. As an electroactive material, it exhibits high specific capacitance of 654.5 and 757 F/g for PTH and PTHA nanocomposites at scan rate of 30mV s-1 respectively.

Structure, morphology and reducibility of ceria-doped zirconia

NASA Astrophysics Data System (ADS)

Aribi, Koubra; Soltani, Zohra; Ghelamallah, Madani; Granger, Pascal

2018-03-01

Zr1-xCexOx has been prepared by hydrolysis, in neutral medium, starting from rough ZrO2 and CeO2 materials as simple and cheaper synthesis method compared to sol-gel routes. The oxy-hydroxide precursors thus obtained were calcined under air at 450 °C, 900 °C and 1200 °C. The impact of those thermal treatments on the structure, texture and related redox properties has been investigated. Higher specific surface area than those observed on ceria were observed after calcination at low temperature, i.e., 450 °C. Above that temperature thermal sintering occurs having a detrimental effect on the specific surface area related to crystal growth more accentuated on CeO2. The formation of several Zrsbnd Ce mixed oxide phases formed by incorporation and substitution of Zr in the structure of ceria was characterized. A complete loss of specific surface area is noticeable after calcination at 1200 °C. XRD and SEM analysis revealed the formation of two mixed oxides structure, i.e. Ce2Zr2O7.04 and Ce2Zr2O7 corresponding to different redox behavior evidenced from H2-TPR experiments.

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods

NASA Astrophysics Data System (ADS)

Sivakami, R.; Dhanuskodi, S.; Karvembu, R.

2016-01-01

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55 eV. BET measurements show a high specific surface area (SSA) of 118-133 m2/g and pore diameter (10-25 nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM.

Tailoring surface and photocatalytic properties of ZnO and nitrogen-doped ZnO nanostructures using microwave-assisted facile hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rangel, R.; Cedeño, V.; Ramos-Corona, A.; Gutiérrez, R.; Alvarado-Gil, J. J.; Ares, O.; Bartolo-Pérez, P.; Quintana, P.

2017-08-01

Microwave hydrothermal synthesis, using an experimental 23 factorial design, was used to produce tunable ZnO nano- and microstructures, and their potential as photocatalysts was explored. Photocatalytic reactions were conducted in a microreactor batch system under UV and visible light irradiation, while monitoring methylene blue degradation, as a model system. The variables considered in the microwave reactor to produce ZnO nano- or microstructures, were time, NaOH concentration and synthesis temperature. It was found that, specific surface area and volume/surface area ratio were affected as a consequence of the synthesis conditions. In the second stage, the samples were plasma treated in a nitrogen atmosphere, with the purpose of introducing nitrogen into the ZnO crystalline structure. The central idea is to induce changes in the material structure as well as in its optical absorption, to make the plasma-treated material useful as photocatalyst in the visible region of the electromagnetic spectrum. Pristine ZnO and nitrogen-doped ZnO compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (BET), XPS, and UV-Vis diffuse reflectance spectroscopy. The results show that the methodology presented in this work is effective in tailoring the specific surface area of the ZnO compounds and incorporation of nitrogen into their structure, factors which in turn, affect its photocatalytic behavior.

Li3PO4 surface coating on Ni-rich LiNi0.6Co0.2Mn0.2O2 by a citric acid assisted sol-gel method: Improved thermal stability and high-voltage performance

NASA Astrophysics Data System (ADS)

Lee, Suk-Woo; Kim, Myeong-Seong; Jeong, Jun Hui; Kim, Dong-Hyun; Chung, Kyung Yoon; Roh, Kwang Chul; Kim, Kwang-Bum

2017-08-01

A surface coating of Li3PO4 was applied to a Ni-rich LiNi0.6Co0.2Mn0.2O2 (NCM) material to improve its thermal stability and electrochemical properties via a citric acid assisted sol-gel method. The addition of citric acid effectively suppressed the instant formation of Li3PO4 in solution, resulting in successful coating of the NCM surface. The improved thermal stability of NCM after Li3PO4 surface coating was demonstrated by differential scanning calorimetry (DSC) analysis and in situ time-resolved X-ray diffraction (TR-XRD). In particular, the TR-XRD results showed that the improved thermal stability after Li3PO4 surface coating originates from suppression of the phase transition of charged NCM at high temperatures. Furthermore, the charge-discharge tests demonstrated that Li3PO4-coated LiNi0.6Co0.2Mn0.2O2 (LP-NCM) has excellent electrochemical properties. LP-NCM exhibited a specific capacity of 192.7 mAh g-1, a capacity retention of 44.1% at 10 C, and a capacity retention of 79.7% after 100 cycles at a high cut-off voltage of 4.7 V; these values represent remarkably improved electrochemical properties compared with those of bare NCM. These improved thermal and electrochemical properties were mainly attributed to the improvement of the structural stability of the material and the suppression of the interface reaction between the cathode and the electrolyte owing to the Li3PO4 coating.

Self-assembled spongy-like MnO2 electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Dong, Meng; Zhang, Yu Xin; Song, Hong Fang; Qiu, Xin; Hao, Xiao Dong; Liu, Chuan Pu; Yuan, Yuan; Li, Xin Lu; Huang, Jia Mu

2012-08-01

Mesoporous spongy-like MnO2 has been synthesized via a facile and biphasic wet method, accompanied with tetraoctylammonium bromide (TOAB) as a soft template under ambient condition. A well-defined spongy morphology of MnO2 with uniform filament diameters 10-20 nm have been observed by FESEM, TEM, HRTEM, XRD, FT-IR,TGA-DSC studies. Further physical characterizations revealed that MnO2 sponges owned a large surface area of 155 m2 g-1 with typical mesoporous appearance. A specific capacitance value as high as 336 F g-1 was obtained. This improved capacitive behavior was attributed to the large surface area, morphology nature of nano-MnO2, and its broad pore size distribution.

Maltodextrin: A consummate carrier for spray-drying of xylooligosaccharides.

PubMed

Zhang, Liangqing; Zeng, Xianhai; Fu, Nan; Tang, Xing; Sun, Yong; Lin, Lu

2018-04-01

The aim of this study was to evaluate the influence of spray-drying on the powder qualities and microstructures of prebiotic xylooligosaccharides (XOS). The relationships between glass transition temperature (T g ) and XOS retention, moisture content, drying yield as well as specific surface area under different inlet air temperatures and maltodextrin concentrations were investigated. Antioxidant activity retention, hygroscopicity, color attributes, X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR) of the spray-dried XOS product were also assessed. The results indicated that an increase in inlet air temperature decreased the moisture content, hence the T g value was increased. Higher maltodextrin concentration increased the T g value, and was attributed to the molecular weight increase. The wall deposition was a tendency to occur when the temperature beyond the T g , reduced the drying yield. Higher temperature and wall deposition promoted the decomposition of XOS into monosaccharide. The crust formation rate of droplets and stickiness of microparticles were affected by T g , and hence, influenced the specific surface area. The antioxidant activity retention of XOS exhibited a concentration-dependent behavior. The hygroscopicity of the microparticles could be reduced by both of the low inlet air temperature and high maltodextrin concentration. According to the results of color attributes, XRD and SEM, the particles were colorless and amorphous, and tended to become more spherical and scattered with the addition of maltodextrin. The FT-IR analysis confirmed that no chemical reaction occurred between XOS and agent, which indicated that maltodextrin is a promising carrier for producing bioactive XOS powder. Copyright © 2018 Elsevier Ltd. All rights reserved.

Facile Synthesis of Self-Assembled Flower-Like Mesoporous Zinc Oxide Nanoflakes for Energy Applications

NASA Astrophysics Data System (ADS)

Saranya, P. E.; Selladurai, S.

Flower-shaped self-assembled zinc oxide (ZnO) nanoflakes were successfully synthesized via a temperature-controlled hydrothermal method. The crystallinity and phase formation of the compound were determined from powder X-ray diffraction (PXRD) result. Surface morphology investigations reveal the self-assembled ZnO nanoflakes to form a spherical flower-like structure. In addition, the particle size was determined from high-resolution transmission electron microscope measurement as 18nm which is in accord with XRD and UV results. X-ray photo electron spectroscopy studies reveal the chemical composition and oxidation state of the ZnO nanoparticle. The specific surface area was calculated, and mesoporous nature was confirmed using Brunauer-Emmett-Teller analysis. Results support the superior interaction between the electrode and electrolyte ions through surface pores. Capacitive performance of the ZnO electrode material was determined using cyclic voltammetry and galvanostatic charge/discharge studies, and a maximum specific capacitance of 322F/g was obtained at 5mV/sec. Electrochemical impedance spectrum reveals the materials fast charge transfer kinetics.

Synthesis of LaVO4/TiO2 heterojunction nanotubes by sol-gel coupled with hydrothermal method for photocatalytic air purification.

PubMed

Zou, Xuejun; Li, Xinyong; Zhao, Qidong; Liu, Shaomin

2012-10-01

With the aim of improving the effective utilization of visible light, the LaVO(4)/TiO(2) heterojunction nanotubes were fabricated by sol-gel coupled with hydrothermal method. The photocatalytic ability was demonstrated through catalytic removal of gaseous toluene species. The nanotube samples were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), surface photovoltage (SPV), Raman spectra and N(2) adsorption-desorption measurements. The characterization results showed that the samples with high specific surface areas were of typical nanotubular morphology, which would lead to the high separation and transfer efficiency of photo induced electron-hole pairs. The as-prepared nanotubes exhibited high photocatalytic activity in decomposing toluene species under visible light irradiation with fine photochemical stability. The enhanced photocatalytic performance of LaVO(4)/TiO(2) nanotubes might be attributed to the matching band potentials, the interconnected heterojunction of LaVO(4) versus TiO(2), and the large specific surface areas of nanotubes. Copyright © 2012 Elsevier Inc. All rights reserved.

Synthesis and characterization of TiO2/graphitic carbon nanocomposites with enhanced photocatalytic performance

NASA Astrophysics Data System (ADS)

Wanag, Agnieszka; Kusiak-Nejman, Ewelina; Kowalczyk, Łukasz; Kapica-Kozar, Joanna; Ohtani, Bunsho; Morawski, Antoni W.

2018-04-01

In this paper titanium dioxide carbon modification with benzene as a carbon source is presented. A TiO2/graphitic carbon nanocomposites were synthesized by thermal modification in the presence of benzene vapours at different temperature (300-700 °C). The new materials were characterized by a various techniques, such as: X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (UV-vis/DR), surface-enhanced Raman spectroscopy. BET specific surface area was also measured. The photocatalytic activity of obtained nanocomposites was measured by the decomposition of acetic acid and methylene blue under UV-vis irradiation. The results show that photocatalytic activity increasing with increase in carbon concentration and temperature of modification. It can be noted that adsorption degree has a very high impact on methylene blue decomposition. The highest photocatalytic activity was found for the photocatalyst modified at 600 °C contains 1.13 wt% of carbon. It should be noted that, the influence of crystallite size, crystal structure changes and specific surface area for photocatalytic activity are presented.

Biocompatible polyurethane/thiacalix[4]arenes functionalized Fe3O4 magnetic nanocomposites: Synthesis and properties.

PubMed

Mohammadi, Abbas; Barikani, Mehdi; Lakouraj, Moslem Mansour

2016-09-01

In this study, a series of magnetic polyurethane/Fe3O4 elastomer nanocomposites were prepared by covalently embedding novel thiacalix[4]arenes (TC4As) functionalized Fe3O4 nanoparticles (TC4As-Fe3O4) which contain macrocycles with reactive hydroxyl groups. Surface functionalization of Fe3O4 nanoparticles with TC4As macrocycles as unique reactive surface modifier not only gives specific characteristics to Fe3O4 nanoparticles but also improves the interphase interaction between nanoparticles and the polyurethane matrices through covalent attachment of polymer chains to nanoparticle surfaces. The novel synthesized TC4As-Fe3O4 nanoparticles were characterized by FTIR, XRD, TGA, VSM and SEM analysis. Furthermore, the effect of functionalization of Fe3O4 nanoparticles on the various properties of resulting nanocomposites was studied by XRD, TGA, DMTA, SEM, and a universal tensile tester. It was found that the functionalization of nanoparticles with TC4As affords better mechanical and thermal properties to polyurethane nanocomposites in comparison with unmodified nanoparticles. The SEM analysis showed finer dispersion of TC4As-Fe3O4 nanoparticles than unmodified Fe3O4 nanoparticles within the polyurethane matrices, which arising from formation of covalent bonding between TC4As functionalized Fe3O4 nanoparticles and polyurethane matrices. Moreover, the investigation of in vitro biocompatibility of novel nanocomposites showed that these samples are excellent candidate for biomedical use. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Pariona, Moises Meza, E-mail: mmpariona@uepg.br; Teleginski, Viviane; Santos, Kelly dos

Laser beam welding has recently been incorporated into the fabrication process of aircraft and automobile structures. Surface roughness is an important parameter of product quality that strongly affects the performance of mechanical parts, as well as production costs. This parameter influences the mechanical properties such as fatigue behavior, corrosion resistance, creep life, etc., and other functional characteristics such as friction, wear, light reflection, heat transmission, lubrification, electrical conductivity, etc. The effects of laser surface remelting (LSR) on the morphology of Al-Fe aerospace alloys were examined before and after surface treatments, using optical microscopy (OM), scanning electron microscopy (SEM), low-angle X-raymore » diffraction (LA-XRD), atomic force microscopy (AFM), microhardness measurements (Vickers hardness), and cyclic voltammetry. This analysis was performed on both laser-treated and untreated sanded surfaces, revealing significant differences. The LA-XRD analysis revealed the presence of alumina, simple metals and metastable intermetallic phases, which considerably improved the microhardness of laser-remelted surfaces. The morphology produced by laser surface remelting enhanced the microstructure of the Al-Fe alloys by reducing their roughness and increasing their hardness. The treated surfaces showed passivity and stability characteristics in the electrolytic medium employed in this study. - Highlights: Black-Right-Pointing-Pointer The samples laser-treated and untreated showed significant differences. Black-Right-Pointing-Pointer The La-XRD revealed the presence of alumina in Al-1.5 wt.% Fe. Black-Right-Pointing-Pointer The laser-treated reducing the roughness and increasing the hardness. Black-Right-Pointing-Pointer The laser-treated surfaces showed characteristic passive in the electrolytic medium. Black-Right-Pointing-Pointer The laser-treated is a promising technique for applications technological.« less

Study on the surface sulfidization behavior of smithsonite at high temperature

NASA Astrophysics Data System (ADS)

Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

2018-04-01

Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

Surface modification of hydroxyapatite nanoparticles by poly( L-phenylalanine) via ROP of L-phenylalanine N-carboxyanhydride (Pha-NCA)

NASA Astrophysics Data System (ADS)

Dai, Yanfeng; Xu, Min; Wei, Junchao; Zhang, Haobin; Chen, Yiwang

2012-01-01

The surface of hydroxyapatite nanoparticles was modified by poly(L-phenylalanine) via the ring opening polymerization (ROP) of L-phenylalanine N-carboxyanhydride. The preparation procedure was monitored by Fourier transform infrared spectroscopy (FTIR), and the modified hydroxyapatite was characterized by thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). The results showed that the surface grafting amounts of poly(L-phenylalanine) on HA ranging from 20.26% to 38.92% can be achieved by tuning the reaction condition. The XRD patterns demonstrated that the crystalline structure of the modified hydroxyapatite was nearly the same with that of HA, implying that the ROP was an efficient surface modification method. The MTT assay proved that the biocompatibility of modified HA was very good, which showed the potential application of modified HA in bone tissue engineering.

SILAR derived CdO films: Effect of triethanolamine on the surface morphology and optical bandgap energy

NASA Astrophysics Data System (ADS)

Sahin, B.; Aydin, R.

2018-07-01

Nanostructured CdO films have been successfully synthesized with different ratios of surfactant triethanolamine (TEA) under SILAR condition. The influence of addition of TEA on the physical properties of CdO nanoparticles was studied. The surface morphology of the films was studied by metallurgical microscope and SEM analysis. Surface topography of the film was studied by AFM. The structural properties of the samples were studied by X-ray diffraction (XRD). The XRD studies confirm that the deposited CdO films has cubic structure (111) preferred orientation with well-crystallinity and purity. The optical bandgap energy was estimated based on the UV-vis spectroscopies which were obtained in the range of 2.16 eV-2.46 eV. Our study is encouraging to get enhanced surface topography by surfactant TEA.

Development and surface characterization of a glucose biosensor based on a nanocolumnar ZnO film

NASA Astrophysics Data System (ADS)

Rodrigues, A.; Castegnaro, M. V.; Arguello, J.; Alves, M. C. M.; Morais, J.

2017-04-01

Highly oriented nanostructured ZnO films were grown on the surface of stainless steel plates (ZnO/SS) by chemical bath deposition (CBD). The films consisted of vertically aligned ZnO nanocolumns, ∼1 μm long and ∼80 nm wide, as observed by SEM (scanning electron microscopy) and FIB (focused ion beam). XRD (X-ray diffraction) confirmed the c-axis preferred orientation of the ZnO columns, which were functionalized with the glucose oxidase (GOx) enzyme into a biosensor of glucose. The electrochemical response studied by CV (cyclic voltammetry) proved that the biosensor was capable of detecting glucose from 1.5 up to 16 mM concentration range. XPS (X-ray photoelectron spectroscopy) analysis, excited with synchrotron radiation, probed the atom specific chemical environment at the electrode's surface and shed some light on the nature of the ZnO-GOx interaction.

Preparation of TiO2-SiO2 via sol-gel method: Effect of Silica precursor on Catalytic and Photocatalytic properties

NASA Astrophysics Data System (ADS)

Fatimah, I.

2017-02-01

TiO2-SiO2have been synthesized by the sol-gel method from titanium isopropoxide and varied silica precursors: tetraethyl orthosilicate and tetra methyl ortho silicate. To study the effect of the precursor, prepared materials were characterized by X-ray diffraction, scanning electron microscopy, Diffuse Reflectance UV-vis optical absorption, and also gas sorption analysis. XRD patterns showed the formation of TiO2 anatase in the TiO2-SiO2 composite with different crystallite size from different silica precursor as well as the different surface morphology. The DRUV-vis absorption spectra exhibit similar band gap energy correspond to 3.21eV value while the surface area, pore volume and pore radius of the materials seems to be affected by the precursor. The higher specific surface area contributes to give the enhanced activity in phenol hydroxylation and methylene blue photodegradation.

Synthesis and properties of ternary mixture of nickel/cobalt/tin oxides for supercapacitors

NASA Astrophysics Data System (ADS)

Ferreira, C. S.; Passos, R. R.; Pocrifka, L. A.

2014-12-01

The present study reports the synthesis and morphological, structural and electrochemical characterization of ternary oxides mixture containing nickel, cobalt and tin. The ternary oxide is synthesized by Pechini method with subsequent deposition onto a titanium substrate in a thin-film form. XRD and EDS analysis confirm the formation of ternary film with amorphous nature. SEM analysis show that cracks on the film favor the gain of the surface area that is an interesting feature for electrochemical capacitors. The ternary film is investigated in KOH electrolyte solution using cyclic voltammetry and charge-discharge study with a specific capacitance of 328 F g-1, and a capacitance retention of 86% over 600 cycles. The values of specific power and specific energy was 345.7 W kg-1 and 18.92 Wh kg-1, respectively.

Experimental study on the effect of calcination on the volcanic ash activity of diatomite

NASA Astrophysics Data System (ADS)

Xiao, Liguang; Pang, Bo

2017-09-01

The volcanic ash activity of diatomite was studied under the conditions of aerobic calcination and vacuum calcination by the combined water rate method, it was characterized by XRD, BET and SEM. The results showed that the volcanic ash activity of diatomite under vacuum conditions was higher than that of aerobic calcination, 600°C vacuum calcination 2h, the combined water rate of diatomite-Ca(OH)2-H2O system was increased from 6.24% to 71.43%, the volcanic ash activity reached the maximum value, the specific surface

Spectroscopic study on variations in illite surface properties after acid-base titration.

PubMed

Liu, Wen-xin; Coveney, R M; Tang, Hong-xiao

2003-07-01

FT-IR, Raman microscopy, XRD, 29Si and 27Al MAS NMR, were used to investigate changes in surface properties of a natural illite sample after acid-base potentiometric titration. The characteristic XRD lines indicated the presence of surface Al-Si complexes, preferable to Al(OH)3 precipitates. In the microscopic Raman spectra, the vibration peaks of Si-O and Al-O bonds diminished as a result of treatment with acid, then increased after hydroxide back titration. The varied ratio of signal intensity between (IV)Al and (VI)Al species in 27Al MAS NMR spectra, together with the stable BET surface area after acidimetric titration, suggested that edge faces and basal planes in the layer structure of illite participated in dissolution of structural components. The combined spectroscopic evidence demonstrated that the reactions between illite surfaces and acid-leaching silicic acid and aluminum ions should be considered in the model description of surface acid-base properties of the aqueous illite.

Synthesis of porous NiO/CeO2 hybrid nanoflake arrays as a platform for electrochemical biosensing

NASA Astrophysics Data System (ADS)

Cui, Jiewu; Luo, Jinbao; Peng, Bangguo; Zhang, Xinyi; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Zheng, Hongmei; Shu, Xia; Wu, Yucheng

2015-12-01

Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing.Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing. Electronic supplementary information (ESI) available: Optical photographs of the as-prepared samples, SEM, TEM, EDS, XRD and BET data of the samples are presented, I-t curves of glucose biosensors based on NiO and NiO/CeO2 NFAs, EIS results of different electrodes. See DOI: 10.1039/c5nr05924k

Microstructure and thermal conductivity of surfactant-free NiO nanostructures

NASA Astrophysics Data System (ADS)

Sahoo, Pranati; Misra, Dinesh K.; Salvador, Jim; Makongo, Julien P. A.; Chaubey, Girija S.; Takas, Nathan J.; Wiley, John B.; Poudeu, Pierre F. P.

2012-06-01

High purity, nanometer sized surfactant-free nickel oxide (NiO) particles were produced in gram scale using a solution combustion method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), gas pycnometry and gas adsorption analysis (BET). The average particle size of the as-synthesized NiO increases significantly with the preheating temperature of the furnace, while the specific surface area decreases. A BET specific surface area of ∼100 m2/g was obtained for NiO nanoparticles with size as small as 3 nm synthesized at 300 °C. The thermal conductivity (κ) of pressed pellets of the synthesized NiO nanoparticles obtained using spark plasma sintering (SPS) and uniaxial hot pressing is drastically decreased (∼60%) compared to that of NiO single crystal. This strong reduction in κ with particle size suggests the suitability of the synthesized surfactant-free NiO nanoparticles for use as nanoinclusions when designing high performance materials for waste heat recovery.

Facile hydrothermal synthesis of mesoporous In2O3 nanoparticles with superior formaldehyde-sensing properties

NASA Astrophysics Data System (ADS)

Zhang, Su; Song, Peng; Yang, Zhongxi; Wang, Qi

2018-03-01

Mesoporous In2O3 nanoparticles were successfully synthesized via a facile, template free, and low-cost hydrothermal method. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG), and N2 adsorption-desorption analyses. The results reveal that mesoporous In2O3 nanoparticles with a size range of 40-60 nm, possess plenty of pores, and average pore size is about 5 nm. Importantly, the mesoporous structure, large specific surface area, and small size endow the mesoporous In2O3 nanoparticles with highly sensing performance for formaldehyde detection. The response value to 10 ppm HCHO is 20 at an operating temperature of 280 °C, and the response and recovery time are 4 and 8 s, respectively. It is expected that the mesoporous In2O3 nanoparticles with large specific surface area and excellent sensing properties will become a promising functional material in monitoring and detecting formaldehyde.

Titania nanotube powders obtained by rapid breakdown anodization in perchloric acid electrolytes

NASA Astrophysics Data System (ADS)

Ali, Saima; Hannula, Simo-Pekka

2017-05-01

Titania nanotube (TNT) powders are prepared by rapid break down anodization (RBA) in a 0.1 M perchloric acid (HClO4) solution (Process 1), and ethylene glycol (EG) mixture with HClO4 and water (Process 2). A study of the as-prepared and calcined TNT powders obtained by both processes is implemented to evaluate and compare the morphology, crystal structure, specific surface area, and the composition of the nanotubes. Longer TNTs are formed in Process 1, while comparatively larger pore diameter and wall thickness are obtained for the nanotubes prepared by Process 2. The TNTs obtained by Process 1 are converted to nanorods at 350 °C, while nanotubes obtained by Process 2 preserve tubular morphology till 350 °C. In addition, the TNTs prepared by an aqueous electrolyte have a crystalline structure, whereas the TNTs obtained by Process 2 are amorphous. Samples calcined till 450 °C have XRD peaks from the anatase phase, while the rutile phase appears at 550 °C for the TNTs prepared by both processes. The Raman spectra also show clear anatase peaks for all samples except the as-prepared sample obtained by Process 2, thus supporting the XRD findings. FTIR spectra reveal the presence of O-H groups in the structure for the TNTs obtained by both processes. However, the presence is less prominent for annealed samples. Additionally, TNTs obtained by Process 2 have a carbonaceous impurity present in the structure attributed to the electrolyte used in that process. While a negligible weight loss is typical for TNTs prepared from aqueous electrolytes, a weight loss of 38.6% in the temperature range of 25-600 °C is found for TNTs prepared in EG electrolyte (Process 2). A large specific surface area of 179.2 m2 g-1 is obtained for TNTs prepared by Process 1, whereas Process 2 produces nanotubes with a lower specific surface area. The difference appears to correspond to the dimensions of the nanotubes obtained by the two processes.

Effect of H2O on the morphological changes of KNO3 formed on K2O/Al2O3 NOx storage materials: Fourier transform infra-red (FTIR) and time-resolved x-ray diffraction (TR-XRD) studies

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

Kim, Do Heui; Mudiyanselage, Kumudu K.; Szanyi, Janos

Based on combined FTIR and XRD studies, we report here that H2O induces a morphological change of KNO3 species formed on model K2O/Al2O3 NOx storage-reduction catalysts. Specifically as evidenced by FTIR, the contact of H2O with NO2 pre-adsorbed on K2O/Al2O3 promotes the transformation from bidentate (surface-like) KNO3 species to ionic (bulk-like) ones irrespective of K loadings. Once H2O is removed from the sample, a reversible transformation into bidentate KNO3 is observed, demonstrating a significant dependence of H2O on such morphological changes. TR-XRD results show the formation of two different types of bulk KNO3 phases (orthorhomobic and rhombohedral) in an as-impregnatedmore » sample. Once H2O begins to desorb above 400 K, the former is transformed into the latter, resulting in the existence of only the rhombohedral KNO3 phase. On the basis of consistent FTIR and TR-XRD results, we propose a model for the morphological changes of KNO3 species with respect to NO2 adsorption/desorption, H2O and/or heat treatments. Compared with the BaO/Al2O3 system, K2O/Al2O3 shows some similarities with respect to the formation of bulk nitrates upon H2O contact. However, there are significant differences that originate from the lower melting temperature of KNO3 relative to Ba(NO3)2.« less

Residual stresses in continuous graphite fiber Al metal matrix composites

NASA Technical Reports Server (NTRS)

Park, Hun Sub; Zong, Gui Sheng; Marcus, Harris L.

1988-01-01

The residual stresses in graphite fiber reinforced aluminum (Gr/Al) composites with various thermal histories are measured using X-ray diffraction (XRD) methods. The XRD stress analysis is based on the determination of lattice strains by precise measurements of the interplanar spacings in different directions of the sample. The sample is a plate consisting of two-ply P 100 Gr/Al 6061 precursor wires and Al 6061 overlayers. Prior to XRD measurement, the 6061 overlayers are electrochemically removed. In order to calibrate the relationship between stress magnitude and lattice spacing shift, samples of Al 6061 are loaded at varying stress levels in a three-point bend fixture, while the stresses are simultaneously determined by XRD and surface-attached strain gages. The stresses determined by XRD closely match those determined by the strain gages. Using these calibrations, the longitudinal residual stresses of P 100 Gr/Al 6061 composites are measured for various heat treatments, and the results are presented.

In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

1996-01-01

Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a pinhole camera (transmission geometry, flat two-dimensional detector perpendicular to the direct beam), the instrument (which we call CHEMIN, for Chemistry and Mineralogy) uses an X-ray sensitive CCD detector which will allow concurrent positional and energy-dispersive analysis of collected photons. Thus XRF (energy) and XRD (geometry) analysis of transmitted X-rays will be performed at the same time. Tests performed with single minerals and simple mixtures give promising results. Refinements of the prototype promise interpretable results on complex samples.

The Structure and Infrastructure of the Global Nanotechnology Literature

DTIC Science & Technology

2005-01-01

transmiss.electron.microscopi 1.3%, morpholog 1.2%, zn 1.0%, cd 1.0%, microscopi 1.0%, synthesi 0.9%, diffract.xrd 0.8%, electron 0.8%, powder 0.8%, surfact 0.8...film 2.3%, product 2.3%, hydrotherm 1.1%, tem 1.0%, synthes 0.9%, reaction 0.9%, xrd 0.9%, layer 0.8%, zn 0.8%, surfac 0.7%, cd 0.7%, magnet 0.7...0.5%, sol.gel 0.5%, thick 0.5%, materi 0.5%, laser 0.5%, reaction 0.5%, capac 0.4%, synthesi 0.4%, thin 0.4%, surfac 0.4%, nanowir 0.4%, nanoparticl

Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Feldman, S. M.; Blake, D. F.; Sarrazin, P.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

2004-01-01

The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

Martensitic phase transformations in the nanostructured surface layers induced by mechanical attrition treatment

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

Ni Zhichun; Wang Xiaowei; Wu Erdong

2005-12-01

Conversion electron Moessbauer spectroscopy (CEMS) and x-ray diffraction (XRD) analysis have been used to investigate the relationship between characteristics of phase transformation and the treatment time in surface nanocrystallized 316L stainless steel induced by surface mechanical attrition treatment (SMAT). A similar trend of development of the martensitic phase upon the treatment time has been observed from both CEMS and XRD measurements. However, in the CEMS measurement, two types of martensite phase with different magnetic hyperfine fields are revealed. Based on a random distribution of the non-iron coordinating atoms, a three-element theoretical model is developed to illustrate the difference of twomore » types of martensite phase. The calculated results indicate the segregation of the non-iron atoms associated with SMAT treatment.« less

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.

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.

Effective reduction in the nanoparticle sizes of NiO obtained via the pyrolysis of nickel malonate precursor modified using oleylamine surfactant

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

Lontio Fomekong, Roussin, E-mail: lonforou@yahoo.fr; Institut de la Matière Condensée et des Nanosciences, Université Catholique de Louvain, Croix du Sud 1, 1348 Louvain-La-Neuve; Ngolui Lambi, John

2016-09-15

Nickel oxide nanoparticles were synthesized via thermal decomposition of two precursors, the first, a simple nickel malonate and the second, a nickel malonate modified by oleylamine, a surfactant, both having been synthesized by precipitation. While FTIR, TGA and ToF-SIMS were used to characterize the two precursors and to show the presence of oleylamine in the modified precursor, XRD, SEM, TEM and BET were employed to investigate the structure, the morphology and the specific surface area of the decomposition products obtained after pyrolysis. The results showed that the modification of nickel malonate by oleylamine was effective. The XRD results, which showedmore » a cubic structure for the NiO obtained, suggest with SEM an important particle size reduction (at least 54%) when oleylamine was used to modify the nickel malonate precursor. The SEM images also showed a well-defined spherical nanoparticle morphology in both cases, not affected by the presence of oleylamine. The TEM also confirmed the reduction of particle size and their spherical nature but at the same time showed that, in the presence of oleylamine, there was no agglomeration resulting in a more uniform particle size distribution. The specific surface area of the NiO obtained by the oleylamine-modified precursor was 4.7 times larger than that obtained with the regular precursor. This again confirms the particle size reduction. - Highlights: • Nickel malonate precursor has been synthesized by precipitation method. • This precursor was successfully modified by a surfactant (oleylamine). • NiO was identified as the decomposition products of the previous precursors. • Oleylamine has provoked around 54% of particle size reduction of the NiO.« less

Kaolinite-supported nanoscale zero-valent iron for removal of Pb2+ from aqueous solution: reactivity, characterization and mechanism.

PubMed

Zhang, Xin; Lin, Shen; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravendra

2011-05-01

The use of nanoscale zero-valent iron (nZVI) to remediate contaminated groundwater is limited due to its lack of durability and mechanical strength. To address this issue, 20% (w/w) nZVI was loaded onto kaolinite as a support material (K-nZVI). More than 96% of Pb(2+) was removed from aqueous solution using K-nZVI at an initial condition of 500 mg/L Pb(2+) within 30 min under the conditions of 10 g/L of K-nZVI, pH 5.10 and a temperature of 30 °C. To understand the mechanism of removal of Pb(2+), various techniques were implemented to characterize K-nZVI. Scanning electron microscopy (SEM) indicated that K-nZVI had a suitable dispersive state with a lower aggregation, where the mean specific surface area and average particle size as determined by the BET-N(2) method and X-ray diffraction (XRD), were 26.11 m(2)/g and 44.3 nm, respectively. The results obtained from XRD, X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) indicated that a small number of iron oxides formed on the surface of K-nZVI, suggesting that free Pb(2+) was adsorbed onto K-nZVI and subsequently reduced to Pb(0). Copyright © 2011 Elsevier Ltd. All rights reserved.

Effect of oxygen partial pressure on oxidation of Mo-metal

NASA Astrophysics Data System (ADS)

Sharma, Rabindar Kumar; Kumar, Prabhat; Singh, Megha; Gopal, Pawar; Reddy, G. B.

2018-05-01

This report explains the effect of oxygen partial pressure (PO2 ) on oxidation of Mo-metal in oxygen plasma. XRD results indulge that oxide layers formed on Mo-surfaces at different oxygen partial pressures have two different oxide phases (i.e. orthorhombic MoO3 and monoclinic Mo8O23). Intense XRD peaks at high pressure (i.e. 2.0×10-1 Torr) points out the formation of thick oxide layer on Mo-surface due to presence of large oxygen species in chamber and less oxide volatilization. Whereas, at low PO2 (6.5×10-2 and 7.5×10-2 Torr.) the reduced peak strength is owing to high oxide volatilization rate. SEM micrographs and thickness measurements also support XRD results and confirm that the optimum -2value of PO2 to deposited thicker and uniform oxide film on glass substrate is 7.5×10-2 Torr through plasma assistedoxidation process. Further to study the compositional properties, EDX of the sample M2 (the best sample) is carried out, which confirms that the stoichiometric ratio is less than 3 (i.e. 2.88). Less stoichiometric ratio again confirms the presence of sub oxides in oxide layers on Mo metal as evidenced by XRD results. All the observed results are well in consonance with each other.

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

Saw, C K

To date a global kinetic rate law has not been written to accurately describe solid-solid phase transformations of HMX and TATB where contributions from grain size effects, binder contents, and impurity levels are explicitly defined. Our recent work presented at the 2001 SCCM topical APS meeting, Atlanta, GA, demonstrated one can not confidently use the second harmonic generation (SHG) diagnostic to study energetic material phase transitions where non-uniform grain size distributions are present. For example, in HMX, the early arrival of SHG before the XRD in the SHG/XRD simultaneous high temperature experiment clearly indicates the partial molecular conversion from centrosymmetricmore » to non-centrosymmetric without any structural changes as exhibit by the XRD pattern. This conversion is attributed to the changes of the surface molecules due to the differences in potential between the surface and the bulk. The present paper reports on accurate XRD measurements following changes of {beta}-HMX to {delta}-HMX at elevated temperature. The results are compared for sample with 2 different grain sizes for HMX. We report accurate temperature dependent lattice parameters and hence volume and linear thermal expansion coefficients along each crystallographic axis. We have also conducted kinetic studies of the behavior of 2 grain-sizes of HMX and concluded that their kinetics, are drastically different.« less

Improved solar-driven photocatalytic performance of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} prepared in-situ

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

Zhong, Junbo, E-mail: junbozhong@163.com; Li, Jianzhang, E-mail: lschmanuscript@163.com; Huang, Shengtian

Highlights: • Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} photocatalysts were prepared in-situ. • The photo-induced charge separation rate has been greatly increased. • The photocatalytic activity has been greatly promoted. - Abstract: Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} composites have been fabricated in-situ via a facile parallel flaw co-precipitation method. The specific surface area, structure, morphology, and the separation rate of photo-induced charge pairs of the photocatalysts were characterized by Brunauer–Emmett–Teller (BET) method, X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy(DRS), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and surface photovoltage (SPV) spectroscopy, respectively. XRD patterns and DRS demonstrated that Ag{submore » 2}CO{sub 3} has no effect on the crystal phase and bandgap of (BiO){sub 2}CO{sub 3}. The existence of Ag{sub 2}CO{sub 3} in the composites enhances the separation rate of photo-induced charge pairs of the photocatalysts. The photocatalytic performance of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} was evaluated by the decolorization of methyl orange (MO) aqueous solution under simulated solar irradiation. It was found that the simulated solar-induced photocatalytic activity of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} copmposites was significantly improved, which was mainly attributed to the enhanced surface area and the separation rate of photo-induced charge pairs.« less

Al3+ ions dependent structural and magnetic properties of Co-Ni nano-alloys.

PubMed

Kadam, R H; Alone, Suresh T; Gaikwad, Anil S; Birajdar, A P; Shirsath, Sagar E

2014-06-01

Ferrite samples with a chemical formula Co0.5Ni0.5Al(x)Fe(2-x)O4 (where x = 0.0, 0.25, 0.5, 0.75 and 1.0) were synthesized by sol-gel auto-combustion method. The synthesized samples were annealed at 600 degrees C for 4 h. An analysis of X-ray diffraction (XRD) patterns reveals the formation of single phase cubic spinel structure. The lattice parameter decreased linearly with the increasing Al content x. Nano size of the powders were confirmed by the transmission electron micrographs (TEM). Particle size, bulk density decreased whereas specific surface area and porosity of the samples increased with the Al substitution. Cation distribution of constituent ions shows linear dependence of Al substitution. Based on the cation distribution obtained from XRD data, structural parameters such as lattice parameters, ionic radii of available sites and the oxygen parameter 'u' is calculated. Saturation magnetization (M(s)), magneton number (n(B)) and coercivity (H(c)) decreased with the Al substitution. Possible explanation for the observed structural and magnetic behavior with various Al content are discussed.

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods.

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55eV. BET measurements show a high specific surface area (SSA) of 118-133m(2)/g and pore diameter (10-25nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of Carbon Nano Materials Originated from Waste Cooking Oil Using a Nebulized Spray Pyrolysis

NASA Astrophysics Data System (ADS)

Arie, A. A.; Hadisaputra, L.; Susanti, R. F.; Devianto, H.; Halim, M.; Enggar, R.; Lee, J. K.

2017-07-01

Synthesis of nanocarbon on snake fruit-peel’s activated carbon from waste cooking oil palm was conducted by a nebulized spray pyrolysis process (NSP) by varying the processing temperature from 650 to 750 °C. Ferrocene was used as a catalyst with constant concentration of 0.015 g/ml of carbon source. The structure of nanocarbon was studied by using scanning electron microscope (SEM),x-ray diffraction (XRD), surface area analyzer and Raman spectroscopy. SEM results showed that the structures of carbon products was in the the form of carbon nanopsheres (CNS). XRD and Raman analysis confirmed the CNS structure. The carbon producs were then tested as electrode’s materials for lithium ion capacitors (LIC) by cyclic voltammetry (CV) instruments. From the CV results the specific capacitance was estimated as 79.57 F / g at a scan rate of 0.1 mV / s and voltage range from 2.5 - 4 V. This study shows that the nano carbons synthesized from the waste cooking oil can be used as prospective electrode materials for LIC.

Mineralogical and morphological constraints on the reduction of Fe(III) minerals by Geobacter sulfurreducens

NASA Astrophysics Data System (ADS)

Cutting, R. S.; Coker, V. S.; Fellowes, J. W.; Lloyd, J. R.; Vaughan, D. J.

2009-07-01

The biologically-mediated reduction of synthetic samples of the Fe(III)-bearing minerals hematite, goethite, lepidocrocite, feroxhyte, ford ferrihydrite, akaganeite and schwertmannite by Geobacter sulfurreducens has been investigated using microbiological techniques in conjunction with X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). This combination of approaches offers unique insights into the influence of subtle variations in the crystallinity of a given mineral on biogeochemical processes, and has highlighted the importance of (oxyhydr)oxide crystallite morphology in determining the changes occurring in a given mineral phase. Problems arising from normalising the biological Fe(III) reduction rates relative to the specific surface areas of the starting materials are also highlighted. These problems are caused primarily by particle aggregation, and compounded when using spectrophotometric assays to monitor reduction. For example, the initial rates of Fe(III) reduction observed for two synthetic feroxyhytes with different crystallinities (as shown by XRD and TEM studies) but almost identical surface areas, differ substantially. Both microbiological and high-resolution TEM studies show that hematite and goethite are susceptible to limited amounts of Fe(III) reduction, as evidenced by the accumulation of Fe(II) during incubation with G. sulfurreducens and the growth of nodular structures on crystalline goethite laths during incubation. Lepidocrocite and akaganeite readily transform into mixtures of magnetite and goethite, and XRD data indicate that the proportion of magnetite increases within the transformation products as the crystallinity of the starting material decreases. The presence of anthraquinone-2,6-disulfonate (AQDS) as an electron shuttle increases both the initial rate and longer term extent of biological Fe(III) reduction for all of the synthetic minerals examined. High-resolution XPS indicates subtle but measurable differences in the Fe(III):Fe(II) ratios at the mineral surfaces following extended incubation. For example, for a poorly crystalline schwertmannite, deconvolution of the Fe2p 3/2 peak suggests that the Fe(III):Fe(II) ratio of the near-surface regions varies from 1.0 in the starting material to 0.9 following 144 h of incubation with G.sulfurreducens, and to 0.75 following the same incubation period in the presence of 10 μM AQDS. These results have important implications for the biogeochemical cycling of iron.

A Combined XRD/XRF Instrument for Lunar Resource Assessment

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

1992-01-01

Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of Rietveld methods for XRD data analysis can provide a powerful tool for quantitative mineralogy and for obtaining crystallographic data on complex minerals.

Fabrication and characterization of a novel hydrophobic CaCO3 grafted by hydroxylated poly(vinyl chloride) chains

NASA Astrophysics Data System (ADS)

Bao, Lixia; Yang, Simei; Luo, Xin; Lei, Jingxin; Cao, Qiue; Wang, Jiliang

2015-12-01

The hydroxylated PVC (PVC-OH) was successfully synthesized by a suspension polymerization of vinyl chloride (VC), butyl acrylate (BA) and hydroxyethyl acrylate (HEA). Novel hydrophobic CaCO3 was then prepared by a urethane formation reaction between methylene diphenyl diisocyanate (MDI) and the sbnd OH groups both in the PVC-OH chains and on the surface of pristine CaCO3 particles. The effect of the PVC-OH content on the grafting ratio of treated CaCO3 particles was extensively investigated. Combining the result of Fourier transform infrared (FTIR) with that of water contact angle, it can be concluded that the hydrophobicity of CaCO3 had been efficiently improved by the PVC-OH segments grafted on the surface of CaCO3 particles. X-ray diffraction (XRD), thermal gravity analysis (TGA), scanning electron microscope (SEM) and transmission electron microscope (TEM) were also used to study crystalline behaviors, thermal stability and surface morphology of the modified CaCO3 particles, respectively. The change of specific surface area implying surface modification was investigated as well.

Influence of surface oxygenated groups on the formation of active Cu species and the catalytic activity of Cu/AC catalyst for the synthesis of dimethyl carbonate

NASA Astrophysics Data System (ADS)

Zhang, Guoqiang; Li, Zhong; Zheng, Huayan; Hao, Zhiqiang; Wang, Xia; Wang, Jiajun

2016-12-01

Activated carbon (AC) supported Cu catalysts are employed to study the influence of surface oxygenated groups on the formation of active Cu species and the catalytic activity of Cu/AC catalyst for oxidative carbonylation of methanol to dimethyl carbonate (DMC). The AC supports are thermal treated under different temperatures in order to adjust the levels of surface oxygenated groups. The AC supports are characterized by BET, TPD-MS and XRD, and the Cu/AC catalysts are characterized by BET, XRD, TEM, XPS, AAS, CH3OH-TPD and N2O chemisorption. The results show that as the treatment temperature is below 800 °C, the BET surface area of the corresponding AC supports are nearly unchanged and close to that of the original AC (1529.6 m2/g). But as the thermal treatment temperature is elevated from 1000 to 1600 °C, the BET surface area of AC supports gradually decreases from 1407.6 to 972.2 m2/g. After loading of Cu, the BET surface area of copper catalysts is in the range of 834.4 to 1545.3 m2/g, which is slightly less than that of the respective supports. When AC is thermal treated at 400 and 600 °C, the unstable carboxylic acid and anhydrides groups are selectively removed, which has weakened the mobility and agglomeration of Cu species during the calcination process, and thus improve the Cu species dispersion over AC support. But as the treatment temperature is elevated from 600 °C to 1200 °C, the Cu species dispersion begins to decline suggesting further removal of stable surface oxygenated groups is unfavorable for Cu species dispersion. Moreover, higher thermal treatment temperature (above 1200 °C) promotes the graphitization degree of AC and leds to the decrease of Cu loading on AC support. Meanwhile, the removal of surface oxygenated groups by thermal treatment is conducive to the formation of more π-sites, and thus promote the reduction of Cu2+ to Cu+ and Cu0 as active centers. The specific surface area of (Cu+ + Cu0) is improved by thermal treatment of AC, however, the space time yield of DMC on unit specific surface area of (Cu+ + Cu0) is in the range of 23.1-49.1 mg h-1 m-2, which is much less than that (77.6 mg h-1 m-2) of the original catalyst. The possible reason is that the removal of surface oxygenated groups results in AC support transforms from hydrophilicity to hydrophobicity, which is detrimental for the adsorption of CH3OH resulting in the decreased local concentration of CH3OH on active Cu species.

Surface characterization studies of walnut-shell biochar catalysts for simultaneously removing of organic sulfur from yellow phosphorus tail gas

NASA Astrophysics Data System (ADS)

Song, Xin; Li, Kai; Ning, Ping; Wang, Chi; Sun, Xin; Tang, Lihong; Ruan, Haotian; Han, Shuang

2017-12-01

The influences of different preparation conditions for surface characteristics on removing organic sulfur were studied. From BET, XRD, FTIR, DRIFTS, TG/DTA, CO2-TPD results, it can be seen that these preparation conditions had great influences on the pore structure, specific surface area, crystal structure and surface functional groups. The micropore volume, amorphous structure and alkalinity site strength played major roles in desulfurization process. H2S was oxidized by oxygen containing functional groups, such as sbnd COO, sbnd Cdbnd O. H2O molecule could be converted into some groups, such as sbnd CH and Csbnd OH groups, and promoted the hydrolysis reaction. The strong alkalinity site was the key factor for chemical adsorption and hydrolysis. H2O molecule, sbnd CH, Csbnd OH groups promoted the hydrolysis reaction and sbnd COO, sbnd Cdbnd O groups promoted the oxidation of H2S on the surface of WSB. Meanwhile, the main desulfurization process over WSB after carbonization was adsorption and it changed to hydrolysis reaction after activation on the surface of WSB. Furthermore, the reaction mechanism was investigated by DRIFTS measurement according to the change of surface functional groups.

Unpredictable adsorption and visible light induced decolorization of nano rutile for the treatment of crystal violet

NASA Astrophysics Data System (ADS)

Dong, Yanling; Liu, Yang; Lu, Dingze; Zheng, Feng; Fang, Pengfei; Zhang, Haining

2017-04-01

Photocatalysts containing different ratios of anatase and rutile are prepared via heat treatment of Degussa P-25 titania. X-ray diffraction (XRD), Bruuauer-Emmett-Teller (BET), ultraviolet-visible light diffuse reflectance spectra (DRS), Raman spectra (Raman), positron annihilation lifetime spectra (PAL) and temperature-programmed desorption (TPD) are applied to investigate the phase composition of the synthesized catalysts. Using crystal violet (CV) as the target pollutant, the unexpected visible light decolorization of rutile is observed. Despite the decreased specific surface area, the as-synthesized rutile samples exhibit much higher adsorption capability of CV than P-25 does, which in turn leads to improved photoreaction efficiency. Since the rutile samples can't absorb the visible light, the degradation under visible light irradiation is attributed to self-sensitization of CV on the surface of rutile.

Preparation of Hierarchical Porous Silicalite-1 Encapsulated Ag NPs and Its Catalytic Performance for 4-Nitrophenol Reduction

NASA Astrophysics Data System (ADS)

Wang, Bin; Wang, Haojiang; Zhang, Fengwei; Sun, Tijian

2018-06-01

A facile and efficient strategy is presented for the encapsulation of Ag NPs within hierarchical porous silicalite-1. The physicochemical properties of the resultant catalyst are characterized by TEM, XRD, FTIR, and N2 adsorption-desorption analytical techniques. It turns out that the Ag NPs are well distributed in MFI zeolite framework, which possesses hierarchical porous characteristics (1.75, 3.96 nm), and the specific surface area is as high as 243 m2 · g-1. More importantly, such catalyst can rapidly transform the 4-nitrophenol to 4-aminophenol in aqueous solution at room temperature, and a quantitative conversion is also obtained after being reused 10 times. The reasons can be attributed to the fast mass transfer, large surface area, and spatial confinement effect of the advanced support.

A study of structural and mechanical properties of nano-crystalline tungsten nitride film synthesis by plasma focus

NASA Astrophysics Data System (ADS)

Hussnain, Ali; Singh Rawat, Rajdeep; Ahmad, Riaz; Hussain, Tousif; Umar, Z. A.; Ikhlaq, Uzma; Chen, Zhong; Shen, Lu

2015-02-01

Nano-crystalline tungsten nitride thin films are synthesized on AISI-304 steel at room temperature using Mather-type plasma focus system. The surface properties of the exposed substrate against different deposition shots are examined for crystal structure, surface morphology and mechanical properties using X-ray diffraction (XRD), atomic force microscope, field emission scanning electron microscope and nano-indenter. The XRD results show the growth of WN and WN2 phases and the development of strain/stress in the deposited films by varying the number of deposition shots. Morphology of deposited films shows the significant change in the surface structure with different ion energy doses (number of deposition shots). Due to the effect of different ion energy doses, the strain/stress developed in the deposited film leads to an improvement of hardness of deposited films.

Surface morphological properties of Ag-Al2O3 nanocermet layers using dip-coating technique

NASA Astrophysics Data System (ADS)

Muhammad, Nor Adhila; Suhaimi, Siti Fatimah; Zubir, Zuhana Ahmad; Daud, Sahhidan

2017-12-01

Ag-Al2O3 nanocermet layer was deposited on Cu coated glass substrate using dip-coating technique. The aim of this study was to observe the surface morphology properties of Ag-Al2O3 nanocermet layers after annealing process at 350°C in H2. The surface morphology of Ag-Al2O3 nanocermet will be characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and X-Ray Diffractometer (XRD), respectively. The results show that nearly isolated Ag particles having a large and small size were present in the Al2O3 dielectric matrix after annealing process. The face centered cubic crystalline structure of Ag nanoparticles inclusion in the amorphous alumina dielectric matrix was confirmed using XRD pattern and supported by EDX spectra analysis.

CuO urchin-nanostructures synthesized from a domestic hydrothermal microwave method

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

Keyson, D.; Laboratorio de Ensino de Ciencias, DME Universidade Federal da Paraiba, PB; Volanti, D.P.

This letter reports the synthesis of CuO urchin-nanostructures by a simple and novel hydrothermal microwave method. The formation and growth of urchin-nanostructures is mainly affected by the addition of polyethylene glycol (PEG). The hierarchical malachite particles are uniform spheres with a diameter of 0.7-1.9 {mu}m. CuO urchin-nanostructures were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FEG-SEM) and nitrogen adsorption (BET). The specific surface area of the CuO nanostructured microspheres was about 170.5 m{sup 2}/g. A possible mechanism for the formation of such CuO urchin-nanostructures is proposed.

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

Diagnosing x-ray power and energy of tungsten wire array z-pinch with a flat spectral response x-ray diode

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

Wang, Kun-lun; Ren, Xiao-dong; Huang, Xian-bin, E-mail: caephxb2003@aliyun.com

2015-11-15

Fast z-pinch is a very efficient way of converting electromagnetic energy to radiation. With an 8-10 MA current on primary test stand facility, about 1 MJ electromagnetic energy is delivered to vacuum chamber, which heats z-pinch plasma to radiate soft x-ray. To develop a pulsed high power x-ray source, we studied the applicability of diagnosing x-ray power from tungsten wire array z-pinch with a flat spectral response x-ray diode (FSR-XRD). The detector was originally developed to diagnose radiation of a hohlraum in SG-III prototype laser facility. It utilized a gold cathode XRD and a specially configured compound gold filter tomore » yield a nearly flat spectral response in photon energy range of 0.1-4 keV. In practice, it was critical to avoid surface contamination of gold cathode. It is illustrated that an exposure of an XRD to multiple shots caused a significant change of response. Thus, in diagnosing x-ray power and energy, we used each XRD in only one shot after calibration. In a shot serial, output of FSR-XRD was compared with output of a nickel bolometer. In these shots, the outputs agreed with each other within their uncertainties which were about 12% for FSR-XRD and about 15% for bolometer. Moreover, the ratios between the FSR-XRD and the bolometer among different shots were explored. In 8 shots, the standard deviation of the ratio was 6%. It is comparable to XRD response change of 7%.« less

Colon-specific pulsatile drug release provided by electrospun shellac nanocoating on hydrophilic amorphous composites

PubMed Central

Yu, Deng-Guang; Wang, Ke; Liu, Ping; Chen, Xiaohong

2018-01-01

Background Colon-specific pulsatile drug release, as a combined drug controlled-release model, is a useful drug delivery manner for a series of diseases. New nanomedicines and related preparation methods are highly desired. Methods With diclofenac sodium (DS) as a model drug, a new type of structural nanocomposite (SC), in which composite polyvinylpyrrolidone (PVP)–DS core was coated by shellac, was fabricated via modified coaxial electrospinning. For comparison, traditional PVP–DS monolithic hydrophilic nanocomposites (HCs) were generated using a traditional blending process. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR-FTIR), water contact angle (WCA), and in vitro dissolution and ex vivo permeation tests were conducted to characterize the composites. Results SEM images demonstrated that both composites were linear nanofibers with smooth surface morphology and cross sections. TEM disclosed that the SCs had a thin shellac sheath layer of approximately 12 nm. XRD and ATR-FTIR results demonstrated that the crystalline DS was converted into amorphous composites with PVP because of favorable secondary interactions. WCA and in vitro dissolution tests demonstrated that the sheath shellac layers in SC could resist acid conditions and provide typical colon-specific pulsatile release, rather than a pulsatile release of HC under acid conditions. Ex vivo permeation results demonstrated that the SCs were able to furnish a tenfold drug permeation rate than the DS particles on the colon membrane. Conclusion A new SC with a shellac coating on hydrophilic amorphous nanocomposites could furnish a colon-specific pulsatile drug release profile. The modified coaxial process can be exploited as a useful tool to create nanocoatings. PMID:29713169

Colon-specific pulsatile drug release provided by electrospun shellac nanocoating on hydrophilic amorphous composites.

PubMed

Yang, Yao-Yao; Liu, Zhe-Peng; Yu, Deng-Guang; Wang, Ke; Liu, Ping; Chen, Xiaohong

2018-01-01

Colon-specific pulsatile drug release, as a combined drug controlled-release model, is a useful drug delivery manner for a series of diseases. New nanomedicines and related preparation methods are highly desired. With diclofenac sodium (DS) as a model drug, a new type of structural nanocomposite (SC), in which composite polyvinylpyrrolidone (PVP)-DS core was coated by shellac, was fabricated via modified coaxial electrospinning. For comparison, traditional PVP-DS monolithic hydrophilic nanocomposites (HCs) were generated using a traditional blending process. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR-FTIR), water contact angle (WCA), and in vitro dissolution and ex vivo permeation tests were conducted to characterize the composites. SEM images demonstrated that both composites were linear nanofibers with smooth surface morphology and cross sections. TEM disclosed that the SCs had a thin shellac sheath layer of approximately 12 nm. XRD and ATR-FTIR results demonstrated that the crystalline DS was converted into amorphous composites with PVP because of favorable secondary interactions. WCA and in vitro dissolution tests demonstrated that the sheath shellac layers in SC could resist acid conditions and provide typical colon-specific pulsatile release, rather than a pulsatile release of HC under acid conditions. Ex vivo permeation results demonstrated that the SCs were able to furnish a tenfold drug permeation rate than the DS particles on the colon membrane. A new SC with a shellac coating on hydrophilic amorphous nanocomposites could furnish a colon-specific pulsatile drug release profile. The modified coaxial process can be exploited as a useful tool to create nanocoatings.

The role of advanced reactive surface area characterization in improving predictions of mineral reaction rates

NASA Astrophysics Data System (ADS)

Beckingham, L. E.; Zhang, S.; Mitnick, E.; Cole, D. R.; Yang, L.; Anovitz, L. M.; Sheets, J.; Swift, A.; Kneafsey, T. J.; Landrot, G.; Mito, S.; Xue, Z.; Steefel, C. I.; DePaolo, D. J.; Ajo Franklin, J. B.

2014-12-01

Geologic sequestration of CO2 in deep sedimentary formations is a promising means of mitigating carbon emissions from coal-fired power plants but the long-term fate of injected CO2 is challenging to predict. Reactive transport models are used to gain insight over long times but rely on laboratory determined mineral reaction rates that have been difficult to extrapolate to field systems. This, in part, is due to a lack of understanding of mineral reactive surface area. Many models use an arbitrary approximation of reactive surface area, applying orders of magnitude scaling factors to measured BET or geometric surface areas. Recently, a few more sophisticated approaches have used 2D and 3D image analyses to determine mineral-specific reactive surface areas that account for the accessibility of minerals. However, the ability of these advanced surface area estimates to improve predictions of mineral reaction rates has yet to be determined. In this study, we fuse X-ray microCT, SEM QEMSCAN, XRD, SANS, and SEM-FIB analysis to determine mineral-specific accessible reactive surface areas for a core sample from the Nagaoka pilot CO2 injection site (Japan). This sample is primarily quartz, plagioclase, smectite, K-feldspar, and pyroxene. SEM imaging shows abundant smectite cement and grain coatings that decrease the fluid accessibility of other minerals. However, analysis of FIB-SEM images reveals that smectite nano-pores are well connected such that access to underlying minerals is not occluded by smectite coatings. Mineral-specific accessible surfaces are determined, accounting for the connectivity of the pore space with and without connected smectite nano-pores. The large-scale impact of variations in accessibility and dissolution rates are then determined through continuum scale modeling using grid-cell specific information on accessible surface areas. This approach will be compared with a traditional continuum scale model using mineral abundances and common surface area estimates. Ultimately, the effectiveness of advanced surface area characterization to improve mineral dissolution rates will be evaluated by comparison of model results with dissolution rates measured from a flow-through column experiment.

Highly surface-roughened quasi-spherical silver powders in back electrode paste for silicon solar cells

NASA Astrophysics Data System (ADS)

Yin, Peng; Liu, Shouchao; Li, Qiuying; Chen, Xiaolei; Guo, Weihong; Wu, Chifei

2017-08-01

In our work, highly surface-roughened quasi-spherical silver powders with controllable size and superior dispersibility, which have narrow size distribution and relatively high tap density, were successfully prepared by reducing silver nitrate with ascorbic acid in aqueous solutions. Gum arabic (AG) was selected as dispersant to prevent the agglomeration of silver particles. Furthermore, the effects of preparation conditions on the characteristics of the powders were systematically investigated. By varying the concentration of the reactants, dosage of dispersant, the feeding modes, synthesis temperature and the pH value of the mixture solution of silver nitrate and AG, the resulted silver particles displayed controllable size, different morphologies and surface roughness. The spherical silver powder with mean particle size of 1.20 µm, tap density of 4.1 g cm-3 and specific area value of 0.46 m2 g-1 was prepared by adjusting preparation conditions. The AG absorbed on the surface preventing the silver particles from diffusion and aggregation was proved by the ultraviolet spectra. Observations of SEM images showed that the as-prepared silver powders were relatively monodisperse silver spheres with highly roughened surface and the particle size was controllable from 1 µm to 5 µm, specific surface area value from approximately 0.2 m2 g-1 to 0.8 m2 g-1. X-ray diffraction (XRD) patterns, energy dispersive spectroscopy (EDS), x-ray photoelectron spectra (XPS) and thermal gravity analysis (TGA) demonstrated high crystallinity and purity of the obtained silver powders.

Potentiometric and electrokinetic signatures of iron(II) interactions with (α,γ)-Fe2O3.

PubMed

Toczydłowska, Diana; Kędra-Królik, Karolina; Nejbert, Krzysztof; Preočanin, Tajana; Rosso, Kevin M; Zarzycki, Piotr

2015-10-21

The electrochemical signatures of Fe(II) interactions with iron(III) oxides are poorly understood, despite their importance in controlling the amount of mobilized iron. Here, we report the potentiometric titration of α,γ-Fe2O3 oxides exposed to Fe(II) ions. We monitored in situ surface and ζ potentials, the ratio of mobilized ferric to ferrous, and the periodically analyzed nanoparticle crystal structure using X-ray diffraction. Electrokinetic potential reveals weak but still noticeable specific sorption of Fe(II) to the oxide surface under acidic conditions, and pronounced adsorption under alkaline conditions that results in a surface potential reversal. By monitoring the aqueous iron(II/III) fraction, we found that the addition of Fe(II) ions produces platinum electrode response consistent with the iron solubility-activity curve. Although, XRD analysis showed no evidence of γ-Fe2O3 transformations along the titration pathway despite iron cycling between aqueous and solid reservoirs, the magnetite formation cannot be ruled out.

Synthesis and Characterization of Chitosan-p-t-Butylcalix[4]arene acid

NASA Astrophysics Data System (ADS)

Handayani, D. S.; Frimadasi, W.; Kusumaningsih, T.; Pranoto

2018-03-01

The synthesis of chitosan-p-t-butylcalix[4]arene acid was done with DIC (N, N’-diisopropylcarbodiimide) as the coupling agent. The structural analysis of the chitosan-p-t-butylcalix[4]arene acid was conducted by spectrophotometer Fourier Transform Infra Red (FTIR) and X-Ray Diffraction (XRD). Meanwhile, the surface area was investigated by Surface Area Analysis, the Scanning Electrone Microscope (SEM) analysed the surface morphology, and also the melting point temperature was determined. FTIR analysis on Chitosan-p-t-butylcalix[4]arene provides an overlapped absorption of -OH and -NH groups at 3438.26 cm-1. Meanwhile, a C = C aromatic bond present at 1480.43 cm-1. XRD analysis shows some broaden peaks due to the amorphous phase of the prepared material. The prepared material is a brownish yellow solid, odorless and porous. The melting point, surface area, and the average pore radius are above 300 °C, 9.42 m2 / g, and 52.5938 Å, respectively.

Crystal Structure Variations of Sn Nanoparticles upon Heating

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lin, Kwang-Lung

2018-04-01

Structural changes in Sn nanoparticles during heating below the melting point have been investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD) analysis, electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). DSC revealed that the heat required to melt the nanoparticles (28.43 J/g) was about half compared with Sn metal (52.80 J/g), which was attributed to the large surface energy contribution for the nanoparticles. ED and XRD analyses of the Sn nanoparticles revealed increased intensity for crystal planes having large interplaner distances compared with regular crystal planes with increasing heat treatment temperature (HTT). HRTEM revealed an increase in interlayer spacing at the surface and near joints between nanoparticles with the HTT, leading to an amorphous structure of nanoparticles at the surface at 220°C. These results highlight the changes that occur in the morphology and crystal structure of Sn nanoparticles at the surface and in the interior with increase of the heat treatment temperature.

Thickness dependence of crystal and optical characterization on ZnO thin film grown by atomic layer deposition

NASA Astrophysics Data System (ADS)

Baek, Seung-Hye; Lee, Hyun-Jin; Lee, Sung-Nam

2018-06-01

We studied the thickness dependence of the crystallographic and optical properties of ZnO thin films grown on c-plane sapphire substrate using atomic layer deposition. High-resolution X-ray diffraction (HR-XRD) revealed two peaks at 34.5° and 36.2° in the initial growth stage of ZnO on the sapphire substrate, corresponding to the (002) and (101) ZnO planes, respectively. However, as the thickness of the ZnO film increased, the XRD intensity of the (002) ZnO peak increased drastically, compared with that of the (101) ZnO peak. This indicated that (002) and (101) ZnO were simultaneously grown on the c-plane sapphire substrate in the initial growth stage, and that (002) ZnO was predominantly grown with the increase in the thickness of ZnO film. The ZnO thin film presented an anisotropic surface structure at the initial stage, whereas the isotropic surface morphology was developed with an increase in the film thickness of ZnO. These observations were consistent with the HR-XRD results.

Mineralogical and physico-chemical characterization of Mbodiene palygorskite for pharmaceutical applications

NASA Astrophysics Data System (ADS)

Sylla Gueye, Rokhaya; Davy, Catherine A.; Cazaux, Frédéric; Ndiaye, Augustin; Diop, Mouhamadou Bassir; Skoczylas, Frédéric; Wele, Alassane

2017-11-01

This contribution provides a wide morphological, mineralogical, chemical and physical characterization of Mbodiene palygorskite (Senegal), to serve as a basis for the formulation of antidiarrheal and cosmetic products. Data are compared with other palygorskite deposits, either in Senegal or on other continents. Qualitative total rock XRD, semi-quantitative XRD of the clay fraction and quantitative X-Ray fluorescence (XRF) show the presence of 72%wt palygorskite (±2%wt), 13%wt montmorillonite (±2%wt), 8%wt dolomite (±2%wt), 5%wt quartz SiO2 (±2%wt) and 2%wt inter-stratified illite/smectite (±2%wt). Coupled SEM + EDX and TEM + EDX confirm the presence of fibrous palygorskite, with greater amounts of Mg than Al, and Fe substitution to Mg and Al, interspersed with dolomite cubes CaMg(CO3)2. The presence of carbonates in Mbodiene palygorskite may limit its use in the Pharmacopoeia, and make its purification necessary. A specific signature of Mbodiene palygorskite, relevant to the palygorskite family, is deduced from both FTIR and TGA analysis. In terms of physico-chemical characterization, Mbodiene palygorskite has usual values when compared to the literature (for its specific surface area, specific gravity, compressibility and Haussner indexes, CEC, loss on ignition, etc.). After grinding (down to a peak grain size of 500 nm), Mbodiene palygorskite is considered a normal clay, extremely highly plastic, with hard consistency owing to the values of its Atterberg plasticity and liquidity limits, with good flowability owing to its compressibility and Haussner indexes. Its physical characteristics are suitable for manufacturing pastes and colloidal suspensions.

Synthesis and characterization of protocatechuic acid-loaded gadolinium-layered double hydroxide and gold nanocomposite for theranostic application

NASA Astrophysics Data System (ADS)

Usman, Muhammad Sani; Hussein, Mohd Zobir; Kura, Aminu Umar; Fakurazi, Sharida; Masarudin, Mas Jaffri; Saad, Fathinul Fikri Ahmad

2018-03-01

A theranostic nanocomposite was developed using anticancer agent, protocatechuic acid (PA) and magnetic resonance imaging (MRI) contrast agent gadolinium nitrate (Gd) for simultaneous delivery using layered double hydroxide (LDH) as the delivery agent. Gold nanoparticles (AuNPs) were adsorbed on the surface of the LDH, which served as a complementary contrast agent. Based on the concept of supramolecular chemistry (SPC) and multimodal delivery system (MDS), the PA and Gd guests were first intercalated into the LDH host and subsequently AuNPs were surface adsorbed as the third guest. The nanohybrid developed was named MAPGAu. The MAPGAu was exposed to various characterizations at different stages of synthesis, starting with XRD analysis, which was used to confirm the intercalation episode and surface adsorption of the guest molecules. Consequently, FESEM, Hi-TEM, XRD, ICP-OES, CHNS, FTIR and UV-Vis analyses were done on the nanohybrids. The result of XRD analysis indicated successful intercalation of the Gd and PA as well the adsorption of AuNPs. The UV-Vis release study showed 90% of the intercalated drug was released at pH 4.8, which is the pH of the cancer cells. The FESEM and TEM micrographs obtained equally confirmed the formation of MAGPAu nanocomposite, with AuNPs conspicuously deposited on the LDH surface. The cytotoxicity study of the nanohybrid also showed insignificant toxicity to normal cell lines and significant toxicity to cancer cell lines. The developed MAGPAu nanocomposite has shown prospects for future theranostic cancer treatment.

Synthesis and property of novel MnO2@polypyrrole coaxial nanotubes as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Yao, Wei; Zhou, Hui; Lu, Yun

2013-11-01

Novel MnO2@polypyrrole (PPy) coaxial nanotubes have been prepared via a simple and green approach without any surfactant and additional oxidant. Under the acidic condition, MnO2 nanotubes act as both template and oxidant to initiate the polymerization of pyrrole monomers on its fresh-activated surface. Fourier transform infrared spectra (FT-IR), X-ray diffraction patterns (XRD), thermo-gravimetric analysis data (TG) and X-ray photoelectron spectra (XPS) suggest the formation of composite structure of MnO2@PPy. Also, FESEM and TEM images intuitively confirm that the PPy shell is coated uniformly on the surface of MnO2 nanotubes. Adjusting the concentrations of sulfuric acid or adding oxidant can modulate the morphology of the products accordingly. Due to the synergic effect between MnO2 core and PPy shell, the MnO2@PPy coaxial nanotubes possess better rate capability, larger specific capacitance of 380 F g-1, doubling the specific capacitance of MnO2 nanotubes, and good capacitance retention of 90% for its initial capacitance after 1000 cycles.

Conversion of "Waste Plastic" into Photocatalytic Nanofoams for Environmental Remediation.

PubMed

de Assis, Geovania C; Skovroinski, Euzébio; Leite, Valderi D; Rodrigues, Marcelo O; Galembeck, André; Alves, Mary C F; Eastoe, Julian; de Oliveira, Rodrigo J

2018-03-07

Plastic debris is a major environmental concern, and to find effective ways to reuse polystyrene (PS) presents major challenges. Here, it is demonstrated that polystyrene foams impregnated with SnO 2 are easily generated from plastic debris and can be applied to photocatalytic degradation of dyes. SnO 2 nanoparticles were synthesized by a polymeric precursor method, yielding specific surface areas of 15 m 2 /g after heat treatment to 700 °C. Crystallinity, size, and shape of the SnO 2 particles were assessed by X-ray diffraction (XRD) and transmission electron microscopy (TEM), demonstrating the preparation of crystalline spherical nanoparticles with sizes around 20 nm. When incorporated into PS foams, which were generated using a thermally induced phase separation (TIPS) process, the specific surface area increased to 48 m 2 /g. These PS/SnO 2 nanofoams showed very good efficiency for photodegradation of rhodamine B, under UV irradiation, achieving up to 98.2% removal. In addition the PS/SnO 2 nanofoams are shown to retain photocatalytic activity for up to five reuse cycles.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

PubMed Central

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-01-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hollow structure and huge specific surface area. The growth of HSS was an inward-growth mechanism along template. Notably, we have provided a new and interesting fundamental principle for HSS materials by precisely controlling the ethanol-to-water volume ratio. In addition, the as-obtained HSS were mixed with waterborne polyurethane (WPU) to prepare WPU/HSS composite membrane. Various characterizations (SEM, TEM, FT-IR and TGA) revealed the morphology, polydispersity and adherence between HSS and WPU. Performance tests showed that the introduction of HSS can improve the water vapor permeability of composite membrane, promoting its water resistance and mechanical performance at the same time. PMID:28429740

Preparation and characterization of uniform nanosized cephradine by combination of reactive precipitation and liquid anti-solvent precipitation under high gravity environment.

PubMed

Zhong, Jie; Shen, Zhigang; Yang, Yan; Chen, Jianfeng

2005-09-14

In this work, a novel direct method, which was combined with reactive precipitation and liquid anti-solvent precipitation under high gravity environment, had been developed to prepare nanosized cephradine with narrow particle size distribution. Compared with commercial crude cephradine, the prepared cephradine showed a significant decrease in particle size, a significant increase in the specific surface area and shorter dissolving time when used for injection. The characteristic particle size was between 200-400 nm. The specific surface area increased from 2.95 to 10.87 m2/g after micronization. When the amount of L-arginin decreased from 0.25 to 0.18 g, the mixture of nanosized cephradine and L-arginine could still dissolve in 1 min. The X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) analysis indicated that the physical characteristics and molecular states remained unchanged after the recrystallization process. This method had potential application in industrial fields because of its low cost, efficient processing and the ease of scaling-up.

Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles.

PubMed

Kuśnieruk, Sylwia; Wojnarowicz, Jacek; Chodara, Agnieszka; Chudoba, Tadeusz; Gierlotka, Stanislaw; Lojkowski, Witold

2016-01-01

Hydroxyapatite (HAp) nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis (MHS). The following parameters of the obtained nanostructured HAp were determined: pycnometric density, specific surface area, phase purity, lattice parameters, particle size, particle size distribution, water content, and structure. HAp nanoparticle morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction measurements confirmed crystalline HAp was synthesized, which was pure in terms of phase. It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. The average diameter of the HAp nanoparticles was determined by Scherrer's equation via the Nanopowder XRD Processor Demo web application, which interprets the results of specific surface area and TEM measurements using the dark-field technique. The obtained nanoparticles with average particle diameter ranging from 8-39 nm were characterized by having homogeneous morphology with a needle shape and a narrow particle size distribution. Strong similarities were found when comparing the properties of some types of nanostructured hydroxyapatite with natural occurring apatite found in animal bones and teeth.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

NASA Astrophysics Data System (ADS)

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-04-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hollow structure and huge specific surface area. The growth of HSS was an inward-growth mechanism along template. Notably, we have provided a new and interesting fundamental principle for HSS materials by precisely controlling the ethanol-to-water volume ratio. In addition, the as-obtained HSS were mixed with waterborne polyurethane (WPU) to prepare WPU/HSS composite membrane. Various characterizations (SEM, TEM, FT-IR and TGA) revealed the morphology, polydispersity and adherence between HSS and WPU. Performance tests showed that the introduction of HSS can improve the water vapor permeability of composite membrane, promoting its water resistance and mechanical performance at the same time.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane.

PubMed

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-04-21

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hollow structure and huge specific surface area. The growth of HSS was an inward-growth mechanism along template. Notably, we have provided a new and interesting fundamental principle for HSS materials by precisely controlling the ethanol-to-water volume ratio. In addition, the as-obtained HSS were mixed with waterborne polyurethane (WPU) to prepare WPU/HSS composite membrane. Various characterizations (SEM, TEM, FT-IR and TGA) revealed the morphology, polydispersity and adherence between HSS and WPU. Performance tests showed that the introduction of HSS can improve the water vapor permeability of composite membrane, promoting its water resistance and mechanical performance at the same time.

Effect of laser irradiation on surface hardness and structural parameters of 7178 aluminium alloy

NASA Astrophysics Data System (ADS)

Maryam, Siddra; Bashir, Farooq

2018-04-01

Aluminium 7178 samples were prepared and irradiated with Nd:YAG laser. The surfaces of exposed samples were investigated using optical microscopy, which revealed that the surface morphology of the samples is changed drastically as a function of laser shots. It is revealed from the micrographs that the laser heat effected area increases with the increase in the number of the laser pulses. Furthermore morphological and mechanical properties were studied using XRD and Vickers hardness testing. XRD study shows an increasing trend in Grain size with the increasing number of laser shots. And the hardness of the samples as a function of the laser shots shows that the hardness first increases and then it decreases gradually. It was observed that the grain size has no pronouncing effect on the hardness. Hardness profile has a decreasing trend with the increase in linear distance from the boundary of the laser heat affected area.

Surface Atomic Structure and Functionality of Metallic Nanoparticles: A Case Study of Au–Pd Nanoalloy Catalysts

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

Petkov, Valeri; Prasai, Binay; Shastri, Sarvjit

The surface atomic structure of metallic nanoparticles (NPs) plays a key role in shaping their physicochemical properties and response to external stimuli. Not surprisingly, current research increasingly focuses on exploiting its prime characteristics, including the amount, location, coordination, and electronic configuration of distinct surface atomic species, as tunable parameters for improving the functionality of metallic NPs in practical applications. The effort requires clear understanding of the extent to which changes in each of these characteristics would contribute to achieving the targeted functionality. This, in the first place, requires good knowledge of the actual surface of metallic NPs at atomic level.more » Through a case study on Au–Pd nanoalloy catalysts of industrial and environmental importance, we demonstrate that the surface atomic structure of metallic NPs can be determined in good detail by resonant high-energy X-ray diffraction (HE-XRD). Furthermore, using our experimental surface structure and CO oxidation activity data, we shed new light on the elusive origin of the remarkable catalytic synergy between surface Au and Pd atoms in the nanoalloys. In particular, we show that it arises from the formation of a specific “skin” on top of the nanoalloys that involves as many unlike, i.e., Au–Pd and Pd–Au, atomic pairs as possible given the overall chemical composition of the NPs. Moreover, unlike atoms from the “skin” interact strongly, including both changing their size and electronic structure in inverse proportions. That is, Au atoms shrink and acquire a partial positive charge of 5d-character whereas Pd atoms expand and become somewhat 4d-electron deficient. Accordingly, the reactivity of Au increases whereas Pd atoms become less reactive, as compared to atoms at the surface of pure Au and Pd NPs, respectively. Ultimately, this renders Au–Pd alloy NPs superb catalysts for CO oxidation reaction over a broad range of alloy compositions. Our findings are corroborated by DFT calculations based on a refined version of d-band center theory on the catalytic properties of late transition metals and alloys. Here, we discuss opportunities for improving the accuracy of current theory on surface-controlled properties of metallic NPs through augmenting the theory with surface structure data obtained by resonant XRD.« less

Surface Atomic Structure and Functionality of Metallic Nanoparticles: A Case Study of Au–Pd Nanoalloy Catalysts

DOE PAGES

Petkov, Valeri; Prasai, Binay; Shastri, Sarvjit; ...

2017-03-23

The surface atomic structure of metallic nanoparticles (NPs) plays a key role in shaping their physicochemical properties and response to external stimuli. Not surprisingly, current research increasingly focuses on exploiting its prime characteristics, including the amount, location, coordination, and electronic configuration of distinct surface atomic species, as tunable parameters for improving the functionality of metallic NPs in practical applications. The effort requires clear understanding of the extent to which changes in each of these characteristics would contribute to achieving the targeted functionality. This, in the first place, requires good knowledge of the actual surface of metallic NPs at atomic level.more » Through a case study on Au–Pd nanoalloy catalysts of industrial and environmental importance, we demonstrate that the surface atomic structure of metallic NPs can be determined in good detail by resonant high-energy X-ray diffraction (HE-XRD). Furthermore, using our experimental surface structure and CO oxidation activity data, we shed new light on the elusive origin of the remarkable catalytic synergy between surface Au and Pd atoms in the nanoalloys. In particular, we show that it arises from the formation of a specific “skin” on top of the nanoalloys that involves as many unlike, i.e., Au–Pd and Pd–Au, atomic pairs as possible given the overall chemical composition of the NPs. Moreover, unlike atoms from the “skin” interact strongly, including both changing their size and electronic structure in inverse proportions. That is, Au atoms shrink and acquire a partial positive charge of 5d-character whereas Pd atoms expand and become somewhat 4d-electron deficient. Accordingly, the reactivity of Au increases whereas Pd atoms become less reactive, as compared to atoms at the surface of pure Au and Pd NPs, respectively. Ultimately, this renders Au–Pd alloy NPs superb catalysts for CO oxidation reaction over a broad range of alloy compositions. Our findings are corroborated by DFT calculations based on a refined version of d-band center theory on the catalytic properties of late transition metals and alloys. Here, we discuss opportunities for improving the accuracy of current theory on surface-controlled properties of metallic NPs through augmenting the theory with surface structure data obtained by resonant XRD.« less

Combined use of FE-SEM+EDS, ToF-SIMS, XPS, XRD and OM for the study of ancient gilded artefacts

NASA Astrophysics Data System (ADS)

Ingo, G. M.; Riccucci, C.; Pascucci, M.; Messina, E.; Giuliani, C.; Biocca, P.; Tortora, L.; Fierro, G.; Di Carlo, G.

2018-07-01

Gilded brooches dating back to 16th-17th centuries CE were investigated by means of integrated and complementary analytical techniques such as high spatial resolution field emission scanning electron microscopy coupled with energy dispersive X-ray spectrometry (FE-SEM+EDS), time of flight secondary ion mass spectrometry (ToF-SIMS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and optical microscopy (OM). The results reveal in detail the surface and subsurface morphology and the chemical features of the micrometric decorative Au layer that has been deposited by means of the so-called fire-gilding technique based on the use of an amalgam. Moreover, the results allow to recognise chlorine, sulphur and phosphorous species as the main degradation agents and to identify the corrosion products naturally formed during the long-term interaction with the burial soil constituents. The findings show also that the galvanic coupling between the two dissimilar metals, i.e. Cu and Au, lead to enhancement of corrosion phenomena causing the spalling of the gold thin film and the disfigurement of the object. From a conservation point of view, the results suggest a targeted use of low-toxic inhibitors to hinder the detrimental role of chlorine as possible responsible of future further severe degradation phenomena. In conclusions, the micro and nano-chemical, structural and morphological investigations in a depth range from a few nanometers to micrometers have revealed the complex nature of corroded surface of ancient gold coated artefacts, highlighting some specific aspects related to their peculiar degradation mechanisms thus extending the scientific relevance of the tailored use of complementary and integrated surface and subsurface analytical techniques for the investigation of ancient coated artefacts.

Hydrothermal synthesis of high surface area ZIF-8 with minimal use of TEA

NASA Astrophysics Data System (ADS)

Butova, V. V.; Budnyk, A. P.; Bulanova, E. A.; Lamberti, C.; Soldatov, A. V.

2017-07-01

In this paper we present, for the first time, a simple hydrothermal recipe for the synthesis of ZIF-8 Metal-Organic Framework (MOF) with a large specific surface area (1340 m2/g by BET). An important feature of the method is that the product forms in aqueous medium under standard hydrothermal conditions without DMF and great excess of linker with the use of TEA as structure directing agent. The ZIF-8 crystal phase of the product was confirmed by XRD; this technique has been also exploited to check the crystallinity and to follow the changes in the MOF structure induced by heating. TGA and temperature dependent XRD testify the high thermal stability of the material (470 °C in N2 and at 400 °C in air). The IR spectral profile of the material provides a complete picture of vibrations assigned to the linker and the metal center. The systematic investigation of the products obtained by increasing the TEA amount in the reacting medium from 0 to 25.5 mol equivalent Zn2+, allowed us to understand its role and to find 2.6 mol equivalent Zn2+ as the minimum amount needed to obtain a single phase ZIF-8 material with the high standard reported above. The stability of the material under severe basic conditions makes it a promising candidate in heterogeneous catalysis. The material has shown high capacity in I2 uptake, making it interesting also for selective molecular adsorption.

Beneficial use of meat and bone meal combustion residue: "an efficient low cost material to remove lead from aqueous effluent".

PubMed

Deydier, Eric; Guilet, Richard; Sharrock, Patrick

2003-07-04

Meat and bone meal (MBM) combustion residues, a natural apatite-rich substance, was evaluated as a low cost substitute for hydroxyapatite in lead sequestration from water effluents. The thermal behaviour of crude meat and bone meal was followed by TGA and 24% inorganic residue was collected. The resulting ashes were characterised by powder X-ray diffraction (XRD), particle size distribution, specific surface area (BET), and elemental analysis confirming apatite contents, with high level of phosphate (56.3%) and calcium (36.8%). Mechanism and kinetics of lead removal by this bioinorganic material were investigated and compared to mechanisms and kinetics involved with synthetic apatite. Batch metal removal experiments were carried out with 500 and 1500ppm (mg/kg) Pb(2+) solutions. Lead concentration, calcium and pH were monitored. We observed that the mechanism is similar to that occurring for pure apatite, and involved both surface complexation and calcium hydroyapatite (CaHA), Ca(10)(PO(4))(6)(OH)(2), dissolution followed by less soluble Pb(10)(PO(4))(6)(OH)(2) precipitation, as confirmed by XRD analysis of ashes after incubation with lead solution. Our results show that this natural apatite-rich material removes in a few minutes a large quantity of lead (275mg/g capacity) which remains however lower than the theoretical maximum capacity (if calcium were totally substituted by lead). Meat and bone meal combustion residues represent a valuable alternative apatite source for environmental application.

Evaluation of Advanced Reactive Surface Area Estimates for Improved Prediction of Mineral Reaction Rates in Porous Media

NASA Astrophysics Data System (ADS)

Beckingham, L. E.; Mitnick, E. H.; Zhang, S.; Voltolini, M.; Yang, L.; Steefel, C. I.; Swift, A.; Cole, D. R.; Sheets, J.; Kneafsey, T. J.; Landrot, G.; Anovitz, L. M.; Mito, S.; Xue, Z.; Ajo Franklin, J. B.; DePaolo, D.

2015-12-01

CO2 sequestration in deep sedimentary formations is a promising means of reducing atmospheric CO2 emissions but the rate and extent of mineral trapping remains difficult to predict. Reactive transport models provide predictions of mineral trapping based on laboratory mineral reaction rates, which have been shown to have large discrepancies with field rates. This, in part, may be due to poor quantification of mineral reactive surface area in natural porous media. Common estimates of mineral reactive surface area are ad hoc and typically based on grain size, adjusted several orders of magnitude to account for surface roughness and reactivity. This results in orders of magnitude discrepancies in estimated surface areas that directly translate into orders of magnitude discrepancies in model predictions. Additionally, natural systems can be highly heterogeneous and contain abundant nano- and micro-porosity, which can limit connected porosity and access to mineral surfaces. In this study, mineral-specific accessible surface areas are computed for a sample from the reservoir formation at the Nagaoka pilot CO2 injection site (Japan). Accessible mineral surface areas are determined from a multi-scale image analysis including X-ray microCT, SEM QEMSCAN, XRD, SANS, and SEM-FIB. Powder and flow-through column laboratory experiments are performed and the evolution of solutes in the aqueous phase is tracked. Continuum-scale reactive transport models are used to evaluate the impact of reactive surface area on predictions of experimental reaction rates. Evaluated reactive surface areas include geometric and specific surface areas (eg. BET) in addition to their reactive-site weighted counterparts. The most accurate predictions of observed powder mineral dissolution rates were obtained through use of grain-size specific surface areas computed from a BET-based correlation. Effectively, this surface area reflects the grain-fluid contact area, or accessible surface area, in the powder dissolution experiment. In the model of the flow-through column experiment, the accessible mineral surface area, computed from the multi-scale image analysis, is evaluated in addition to the traditional surface area estimates.

A facile hydrothermal approach to synthesize rGO/BiVO4 photocatalysts for visible light induced degradation of RhB dye

NASA Astrophysics Data System (ADS)

Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

2018-05-01

RGO/BiVO4 composites were synthesized by a simple hydrothermal method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM) and surface analysis (BET). The photocatalytic activity of the as-prepared samples was evaluated by studying the degradation of model dyes rhodamine B (RhB) under visible light. The prepared rGO/BiVO4 composites exhibited higher photocatalytic activity for the degradation of RhB with a maximum removal rate of 86% under visible light irradiation under visible-light irradiation than pure BiVO4 nanoparticles (63%). This behavior could be associated to their higher specific surface area (BET), increased light absorption intensity and the degradation of electron-hole pair recombination in BiVO4 with the introduction of the rGO.

Production of nanotubes in delignified porous cellulosic materials after hydrolysis with cellulase.

PubMed

Koutinas, Αthanasios Α; Papafotopoulou-Patrinou, Evgenia; Gialleli, Angelika-Ioanna; Petsi, Theano; Bekatorou, Argyro; Kanellaki, Maria

2016-08-01

In this study, tubular cellulose (TC), a porous cellulosic material produced by delignification of sawdust, was treated with a Trichoderma reesei cellulase in order to increase the proportion of nano-tubes. The effect of enzyme concentration and treatment duration on surface characteristics was studied and the samples were analyzed with BET, SEM and XRD. Also, a composite material of gelatinized starch and TC underwent enzymatic treatment in combination with amylase (320U) and cellulase (320U) enzymes. For TC, the optimum enzyme concentration (640U) led to significant increase of TC specific surface area and pore volume along with the reduction of pore diameter. It was also shown that the enzymatic treatment did not result to a significant change of cellulose crystallinity index. The produced nano-tubular cellulose shows potential for application to drug and chemical preservative delivery systems. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis and characterization of MOF-aminated graphite oxide composites for CO2 capture

NASA Astrophysics Data System (ADS)

Zhao, Yunxia; Ding, Huiling; Zhong, Qin

2013-11-01

A kind of metal-organic frameworks (MOF-5) and aminated graphite oxide (AGO) composites were prepared for CO2 capture to mitigate global warming. MOF-5, MOF-5/GO (composite of MOF-5 and graphite oxide) and MOF-5/AGO samples were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscope (SEM), nitrogen adsorption as well as thermogravimetric analysis to figure out their chemistry and structure information. Three types of samples with suitable specific surface area and pore diameter were chosen to test CO2 adsorption performance and stability under humidity conditions. The results indicate that high surface area and pore volume, pore similar in size to the size of gas adsorbate, and extra reactive sites modified in the composites contributes to the high CO2 capacity. Besides, the composites involved by GO or AGO show better anti-moisture performance than the parent MOF.

Facile fabrication of Cu(II)-porphyrin MOF thin films from tetrakis(4-carboxyphenyl)porphyrin and Cu(OH)2 nanoneedle array

NASA Astrophysics Data System (ADS)

La, Duong Duc; Thi, Hoai Phuong Nguyen; Kim, Yong Shin; Rananaware, Anushri; Bhosale, Sheshanath V.

2017-12-01

Herein, we report a facile synthetic protocol to grow thin films of Cu(II) tetrakis(4-carboxyphenyl)porphyrin (CuTCPP) metal-organic frameworks (MOF) from a tetrakis(4-carboxyphenyl)porphyrin (H2TCPP) solution and the copper hydroxide (Cu(OH)2) nanoneedle array formed on a Cu substrate at room temperature. The formations of Cu-centered TCPP ligands and crystalline platelet-like Cu MOFs were successfully probed by SEM, XRD, FTIR, UV-vis and XPS. The formation process from Cu(OH)2 was monitored by using SEM images obtained at different reaction times during the first 24 h, thus suggesting the reaction pathway of Cu(OH)2 dissolution followed by the reprecipitation of CuTCPP MOFs at a near surface. In addition, the CuTCPP MOFs exhibited a high specific surface area of 408 m2/g.

Mineralogy of mine waste at the Vermont Asbestos Group mine, Belvidere Mountain, Vermont

USGS Publications Warehouse

Levitan, D.M.; Hammarstrom, J.M.; Gunter, M.E.; Seal, R.R.; Chou, I.-Ming; Piatak, N.M.

2009-01-01

Samples from the surfaces of waste piles at the Vermont Asbestos Group mine in northern Vermont were studied to determine their mineralogy, particularly the presence and morphology of amphiboles. Analyses included powder X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and Raman spectroscopy. Minerals identified by XRD were serpentine-group minerals, magnetite, chlorite, quartz, olivine, pyroxene, and brucite; locally, mica and carbonates were also present. Raman spectroscopy distinguished antigorite and chrysotile, which could not be differentiated using XRD. Long-count, short-range XRD scans of the (110) amphibole peak showed trace amounts of amphibole in most samples. Examination of amphiboles in tailings by optical microscopy, SEM, and EPMA revealed non-fibrous amphiboles compositionally classified as edenite, magnesiohornblende, magnesiokatophorite, and pargasite. No fibrous amphibole was found in the tailings, although fibrous tremolite was identified in a sample of host rock. Knowledge of the mineralogy at the site may lead to better understanding of potential implications for human health and aid in designing a remediation plan.

Variable-focus microscopy and UV surface dissolution imaging as complementary techniques in intrinsic dissolution rate determination.

PubMed

Ward, Adam; Walton, Karl; Box, Karl; Østergaard, Jesper; Gillie, Lisa J; Conway, Barbara R; Asare-Addo, Kofi

2017-09-15

This work reports a novel approach to the assessment of the surface properties of compacts used in Surface Dissolution Imaging (SDI). SDI is useful for determining intrinsic dissolution rate (IDR), an important parameter in early stage drug development. Surface topography, post-compaction and post-SDI run, have been measured using a non-contact, optical, three-dimensional microscope based on focus variation, the Alicona Infinite Focus Microscope, with the aim of correlating the IDRs to the surface properties. Ibuprofen (IBU) was used as a model poorly-soluble drug. DSC and XRD were used to monitor possible polymorphic changes that may have occurred post-compaction and post-SDI run. IBUs IDR decreased from 0.033mg/min/cm 2 to 0.022mg/min/cm 2 from 10 to 20min, respectively, during the experiment. XRD and DSC showed no form changes during the SDI run. The surface topography images showed that a distinct imprint was embossed on the surfaces of some compacts which could affect IDRs. Surface parameter values were associated with the SDI experiments which showed strong correlations with the IDR values. The variable-focus microscope can be used as a complimentary tool in the determination of IDR values from the SDI. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Surface Morphology and Hardness Analysis of TiCN Coated AA7075 Aluminium Alloy

NASA Astrophysics Data System (ADS)

Srinath, M. K.; Ganesha Prasad, M. S.

2017-12-01

Successful titanium carbonitride (TiCN) coating on AA7075 plates using the PVD technique depends upon many variables, including temperature, pressure, incident angle and energy of the reactive ions. Coated specimens have shown an increase in their surface hardness of 2.566 GPa. In this work, an attempt to further augment the surface hardness and understand its effects on the surface morphology was performed through heat treatments at 500°C for different duration of times. Specimen's heat treated at 500°C for 1 h exhibited a maximum surface hardness of 6.433 GPa, corresponding to an increase of 92.07%. The XRD results showed the presence of Al2Ti and AlTi3N and indicate the bond created between them. Unit cell lattice parameters in the XRD data are calculated using Bragg's law. The SEM images exhibit increasing crack sizes as the heat treatment time is increased. From the studies, the heat treatment duration can be optimized to 1 h, which exhibited an augmented surface hardness, as further increases in durations caused a drop in the surface hardness. The heat treatment effectively modified the surface hardness. Equations providing the relationships that temperature and time have with the reaction parameters are presented.

Adequacy of surface analytical tools for studying the tribology of ceramics

NASA Technical Reports Server (NTRS)

Sliney, H. E.

1986-01-01

Surface analytical tools are very beneficial in tribological studies of ceramics. Traditional methods of optical microscopy, XRD, XRF, and SEM should be combined with newer surface sensitive techniques especially AES and XPS. ISS and SIMS can also be useful in providing additional compositon details. Tunneling microscopy and electron energy loss spectroscopy are less known techniques that may also prove useful.

Fabrication of multicolor fluorescent polyvinyl alcohol through surface modification with conjugated polymers by oxidative polymerization

NASA Astrophysics Data System (ADS)

Hai, Thien An Phung; Sugimoto, Ryuichi

2018-06-01

A simple method for the preparation of multicolor polyvinyl alcohol (PVA) by chemical oxidative polymerization is introduced. The PVA surface was successfully modified with conjugated polymers composed of 3-hexylthiophene (3HT) and fluorene (F). The incorporation of the 3HT/F copolymer onto the PVA surface was confirmed by Fourier-transform infrared (FT-IR), ultraviolet-visible (UV-vis), and fluorescence spectroscopies, X-ray diffraction (XRD), as well as thermogravimetric analysis (TGA), contact angle, and field-emission scanning electron microscopy (FE-SEM) coupled with energy dispersive X-ray (EDX) analysis. Different 3HT/F ratios on the PVA surface result in optical properties that include multicolor-emission and absorption behavior. The color of the resultant (3HT/F)-g-PVA shifted from red to blue, and the quantum yield increased with increasing F content. The surface hydrophobicity of the modified PVA increased significantly through grafting with the conjugated polymers, with the water contact angle increasing by 30° compared to pristine PVA. The PVA XRD peaks were less intense following surface modification. Thermogravimetric analyses reveal that the thermal stability of the PVA decreases as a result of grafting with the 3HT/F copolymers.

Chemical synthesis and supercapacitive properties of lanthanum telluride thin film.

PubMed

Patil, S J; Lokhande, A C; Lee, D-W; Kim, J H; Lokhande, C D

2017-03-15

Lanthanum telluride (La 2 Te 3 ) thin films are synthesized via a successive ionic layer adsorption and reaction (SILAR) method. The crystal structure, surface morphology and surface wettability properties are investigated using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FE-SEM) and contact angle goniometer techniques, respectively. The La 2 Te 3 material exhibits a specific surface area of 51m 2 g -1 determined by Brunauer-Emmett-Teller (BET) method. La 2 Te 3 thin film electrode has a hydrophilic surface which consists of interconnected pine leaf-like flaky arrays that affect the performance of the supercapacitor. The supercapacitive performance of La 2 Te 3 film electrode is evaluated in 1M LiClO 4 /PC electrolyte using cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy techniques. La 2 Te 3 film electrode exhibits a specific capacitance of 194Fg -1 at a scan rate of 5mVs -1 and stored energy density of 60Whkg -1 with delivering power density of 7.22kWkg -1 . La 2 Te 3 film electrode showed capacitive retention of 82% over 1000cycles at a scan rate of 100mVs -1 . Further, flexible La 2 Te 3 |LiClO 4 -PVA|La 2 Te 3 supercapacitor cell is fabricated. Copyright © 2016 Elsevier Inc. All rights reserved.

Photocatalytic activity of titania coatings synthesised by a combined laser/sol–gel technique

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

Adraider, Y.; Pang, Y.X., E-mail: F6098038@tees.ac.uk; Nabhani, F.

2014-06-01

Highlights: • Sol–gel method was used to prepare titania coatings. • Titania thin films were coated on substrate surface by dip coating. • Fibre laser was employed to irradiate the titania coated surfaces. • Photocatalytic efficiency of titania coatings was significantly improved after laser processing. - Abstract: Titania coatings were prepared using sol–gel method and then applied on the substrate surface by dip coating. Fibre laser (λ = 1064 nm) in continuous wave mode was used to irradiate the titania coated surfaces at different specific energies. The ATR-FTIR, XRD, SEM, EDS and contact angle measurement were employed to analyse surfacemore » morphology, phase composition and crystalline structure of laser-irradiated titania coatings, whilst the photocatalytic activity was evaluated by measuring the decomposition of methylene blue (MB) after exposure to the visible light for various illumination times. Results showed that the laser-irradiated titania coatings demonstrate significant different composition and microstructure in comparison with the as-coated from the same sol–gel titania. Photocatalytic efficiency of titania coatings was significantly improved after laser processing. The photocatalytic activity of laser-irradiated titania coatings was higher than that of the as-coated titania. The titania coating processed at laser specific energy of 6.5 J/mm{sup 2} exhibited the highest photocatalytic activity among all titania samples.« less

A study of thermal properties of sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method

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

Preda, Silviu, E-mail: predas01@yahoo.co.uk; Rutar, Melita; Jožef Stefan International Postgraduate School, Jamova cesta 39, SI-1000 Ljubljana

2015-11-15

Highlights: • The microwave-assisted hydrothermal route was used for titanate nanotubes synthesis. • Conversion to single-phase nanotube morphology completes after 8 h reaction time. • The nanotube morphology is stable up to 600 °C, as determined by in-situ XRD and SEM. • Sodium ions migrate to the surface due to thermal motion and structure condensation. - Abstract: Sodium titanate nanotubes (NaTiNTs) were synthesized by microwave-assisted hydrothermal treatment of commercial TiO{sub 2}, at constant temperature (135 °C) and different irradiation times (15 min, 1, 4, 8 and 16 h). The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electronmore » microscopy, differential scanning calorimetry and specific surface area measurements. The irradiation time turned out to be the key parameter for morphological control of the material. Nanotubes were observed already after 15 min of microwave irradiation. The analyses of the products irradiated for 8 and 16 h confirm the complete transformation of the starting TiO{sub 2} powder to NaTiNTs. The nanotubes are open ended with multi-wall structures, with the average outer diameter of 8 nm and specific surface area up to 210 m{sup 2}/g. The morphology, surface area and crystal structure of the sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method were similar to those obtained by conventional hydrothermal method.« less

Temperature dependent surface and spectral modifications of nano V2O5 films

NASA Astrophysics Data System (ADS)

Manthrammel, M. Aslam; Fatehmulla, A.; Al-Dhafiri, A. M.; Alshammari, A. S.; Khan, Aslam

2017-03-01

Nanocrystalline V2O5 films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO2 (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.

Synthesis, structural and magnetic properties of Mg0.6Zn0.4CrxFe2-xO4 (0.0 ≤ x ≤ 2.0) nano ferrite

NASA Astrophysics Data System (ADS)

Verma, R.; Kane, S. N.; Raghuvanshi, S.; Satalkar, M.; Modak, S. S.; Mazaleyrat, F.

2018-05-01

Present study reports, effect on structural, magnetic properties of Cr doped Mg-Zn nano-ferrite: Mg0.6Zn0.4CrxFe2-xO4 (0.0≤ x≤2.0), synthesized by sol-gel auto combustion method. X-ray diffraction (XRD), vibrating sample magnetometer (VSM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) techniques were utilized to monitor the effect of Cr substitution on structural, magnetic properties, and correlation between them. XRD confirms the formation of single phase spinel nano ferrite with particle size ranging between 3.9 - 40.5 nm, whereas EDS confirms the formation of the estimated ferrite composition. Distribution of Mg, Zn, Cr, Fe cations on tetrahedral (A), octahedral (B) site show mixed spinel structure. Increase of Cr content leads to increase of specific surface area (4.35 - 28.28 m2/g), decrease of experimental saturation magnetization at 300 K (varies between 0.57 - 40.95 Am2/kg), and theoretical magnetization at 0 K (range between 13.37 - 56.77 Am2/kg). Observed changes in coercivity values reflect soft magnetic nature of the studied ferrites.

Preparation of hydroxyapatite from animal bones.

PubMed

Sobczak, Agnieszka; Kowalski, Zygmunt; Wzorek, Zbigniew

2009-01-01

This paper presents the method of obtaining hydroxyapatite from animal bones. Bone sludge and calcined products were characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Calcium concentration was determined with titration, and phosphorus--spectrophotometrically. Making use of the AAS and ICP methods the content of microelements was determined. In all the products, hydroxyapatite was the only crystalline phase indicated. The FT-IR spectra confirmed that calcination removed the total of organic substances. Calcium and phosphorus contents were 38% and 18%, respectively, which corresponded to the Ca/P molar ratio of nonstoichiometric hydroxyapatite. The specific surfaces of products were measured by BET method. The volume of micro- and mesopores was determined.

Tailoring pore properties of MCM-48 silica for selective adsorption of CO2.

PubMed

Kim, Sangil; Ida, Junichi; Guliants, Vadim V; Lin, Jerry Y S

2005-04-07

Four different types of amine-attached MCM-48 silicas were prepared and investigated for CO(2) separation from N(2). Monomeric and polymeric hindered and unhindered amines were attached to the pore surface of the MCM-48 silica and characterized with respect to their CO(2) sorption properties. The pore structures and amino group content in these modified silicas were investigated by XRD, FT-IR, TGA, N(2) adsorption/desorption at 77 K and CHN/Si analysis, which confirmed that in all cases the amino groups were attached to the pore surface of MCM-48 at 1.5-5.2 mmol/g. The N(2) adsorption/desorption analysis showed a considerable decrease of the pore volume and surface area for the MCM-48 silica containing a polymeric amine (e.g., polyethyleneimine). The CO(2) adsorption rates and capacities of the amine-attached MCM-48 samples were studied employing a sorption microbalance. The results obtained indicated that in addition to the concentration of surface-attached amino groups, specific interactions between CO(2) and the surface amino groups, and the resultant pore structure after amine group attachment have a significant impact on CO(2) adsorption properties of these promising adsorbent materials.

Characteristics of nano-sized yttria powder synthesized by a polyvinyl alcohol solution route at low temperature.

PubMed

Lee, Sang-Jin; Jung, Choong-Hwan

2012-01-01

Nano-sized yttria (Y2O3) powders were successfully synthesized at a low temperature of 400 degrees C by a simple polymer solution route. PVA polymer, as an organic carrier, contributed to an atom-scale homogeneous precursor gel and it resulted in fully crystallized, nano-sized yttria powder with high specific surface area through the low temperature calcination. In this process, the content of PVA, calcination temperature and heating time affected the microstructure and crystallization behavior of the powders. The development of crystalline phase and the final particle size were strongly dependant on the oxidation reaction from the polymer burn-out step and the PVA content. In this paper, the PVA solution technique for the fabrication of nano-sized yttria powders is introduced. The effects of PVA content and holding time on the powder morphology and powder specific surface area are also studied. The characterization of the synthesized powders is examined by using XRD, DTA/TG, SEM, TEM and nitrogen gas adsorption. The yttria powder synthesized from the PVA content of 3:1 ratio and calcined at 400 degrees C had a crystallite size of about 20 nm or less with a high surface areas of 93.95-120.76 m2 g(-1).

Mesoporous tungsten oxynitride as electrocatalyst for promoting redox reactions of vanadium redox couple and performance of vanadium redox flow battery

NASA Astrophysics Data System (ADS)

Lee, Wonmi; Jo, Changshin; Youk, Sol; Shin, Hun Yong; Lee, Jinwoo; Chung, Yongjin; Kwon, Yongchai

2018-01-01

For enhancing the performance of vanadium redox flow battery (VRFB), a sluggish reaction rate issue of V2+/V3+ redox couple evaluated as the rate determining reaction should be addressed. For doing that, mesoporous tungsten oxide (m-WO3) and oxyniride (m-WON) structures are proposed as the novel catalysts, while m-WON is gained by NH3 heat treatment of m-WO3. Their specific surface area, crystal structure, surface morphology and component analysis are measured using BET, XRD, TEM and XPS, while their catalytic activity for V2+/V3+ redox reaction is electrochemically examined. As a result, the m-WON shows higher peak current, smaller peak potential difference, higher electron transfer rate constant and lower charge transfer resistance than other catalysts, like the m-WO3, WO3 nanoparticle and mesoporous carbon, proving that it is superior catalyst. Regarding the charge-discharge curve tests, the VRFB single cell employing the m-WON demonstrates high voltage and energy efficiencies, high specific capacity and low capacity loss rate. The excellent results of m-WON are due to the reasons like (i) reduced energy band gap, (ii) reaction familiar surface functional groups and (ii) greater electronegativity.

Phase study and surface morphology of beta-alumina

NASA Astrophysics Data System (ADS)

Tak, S. K.

2018-05-01

Beta alumina ceramic is well known as a polycrystalline ceramic material. The characteristic crystal structure of beta-alumina makes it useful as a separator in sodium sulphur batteries and other electrochemical devices requiring the passage of sodium ions. β"-alumina powders for this study were prepared by zeta process. The pellets were sintered at different microwave power levels and power schedule to optimize the sintering conditions to obtain preferred β" phase with improved microstructure. Phase identification was studied by X-ray diffraction (XRD). XRD analysis shows increase in β'' phase as the sintering temperature was increased from 1400°C to 1600°C. Surface morphology of the pellets was carried out by Scanning Electron microscopy (SEM). SEM studies revealed the formation and growth of platelet grains with interconnected porosity.

Synthesis, structural, thermal and Hirshfeld surface analysis of novel [1,2,4]triazolo[3,4-b][1,3,4] thiadiazine carrying 1,4-benzothiazine-3-one moiety

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped single crystal of the title compound was grown by slow evaporation solution growth technique using ethanol as solvent. The grown single crystal was characterized using FT-IR, Single crystal XRD and Thermal analysis. The FT-IR spectrum confirms the molecular structure and identifies the different functional groups present in the compound. Single crystal XRD study reveals that the crystallized compound belongs to the monoclinic crystal system with P21/c space group and the corresponding cell parameters were identified. The thermal stability of the material was determined using both TGA and DTA analysis. The intermolecular interaction of each individual atom in the crystal lattice was estimated using Hirshfeld surface and finger print analysis.

Staircase polymetalsilicon nanocomplexes - Polymetalphenyl siloxanes: Structure and properties

NASA Astrophysics Data System (ADS)

Shapkin, N. P.; Balanov, M. I.; Razov, V. I.; Gardionov, S. V.; Mayorov, V. Yu; Tokar, E. A.; Papynov, E. K.; Korochentsev, V. V.; Leont'ev, L. B.; Slobodyuk, A. B.; Modin, E. B.

2018-03-01

Polyphenyl siloxanes containing chromium, iron, and aluminum in the backbone chain have been synthesized. The structure of the obtained staircase nano-metal complexes has been studied by the methods of XRD analysis and IR, 29Si and 27Al NMR, and XPS spectroscopy and scanning electron microscopy. Physical-chemical characteristics of these compounds have been investigated by the positron annihilation spectroscopy (PAS) and low-temperature nitrogen adsorption. The data of X-ray diffraction analysis (XRD) enabled us to calculate the size and volume of coherent scattering regions (CSR) and the cross-section area of the polymer chains. By means of the PAS method, the specific volumes of positron (Ve+) and positronium (Vps) "traps" have been calculated. The data of 29Si NMR spectroscopy have shown the presence of T2 and T3 fragments in the structure. As was shown on the basis of the data of 27Al NMR and XPS spectroscopy, tetrahedral (66%) and octahedral surroundings of the metal atom were realized in the backbone chain. The obtained data were used to describe a spatial layered structure of phenyl siloxanes containing trivalent metals. The electron microscopy of nanocomplexes revealed the presence of spherical particles, whose size changes in cases of chromium, iron, and aluminum. Using the data of low-temperature nitrogen adsorption, it was assumed that the specific surface area was filled with a layer of compacted spherical particles, whereas the layer thickness was determined, in its turn, by the specific polarizing potential (SPP) calculated as a ratio of the polarizing potential (PP) to the volume of voids between coherent scattering regions. Similar dependence is observed between the layer thickness and the specific polarizing potential calculated as a ratio of the polarizing potential to the positronium "trap" volume. A direct dependence between the thickness of the spherical particles layer and the specific polarizing potential has been demonstrated. The assumption on a fractal structure of spherical particles was made. Tribotechnical properties of the motor oil with metal siloxane additives have been studied.

Spherical V-Fe-MCM-48: The Synthesis, Characterization and Hydrothermal Stability.

PubMed

Qian, Wang; Wang, Haiqing; Chen, Jin; Kong, Yan

2015-04-14

Spherical MCM-48 mesoporous sieve co-doped with vanadium and iron was successfully synthesized via one-step hydrothermal method. The material was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, inductively coupled plasma (ICP), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-vis spectra, and X-ray photoelectron spectra (XPS) techniques. Results indicated that the V-Fe-MCM-48 showed an ordered 3D cubic mesostructure with spherical morphology, narrow pore size distribution and high specific surface area. Most of vanadium and iron atoms existing as tetrahedral V 4+ and Fe 3+ species were co-doped into the silicate framework. The particle sizes of V-Fe-MCM-48 were smaller and the specific area was much higher than those of of V-MCM-48. Additionally, the synthesized V-Fe-MCM-48 exhibited improved hydrothermal stability compared with the pure MCM-48.

Spherical V-Fe-MCM-48: The Synthesis, Characterization and Hydrothermal Stability

PubMed Central

Qian, Wang; Wang, Haiqing; Chen, Jin; Kong, Yan

2015-01-01

Spherical MCM-48 mesoporous sieve co-doped with vanadium and iron was successfully synthesized via one-step hydrothermal method. The material was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, inductively coupled plasma (ICP), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-vis spectra, and X-ray photoelectron spectra (XPS) techniques. Results indicated that the V-Fe-MCM-48 showed an ordered 3D cubic mesostructure with spherical morphology, narrow pore size distribution and high specific surface area. Most of vanadium and iron atoms existing as tetrahedral V4+ and Fe3+ species were co-doped into the silicate framework. The particle sizes of V-Fe-MCM-48 were smaller and the specific area was much higher than those of of V-MCM-48. Additionally, the synthesized V-Fe-MCM-48 exhibited improved hydrothermal stability compared with the pure MCM-48. PMID:28788030

Understanding the effect of surface/bulk defects on the photocatalytic activity of TiO2: anatase versus rutile.

PubMed

Yan, Junqing; Wu, Guangjun; Guan, Naijia; Li, Landong; Li, Zhuoxin; Cao, Xingzhong

2013-07-14

The sole effect of surface/bulk defects of TiO2 samples on their photocatalytic activity was investigated. Nano-sized anatase and rutile TiO2 were prepared by hydrothermal method and their surface/bulk defects were adjusted simply by calcination at different temperatures, i.e. 400-700 °C. High temperature calcinations induced the growth of crystalline sizes and a decrease in the surface areas, while the crystalline phase and the exposed facets were kept unchanged during calcination, as indicated by the characterization results from XRD, Raman, nitrogen adsorption-desorption, TEM and UV-Vis spectra. The existence of surface/bulk defects in calcined TiO2 samples was confirmed by photoluminescence and XPS spectra, and the surface/bulk defect ratio was quantitatively analyzed according to positron annihilation results. The photocatalytic activity of calcined TiO2 samples was evaluated in the photocatalytic reforming of methanol and the photocatalytic oxidation of α-phenethyl alcohol. Based on the characterization and catalytic results, a direct correlation between the surface specific photocatalytic activity and the surface/bulk defect density ratio could be drawn for both anatase TiO2 and rutile TiO2. The surface defects of TiO2, i.e. oxygen vacancy clusters, could promote the separation of electron-hole pairs under irradiation, and therefore, enhance the activity during photocatalytic reaction.

Hot Corrosion Behavior of Ti-48Al and Ti-48Al-2Cr Intermetallic Alloys Produced by Electric Current Activated Sintering

NASA Astrophysics Data System (ADS)

Garip, Y.; Ozdemir, O.

2018-06-01

In this study, Ti-48Al and Ti-48Al-2Cr (at. pct) intermetallic alloys were produced by electric current activated sintering (ECAS). In order to characterize the phase formation and microstructures of these alloys, scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis were used. The XRD result shows that the intermetallic alloys are composed of γ-TiAl and α 2-Ti3Al phases. The microstructure is dense with a low amount of porosity. The hot corrosion behavior of intermetallic alloys was carried out in a salt mixture of 25 wt pct K2SO4 and 75 wt pct Na2SO4 at 700 °C for 180 hours. The morphology of corroded surfaces was observed by SEM-EDS and XRD. Corrosion phases were identified as TiO2 and Al2O3. Well-adhering oxide scale was detected on the corroded sample surface at the end of 180 hours, and no spallation was observed. In addition, a parabolic curve was obtained at the weight change rate vs time.

Visible light activated TiO2/microcrystalline cellulose nanocatalyst to destroy organic contaminants in water.

EPA Science Inventory

Hybrid TiO2/microcrystalline cellulose (MC) nanophotocatalyst was prepared in situ by a facile and simple synthesis utilizing benign precursors such as MC and TiCl4. The as-prepared nanocomposite was characterized by XRD, XPS, BET surface area analyzer, UV–vis DRS and TGA. Surfac...

Surface photoelectric and visible light driven photocatalytic properties of zinc antimonate-based photocatalysts

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

Wu, Shaojun; Li, Guoqiang; Zhang, Yang

2013-03-15

Highlights: ► N-doped and pristine ZnSb{sub 2}O{sub 6} photocatalysts were synthesized by a facile method. ► N-doped ZnSb{sub 2}O{sub 6} shows a significant enhanced visible light photocatalytic activity. ► The N-doped ZnSb{sub 2}O{sub 6} shows the reduced surface photovoltage signals. - Abstract: The N-doped and pristine ZnSb{sub 2}O{sub 6} photocatalysts were synthesized by a facile method. The samples were characterized by X-ray diffraction (XRD), UV–vis spectroscopy, surface photovoltage spectroscopy and scanning electron microscopy. The photocatalytic activities of the prepared samples were evaluated from the degradation of rhodamine B (RhB) under full arc and visible light irradiation of Xe lamp. Themore » XRD and UV–vis results indicated that the N-doping did not change the crystal structure, but decrease the band gap in comparison with the pristine one. The N-doped ZnSb{sub 2}O{sub 6} shows the reduced surface photovoltage signals and the significantly enhanced photocatalytic activity under two irradiation conditions.« less

Structure evolution of zinc oxide thin films deposited by unbalance DC magnetron sputtering

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

Aryanto, Didik, E-mail: didi027@lipi.go.id; Materials Research Group, Physics Department, Universitas Negeri Semarang, Gunungpati, Semarang 50229 Jawa Tengah; Marwoto, Putut

Zinc oxide (ZnO) thin films are deposited on corning glass substrates using unbalanced DC magnetron sputtering. The effect of growth temperature on surface morphology and crystallographic orientation of ZnO thin film is studied using atomic force microscopy (AFM) and X-ray diffraction (XRD) techniques. The surface morphology and crystallographic orientation of ZnO thin film are transformed against the increasing of growth temperature. The mean grain size of film and the surface roughness are inversely and directly proportional towards the growth temperature from room temperature to 300 °C, respectively. The smaller grain size and finer roughness of ZnO thin film are obtainedmore » at growth temperature of 400 °C. The result of AFM analysis is in good agreement with the result of XRD analysis. ZnO thin films deposited in a series of growth temperatures have hexagonal wurtzite polycrystalline structures and they exhibit transformations in the crystallographic orientation. The results in this study reveal that the growth temperature strongly influences the surface morphology and crystallographic orientation of ZnO thin film.« less

Effect of black clay soil moisture on the electrochemical behavior of API X70 pipeline steel

NASA Astrophysics Data System (ADS)

Hendi, R.; Saifi, H.; Belmokre, K.; Ouadah, M.; Smili, B.; Talhi, B.

2018-03-01

The effect of moisture content variation (20–100 wt.%) on the electrochemical behavior of API X70 pipeline steel buried in the soil of Skikda (East of Algeria) was studied using electrochemical techniques, scanning electron microscopy (SEM), X ray diffraction analysis (XRD) and weight loss measurement. The electrochemical measurements showed that the corrosion current Icorr is directly proportional to the moisture content up to 50 wt.%, beyond this content, this value becomes almost constant. The result were confirmed by electrochemical impedance spectroscopy; the capacitance of the double layer formed on the surface is the highest at 50 wt.%. A single time constant was detected by plotting the Bode diagrams. The steel surface degradation has been appreciated using the scanning electron microscopy observations. A few pitting corrosion at 20 wt.% moisture, followed by more degradation at 50 wt.% have been revealed. However, when the moisture amount exceeded 50 wt.%, the surface became entirely covered by a corrosion product. XRD analysis revealed the dominance of FeOOH and Fe3O4 phases on steel surface for a moisture content of 50 wt.%.

Laser irradiation effects on the surface, structural and mechanical properties of Al-Cu alloy 2024

NASA Astrophysics Data System (ADS)

Yousaf, Daniel; Bashir, Shazia; Akram, Mahreen; kalsoom, Umm-i.-; Ali, Nisar

2014-02-01

Laser irradiation effects on surface, structural and mechanical properties of Al-Cu-Mg alloy (Al-Cu alloy 2024) have been investigated. The specimens were irradiated for various fluences ranging from 3.8 to 5.5 J/cm2 using an Excimer (KrF) laser (248 nm, 18 ns, 30 Hz) under vacuum environment. The surface and structural modifications of the irradiated targets have been investigated by scanning electron microscope (SEM) and X-ray diffractometer (XRD), respectively. SEM analysis reveals the formation of micro-sized craters along the growth of periodic surface structures (ripples) at their peripheries. The size of the craters initially increases and then decreases by increasing the laser fluence. XRD analysis shows an anomalous trend in the peak intensity and crystallite size of the specimen irradiated for various fluences. A universal tensile testing machine and Vickers microhardness tester were employed in order to investigate the mechanical properties of the irradiated targets. The changes in yield strength, ultimate tensile strength and microhardness were found to be anomalous with increasing laser fluences. The changes in the surface and structural properties of Al-Cu alloy 2024 after laser irradiation have been associated with the changes in mechanical properties.

Synthesis and characterization of a stable, label-free optical biosensor from TiO2-coated porous silicon.

PubMed

Li, Jianlin; Sailor, Michael J

2014-05-15

A nanoscale layer of TiO2 is coated on the inner pore walls of a porous silicon (PSi) film by room-temperature infiltration of a TiO2 sol-gel precursor and firing at 500 °C. The PSi:TiO2 composite films are characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD), energy dispersive X-ray spectral analysis (EDS), scanning electron microscopy (SEM) and reflective interferometric Fourier transform spectroscopy (RIFTS). The analysis indicates that TiO2 conformally coats the inner pore surfaces of the PSi film. The film displays greater aqueous stability in the pH range 2-12 relative to a PSi:SiO2 surface. A label-free optical interference immunosensor based on the TiO2-coated PSi film is demonstrated by real-time monitoring of the physical adsorption of protein A, followed by the specific binding of rabbit anti-sheep immunoglobulin (IgG) and then specific capture of sheep IgG. The time to achieve equilibrium for the physical adsorption of protein A on the surface of TiO2-coated PSi film is significantly greater than that of PSi film. The specificity of the protein A and rabbit anti-sheep IgG construct on the sensor is confirmed by tests with non-binding chicken IgG. The sensitivity of the immunosensor is shown to be 8210 ± 170 nm/refractive index unit (RIU). Copyright © 2013 Elsevier B.V. All rights reserved.

Dissolution Rates of Allophane, FE-Containing Allophane, and Hisingerite and Implications for Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Ralston, S. J.; Hausrath, E. M.; Tschauner, O.; Rampe, E. B.; Christoffersen, R.

2018-01-01

Investigations with the CheMin Xray Diffractometer (XRD) onboard the Curiosity rover in Gale Crater demonstrate that all rock and soil samples measured to date contain approximately 15-70 weight percentage X-ray amorphous materials. The diffuse scattering hump from the X-ray amorphous materials in CheMin XRD patterns can be fit with a combination of allophane, ferrihydrite, and rhyolitic and basaltic glass. Because of the iron-rich nature of Mars' surface, Fe-rich poorly-crystalline phases, such as hisingerite, may be present in addition to allophane.

Effects of Small Polar Molecules (MA+ and H2O) on Degradation Processes of Perovskite Solar Cells.

PubMed

Ma, Chunqing; Shen, Dong; Qing, Jian; Thachoth Chandran, Hrisheekesh; Lo, Ming-Fai; Lee, Chun-Sing

2017-05-03

Degradation mechanisms of methylammonium lead halide perovskite solar cells (PSCs) have drawn much attention recently. Herein, the bulk and surface degradation processes of the perovskite were differentiated for the first time by employing combinational studies using electrochemical impedance spectroscopy (EIS), capacitance frequency (CF), and X-ray diffraction (XRD) studies with particular attention on the roles of small polar molecules (MA + and H 2 O). CF study shows that short-circuit current density of the PSCs is increased by H 2 O at the beginning of the degradation process coupled with an increased surface capacitance. On the basis of EIS and XRD analysis, we show that the bulk degradation of PSCs involves a lattice expansion process, which facilitates MA + ion diffusion by creating more efficient channels. These results provide a better understanding of the roles of small polar molecules on degradation processes in the bulk and on the surface of the perovskite film.

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.

An Investigation of the Interatomic Bonding Characteristics of a Ti - 51at.% Al Alloy by X-Ray Diffraction

DTIC Science & Technology

1991-06-01

GROUP SUBGROUP X-ray Diffraction, XRD, TiAI, titanium , aluminum, bonding characteristics, titanium aluminides , Debye-Waller temperature factor...XRD Powder Particles (575X) .............. 47 viii I. INTRODUCTION Titanium aluminides are recognized for their high specific strength, particularly at...bonding characteristics of binary titanium aluminides . Upon the introduction of a third element to the system, a rearrangement of the valence

Evaluation of Cation Migration in Lanthanum Strontium Cobalt Ferrite Solid Oxide Fuel Cell Cathodes via In-operando X-ray Diffraction

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

Hardy, John S.; Coyle, Christopher A.; Bonnett, Jeff F.

2018-01-28

Anode-supported SOFCs with LSCF-6428 cathodes were operated at various temperatures for hundreds of hours in dry or humid (~3% water) cathode air with continuous cathode XRD. Additionally, one cell in dry air was held at OCV and another had 12% CO2 added to the humid air. Long cumulative XRD count times allowed identification of minor phases at <0.1 wt%. In humid air, performance improved during the first couple of hundred hours and Fe-rich Fe,Co spinel XRD peaks gradually shifted to lower angles while nano-nodules formed on LSCF surfaces. With 12% CO2 added, performance degraded after initial activation, unlike without CO2,more » where stability followed activation. In CO2, LSCF XRD peaks shifted indicating gradual decomposition. In dry air, fast initial degradation that decelerated over time occurred at constant current while the cell at OCV was stable. At OCV and 750°C or at constant current and 700°C in dry air, Fe-rich spinel XRD peaks shifted more slowly than in humid air tests; Co-rich Fe,Co spinel peaks shifted to higher angles; and SEM discovered smaller nano-nodules on LSCF than after humid air tests. At constant current at 750°C and 800°C in dry air, no nano-nodules or gradual changes in the XRD patterns were discovered.« less

Synthesis, characterization and catalytic activity of indium substituted nanocrystalline Mobil Five (MFI) zeolite

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

Shah, Kishor Kr.; Nandi, Mithun; Talukdar, Anup K., E-mail: anup_t@sify.com

2015-06-15

Highlights: • In situ modification of the MFI zeolite by incorporation of indium. • The samples were characterized by XRD, FTIR, TGA, UV–vis (DRS), SAA, EDX and SEM. • The incorporation of indium was confirmed by XRD, FT-IR, UV–vis (DRS), EDX and TGA. • Hydroxylation of phenol reaction was studied on the synthesized catalysts. - Abstract: A series of indium doped Mobil Five (MFI) zeolite were synthesized hydrothermally with silicon to aluminium and indium molar ratio of 100 and with aluminium to indium molar ratios of 1:1, 2:1 and 3:1. The MFI zeolite phase was identified by XRD and FT-IRmore » analysis. In XRD analysis the prominent peaks were observed at 2θ values of around 6.5° and 23° with a few additional shoulder peaks in case of all the indium incorporated samples suggesting formation of pure phase of the MFI zeolite. All the samples under the present investigation were found to exhibit high crystallinity (∼92%). The crystallite sizes of the samples were found to vary from about 49 to 55 nm. IR results confirmed the formation of MFI zeolite in all cases showing distinct absorbance bands near 1080, 790, 540, 450 and 990 cm{sup −1}. TG analysis of In-MFI zeolites showed mass losses in three different steps which are attributed to the loss due to adsorbed water molecules and the two types TPA{sup +} cations. Further, the UV–vis (DRS) studies reflected the position of the indium metal in the zeolite framework. Surface area analysis of the synthesized samples was carried out to characterize the synthesized samples The analysis showed that the specific surface area ranged from ∼357 to ∼361 m{sup 2} g{sup −1} and the pore volume of the synthesized samples ranged from 0.177 to 0.182 cm{sup 3} g{sup −1}. The scanning electron microscopy studies showed the structure of the samples to be rectangular and twinned rectangular shaped. The EDX analysis was carried out for confirmation of Si, Al and In in zeolite frame work. The catalytic activities of the synthesized samples were investigated with respect to hydroxylation of phenol, in which catechol and hydroquinone were found to be the major products. It is observed that under all reaction conditions catechol selectivity was higher than the hydroquinone selectivity. In-MFI zeolites were successfully synthesized and were used as an effective catalyst for the hydroxylation of phenol to synthesize catechol and hydroquinone as the major product.« less

Interface morphology of a Cr(001)/Fe(001) superlattice determined by scanning tunneling microscopy and x-ray diffraction: A comparison

NASA Astrophysics Data System (ADS)

Schmidt, C. M.; Bürgler, D. E.; Schaller, D. M.; Meisinger, F.; Güntherodt, H.-J.; Temst, K.

2001-01-01

A Cr(001)/Fe(001) superlattice with ten bilayers grown by molecular beam epitaxy on a Ag(001) substrate is studied by in situ scanning tunneling microscopy (STM) and ex situ x-ray diffraction (XRD). Layer-resolved roughness parameters determined from STM images taken in various stages of the superlattice fabrication are compared with average values reported in the literature or obtained from the fits of our XRD data. Good agreement is found for the rms roughnesses describing vertical roughness and for the lateral correlation lengths characterizing correlated as well as uncorrelated interface roughness if peculiarities of STM and XRD are taken into account. We discuss in detail (i) the possible differences between the STM topography of a free surface and the morphology of a subsequently formed interface, (ii) contributions due to chemical intermixing at the interfaces, (iii) the comparison of XRD parameters averaged over all interfaces versus layer-resolved STM parameters, and (iv) the question of the coherent field of view for the determination of rms values.

Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

PubMed

Zbik, Marek S; Frost, Ray L

2010-06-15

The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction. 2010 Elsevier Inc. All rights reserved.

SAPO-34/AlMCM-41, as a novel hierarchical nanocomposite: preparation, characterization and investigation of synthesis factors using response surface methodology

NASA Astrophysics Data System (ADS)

Roohollahi, Hossein; Halladj, Rouein; Askari, Sima; Yaripour, Fereydoon

2018-06-01

SAPO-34/AlMCM-41, as a new hierarchical nanocomposite was successfully synthesized via hydrothermal and dry-gel conversion. In an experimental and statistical study, effect of five input parameters including synthesis period, drying temperature, NaOH/Si, water/dried-gel and SAPO% were investigated on range-order degree of mesochannels and the relative crystallinity. X-ray diffraction (XRD) patterns were recorded to characterize the ordered AlMCM-41 and crystalline SAPO-34 structures. Nitrogen adsorption-desorption technique, scanning electron microscopy (SEM), field-emission SEM (FESEM) equipped with an energy-dispersive X-ray spectroscopy (EDS-Map) and transmission electron microscopy (TEM) were used to study the textural properties, morphology and surface elemental composition. Two reduced polynomials were fitted to the responses with good precision. Further, based on analysis of variances, SAPO% and time duration of dry-gel conversion were observed as the most effective parameters on the composite structure. The hierarchical porosity, narrow pore size distribution, high external surface area and large specific pore volume were of interesting characteristics for this novel nanocomposite.

Surface modification of ZSM-5 zeolite: effect of cation on selective conversion of biomass-derived oil

NASA Astrophysics Data System (ADS)

Widayatno, W. B.

2017-04-01

This paper reports the surface modification of high silica ZSM-5 zeolite, particularly emphasizing the effect of cation type on selective conversion of biomass-derived oil. XRD spectra of the NaOH-treated HZSM-5 showed notable crystallinity decrease at specific crystal plane orientation. The N2-physisorption tests confirmed mesoporosity evolution as NaOH concentration was increased. NH3-desorption tests revealed a significant change on surface acidity which involved realumination and cation replacement processes. The utilization of untreated HZSM-5 as well as hierarchical NaZSM-5 for catalytic conversion of bio-oil showed the effect of cation type and mesoporosity on chemicals distribution. The untreated HZSM-5 showed high selectivity to aromatics, which degraded gradually due to deactivation and poisoning of the acid sites. Meanwhile, hierarchical NaZSM-5 showed high selectivity to phenolic compound, which became more stable for 0.4M NaOH-treated zeolite (Na04). The current findings provide an additional insight on the potentials of NaZSM-5 for bio-oil valorization.

Nonlinear electronic transport and enhanced catalytic behavior caused by native oxides on Cu nanowires

NASA Astrophysics Data System (ADS)

Hajimammadov, Rashad; Csendes, Zita; Ojakoski, Juha-Matti; Lorite, Gabriela Simone; Mohl, Melinda; Kordas, Krisztian

2017-09-01

Electrical transport properties of individual nanowires (both in axial and transversal directions) and their random networks suggest rapid oxidation when Cu is exposed to ambient conditions. The oxidation process is elucidated by thorough XRD, XPS and Raman analyzes conducted for a period of 30 days. Based on the obtained experimental data, we may conclude that first, cuprous oxide and copper hydroxide form that finally transform to cupric oxide. In electrical applications, oxidation of copper is not a true problem as long as thin films or bulk metal is concerned. However, as highlighted in our work, this is not the case for nanowires, since the oxidized surface plays quite important role in the contact formation and also in the conduction of percolated nanowire networks. On the other hand, by taking advantage of the mixed surface oxide states present on the nanowires along with their large specific surface area, we tested and found excellent catalytic activity of the oxidized nanowires in phenol oxidation, which suggests further applications of these materials in catalysis.

Synthesis of silica aerogel monoliths with controlled specific surface areas and pore sizes

NASA Astrophysics Data System (ADS)

Gao, Bingying; Lu, Shaoxiang; Kalulu, Mulenga; Oderinde, Olayinka; Ren, Lili

2017-07-01

To replace traditional preparation methods of silica aerogels, a small-molecule 1,2-epoxypropane (PO) has been introduced into the preparation process instead of using ammonia as the cross-linking agent, thus generating a lightweight, high porosity, and large surface area silica aerogel monolithic. We put forward a simple solution route for the chemical synthesis of silica aerogels, which was characterized by scanning electron microscopy (SEM), TEM, XRD, FTIR, thermogravimetric analysis (TGA) and the Brunauer-Emmett-Teller (BET) method In this paper, the effect of the amount of PO on the microstructure of silica aerogels is discussed. The BET surface areas and pore sizes of the resulting silica aerogels can be freely adjusted by changing the amount of PO, which will be helpful in promoting the development of silica aerogels to fabricate other porous materials with similar requirements. We also adopted a new organic solvent sublimation drying (OSSD) method to replace traditional expensive and dangerous drying methods such as critical point drying and freeze drying. This simple approach is easy to operate and has good repeatability, which will further facilitate actual applications of silica aerogels.

Single-step uncalcined N-TiO2 synthesis, characterizations and its applications on alachlor photocatalytic degradations

NASA Astrophysics Data System (ADS)

Suwannaruang, Totsaporn; Wantala, Kitirote

2016-09-01

The aims of this research were to synthesize nitrogen doped TiO2 (N-TiO2) photocatalysts produced by hydrothermal technique and to test the degradation performance of alachlor by photocatalytic process under UV irradiations in the effect of aging temperature and time in the preparation process. The characterizations of synthesized TiO2 such as specific surface area, particle size, phase structure and elements were analyzed by using the Brunauer-Emmett-Teller (BET) technique, Transmission Electron Microscopy (TEM), X-ray Diffractometer (XRD) and Energy Dispersive X-ray spectrometer (EDX), respectively. The Central Composite Design (CCD) was used to design the experiment to determine the optimal condition, main effects and their interactions by using specific surface area, percent alachlor removal and observed first-order rate constant as responses. The kinetic reactions of alachlor degradation were explained by using Langmuir-Hinshelwood expression to confirm the reaction took place on the surface of photocatalyst. The results showed that the effect of aging temperatures was significant on surface area, whereas aging time was insignificant. Additionally, the square term of aging temperature and interaction term were shown significant on the specific surface area as well. The highest specific surface area from response surface at aging temperature between 150-175 °C and aging time between 6-13 h was found in a range of 100-106 m2/g. The average particle size of TiO2 was similar to crystallite size. Therefore, it can be concluded that one particle has only one crystal. The element analysis has shown 10% of nitrogen in TiO2 structure that the energy band-gap about 2.95 eV was found. Although, the effects of aging temperature and time on percent alachlor removal and observed first-order rate constants were insignificant, both terms were significant in term of the square for alachlor photocatalytic degradation. The optimal condition of both responses was achieved at an aging temperature of 145 °C and aging time of 12 h.

Fabrication and characterization of iron oxide dextran composite layers

NASA Astrophysics Data System (ADS)

Iconaru, S. L.; Predoi, S. A.; Beuran, M.; Ciobanu, C. S.; Trusca, R.; Ghita, R.; Negoi, I.; Teleanu, G.; Turculet, S. C.; Matei, M.; Badea, Monica; Prodan, A. M.

2018-02-01

Super paramagnetic iron oxide nanoparticles such as maghemite have been shown to exhibit antimicrobial properties [1-5]. Moreover, the iron oxide nanoparticles have been proposed as a potential magnetically controllable antimicrobial agent which could be directed to a specific infection [3-5]. The present research has focused on studies of the surface and structure of iron oxide dextran (D-IO) composite layers surface and structure. These composite layers were deposited on Si substrates. The structure of iron oxide dextran composite layers was investigated by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) while the surface morphology was evaluated by Scanning Electron Microscopy (SEM). The structural characterizations of the iron oxide dextran composite layers revealed the basic constituents of both iron and dextran structure. Furthermore, the in vitro evaluation of the antifungal effect of the complex layers, which have been shown revealed to be active against C. albicans cells at distinct intervals of time, is exhibited. Our research came to confirm the fungicidal effect of iron oxide dextran composite layers. Also, our results suggest that iron oxide dextran surface may be used for medical treatment of biofilm associated Candida infections.

Light-induced covalent immobilization of monolayers of magnetic nanoparticles on hydrogen-terminated silicon.

PubMed

Leem, Gyu; Zhang, Shishan; Jamison, Andrew C; Galstyan, Eduard; Rusakova, Irene; Lorenz, Bernd; Litvinov, Dmitri; Lee, T Randall

2010-10-01

Specifically tailored ω-alkenyl-1-carboxylic acids were synthesized for use as surfactants in the single-step preparation of manganese ferrite (MnFe2O4) nanoparticles (NPs). Monodisperse manganese ferrite NPs terminated with ω-alkenyl moieties were prepared via a one-pot reaction at high temperature without the need of ligand exchange. Using this approach, simple adjustment of the rate of heating allowed precise tuning of the size of the nanoparticles, which were characterized in bulk form by transmission electron microscopy (TEM), Fourier-transform infrared (FT-IR) spectroscopy, and X-ray diffraction (XRD). These surfactant-coated magnetic nanoparticles were then deposited onto hydrogen-terminated silicon(111) wafers and covalently anchored to the surface by UV-initiated covalent bonding. Analysis by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) confirmed that the UV treatment led to covalent immobilization of the NPs on the silicon surface with a consistent packing density across the surface. The magnetic properties of the stable, surface-bound nanoparticle arrays were characterized using a superconducting quantum interference device (SQUID) magnetometer. The materials and methods described here are being developed for use in bit-patterned ultrahigh density magnetic recording media and nanoscale biomagnetic sensing.

Effects of copper-precursors on the catalytic activity of Cu/graphene catalysts for the selective catalytic oxidation of ammonia

NASA Astrophysics Data System (ADS)

Li, Jingying; Tang, Xiaolong; Yi, Honghong; Yu, Qingjun; Gao, Fengyu; Zhang, Runcao; Li, Chenlu; Chu, Chao

2017-08-01

Different copper-precursors were used to prepare Cu/graphene catalysts by an impregnation method. XRD, Raman spectra, TEM, BET, XPS, H2-TPR, NH3-TPD, DRIFTS and catalytic activity test were used to characterize and study the effect of precursors on the catalytic activity of Cu/graphene catalysts for NH3-SCO reaction. The large specific surface area of Cu/graphene catalysts and high dispersion of the metal particles on the graphene caused the well catalytic activity of NH3-SCO reaction. Compared to Cu/GE(AC), Cu/GE(N) showed better catalytic performance, and the complete NH3 removal efficiency was obtained at 250 °C with N2 selectivity of 85%. The copper-precursors had influence on the distribution of surface Cu species and further affected the catalytic activity of Cu/GE catalysts. The more amount of surface Cu species and highly dispersed CuO particles on the graphene surface formed by using copper nitrate as precursor could significantly improve the reducibility of catalysts and enhance NH3 adsorption, thereby improving the catalytic activity of Cu/graphene catalyst.

Insitu grown superhydrophobic Zn-Al layered double hydroxides films on magnesium alloy to improve corrosion properties

NASA Astrophysics Data System (ADS)

Zhou, Meng; Pang, Xiaolu; Wei, Liang; Gao, Kewei

2015-05-01

A hierarchical superhydrophobic zinc-aluminum layered double hydroxides (Zn-Al LDHs) film has been fabricated on a magnesium alloy substrate via a facile hydrothermal crystallization method following chemical modification. The characteristics of the films were investigated by X-ray diffraction (XRD), scanning electronic microscope (SEM), and energy dispersive spectroscopy (EDS). XRD patterns and SEM images showed that the micro/nanoscale hierarchical LDHs film surfaces composed of ZnO nanorods and Zn-Al LDHs nanowalls structures. The static contact angle (CA) for the prepared surfaces was observed at around 165.6°. The corrosion resistance of the superhydrophobic films was estimated by electrochemical impedance spectroscopy (EIS) and potentiondynamic polarization measurement. EIS and polarization measurements revealed that the superhydrophobic Zn-Al LDHs coated magnesium alloy had better corrosion resistance in neutral 3.5 wt.% NaCl solution.

Optimization Study of Pulsed DC Nitrogen-Hydrogen Plasma in the Presence of an Active Screen Cage

NASA Astrophysics Data System (ADS)

Saeed, A.; W. Khan, A.; F., Jan; U. Shah, H.; Abrar, M.; Zaka-Ul-Islam, M.; Khalid, M.; Zakaullah, M.

2014-05-01

A glow discharge plasma nitriding reactor in the presence of an active screen cage is optimized in terms of current density, filling pressure and hydrogen concentrations using optical emission spectroscopy (OES). The samples of AISI 304 are nitrided for different treatment times under optimum conditions. The treated samples were analyzed by X-ray diffraction (XRD) to explore the changes induced in the crystallographic structure. The XRD pattern confirmed the formation of iron and chromium nitrides arising from incorporation of nitrogen as an interstitial solid solution in the iron lattice. A Vickers microhardness tester was used to evaluate the surface hardness as a function of treatment time (h). The results showed clear evidence of improved surface hardness and a substantial amount of decrease in the treatment time compared with the previous work.

Physicochemical characterizations of nano-palm oil fuel ash

NASA Astrophysics Data System (ADS)

Rajak, Mohd Azrul Abdul; Majid, Zaiton Abdul; Ismail, Mohammad

2015-07-01

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m2/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.

Fabrication of Co0.5Ni0.5CrxFe2-xO4 materials via sol-gel method and their characterizations

NASA Astrophysics Data System (ADS)

Kadam, R. H.; Birajdar, A. P.; Alone, Suresh T.; Shirsath, Sagar E.

2013-02-01

Co0.5Ni0.5CrxFe2-xO4 nanoparticles have been designed by the sol-gel auto combustion method, using nitrates of the respective metal ions, and citric acid as the starting materials. The process takes only a few minutes to obtain as-received Cr-substituted Co-Ni ferrite powders. X-ray diffraction (XRD), vibrational sample magnetometer (VSM), transmission electron microscopy (TEM) are utilized in order to study the effect of variation in the Cr3+ substitution and its impact on particle size, lattice constant, specific surface area, cation distribution and magnetic properties. Lattice parameter, particle size found to decrease with increasing Cr3+ content, whereas specific surface area showed increasing trend with the Cr3+ substitution. Cation distribution indicates that the Cr, Co and Ni ions show preference toward octahedral [B] site, whereas Fe occupies both tetrahedral (A) and octahedral [B] sites. Saturation magnetization (MS) decreased from 65.1 to 40.6 emu/g with the increase in Cr3+ substitution. However, Coercivity increased from 198 to 365 Oe with the Cr3+ substitution.

Preparation of zeolite supported TiO{sub 2}, ZnO and ZrO{sub 2} and the study on their catalytic activity in NO{sub x} reduction and 1-pentanol dehydration

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

Fatimah, Is

Preparation of zeolite supported TiO{sub 2}, ZnO and ZrO{sub 2} and their catalytic activity was studied. Activated natural zeolite from Indonesia was utilized for the preparation and catalytic activity test on NO{sub x} reduction by NH{sub 3} and also 1-pentanol dehydration were examined. Physicochemical characterization of materials was studied by x-ray diffraction (XRD) measurement, scanning electron microscope, solid acidity determination and also gas sorption analysis. The results confirmed that the preparation gives some improvements on physicochemical characters suitable for catalysis mechanism in those reactions. Solid acidity and specific surface area contributed significantly to the activity.

Influence of Synthesis Temperature on the Growth and Surface Morphology of Co₃O₄ Nanocubes for Supercapacitor Applications.

PubMed

Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Sanjay, Kali; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

2017-10-31

A facile hydrothermal route to control the crystal growth on the synthesis of Co₃O₄ nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co₃O₄ nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co₃O₄ synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes.

Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

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

Pakharukova, V.P., E-mail: verapakh@catalysis.ru; Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk; Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol–gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, includingmore » anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor. - Graphical abstract: Pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. - Highlights: • Silica-doped boehmites were prepared by sol–gel method with supercritical drying. • Ultrathin two-dimensional crystallites of pseudoboehmite were obtained. • Changes in structure and morphology upon calcination were studied. • Simulation of XRD patterns was performed with use of the Debye Scattering Equation. • Thermal stability of alumina depended on morphology inherited from pseudoboehmite.« less

Characterization of a Diamond Ground Y-TZP and Reversion of the Tetragonal to Monoclinic Transformation.

PubMed

Candido, L M; Fais, Lmg; Ferreira, E B; Antonio, S G; Pinelli, Lap

To characterize the surface of an yttria-stabilized zirconia (Y-TZP) ceramic after diamond grinding in terms of its crystalline phase, morphology, mean roughness (Ra), and wettability as well as to determine a thermal treatment to reverse the resulting tetragonal to monoclinic (t-m) transformation. Y-TZP specimens were distributed into different groups according to the actions (or no action) of grinding and irrigation. Grinding was accomplished using a diamond stone at a low speed. The samples were characterized by x-ray diffraction (XRD), scanning electron microscopy, goniometry, and profilometry. In situ high-temperature XRD was used to determine an annealing temperature to reverse the t-m transformation. Ra was submitted to the Kruskal-Wallis test, followed by the Dunn test (α=0.05). The volume fraction of the monoclinic phase and contact angle were submitted to one-way analysis of variance, followed by the Tukey test (α=0.05). Monoclinic zirconia was observed on the surface of samples after dry and wet grinding with a diamond stone. The volume fraction of the monoclinic phase was smaller on the dry ground samples (3.6%±0.3%) than on the wet ground samples (5.6%±0.3%). High-temperature XRD showed reversion of the t-m phase transformation, which started at 700°C and completed at 800°C in a conventional oven. Grinding with a diamond stone partially transformed the crystalline phase on the surface of a Y-TZP ceramic from tetragonal to monoclinic zirconia while simultaneously increasing the surface roughness and wettability. The t-m transformation could be reversed by heat treatment at 800°C or 900°C for 60 minutes or 1000°C for 30 minutes.

Effect of Arsenic on the Formation and Adsorption Property of Ferric Hydroxide Precipitates in ZVI Treatment

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

Peng, Xing; Xi, Beidou; Zhao, Ying

Treatment of arsenic by zerovalent iron (ZVI) has been studied extensively. However, the effect of arsenic on the formation of ferric hydroxide precipitates in the ZVI treatment has not been investigated. We discovered that the specific surface area (ca. 187 m2/g) and arsenic content (ca. 67 mg/g) of the suspended solids (As-containing solids) generated in the ZVI treatment of arsenic solutions were much higher than the specific surface area (ca. 37 m2/g) and adsorption capacity (ca.12 mg/g) of the suspended solids (As-free solids) generated in the arsenic-free solutions. Arsenic in the As-containing solids was much more stable than the adsorbedmore » arsenic in As-free solids. XRD, SEM, TEM, and selected area electron diffraction (SAED) analyses showed that the As-containing solids consisted of amorphous nanoparticles, while the As-free solids were composed of micron particles with weak crystallinity. Extended X-ray absorption fine structure (EXAFS) analysis determined that As(V) was adsorbed on the As-containing suspended solids and magnetic solid surfaces through bidentate binuclear complexation; and As(V) formed a mononuclear complex on the As-free suspended solids. The formation of the surface As(V) complexes retarded the bonding of free FeO6 octahedra to the oxygen sites on FeO6 octahedral clusters and prevented the growth of the clusters and their development into 3-dimensional crystalline phases.« less

Structural and surface properties of CuO-ZnO-Cr{sub 2}O{sub 3} catalysts and their relationship with selectivity to higher alcohol synthesis

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

Campos-Martin, J.M.; Fierro, J.L.G.; Guerrero-Ruiz, A.

1995-10-01

A series of copper-zinc-chromium catalysts of different compositions and calcination temperatures has been prepared, characterized by several techniques (BET specific surface area, XRD, gravimetric TPR, TPD-CO, and XPS), and tested under high alcohol synthesis (HAS) conditions. CO hydrogenation was carried out at reaction temperatures of 523-598 K and 50 bar total pressure. The influence of catalyst composition, calcination temperature, and surface characteristics on the HAS selectivity was studied. The optimum HAS yields were found in the low Cr content region, but chromium was needed. Although chromium oxide does not seem to be involved in the catalytic site, its presence inmore » the catalyst composition is essential, owing to the larger specific surfaces and catalyst stability obtained at the highest reaction temperatures. For low Cr content composition, the temperature-programmed reduction (TPR) profiles were shifted to higher temperatures and simultaneously larger CO{sub 2} amounts were found in the temperature-programmed desorption profiles of adsorbed CO (TPD-CO). Photoelectron spectra (XPS) revealed that the oxidation state of copper is Cu{sup 2+} in the calcined catalysts and Cu{sup O} in the reduced ones; Cu{sup +} was only stabilized in a CuCr{sub 2}O{sub 4} spinel in the Cr-rich catalysts. These features derived from catalyst characterization are discussed in the framework of the catalytic behaviour for HAS synthesis. 53 refs., 7 figs., 4 tabs.« less

Graphite intercalated polyaniline composite with superior anticorrosive and hydrophobic properties, as protective coating material on steel surfaces

NASA Astrophysics Data System (ADS)

Rathnayake, R. M. N. M.; Mantilaka, M. M. M. G. P. G.; Hara, Masanori; Huang, Hsin-Hui; Wijayasinghe, H. W. M. A. C.; Yoshimura, Masamichi; Pitawala, H. M. T. G. A.

2017-07-01

Solid polymer composite systems are widely being used for potential technological applications in secondary energy sources and electrochromic devices. In this study, we synthesized and characterized a composite material composed of polyaniline (PANI) and natural needle platy (NPG) vein graphite. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), cyclic voltammetry (CV), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), micro-Raman analysis, thermogravimetric and differential thermal analysis (TGA/DTA), transmission electron microscopy (TEM) were used to study the structural and electrochemical properties of the prepared PANI/NPG graphite composite. XPS, FTIR, and micro-Raman analysis confirmed the existence of relevant functional groups and bonding in the prepared PANI/NPG composite material. The composite shows a very low corrosion rate, approximately 29 μm per year, and high hydrophobicity on steel surfaces, which helps to prevent the corrosion due to O2 penetration towards the metal surface. It indicates that the composite can be used as a high potential surface coating material to anticorrosion. The specific capacitance of PANI/NPG composite is 833.3 F g-1, which is higher than that of PANI. This synergistic electrical performance result proves the prepared PANI/NPG graphite composite as a suitable protective coating material for steel surfaces.

Correlation between the microstructures of graphite oxides and their catalytic behaviors in air oxidation of benzyl alcohol.

PubMed

Geng, Longlong; Wu, Shujie; Zou, Yongcun; Jia, Mingjun; Zhang, Wenxiang; Yan, Wenfu; Liu, Gang

2014-05-01

A series of graphite oxide (GO) materials were obtained by thermal treatment of oxidized natural graphite powder at different temperatures (from 100 to 200 °C). The microstructure evolution (i.e., layer structure and surface functional groups) of the graphite oxide during the heating process is studied by various characterization means, including XRD, N2 adsorption, TG-DTA, in situ DRIFT, XPS, Raman, TEM and Boehm titration. The characterization results show that the structures of GO materials change gradually from multilayer sheets to a transparent ultrathin 2D structure of the carbon sheets. The concentration of surface COH and HOCO groups decrease significantly upon treating temperature increasing. Benzyl alcohol oxidation with air as oxidant source was carried out to detect the catalytic behaviors of different GO materials. The activities of GO materials decrease with the increase of treating temperatures. It shows that the structure properties, including ultrathin sheets and high specific surface area, are not crucial factors affecting the catalytic activity. The type and amount of surface oxygen-containing functional groups of GO materials tightly correlates with the catalytic performance. Carboxylic groups on the surface of GO should act as oxidative sites for benzyl alcohol and the reduced form could be reoxidized by molecular oxygen. Copyright © 2014 Elsevier Inc. All rights reserved.

The effect of nanoparticles size on photocatalytic and antimicrobial properties of Ag-Pt/TiO2 photocatalysts

NASA Astrophysics Data System (ADS)

Zielińska-Jurek, Anna; Wei, Zhishun; Wysocka, Izabela; Szweda, Piotr; Kowalska, Ewa

2015-10-01

Ag-Pt-modified TiO2 nanocomposites were synthesized using the sol-gel method. Bimetallic modified TiO2 nanoparticles exhibited improved photocatalytic activity under visible-light irradiation, better than monometallic Ag/TiO2 and Pt/TiO2 nanoparticles (NPs). All modified powders showed localized surface plasmon resonance (LSPR) in visible region. The photocatalysts' characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption (BET method for specific surface area) showed that sample with the highest photocatalytic activity had anatase structure, about 93 m2/g specific surface area, maximum plasmon absorption at ca. 420 nm and contained small NPs of silver of 6 nm and very fine platinum NPs of 3 nm. The photocatalytic activity was estimated by measuring the decomposition rate of phenol in 0.2 mM aqueous solution under Vis and UV/vis light irradiation. It was found that size of platinum was decisive for the photocatalytic activity under visible light irradiation, i.e., the smaller Pt NPs were, the higher was photocatalytic activity. While, antimicrobial activities, estimated for bacteria Escherichia coli and Staphylococcus aureus, and pathogenic fungi belonging to Candida family, were only observed for photocatalysts containing silver, i.e., Ag/TiO2 and Ag-Pt/TiO2 nanocomposites.

Effect of substrate temperature in the synthesis of BN nanostructures

NASA Astrophysics Data System (ADS)

Sajjad, M.; Zhang, H. X.; Peng, X. Y.; Feng, P. X.

2011-06-01

Boron nitride (BN) nanostructures were grown on molybdenum discs at different substrate temperatures using the short-pulse laser plasma deposition technique. Large numbers of randomly oriented nanorods of fiber-like structures were obtained. The variation in the length and diameter of the nanorods as a function of the substrate temperature was systematically studied. The surface morphologies of the samples were studied using scanning electron microscopy. Energy dispersive x-ray spectroscopy confirmed that both the elements boron and nitrogen are dominant in the nanostructure. The x-ray diffraction (XRD) technique was used to analyse BN phases. The XRD peak that appeared at 26° showed the presence of hexagonal BN phase, whereas the peak at 44° was related to cubic BN content in the samples. Raman spectroscopic analysis showed vibrational modes of sp2- and sp3-type bonding in the sample. The Raman spectra agreed well with XRD results.

Improvement of the overall performances of LiMn{sub 2}O{sub 4} via surface-modification by polypyrrole

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

Wang, Ting; Wang, Wan; Zhu, Ding

2015-11-15

Graphical abstract: Polypyrrole(PPy) film has improved the rate performance of LiMn{sub 2}O{sub 4} efficiently due to its excellent conductivity. PPy@LiMn{sub 2}O{sub 4} could provide more energy under the higher power than pristine LMO. - Highlights: • The PPy layer on the surface of LMO particles hasn’t been studied in LiMn{sub 2}O{sub 4} so far. • The solvent in the synthesis process of PPy@LMO is absolute ethyl alcohol. • The differences of surface-modification between the PPy and PI for LMO. • The analyses of rate performances are through specific power. - Abstract: Polypyrrole (PPy) is an excellent conductive polymer and themore » study on its utilization in the surface modification of the LiMn{sub 2}O{sub 4} (LMO) is few. In this work, the structure, morphology and electrochemical performance of surface-modified LiMn{sub 2}O{sub 4} composites with PPy and polyimides (PI) were discussed. The crystal structure, chemical bonds and morphology were characterized through X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), respectively. Moreover, the specific power and cycling performance were tested at room and high (55 °C) temperature. The PPy@LMO (surface-modified LMO composites with PPy) shows better performances than the pristine LMO. The addition of PPy not only weakens the corrosion caused by electrolyte, but also improves the discharge capacity at higher rates. The charge transfer resistance of the PPy@LMO is much lower than that of the pristine LMO after cycling.« less

Morphological, chemical and structural characterisation of deciduous enamel: SEM, EDS, XRD, FTIR and XPS analysis.

PubMed

Zamudio-Ortega, C M; Contreras-Bulnes, R; Scougall-Vilchis, R J; Morales-Luckie, R A; Olea-Mejía, O F; Rodríguez-Vilchis, L E

2014-09-01

The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.

The influence of Ce doping of titania on the photodegradation of phenol.

PubMed

Martin, Marcela V; Villabrille, Paula I; Rosso, Janina A

2015-09-01

Pure and cerium-doped [0.05, 0.1, 0.3, 0.5, and 1.0 Ce nominal atomic % (at.%)] TiO2 was synthesized by the sol-gel method. The obtained catalysts were characterized by X-ray diffraction (XRD), UV-visible diffused reflectance spectroscopy (DRS), Raman, and BET surface area measurement. The photocatalytic activity of synthesized samples for the oxidative degradation of phenol in aqueous suspension was investigated. The content of Ce in the catalysts increases both the transition temperature for anatase to rutile phase transformation and the specific surface area, and decreases the crystallite size of anatase phase, the crystallinity, and the band gap energy value. The material with higher efficiency corresponds to 0.1 Ce nominal at.%. Under irradiation with 350 nm lamps, the degradation of phenol could be described as an exponential trend, with an apparent rate constant of (9.1 ± 0.6) 10(-3) s(-1) (r(2) = 0.98). Hydroquinone was identified as the main intermediate.

Synthesis of Co3O4/TiO2 composite by pyrolyzing ZIF-67 for detection of xylene

NASA Astrophysics Data System (ADS)

Bai, Shouli; Tian, Ke; Tian, Ye; Guo, Jun; Feng, Yongjun; Luo, Ruixian; Li, Dianqing; Chen, Aifan; Liu, Chung Chiun

2018-03-01

Co3O4/TiO2 composites with p-n heterojunction have been successfully prepared by pyrolyzing sacrificial template of Ti ion loaded Co-based Zeolitic imidazolate framework (ZIF-67). The structure and morphology of composite have been characterized by means of the analysis of XRD, FESEM, HRTEM and XPS spectra. The composite with a Co/Ti molar ratio of 4:1 exhibits the maximum sensing response of 6.17-50 ppm xylene, which is 5 times higher than pristine Co3O4. Moreover, Co3O4/TiO2 composite also shows good selectivity, long-term stability and rapid response and recovery. Such excellent sensing performances are attributed to material porous structure, high specific surface and the formation of abundant p-n heterojunction that permits the gas adsorption, diffusion and surface reaction and then improve the gas sensing performance. This work develops a promising synthesized approach of metal oxide composites for broader MOFs application in gas sensor field.

Chemical degradation of trimethyl phosphate as surrogate for organo-phosporus pesticides on nanostructured metal oxides

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

Štengl, Václav, E-mail: stengl@iic.cas.cz; Henych, Jiří; Grygar, Tomáš

Nanostructured TiO{sub 2} and mixed oxides of Ti and Fe, Hf, In, Mn or Zr -were prepared by homogeneous hydrolysis of aqueous solution of metal sulphates with urea. The oxides were characterised by X-ray powder diffraction (XRD), scanning electron microscopy, particle size distribution, surface area and porosity. The oxide materials consists of a few nanometre primary crystals (mainly anatase) arranged in a few micrometre regular spherical agglomerates with specific surface area 133–511 m{sup 2} g{sup −1}. The FTIR diffuse spectroscopy was used for monitoring chemical degradation of trimethylphosphate (TMP) as a surrogate for organo-phosphorus pesticides under ambient and higher temperatures.more » Undoped TiO{sub 2} and Ti,Mn-mixed oxide were most active in cleavage (hydrolysis) of CH{sub 3}O from TMP at room temperature and 100 °C. Cleavage of CH{sub 3}O in the other studied mixed oxides was not complete until temperature exceeds the boiling point of TMP.« less

Native defects in silver orthophosphate and their effects on photocatalytic activity under visible light irradiation

NASA Astrophysics Data System (ADS)

Sulaeman, Uyi; Hermawan, Dadan; Andreas, Roy; Abdullah, Ahmad Zuhairi; Yin, Shu

2018-01-01

Native defects in silver orthophosphate could be generated by simple co-precipitation method under ethanol-aqueous solution using AgNO3 and Na2HPO4.12H2O. AgNO3 ethanol-aqueous solution with the ethanol contents of 0%, 25%, 50%, 75%, 90% and 100% was reacted with Na2HPO4 aqueous solution. The produced catalysts were characterized using XRD, DRS, FE-SEM, BET specific surface area and XPS. The increase of ethanol content in the synthesis process decreased the Ag/P atomic ratio of Ag3PO4. The native defects of silver vacancy might be generated on the surface of Ag3PO4. The activity of Ag3PO4 for Rhodamine B degradation dramatically increased by 5.8 times higher compared to that of the pristine Ag3PO4. The defect states of Ag vacancies enhanced the separation of electron-hole pairs, leading to the improvement of photocatalytic activity.

Sol-gel synthesis and adsorption properties of mesoporous manganese oxide

NASA Astrophysics Data System (ADS)

Ivanets, A. I.; Kuznetsova, T. F.; Prozorovich, V. G.

2015-03-01

Sol-gel synthesis of mesoporous xerogels of manganese oxide with different phase compositions has been performed. The manganese oxide sols were obtained by redox reactions of potassium permanganate with hydrogen peroxide or manganese(II) chloride in aqueous solutions. The isotherms of the low-temperature adsorption-desorption of nitrogen with manganese oxide xerogels treated at 80, 200, 400, and 600°C were measured. The samples were studied by electron microscopy and thermal and XRD analysis. The phase transformation and the changes in the adsorption and capillary-condensation properties of manganese oxide were shown to depend on the sol synthesis conditions and the temperature of the thermal treatment of the gel. The X-ray amorphous samples heated at 80°C were shown to have low values of the specific surface; at higher temperatures, the xerogel crystallized into mixed phases with various compositions and its surface area increased at 200-400°C and decreased at 600°C.

Studies on the sensing behaviour of nanocrystalline CuGa(2)O(4) towards hydrogen, liquefied petroleum gas and ammonia.

PubMed

Biswas, Soumya Kanti; Sarkar, Arpita; Pathak, Amita; Pramanik, Panchanan

2010-06-15

In the present article, the gas sensing behaviour of nanocrystalline CuGa(2)O(4) towards H(2), liquefied petroleum gas (LPG) and NH(3) has been reported for the first time. Nanocrystalline powders of CuGa(2)O(4) having average particle sizes in the range of 30-60nm have been prepared through thermal decomposition of an aqueous precursor solution comprising copper nitrate, gallium nitrate and triethanol amine (TEA), followed by calcination at 750 degrees C for 2h. The synthesized nanocrystalline CuGa(2)O(4) powders have been characterised through X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM) study, energy dispersive X-ray (EDX) analysis and BET (Brunauer-Emmett-Teller) surface area measurement. The synthesized CuGa(2)O(4) having spinel structure with specific surface area of 40m(2)/g exhibits maximum sensitivity towards H(2), LPG, and NH(3) at 350 degrees C.

Preparation and catalytic activities of LaFeO3 and Fe2O3 for HMX thermal decomposition.

PubMed

Wei, Zhi-Xian; Xu, Yan-Qing; Liu, Hai-Yan; Hu, Chang-Wen

2009-06-15

Perovskite-type LaFeO(3) and alpha-Fe(2)O(3) with high specific surface areas were directly prepared with appropriate stearic acid-nitrates ratios by a novel stearic acid solution combustion method. The obtained powders were characterized by XRD, FT-IR and XPS techniques. The catalytic activities of perovskite-type LaFeO(3) and alpha-Fe(2)O(3) for the thermal decomposition of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) were investigated by TG and TG-EGA techniques. The experimental results show that the catalytic activity of perovskite-type LaFeO(3) was much higher than that of alpha-Fe(2)O(3) because of higher concentration of surface-adsorbed oxygen (O(ad)) and hydroxyl of LaFeO(3). The study points out a potential way to develop new and more active perovskite-type catalysts for the HMX thermal decomposition.

Study the target effect on the structural, surface and optical properties of TiO2 thin film fabricated by RF sputtering method

NASA Astrophysics Data System (ADS)

Vyas, Sumit; Tiwary, Rohit; Shubham, Kumar; Chakrabarti, P.

2015-04-01

The effect of target (Ti metal target and TiO2 target) on Titanium Dioxide (TiO2) thin films grown on ITO coated glass substrate by RF magnetron sputtering has been investigated. A comparative study of both the films was done in respect of crystalline structure, surface morphology and optical properties by using X-ray diffractometer (XRD), Atomic Force Microscopy (AFM) studies and ellipsometric measurements. The XRD results confirmed the crystalline structure and indicated that the deposited films have the intensities of anatase phase. The surface morphology and roughness values indicated that the film using Ti metal target has a smoother surface and densely packed with grains as compared to films obtained using TiO2 target. A high transmission in the visible region, and direct band gap of 3.67 eV and 3.75 eV for films derived by using Ti metal and TiO2 target respectively and indirect bandgap of 3.39 eV for the films derived from both the targets (Ti metal and TiO2 target) were observed by the ellipsometric measurements.

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

DOE PAGES

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro; ...

2018-06-12

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

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

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

Field-induced polarization rotation and phase transitions in 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 piezoceramics observed by in situ high-energy x-ray scattering

NASA Astrophysics Data System (ADS)

Hou, Dong; Usher, Tedi-Marie; Fulanovic, Lovro; Vrabelj, Marko; Otonicar, Mojca; Ursic, Hana; Malic, Barbara; Levin, Igor; Jones, Jacob L.

2018-06-01

Changes to the crystal structure of 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic C m at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF results show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. This study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-x PT piezoceramics.

Synthesis and catalytic activity of polysaccharide templated nanocrystalline sulfated zirconia

NASA Astrophysics Data System (ADS)

Sherly, K. B.; Rakesh, K.

2014-01-01

Nanoscaled materials are of great interest due to their unique enhanced optical, electrical and magnetic properties. Sulfate-promoted zirconia has been shown to exhibit super acidic behavior and high activity for acid catalyzed reactions. Nanocrystalline zirconia was prepared in the presence of polysaccharide template by interaction between ZrOCl2ṡ8H2O and chitosan template. The interaction was carried out in aqueous phase, followed by the removal of templates by calcination at optimum temperature and sulfation. The structural and textural features were characterized by powder XRD, TG, SEM and TEM. XRD patterns showed the peaks of the diffractogram were in agreement with the theoretical data of zirconia with the catalytically active tetragonal phase and average crystalline size of the particles was found to be 9 nm, which was confirmed by TEM. TPD using ammonia as probe, FTIR and BET surface area analysis were used for analyzing surface features like acidity and porosity. The BET surface area analysis showed the sample had moderately high surface area. FTIR was used to find the type species attached to the surface of zirconia. UV-DRS found the band gap of the zirconia was found to be 2.8 eV. The benzylation of o-xylene was carried out batchwise in atmospheric pressure and 433K temperature using sulfated zirconia as catalyst.

Stable superhydrophilic coating on superhydrophobic porous media by functionalized nanoparticles

NASA Astrophysics Data System (ADS)

Khazaei, Masoud; Taghi Sadeghi, Mohammad; Sadat Hosseini, Marzieh

2018-01-01

In this study, the hydrophilicity property of TiO2 nano-coating was improved by zinc acetate-assisted sol-gel method. The stable superhydrophilic coating was fabricated on a superhydrophobic mineral rock surface. The wettability of surface before and after coating was characterized by contact angle measurements. The n-heptane and water droplet contact angle was 0° and 168° respectively, so the untreated rock was superhydrophobic. After nano-treatment, the n-heptane and water contact angle changed to 172° and 0° respectively, so the superhydrophilic coating was formed on the superhydrophobic surface. The thermal, mechanical and salinity stability of the fabricated coatings was investigated. The coatings had high thermal and salinity stability; they also had moderate mechanical stability that was evaluated by abrasion test. The morphology and composition of synthesized nanoparticles were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy and x-ray diffraction (XRD) analyses. Characterization of the coated surfaces was conducted by SEM and XRD analyses. Applications of these nano-coatings include surfaces where cleanliness is paramount such as in hospitals as well as the protection of public monuments and building facades from weathering. Novel industrial application includes wettability alteration of oil wet carbonate rock for enhanced oil recovery.

Surface structure of coherently strained ceria ultrathin films

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

Shi, Yezhou; Stone, Kevin H.; Guan, Zixuan

2016-11-14

Cerium oxide, or ceria, is an important material for solid oxide fuel cells and water splitting devices. Although the ceria surface is active in catalytic and electrochemical reactions, how its catalytic properties are affected by the surface structure under operating conditions is far from understood. We investigate the structure of the coherently strained CeO 2 ultrathin films on yttria-stabilized zirconia (001) single crystals by specular synchrotron x-ray diffraction (XRD) under oxidizing conditions as a first step to study the surface structure in situ. An excellent agreement between the experiment data and the model is achieved by using a “stacks andmore » islands” model that has a two-component roughness. One component is due to the tiny clusters of nanometer scale in lateral dimensions on each terrace, while the other component is due to slightly different CeO 2 thickness that span over hundreds of nanometers on neighboring terraces. We attribute the nonuniform thickness to step depairing during the thin film deposition that is supported by the surface morphology results on the microscopic level. Importantly, our model also shows that the polarity of the ceria surface is removed by a half monolayer surface coverage of oxygen. In conclusion, the successful resolution of the ceria surface structure using in situ specular synchrotron XRD paves the way to study the structural evolution of ceria as a fuel cell electrode under catalytically relevant temperatures and gas pressures.« less

Synthesis H-Zeolite catalyst by impregnation KI/KIO3 and performance test catalyst for biodiesel production

NASA Astrophysics Data System (ADS)

Widayat, W.; Rizky Wicaksono, Adit; Hakim Firdaus, Lukman; Okvitarini, Ndaru

2016-02-01

The objective of this research is to produce H-catalyst catalyst that was impregnated with KI/KIO3. The catalyst was analyzed about surface area, X-Ray Diffraction (XRD) and performance test of catalyst for biodiesel production. An H-Zeolite catalyst was synthesized from natural zeolite with chemical treatment processing, impregnation KI/KIO3 and physical treatment. The results shows that the surface area of the catalyst by 27.236 m2/g at a concentration of 5% KI. XRD analysis shows peak 2-θ at 23.627o indicating that KI was impregnated on H-zeolite catalyst. The catalyst was tested in production of biodiesel using palm oil with conventional methods for 3 hour at temperature of 70-80 oC. The result for conversion Fatty Acid Methyl Ester (FAME) reached maximum value on 87.91% under production process using catalyst 5% KIO3-H zeolite.

In-vitro bioactivity of zirconia doped borosilicate glasses

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

Samudrala, Rajkumar; Azeem, P. Abdul, E-mail: rk.satyaswaroop@gmail.com, E-mail: drazeem2002@yahoo.com

2015-06-24

Glass composition 31B{sub 2}O{sub 3}-20SiO{sub 2}-24.5Na{sub 2}O-(24.5-x) CaO-xZrO{sub 2} x=1,2,3,4,5 were prepared by melt-quenching Technique. The formation of hydroxyapatite layer on the surface of glasses after immersion in simulated body fluid (SBF) was explored through XRD, Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM-EDX) analyses. In this report, we observed that hydroxyapatite formation for 5days of immersion time. Also observed that with increasing the immersion time up to 15days, higher amount of hydroxyapatite layer formation on the surface of glasses. The varying composition of zirconia in glass samples influences shown by XRD, FTIR studies. The present results indicate that,more » in-vitro bioactivity of glasses decreased with increasing zirconia incorporation.« less

Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis.

PubMed

Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

2015-03-05

ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigations of the Failure in Boilers Economizer Tubes Used in Power Plants

NASA Astrophysics Data System (ADS)

Moakhar, Roozbeh Siavash; Mehdipour, Mehrad; Ghorbani, Mohammad; Mohebali, Milad; Koohbor, Behrad

2013-09-01

In this study, failure of a high pressure economizer tube of a boiler used in gas-Mazut combined cycle power plants was studied. Failure analysis of the tube was accomplished by taking into account visual inspection, thickness measurement, and hardness testing as well as microstructural observations using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and x-ray diffraction (XRD). Optical microscopy images indicate that there is no phase transformation during service, and ferrite-pearlite remained. The results of XRD also revealed Iron sulfate (FeSO4) and Iron hydroxide sulfate (FeOH(SO4)) phases formed on the steel surface. A considerable amount of Sulfur was also detected on the outer surface of the tube by EDS analysis. Dew-point corrosion was found to be the principal reason for the failure of the examined tube while it has been left out-of-service.

Evolution of microstructure and surface topography of gold thin films under thermal annealing

NASA Astrophysics Data System (ADS)

Dash, P.; Rath, H.; Dash, B. N.; Mallick, P.; Basu, T.; Som, T.; Singh, U. P.; Mishra, N. C.

2012-07-01

In the present study, we probe into evolution of microstructure and surface morphology of gold thin films of 10 to 50 nm thickness deposited on Si (100) substrate by thermal evaporation method. These films were annealed at 250°C under vacuum. The as-deposited and annealed films were characterized by glancing angle X-Ray diffraction (GAXRD) and atomic force microscopy (AFM), techniques. XRD indicated improvement of crystallinity up to 2 hours of annealing and degradation of the same thereafter. In agreement with XRD result, the grain size distribution histogram obtained from AFM indicated grain growth with annealing time up to 2 hours and saturation or decrease of grain size thereafter. The observed result is explained by the occurrence of two competing phenomena like roughening induced grain growth and smoothening induced inhibition of grain growth with increasing annealing time.

Synthesis, crystal structure, NLO and Hirshfeld surface analysis of 1,2,3-triazolyl chalcone single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped brown coloured single crystal of the title compound was grown by slow evaporation technique using methanol as solvent. The grown crystal was characterized using FT-IR, Single crystal XRD, UV-visible and NLO studies. Crystal structure was confirmed by FT-IR study and the functional groups were identified. XRD study reveals that the crystal belongs to orthorhombic crystal system with pnaa space group and the corresponding cell parameters were calculated. UV-visible spectrum shows that the crystal is transparent in the entire visible region and absorption takes place in the UV-range. NLO efficiency of the crystal obtained 0.66 times that of urea was determined by SHG test. The intermolecular interaction and percentage contribution of each individual atom in the crystal lattice was quantized using Hirshfeld surface and 2D finger print analysis.

Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials

NASA Technical Reports Server (NTRS)

Rampe, Elizabeth B.; Morris, Richard V.; Chipera, Steve; Bish, David L.; Bristow, Thomas; Archer, Paul Douglas; Blake, David; Achilles, Cherie; Ming, Douglas W.; Vaniman, David;

Spectral identification and quantification of salts in the Atacama Desert

NASA Astrophysics Data System (ADS)

Harris, J. K.; Cousins, C. R.; Claire, M. W.

2016-10-01

Salt minerals are an important natural resource. The ability to quickly and remotely identify and quantify salt deposits and salt contaminated soils and sands is therefore a priority goal for the various industries and agencies that utilise salts. The advent of global hyperspectral imagery from instruments such as Hyperion on NASA's Earth-Observing 1 satellite has opened up a new source of data that can potentially be used for just this task. This study aims to assess the ability of Visible and Near Infrared (VNIR) spectroscopy to identify and quantify salt minerals through the use of spectral mixture analysis. The surface and near-surface soils of the Atacama Desert in Chile contain a variety of well-studied salts, which together with low cloud coverage, and high aridity, makes this region an ideal testbed for this technique. Two forms of spectral data ranging 0.35 - 2.5 μm were collected: laboratory spectra acquired using an ASD FieldSpec Pro instrument on samples from four locations in the Atacama desert known to have surface concentrations of sulfates, nitrates, chlorides and perchlorates; and images from the EO-1 satellite's Hyperion instrument taken over the same four locations. Mineral identifications and abundances were confirmed using quantitative XRD of the physical samples. Spectral endmembers were extracted from within the laboratory and Hyperion spectral datasets and together with additional spectral library endmembers fed into a linear mixture model. The resulting identification and abundances from both dataset types were verified against the sample XRD values. Issues of spectral scale, SNR and how different mineral spectra interact are considered, and the utility of VNIR spectroscopy and Hyperion in particular for mapping specific salt concentrations in desert environments is established. Overall, SMA was successful at estimating abundances of sulfate minerals, particularly calcium sulfate, from both hyperspectral image and laboratory sample spectra, while abundance estimation of other salt phase spectral end-members was achieved with a higher degree of error.

The effect of low energy helium ion irradiation on tungsten-tantalum (W-Ta) alloys under fusion relevant conditions

NASA Astrophysics Data System (ADS)

Gonderman, S.; Tripathi, J. K.; Novakowski, T. J.; Sizyuk, T.; Hassanein, A.

2017-08-01

Currently, tungsten remains the best candidate for plasma-facing components (PFCs) for future fusion devices because of its high melting point, low erosion, and strong mechanical properties. However, continued investigation has shown tungsten to undergo severe morphology changes under fusion-like conditions. These results motivate the study of innovative PFC materials which are resistant to surface morphology evolution. The goal of this work is to examine tungsten-tantalum (W-Ta) alloys, a potential PFC material, and their response to low energy helium ion irradiation. Specifically, W-Ta samples are exposed to 100 eV helium irradiations with a flux of 1.15 × 1021 ions m-2 s-1, at 873 K, 1023 K, and 1173 K for 1 h duration. Scanning electron microscopy (SEM) reveals significant changes in surface deterioration due to helium ion irradiation as a function of both temperature and tantalum concentration in W-Ta samples. X-Ray Diffraction (XRD) studies show a slight lattice parameter expansion in W-Ta alloy samples compared to pure W samples. The observed lattice parameter expansion in W-Ta alloy samples (proportional to increasing Ta wt.% concentrations) reflect significant differences observed in the evolution of surface morphology, i.e., fuzz development processes for both increasing Ta wt.% concentration and target temperature. These results suggest a correlation between the observed morphology differences and the induced crystal structure change caused by the presence of tantalum. Shifts in the XRD peaks before and after 100 eV helium irradiation with a flux of 1.15 × 1021 ions m-2 s-1, 1023 K, for 1 h showed a significant difference in the magnitude of the shift. This has suggested a possible link between the atomic spacing of the material and the accumulated damage. Ongoing research is needed on W-Ta alloys and other innovative materials for their application as irradiation resistant materials in future fusion or irradiation environments.

High-capacity cathodes for lithium-ion batteries from nanostructured LiFePO4 synthesized by highly-flexible and scalable flame spray pyrolysis

NASA Astrophysics Data System (ADS)

Hamid, N. A.; Wennig, S.; Hardt, S.; Heinzel, A.; Schulz, C.; Wiggers, H.

2012-10-01

Olivine, LiFePO4 is a promising cathode material for lithium-ion batteries due to its low cost, environmental acceptability and high stability. Its low electric conductivity prevented it for a long time from being used in large-scale applications. Decreasing its particle size along with carbon coating significantly improves electronic conductivity and lithium diffusion. With respect to the controlled formation of very small particles with large specific surface, gas-phase synthesis opens an economic and flexible route towards high-quality battery materials. Amorphous FePO4 was synthesized as precursor material for LiFePO4 by flame spray pyrolysis of a solution of iron acetylacetonate and tributyl phosphate in toluene. The pristine FePO4 with a specific surface from 126-218 m2 g-1 was post-processed to LiFePO4/C composite material via a solid-state reaction using Li2CO3 and glucose. The final olivine LiFePO4/C particles still showed a large specific surface of 24 m2 g-1 and were characterized using X-ray diffraction (XRD), electron microscopy, X-ray photoelectron spectrocopy (XPS) and elemental analysis. Electrochemical investigations of the final LiFePO4/C composites show reversible capacities of more than 145 mAh g-1 (about 115 mAh g-1 with respect to the total coating mass). The material supports high drain rates at 16 C while delivering 40 mAh g-1 and causes excellent cycle stability.

Reaction Heterogeneity in LiNi 0.8 Co 0.15 Al 0.05 O 2 Induced by Surface Layer

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

Grenier, Antonin; Liu, Hao; Wiaderek, Kamila M.

2017-08-15

Through operando synchrotron powder X-ray diffraction (XRD) analysis of layered transition metal oxide electrodes of composition LiNi0.8Co0.15Al0.05O2 (NCA), we decouple the intrinsic bulk reaction mechanism from surface-induced effects. For identically prepared and cycled electrodes stored in different environments, we demonstrate that the intrinsic bulk reaction for pristine NCA follows solid-solution mechanism, not a two-phase as suggested previously. By combining high resolution powder X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and surface sensitive X-ray photoelectron spectroscopy (XPS), we demonstrate that adventitious Li2CO3 forms on the electrode particle surface during exposure to air, through reaction with atmospheric CO2. This surfacemore » impedes ionic and electronic transport to the underlying electrode, with progressive erosion of this layer during cycling giving rise to different reaction states in particles with an intact vs an eroded Li2CO3 surface-coating. This reaction heterogeneity, with a bimodal distribution of reaction states, has previously been interpreted as a “two-phase” reaction mechanism for NCA, as an activation step that only occurs during the first cycle. Similar surface layers may impact the reaction mechanism observed in other electrode materials using bulk probes such as operando powder XRD.« less

An investigation of phase transformation and crystallinity in laser surface modified H13 steel

NASA Astrophysics Data System (ADS)

Aqida, S. N.; Brabazon, D.; Naher, S.

2013-03-01

This paper presents a laser surface modification process of AISI H13 tool steel using 0.09, 0.2 and 0.4 mm size of laser spot with an aim to increase hardness properties. A Rofin DC-015 diffusion-cooled CO2 slab laser was used to process AISI H13 tool steel samples. Samples of 10 mm diameter were sectioned to 100 mm length in order to process a predefined circumferential area. The parameters selected for examination were laser peak power, overlap percentage and pulse repetition frequency (PRF). X-ray diffraction analysis (XRD) was conducted to measure crystallinity of the laser-modified surface. X-ray diffraction patterns of the samples were recorded using a Bruker D8 XRD system with Cu K α ( λ=1.5405 Å) radiation. The diffraction patterns were recorded in the 2 θ range of 20 to 80°. The hardness properties were tested at 981 mN force. The laser-modified surface exhibited reduced crystallinity compared to the un-processed samples. The presence of martensitic phase was detected in the samples processed using 0.4 mm spot size. Though there was reduced crystallinity, a high hardness was measured in the laser-modified surface. Hardness was increased more than 2.5 times compared to the as-received samples. These findings reveal the phase source of the hardening mechanism and grain composition in the laser-modified surface.

Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

NASA Astrophysics Data System (ADS)

Pakharukova, V. P.; Shalygin, A. S.; Gerasimov, E. Yu.; Tsybulya, S. V.; Martyanov, O. N.

2016-01-01

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol-gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, including anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor.

The equation of state of 5-nitro-2,4-dihydro-1,2,4,-triazol-3-one determined via in-situ optical microscopy and interferometry measurements

DOE PAGES

Stavrou, Elissaios; Zaug, Joseph M.; Bastea, Sorin; ...

2016-04-07

Quasi-hydrostatic high-pressure equations of state (EOS) are typically determined, for crystalline solids, by measuring unit-cell volumes using x-ray diffraction (XRD) techniques. However, when characterizing low-symmetry materials with large unit cells, conventional XRD approaches may become problematic. To overcome this issue, we examined the utility of a "direct" approach toward determining high pressure material volume by measuring surface area and sample thickness using optical microscopy and interferometry (OMI) respectively. We have validated this experimental approach by comparing results obtained for TATB (2,4,6-triamino-1,3,5-trinitrobenzene) with an EOS determined from synchrotron XRD measurements; and, a good match is observed. We have measured the highmore » pressure EOS of 5-nitro-2,4-dihydro-1,2,4-triazol-3-one (α-NTO) up to 33 GPa. No high-pressure XRD EOS data have been published on α-NTO, probably due to its complex crystal structure. Furthermore, the results of this study suggest that OMI is a reliable and versatile alternative for determining EOSs, especially when conventional methodologies are impractical.« less

First X-Ray Diffraction Results from Mars Science Laboratory: Mineralogy of Rocknest Aeolian Bedform at Gale Crater

NASA Technical Reports Server (NTRS)

Bish, D. L.; Blake, D. F.; Vaniman, D. T.; Chipera, S. J.; Sarrazin, P.; Morris, R. V.; Ming, D. W.; Treiman, A. H.; Downs, R. T.; Morrison, S. M.;

In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

NASA Astrophysics Data System (ADS)

Takahasi, Masamitu

2018-05-01

The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

Anatomy of a metabentonite: nucleation and growth of illite crystals and their colescence into mixed-layer illite/smectite

USGS Publications Warehouse

Eberl, D.D.; Blum, A.E.; Serravezza, M.

2011-01-01

The illite layer content of mixed-layer illite/smectite (I/S) in a 2.5 m thick, zoned, metabentonite bed from Montana decreases regularly from the edges to the center of the bed. Traditional X-ray diffraction (XRD) pattern modeling using Markovian statistics indicated that this zonation results from a mixing in different proportions of smectite-rich R0 I/S and illite-rich R1 I/S, with each phase having a relatively constant illite layer content. However, a new method for modeling XRD patterns of I/S indicates that R0 and R1 I/S in these samples are not separate phases (in the mineralogical sense of the word), but that the samples are composed of illite crystals that have continuous distributions of crystal thicknesses, and of 1 nm thick smectite crystals. The shapes of these distributions indicate that the crystals were formed by simultaneous nucleation and growth. XRD patterns for R0 and R1 I/S arise by interparticle diffraction from a random stacking of the crystals, with swelling interlayers formed at interfaces between crystals from water or glycol that is sorbed on crystal surfaces. It is the thickness distributions of smectite and illite crystals (also termed fundamental particles, or Nadeau particles), rather than XRD patterns for mixed-layer I/S, that are the more reliable indicators of geologic history, because such distributions are composed of well-defined crystals that are not affected by differences in surface sorption and particle arrangements, and because their thickness distribution shapes conform to the predictions of crystal growth theory, which describes their genesis.

Physicochemical characterizations of nano-palm oil fuel ash

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

Rajak, Mohd Azrul Abdul, E-mail: azrulrajak88@gmail.com; Preparatory Centre of Science and Technology, Universiti Malaysia Sabah, Jalan UMS, 88400, Kota Kinabalu, Sabah; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my

2015-07-22

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM)more » and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m{sup 2}/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.« less

Surface topographical and structural analysis of Ag+-implanted polymethylmethacrylate

NASA Astrophysics Data System (ADS)

Arif, Shafaq; Rafique, M. Shahid; Saleemi, Farhat; Naab, Fabian; Toader, Ovidiu; Sagheer, Riffat; Bashir, Shazia; Zia, Rehana; Siraj, Khurram; Iqbal, Saman

2016-08-01

Specimens of polymethylmethacrylate (PMMA) were implanted with 400-keV Ag+ ions at different ion fluences ranging from 1 × 1014 to 5 × 1015 ions/cm2 using a 400-kV NEC ion implanter. The surface topographical features of the implanted PMMA were investigated by a confocal microscope. Modifications in the structural properties of the implanted specimens were analyzed in comparison with pristine PMMA by X-ray diffraction (XRD) and Raman spectroscopy. UV-Visible spectroscopy was applied to determine the effects of ion implantation on optical transmittance of the implanted PMMA. The confocal microscopic images revealed the formation of hillock-like microstructures along the ion track on the implanted PMMA surface. The increase in ion fluence led to more nucleation of hillocks. The XRD pattern confirmed the amorphous nature of pristine and implanted PMMA, while the Raman studies justified the transformation of Ag+-implanted PMMA into amorphous carbon at the ion fluence of ⩾5 × 1014 ions/cm2. Moreover, the decrease in optical transmittance of PMMA is associated with the formation of hillocks and ion-induced structural modifications after implantation.

Surface modification of calcium hydroxyapatite by grafting of etidronic acid

NASA Astrophysics Data System (ADS)

Othmani, Masseoud; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2013-06-01

The surface of prepared calcium hydroxyapatite CaHAp has been modified by grafting the etidronic acid (ETD). For that purpose, CaHAp powders have been suspended in an aqueous etidronate solution with different concentrations. The obtained composites CaHAp-(ETD) were characterized by TEM and AFM techniques to determinate morphological properties and were also characterized by XRD, IR, NMR and chemical and thermal analysis to determinate their physico-chemical properties and essentially the nature of the interaction between the inorganic support and the grafted organic ETD. After reaction with ETD, XRD powder analysis shows that the apatitic structure remains unchanged with slight affectation of its crystallinity. The presence of etidronate fragment bounded to hydroxyapatite was confirmed by IR and solid-state NMR spectroscopy. TEM and AFM techniques indicate that the presence of etidronate changes the morphology of the particles. Basing on the obtained results, a reactional mechanism was proposed to explain the formation of covalent Casbnd Osbnd Porg bonds on the hydroxyapatite surface between the superficial hydroxyl groups (tbnd Casbnd OH) of the apatite and phosphonate group (Psbnd OH) of etidronate.

Direct Synthesis of Anatase Films with ~100% (001) Facets and [001] Preferred Orientation.

PubMed

Ichimura, Andrew S; Mack, Brianne; Usmani, Shirin M; Mars, Diana

2012-06-26

Anatase films exhibiting ~100% (001) reactive facets at the surface were grown hydrothermally on gold substrate from a homogeneous solution of TiF(4) and NaF. In addition to NaF, it was found that TiO(2) films with very similar properties could be prepared with the fluoride salts LiF, CsF, HF, NH(4)F, and N(CH(2)CH(3))(4)F. The polycrystalline anatase films are continuous, approximately 1 μm thick, and evenly coat the substrate. The surface grain size is ~400 nm. Grazing angle XRD measurements show that the films exhibit a high degree of preferred orientation with the c-axis normal to the substrate surface. SEM images reveal that the grains span the thickness of the films. Annealing the films at 500 °C removes fluorine and causes crystallites within the grains to restructure as shown by SEM, XRD, and Raman spectroscopy. Supported anatase films grown from this one-pot method may serve as oxidative photocatalysts and electrodes for photoelectrochemical applications such as solar cells and hydrogen evolution.

Study of benzotriazole as corrosion inhibitors of carbon steel in chloride solution containing hydrogen sulfide using electrochemical impedance spectroscopy (EIS)

NASA Astrophysics Data System (ADS)

Solehudin, Agus; Nurdin, Isdiriayani

2014-03-01

Corrosion and inhibition studies on API 5LX65 carbon steel in chloride solution containing various concentrations of benzotriazole has been conducted at temperature of 70°C using Electrochemical Impedance Spectroscopy (EIS). Corroded carbon steel surface with and without inhibitor have been observed using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Energy Dispersive Spectroscopy (EDS). The objectives of this research are to study the performance of benzotriazole as corrosion inhibitors. The experimental results of carbon steel corrosion in 3.5% NaCl solution containing 500 mg/l H2S at different BTAH concentrations showed that corrosion rate of carbon steel decreases with increasing of BTAH concentrations from 0 to 10 mmol/l. The inhibition efficiency of BTAH was found to be affected by its concentration. The optimum efficiency obtained of BTAH is 93% at concentration of 5 mmol/l. The result of XRD and EDS analysis reveal the iron sulfide (FeS) formation on corroded carbon steel surface without inhibitor. The EDS spectrum show the Nitrogen (N) bond on carbon steel surface inhibited by BTAH.

Effect of chromium substitution on the dielectric properties of mixed Ni-Zn ferrite prepared by WOWS sol–gel technique

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

Ashtar, M.; Munir, A.; Anis-ur-Rehman, M.

2016-07-15

Graphical abstract: Variation of AC conductivity (σ{sub AC}) as a function of natural log of angular frequency (lnω) for Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2-x}Cr{sub x}O{sub 4} nanoferrites at room temperature. - Highlights: • Cr doped mixed Ni-Zn ferrites were successfully synthesized by a newly developed WOWS sol gel technique. • The specific surface area and specific surface area to volume ratio increased with decrease in particle size. • The resonance peaks appeared in dielectric loss graphs, shifting towards low frequency with the increase in Cr concentration. • The prepared samples have the lowest values of the dielectric constant. • The dielectricmore » constant were observed to be inversely proportional to square root of the AC resistivity. - Abstract: Cr{sup +3} doped Ni-Zn nanoferrite samples with composition Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2-x}Cr{sub x}O{sub 4}(x = 0.1, 0.2, 0.3, 0.4) were synthesized With Out Water and Surfactant (WOWS) sol-gel technique. The structural, morphological and dielectric properties of the samples were investigated. The lattice constant, crystallite size, theoretical density and porosity of each sample were obtained from X-ray diffraction (XRD) data. The specific surface area and specific surface area to volume ratio increased with the decrease in the size of Cr{sup +3} doped Ni-Zn ferrite nanoparticles, as the concentration of Cr{sup +3} increased. The SEM analysis revealed that the particles were of nano size and of spherical shape. The dielectric parameters such as dielectric constant (ε′) and dielectric loss (tanδ) of all the samples as a function of frequency at room temperature were measured. The AC conductivity (σ{sub AC}) was determined from the dielectric parameters, which showed increasing trend with the rise in frequency.« less

A novel particle engineering technology to enhance dissolution of poorly water soluble drugs: spray-freezing into liquid.

PubMed

Rogers, True L; Nelsen, Andrew C; Hu, Jiahui; Brown, Judith N; Sarkari, Marazban; Young, Timothy J; Johnston, Keith P; Williams, Robert O

2002-11-01

A novel cryogenic spray-freezing into liquid (SFL) process was developed to produce microparticulate powders consisting of an active pharmaceutical ingredient (API) molecularly embedded within a pharmaceutical excipient matrix. In the SFL process, a feed solution containing the API was atomized beneath the surface of a cryogenic liquid such that the liquid-liquid impingement between the feed and cryogenic liquids resulted in intense atomization into microdroplets, which were frozen instantaneously into microparticles. The SFL micronized powder was obtained following lyophilization of the frozen microparticles. The objective of this study was to develop a particle engineering technology to produce micronized powders of the hydrophobic drug, danazol, complexed with hydroxypropyl-beta-cyclodextrin (HPbetaCD) and to compare these SFL micronized powders to inclusion complex powders produced from other techniques, such as co-grinding of dry powder mixtures and lyophilization of bulk solutions. Danazol and HPbetaCD were dissolved in a water/tetrahydrofuran cosolvent mixture prior to SFL processing or slow freezing. Identical quantities of the API and HPbetaCD used in the solutions were co-ground in a mortar and pestle and blended to produce a co-ground physical mixture for comparison. The powder samples were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy, surface area analysis, and dissolution testing. The results provided by DSC, XRD, and FTIR suggested the formation of inclusion complexes by both slow-freezing and SFL. However, the specific surface area was significantly higher for the latter. Dissolution results suggested that equilibration of the danazol/HPbetaCD solution prior to SFL processing was required to produce the most soluble conformation of the resulting inclusion complex following SFL. SFL micronized powders exhibited better dissolution profiles than the slowly frozen aggregate powder. Results indicated that micronized SFL inclusion complex powders dissolved faster in aqueous dissolution media than inclusion complexes formed by conventional techniques due to higher surface areas and stabilized inclusion complexes obtained by ultra-rapid freezing.

Preparation of WO3/g-C3N4 composites and their application in oxidative desulfurization

NASA Astrophysics Data System (ADS)

Zhao, Rongxiang; Li, Xiuping; Su, Jianxun; Gao, Xiaohan

2017-01-01

WO3/graphitic carbon nitride (g-C3N4) composites were successfully synthesized through direct calcining of a mixture of WO3 and g-C3N4 at 400 °C for 2 h. The WO3 was prepared by calcination of phosphotungstic acid at 550 °C for 4 h, and the g-C3N4 was obtained by calcination of melamine at 520 °C for 4 h. The WO3/g-C3N4 composites were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), and Brunner-Emmett-Teller analysis (BET). The WO3/g-C3N4 composites exhibited stronger XRD peaks of WO3 and g-C3N4 than the WO3 and pure g-C3N4. In addition, two WO3 peaks at 25.7° and 26.6° emerged for the 36% -WO3/g-C3N4 composite. This finding indicated that WO3 was highly dispersed on the surface of the g-C3N4 nanosheets and interacted with the nanosheets, which resulted in the appearance of (012) and (022) planes of WO3. The WO3/g-C3N4 composite also exhibited a larger specific surface area and higher degree of crystallization than WO3 or pure g-C3N4, which resulted in high catalytic activity of the catalyst. Desulfurization experiments demonstrated that the desulfurization rate of dibenzothiophene (DBT) in model oil reached 91.2% under optimal conditions. Moreover, the activity of the catalyst was not significantly decreased after five recycles.

Surface morphology and electrochemical studies on polyaniline/CuO nano composites

NASA Astrophysics Data System (ADS)

Ashokkumar, S. P.; Vijeth, H.; Yesappa, L.; Niranjana, M.; Vandana, M.; Basappa, M.; Devendrappa, H.

2018-05-01

An electrochemically synthesized Polyaniline (PANI) and Polyaniline/copper oxide (PCN) nano composite have studied the morphology and electrochemical properties. The composite is characterized by X-ray diffraction (XRD) and surface morphology was studied using FESEM and electrochemical behavior is studied using cyclic voltammetry (CV) technique. The CV curves shows rectangular shaped curve and they have contribution to electrical double layer capacitance (EDCL).

Gd-DTPA Adsorption on Chitosan/Magnetite Nanocomposites

NASA Astrophysics Data System (ADS)

Pylypchuk, Ie. V.; Kołodyńska, D.; Kozioł, M.; Gorbyk, P. P.

2016-03-01

The synthesis of the chitosan/magnetite nanocomposites is presented. Composites were prepared by co-precipitation of iron(II) and iron(III) salts by aqueous ammonia in the 0.1 % chitosan solution. It was shown that magnetite synthesis in the chitosan medium does not affect the magnetite crystal structure. The thermal analysis data showed 4.6 % of mass concentration of chitosan in the hybrid chitosan/magnetite composite. In the concentration range of initial Gd-DTPA solution up to 0.4 mmol/L, addition of chitosan to magnetite increases the adsorption capacity and affinity to Gd-DTPA complex. The Langmuir and Freundlich adsorption models were applied to describe adsorption processes. Nanocomposites were characterized by scanning electron microscopy (SEM), differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and specific surface area determination (ASAP) methods.

Iron oxide inside SBA-15 modified with amino groups as reusable adsorbent for highly efficient removal of glyphosate from water

NASA Astrophysics Data System (ADS)

Fiorilli, Sonia; Rivoira, Luca; Calì, Giada; Appendini, Marta; Bruzzoniti, Maria Concetta; Coïsson, Marco; Onida, Barbara

2017-07-01

Iron oxide clusters were incorporated into amino-functionalized SBA-15 in order to obtain a magnetically recoverable adsorbent. The physical-chemical properties of the material were characterized by FE-SEM, STEM, XRD, TGA, XPS, FT-IR and acid-base titration analysis. Iron oxide nanoparticles were uniformly dispersed into the pore of mesoporous silica and that the adsorbent is characterized high specific surface area (177 m2/g) and accessible porosity. The sorbent was successfully tested for the removal of glyphosate in real water matrices. Despite the significant content of inorganic ions, a quantitative removal of the contaminant was found. The complete regeneration of the sorbent after the adsorption process through diluted NaOH solution was also proved.

Influence of Synthesis Temperature on the Growth and Surface Morphology of Co3O4 Nanocubes for Supercapacitor Applications

PubMed Central

Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

2017-01-01

A facile hydrothermal route to control the crystal growth on the synthesis of Co3O4 nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co3O4 nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co3O4 synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes. PMID:29088061

Investigation on the Activity Activation and Cementitious Property of Coal Gangue with High Iron and Silica Contents

NASA Astrophysics Data System (ADS)

Wu, Hong; Li, Yu; Teng, Min; Yang, Yu

2017-11-01

The activity of coal gangue by thermal activation and composite activation technologies was investigated. The crystal composition, framework structure and morphology change were analyzed by XRD, FT-IR and SEM, respectively. The cementitious property of coal gangue was measured by strength test. The results showed that thermal activation decomposed kaolinite in coal gangue, and formed the metastable structure with a porous state, multiple internal broken bonds and large specific surface areas. Based on thermal activation, the added lime provided the alkaline environment, then this reduced the bond energy of reactant particles and the degree of crystallinity of quartz in coal gangue. The two activation methods could effectively improve the cementitious property of coal gangue based unburned bricks, and that the composite activation technology was superior performance.

Preparation and characterization of carbon-supported sub-monolayer palladium decorated gold nanoparticles for the electro-oxidation of ethanol in alkaline media

NASA Astrophysics Data System (ADS)

Zhu, L. D.; Zhao, T. S.; Xu, J. B.; Liang, Z. X.

Carbon-supported gold nanoparticles (Au/C) are successfully decorated with mono- or sub-monolayer palladium atoms with different Pd/Au atomic ratios by a chemically epitaxial seeded growth method. TEM, UV-vis spectrometry and XRD techniques are used to characterize the particle size, dispersion, palladium coverage on gold seeds and crystal structures of the prepared catalysts. Cyclic voltammetric tests show that the Pd-decorated Au/C (denoted by Pd@Au/C) have higher specific activities than that of Pd/C for the oxidation of ethanol in alkaline media. This suggests that the Pd utilization is improved with such a surface-alloyed nanostructure. In addition, stable chronoamperometric responses are achieved with the so-prepared electrocatalysts during ethanol oxidation.

Porous carbons prepared by direct carbonization of MOFs for supercapacitors

NASA Astrophysics Data System (ADS)

Yan, Xinlong; Li, Xuejin; Yan, Zifeng; Komarneni, Sridhar

2014-07-01

Three porous carbons were prepared by direct carbonization of HKUST-1, MOF-5 and Al-PCP without additional carbon precursors. The carbon samples obtained by carbonization at 1073 K were characterized by XRD, TEM and N2 physisorption techniques followed by testing for electrochemical performance. The BET surface areas of the three carbons were in the range of 50-1103 m2/g. As electrode materials for supercapacitor, the MOF-5 and Al-PCP derived carbons displayed the ideal capacitor behavior, whereas the HKUST-1 derived carbon showed poor capacitive behavior at various sweep rates and current densities. Among those carbon samples, Al-PCP derived carbons exhibited highest specific capacitance (232.8 F/g) in 30% KOH solution at the current density of 100 mA/g.

Nitrogen-doped porous carbon derived from biomass waste for high-performance supercapacitor.

PubMed

Ma, Guofu; Yang, Qian; Sun, Kanjun; Peng, Hui; Ran, Feitian; Zhao, Xiaolong; Lei, Ziqiang

2015-12-01

High capacitance property and low cost are the pivotal requirements for practical application of supercapacitor. In this paper, a low cost and high capacitance property nitrogen-doped porous carbon with high specific capacitance is prepared. The as-prepared nitrogen-doped porous carbon employing potato waste residue (PWR) as the carbon source, zinc chloride (ZnCl2) as the activating agent and melamine as nitrogen doping agent. The morphology and structure of the carbon materials are studied by scanning electron microscopy (SEM), N2 adsorption/desorption, X-ray diffraction (XRD) and Raman spectra. The surface area of the nitrogen-doped carbon which prepared under 700°C is found to be 1052m(2)/g, and the specific capacitance as high as 255Fg(-1) in 2M KOH electrolyte is obtained utilize the carbon as electrode materials. The electrode materials also show excellent cyclability with 93.7% coulombic efficiency at 5Ag(-1) current density of for 5000cycles. Copyright © 2015 Elsevier Ltd. All rights reserved.

A high-capacity carbon prepared from renewable chicken feather biopolymer for supercapacitors

NASA Astrophysics Data System (ADS)

Wang, Qiang; Cao, Qi; Wang, Xianyou; Jing, Bo; Kuang, Hao; Zhou, Ling

2013-03-01

Micropopous chicken feather carbon (CFC) severing as electrode materials for the first time is prepared via the activation with KOH agent to different extents. The structure and electrochemical properties of CFC materials are characterized with N2 adsorption/desorption measurements, X-ray diffraction (XRD), transmission electron microscope (TEM), cyclic voltammetry (CV), galvanostatic charge/discharge cycling and electrochemical impedance spectroscopy (EIS). The obtained results show that CFC activated by KOH with KOH/CFC weight ratio of 4/1 (CFCA4) possesses the specific surface area of 1839 m2 g-1, average micropore diameter of 1.863 nm, and exhibits the highest initial specific capacitance of 302 F g-1 at current density of 1 A g-1 in 1 M H2SO4, and that even after 5000 cycles, CFCA4 specific capacitance is still as high as 253 F g-1. Furthermore, CFCA4 also delivers specific capacitance of 181 F g-1 at current density of 5 A g-1 and 168 F g-1 at current density of 10 A g-1. Accordingly, the microporous activated carbon material derived from chicken feather provides favorable prospect in electrode materials application in supercapacitors.

Development of stress corrosion cracking resistant welds of 321 stainless steel by simple surface engineering

NASA Astrophysics Data System (ADS)

Mankari, Kamal; Acharyya, Swati Ghosh

2017-12-01

We hereby report a simple surface engineering technique to make AISI grade 321 stainless steel (SS) welds resistant to stress corrosion cracking (SCC) in chloride environment. Heat exchanger tubes of AISI 321 SS, welded either by (a) laser beam welding (LBW) or by (b) metal inert gas welding (MIG) were used for the study. The welds had high magnitude of tensile residual stresses and had undergone SCC in chloride environment while in service. The welds were characterized using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). Subsequently, the welded surfaces were subjected to buffing operation followed by determination of residual stress distribution and surface roughness by XRD and surface profilometer measurements respectively. The susceptibility of the welds to SCC was tested in buffed and un-buffed condition as per ASTM G-36 in boiling MgCl2 for 5 h and 10 h, followed by microstructural characterization by using optical microscope and FESEM. The results showed that the buffed surfaces (both welds and base material) were resistant to SCC even after 10 h of exposure to boiling MgCl2 whereas the un-buffed surfaces underwent severe SCC for the same exposure time. Buffing imparted high magnitude of compressive stresses on the surface of stainless steel together with reduction in its surface roughness and reduction in plastic strain on the surface which made the welded surface, resistant to chloride assisted SCC. Buffing being a very simple, portable and economic technique can be easily adapted by the designers as the last step of component fabrication to make 321 stainless steel welds resistant to chloride assisted SCC.

Tuning the relative concentration ratio of bulk defects to surface defects in TiO2 nanocrystals leads to high photocatalytic efficiency.

PubMed

Kong, Ming; Li, Yuanzhi; Chen, Xiong; Tian, Tingting; Fang, Pengfei; Zheng, Feng; Zhao, Xiujian

2011-10-19

TiO(2) nanocrystals with tunable bulk/surface defects were synthesized and characterized with TEM, XRD, BET, positron annihilation, and photocurrent measurements. The effect of defects on photocatalytic activity was studied. It was found for the first time that decreasing the relative concentration ratio of bulk defects to surface defects in TiO(2) nanocrystals could significantly improve the separation efficiency of photogenerated electrons and holes, thus significantly enhancing the photocatalytic efficiency.

Sb:SnO2 thin films-synthesis and characterization

NASA Astrophysics Data System (ADS)

Bhadrapriya B., C.; Varghese, Anitta Rose; Amarendra, G.; Hussain, Shamima

2018-04-01

Transparent thin films of antimony doped SnO2 have been synthesized and characterized using optical spectroscopy, XRD, RAMAN and FESEM. The band gap of Sb doped tin oxide thin film samples were found to vary from 3.26 eV to 3.7 eV. The XRD peaks showed prominent rutile SnO2 peaks with diminished intensity due to antimony doping. A wide band in the range 550-580 cm-1 was observed in raman spectra and is a feature of nano-sized SnO2. SEM images showed flower-like structures on thin film surface, a characteristic feature of antimony.

Structural and magnetic analysis of Cu, Co substituted NiFe2O4 thin films

NASA Astrophysics Data System (ADS)

Sharma, Hakikat; Bala, Kanchan; Negi, N. S.

2016-05-01

In the present work we prepared NiFe2O4, Ni0.95Cu0.05Fe2O4 and Ni0.94Cu0.05Co0.01 Fe2O4 thin films by metallo-organic decomposition method (MOD) using spin coating technique. The thin films were analyzed by X-ray diffractometer (XRD) and Atomic force microscope (AFM) for structural studies. The XRD patterns confirmed the ferrite phase of thin films. From AFM, we analyzed surface morphology, calculated grain size (GS) and root mean square roughness (RMSR). Room temperature magnetic properties were investigated by vibrating sample magnetometer (VSM).

Operando XRD studies as a tool for determination of transport parameters of mobile ions in electrode materials

NASA Astrophysics Data System (ADS)

Kondracki, Łukasz; Kulka, Andrzej; Świerczek, Konrad; Ziąbka, Magdalena; Molenda, Janina

2017-11-01

In this work a detailed operando XRD investigations of structural properties of LixMn2O4 manganese spinel are shown to be a complementary, successful method of determination of diffusion coefficient D and surface exchange coefficient k in the working electrode. Kinetics of lithium ions transport are estimated on the basis of rate of structural changes of the cathode material during a relaxation stage after a high current charge, i.e. during structural relaxation of the material. The presented approach seems to be applicable as a complementary method of determination of transport coefficients for all intercalation-type electrode materials.

Investigating the Influence of Temperature on the Kaolinite-Base Synthesis of Zeolite and Urease Immobilization for the Potential Fabrication of Electrochemical Urea Biosensors.

PubMed

Anderson, David Ebo; Balapangu, Srinivasan; Fleischer, Heidimarie N A; Viade, Ruth A; Krampa, Francis D; Kanyong, Prosper; Awandare, Gordon A; Tiburu, Elvis K

2017-08-08

Temperature-dependent zeolite synthesis has revealed a unique surface morphology, surface area and pore size which influence the immobilization of urease on gold electrode supports for biosensor fabrication. XRD characterization has identified zeolite X (Na) at all crystallization temperatures tested. However, N₂ adsorption and desorption results showed a pore size and pore volume of zeolite X (Na) 60 °C, zeolite X (Na) 70 °C and zeolite X (Na) 90 °C to range from 1.92 nm to 2.45 nm and 0.012 cm³/g to 0.061 cm³/g, respectively, with no significant differences. The specific surface area of zeolite X (Na) at 60, 70 and 90 °C was 64 m²/g, 67 m²/g and 113 m²/g, respectively. The pore size, specific surface area and pore volumes of zeolite X (Na) 80 °C and zeolite X (Na) 100 °C were dramatically increased to 4.21 nm, 295 m²/g, 0.762 cm³/g and 4.92 nm, 389 m²/g, 0.837 cm³/g, in that order. The analytical performance of adsorbed urease on zeolite X (Na) surface was also investigated using cyclic voltammetry measurements, and the results showed distinct cathodic and anodic peaks by zeolite X (Na) 80 °C and zeolite X (Na) 100 °C. These zeolites' molar conductance was measured as a function of urea concentration and gave an average polynomial regression fit of 0.948. The findings in this study suggest that certain physicochemical properties, such as crystallization temperature and pH, are critical parameters for improving the morphological properties of zeolites synthesized from natural sources for various biomedical applications.

Investigating the Influence of Temperature on the Kaolinite-Base Synthesis of Zeolite and Urease Immobilization for the Potential Fabrication of Electrochemical Urea Biosensors

PubMed Central

Anderson, David Ebo; Balapangu, Srinivasan; Fleischer, Heidimarie N. A.; Viade, Ruth A.; Awandare, Gordon A.; Tiburu, Elvis K.

2017-01-01

Temperature-dependent zeolite synthesis has revealed a unique surface morphology, surface area and pore size which influence the immobilization of urease on gold electrode supports for biosensor fabrication. XRD characterization has identified zeolite X (Na) at all crystallization temperatures tested. However, N2 adsorption and desorption results showed a pore size and pore volume of zeolite X (Na) 60 °C, zeolite X (Na) 70 °C and zeolite X (Na) 90 °C to range from 1.92 nm to 2.45 nm and 0.012 cm3/g to 0.061 cm3/g, respectively, with no significant differences. The specific surface area of zeolite X (Na) at 60, 70 and 90 °C was 64 m2/g, 67 m2/g and 113 m2/g, respectively. The pore size, specific surface area and pore volumes of zeolite X (Na) 80 °C and zeolite X (Na) 100 °C were dramatically increased to 4.21 nm, 295 m2/g, 0.762 cm3/g and 4.92 nm, 389 m2/g, 0.837 cm3/g, in that order. The analytical performance of adsorbed urease on zeolite X (Na) surface was also investigated using cyclic voltammetry measurements, and the results showed distinct cathodic and anodic peaks by zeolite X (Na) 80 °C and zeolite X (Na) 100 °C. These zeolites’ molar conductance was measured as a function of urea concentration and gave an average polynomial regression fit of 0.948. The findings in this study suggest that certain physicochemical properties, such as crystallization temperature and pH, are critical parameters for improving the morphological properties of zeolites synthesized from natural sources for various biomedical applications. PMID:28786961

Electrodeposition of Sn-Ni Alloy Coatings for Water-Splitting Application from Alkaline Medium

NASA Astrophysics Data System (ADS)

Shetty, Sandhya; Hegde, A. Chitharanjan

2017-02-01

In this work, Sn-Ni alloy coatings were developed onto the surface of copper from a newly formulated electrolytic bath by a simple and cost-effective electrodeposition technique using gelatin as an additive. The electrocatalytic behavior of coatings deposited at different current densities (c.d.'s) for water-splitting applications, in terms of hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), has been researched. The experimental results showed that the electrocatalytic activity of Sn-Ni coatings has a close relationship with its composition, surface morphology, and phase structure depending on the c.d. used, supported by scanning electron microscopy (SEM-EDX) and X-ray diffraction (XRD) analyses. Cyclic voltammetry and chronopotentiometry techniques have demonstrated that Sn-Ni alloy deposited at 4.0 A dm-2 (having 37.6 wt pct Ni) and 1.0 A dm-2 (having 19.6 wt pct Ni) exhibit, respectively, the highest electrocatalytic behavior for HER and OER in 1.0-M KOH solution. Sn-Ni alloy coatings were found to be stable under working conditions of electrolysis, confirmed by electrochemical corrosion tests. High electrocatalytic activity of Sn-Ni alloy coatings for both HER and OER is specific to their composition, surface morphology, and active surface area.

The Effect of Eu Doping on Microstructure, Morphology and Methanal-Sensing Performance of Highly Ordered SnO2 Nanorods Array

PubMed Central

Zhao, Yanping; Li, Yuehua; Ren, Xingping; Gao, Fan; Zhao, Heyun

2017-01-01

Layered Eu-doped SnO2 ordered nanoarrays constructed by nanorods with 10 nm diameters and several hundred nanometers length were synthesized by a substrate-free hydrothermal route using alcohol and water mixed solvent of sodium stannate and sodium hydroxide at 200 °C. The Eu dopant acted as a crystal growth inhibitor to prevent the SnO2 nanorods growth up, resulting in tenuous SnO2 nanorods ordered arrays. The X-ray diffraction (XRD) revealed the tetragonal rutile-type structure with a systematic average size reduction and unit cell volume tumescence, while enhancing the residual strain as the Eu-doped content increases. The surface defects that were caused by the incorporation of Eu ions within the surface oxide matrix were observed by high-resolution transmission electron microscope (HRTEM). The results of the response properties of sensors based on the different levels of Eu-doped SnO2 layered nanoarrays demonstrated that the 0.5 at % Eu-doped SnO2 layered nanorods arrays exhibited an excellent sensing response to methanal at 278 °C. The reasons of the enhanced sensing performance were discussed from the complicated defect surface structure, the large specific surface area, and the excellent catalytic properties of Eu dopant. PMID:29168796

A laboratory study of supercritical CO2 adsorption on cap rocks in the geological storage conditions

NASA Astrophysics Data System (ADS)

Jedli, Hedi; Jbara, Abdessalem; Hedfi, Hachem; Bouzgarrou, Souhail; Slimi, Khalifa

2017-04-01

In the present study, various cap rocks have been experimentally reacted in water with supercritical CO2 in geological storage conditions ( P = 8 × 106 Pa and T = 80 °C) for 25 days. To characterize the potential CO2-water-rock interactions, an experimental setup has been built to provide additional information concerning the effects of structure, thermal and surface characteristics changes due to CO2 injection with cap rocks. In addition, CO2 adsorption capacities of different materials (i.e., clay evaporate and sandstone) are measured. These samples were characterized by XRD technique. The BET specific surface area was determined by nitrogen isotherms. In addition, thermal characteristics of untreated adsorbents were analyzed via TGA method and topography surfaces are identified by Scanning Electron Microscope (SEM). Taking into account pressure and temperature, the physical as well as chemical mechanisms of CO2 retention were determined. Isotherm change profiles of samples for relative pressure range indicate clearly that CO2 was adsorbed in different quantities. In accordance with the X-ray diffraction, a crystalline phase was formed due to the carbonic acid attack and precipitation of some carbonate.

Application of zeolitic material synthesized from thermally treated sediment to the removal of trivalent chromium from wastewater.

PubMed

Guan, Qingyu; Wu, Deyi; Lin, Yan; Chen, Xuechu; Wang, Xinze; Li, Chunjie; He, Shengbing; Kong, Hainan

2009-08-15

Zeolitic materials were synthesized from thermally treated sediment by alkali treatment using different NaOH/sediment ratios. Characterization of the materials was done by XRD, FTIR, cation exchange capacity and specific surface area. Use of high NaOH/sediment ratio favored the formation of zeolite. The potential value of the zeolitic materials for the retention of trivalent chromium from water was examined. The maximum of Cr(III) sorption by the zeolitic materials, determined by a repeated batch equilibration method, ranged from 38.9 to 75.8 mg/g which was much greater than that of the thermally treated sediment (6.3 mg/g). No release of sorbed Cr(III) by 1.0M MgCl(2) at pH 7 was observed but Cr(III) desorption by ionic electrolyte increased with decreasing pH. The zeolitic materials could completely remove Cr(III) from wastewater even in the presence of Na(+) and Ca(2+) with high concentrations with a dose above 2.5 g/L. The pH-dependent desorption behavior and the high selectivity of zeolitic material for Cr(III) were explained by sorption at surface hydroxyl sites and formation of surface precipitates.

Laser bioengineering of glass-titanium implants surface

NASA Astrophysics Data System (ADS)

Lusquiños, F.; Arias-González, F.; Penide, J.; del Val, J.; Comesaña, R.; Quintero, F.; Riveiro, A.; Boutinguiza, M.; Pascual, M. J.; Durán, A.; Pou, J.

2013-11-01

Osseointegration is the mean challenge when surgical treatments fight against load-bearing bone diseases. Absolute bone replacement by a synthetic implant has to be completed not only from the mechanics point of view, but also from a biological approach. Suitable strength, resilience and stress distribution of titanium alloy implants are spoiled by the lack of optimal biological characteristics. The inert quality of extra low interstitial titanium alloy, which make it the most attractive metallic alloy for biomedical applications, oppose to an ideal surface with bone cell affinity, and capable to stimulate bone attachment bone growth. Diverse laser treatments have been proven as effective tools to modify surface properties, such as wettability in contact to physiological fluids, or osteoblast guided and slightly enhanced attachment. The laser surface cladding can go beyond by providing titanium alloy surfaces with osteoconduction and osteoinduction properties. In this research work, the laser radiation is used to produce bioactive glass coatings on Ti6Al4V alloy substrates. Specific silicate bioactive glass compositions has been investigated to achieve suitable surface tension and viscosity temperature behavior during processing, and to provide with the required release of bone growth gene up regulation agents in the course of resorption mediated by physiological fluids. The produced coatings and interfaces, the surface osteoconduction properties, and the chemical species release in simulated physiological fluid were characterized by scanning electron microscopy (SEM), hot stage microscopy (HSM), X-ray diffraction (XRD), X ray fluorescence (XRF), and Fourier transform infrared spectroscopy (FTIR).

ASR prevention — Effect of aluminum and lithium ions on the reaction products

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

Leemann, Andreas, E-mail: andreas.leemann@empa.ch; Bernard, Laetitia; Alahrache, Salaheddine

2015-10-15

In spite of the recent progress in the understanding of the mechanisms enabling aluminum-containing SCM like metakaolin and added LiNO{sub 3} to limit the extent of ASR in mortar and concrete, some gaps still remain. They concern mainly the effect of aluminum-containing SCM on the formed ASR products and the influence of aggregate characteristics on the effectiveness of LiNO{sub 3}. In this study, a model system, concrete and mortar were investigated by pore solution analysis, TGA, XRD, NMR, SEM combined with EDX and ToF-SIMS to address these questions. The amount of aluminum present in the pore solution of concrete andmore » mortar is only able to slow down SiO{sub 2} dissolution but not to alter morphology, structure and composition of the reaction products. LiNO{sub 3} can suppress ASR by forming dense products protecting reactive minerals from further reaction. But its effectiveness is decreasing with increasing specific surface area of the reactive minerals in aggregates. - Highlights: • Aluminum of SCM slows down SiO{sub 2} dissolution. • Aluminum of SCM does not alter morphology and structure of ASR product. • ASR suppressing effect of LiNO{sub 3} depends on specific surface area of the aggregates.« less

Double-shell Fe2O3 hollow box-like structure for enhanced photo-Fenton degradation of malachite green dye

NASA Astrophysics Data System (ADS)

Jiang, De Bin; Liu, Xiaoying; Xu, Xuan; Zhang, Yu Xin

2018-01-01

In this work we demonstrate the synthesis of novel Fe2O3 nanosheets with double-shell hollow morphology by replica molding from diatomite framework. The nanostructures of Fe2O3 nanosheets were examined by focused-ion-beam scanning electron microscopy (FIB/SEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET) specific surface area measurements and Fourier transform infrared (FT-IR) spectroscopy. The results reveal that (1) Pure Fe2O3 nanosheets were successfully obtained; (2) The double-shell Fe2O3 hollow structure achieved via the NaOH etching silica method was observed; (3) Fe2O3 nanosheets possessed uniformly distributed porous nanosheets. Such structural features enlarged the specific surface area of Fe2O3 nanosheets and led to more catalytic active sites. In the heterogeneous photo-Fenton reaction, the double-shell Fe2O3 hollow morphology exhibited excellent catalytic capability for the degradation of malachite green (MG) at circumneutral pH condition. Under optimum condition, MG solution was almost completely decolorized in 60 min (99.9%). The Fe2O3 nanosheets also showed good stability and recyclability, demonstrating great potential as a promising photo-Fenton catalyst for the effective degradation of MG dye in wastewater.

Silicon-on-insulator with hybrid orientations for heterogeneous integration of GaN on Si (100) substrate

NASA Astrophysics Data System (ADS)

Zhang, Runchun; Zhao, Beiji; Huang, Kai; You, Tiangui; Jia, Qi; Lin, Jiajie; Zhang, Shibin; Yan, Youquan; Yi, Ailun; Zhou, Min; Ou, Xin

2018-05-01

Heterogeneous integration of materials pave a new way for the development of the microsystem with miniaturization and complex functionalities. Two types of hybrid silicon on insulator (SOI) structures, i.e., Si (100)-on-Si (111) and Si (111)-on-Si (100), were prepared by the smart-cut technique, which is consist of ion-slicing and wafer bonding. The precise calculation of the lattice strain of the transferred films without the epitaxial matching relationship to the substrate was demonstrated based on X-ray diffraction (XRD) measurements. The XRD and Raman measurement results suggest that the transferred films possess single crystalline quality. With a chemical mechanical polishing (CMP) process, the surface roughness of the transferred thin films can be reduced from 5.57 nm to 0.30 nm. The 4-inch GaN thin film epitaxially grown on the as-prepared hybrid SOI of Si (111)-on-Si (100) by metalorganic chemical vapor deposition (MOCVD) is of improved quality with a full width at half maximum (FWHM) of 672.54 arcsec extracted from the XRD rocking curve and small surface roughness of 0.40 nm. The wafer-scale GaN on Si (111)-on-Si (100) can serve as a potential platform for the one chip integration of GaN-based high electron mobility transistors (HEMT) or photonics with the Si (100)-based complementary metal oxide semiconductor (CMOS).

Zinc-Containing Hydroxyapatite Enhances Cold-Light-Activated Tooth Bleaching Treatment In Vitro

PubMed Central

Shi, Xinchang

2017-01-01

Cold-light bleaching treatment has grown to be a popular tooth whitening procedure in recent years, but its side effect of dental enamel demineralization is a widespread problem. The aim of this study was to synthesize zinc-substituted hydroxyapatite as an effective biomaterial to inhibit demineralization or increase remineralization. We synthesized zinc-substituted hydroxyapatite containing different zinc concentrations and analysed the product using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and energy dispersive spectrometer (EDS). The biological assessment of Zn-HA was conducted by CCK-8 assay and bacterial inhibition tests. pH cycling was performed to estimate the effect of Zn-HA on the enamel surface after cold-light bleaching treatment. The XRD, FTIR, and EDS results illustrated that zinc ions and hydroxyapatite combined in two forms: (1) Zn2+ absorbed on the surface of HA crystal and (2) Zn2+ incorporated into the lattice of HA. The results indicated that 2% Zn-HA, 4% Zn-HA, and 8% Zn-HA effectively inhibited the growth of bacteria yet showed poor biocompatibility, whereas 1% Zn-HA positively affected osteoblast proliferation. The XRD and scanning electron microscopy (SEM) results showed that the use of Zn-HA in pH cycling is obviously beneficial for enamel remineralization. Zinc-substituted hydroxyapatite could be a promising biomaterial for use in cold-light bleaching to prevent enamel demineralization. PMID:29159178

In situ assembly of well-dispersed Ni nanoparticles on silica nanotubes and excellent catalytic activity in 4-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Zhang, Shenghuan; Gai, Shili; He, Fei; Ding, Shujiang; Li, Lei; Yang, Piaoping

2014-09-01

The easy aggregation nature of ferromagnetic nanoparticles (NPs) prepared by conventional routes usually leads to a large particle size and low loading, which greatly limits their applications to the reduction of 4-nitrophenol (4-NP). Herein, we developed a novel in situ thermal decomposition and reduction strategy to prepare Ni nanoparticles/silica nanotubes (Ni/SNTs), which can markedly prevent the aggregation and growth of Ni NPs, resulting in an ultra-small particle size (about 6 nm), good dispersion and especially high loading of Ni NPs. It was found that Ni/SNTs, which have a high specific surface area (416 m2 g-1), exhibit ultra-high catalytic activity in the 4-NP reduction (complete reduction of 4-NP within only 60 s at room temperature), which is superior to most noble metal (Au, Pt, and Pd) supported catalysts. Ni/SNTs still showed high activity even after re-use for several cycles, suggesting good stability. In particular, the magnetic property of Ni/SNTs makes it easy to recycle for reuse.The easy aggregation nature of ferromagnetic nanoparticles (NPs) prepared by conventional routes usually leads to a large particle size and low loading, which greatly limits their applications to the reduction of 4-nitrophenol (4-NP). Herein, we developed a novel in situ thermal decomposition and reduction strategy to prepare Ni nanoparticles/silica nanotubes (Ni/SNTs), which can markedly prevent the aggregation and growth of Ni NPs, resulting in an ultra-small particle size (about 6 nm), good dispersion and especially high loading of Ni NPs. It was found that Ni/SNTs, which have a high specific surface area (416 m2 g-1), exhibit ultra-high catalytic activity in the 4-NP reduction (complete reduction of 4-NP within only 60 s at room temperature), which is superior to most noble metal (Au, Pt, and Pd) supported catalysts. Ni/SNTs still showed high activity even after re-use for several cycles, suggesting good stability. In particular, the magnetic property of Ni/SNTs makes it easy to recycle for reuse. Electronic supplementary information (ESI) available: XRD pattern and TEM image of SNTs after calcination, XRD pattern and EDS of NiSNTs, SEM images of a single SNT, NiSNTs and Ni/SNTs, enlarged HRTEM of Ni/SNTs, XRD pattern of NiO/SNTs, UV-vis spectra of the catalytic reduction of 4-NP to 4-AP over Ni/SNTs with different loading amounts, Ni/SNTs synthesized by wet impregnation and Ni/CNTs, TEM images of Ni/SNTs synthesized by wet impregnation and Ni/CNTs. See DOI: 10.1039/c4nr02096k

Oriented Nucleation of both Ge-Fresnoite and Benitoite/BaGe4O9 during the Surface Crystallisation of Glass Studied by Electron Backscatter Diffraction

PubMed Central

Wisniewski, Wolfgang; Patschger, Marek; Murdzheva, Steliana; Thieme, Christian; Rüssel, Christian

2016-01-01

Two glasses of the compositions 2 BaO - TiO2 - 2.75 GeO2 and 2 BaO – TiO2 –3.67 GeO2 (also known as BTG55) are annealed at temperatures from 680 to 970 °C to induce surface crystallization. The resulting samples are analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) including electron backscatter diffraction (EBSD). Ge-Fresnoite (Ba2TiGe2O8, BTG) is observed at the immediate surface of all samples and oriented nucleation is proven in both compositions. After a very fast kinetic selection, the crystal growth of BTG into the bulk occurs via highly oriented dendrites where the c-axes are oriented perpendicular to the surface. The growth of this oriented layer is finally blocked by dendritc BTG originating from bulk nucleation. The secondary phases BaTiGe3O9 (benitoite) and BaGe4O9 are also identified near the surface by XRD and localized by EBSD which additionally indicates orientation preferences for these phases. This behaviour is in contrast with previous reports from the Ba2TiSi2O8 as well as the Sr2TiSi2O8 systems. PMID:26853738

Synthesis and catalytic activity of polysaccharide templated nanocrystalline sulfated zirconia

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

Sherly, K. B.; Rakesh, K.

Nanoscaled materials are of great interest due to their unique enhanced optical, electrical and magnetic properties. Sulfate-promoted zirconia has been shown to exhibit super acidic behavior and high activity for acid catalyzed reactions. Nanocrystalline zirconia was prepared in the presence of polysaccharide template by interaction between ZrOCl{sub 2}⋅8H{sub 2}O and chitosan template. The interaction was carried out in aqueous phase, followed by the removal of templates by calcination at optimum temperature and sulfation. The structural and textural features were characterized by powder XRD, TG, SEM and TEM. XRD patterns showed the peaks of the diffractogram were in agreement with themore » theoretical data of zirconia with the catalytically active tetragonal phase and average crystalline size of the particles was found to be 9 nm, which was confirmed by TEM. TPD using ammonia as probe, FTIR and BET surface area analysis were used for analyzing surface features like acidity and porosity. The BET surface area analysis showed the sample had moderately high surface area. FTIR was used to find the type species attached to the surface of zirconia. UV-DRS found the band gap of the zirconia was found to be 2.8 eV. The benzylation of o-xylene was carried out batchwise in atmospheric pressure and 433K temperature using sulfated zirconia as catalyst.« less

Formation and characterization of high surface area thermally stabilized titania/silica composite materials via hydrolysis of titanium(IV) tetra-isopropoxide in sols of spherical silica particles.

PubMed

Khalil, Kamal M S; Elsamahy, Ahmed A; Elanany, Mohamed S

2002-05-15

A direct synthetic route leading to titania particles dispersed on nonporous spherical silica particles has been investigated; 5, 10, and 20% (w/w) titania/silica sols mixtures were achieved via hydrolyzation of titanium tetra-isopropxide solution in the mother liquor of a freshly prepared sol of spherical silica particles (Stöber particles). Titania/silica materials were produced by subsequent drying and calcination of the xerogels so obtained for 3 h at 400 and 600 degrees C. The materials were investigated by means of thermal analyses (TGA and DSC), FT-IR, N(2) gas adsorption-desorption, powder X-ray diffraction (XRD), and transmission electron microscopy (TEM). In spite of the low surface area (13.1 m(2)/g) of the pure spherical silica particles calcined at 400 degrees C, high surface area and mesoporous texture titania/silica materials were obtained (e.g., S(BET) ca. 293 m(2)/g for the 10% titania/silica calcined at 400 degrees C). Moreover, the materials were shown to be amorphous toward XRD up to 600 degrees C, while reasonable surface areas were preserved. It has been concluded that dispersion of titania particles onto the surface of the nonporous spherical silica particles increase their roughness, therefore leading to composite materials of less firm packing and mesoporosity.

Optimization and Surface Modification of Al-6351 Alloy Using SiC-Cu Green Compact Electrode by Electro Discharge Coating Process

NASA Astrophysics Data System (ADS)

Chakraborty, Sujoy; Kar, Siddhartha; Dey, Vidyut; Ghosh, Subrata Kumar

2017-06-01

This paper introduces the surface modification of Al-6351 alloy by green compact SiC-Cu electrode using electro-discharge coating (EDC) process. A Taguchi L-16 orthogonal array is employed to investigate the process by varying tool parameters like composition and compaction load and electro-discharge machining (EDM) parameters like pulse-on time and peak current. Material deposition rate (MDR), tool wear rate (TWR) and surface roughness (SR) are measured on the coated specimens. An optimum condition is achieved by formulating overall evaluation criteria (OEC), which combines multi-objective task into a single index. The signal-to-noise (S/N) ratio, and the analysis of variance (ANOVA) is employed to investigate the effect of relevant process parameters. A confirmation test is conducted based on optimal process parameters and experimental results are provided to illustrate the effectiveness of this approach. The modified surface is characterized by optical microscope and X-ray diffraction (XRD) analysis. XRD analysis of the deposited layer confirmed the transfer of tool materials to the work surface and formation of inter-metallic phases. The micro-hardness of the resulting composite layer is also measured which is 1.5-3 times more than work material’s one and highest layer thickness (LT) of 83.644μm has been successfully achieved.

An evaluation of controlled permeability formwork for long-term durability of structural concrete elements

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

Suryavanshi, A.K.; Swamy, R.N.

1997-07-01

The long-term performance of a concrete slab (CPF slab) exposed to chloride ingress and atmospheric carbonation from the surface generated by controlled permeability formwork (CPF) is investigated. The results are compared with a similar slab exposed to long-term chloride ingress and atmospheric carbonation from the cast face (Control slab). Techniques such as X-ray diffraction (XRD) and differential thermal analyses (DTA) were employed to determine the resistance against carbonation while, mercury porosimetry was used for investigating the pore size distribution at the surface of the slabs. Amount of acid soluble chlorides was determined by using Volhard`s method. The CPF employed atmore » the bottom of the mould was not fully effective in its intended purpose of generating a permanent and dense impermeable concrete layer adjacent to it when the design water-cement (w/c) ration of the concrete mix was 0.60. This resulted in an almost similar extent of carbonation at the surface for both CPF and control slabs as shown by XRD and DTA studies. Similarly, there were no significant differences in the amount of chlorides and their depths of penetration for both CPF and control slabs, although the former was marginally superior in chloride penetration resistance at the surface.« less

Catalytic oxidation of 1,2-DCBz over V2O5/TiO2-CNTs: effect of CNT diameter and surface functional groups.

PubMed

Du, Cuicui; Wang, Qiulin; Peng, Yaqi; Lu, Shengyong; Ji, Longjie; Ni, Mingjiang

2017-02-01

A series of V 2 O 5 /TiO 2 -carbon nanotube (CNT) catalysts were prepared and tested to decompose gaseous 1,2-dichlorobenzene (1,2-DCBz). Several physicochemical methods, including nitrogen adsorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and H 2 temperature-programmed reduction (TPR) were employed to characterise their physicochemical properties. To better understand the effect of CNT properties on the reactivity of V 2 O 5 /TiO 2 -CNT catalysts, the 1,2-DCBz residue remaining in the off-gas and on the catalyst surface were both collected and analysed. The results indicate that the outer diameter and the surface functional groups (hydroxide radical and carboxyl) of CNTs significantly influence upon the catalytic activity of CNT-containing V 2 O 5 /TiO 2 catalysts: the CNT outer diameter mainly affects the aggregation of CNTs and the π-π interaction between the benzene ring and CNTs, while the introduction of -OH and -COOH groups by acid treatment can further enlarge specific surface area (SSA) and contribute to a higher average oxidation state of vanadium (V aos ) and supplemental surface chemisorbed oxygen (O ads ). In addition, the enhanced mobility of lattice oxygen (O latt) also improves the oxidation ability of the catalysts.

The origin of high electrolyte-electrode interfacial resistances in lithium cells containing garnet type solid electrolytes.

PubMed

Cheng, Lei; Crumlin, Ethan J; Chen, Wei; Qiao, Ruimin; Hou, Huaming; Franz Lux, Simon; Zorba, Vassilia; Russo, Richard; Kostecki, Robert; Liu, Zhi; Persson, Kristin; Yang, Wanli; Cabana, Jordi; Richardson, Thomas; Chen, Guoying; Doeff, Marca

2014-09-14

Dense LLZO (Al-substituted Li7La3Zr2O12) pellets were processed in controlled atmospheres to investigate the relationships between the surface chemistry and interfacial behavior in lithium cells. Laser induced breakdown spectroscopy (LIBS), scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, synchrotron X-ray photoelectron spectroscopy (XPS) and soft X-ray absorption spectroscopy (XAS) studies revealed that Li2CO3 was formed on the surface when LLZO pellets were exposed to air. The distribution and thickness of the Li2CO3 layer were estimated by a combination of bulk and surface sensitive techniques with various probing depths. First-principles thermodynamic calculations confirmed that LLZO has an energetic preference to form Li2CO3 in air. Exposure to air and the subsequent formation of Li2CO3 at the LLZO surface is the source of the high interfacial impedances observed in cells with lithium electrodes. Surface polishing can effectively remove Li2CO3 and dramatically improve the interfacial properties. Polished samples in lithium cells had an area specific resistance (ASR) of only 109 Ω cm(2) for the LLZO/Li interface, the lowest reported value for Al-substituted LLZO. Galvanostatic cycling results obtained from lithium symmetrical cells also suggest that the quality of the LLZO/lithium interface has a significant impact on the device lifetime.

Rapid synthesis of rutile TiO2 nano-flowers by dealloying Cu60Ti30Y10 metallic glasses

NASA Astrophysics Data System (ADS)

Wang, Ning; Pan, Ye; Wu, Shikai; Zhang, Enming; Dai, Weiji

2018-01-01

The 3D nanostructure rutile TiO2 photocatalyst was rapidly synthesized by dealloying method using Cu60Ti30Y10 amorphous ribbons as precursors. The preparation period was kept down to just 3 h, which is much shorter than those of the samples by dealloying Cu60Ti30Al10, Cu70Ti30 and Cu60Ti30Sn10. The synthesized sample was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). XRD and XPS reveal the successful synthesis of rutile TiO2. The SEM and TEM images show that the synthesized rutile TiO2 nano-material presents homogeneous distributed 3D nanoflowers structure, which is composed of large quantities of fine rice-like nanorods (40-150 nm in diameter and 100-250 nm in length). BET specific surface areas of the samples were investigated by N2 adsorption-desorption isotherms, the fabricated rutile TiO2 exhibits very high specific surface area (194.08 m2/g). The photocatalytic activities of the samples were evaluated by degrading rhodamine B (RhB) dye (10 mg/L) under the irradiation of both simulated visible light (λ > 420 nm) and ultraviolet (UV) light (λ = 365 nm). The results show that the photocatalytic activity of rutile TiO2 prepared by dealloying Cu60Ti30Y10 amorphous ribbons is higher than those of commercial rutile and the sample synthesized by dealloying Cu70Ti30 precursors. The advantages of both short preparation period and superior photocatalytic activity suggest that Cu60Ti30Y10 metallic glasses are really a kind of perfect titanium source for rapidly fabricating high efficient TiO2 nano-materials. In addition, the influence of chemical composition of the amorphous precursors on preparation period of the rutile TiO2 nano-material was investigated from the point of view of standard electrode potentials.

The functionalization and characterization of multi-walled carbon nanotubes (MWCNTs)

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

Abdullah, Mohd Pauzi; Center of Water Analysis and Research; Zulkepli, Siti Aminah

2015-09-25

Functionalization is the process of introducing chemical functional groups on the surface of the material. In this study, a multi-walled carbon nanotube (MWCNTs) was functionalized by oxidation treatment using concentrated nitric acid. The functionalized and pristine MWCNTs were analyzed by using Fourier Transform Infrared Spectroscopy (FT-IR) and X-Ray Diffraction (XRD). The XRD patterns exhibit the graphitic properties for all samples. Besides, the XRD results also demonstrate that the percent of crystallinity of MWCNTs increases as the duration of acid treatment increases. The percent of crystallinity increases from 66% to 80% when the pristine MWCNT treated for 12 hours with additionalmore » 12 hours reflux process with nitric acid. The IR spectrum for the 12 hours-treated MWCNTs shows the formation of carboxyl functional group. Additional 12 hours reflux process with nitric acid on the 12 hours-treated MWCNTs have shown the loss of existing carboxyl group and only hydroxyl group formed.« less

Inhibitive effect of Pt on Pd-hydride formation of Pd@Pt core-shell electrocatalysts: An in situ EXAFS and XRD study

DOE PAGES

Wise, Anna M.; Richardson, Peter W.; Price, Stephen W. T.; ...

2017-12-27

In situ EXAFS and XRD have been used to study the electrochemical formation of hydride phases, H abs, in 0.5 M H 2SO 4 for a Pd/C catalyst and a series of Pd@Pt core-shell catalysts with varying Pt shell thickness, from 0.5 to 4 monolayers. Based on the XRD data a 3% lattice expansion is observed for the Pd/C core catalyst upon hydride formation at 0.0 V. In contrast, the expansion was ≤0.6% for all of the core-shell catalysts. The limited extent of the lattice expansion observed suggests that hydride formation, which may occur during periodic active surface area measurementsmore » conducting during accelerated aging tests or driven by H 2 crossover in PEM fuel cells, is unlikely to contribute significantly to the degradation of Pd@Pt core-shell electrocatalysts in contrast to the effects of oxide formation.« less

Inhibitive effect of Pt on Pd-hydride formation of Pd@Pt core-shell electrocatalysts: An in situ EXAFS and XRD study

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

Wise, Anna M.; Richardson, Peter W.; Price, Stephen W. T.

In situ EXAFS and XRD have been used to study the electrochemical formation of hydride phases, H abs, in 0.5 M H 2SO 4 for a Pd/C catalyst and a series of Pd@Pt core-shell catalysts with varying Pt shell thickness, from 0.5 to 4 monolayers. Based on the XRD data a 3% lattice expansion is observed for the Pd/C core catalyst upon hydride formation at 0.0 V. In contrast, the expansion was ≤0.6% for all of the core-shell catalysts. The limited extent of the lattice expansion observed suggests that hydride formation, which may occur during periodic active surface area measurementsmore » conducting during accelerated aging tests or driven by H 2 crossover in PEM fuel cells, is unlikely to contribute significantly to the degradation of Pd@Pt core-shell electrocatalysts in contrast to the effects of oxide formation.« less

Synthesis and characterization of Ag-doped TiO2 nanotubes on Ti-6Al-4V and Ti-6Al-7Nb alloy

NASA Astrophysics Data System (ADS)

Ulfah, Ika Maria; Bachtiar, Boy M.; Murnandityas, Arnita Rut; Slamet

2018-05-01

The present paper is focused on comparative behavior of nanotubes growth on Ti-6Al-4V and Ti-6Al-7Nb alloy using electrochemical anodization method. These alloys were anodized in electrolytes solution containing glycerol, water and 0.5wt.% of NH4F. Silver-doped TiO2 nanotubes were synthesized using photo-assisted deposition (PAD) at various Ag loading concentration in 0.05 M, 0.10 M, and 0.15 M. The phase composition and morphological characteristics were investigated by XRD and FESEM/EDX, respectively. The surface wettability was measured by contact angle meter. The results showed that TiO2 nanotubes can be grown on these surface alloys. XRD profiles revealed crystal formation of anatase, rutile and Ag on these surface alloys. According to FESEM images, the average nanotube diameter of Ti-6Al-4V alloy and Ti-6Al-7Nb alloy are 134 nm and 120 nm, respectively. EDX-Mapping analysis showed that Ag desposited over surface of TiO2 nanotubes. The surface wettability indicated hydrophilicity properties on Ti-4Al-4V alloy and Ti-6Al-7Nb alloy surface. This study may contribute to the development of silver-doped TiO2 nanotubes on Ti-6Al-4V alloy and Ti-6Al-7Nb alloy can be considered in various photocatalytic applications such as biomedical devicesdue to photocatalytic mechanism and antibacterial ability.

Phosphorus Sorption Characteristics in Aluminum-based Water Treatment Residuals Reacted with Dairy Wastewater: 1. Isotherms, XRD, and SEM-EDS Analysis.

PubMed

Zohar, Iris; Massey, Michael S; Ippolito, James A; Litaor, M Iggy

2018-05-01

We examined P sorption characteristics in Al-based water treatment residuals (Al-WTR) generated from slightly alkaline surface water and in an organic residual composite (WW-Al/O-WTR), produced by using the Al-WTR to treat organic-rich and high P concentration dairy wastewater. Solids from both residuals were examined using scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD), and exposed to P additions of 0 to 4000 mg L in a sorption experiment. The Al-WTR removed ∼97% of the added P, whereas WW-Al/O-WTR removed only 78% of the added P in the addition range of 0 to 100 mg P L. With P additions of ≥100 mg L, the removal rate declined to <38% by Al-WTR and to 16% by WW-Al/O-WTR, possibly implying a change in sorption mechanisms. Analysis by XRD indicated that the major mineral was calcite, with some silica and poorly crystalline Al hydroxides. Analysis by SEM-EDS, which used three-element overlay maps of the residual surfaces, indicated that P was sparsely sorbed on both calcic and Al (hydr)oxide surfaces, along with a few clusters, even at low P concentrations of the treated waters. Ternary clusters of P, Al, and Ca were more abundant on the WW-Al/O-WTR. Carbon distribution suggested that organic substances covered Al surfaces. Sorption of P onto WW-Al/O-WTR may be reversible due to relatively weak Ca-P and Al-P bonds induced by the slight alkaline nature and in the presence of organic moieties, enhancing the WW-Al/O-WTR potential to act as a P source, rather than a P sink, in agricultural applications. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Effect of Acetylene Black Content to Half Cells Li-ion Battery Performance Based on Li4Ti5O12 using Li2CO3 as Lithium Ion Source with Hydrothermal Mechanochemical Process

NASA Astrophysics Data System (ADS)

Priyono, B.; Faizah; Syahrial, A. Z.; Subhan, A.

2017-07-01

Lithium titanate (Li4Ti5O12)/LTO is a promising candidate to be used as anode electrode in Li-ion battery, to replace graphite in Li-ion battery application. Crystal structure of lithium titanate/LTO is more stable or undergoes less strain than graphite during intercalation and de-intercalation process Li+ ions. However, although lithium titanate has good stability, the material has low electrical conductivity and lithium ion diffusion. The purpose of this research is to synthesis the spinel LTO using combinated hydrothermal and mechanochemical processes from xerogel TiO2. Then, to increase the conductivity, in the half-cell battery assembly process it was added acetylene black conductive (AB) additive with various from 10%, to 15% in wt. The LTO obtained were characterized using scanning electron microscope (SEM), X-Ray Diffraction (XRD) and Brunauer-Emmett-Teller (BET). The XRD showed a rutile as minor phase, while SEM showed homogeneous distribution of particle with an average particle size of 0.35 μm. The BET showed that the surface area of LTO formed is 2.26 m2/g. The assembled coin half cells used this Li4Ti5O12 as a cathode and lithium metal foil as the anode were tested using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and charge discharge (CD). The conductivity value obtained from EIS corresponds to the contents of AB. Meanwhile, the CV and CD testing showed that higher percentage of AB causing the decrease of battery specific capacity. The highest specific capacity at the rate of 10C is obtained at the mixture of 10wt% AB with the value of 40.91 mAh/g.

Microstructural characterization of Charpy-impact-tested nanostructured bainite

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

Tsai, Y.T.; Chang, H.T.; Huang, B.M.

2015-09-15

In this work, a possible cause of the extraordinary low impact toughness of nanostructured bainite has been investigated. The microstructure of nanostructured bainite consisted chiefly of carbide-free bainitic ferrite with retained austenite films. X-ray diffractometry (XRD) measurement indicated that no retained austenite existed in the fractured surface of the Charpy-impact-tested specimens. Fractographs showed that cracks propagated mainly along bainitic ferrite platelet boundaries. The change in microstructure after impact loading was verified by transmission electron microscopy (TEM) observations, confirming that retained austenite was completely transformed to strain-induced martensite during the Charpy impact test. However, the zone affected by strained-induced martensite wasmore » found to be extremely shallow, only to a depth of several micrometers from the fracture surface. It is appropriately concluded that upon impact, as the crack forms and propagates, strain-induced martensitic transformation immediately occurs ahead of the advancing crack tip. The successive martensitic transformation profoundly facilitates the crack propagation, resulting in the extremely low impact toughness of nanostructured bainite. Retained austenite, in contrast to its well-known beneficial role, has a deteriorating effect on toughness during the course of Charpy impact. - Highlights: • The microstructure of nanostructured bainite consisted of nano-sized bainitic ferrite subunits with retained austenite films. • Special sample preparations for SEM, XRD and TEM were made, and the strain-affected structures have been explored. • Retained austenite films were found to transform into martensite after impact loading, as evidenced by XRD and TEM results. • The zone of strain-induced martensite was found to extend to only several micrometers from the fracture surface. • The poor Charpy impact toughness is associated with the fracture of martensite at a high strain rate during impact loading.« less

Synthesis and characterization of the Cu2ZnSnS4 system for photovoltaic applications

NASA Astrophysics Data System (ADS)

Sánchez Pinzón, D. L.; Soracá Perez, G. Y.; Gómez Cuaspud, J. A.; López, E. Vera

2017-01-01

This paper focuses on the synthesis and characterization of a ceramic material based on the Cu2ZnSnS4 system, through the implementation of a hydrothermal route. For this purpose, we started from nitrate dissolutions in a 1.0mol L-1 concentration, which were mixed and treated in a teflon lined vessel steel at 280°C for 48h. The Physicochemical characterization of the solid was evaluated by means of ultraviolet visible spectroscopy (UV-VIS), X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (SEM-TEM) and solid state impedance spectroscopy (IS). The initial characterization through UV measurements confirms a Band-gap around 1.46eV obtained by the Kubelka-Munk method, which demonstrates the effectiveness of the synthesis method in the obtaining of a semiconductor material. The XRD results confirm the obtaining of a crystalline material of pure phase with tetragonal geometry and I-42m space group. The preferential crystalline orientation was achieved along (2 2 0) facet, with crystallite sizes of nanometric order (6.0nm). The morphological aspects evaluated by means electron microscopy, confirmed the homogeneity of the material, showing specifically a series of textural and surface properties of relevant importance. Finally, the electrical characterizations allow to validate the semiconductor behaviour of CZTS system for development of photovoltaic technologies.

Local configurations and atomic intermixing in as-quenched and annealed Fe1-xCrx and Fe1-xMox ribbons

NASA Astrophysics Data System (ADS)

Stanciu, A. E.; Greculeasa, S. G.; Bartha, C.; Schinteie, G.; Palade, P.; Kuncser, A.; Leca, A.; Filoti, G.; Birsan, A.; Crisan, O.; Kuncser, V.

2018-04-01

Local atomic configuration, phase composition and atomic intermixing in Fe-rich Fe1-xCrx and Fe1-xMox ribbons (x = 0.05, 0.10, 0.15), of potential interest for high-temperature applications and nuclear devices, are investigated in this study in relation to specific processing and annealing routes. The Fe-based thin ribbons have been prepared by induction melting, followed by melt spinning and further annealed in He at temperatures up to 1250 °C. The complex structural, compositional and atomic configuration characterisation has been performed by means of X-ray diffraction (XRD), transmission Mössbauer spectroscopy and differential scanning calorimetry (TG-DSC). The XRD analysis indicates the formation of the desired solid solutions with body-centred cubic (bcc) structure in the as-quenched state. The Mössbauer spectroscopy results have been analysed in terms of the two-shell model. The distribution of Cr/Mo atoms in the first two coordination spheres is not homogeneous, especially after annealing, as supported by the short-range order parameters. In addition, high-temperature annealing treatments give rise to oxidation of Fe (to haematite, maghemite and magnetite) at the surface of the ribbons. Fe1-xCrx alloys are structurally more stable than the Mo counterpart under annealing at 700 °C. Annealing at 1250 °C in He enhances drastically the Cr clustering around Fe nuclei.

An exploratory method to detect tephras from quantitative XRD scans: Examples from Iceland and east Greenland marine sediments

USGS Publications Warehouse

Andrews, John T.; Eberl, D.D.; Kristjansdottir, G.B.

2006-01-01

Tephras, mainly from Iceland, are becoming increasingly important in interpreting leads and lags in the Holocene climate system across NW Europe. Here we demonstrate that Quantitative Phase Analysis of x-ray diffractograms of the 150 um fraction and identify these same peaks in XRD scans - two of these correlate geochemically and chronologically with Hekla 1104 and 3. At a distal site to the WNW of Iceland, on the East Greenland margin (core MD99-2317), the weight% of volcanic glass reaches values of 11% at about the time of the Saksunarvatn tephra. The XRD method identifies the presence of volcanic glass but not its elemental composition; hence it will assist in focusing attention on specific sections of sediment cores for subsequent geochemical fingerprinting of tephras. ?? 2006 SAGE Publications.

X-Ray Amorphous Phases in Terrestrial Analog Volcanic Sediments: Implications for Amorphous Phases in Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Smith, R. J.; Horgan, B.; Rampe, E.; Dehouck, E.; Morris, R. V.

2017-01-01

X-ray diffraction (XRD) amorphous phases have been found as major components (approx.15-60 wt%) of all rock and soil samples measured by the CheMin XRD instrument in Gale Crater, Mars. The nature of these phases is not well understood and could be any combination of primary (e.g., glass) and secondary (e.g., allophane) phases. Amorphous phases form in abundance during surface weathering on Earth. Yet, these materials are poorly characterized, and it is not certain how properties like composition and structure change with formation environment. The presence of poorly crystalline phases can be inferred from XRD patterns by the appearance of a low angle rise (< or approx.10deg 2(theta)) or broad peaks in the background at low to moderate 2(theta) angles (amorphous humps). CheMin mineral abundances combined with bulk chemical composition measurements from the Alpha Particle X-ray Spectrometer (APXS) have been used to estimate the abundance and composition of the XRD amorphous materials in soil and rock samples on Mars. Here we apply a similar approach to a diverse suite of terrestrial samples - modern soils, glacial sediments, and paleosols - in order to determine how formation environment, climate, and diagenesis affect the abundance and composition of X-ray amorphous phases.

In situ supported MnOx-CeOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

NASA Astrophysics Data System (ADS)

Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

2013-01-01

The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods. Electronic supplementary information (ESI) available: SEM images and EDS analysis, TEM images, and XPS spectrum of samples. See DOI: 10.1039/c2nr33006g

Surface Characteristics of Machined NiTi Shape Memory Alloy: The Effects of Cryogenic Cooling and Preheating Conditions

NASA Astrophysics Data System (ADS)

Kaynak, Y.; Huang, B.; Karaca, H. E.; Jawahir, I. S.

2017-07-01

This experimental study focuses on the phase state and phase transformation response of the surface and subsurface of machined NiTi alloys. X-ray diffraction (XRD) analysis and differential scanning calorimeter techniques were utilized to measure the phase state and the transformation response of machined specimens, respectively. Specimens were machined under dry machining at ambient temperature, preheated conditions, and cryogenic cooling conditions at various cutting speeds. The findings from this research demonstrate that cryogenic machining substantially alters austenite finish temperature of martensitic NiTi alloy. Austenite finish ( A f) temperature shows more than 25 percent increase resulting from cryogenic machining compared with austenite finish temperature of as-received NiTi. Dry and preheated conditions do not substantially alter austenite finish temperature. XRD analysis shows that distinctive transformation from martensite to austenite occurs during machining process in all three conditions. Complete transformation from martensite to austenite is observed in dry cutting at all selected cutting speeds.

Study on defect properties of nanocrystalline TiO2 during phase transition by positron annihilation lifetime

NASA Astrophysics Data System (ADS)

Zheng, F.; Liu, Y.; Liu, Z.; Dai, Y.-Q.; Fang, P.-F.; Wang, S.-J.

2012-08-01

The defect properties of nanocrystalline TiO2 were investigated by positron annihilation lifetime spectroscopy (PALS) and X-ray diffraction (XRD) as a function of annealed temperature that ranged from 300 to 850 °C. Below 500 °C, the measured positron lifetimes of τ1 (200-206 ps) and τ2 (378-402 ps) revealed the existence of mono-vacancy and vacancy-clusters at grain surface and in the micro-void of intergranular region. Between 500 and 750 °C, the phase transition from anatase to rutile was probed by the variations of positron lifetime and XRD pattern. With the increasing temperature from 500 to 850 °C, the positron lifetime τ1, τ2 and its intensity I2 sharply decreased from 200 ps, 378 ps, and 60% to 135 ps, 274 ps, and 33%, respectively. The results clearly indicate that the mono-vacancy or vacancy-clusters at grain surface and micro-voids between the grains were annealed out during the phase transition.

Study of lattice strain and optical properties of nanocrystalline SnO2

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Bhargava, Richa; Ansari, Mohd Mohsin Nizam

2018-05-01

Nanocrystalline SnO2 has been synthesized by co-precipitation method by using two solvents (water and ethylene glycol). The structure and surface morphology were investigated using XRD and scanning electron microscope (SEM). The optical properties were studied using diffused reflectance spectroscopy (DRS). From the XRD analysis, the prepared materials are found to be pure crystalline with tetragonal rutile structure. The lattice strain and crystallite size, were calculated using Williamson-Hall method, are found to be 0.00413 & 16.3 nm in water assisted SnO2 and 0.00495 & 35.6 nm for EG assisted SnO2. Study of surface morphology of the samples was carried out using SEM. It has been seen that the solvents which are used in synthesis can also alter the optical properties of the materials. The optical band gap of the water based SnO2 and EG based SnO2 are found to be 3.92eV and 3.86eV respectively.

Metal copper films deposited on cenosphere particles by magnetron sputtering method

NASA Astrophysics Data System (ADS)

Yu, Xiaozheng; Xu, Zheng; Shen, Zhigang

2007-05-01

Metal copper films with thicknesses from several nanometres to several micrometres were deposited on the surface of cenosphere particles by the magnetron sputtering method under different working conditions. An ultrasonic vibrating generator equipped with a conventional magnetron sputtering apparatus was used to prevent the cenosphere substrates from accumulating during film growth. The surface morphology, the chemical composition, the average grain size and the crystallization of cenosphere particles were characterized by field emission scanning electron microscopy (FE-SEM), inductively coupled plasma-atom emission spectrometer, x-ray photoelectron spectroscopy and x-ray diffraction (XRD) analysis, respectively, before and after the plating process. The results indicate that the copper films were successfully deposited on cenosphere particles. It was found from the FE-SEM results that the films were well compacted and highly uniform in thickness. The XRD results show that the copper film coated on cenospheres has a face centred cubic structure and the crystallization of the film sample increases with increasing sputtering power.

A green chemistry approach for the synthesis and characterization of bioactive gold nanoparticles using Azolla microphylla methanol extract

NASA Astrophysics Data System (ADS)

Kunjiappan, Selvaraj; Chowdhury, Ranjana; Bhattacharjee, Chiranjib

2014-06-01

This article reports the environmentally benign synthesis of gold nanoparticles (GNPs) using methanol extract of Azolla microphylla as the stabilizing and reducing agent. The GNPs were characterized by UV-vis spectrophotometry and FTIR, and the morphological characteristics were analyzed by XRD, FESEM-EDX and HRTEM. The GNPs could be formed in very short time, even in less than 30 min. The nanoparticles measured by UV-spectrophotometer demonstrated a peak at 540 nm corresponding to surface plasmon resonance spectra, and the peaks showed by FTIR suggested the presence of organic biomolecules on the surface of the GNPs. XRD results confirmed the crystalline nature of the GNPs, and FESEM-EDX and HRTEM analyses had been performed in the size ranges of 17-40 nm and 1.25-17.5 nm respectively. The synthesized GNPs showed excellent antioxidant activity. This study shows the feasibility of using plant sources for the biosynthesis of GNPs.

Conversion of glycerol to polyglycerol over waste duck-bones as a catalyst in solvent free etherification process

NASA Astrophysics Data System (ADS)

Ayoub, Muhammad; Sufian, Suriati; Mekuria Hailegiorgis, Sintayehu; Ullah, Sami; Uemura, Yoshimitsu

2017-08-01

The alkaline catalyst derived from the duck-bones was used for conversion of glycerol to polyglycerol via solvent free etherification process. The physicochemical properties of prepared materials were duck-bones were systematically investigated as a catalyst by latest techniques of Thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) surface properties. TGA showed different trends of duck-bones decomposition from room temperature to 1000C. XRD pattern showed a clear and sharp peaks of a crystalline phase of CaO. The activity of the catalysts was in line with the basic amount of the strong base sites, surface area, and crystalline phase in the catalysts. The prepared catalyst derived from duck-bones provided high activity (99 %) for glycerol conversion and around 68 % yield for polyglycerol production. These ample wastes of duck-bones have good potential to be used as polyglycerol production catalysts due to have high quantity of Ca compare to other types of bones like cow, chicken and fish bones.

Metallization of Kevlar fibers with gold.

PubMed

Little, Brian K; Li, Yunfeng; Cammarata, V; Broughton, R; Mills, G

2011-06-01

Electrochemical gold plating processes were examined for the metallization of Kevlar yarn. Conventional Sn(2+)/Pd(2+) surface activation coupled with electroless Ni deposition rendered the fibers conductive enough to serve as cathodes for electrochemical plating. The resulting coatings were quantified gravimetrically and characterized via adhesion tests together with XRD, SEM, TEM; the coatings effect on fiber strength was also probed. XRD data showed that metallic Pd formed during surface activation whereas amorphous phases and trace amounts of pure Ni metal were plated via the electroless process. Electrodeposition in a thiosulfate bath was the most efficient Au coating process as compared with the analogous electroless procedure, and with electroplating using a commercial cyanide method. Strongly adhering coatings resulted upon metallization with three consecutive electrodepositions, which produced conductive fibers able to sustain power outputs in the range of 1 W. On the other hand, metallization affected the tensile strength of the fiber and defects present in the metal deposits make questionable the effectiveness of the coatings as protective barriers. © 2011 American Chemical Society

Immobilized copper(II) macrocyclic complex on MWCNTs with antibacterial activity

NASA Astrophysics Data System (ADS)

Tarlani, Aliakbar; Narimani, Khashayar; Mohammadipanah, Fatemeh; Hamedi, Javad; Tahermansouri, Hasan; Amini, Mostafa M.

2015-06-01

In a new approach, a copper(II) tetraaza macrocyclic complex (CuTAM) was covalently bonded on modified multi-walled carbon nanotubes (MWCNTs). To achieve this purpose, MWCNTs were converted to MWCNT-COCl and then reacted to NH groups of TAM ligand. The prepared material was characterized by Fourier Transform Infrared (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, thermal gravimetric analysis (TGA), and FESEM (field emission scanning electron microscopy). FT-IR and TGA demonstrated the presence of the organic moieties, and XRD proved that the structure of MWCNTs remained intact during the three modification steps. An increase in the ID/IG ratio in Raman spectra confirmed the surface modifications. Finally, the samples were subjected to an antibacterial assessment to compare their biological activity. The antibacterial test showed that the grafted complex on the surface of the nanotube (MWCNT-CO-CuTAM) has higher antibacterial activity against Bacillus subtilis ATCC 6633 than the MWCNT-COOH and CuTAM with 1000 and 2000 μg/mL.

Characterization of bio char derived from tapioca skin

NASA Astrophysics Data System (ADS)

Hasnan, F. I.; Iamail, K. N.; Musa, M.; Jaapar, J.; Alwi, H.; Hamid, K. K. K.

2018-03-01

Pyrolysis of tapioca skin was conducted to produce bio chars in the range between 500°C–800°C. Surface modification treatment were performed on bio chars by using chemicals within 24 hours at 30°C and hot water within 1 hour to enhance the bio char’s adsorption properties according to surface area, pore volume, pore size, crystallinity structure and functional groups. The samples were characterized by using BET, XRD, FTIR and Methylene Blue adsorption. Based on BET result, it showed the surface area increased as the pyrolysis temperature increased followed by pore volume and pore size for S0. The optimum temperature for SNaOH, SHW and SMeOH was at 600°C, 700°C and 800°C with the surface area of 75.9874, 274.5066 and 351.5531 m2/g respectively compared to S0 while SP3HO4 has the worst result since it felt on macroporous structure. The percentage of MB adsorption was followed the size of bio chars surface area. Based on FTIR result, at temperature 500°C to 700°C, the bio chars still have functional groups while at 800°C, many functional groups were diminished due to high temperature struck on them. XRD result showed all the bio chars were amorphous. In conclusion, the best surface modification treatment was by Methanol followed by hot water and Sodium Hydroxide at temperature of 700°C and 800°C while Ortho-Phosphoric acid was the worst one and was not suitable for bio char’s surface modification for adsorption purpose.

Deuterium permeation behaviors in tungsten implanted with nitrogen

NASA Astrophysics Data System (ADS)

Liang, Chuan-hui; Wang, Dongping; Jin, Wei; Lou, Yuanfu; Wang, Wei; Ye, Xiaoqiu; Chen, Chang-an; Liu, Kezhao; Xu, Haiyan; Wang, Xiaoying; Kleyn, Aart W.

2018-07-01

Surface modification of tungsten due to the cooling species nitrogen seeded in the divertor region, i.e., by nitrogen ion implantation or re-deposition, is considered to affect the permeation behavior of H isotopes. This work focuses on the effect of nitrogen ion implantation into tungsten (W-N) on the deuterium gas-driven permeation behavior. For comparison, both permeation in tungsten implanted with W ion (W-W) and without implantation (pristine W) are studied. These three samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photo-electron spectroscopy (XPS). The SEM results revealed that the W-W sample has various voids on the surface, and the W-N sample has a rough surface with pretty fine microstructures. These are different from the pristine W sample with a smooth and compact surface. The XRD patterns show the disappearance of crystallinity on both W-W and W-N sample surfaces. It indicates that the ion implantation process results in an almost complete conversion from crystalline to amorphous in the sample surfaces. The sputter-depth profiling XPS spectra show that the implanted nitrogen prefers to form a 140 nm thick tungsten nitride layer. In permeation experiments, it was found that the D permeability is temperature dependent. Interestingly, the W-N sample presented a lower D permeability than the W-W sample, but higher than the pristine W sample. Such behavior implies that tungsten nitride acts as a permeation barrier, while defects created by ions implantation can promote permeability. The possible permeation mechanism correlated with sample surface composition and microstructure is consequently discussed in this work.

Blast Coating of Superelastic NiTi Wire with PTFE to Enhance Wear Properties

NASA Astrophysics Data System (ADS)

Dunne, Conor F.; Roche, Kevin; Twomey, Barry; Hodgson, Darel; Stanton, Kenneth T.

2015-03-01

This work investigates the deposition of polytetrafluoroethylene (PTFE) onto a superelastic NiTi wire using an ambient temperature-coating technique known as CoBlast. The process utilises a stream of abrasive (Al2O3) and a coating medium (PTFE) sprayed simultaneously at the surface of the substrate. Superelastic NiTi wire is used in guidewire applications, and PTFE coatings are commonly applied to reduce damage to vessel walls during insertion and removal, and to aid in accurate positioning by minimising the force required to advance, retract or rotate the wire. The CoBlast coated wires were compared to wire treated with PTFE only. The coated samples were examined using variety of techniques: X-ray diffraction (XRD), microscopy, surface roughness, wear testing and flexural tests. The CoBlast coated samples had an adherent coating with a significant resistance to wear compared to the samples coated with PTFE only. The XRD revealed that the process gave rise to a stress-induced martensite phase in the NiTi which may enhance mechanical properties. The study indicates that the CoBlast process can be used to deposit thin adherent coatings of PTFE onto the surface of superelastic NiTi.

Structural, mechanical and magnetic study on galvanostatic electroplated nanocrystalline NiFeP thin films

NASA Astrophysics Data System (ADS)

Kalaivani, A.; Senguttuvan, G.; Kannan, R.

2018-03-01

Nickel based alloys has a huge applications in microelectronics and micro electromechanical systems owing to its superior soft magnetic properties. With the advantages of simplicity, cost-effectiveness and controllable patterning, electroplating processes has been chosen to fabricate thin films in our work. The soft magnetic NiFeP thin film was successfully deposited over the surface of copper plate through galvanostatic electroplating method by applying constant current density of 10 mA cm-2 for a deposition rate for half an hour. The properties of the deposited NiFeP thin films were analyzed by subjecting it into different physio-chemical characterization such as XRD, SEM, EDAX, AFM and VSM. XRD pattern confirms the formation of NiFeP particles and the structural analysis reveals that the NiFeP particles were uniformly deposited over the surface of copper substrate. The surface roughness analysis of the NiFeP films was done using AFM analysis. The magnetic studies and the hardness of the thin film were evaluated from the VSM and hardness test. The NiFeP thin films possess lower coercivity with higher magnetization value of 69. 36 × 10-3 and 431.92 Gauss.

Cooked Food Waste-An Efficient and Less Expensive Precursor for the Generation of Activated Carbon.

PubMed

Krithiga, Thangavelu; Sabina, Xavier Janet; Rajesh, Baskaran; Ilbeygi, Hamid; Shetty, Adka Nityananda; Reddy, Ramanjaneya; Karthikeyan, Jayabalan

2018-06-01

Activated carbon was synthesized from cooked food waste, especially dehydrated rice kernels, by chemical activation method using NaOH and KOH as activating agents. It was then characterized by ultimate and proximate analysis, BET surface analysis, XRD, FTIR, Raman and SEM. The XRD patterns and Raman spectra confirmed the amorphous nature of the prepared activated carbons. Ultimate analysis showed an increase in the carbon content after activation of the raw carbon samples. Upon activation with NaOH and KOH, the surface area of the carbon sample was found to have increased from 0.3424 to 539.78 and 306.83 m2g-1 respectively. The SEM images revealed the formation of heterogeneous pores on the surface of the activated samples. The samples were then tested for their adsorption activity using acetic acid and methylene blue. Based on the regression coefficients, the adsorption kinetics of methylene blue dye were fitted with pseudo-second order model for both samples. Similarly, the Freundlich isotherm was found to be a better fit than Langmuir isotherm for both samples. The activity of thus prepared activated carbons was found to be comparable with the commercial carbon.

Effect of different conventional melt quenching technique on purity of lithium niobate (LiNbO3) nano crystal phase formed in lithium borate glass

NASA Astrophysics Data System (ADS)

Kashif, Ismail; Soliman, Ashia A.; Sakr, Elham M.; Ratep, Asmaa

2012-01-01

The glass system (45Li2O + 45B2O3 + 10Nb2O5) was fabricated by the conventional melt quenching technique poured in water, at air, between two hot plates and droplets at the cooled surface. The glass and glass ceramics were studied by differential thermal analysis (DTA) and X-ray diffraction (XRD). The as quenched samples poured in water and between two hot plates were amorphous. The samples poured at air and on cooled surface were crystalline as established via X-ray powder diffraction (XRD) studies. Differential thermal analysis was measured. The glass transition temperature (Tg) and the crystallization temperatures were calculated. Lithium niobate (LiNbO3) was the main phase in glass ceramic poured at air, droplets at the cooled surface and the heat treated glass sample at 500, 540 and 580 °C in addition to traces from LiNb3O8. Crystallite size of the main phases determined from the X-ray diffraction peaks is in the range of <100 nm. The fraction of crystalline (LiNbO3) phase decreases with increase in the heat treatment temperature.

Study of benzotriazole as corrosion inhibitors of carbon steel in chloride solution containing hydrogen sulfide using electrochemical impedance spectroscopy (EIS)

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

Solehudin, Agus, E-mail: asolehudin@upi.edu; Nurdin, Isdiriayani

2014-03-24

Corrosion and inhibition studies on API 5LX65 carbon steel in chloride solution containing various concentrations of benzotriazole has been conducted at temperature of 70°C using Electrochemical Impedance Spectroscopy (EIS). Corroded carbon steel surface with and without inhibitor have been observed using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Energy Dispersive Spectroscopy (EDS). The objectives of this research are to study the performance of benzotriazole as corrosion inhibitors. The experimental results of carbon steel corrosion in 3.5% NaCl solution containing 500 mg/l H{sub 2}S at different BTAH concentrations showed that corrosion rate of carbon steel decreases with increasing of BTAHmore » concentrations from 0 to 10 mmol/l. The inhibition efficiency of BTAH was found to be affected by its concentration. The optimum efficiency obtained of BTAH is 93% at concentration of 5 mmol/l. The result of XRD and EDS analysis reveal the iron sulfide (FeS) formation on corroded carbon steel surface without inhibitor. The EDS spectrum show the Nitrogen (N) bond on carbon steel surface inhibited by BTAH.« less

Characteristics of Iron-Palladium alloy thin films deposited by magnetron sputtering

NASA Astrophysics Data System (ADS)

Chiu, Y.-J.; Shen, C.-Y.; Chang, H.-W.; Jian, S.-R.

2018-06-01

The microstructural features, magnetic, nanomechanical properties and wettability behaviors of Iron-Palladium (FePd) alloy thin films are investigated by using X-ray diffraction (XRD), atomic force microscopy (AFM), vibrating sample magnetometer (VSM), nanoindentation and water contact angle (CA) techniques, respectively. The FePd alloy thin films were deposited on glass substrates using a magnetron sputtering system. The post-annealing processes of FePd alloy thin films were carried out at 400 °C and 750 °C and resulted in a significant increase of both the average grain size and surface roughness. The XRD analysis showed that FePd alloy thin films exhibited a predominant (1 1 1) orientation. The magnetic field dependence of magnetization of all FePd thin films are measured at room temperature showed the ferromagnetic characteristics. The nanoindentation with continuous stiffness measurement (CSM) is used to measure the hardness and Young's modulus of present films. The contact angle (θCA) increased with increasing surface roughness. The maximum θCA of 75° was achieved for the FePd alloy thin film after annealing at 750 °C and a surface roughness of 4.2 nm.

Feasibility of an integrated X-ray instrument for Mars exobiology and geology. [Abstract only

NASA Technical Reports Server (NTRS)

Fonda, M. L.; Schwartz, D. E.; Koppel, L. N.; Franco, E. D.; Kerner, J. A.

1994-01-01

By employing an integrated X-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details relevant to the possibility of the origin and evolution of life on Mars will be acquired. An integrated combined X Ray Fluorescence/X Ray Detection (XRF/XRD) instrument has been breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for Mars Environmental Survey (MESUR) and future Mars missions. Among others, primary objectives for the exploration of Mars include: the intense study of local areas on Mars to 'establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epochs; and to establish the global chemical and physical characteristics of the Martian surface'. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment.

Electrochemical properties of reduced graphene oxide derived through camphor assisted combustion of graphite oxide.

PubMed

Ramesh, A; Jeyavelan, M; Leo Hudson, M Sterlin

2018-04-17

A facile method was demonstrated for the one-step synthesis of reduced graphene oxide (rGO) from graphite oxide (GO) using a camphor assisted combustion (CAC) process. Analysis of samples was carried out using FT-IR, XRD, TGA, Raman, BET, SEM and TEM techniques. The electrochemical properties of the rGO samples derived through the CAC process were determined using cyclic voltammetry, galvanostatic charge/discharge and impedance spectroscopy. It has been observed that the specific surface area and porosity of the rGO samples decrease with the increasing concentration of camphor during the CAC synthesis process. Thus, different mass ratios of GO and camphor such as 1 : 12, 1 : 16, and 1 : 20 in the CAC process yield rGO samples having surface areas (SBET) of 313.3, 297.5 and 177.4 m2 g-1. The pore volumes of the respective samples are 0.44, 0.45 and 0.23 cm3 g-1, respectively. The rGO derived using the 1 : 12 mass ratio of GO and camphor (rGO-12C) exhibits a high specific capacitance of 241 F g-1, which is significantly higher than that observed for chemically reduced graphene oxide (rGO-CR), which exhibits a specific capacitance value of only 153 F g-1. The capacitance retention of rGO-12C was found to be 98% even after 1000 galvanostatic charge-discharge (GCD) cycles, suggesting its potential applications in electrochemical energy storage.

Spectral properties of Dy3+ doped ZnAl2O4 phosphor

NASA Astrophysics Data System (ADS)

Prakash, Ram; Kumar, Sandeep; Mahajan, Rubby; Khajuria, Pooja; Kumar, Vinay; Choudhary, R. J.; Phase, D. M.

2018-05-01

Herein, Dy3+ doped ZnAl2O4 phosphor was synthesized by the solution combustion method. The synthesized phosphor was characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS). The phase purity of the phosphor was confirmed by the XRD studies that showed cubic symmetry of the synthesized phosphor. Under UV excitation (388 nm) the PL emission spectrum of the phosphor shows characteristic transition from the Dy3+ ion. A band gap of 5.2 eV was estimated from the diffused reflectance spectroscopy. The surface properties of the phosphor were studied using the X-ray photoelectron spectroscopy.

Synthesis and structural studies of Mg doped LiNi0.5Mn0.5O2 cathode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Murali, N.; Margarette, S. J.; Madhuri Sailaja, J.; Kondala Rao, V.; Himakar, P.; Kishore Babu, B.; Veeraiah, V.

2018-02-01

Layered Mg doped LiNi0.5Mn0.5O2 materials have been synthesized by sol-gel method. The physical properties of these materials were examined by XRD, FESEM and FT-IR studies. From XRD patterns, the phase formation of α-NaFeO2 layered structure with R\\bar 3m space group is confirmed. The surface morphology of the synthesized materials has been examined by FESEM analysis in which the average particle size is found to be about 2 - 2.5 µm. These materials show some changes in the local ion environment, as examined by FT-IR studies.

A mineralogical instrument for planetary applications

NASA Technical Reports Server (NTRS)

Blake, David F.; Vaniman, David T.; Bish, David L.

1994-01-01

The mineralogy of a planetary surface can be used to identify the provenance of soil or sediment and reveal the volcanic, metamorphic and/or sedimentological history of a particular region. We have discussed elsewhere the applications and the instrument design of possible X-ray diffraction and X-ray fluorescence (XRD/XRF) devices for the mineralogical characterization of planetary surfaces. In this abstract we evaluate some aspects of sample-detector geometry and sample collection strategies.

Green synthesis of silica nanoparticles using sugarcane bagasse

NASA Astrophysics Data System (ADS)

Mohd, Nur Kamilah; Wee, Nik Nur Atiqah Nik; Azmi, Alyza A.

2017-09-01

Silica nanoparticles have been great attention as it being evaluated for used in abundant fields and applications. Due to this significance, this research was conducted to synthesis silica nanoparticles using local agricultural waste, sugarcane bagasse. We executed extraction and precipitation process as it involved low cost, less toxic and low energy process compared to other methods. The Infrared (IR) spectra showed the vibration peak of Si-O-Si, which clearly be the evidence for the silica characteristics in the sample. In this research, amorphous silica nanoparticles with spherical morphology with an average size of 30 nm, and specific surface area of 111 m2/g-1 have been successfully synthesized. The XRD patterns showed the amorphous nature of silica nanoparticles. As a comparison, the produced silica nanoparticles from sugarcane bagasse are compared with the respective nanoparticles synthesized using Stöber method.

Synthesis and adsorption properties of flower-like layered double hydroxide by a facile one-pot reaction with an eggshell membrane as assistant

NASA Astrophysics Data System (ADS)

Li, Songnan; Zhang, Jiawei; Jamil, Saba; Cai, Qinghai; Zang, Shuying

In this paper, flower-like layered double hydroxides were synthesized with eggshell membrane assistant. The as-prepared samples were characterized by a series of techniques including X-ray diffraction (XRD), Fourier transform infrared spectroscopy, Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Thermal gravity-differential thermal analysis and Nitrogen sorption/desorption. The resulting layered double hydroxides were composed of nanoplates with edge-to-face particle interactions. The specific surface area and total pore volume of the as-prepared flower-like layered double hydroxides were 160m2/g and 0.65m3/g, respectively. The adsorption capacity of flower-like layered double hydroxides to Congo Red was 258mg/g, which was higher than that of layered double hydroxides synthesized by the traditional method.

A simple large-scale synthesis of mesoporous In2O3 for gas sensing applications

NASA Astrophysics Data System (ADS)

Zhang, Su; Song, Peng; Yan, Huihui; Yang, Zhongxi; Wang, Qi

2016-08-01

In this paper, large-scale mesoporous In2O3 nanostructures were synthesized by a facile Lewis acid catalytic the furfural alcohol resin (FAR) template route for the high-yield. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG) and the Brunauer-Emmett-Teller (BET) approach. The as-obtained mesoporous In2O3 nanostructures possess excellent mesoporous and network structure, which increases the contact area with the gases, it is conducive for adsorption-desorption of gas on the surface of In2O3. The In2O3 particles and pores were both about 15 nm and very uniform. In gas-sensing measurements with target gases, the gas sensor based on mesoporous In2O3 nanostructures showed a good response, short response-recovery time, good selectivity and stability to ethanol. These properties are due to the large specific surface area of mesoporous structure. This synthetic method could use as a new design concept for functional mesoporous nanomaterials and for mass production.

Unzipping of multi-wall carbon nanotubes with different diameter distributions: Effect on few-layer graphene oxide obtention

NASA Astrophysics Data System (ADS)

Torres, D.; Pinilla, J. L.; Suelves, I.

2017-12-01

Few-layer graphene oxide (FLGO) was obtained by chemical unzipping of multi-wall carbon nanotubes (MWCNT) of different diameter distributions. MWCNT were synthesized by catalytic decomposition of methane using Fe-Mo/MgO catalysts. The variation in the Fe/Mo ratio (1, 2 and 5) was very influential in MWCNT diameter distribution and type of MWCNT obtained, including textural, chemical, structural and morphological characteristics. MWCNT diameter distribution and surface defects content had a profound impact on the characteristics of the resulting FLGO. Thus, MWCNT obtained with the catalyst with a Fe/Mo: 5 and presenting a narrow diameter distribution centered at 8.6 ± 3.3 nm led to FLGO maintaining non-oxidized graphite stacking (according to XRD analysis), lower specific surface area and higher thermostability as compared to FLGO obtained from MWCNT showing wider diameter distributions. The presence of more oxygen-containing functionalities and structural defects in large diameter nanotubes promotes the intercalation of species towards the inner layers of the nanotube, resulting in an enhanced MWCNT oxidation and opening into FLGO, what improves both micro- and mesoporosity.

DMSO-Li2O2 Interface in the Rechargeable Li-O2 Battery Cathode: Theoretical and Experimental Perspectives on Stability.

PubMed

Schroeder, Marshall A; Kumar, Nitin; Pearse, Alexander J; Liu, Chanyuan; Lee, Sang Bok; Rubloff, Gary W; Leung, Kevin; Noked, Malachi

2015-06-03

One of the greatest obstacles for the realization of the nonaqueous Li-O2 battery is finding a solvent that is chemically and electrochemically stable under cell operating conditions. Dimethyl sulfoxide (DMSO) is an attractive candidate for rechargeable Li-O2 battery studies; however, there is still significant controversy regarding its stability on the Li-O2 cathode surface. We performed multiple experiments (in situ XPS, FTIR, Raman, and XRD) which assess the stability of the DMSO-Li2O2 interface and report perspectives on previously published studies. Our electrochemical experiments show long-term stable cycling of a DMSO-based operating Li-O2 cell with a platinum@carbon nanotube core-shell cathode fabricated via atomic layer deposition, specifically with >45 cycles of 40 h of discharge per cycle. This work is complemented by density functional theory calculations of DMSO degradation pathways on Li2O2. Both experimental and theoretical evidence strongly suggests that DMSO is chemically and electrochemically stable on the surface of Li2O2 under the reported operating conditions.

A low cost preparation of WO3 nanospheres film with improved thermal stability of gasochromic and its application in smart windows

NASA Astrophysics Data System (ADS)

Zhou, Baoyu; Feng, Wei; Gao, Guohua; Wu, Guangming; Chen, Yue; Li, Wen

2017-11-01

Porous WO3 nanospheres film was successfully synthesized by employing a low-cost and facile template-assisted sol-gel method. The effects of template agent (Pluronic F127) on structure, morphology and specific surface area were systematically studied by Fourier transform infrared (FTIR), x-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and N2 physisorption. It was found that F127 played a significant role in governing the morphology of WO3 sol clusters, and the optimal post-processing for ‘naked’ WO3 nanospheres film is acetone extraction and subsequent annealing treatment at 350 °C. As anticipated, the relative fast coloring/bleaching rates of WO3 nanospheres film are believed to be the results of porous microstructure and nanocrystalline, where provides much surface active position (166 m2 g-1) and shortens the proton diffusion distance. We believe that this unique approach to synthesize nanospheres structure may has beneficial effects on applications which also are based on insertion/extraction and diffusion abilities, such as supercapacitor, batteries and gas sensors.

Thin film rechargeable electrodes based on conductive blends of nanostructured olivine LiFePO4 and sucrose derived nanocarbons for lithium ion batteries.

PubMed

Praveen, P; Jyothsna, U; Nair, Priya; Ravi, Soumya; Balakrishnan, A; Subramanian, K R V; Nair, A Sreekumaran; Nair, V Shantikumar; Sivakumar, N

2013-08-01

The present study provides the first reports of a novel approach of electrophoretic co-deposition technique by which titanium foils are coated with LiFePO4-carbon nanocomposites synthesized by sol gel route and processed into high-surface area cathodes for lithium ion batteries. The study elucidates how sucrose additions as carbon source can affect the surface morphology and the redox reaction behaviors underlying these cathodes and thereby enhance the battery performance. The phase and morphological analysis were done using XRD and XPS where the LiFePO4 formed was confirmed to be a high purity orthorhombic system. From the analysis of the relevant electrochemical parameters using cyclic voltammetry and electrochemical impedance spectroscopy, a 20% increment and 90% decrement in capacity and impedance values were observed respectively. The composite electrodes also exhibited a specific capacity of 130 mA h/g. It has been shown that cathodes based on such composite systems can allow significant room for improvement in the cycling performance at the electrode/electrolyte interface.

Effective visible light-active boron and europium co-doped BiVO4 synthesized by sol-gel method for photodegradion of methyl orange.

PubMed

Wang, Min; Che, Yinsheng; Niu, Chao; Dang, Mingyan; Dong, Duo

2013-11-15

Eu-B co-doped BiVO4 visible-light-driven photocatalysts have been synthesized using the sol-gel method. The resulting materials were characterized by a series of joint techniques, including XPS, XRD, SEM, BET, and UV-vis DRS analyses. Compared with BiVO4 and B-BiVO4 photocatalysts, the Eu-B-BiVO4 photocatalysts exhibited much higher photocatalytic activity for methyl orange (MO) degradation under visible light irradiation. The optimal Eu doping content is 0.8 mol%. It was revealed that boron and europium were doped into the lattice of BiVO4 and this led to more surface oxygen vacancies, high specific surface areas, small crystallite size, a narrower band gap and intense light absorbance in the visible region. The doped Eu(III) cations can help in the separation of photogenerated electrons. The synergistic effects of boron and europium in doped BiVO4 were the main reason for improving visible light photocatalytic activity. Copyright © 2013 Elsevier B.V. All rights reserved.

Graphene oxide/MnO2 nanocomposite as destructive adsorbent of nerve-agent simulants in aqueous media

NASA Astrophysics Data System (ADS)

Šťastný, Martin; Tolasz, Jakub; Štengl, Václav; Henych, Jiří; Žižka, David

2017-08-01

Graphene oxide/MnO2 nanocomposite was prepared by thermal hydrolysis of potassium permanganate (KMnO4) and 2-chloroacetamide aqueous solutions with graphene oxide (GO) suspension. The synthesized samples were characterized by specific surface area (BET) and porosity determination (BJH), X-ray Diffraction (XRD) and high-resolution electron microscopes (HRSEM, HRTEM). These nanocomposites were used in an experimental evaluation of their adsorption activity with nerve agent simulants dimethyl methyl phosphonate (DMMP) and triethyl phosphate (TEP) in aqueous media. The nanocomposites exhibited enhanced adsorptive degradation ability compared to pure manganese oxide (MnO2) and GO. The GO amount in the nanocomposites affected their degradation activity substantially. The best adsorption efficiency was observed for samples with moderate GO amount. Three methods were used to observe the mechanism of the nerve-agent simulants deactivation: Gas chromatography with mass spectrometry (GC-MS), High-Performance Liquid Chromatography (HPLC) and in situ Infrared spectroscopy (FTIR). It was shown that the hydrolysis on the surface of prepared nanocomposites yields volatile primary alcohols (methanol and ethanol) as the main hydrolysis products.

Preparation of InYO3 catalyst and its application in photodegradation of molasses fermentation wastewater.

PubMed

Qin, Zuzeng; Liang, Yi; Liu, Zili; Jiang, Weiqing

2011-01-01

An InYO3 photocatalyst was prepared through a precipitation method and used for the degradation of molasses fermentation wastewater. The InYO3 photocatalyst characterized by X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy, surface area and porosimetry. Energy band structures and density of states were achieved using the Cambridge Serial Total Energy package (CASTEP). The results indicated that the photodegradation of molasses fermentation wastewater was significantly enhanced in the presence of InYO3 when compared with PbWO4. The calcination temperature was found to have a significant effect on the photocatalytic activity of InYO3. Specifically, InYO3 calcined at 700 degrees C had a considerably larger surface area and lower reflectance intensity and showed higher photocatalytic activity. The mathematical simulation results indicated that InYO3 is a direct band gap semiconductor, and its conduction band is composed of In 5p and Y 4d orbitals, whereas its valence band is composed of O 2p and In 5s orbitals.

Nanocrystalline TiO₂ Composite Films for the Photodegradation of Formaldehyde and Oxytetracycline under Visible Light Irradiation.

PubMed

Wei, Min; Peng, Xue-Lei; Liu, Qi-Sheng; Li, Fang; Yao, Ming-Ming

2017-06-14

In order to effectively photodegradate organic pollutants, ZnO composite and Co-B codoped TiO₂ films were successfully deposited on glass substrates via a modified sol-gel method and a controllable dip-coating technique. Combining with UV-Vis diffuse reflectance spectroscopy (DRS) and photoluminescence spectra (PL) analyses, the multi-modification could not only extend the optical response of TiO₂ to visible light region but also decrease the recombination rate of electron-hole pairs. XRD results revealed that the multi-modified TiO₂ film had an anatase-brookite biphase heterostructure. FE-SEM results indicated that the multi-modified TiO₂ film without cracks was composed of smaller round-like nanoparticles compared to pure TiO₂. BET surface area results showed that the specific surface area of pure TiO₂ and the multi-modified TiO₂ sample was 47.8 and 115.8 m²/g, respectively. By degradation of formaldehyde and oxytetracycline, experimental results showed that the multi-modified TiO₂ film had excellent photodegradation performance under visible light irradiation.

X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

NASA Astrophysics Data System (ADS)

Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

2011-12-01

The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I., Baliva, A., Stevoli, A., Ambrosi, R., Critani, F., Delhez, R., Scandelli, L., Holland, A., Nelms, N. & the Mars-XRD Team, Proceedings of the 38th Lunar and Planetary Science Conference, 12 - 16 March 2007, League City, Texas, USA. [2] L. Marinangeli, I. B. Hutchinson, A. Stevoli, G. Adami, R. Ambrosi, R. Amils, V. Assis Fernandes, A. Baliva, A. T. Basilevsky, G. Benedix, P. Bland, A. J. Böttger, J. Bridges, G. Caprarelli, G. Cressey, F. Critani, N. d'Alessandro, R. Delhez, C. Domeneghetti, D. Fernandez-Remolar, R. Filippone, A. M. Fioretti, J. M. Garcia Ruiz, M. Gilmore, G. M. Hansford, G. Iezzi, R. Ingley, M. Ivanov, G. Marseguerra, L. Moroz, C. Pelliciari, P. Petrinca, E. Piluso, L. Pompilio, J. Sykes, F. Westall and the MARS-XRD Team, EPSC-DPS Joint Meeting 2011, 3 - 7 October 2011, La Cité Internationale des Congrès Nantes Métropole, Nantes, France.

Comparing two tetraalkylammonium ionic liquids. II. Phase transitions.

PubMed

Lima, Thamires A; Paschoal, Vitor H; Faria, Luiz F O; Ribeiro, Mauro C C; Ferreira, Fabio F; Costa, Fanny N; Giles, Carlos

2016-06-14

Phase transitions of the ionic liquids n-butyl-trimethylammonium bis(trifluoromethanesulfonyl)imide, [N1114][NTf2], and methyl-tributylammonium bis(trifluoromethanesulfonyl)imide, [N1444][NTf2], were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) measurements, and Raman spectroscopy. XRD and Raman spectra were obtained as a function of temperature at atmospheric pressure, and also under high pressure at room temperature using a diamond anvil cell (DAC). [N1444][NTf2] experiences glass transition at low temperature, whereas [N1114][NTf2] crystallizes or not depending on the cooling rate. Both the ionic liquids exhibit glass transition under high pressure. XRD and low-frequency Raman spectra provide a consistent physical picture of structural ordering-disordering accompanying the thermal events of crystallization, glass transition, cold crystallization, pre-melting, and melting. Raman spectra in the high-frequency range of some specific cation and anion normal modes reveal conformational changes of the molecular structures along phase transitions.

Characterization of crystallographic properties of thin films using X-ray diffraction

NASA Astrophysics Data System (ADS)

Zoo, Yeongseok

2007-12-01

Silver (Ag) has been recognized as one of promising candidates in Ultra-Large Scale Integrated (ULSI) applications in that it has the lowest bulk electrical resistivity of all pure metals and higher electromigration resistance than other interconnect materials. However, low thermal stability on Silicon Dioxide (Si02) at high temperatures (e.g., agglomeration) is considered a drawback for the Ag metallization scheme. Moreover, if a thin film is attached on a substrate, its properties may differ significantly from that of the bulk, since the properties of thin films can be significantly affected by the substrate. In this study, the Coefficient of Thermal Expansion (CTE) and texture evolution of Ag thin films on different substrates were characterized using various analytical techniques. The experimental results showed that the CTE of the Ag thin film was significantly affected by underlying substrate and the surface roughness of substrate. To investigate the alloying effect for Ag meatallization, small amounts of Copper (Cu) were added and characterized using theta-2theta X-ray Diffraction (XRD) scan and pole figure analysis. These XRD techniques are useful for investigating the primary texture of a metal film, (111) in this study, which (111) is the notation of a specific plane in the orthogonal coordinate system. They revealed that the (111) textures of Ag and Ag(Cu) thin films were enhanced with increasing temperature. Comparison of texture profiles between Ag and Ag(Cu) thin films showed that Cu additions enhanced (111) texture in Ag thin films. Accordingly, the texture enhancement in Ag thin films by Cu addition was discussed. Strained Silicon-On-Insulator (SSOI) is being considered as a potential substrate for Complementary Metal-Oxide-Semiconductor (CMOS) technology since the induced strain results in a significant improvement in device performance. High resolution X-ray diffraction (XRD) techniques were used to characterize the perpendicular and parallel strains in SSOI layers. XRD diffraction profiles generated from the crystalline SSOI layer provided a direct measurement of the layer's strain components. In addition, it has demonstrated that the rotational misalignment between the layer and the substrate can be incorporated within the biaxial strain equations for epitaxial layers. Based on these results, the strain behavior of the SSOI layer and the relation between strained Si and SiO2 layers are discussed for annealed samples.

Landed XRD/XRF analysis of prime targets in the search for past or present Martian life.

PubMed

Vaniman, D; Bish, D; Blake, D; Elliott, S T; Sarrazin, P; Collins, S A; Chipera, S

1998-12-25

Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these "special" deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossil-bearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument. CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and discrimination of diffracted and fluoresced X rays. The ability to accumulate and integrate the entire circumference of each complete Debye diffraction ring compensates for poor powder preparations, as might be produced by robotic sampling systems. With CHEMIN, a wide range of minerals can be uniquely identified. Using Rietveld analysis of the XRD results, mineral quantification is also possible. Expanded capabilities in phase analysis and constrained data solutions using quantitative XRD and XRF are within reach.

Facile hydrothermal synthesis of one-dimensional nanostructured α-MnO2 for supercapacitors

NASA Astrophysics Data System (ADS)

Wei, Hongmei; Wang, Jinxing; Yang, Shengwei; Zhang, Yangyang; Li, Tengfei; Zhao, Shuoqing

2016-09-01

α-MnO2 recently becomes a promising candidate of electrode materials for high effective supercapacitors in which it possesses of unique structure of 2×2 tunnels that can provide more electrons and ions diffusion paths. In this work, different morphologies MnO2 with α-phase crystalline structure have been prepared via a one-step facile hydrothermal method by adding various reagents. Compositions, microstructures and morphologies of these as-synthesized materials were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and electrochemical properties of α-MnO2 electrodes were studied by the cyclic voltammetry (CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS) in 1 M Na2SO4 aqueous solution. The specific capacitance of nanowires were 158 F g-1 while the specific capacitance of nanorods were 106 F g-1 at current density of 4 A g-1, and improved performance of the wire-like electrode material was probably ascribed to the larger specific surface area that can provide relatively more active sites for high capacity. Meanwhile, both the nanowires and nanorods of MnO2 presented fine cycle stability after continuous multiple charge/discharge times.

Improved electrochemical performance of polyindole/carbon nanotubes composite as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Cai, Zhi-Jiang; Zhang, Qin; Song, Xian-You

2016-09-01

Polyindole/carbon nanotubes (PIN/CNTs) composite was prepared by an in-situ chemical oxidative polymerization of indole monomer with CNTs using ammonium persulfate as oxidant. The obtained composite material was characterized by SEM, TEM, FT-IR, Raman spectroscopy, XPS, XRD and BET surface areas measurements. It was found that the CNTs were incorporated into the PIN matrix and nanoporous structure was formed. Spectroscopy results showed that interfacial interaction bonds might be formed between the polyindole chains and CNTs during the in-situ polymerization. PIN/CNTs composite was evaluated by electrochemical impedance spectroscopy, cyclic voltammetry and charge/discharge tests to determine electrode performances in relation to supercapacitors properties in both aqueous and non-aqueous system. A maximum specific capacitance and specific volumetric capacitance of 555.6 F/g and 222.2 F/cm3 can be achieved at 0.5 A/g in non-aqueous system. It also displayed good rate performance and cycling stability. The specific capacitance retention is over 60% at 10 A/g and 91.3% after 5000 cycles at 2 A/g, respectively. These characteristics point to its promising applications in the electrode material for supercapacitors.

Synthesis of strontium hexaferrite nanoparticles prepared using co-precipitation method and microemulsion processing

NASA Astrophysics Data System (ADS)

Drmota, A.; Žnidaršič, A.; Košak, A.

2010-01-01

Strontium hexaferrite (SrFe12O19) nanoparticles have been prepared with co-precipitation in aqueous solutions and precipitation in microemulsion system water/SDS/n-butanol/cyclohexane, using iron and strontium nitrates in different molar rations as a starting materials. The mixed Sr2+, Fe3+ hydroxide precursors obtained during the reaction between corresponding metal nitrates and tetramethylammonium hydroxide (TMAH), which served as a precipitating reagent, were calcined in a wide temperature range, from 350 °C to 1000 °C in a static air atmosphere. The influence of the Sr2+/Fe3+ molar ratio and the calcination temperature to the chemistry of the product formation, its crystallite size, morphology and magnetic properties were investigated. It was found that the formation of single phase SrFe12O19 with relatively high specific magnetization (54 Am2/kg) was achieved at the Sr2+/Fe3+ molar ration of 6.4 and calcination at 800 °C for 3h with heating/cooling rate 5 °C/min. The prepared powders were characterized using X-ray diffractometry (XRD) and specific surface area measurements (BET). The specific magnetization (DSM-10, magneto-susceptometer) of the prepared samples was measured.

Acid activation of upper Eocene Ca-bentonite for soybean oil clarification.

PubMed

Chakroun, Salima; Herchi, Mongi; Mechti, Wafa; Gaied, Mohamed Essghaier

2017-10-01

In central Tunisia, many upper Eocene outcrops supply smectitic claystone which are characterized by several analytical techniques (calcimetry, XRD, SediGraph, chemical analysis, surface area, etc.). Beidellite is the main mineral detected by the XRD method. Representative raw samples M1, taken from Henchir Souar (Zaghouan, Tunisia), were acid activated in order to improve their physicochemical properties. This study consists in optimizing the activation conditions with HCl 3 N by varying the following parameters: time (2, 4, and 6 h) and temperature (25, 50, 75, and 90 °C). The characterization by XRD and chemical analysis was carried out on the samples (M1, activated for 2 and 6 h at 75 °C), showing a structural modification of the clay by reduction of intensity reflection 001 order of smectite and dissolution of metal ions (Al 3+ , Fe 3+ , and Mg 2+ ) from clay structure. Optimum condition for soybean oil clarification is obtained using a variety of amount raw clays (0.5, 0.75, and 1%). Thus, the best clarification yield is given at 0.75% of clay, showing a capacity of about 55%. Various forms of activated materials were used with a 75% proportion to leach soybean oil. Results were compared with commercial bentonite (Tonsil) having surface area (378 m 2 /g). The activated sample M1 during 4 h at 75 °C possesses a decolorizing capacity of about 85% greater than the oil treated by Tonsil in laboratory (58%).

Synthesis, characterization and magnetic behavior of Co/MCM-41 nano-composites

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

Cuello, N.; Elías, V.; CONICET

2013-09-15

Synthesis, structure and magnetic properties of Co/MCM-41 as magnetic nano-composites have been investigated. Mesoporous materials with different degrees of metal loading were prepared by wet impregnation and characterized by ICP, XRD, N{sub 2} adsorption, UV–vis DRS, TPR and EPMA-EDS. Cobalt oxide clusters and Co{sub 3}O{sub 4} nano-particles could be confined inside the mesopores of MCM-41, being this fact favored by the Co loading increasing. In addition, larger crystals of Co{sub 3}O{sub 4} detectable by XRD also grow on the surface when the Co loading is enhanced. The magnetic characterization was performed in a SQUID magnetometer using a maximum magnetic appliedmore » field µ{sub 0}Ha=1 T. While the samples with the higher Co loadings showed a behavior typically paramagnetic, a superparamagnetic contribution is more notorious for lower loadings, suggesting high Co species dispersion. - Graphical abstract: Room temperature hysteresis loops as a function of the Co content. Display Omitted - Highlights: • Co species as isolated Co{sup 2+}, oxide clusters and Co{sub 3}O{sub 4} nano-particles were detected. • For higher Co loads were detected, by XRD, Co{sub 3}O{sub 4} particles on the external surface. • The confining of Co species inside the mesopores was achieved by increasing Co load. • Paramagnetism from oxide clusters/nano-particles becomes dominant for higher Co loads. • Superparamagnetism can be assigned to Co species of small size and finely dispersed.« less

Magnetic transition in Y-site doped multiferroic YMnO3

NASA Astrophysics Data System (ADS)

Thakur, Rajesh K.; Thakur, Rasna; Gaur, N. K.

2016-05-01

We have synthesized polycrystalline hexagonal Y1-xSrxMnO3 (x=0.02, 0.1) compounds by using conventional solid state reaction method. The detailed structural investigations are carried out by using XRD studies which reveals the single phase formation of the reported compounds with hexagonal structure and space group P63cm (JCPDS: 25-1079). Further the XRD data of reported compounds were analyzed by RIETVELD (FULLPROFF) method which shows the decrease in the lattice parameter with increasing concentration of divalent strontium to Y-site. The observed pointed kinks in the specific heat study are indicative of the probable coupling in between the electric and magnetic orders in this class of materials. The reported systematic specific heat studies shows that the antiferromagnetic (AFM) transition temperature (TN) shifts to higher value with increasing concentration of Sr2+ ion in the YMnO3 compound which is attributed to the enhanced lattice contribution to the specific heat in the this compound. The present compound shows the independence of specific heat and magnetic transition temperature with applied magnetic field of 8T and 12T.

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

Adsorption of Lysine on Na-Montmorillonite and Competition with Ca(2+): A Combined XRD and ATR-FTIR Study.

PubMed

Yang, Yanli; Wang, Shengrui; Liu, Jingyang; Xu, Yisheng; Zhou, Xiaoyun

2016-05-17

Lysine adsorption at clay/aqueous interfaces plays an important role in the mobility, bioavailability, and degradation of amino acids in the environment. Knowledge of these interfacial interactions facilitates our full understanding of the fate and transport of amino acids. Here, X-ray diffraction (XRD) and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) measurements were used to explore the dynamic process of lysine adsorption on montmorillonite and the competition with Ca(2+) at the molecular level. Density functional theory (DFT) calculations were employed to determine the peak assignments of dissolved lysine in the solution phase. Three surface complexes, including dicationic, cationic, and zwitterionic structures, were observed to attach to the clay edge sites and penetrate the interlayer space. The increased surface coverage and Ca(2+) competition did not affect the interfacial lysine structures at a certain pH, whereas an elevated lysine concentration contributed to zwitterionic-type coordination at pH 10. Moreover, clay dissolution at pH 4 could be inhibited at a higher surface coverage with 5 and 10 mM lysine, whereas the inhibition effect was inconspicuous or undetected at pH 7 and 10. The presence of Ca(2+) not only could remove a part of the adsorbed lysine but also could facilitate the readsorption of dissolved Si(4+) and Al(3+) and surface protonation. Our results provide new insights into the process of lysine adsorption and its effects on montmorillonite surface sites.

A Defect Structure for 6-Line Ferrihydrite Nanoparticles (Invited)

NASA Astrophysics Data System (ADS)

Gilbert, B.; Spagnoli, D.; Fakra, S.; Petkov, V.; Penn, R. L.; Banfield, J. F.; Waychunas, G.

2010-12-01

Ferrihydrite is an environmental iron oxyhydroxide mineral that is only found in the form of nanoscale particles yet exerts significant impacts on the biogeochemistry of soils, sediments and surface waters. This material has remained poorly characterized due to significant experimental challenges in determining stoichiometry and structure. In a breakthrough, Michel et al., Science 316, 1726 (2007), showed that real-space pair distribution function (PDF) data from ferrihydrite samples with a range of particle sizes could be modeled by a single newly proposed crystal phase. However, ambiguity remained as to the relationship between this model and real ferrihydrite structure because that model does not perfectly reproduce the reciprocal-space X-ray diffraction data (XRD). Subsequently, Michel et al. PNAS 107, 2787 (2010), demonstrated that ferrihydrite could be thermally coarsened to form an annealed nanomaterial for which both XRD and PDF data are reproduced by a refined version of their original structure. These findings confirmed that the Michel et al. structure is a true mineral phase, but do not resolve the question of how to adequately describe the structure of ferrihydrite nanoparticles formed by low-temperature precipitation in surface waters. There is agreement that a model based upon a single unit cell cannot capture the structural diversity present in real nanoparticles, which can include defects, vacancies and disorder, particularly surface strain. However, for the Michel et al. model of ferrihydrite the disagreement between simulated and experimental XRD is significant, indicating either that the underlying structural model is incorrect; that the assumption that a single phase is sufficient to describe the nanomaterial is not valid; or that ferrihydrite nanoparticles possess an unusually large amount of disorder that must be characterized. Thus, quantitative tests of explicit structural configurations are essential to understand the real nanoparticle disorder and to test the correctness of an underlying phase described by a single unit cell. We reviewed the crystal chemistry of the Michel et al. structure and alternatives and developed hypotheses for plausible structural defects. We developed a novel reverse Monte Carlo (RMC) algorithm that generates defects and disorder within full-nanoparticle structural models and simulates the corresponding PDF and wide-angle XRD patterns for comparison with experimental data. This successfully generated full-nanoparticle structures that are in agreement with both real- and reciprocal-space X-ray scattering data. RMC-derived structures may be incorrect, and are not unique, and must therefore be evaluated for chemical plausibility as emphasized by Manceau, Clay Minerals 44, 19 (2009). Nevertheless, the results show that the inclusion of disorder and defects in full-nanoparticle model of ferrihydrite can resolve the discrepancy between XRD and PDF results found for a model based upon a single unit cell.

Surface characterization of cottonseed meal products by SEM, SEM-EDS, XRD and XPS analysis

USDA-ARS?s Scientific Manuscript database

The utilization of cottonseed meal as a valuable industrial feedstock needs to be exploited. We have recently produced water-washed cottonseed meal, total cottonseed protein, sequentially extracted water- and alkali-soluble proteins, and two residues after the total and sequential protein extraction...

Methanol Oxidation Using Ozone on Titania-Supported Vanadium Catalyst

EPA Science Inventory

Ozone-enhanced catalytic oxidation of methanol has been conducted at mild temperatures of 100 to 250NC using V2O5/TiO2 catalyst prepared by the sol-gel method. The catalyst was characterized using XRD, surface area measurements, and temperature-programmed desorption of methanol. ...

Facile synthesis of high surface area molybdenum nitride and carbide

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

Roy, Aaron; Serov, Alexey; Artyushkova, Kateryna

2015-08-15

The synthesis of high surface area γ-Mo{sub 2}N and α-Mo{sub 2}C is reported (116 and 120 m{sup 2}/g) without the temperature programmed reduction of MoO{sub 3}. γ-Mo{sub 2}N was prepared in an NH{sub 3}-free synthesis using forming gas (7 at% H{sub 2}, N{sub 2}-balance) as the reactive atmosphere. Three precursors were studied ((NH{sub 4}){sub 6}Mo{sub 7}O{sub 24}·4H{sub 2}O, (NH{sub 4}){sub 2} Mg(MoO{sub 4}){sub 2}, and MgMoO{sub 4}) along with the sacrificial support method (SSM) as a means of reducing the particle size of Mo{sub 2}N and Mo{sub 2}C. In situ X-ray diffraction (XRD) studies were carried out to identify reactionmore » intermediates, the temperature at which various intermediates form, and the average domain size of the Mo{sub 2}N products. Materials were synthesized in bulk and further characterized by XRD, HRTEM, XPS, and BET. - Highlights: • Facile synthesis of γ-Mo2N and α-Mo2C with surface area exceeding 100 m{sup 2}/g. • Sacrificial support method was used to achieve these high surface areas. • Materials can serve as catalysts or supports in (electro)chemical processes.« less

Surface morphological, structural, electrical and optical properties of GaN-based light-emitting diodes using submicron-scaled Ag islands and ITO thin films

NASA Astrophysics Data System (ADS)

Lee, Young-Woong; Reddy, M. Siva Pratap; Kim, Bo-Myung; Park, Chinho

2018-07-01

An ITO-Ag islands complex as a new transparent conducting electrode (TCE) structure (on the 5 nm-thick p-InGaN/90 nm-thick p-GaN) for achieving high-performance and more reliable GaN-based LEDs were fabricated. A normal LED with a conventional ITO TCE was also compared. The surface morphological, structural, electrical and optical properties of fabricated GaN-based light-emitting diodes using a complex electrode of submicron-scaled Ag islands and ITO thin films are explored by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), current-voltage (I-V) and output power-current (L-I) techniques. Surface morphology investigations revealed Ag islands formed uniformly on the p-InGaN/p-GaN surface during rapid thermal annealing at 400 °C for 1 min in N2 ambient. The ohmic properties and overall device-performance of the suggested contact and device structures were superior to those in the conventional ITO contact and normal ITO LED structures. Based on the results of XRD and XPS measurements, the formation of the intermetallic gallide phases (AgGa) is responsible for better performance characteristics of the ITO-Ag islands device. The significant improvements are described in terms of the conducting bridge influence, highly effective micro-mirror effect, and wider photon window via the roughened structure.

Multiple techniques for mineral identification of terrestrial evaporites relevant to Mars exploration

NASA Astrophysics Data System (ADS)

Stivaletta, N.; Dellisanti, F.; D'Elia, M.; Fonti, S.; Mancarella, F.

2013-05-01

Sulfates, commonly found in evaporite deposits, were observed on Mars surface during orbital remote sensing and surface exploration. In terrestrial environments, evaporite precipitation creates excellent microniches for microbial colonization, especially in desert areas. Deposits comprised of gypsum, calcite, quartz and silicate deposits (phyllosilicates, feldspars) from Sahara Desert in southern Tunisia contain endolithic colonies just below the rock surface. Previous optical observations verified the presence of microbial communities and, as described in this paper, spectral visible analyses have led to identification of chlorophylls belonging to photosynthetic bacteria. Spectral analyses in the infrared region have clearly detected the presence of gypsum and phyllosilicates (mainly illite and/or smectite), as well as traces of calcite, but not quartz. X-ray diffraction (XRD) analysis has identified the dominant presence of gypsum as well as that of other secondary minerals such as quartz, feldspars and Mg-Al-rich phyllosilicates, such as chlorite, illite and smectite. The occurrence of a small quantity of calcite in all the samples was also highlighted by the loss of CO2 by thermal analysis (TG-DTA). A normative calculation using XRD, thermal data and X-ray fluorescence (XRF) analysis has permitted to obtain the mineralogical concentration of the minerals occurring in the samples. The combination of multiple techniques provides information about the mineralogy of rocks and hence indication of environments suitable for supporting microbial life on Mars surface.

[Effects of magnetron sputtered ZrN on the bonding strength of titanium porcelain].

PubMed

Zhou, Shu; Zhang, Wen-yan; Guang, Han-bing; Xia, Yang; Zhang, Fei-min

2009-04-01

To investigate the effect of magnetron sputtered ZrN on the bonding strength between a low-fusing porcelain (Ti/Vita titankeramik system) and commercially pure cast titanium. Sixteen specimens were randomly assigned to test group and control group (n=8). The control group received no surface treated. Magnetron sputtered ZrN film was deposited on the surface of specimens in the test group. Then the sixteen titanium-porcelain specimens were prepared in a rectangular shape and went through three-point bending test on a universal test machine. The bond strength of Ti/porcelain was recorded. The phase composition of the specimens was analyzed using X-ray diffraction (XRD). The interface at titanium and porcelain and the titanium surface after debonding were observed with a scanning electron microscopy (SEM) and analyzed using energy depressive spectrum (EDS). New phase of ZrN was found with XRD in the test group. Statistical analysis showed higher bond strength following ZrN surface treatment in the test group [(45.991+/-0.648) MPa] than that in the control group [(29.483+/-1.007) MPa] (P=0.000). Bonded ceramic could be observed in test group, the amount of bonded ceramic was more than that in the control group. No obvious bonded ceramic in control group was found. Magnetron sputtered ZrN can improve bond strength of Ti/Vita titankeramik system significantly.

Crystal structure, Hirshfeld surfaces computational study and physicochemical characterization of the hybrid material (C7H10N)2[SnCl6]·H2O

NASA Astrophysics Data System (ADS)

BelhajSalah, S.; Abdelbaky, Mohammed S. M.; García-Granda, Santiago; Essalah, K.; Ben Nasr, C.; Mrad, M. L.

2018-01-01

A novel hybrid compound, bis(4-methylanilinium)hexachlorostannate(IV) monohydrate, formulated as (C7H10N)2[SnCl6]·H2O, has been prepared and characterized by powder and single crystal X-ray diffraction (XRD), Hirshfeld surface analysis, infrared spectroscopy (IR), optical study, differential thermal analysis(DTA) and X-ray photoelectron spectroscopy analysis (XPS). The title compound crystallizes in the monoclinic space group P21/c with a = 13.093(1)Å, b = 7.093(6)Å, c = 24.152(2)Å, β = 98.536(4)⁰ and V = 2218.4(4) Å3. Their crystal structure exhibits alternating inorganic layers parallel to the (ab) plane at z = n/2. The different entities, [SnCl6]2-, organic cations and water molecules, are connected via hydrogen bonds to form a three-dimensional network. The powder XRD data confirms the phase purity of the crystalline sample. The intermolecular interactions were investigated by Hirshfeld surfaces. The vibrational absorption bands were identified by IR spectroscopy and have been discussed. The optical properties of the crystal were studied by using optical absorption, UV-visible absorption and photoluminescence spectroscopy studies. The compound was also characterized by DTA to determine its thermal behavior with respect to the temperature. Finally, XPS technique is reported for analyzing the surface chemistry of this compound.

Study of irradiation induced surface pattern and structural changes in Inconel 718 alloy

NASA Astrophysics Data System (ADS)

Wan, Hao; Si, Naichao; Zhao, Zhenjiang; Wang, Jian; Zhang, Yifei

2018-05-01

Helium ions irradiation induced surface pattern and structural changes of Inconel 718 alloy were studied with the combined utilization of atomic force microscopy (AFM), x-ray diffraction (XRD) and transmission electron microscopy (TEM). In addition, SRIM-2013 software was used to calculate the sputtering yield and detailed collision events. The result shows that, irradiation dose play an important role in altering the pattern of the surface. Enhanced irradiation aggravated the surface etching and increased the surface roughness. In ion irradiated layer, large amount of interstitials, vacancies and defect sinks were produced. Moreover, in samples with increasing dose irradiation, the dependence of interplanar spacing variation due to point defects clustering on sink density was discussed.

Improved wear resistance by phase transformation of surface nanocrystalline 1090 steel prepared by sandblasting technique

NASA Astrophysics Data System (ADS)

Peng, Rong; Fu, Licai; Zhou, Lingping

2016-12-01

A surface nanocrystalline 1090 steel has been fabricated by using sandblasting technique. The surface average grain size was about 78 nm. The high strain rate and strain in sandblasting were main reasons for surface nanocrystallization. The wear resistance of 1090 steel was considerably enhanced as grain size decreased. The microstructure and hardness of contact zones before and after wear tests have been examined by XRD, SEM and TEM. Except the higher hardness, the results demonstrated that parts of ferrite transferred to cementite and martensite. It was additional beneficial for improving the wear resistance of 1090 steel as the grain size decreased.

Enhanced removal of As (V) from aqueous solution using modified hydrous ferric oxide nanoparticles

PubMed Central

Huo, Lijuan; Zeng, Xibai; Su, Shiming; Bai, Lingyu; Wang, Yanan

2017-01-01

Hydrous ferric oxide (HFO) is most effective with high treatment capacity on arsenate [As(V)] sorption although its transformation and aggregation nature need further improvement. Here, HFO nanoparticles with carboxymethyl cellulose (CMC) or starch as modifier was synthesized for the purpose of stability improvement and As(V) removal from water. Comparatively, CMC might be the optimum stabilizer for HFO nanoparticles because of more effective physical and chemical stability. The large-pore structure, high surface specific area, and the non-aggregated nature of CMC-HFO lead to increased adsorption sites, and thus high adsorption capacities of As(V) without pre-treatment (355 mg·g−1), which is much greater than those reported in previous studies. Second-order equation and dual-mode isotherm model could be successfully used to interpret the sorption kinetics and isotherms of As(V), respectively. FTIR, XPS and XRD analyses suggested that precipitation and surface complexation were primary mechanisms for As(V) removal by CMC modified HFO nanoparticles. A surface complexation model (SCM) was used to simulate As adsorption over pH 2.5–10.4. The predominant adsorbed arsenate species were modeled as bidentate binuclear surface complexes at low pH and as monodentate complexes at high pH. The immobilized arsenic remained stable when aging for 270 d at room temperature. PMID:28098196

Enhanced removal of As (V) from aqueous solution using modified hydrous ferric oxide nanoparticles

NASA Astrophysics Data System (ADS)

Huo, Lijuan; Zeng, Xibai; Su, Shiming; Bai, Lingyu; Wang, Yanan

2017-01-01

Hydrous ferric oxide (HFO) is most effective with high treatment capacity on arsenate [As(V)] sorption although its transformation and aggregation nature need further improvement. Here, HFO nanoparticles with carboxymethyl cellulose (CMC) or starch as modifier was synthesized for the purpose of stability improvement and As(V) removal from water. Comparatively, CMC might be the optimum stabilizer for HFO nanoparticles because of more effective physical and chemical stability. The large-pore structure, high surface specific area, and the non-aggregated nature of CMC-HFO lead to increased adsorption sites, and thus high adsorption capacities of As(V) without pre-treatment (355 mg·g-1), which is much greater than those reported in previous studies. Second-order equation and dual-mode isotherm model could be successfully used to interpret the sorption kinetics and isotherms of As(V), respectively. FTIR, XPS and XRD analyses suggested that precipitation and surface complexation were primary mechanisms for As(V) removal by CMC modified HFO nanoparticles. A surface complexation model (SCM) was used to simulate As adsorption over pH 2.5-10.4. The predominant adsorbed arsenate species were modeled as bidentate binuclear surface complexes at low pH and as monodentate complexes at high pH. The immobilized arsenic remained stable when aging for 270 d at room temperature.

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.

Crystallization processes in Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass

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

Svoboda, Roman, E-mail: roman.svoboda@upce.cz; Bezdička, Petr; Gutwirth, Jan

2015-01-15

Highlights: • Crystallization kinetics of Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass was studied in dependence on particle size by DSC. • All studied fractions were described in terms of the SB autocatalytic model. • Relatively high amount of Te enhances manifestation of bulk crystallization mechanisms. • XRD analysis of samples crystallized under different conditions showed correlation with DSC data. • XRD analysis revealed a new crystallization mechanism indistinguishable by DSC. - Abstract: Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) analysis were used to study crystallization in Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass under non-isothermal conditions as a function of the particlemore » size. The crystallization kinetics was described in terms of the autocatalytic Šesták–Berggren model. An extensive discussion of all aspects of a full-scale kinetic study of a crystallization process was undertaken. Dominance of the crystallization process originating from mechanically induced strains and heterogeneities was confirmed. Substitution of Se by Te was found to enhance the manifestation of the bulk crystallization mechanisms (at the expense of surface crystallization). The XRD analysis showed significant dependence of the crystalline structural parameters on the crystallization conditions (initial particle size of the glassy grains and applied heating rate). Based on this information, a new microstructural crystallization mechanism, indistinguishable by DSC, was proposed.« less

Effect of calcination temperature on structure and photocatalytic activity under UV and visible light of nanosheets from low-cost magnetic leucoxene mineral

NASA Astrophysics Data System (ADS)

Charerntanom, Wissanu; Pecharapa, Wisanu; Pavasupree, Suttipan; Pavasupree, Sorapong

2017-07-01

This research has experimentally synthesized the nanosheets from the naturally-mineral magnetic leucoxene under the hydrothermal synthesis condition of 105 °C for 24 h. Magnetic leucoxene was utilized as the starting material due to its high TiO2 content (70-80%) and inexpensiveness. The characterization of the synthesized nanosheets was subsequently carried out: the crystalline structure, the chemical composition, the shape, the size and the specific surface area, by the X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) specific surface area analysis. The analysis results indicated that the starting magnetic leucoxene is of rutile phase while the synthesized nanosheets are of titanate structure (H2TixO2x + 1). After calcination at the temperature range of 300 and 400 °C, the calcined samples demonstrated TiO2 (B). At 500 and 600 °C, the calcined nanosheets revealed a bi-crystalline mixture consisting of TiO2 (B) and anatase TiO2. At 700-1000 °C, the crystalline structure shows anatase and rutile phase. At 1100 °C, the prepared samples consisted of a mixture of anatase, rutile phase of TiO2, and Fe2O3 phase. The synthesized product also exhibited the flower-like morphology with 2-5 μm in diameter, and the nanosheets structure was slightly curved, with 100 nm to 2 μm in width and 1-3 nm in thickness. At 100-200 °C showed sheets-like structure. At 300-1100 °C, the calcined nanosheets became unstable and began to decompose and transform into nanoparticles. The increasing size of nanoparticle decreased the specific surface area of the nanosheets, caused by increasing calcination temperature. Furthermore, the BET specific surface area of the nanosheets was approximately 279.8 m2/g. More importantly, the synthesized nanosheets achieved the higher photocatalytic activity under UV and visible light than did the commercial TiO2 nanoparticles (JRC-01, JRC-03, ST-01 and P-25).

The synergistic effects of combining the high energy mechanical milling and wet milling on Si negative electrode materials for lithium ion battery

NASA Astrophysics Data System (ADS)

Hou, Shang-Chieh; Su, Yuh-Fan; Chang, Chia-Chin; Hu, Chih-Wei; Chen, Tsan-Yao; Yang, Shun-Min; Huang, Jow-Lay

2017-05-01

The submicro-sized and nanostructured Si aggregated powder is prepared by combinational routes of high energy mechanical milling (HEMM) and wet milling. Milled Si powder is investigated by particle size analyzer, SEM, TEM, XPS and XRD as well as the control ones. Its electrode is also investigated by in situ XRD and electrochemical performance. Morphology reveals that combining the high energy mechanical milling and wet milling not only fracture primary Si particles but also form submicro-sized Si aggregates constructed by amorphous and nanocrystalline phases. Moreover, XPS shows that wet milling in ethanol trigger Sisbnd Osbnd CH2CH3 bonding on Si surface might enhance the SEI formation. In situ XRD analysis shows negative electrode made of submicro-sized Si aggregated powder can effectively suppress formation of crystalline Li15Si4 during lithiation and delithiation due to amorphous and nanocrystalline construction. Thus, the submicro-sized Si powder with synergistic effects combining the high energy mechanical milling and wet milling in ethanol as negative electrode performs better capacity retention.

Nanocomposite bulk of mechanically milled Al-Pb samples consolidated pore-free by the high-energy rate forming technique.

PubMed

Csanády, Agnes; Sajó, István; Lábár, János L; Szalay, András; Papp, Katalin; Balaton, Géza; Kálmán, Erika

2005-06-01

It is shown that pore-free bulk samples were produced by the high-energy rate forming axis-symmetrical powder compaction method for different application purposes in case of the very different, immiscible Al and Pb metal pair. The starting Al-Pb nanocomposites were made by mechanical milling of atomized Al and Pb powders either in a SPEX 9000 or a Fritsch Pulverisette 4 mill. Due to the conditions that milling was carried out in air, the PbO layer, originally existing at the surface of the atomized Pb powder, ruptured and was also dispersed in the composite. The presence of the nano PbO particles was proven by XRD and TEM (BF, DF, SAED). When the energy of milling was high, the PbO crystallites became so small that they could hardly be seen by XRD technique. Local distribution of the PbO nanoparticles was still visible in a TEM, using the process diffraction method. Both XRD and SAED proved to be useful for the evaluation of the results of the milling process and compaction.

Structural and magnetic properties of nanocomposite iron-containing SiCxNy films

NASA Astrophysics Data System (ADS)

Pushkarev, R. V.; Fainer, N. I.; Maurya, K. K.

2017-02-01

New ferromagnetic films with composition SiCxNyFez were synthesized using chemical vapor deposition technique. Films were deposited using ferrocene, 1,1,1,3,3,3-hexamethyldisilazane (HMDS) and hydrogen gaseous mixture. Chemical and phase composition of the films were studied by FTIR, Raman spectroscopy and X-ray diffraction with grazing incidence (GI-XRD). FTIR spectra analysis confirmed the existence of Si-C and Si-N bonds. Graphite inclusions and amorphous carbon were determined by Raman spectra analysis. The surface of the SiCxNyFez films studied by SEM is covered by nanocrystallites of iron oxide Fe3O4 phase. The main purpose of GI-XRD analysis is to describe the layered structure of the films in detail. It was shown by GI-XRD study, that phase composition of the SiCxNyFez films varies from iron oxide Fe3O4 to iron silicide Fe3Si and silicon carbide SiC with the deposition temperature growing. It was established, that SiCxNyFez films are perspective for application in the spintronic field.

Synthesis, structural, characterization and dielectric spectroscopy of PVDF - BaTiO3 polymer composite

NASA Astrophysics Data System (ADS)

Kulkarni, S. S.; Belavi, P. B.; Khadke, U. V.

2018-05-01

In this paper we report the method of synthesis of ferroelectric polymer Polyvinyldene fluoride (PVDF) and Barium Titanate (BaTiO3) composite self supporting thin films and its dielectric response. BaTiO3 was synthesized by solid state reaction method. The PVDF - BaTiO3 polymer composites with various concentrations were synthesized by solution mixing method using Dimethylformadide (DMF) as a solvent. The phase transformation and surface methodology of the prepared composites were characterized by X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) respectively. The XRD pattern confirms the formation of tetragonal pervoskite structure of ferroelectric phase. The XRD pattern shows the proper mixing of BaTiO3 particles intestinally and found to be improving its crystallinity with increase of BaTiO3 composition in the PVDF matrix. The dielectric properties of the composites as a function of frequency were computed using impedance analyzer. The dielectric constant decreases with increase of frequency shows the Maxwell - Wagner type of interfacial polarization in accordance with Koop's phenomenological theory.

Microwave Synthesis, Characterization, and Photoluminescence Properties of Nanocrystalline Zirconia

PubMed Central

Singh, A. K.; Nakate, Umesh T.

2014-01-01

We report synthesis of ZrO2 nanoparticles (NPs) using microwave assisted chemical method at 80°C temperature. Synthesized ZrO2 NPs were calcinated at 400°C under air atmosphere and characterized using FTIR, XRD, SEM, TEM, BET, and EDS for their formation, structure, morphology, size, and elemental composition. XRD results revealed the formation of mixed phase monoclinic and tetragonal ZrO2 phases having crystallite size of the order 8.8 nm from most intense XRD peak as obtained using Scherrer formula. Electron microscope analysis shows that the NPs were less than 10 nm and highly uniform in size having spherical morphology. BET surface area of ZrO2 NPs was found to be 65.85 m2/g with corresponding particle size of 16 nm. The band gap of synthesized NPs was found to be 2.49 eV and PL spectra of ZrO2 synthesized NPs showed strong peak at 414 nm, which corresponds to near band edge emission (UV emission) and a relatively weak peak at 475 and 562 nm. PMID:24578628

Influence of Te and Se doping on ZnO films growth by SILAR method

NASA Astrophysics Data System (ADS)

Güney, Harun; Duman, Ćaǧlar

2016-04-01

The AIP Successive ionic layer adsorption and reaction (SILAR) is an economic and simple method to growth thin films. In this study, SILAR method is used to growth Selenium (Se) and Tellurium (Te) doped zinc oxide (ZnO) thin films with different doping rates. For characterization of the films X-ray diffraction (XRD), absorbance and scanning electron microscopy (SEM) are used. XRD results are showed well-defined strongly (002) oriented crystal structure for all samples. Also, absorbance measurements show, Te and Se concentration are proportional and inversely proportional with band gap energy, respectively. SEM measurements show that the surface morphology and thickness of the material varied with Se and/or Te and varying concentrations.

Morphology-controllable of Sn doped ZnO nanorods prepared by spray pyrolysis for transparent electrode application

NASA Astrophysics Data System (ADS)

Hameed, M. Shahul; Princice, J. Joseph; Babu, N. Ramesh; Zahirullah, S. Syed; Deshmukh, Sampat G.; Arunachalam, A.

2018-05-01

Transparent conductive Sn doped ZnO nanorods have been deposited at various doping level by spray pyrolysis technique on glass substrate. The structural, surface morphological and optical properties of these films have been investigated with the help of X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscope (AFM) and UV-Vis spectrophotometer respectively. XRD patterns revealed a successful high quality growth of single crystal ZnO nanorods with hexagonal wurtzite structure having (002) preferred orientation. The scanning electron microscope (SEM) image of the prepared films exposed the uniform distribution of Sn doped ZnO nanorod shaped grains. All these films were highly transparent in the visible region with average transmittance of 90%.

Influence of Te and Se doping on ZnO films growth by SILAR method

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

Güney, Harun, E-mail: harunguney25@hotmail.com; Duman, Çağlar, E-mail: caglarduman@erzurum.edu.tr

2016-04-18

The AIP Successive ionic layer adsorption and reaction (SILAR) is an economic and simple method to growth thin films. In this study, SILAR method is used to growth Selenium (Se) and Tellurium (Te) doped zinc oxide (ZnO) thin films with different doping rates. For characterization of the films X-ray diffraction (XRD), absorbance and scanning electron microscopy (SEM) are used. XRD results are showed well-defined strongly (002) oriented crystal structure for all samples. Also, absorbance measurements show, Te and Se concentration are proportional and inversely proportional with band gap energy, respectively. SEM measurements show that the surface morphology and thickness ofmore » the material varied with Se and/or Te and varying concentrations.« less

Synthesis of new oligothiophene derivatives and their intercalation compounds: Orientation effects

USGS Publications Warehouse

Ibrahim, M.A.; Lee, B.-G.; Park, N.-G.; Pugh, J.R.; Eberl, D.D.; Frank, A.J.

1999-01-01

The orientation dependence of intercalated oligothiophene derivatives in vermiculite and metal disulfides MS2 (M = Mo, Ti and Zr) on the pendant group on the thiophene ring and the host material was studied by X-ray diffraction (XRD) and solid state nuclear magnetic resonance spectroscopy. Amino and nitro derivatives of bi-, ter- and quarter-thiophenes were synthesized for the first time. The amino-oligothiophenes were intercalated into vermiculite by an exchange reaction with previously intercalated octadecylammonium vermiculite and into MS2 by the intercalation-exfoliation technique. Analysis of the XRD data indicates that a monolayer of amino-oligothiophene orients perpendicularly to the silicate surface in vermiculite and lies flat in the van der Waals gap of MS2.

Structural and magnetic analysis of Cu, Co substituted NiFe{sub 2}O{sub 4} thin films

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

Sharma, Hakikat; Bala, Kanchan; Negi, N. S.

2016-05-23

In the present work we prepared NiFe{sub 2}O{sub 4}, Ni{sub 0.95}Cu{sub 0.05}Fe{sub 2}O{sub 4} and Ni{sub 0.94}Cu{sub 0.05}Co{sub 0.01} Fe{sub 2}O{sub 4} thin films by metallo-organic decomposition method (MOD) using spin coating technique. The thin films were analyzed by X-ray diffractometer (XRD) and Atomic force microscope (AFM) for structural studies. The XRD patterns confirmed the ferrite phase of thin films. From AFM, we analyzed surface morphology, calculated grain size (GS) and root mean square roughness (RMSR). Room temperature magnetic properties were investigated by vibrating sample magnetometer (VSM).

Combustion synthesis and structural analysis of nanocrystalline nickel ferrite at low temperature regime

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

Shanmugavel, T., E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Raj, S. Gokul, E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Rajarajan, G.

2015-06-24

Combustion synthesis of single phase Nickel ferrite was successfully achieved at low temperature regime. The obtained powders were calcinated to increase the crystallinity and their characterization change due to calcinations is investigated in detail. Citric acid used as a chelating agent for the synthesis of nickel ferrite. Pure single phase nickel ferrites were found at this low temperature. The average crystalline sizes were measured by using powder XRD measurements. Surface morphology was investigated through Transmission Electron Microscope (TEM). Particle size calculated in XRD is compared with TEM results. Magnetic behaviour of the samples is analyzed by using Vibrating Sample Magnetometermore » (VSM). Saturation magnetization, coercivity and retentivity are measured and their results are discussed in detail.« less

Particle size distribution control of Pt particles used for particle gun

NASA Astrophysics Data System (ADS)

Ichiji, M.; Akiba, H.; Nagao, H.; Hirasawa, I.

2017-07-01

The purpose of this study is particle size distribution (PSD) control of submicron sized Pt particles used for particle gun. In this report, simple reaction crystallization is conducted by mixing H2PtCl6 and ascorbic acid. Without the additive, obtained Pt particles have broad PSD and reproducibility of experiment is low. With seeding, Pt particles have narrow PSD and reproducibility improved. Additionally, mean particle diameter of 100-700 nm is controlled by changing seeding amount. Obtained particles are successfully characterized as Pt by XRD results. Moreover, XRD spectra indicate that obtained particles are polycrystals. These experimental results suggest that seeding consumed nucleation, as most nuclei attached on the seed surface. This mechanism virtually restricted nucleation to have narrow PSD can be obtained.

The PM2.5 capture of poly (lactic acid)/nano MOFs eletrospinning membrane with hydrophilic surface

NASA Astrophysics Data System (ADS)

Wang, Yating; Dai, Xiu; Li, Xu; Wang, Xinlong

2018-03-01

In this article, metal organic frameworks (MOFs) material is introduced in the poly (lactic acid) (PLA) by electrospinning to fabricate the nanocomposite membrane. The acrylic acid (AA) is grafted onto the membrane under UV light. The prepared membrane is studied by scanning electron microscopy (SEM), x-ray diffraction (XRD), thermogravimetry (TG), contact angle test and tensile strength test. The SEM image and XRD indicate that nano MOFs particles adhere to the membrane. Contact angle test shows that grafting AA on the composite fiber membrane improves its hydrophilicity effectively. TG analyses show that the particulate matter (PM) capture capacity of PLA membrane with 2 wt% ZIF-8 content is 22%, which rises to 37% after grafting.

Synthesis of TiN/a-Si3N4 thin film by using a Mather type dense plasma focus system

NASA Astrophysics Data System (ADS)

Hussain, T.; R., Ahmad; Khalid, N.; A. Umar, Z.; Hussnain, A.

2013-05-01

A 2.3 kJ Mather type pulsed plasma focus device was used for the synthesis of a TiN/a-Si3N4 thin film at room temperature. The film was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The XRD pattern confirms the growth of polycrystalline TiN thin film. The XPS results indicate that the synthesized film is non-stoichiometric and contains titanium nitride, silicon nitride, and a phase of silicon oxy-nitride. The SEM and AFM results reveal that the surface of the synthesized film is quite smooth with 0.59 nm roughness (root-mean-square).

Structural, morphological and optical studies of F doped SnO2 thin films

NASA Astrophysics Data System (ADS)

Chandel, Tarun; Thakur, Vikas; Dwivedi, Shailendra Kumar; Zaman, M. Burhanuz; Rajaram, Poolla

2018-05-01

Highly conducting and transparent FTO (flourine doped tin Oxide) thin films were grown on the glass substrates using a low cost spray pyrolysis technique. The films were characterized for their structural, morphological and optical studies using XRD, SEM and UV-Vis spectroscopy. XRD studies show that the FTO films crystallize in Tetragonal cassiterite structure. Morphological analysis using SEM show that the films are uniformly covered with spherical grains albeit high in surface roughness. The average optical transmission greater than 80% in the visible region along with the appearance of interference fringes in the transmission curves confirms the high quality of the films. Electrical studies show that the films exhibit sheet resistance below 10 Ω ϒ-1.

A study on optimal pore development of modified commercial activated carbons for electrode materials of supercapacitors

NASA Astrophysics Data System (ADS)

Bang, Joon Hyuk; Lee, Hye-Min; An, Kay-Hyeok; Kim, Byung-Joo

2017-09-01

This study aimed to understand the impact of CO2 activation of commercial activated carbons (AC) on the changes in pore characteristics and the electrochemical property. The surface structure of manufactured AC was observed with a X-ray diffraction (XRD); the pore characteristics were analyzed at N2/77 K isothermal absorption using the Brunauer-Emmett-Teller (BET) and Dubinin-Radushkevich (DR) equations. In addition, the electrochemical characteristics were analyzed by means of an electrolyte of 1 M (C2H5)4NBF4/propylene carbonate, using a charge/discharge test, cyclic voltammetry (CV), and impedance. The N2/77 K isothermal absorption curve of the manufactured AC falls under Type I in the classification of the International Union of Pure and Applied Chemistry (IUPAC) and was found to largely comprise micropores. The specific surface area increased from 1690 m2/g to 2290 m2/g, and the pore volume grew from 0.80 cm3/g to 1.10 cm3/g. The analysis of electrochemical characteristics also found that the specific capacity increased from 17 F/g to 20 F/g (in a full cell condition). Based on these results, we were able to determine the pore characteristics of commercial AC through an additional activation process, which consequently allowed us to manufacture the AC with an advanced electrochemical property.

Physicochemical and adsorptive characteristics of activated carbons from waste polyester textiles utilizing MgO template method.

PubMed

Xu, Zhihua; Zhang, Daofang; Yuan, Zhihang; Chen, Weifang; Zhang, Tianqi; Tian, Danqi; Deng, Haixuan

2017-10-01

Activated carbons with high specific surface areas were produced, utilizing waste polyester textiles as carbon precursor by magnesium oxide (MgO) template method. Magnesium chloride (MgCl 2 ), magnesium citrate (MgCi), and MgO were employed as MgO precursors to prepare activated carbons (AC-MgCl 2 , AC-MgCi, and AC-MgO). Thermogravimetry-differential scanning calorimetry was conducted to investigate the pore-forming mechanism, and N 2 adsorption/desorption isotherms, XRD, SEM-EDS, TEM, FTIR and pH pzc were achieved to analyze physicochemical characteristics of the samples. The specific surface areas of AC-MgCl 2 (1173 m 2 /g) and AC-MgCi (1336 m 2 /g) were much higher than that of AC-MgO (450 m 2 /g), and the pores sizes of which were micro-mesoporous, mesoporous, and macropores, respectively, due to the formation of MgO crystal with different sizes. All activated carbons had abundant acidic oxygen groups. In addition, batch adsorption experiments were carried out to investigate the adsorptive characteristics of the prepared activated carbons toward Cr(VI). The adsorption kinetics fitted well with the pseudo-second order, and the adsorptive capacity of AC-MgCl 2 (42.55 mg/g) was higher than those of AC-MgCi (40.93 mg/g) and AC-MgO (35.87 mg/g).

Synthesis of cobalt ferrite nanoparticles from thermolysis of prospective metal-nitrosonaphthol complexes and their photochemical application in removing methylene blue

NASA Astrophysics Data System (ADS)

Tavana, Jalal; Edrisi, Mohammad

2016-03-01

In this study, cobalt ferrite (CoFe2O4) nanoparticles were synthesized by two novel methods. The first method is based on the thermolysis of metal-NN complexes. In the second method, a template free sonochemical treatment of mixed cobalt and iron chelates of α-nitroso-β-naphthol (NN) was applied. Products prepared through method 1 were spherical, with high specific surface area (54.39 m2 g-1) and small average crystalline size of 13 nm. However, CoFe2O4 nanoparticles prepared by method 2 were in random shapes, a broad range of crystalline sizes and a low specific surface area of 25.46 m2 g-1 though highly pure. A Taguchi experimental design was implemented in method 1 to determine and obtain the optimum catalyst. The structural and morphological properties of products were investigated by x-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Fourier transform infrared, Brunauer-Emmett-Teller and dynamic laser light scattering. The crystalline size calculations were performed using Williamson-Hall method on XRD spectrum. The photocatalytic activity of the optimum nanocrystalline cobalt ferrite was investigated for degradation of a representative pollutant, methylene blue (MB), and visible light as energy source. The results showed that some 92% degradation of MB could be achieved for 7 h of visible light irradiation.

Carbon nanofiber growth optimization for their use as electrocatalyst support in proton exchange membrane (PEM) fuel cells.

PubMed

Lázaro, M J; Sebastián, D; Suelves, I; Moliner, R

2009-07-01

Carbon nanofiber (CNF) growth by catalytic decomposition of methane in a fixed-bed reactor was studied out to elucidate the influence of some important reaction conditions: temperature, space velocity and reactant partial pressure, in the morphological properties of the carbonaceous material obtained. The main objective is to synthesize a suitable carbonaceous nanomaterial to be used as support in platinum based electrocatalysts for Proton Exchange Membrane Fuel Cells (PEMFC) which improves current carbon blacks. High specific surface area is required in an electrocatalyst support since platinum dispersion is enhanced and so a cost-effective usage and high catalytic activity. Good electrical conductivity of carbon support is also required since the fuel cell power density is improved. With this proposal, characterization was carried out by nitrogen physisorption, XRD, SEM and TPO. The results were analysed by a factorial design and analysis of variance (ANOVA) in order to find an empirical correlation between operating conditions and CNF characteristics. It was found that the highest specific surface area and pore volume were found at 823 K and at a space velocity of 10 L gcat(-1) h(-1). The graphitic character of CNF, which is known to influence the electrical conductivity, presented a maximum value at temperatures between 923 K and 973 K. SEM images showed a narrow size distribution of CNF diameter between 40 and 90 nm and homogeneous appearance.

Correlating capacity and Li content in layered material for Li-ion battery using XRD and particle size distribution measurements

NASA Astrophysics Data System (ADS)

Al-Tabbakh, A. A. A.; Al-Zubaidi, A. B.; Kamarulzaman, N.

2016-03-01

A lithiated transition-metal oxide material was successfully synthesized by a combustion method for Li-ion battery. The material was characterized using thermogravimetric and particle size analyzers, scanning electron microscope and X-ray diffractometer. The calcined powders of the material exhibited a finite size distribution and a single phase of pure layered structure of space group Roverline{3} m . An innovative method was developed to calculate the material electrochemical capacity based on considerations of the crystal structure and contributions of Li ions from specified unit cells at the surfaces and in the interiors of the material particles. Results suggested that most of the Li ions contributing to the electrochemical current originated from the surface region of the material particles. It was possible to estimate the thickness of the most delithiated region near the particle surfaces at any delithiation depth accurately. Furthermore, results suggested that the core region of the particles remained electrochemically inaccessible in the conventional applied voltages. This result was justified by direct quantitative comparison of specific capacity values calculated from the particle size distribution with those measured experimentally. The present analysis is believed to be of some value for estimation of the failure mechanism in cathode compounds, thus assisting the development of Li-ion batteries.

Preparation and Characterization of Cu and Ni on Alumina Supports and Their Use in the Synthesis of Low-Temperature Metal-Phthalocyanine Using a Parallel-Plate Reactor.

PubMed

Sánchez-De la Torre, Fernando; De la Rosa, Javier Rivera; Kharisov, Boris I; Lucio-Ortiz, Carlos J

2013-09-30

Ni- and Cu/alumina powders were prepared and characterized by X-ray diffraction (XRD), scanning electronic microscope (SEM), and N₂ physisorption isotherms were also determined. The Ni/Al₂O₃ sample reveled agglomerated (1 μm) of nanoparticles of Ni (30-80 nm) however, NiO particles were also identified, probably for the low temperature during the H 2 reduction treatment (350 °C), the Cu/Al₂O₃ sample presented agglomerates (1-1.5 μm) of nanoparticles (70-150 nm), but only of pure copper. Both surface morphologies were different, but resulted in mesoporous material, with a higher specificity for the Ni sample. The surfaces were used in a new proposal for producing copper and nickel phthalocyanines using a parallel-plate reactor. Phthalonitrile was used and metallic particles were deposited on alumina in ethanol solution with CH₃ONa at low temperatures; ≤60 °C. The mass-transfer was evaluated in reaction testing with a recent three-resistance model. The kinetics were studied with a Langmuir-Hinshelwood model. The activation energy and Thiele modulus revealed a slow surface reaction. The nickel sample was the most active, influenced by the NiO morphology and phthalonitrile adsorption.

Polyimide encapsulated lithium-rich cathode material for high voltage lithium-ion battery.

PubMed

Zhang, Jie; Lu, Qingwen; Fang, Jianhua; Wang, Jiulin; Yang, Jun; NuLi, Yanna

2014-10-22

Lithium-rich materials represented by xLi2MnO3·(1 - x)LiMO2 (M = Mn, Co, Ni) are attractive cathode materials for lithium-ion battery due to their high specific energy and low cost. However, some drawbacks of these materials such as poor cycle and rate capability remain to be addressed before applications. In this study, a thin polyimide (PI) layer is coated on the surface of Li1.2Ni0.13Mn0.54Co0.13O2 (LNMCO) by a polyamic acid (PAA) precursor with subsequently thermal imidization process. X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM) results confirm the successful formation of a PI layer (∼3 nm) on the surface of LNMCO without destruction of its main structure. X-ray photoelectron spectroscopy (XPS) spectra show a slight shift of the Mn valence state from Mn(IV) to Mn(III) in the PI-LNMCO treated at 450 °C, elucidating that charge transfer takes place between the PI layer and LNMCO surface. Electrochemical performances of LNMCO including cyclic stability and rate capability are evidently improved by coating a PI nanolayer, which effectively separates the cathode material from the electrolyte and stabilizes their interface at high voltage.

Hydrothermal synthesis of graphene/nickel oxide nanocomposites used as the electrode for supercapacitors.

PubMed

Zhou, Zhongnian; Ni, Haifang; Fan, Li-Zhen

2014-07-01

Graphene (GR)-based nanocomposites with different mass ratios of NiO and GR are prepared via hydrothermal method using Ni(NO3)2 as the origin of nickel and urea as the hydrolysis-controlling agent. The morphology and electrochemical performance of the GR/NiO nanocomposites are closely associated with the mass ratios of GR to NiO. The chemical composition and morphology of the composites together with the pure GR and NiO are characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM). It is found that the GR sheets and NiO particles form uniform nanocomposites with the NiO particles absorbed on the GR surface. A specific capacitance of 384 F g(-1) at a current density of 0.1 A g(-1) is achieved when the coating amount of NiO is up to 74 wt%. In addition, the attenuation of the specific capacitance is less than 6% after 500 cycles, indicating such nanocomposite has excellent cycling performance.

Design and synthesis of inorganic/organic hybrid electrochemical materials

NASA Astrophysics Data System (ADS)

Harreld, John H.

An ambient pressure method for drying sol-gel materials is developed to synthesize high porosity (80--90%), high surface area vanadium oxide and silica aerogel materials (150--300 and 1000 m2/g for vanadium pentoxide and silica, respectively). The synthesis approach uses liquid exchange to replace the pore fluid with a low surface tension, nonpolar solvent which reduces the capillary pressures developed during drying. The Good-Girifalco interaction parameter is used to calculate pore stresses resulting from drying silica gels from various liquids. Vanadium oxide/polypyrrole hybrid aerogels are prepared using three strategies. These approaches focus on either sequential or consecutive polymerization of the inorganic and organic networks. Microcomposite aerogels are synthesized by encapsulating a dispersion of preformed polypyrrole in a vanadium pentoxide gel. In the second approach, pyrrole is polymerized and doped within the pore volume of preformed vanadium pentoxide gel. When the inorganic and organic precursors are polymerized simultaneously, the resulting gels exhibited a nanometer scaled microstructure with homogeneous distributions of either phases. Through this route, a suitable microstructure and composition for a lithium secondary battery cathode is obtained. Lithiated aerogels of hydrated nickel, cobalt, and mixed nickel-cobalt oxides are synthesized from lithium hydroxide and transition metal acetate precursors. The XRD analyses indicate that the nickel containing gels exhibit a lithium deficiency (less than 1 Li/transition metal. By increasing the concentration of the lithium precursor the lithium content in nickel oxides is increased, and additional base solution is no longer required to catalyze gelation. A non-hydrolytic sol-gel approach is utilized to create tin oxide and tin-aluminum binary oxide aerogels with high porosity (90%) and high surface area (300 m2/g). XRD data from single phase tin oxide aerogel indicates the growth of SnO2 crystallites between 150--400°C in air, accompanied by a reduction in surface area (30 m2/g). Heated tin oxide aerogel exhibits comparable reversible specific capacity (390 mAh/g) as that of commercial SnO2 (420 mAh/g). Amorphous tin oxide aerogel is stabilized to higher temperatures when aluminum oxide is incorporated into the structure. The tin oxide phase remains electrochemically active towards lithium insertion and exhibits excellent reversibility during cycling.

Performance of magnetic zirconium-iron oxide nanoparticle in the removal of phosphate from aqueous solution

NASA Astrophysics Data System (ADS)

Zhang, Chang; Li, Yongqiu; Wang, Fenghua; Yu, Zhigang; Wei, Jingjing; Yang, Zhongzhu; Ma, Chi; Li, Zihao; Xu, ZiYi; Zeng, Guangming

2017-02-01

In this study, magnetic zirconium-iron oxide nanoparticles (MZION) of different Fe/Zr molar ratios were successfully prepared using the co-precipitation method, and their performance for phosphate removal was systematically evaluated. The as-obtained adsorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential analyzer, Fourier transform infrared spectroscopy (FT-IR) and Brunauer Emmett Teller (BET) specific surface area analysis. The effects of pH, ionic strength, and co-existing ions (including Cl-, SO42-, NO3- and HCO3-) were measured to evaluate the adsorption performance in batch experiments. The results showed that decreasing the Fe/Zr molar ratios increased the specific surface area that was propitious to adsorption process, but the adsorption capacity enhanced with the decrease of Fe/Zr molar ratios. Phosphate adsorption on MZION could be well described by the Freundlich equilibrium model and pseudo-second-order kinetics. The adsorption of phosphate was highly pH dependent and decreased with increasing pH from 1.5 to 10.0. The adsorption was slightly affected by ionic strength. With the exception of HCO3-, co-existing anions showed minimum or no effect on their adsorption performance. After adsorption, phosphate on these MZION could be easily desorbed by 0.1 M NaOH solution. The phosphate adsorption mechanism of MZION followed the inner-sphere complexing mechanism, and the surface sbnd OH groups played a significant role in the phosphate adsorption. Additionally, the main advantages of MZION consisted in its separation convenience and highly adsorption capacity compared to other adsorbents.

Characterization of a Ultra-high Temperature Ceramic Composite

NASA Technical Reports Server (NTRS)

Levine, Stanley R.; Opila, Elizabeth J.; Robinson, Raymond C.; Lorincz, Jonathan A.

2003-01-01

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Structural and electrochemical analysis of chemically synthesized microcubic architectured lead selenide thin films

NASA Astrophysics Data System (ADS)

Bhat, T. S.; Shinde, A. V.; Devan, R. S.; Teli, A. M.; Ma, Y. R.; Kim, J. H.; Patil, P. S.

2018-01-01

The present work deals with the synthesis of lead selenide (PbSe) thin films by simple and cost-effective chemical bath deposition method with variation in deposition time. The structural, morphological, and electrochemical properties of as-deposited thin films were examined using characterization techniques such as X-ray diffraction spectroscopy (XRD), field-emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy. XRD reveals formation of rock salt phase cubic structured PbSe. FE-SEM images show the formation of microcubic structured morphology. The existence of the PbSe is confirmed from the XPS analysis. On the other hand, CV curves show four reaction peaks corresponding to oxidation [PbSe and Pb(OH)2] and reduction (PbO2 and Pb(OH)2) at the surface of PbSe thin films. The PbSe:2 sample deposited for 80 min. shows maximum specific capacitance of 454 ± 5 F g- 1 obtained at 0.25 mA cm- 2 current density. The maximum energy density of 69 Wh kg- 1 was showed by PbSe:2 electrode with a power density of 1077 W kg- 1. Furthermore, electrochemical impedance studies of PbSe:2 thin film show 80 ± 3% cycling stability even after 500 CV cycles. Such results show the importance of microcubic structured PbSe thin film as an anode in supercapacitor devices.

Projection of the Liquidus Surface of the Co - Sn - Bi System

NASA Astrophysics Data System (ADS)

Abilov, Ch. I.; Allazov, M. R.; Sadygova, S. G.

2016-11-01

The crystallization behavior of phases in alloys of the Co - Sn - Bi system is studied by the methods of differential thermal (DTA), x-ray phase (XRP) and x-ray diffraction (XRD) analyses and hardness measurement. The projection of the liquidus surface is plotted. The boundaries of layering, the development of the monovariant processes, and the coordinates of the nonvariant equilibrium compositions are determined. Compositions of (Co3Sn2)1 - x Bi x solid solutions suitable for the production of antifriction materials are suggested.

A facile production of microporous carbon spheres and their electrochemical performance in EDLC

NASA Astrophysics Data System (ADS)

Xia, Xiaohong; Shi, Lei; Liu, Hongbo; Yang, Li; He, Yuede

2012-03-01

In the absence of activation process, we prepared a series of carbon particles from saccharine, in which hydrothermal carbonization method was used. These particles have spherical or near-spherical morphology, controllable monodisperse particle size from the analyses of SEM. Raman and XRD results show that they are nongraphitizable. The BET surface area of these carbon spherules is around 400-500 m2 g-1 and the microporosity is about 84%, suggesting that the carbon particles are rich in micropores. The electrochemical behaviors were characterized by means of galvanostatic charging/discharging, cycle voltammetry and impedance spectroscopy. The results show that the specific capacitance of sucrose-based carbon spherule reached 164 F g-1 in 30% KOH electrolyte and a high volumetric capacitance over 170 F cm-3 was obtained. These carbon spherules could be promising materials for EDLC according to their facile preparation way, low cost and high packing density.

Hydrogen storage behaviors of Ni-doped graphene Oxide/MIL-101 hybrid composites.

PubMed

Lee, Seul-Yi; Park, Soo-Jin

2013-01-01

In this work, Ni-doped graphene oxide/MIL-101 hybrid composites (Ni--GO/MIL) were prepared to investigate their hydrogen storage behaviors. Ni--GO/MIL was synthesized by adding Ni--GO in situ during the synthesis of MIL-101 using a hydrothermal process, which was conducted by conventional convection heating with Cr(III) ion as a metal center and telephthalic acid as organic ligands. The crystalline structures and morphologies were measured by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The specific surface area and micropore volume were investigated by N2/77 K adsorption isotherms using the Brunauer-Emmett-Teller (BET) method and Dubinin-Radushkevic (D-R) equation, respectively. The hydrogen storage capacity was investigated by BEL-HP at 77 K and 1 bar. The obtained results show that Ni--GO/MIL presents new directions for achieving novel hybrid materials with higher hydrogen storage capacity.

Uniform Fe3O4 microflowers hierarchical structures assembled with porous nanoplates as superior anode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Wang, Xiaoliang; Liu, Yanguo; Arandiyan, Hamidreza; Yang, Hongping; Bai, Lu; Mujtaba, Jawayria; Wang, Qingguo; Liu, Shanghe; Sun, Hongyu

2016-12-01

Uniform Fe3O4 microflowers assembled with porous nanoplates were successfully synthesized by a solvothermal method and subsequent annealing process. The structural and compositional analysis of the Fe3O4 microflowers were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The Bruauer-Emmett-Teller (BET) specific surface area was calculated by the nitrogen isotherm curve and pore size distribution of Fe3O4 microflowers was determined by the Barret-Joyner-Halenda (BJH) method. When evaluated as anode material for lithium-ion batteries, the as-prepared Fe3O4 microflowers electrodes delivered superior capacity, better cycling stability and rate capability than that of Fe3O4 microspheres electrodes. The improved electrochemical performance was attributed to the microscale flowerlike architecture and the porous sheet structural nature.

P-type sub-tungsten-oxide based urchin-like nanostructure for superior room temperature alcohol sensor

NASA Astrophysics Data System (ADS)

Yao, Yao; Yin, Mingli; Yan, Junqing; Liu, Shengzhong (Frank)

2018-05-01

Nanowires assembled sub-WO3 urchin-like nanostructures have been fabricated via a solvothermal method. The detailed structure and morphology features were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The results reveal that the individual nanowires are grown along the [0 0 1] direction, and assembled together to form an urchin-like nanostructure. Sensing performance of the sub-WO3 was investigated toward alcohol vapor. At room temperature, the sensor devices based on the WO3-x exhibit significantly higher sensitivity comparing to that of the stoichiometric WO3. The superior sensing performance of this WO3-x sensor is ascribed to the large specific surface area and abundant oxygen vacancies. The obvious enhancement of the gas sensing property can be very useful for the future design and development of room temperature gas sensors for other volatile organic compounds.

Electrochemical capacitance of nanostructured ruthenium-doped tin oxide Sn1- x Ru x O2 by the microemulsion method

NASA Astrophysics Data System (ADS)

Saraswathy, Ramanathan

2017-12-01

Synthesis of nanostructured Ru-doped SnO2 was successfully carried out using the reverse microemulsion method. The phase purity and the crystallite size were analyzed by XRD. The surface morphology and the microstructure of synthesized nanoparticles were analyzed by SEM and TEM. The vibration mode of nanoparticles was investigated using FTIR and Raman studies. The electrochemical behavior of the Ru-doped SnO2 electrode was evaluated in a 0.1 mol/L Na2SO4 solution using cyclic voltammetry. The 5% Ru-doped SnO2 electrode exhibited a high specific capacitance of 535.6 F/g at a scan rate 20 mV/s, possessing good conductivity as well as the electrocycling stability. The Ru-doped SnO2 composite shows excellent electrochemical properties, suggesting that this composite is a promising material for supercapacitors.

Nanoscale Structure and Interaction of Compact Assemblies of Carbon Nano-Materials

NASA Astrophysics Data System (ADS)

Timsina, Raju; Qiu, Xiangyun

Carbon-based nano-materials (CNM) are a diverse family of multi-functional materials under research and development world wide. Our work is further motivated by the predictive power of the physical understanding of the underlying structure-interaction-function relationships. Here we present results form recent studies of the condensed phases of several model CNMs in complexation with biologically derived molecules. Specifically, we employ X-ray diffraction (XRD) to determine nanoscale structures and use the osmotic stress method to quantify their interactions. The systems under investigation are dsDNA-dispersed carbon nanotubes (dsDNA-CNT), bile-salt-dispersed carbon nanotubes, and surfactant-assisted assemblies of graphene oxides. We found that salt and molecular crowding are both effective in condensing CNMs but the resultant structures show disparate phase behaviors. The molecular interactions driving the condensation/assembly sensitively depend on the nature of CNM complex surface chemistry and range from hydrophobic to electrostatic to entropic forces.

Fabrication of aligned porous LaNi0.6Fe0.4O3 perovskite by water based freeze casting

NASA Astrophysics Data System (ADS)

Soltani, Niloofar; Martínez-Bautista, Rubén; Bahrami, Amin; Huerta Arcos, Lázaro; Cassir, Michel; Chávez Carvayar, José

2018-05-01

A novel porous cathode of LaNi0.6Fe0.4O3 perovskite with aligned porosities was engineered for solid oxide fuel cells. LaNi0.6Fe0.4O3 was produced through metal nitrate and acid citric combustion method and calcined at different temperatures. The synthesized LNF at 600 °C shows specific surface area (SBET) of 24.4 m2 g-1 and an average pore size of 12.2 nm. The chemical composition and structure of LaNi0.6Fe0.4O3 synthesized at temperature 600-1400 °C, were analyzed by XRD, XPS and HRTEM. SEM observations of freeze cast nano-sized LNF showed the vertically aligned hexagonal walls. These walls contain a great value of fine pores which accelerate the gas transportation.

Monolithic porous graphitic carbons obtained through catalytic graphitization of carbon xerogels

NASA Astrophysics Data System (ADS)

Kiciński, Wojciech; Norek, Małgorzata; Bystrzejewski, Michał

2013-01-01

Pyrolysis of organic xerogels accompanied by catalytic graphitization and followed by selective-combustion purification was used to produce porous graphitic carbons. Organic gels impregnated with iron(III) chloride or nickel(II) acetate were obtained through polymerization of resorcinol and furfural. During the pyrolysis stage graphitization of the gel matrix occurs, which in turn develops mesoporosity of the obtained carbons. The evolution of the carbon into graphitic structures is strongly dependent on the concentrations of the transition metal. Pyrolysis leads to monoliths of carbon xerogel characterized by substantially enhanced mesoporosity resulting in specific surface areas up to 400 m2/g. Removal of the amorphous carbon by selective-combustion purification reduces the xerogels' mesoporosity, occasionally causing loss of their mechanical strength. The graphitized carbon xerogels were investigated by means of SEM, XRD, Raman scattering, TG-DTA and N2 physisorption. Through this procedure well graphitized carbonaceous materials can be obtained as bulk pieces.

Removal of fluoride from drinking water by cellulose@hydroxyapatite nanocomposites.

PubMed

Yu, Xiaolin; Tong, Shengrui; Ge, Maofa; Zuo, Junchao

2013-01-30

Cellulose@hydroxyapatite (HA) nanocomposites were prepared in NaOH/thiourea/urea/H(2)O solution via situ hybridization. The composite materials combine the advantage of cellulose and HA with the high specific surface area and the strong affinity toward fluoride. The composite materials were characterized by FTIR, SEM, XRD, TG and XPS, and the adsorption of fluoride was investigated. Adsorption kinetics indicated the adsorption equilibrium of fluoride was within 360 min and the adsorption process was well described by the pseudo-second-order kinetic model. The Langmuir and Freundlich isotherm models could fit the experimental data well. At the initial fluoride concentration of 10mg/L, the residual concentration using above 3g/L adsorbent dose could meet the drinking water standard of WHO norms. Furthermore, the coexisting anions had no significant effect on fluoride adsorption. Copyright © 2012 Elsevier Ltd. All rights reserved.

Optimization of chemical displacement deposition of copper on porous silicon.

PubMed

Bandarenka, Hanna; Redko, Sergey; Nenzi, Paolo; Balucani, Marco; Bondarenko, Vitaly

2012-11-01

Copper (II) sulfate was used as a source of copper to achieve uniform distribution of Cu particles deposited on porous silicon. Layers of the porous silicon were formed by electrochemical anodization of Si wafers in a mixture of HF, C3H7OH and deionized water. The well-known chemical displacement technique was modified to grow the copper particles of specific sizes. SEM and XRD analysis revealed that the outer surface of the porous silicon was covered with copper particles of the crystal orientation inherited from the planes of porous silicon skeleton. The copper crystals were found to have the cubic face centering elementary cell. In addition, the traces of Cu2O cubic primitive crystalline phases were identified. The dimensions of Cu particles were determined by the Feret's analysis of the SEM images. The sizes of the particles varied widely from a few to hundreds of nanometers. A phenomenological model of copper deposition was proposed.

Fe2O3 hollow sphere nanocomposites for supercapacitor applications

NASA Astrophysics Data System (ADS)

Zhao, Yu; Wen, Yang; Xu, Bing; Lu, Lu; Ren, Reiming

2018-02-01

Nanomaterials have attracted increasing interest in electrochemical energy storage and conversion. Hollow sphere Fe2O3 nanocomposites were successfully prepared through facile low temperature water-bath method with carbon sphere as hard template. The morphology and microstructure of samples were characterized by X-ray diffraction (XRD) and Scanning electron microscope (SEM), respectively. Through hydrolysis mechanism, using ferric chloride direct hydrolysis, iron hydroxide coated on the surface of carbon sphere, after high temperature calcination can form the hollow spherical iron oxide materials. Electrochemical performances of the hollow sphere Fe2O3 nanocomposites electrodes were investigated by cyclic voltammery (CV) and galvanostatic charge/discharge. The Pure hollow sphere Fe2O3 nanocomposites achieves a specific capacitance of 125 F g-1 at the current density of 85 mA g-1. The results indicate that the uniform dispersion of hollow ball structure can effectively reduce the particle reunion in the process of charging and discharging.

The Adsorption Capacity of GONs/CMC/Fe₃O₄ Magnetic Composite Microspheres and Applications for Purifying Dye Wastewater.

PubMed

Lv, Shenghua; Zhu, Linlin; Li, Ying; Jia, Chunmao; Sun, Shiyu

2017-01-11

Graphene oxide nanosheets (GONs)/carboxymethyl chitosan (CMC)/Fe₃O₄ magnetic composite microspheres (MCMs) were prepared by enclosing Fe₃O₄ particles with CMC and GONs in turn. The microstructures of GONs and GONs/CMC/Fe₃O₄ MCMs were characterized by FTIR, XRD, TEM, and SEM. The effects of GON content, pH value, and adsorption time on the adsorption capacity of the MCMs were investigated. The results show that the GONs/CMC/Fe₃O₄ MCMs have a greater specific surface area and a strong adsorption capacity for dye wastewater. Meanwhile, the adsorption mechanism was investigated, and the results accorded with the pseudo-second-order kinetic model and the Freundlich isotherm model. The search results indicate that GONs/CMC/Fe₃O₄ MCMs can be used to purify dye wastewater and has an important potential use in the practical purification of dye wastewater.

Effect of heat treatment on CO2 adsorption of KOH-activated graphite nanofibers.

PubMed

Meng, Long-Yue; Park, Soo-Jin

2010-12-15

In this work, graphite nanofibers (GNFs) were successfully expanded intercalating KOH followed by heat treatment in the temperature range of 700-1000 °C. The aim was to improve the CO(2) adsorption capacity of the GNFs by increasing the porosity of GNFs. The effects of heat treatment on the pore structures of GNFs were investigated by N(2) full isotherms, XRD, SEM, and TEM. The CO(2) adsorption capacity was measured by CO(2) isothermal adsorption at 25 °C and 1 atm. From the results, it was found that the activation temperature had a major influence on CO(2) adsorption capacity and textural properties of GNFs. The specific surface area, total pore volume, and mesopore volume of the GNFs increased after heat treatment. The CO(2) adsorption isotherms showed that G-900 exhibited the best CO(2) adsorption capacity with 59.2 mg/g. Copyright © 2010 Elsevier Inc. All rights reserved.

[Photocatalysis characterization of titanium dioxide supported on natural clinoplilolite].

PubMed

Fang, Songsheng; Jiang, Yinshan; Wang, Yujie; Bao, Changli; Song, Bo

2003-07-01

This paper studied preparing photocatalyst supported on natural clinoplilolite, photocatalysis degrading to methyl orange solution as photocatalysis function test, solar as light resource, explored the synthesize condition and affect factors of its catalysis activity. The capability of catalyst was evaluated by decolor rate and COD removal rate. The samples was described by XRD, IR and specific surface area. Studied result showed that catalyst prepared by combination of tetrabutyl titanate and natural clinoplilolite dryed under 120 degrees C for 6 hours then calcined under 200 degrees C had the best photocatalysis activity. Degrading rate of methyl orange solution increased with the quantity of TiO2/zeolite and additional oxidant H2O2 increasing, but superfluous H2O2 can also restrain the photocatalysis activity of titanium dioxide supported on clinoplilolite. Methyl orange solution had the best degrading rate as pH value between 2 to 5.

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

Wang, Yong; State Key Laboratory of Multiphase Complex System, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100080; Zhu, Qingshan, E-mail: qszhu@home.ipe.ac.cn

{beta}-Ni(OH){sub 2} hierarchical micro-flowers, hierarchical hollow microspheres and nanosheets were synthesized via a facile, single-step and selected-control hydrothermal method. Both hierarchical micro-flowers and hierarchical hollow microspheres were built from two-dimensional nanosheets with thickness of 50-100 nm. The as-obtained products were characterized by Brunauer-Emmett-Teller (BET) surface area analysis, X-ray powder diffraction (XRD) and field emission scanning electron microscopy (FESEM). It was observed that marked morphological changes in {beta}-Ni(OH){sub 2} depended on the initial concentrations of Ni{sup 2+} ions and glycine. A possible growth mechanism was proposed based on experimental results. In addition, the effect of morphology on the electrochemical properties wasmore » also investigated. Both hierarchical micro-flowers and hierarchical hollow microspheres exhibited enhanced specific capacity and high-rate discharge ability as compared with pure Ni(OH){sub 2} nanosheets. Investigations confirmed that hierarchical structures had a pronounced influence upon the electrochemical performance of nickel hydroxide.« less

Comparative analysis of the effect of low-dimensional alumina structures on cell lines L929 and Neuro-2a

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

Fomenko, A. N., E-mail: alserova@ispms.tsc.ru; Korovin, M. S., E-mail: msk@ispms.tsc.ru

The paper presents the toxicity evaluation of nanostructures on the basis of alumina of different shape (nanofibers, nanoplates, nanosheets, nanosheet agglomerates) and with similar physical and chemical properties (particle size, specific surface area, phase composition, and zeta potential). The nanostructures were examined by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), low-temperature nitrogen adsorption, and dynamic light scattering (DLS). The cytotoxicity of nanostructures was estimated using L929 fibroblast cells and Neuro-2a tumor cells. It has been found that the L929 cells are less subject to the influence of alumina nanoparticles than the Neuro-2a tumor cells. Probably, themore » differences in the proliferation activity of normal and tumor cells in contact with the synthesized nanostructures are due to a change in the pH of the cell microenvironment.« less

Comparative analysis of the effect of low-dimensional alumina structures on cell lines L929 and Neuro-2a

NASA Astrophysics Data System (ADS)

Fomenko, A. N.; Korovin, M. S.

2016-08-01

The paper presents the toxicity evaluation of nanostructures on the basis of alumina of different shape (nanofibers, nanoplates, nanosheets, nanosheet agglomerates) and with similar physical and chemical properties (particle size, specific surface area, phase composition, and zeta potential). The nanostructures were examined by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), low-temperature nitrogen adsorption, and dynamic light scattering (DLS). The cytotoxicity of nanostructures was estimated using L929 fibroblast cells and Neuro-2a tumor cells. It has been found that the L929 cells are less subject to the influence of alumina nanoparticles than the Neuro-2a tumor cells. Probably, the differences in the proliferation activity of normal and tumor cells in contact with the synthesized nanostructures are due to a change in the pH of the cell microenvironment.

Characterization of organo-modified bentonite sorbents: The effect of modification conditions on adsorption performance

NASA Astrophysics Data System (ADS)

Parolo, María E.; Pettinari, Gisela R.; Musso, Telma B.; Sánchez-Izquierdo, María P.; Fernández, Laura G.

2014-11-01

The organic modification of a natural bentonite was evaluated using two methods: exchanging the interlayer cations by hexadecyltrimethylammonium (HDTMA) and grafting with vinyltrimethoxysilane (VTMS) and γ-methacryloyloxy propyl trimethoxysilane (TMSPMA) on montmorillonite surface. The physicochemical characterization of all materials was made by X-ray diffraction (XRD), IR spectroscopy, thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) surface area techniques. HDTMA cations and organosilanes were intercalated into the interlayer space of montmorillonite, as deduced from the increase of the basal spacing. IR spectroscopy, TGA and BET area give evidence of successful organic modification. The studies show a decrease in the IR absorption band intensity at 3465 cm-1 with surfactant modification, and also a decrease of mass loss due to adsorbed water observed in two samples: the organoclay and functionalized bentonites, which are evidences of a lower interlayer hydrophilicity. The efficiency of aniline removal onto natural bentonite, organobentonite and functionalized bentonites from aqueous solutions was evaluated. Aniline sorption on natural bentonite was studied using batch experiments, XRD and IR spectroscopy. The hydrophobic surface of organobentonite and functionalized bentonites increased the retention capacity for nonionic organic substances such as aniline on bentonites. The sorption properties of modified bentonite, through different modification methods, enhanced the potential industrial applications of bentonites in water decontamination.

Biocompatibility and Surface Properties of TiO2 Thin Films Deposited by DC Magnetron Sputtering

PubMed Central

López-Huerta, Francisco; Cervantes, Blanca; González, Octavio; Hernández-Torres, Julián; García-González, Leandro; Vega, Rosario; Herrera-May, Agustín L.; Soto, Enrique

2014-01-01

We present the study of the biocompatibility and surface properties of titanium dioxide (TiO2) thin films deposited by direct current magnetron sputtering. These films are deposited on a quartz substrate at room temperature and annealed with different temperatures (100, 300, 500, 800 and 1100 °C). The biocompatibility of the TiO2 thin films is analyzed using primary cultures of dorsal root ganglion (DRG) of Wistar rats, whose neurons are incubated on the TiO2 thin films and on a control substrate during 18 to 24 h. These neurons are activated by electrical stimuli and its ionic currents and action potential activity recorded. Through X-ray diffraction (XRD), the surface of TiO2 thin films showed a good quality, homogeneity and roughness. The XRD results showed the anatase to rutile phase transition in TiO2 thin films at temperatures between 500 and 1100 °C. This phase had a grain size from 15 to 38 nm, which allowed a suitable structural and crystal phase stability of the TiO2 thin films for low and high temperature. The biocompatibility experiments of these films indicated that they were appropriated for culture of living neurons which displayed normal electrical behavior. PMID:28788667

The synthesis of Ba2+ doped multiferroic BiFeO3 nanoparticles by using a hydrothermal approach in the presence of different surface activators and the investigation of structural and magnetic features

NASA Astrophysics Data System (ADS)

Mardani, Reza

2017-05-01

In this work, Bi1-x Ba x FeO3 nanoparticles were synthesized by a hydrothermal method in the presence of various surface activators, and different amounts of barium were inserted in a bismuth ferrite (x  =  0.1, 0.15, 0.2) structure instead of bismuth. The structural and magnetic properties, morphology, and size of the synthesized nanoparticles were investigated by XRD, FT-IR, FE-SEM, TEM, DLS and VSM. The XRD analysis results reveal that the synthetic nanoparticles have a single phase. A phase shift from a rhombohedral structure to a tetragonal structure occurs due to the enhanced barium amount in the bismuth ferrite structure. The SEM analysis exhibits a uniform shape of the Bi0.85Ba0.15FeO3 particles and the image observed by TEM clarifies the size of the particles as 11 nm. Furthermore, the effect of the diverse surfaces of activators in the synthesis of Bi0.85Ba0.15FeO3 nanoparticles was studied, revealing that when sugar was used as a surfactant, the particle size reduced and the magnetic properties increased notably.

Chemical bath deposited and dip coating deposited CuS thin films - Structure, Raman spectroscopy and surface study

NASA Astrophysics Data System (ADS)

Tailor, Jiten P.; Khimani, Ankurkumar J.; Chaki, Sunil H.

2018-05-01

The crystal structure, Raman spectroscopy and surface microtopography study on as-deposited CuS thin films were carried out. Thin films deposited by two techniques of solution growth were studied. The thin films used in the present study were deposited by chemical bath deposition (CBD) and dip coating deposition techniques. The X-ray diffraction (XRD) analysis of both the as-deposited thin films showed that both the films possess covellite phase of CuS and hexagonal unit cell structure. The determined lattice parameters of both the films are in agreement with the standard JCPDS as well as reported data. The crystallite size determined by Scherrer's equation and Hall-Williamsons relation using XRD data for both the as-deposited thin films showed that the respective values were in agreement with each other. The ambient Raman spectroscopy of both the as-deposited thin films showed major emission peaks at 474 cm-1 and a minor emmision peaks at 265 cm-1. The observed Raman peaks matched with the covellite phase of CuS. The atomic force microscopy of both the as-deposited thin films surfaces showed dip coating thin film to be less rough compared to CBD deposited thin film. All the obtained results are presented and deliberated in details.

Activated carbon coated palygorskite as adsorbent by activation and its adsorption for methylene blue.

PubMed

Zhang, Xianlong; Cheng, Liping; Wu, Xueping; Tang, Yingzhao; Wu, Yucheng

2015-07-01

An activation process for developing the surface and porous structure of palygorskite/carbon (PG/C) nanocomposite using ZnCl2 as activating agent was investigated. The obtained activated PG/C was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy (SEM), and Brunauer-Emmett-Teller analysis (BET) techniques. The effects of activation conditions were examined, including activation temperature and impregnation ratio. With increased temperature and impregnation ratio, the collapse of the palygorskite crystal structure was found to accelerate and the carbon coated on the surface underwent further carbonization. XRD and SEM data confirmed that the palygorskite structure was destroyed and the carbon structure was developed during activation. The presence of the characteristic absorption peaks of CC and C-H vibrations in the FTIR spectra suggested the occurrence of aromatization. The BET surface area improved by more than 11-fold (1201 m2/g for activated PG/C vs. 106 m2/g for PG/C) after activation, and the material appeared to be mainly microporous. The maximum adsorption capacity of methylene blue onto the activated PG/C reached 351 mg/g. The activated PG/C demonstrated better compressive strength than activated carbon without palygorskite clay. Copyright © 2015. Published by Elsevier B.V.

The effects of fuel type in synthesis of NiFe2O4 nanoparticles by microwave assisted combustion method

NASA Astrophysics Data System (ADS)

Karcıoğlu Karakaş, Zeynep; Boncukçuoğlu, Recep; Karakaş, İbrahim H.

2016-04-01

In this study, it was investigated the effects of the used fuels on structural, morphological and magnetic properties of nanoparticles in nanoparticle synthesis with microwave assisted combustion method with an important method in quick, simple and low cost at synthesis of the nanoparticles. In this aim, glycine, urea and citric acid were used as fuel, respectively. The synthesised nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmet-Teller surface area (BET), and vibrating sample magnetometry (VSM) techniques. We observed that fuel type is quite effective on magnetic properties and surface properties of the nanoparticles. X-ray difractograms of the obtained nanoparticles were compared with standard powder diffraction cards of NiFe2O4 (JCPDS Card Number 54-0964). The results demonstrated that difractograms are fully compatible with standard reflection peaks. According to the results of the XRD analysis, the highest crystallinity was observed at nanoparticles synthesized with glycine. The results demonstrated that the nanoparticles prepared with urea has the highest surface area. The micrographs of SEM showed that all of the nanoparticles have nano-crystalline behaviour and particles indication cubic shape. VSM analysis demonstrated that the type of fuel used for synthesis is highly effective a parameter on magnetic properties of nanoparticles.

Bi2O3 nanoparticles encapsulated in surface mounted metal-organic framework thin films

NASA Astrophysics Data System (ADS)

Guo, Wei; Chen, Zhi; Yang, Chengwu; Neumann, Tobias; Kübel, Christian; Wenzel, Wolfgang; Welle, Alexander; Pfleging, Wilhelm; Shekhah, Osama; Wöll, Christof; Redel, Engelbert

2016-03-01

We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye.We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr00532b

Platinum nanocatalysts prepared with different surfactants for C1-C3 alcohol oxidations and their surface morphologies by AFM

NASA Astrophysics Data System (ADS)

Ertan, Salih; Şen, Fatih; Şen, Selda; Gökağaç, Gülsün

2012-06-01

In this study, platinum nanoparticle catalysts have been prepared using PtCl4 as a starting material and 1-octanethiol, 1-decanethiol, 1-dodecanethiol, and 1-hexadecanethiol as surfactants for methanol, ethanol, and 2-propanol oxidation reactions. The structure, particle sizes, and surface morphologies of the catalysts were characterized by X-ray diffraction (XRD), atomic force microscopy and transmission electron microscopy (TEM). XRD and TEM results indicate that all prepared catalysts have a face-centered cubic structure and are homogeneously dispersed on the carbon support with a narrow size distribution (2.0-1.3 nm). X-ray photoelectron spectra of the catalysts were examined and it is found that platinum has two different oxidation states, Pt (0) and Pt(IV), oxygen and sulfur compounds are H2Oads and OHads, bound and unbound thiols. The electrochemical and electrocatalytic properties of these catalysts were investigated with respect to C1-C3 alcohol oxidations by cyclic voltammetry and chronoamperometry. The highest electrocatalytic activity was obtained from catalyst I which was prepared with 1-octanethiol. This may be attributed to a decrease in the ratio of bound to unbound thiol species increase in Pt (0)/Pt(IV), H2Oads/OHads ratios, electrochemical surface area, CO tolerance and percent platinum utility.

OXIDATION OF METHANOL USING OZONE ON TITANIA-SUPPORTED VANADIUM CATALYST

EPA Science Inventory

Catalytic ozone decomposition of methanol has been conducted at mild temperatures of 100 to 250°C using V2O5/TiO2 catalyst prepared by either sol-gel or wet impregnation methods. The catalysts were characterized using XRD, surface area measurements, and desorption of CH3OH. Gas p...

Kinetics and thermodynamics studies on the BMP-2 adsorption onto hydroxyapatite surface with different multi-morphological features.

PubMed

Lu, Zhiwei; Huangfu, Changxin; Wang, Yanying; Ge, Hongwei; Yao, Yao; Zou, Ping; Wang, Guangtu; He, Hua; Rao, Hanbing

2015-01-01

The effect of the surface topography on protein adsorption process is of great significance for designing hydroxyapatite (HA) ceramic material surfaces. In this work, three different topographies of HA materials HA-sheet, HA-rod, and HA-whisker were synthesized and testified by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Brunauer-Emmett-Teller (BET) and a field emission scanning electron microscopy (FE-SEM). We have systematically investigated the adsorption kinetics and thermodynamics of bone morphogenetic proteins (BMP-2) on the three different topography surfaces of HA, respectively. The results showed that the maximum adsorption capacities of HA-sheet, HA-rod and HA-whisker were (219.96 ± 10.18), (247.13 ± 12.35), and (354.67 ± 17.73) μg · g(-1), respectively. Kinetic parameters, rate constants, equilibrium adsorption capacities and related correlation coefficients, for each kinetic model were calculated as well as discussed. It demonstrated that the adsorption of BMP-2 onto HA could be described by the pseudo second-order equation. Adsorption of BMP-2 onto HA followed the Langmuir isotherm. It confirmed that compared with other samples HA-whisker had more adsorption sites for its high specific surface area which could provide more opportunities for protein molecules. The adsorption processes were endothermic (ΔH > 0), spontaneous (ΔG < 0) and entropy increasing (ΔS > 0). A possible adsorption mechanism has been proposed. In addition, the BMP-2 could be adsorbed to the surface which existed slight conformational changes by FT-IR. Copyright © 2015 Elsevier B.V. All rights reserved.

2011 Final Report - Nano-Oxide Photocatalysis for Solar Energy Conversion

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

Eckstein, James N.; Suslick, Kenneth S.

2011-10-19

We have very recently discovered a new hydrogen-producing photocatalyst is BiNbO4. BiNbO4 powders prepared by solid state reaction were tested for photocatalytic activity in methanol solutions under UV irradiation. When the material is tested without the presence of a Pt co-catalyst, photocatalytic activity for H2 evolution is superior to that of TiO2. It was also found that BiNbO4 photodegrades into metallic Bi and reduced Nb oxides after use; materials were characterized by SEM, XRD, and XPS. Adding Pt to the surface of the photocatalyst increases photocatalytic activity and importantly, helps to prevent photodegradation of the oxide material. With 1 wt.more » % Pt loading, photodegradation is essentially absent. BiNbO4 photodegrades into metallic Bi and reduced Nb oxides after use; materials were characterized by SEM, XRD, and XPS. Adding Pt to the surface of the photocatalyst increases photocatalytic activity and importantly, helps to prevent photodegradation of the oxide material. With 1 wt. % Pt loading, photodegradation is essentially absent.« less

The crystallization behavior of amorphous Ge2Sb2Te5 films induced by a multi-pulsed nanosecond laser

NASA Astrophysics Data System (ADS)

Fan, T.; Liu, F. R.; Li, W. Q.; Guo, J. C.; Wang, Y. H.; Sun, N. X.; Liu, F.

2017-09-01

In this paper, accumulated crystallization of amorphous Ge2Sb2Te5 (a-GST) films induced by a multi-pulsed nanosecond (ns) excimer laser was investigated by x-ray diffraction (XRD), atomic force microscopy, field-emission scanning electron microscopy, x-ray photoelectron spectroscopy (XPS) and a spectrophotometer. XRD analyses revealed that detectable crystallization was firstly observed in the preferred orientation (200), followed by the orientations (220) and (111) after two pulses. Optical contrast, determined by crystallinity as well as surface roughness, was found to retain a linear relation within the first three pulses. A layered growth mechanism from the top surface to the interior of a-GST films was used to explain the crystallization behavior induced by the multi-pulse ns laser. XPS analyses for bond rearrangement and electronic structure further suggested that the crystallization process was performed by generating new bonds of Ge-Te and Sb-Te after laser irradiations. This paper presents the potential of multi-level devices and tunable thermal emitters based on controllable crystallization of phase-change materials.

In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

NASA Astrophysics Data System (ADS)

Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

2018-01-01

The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

Measurement and characterization of external oil in the fried waxy maize starch granules using ATR-FTIR and XRD.

PubMed

Chen, Long; Tian, Yaoqi; Sun, Binghua; Cai, Canxin; Ma, Rongrong; Jin, Zhengyu

2018-03-01

Concerns regarding increased dietary oil uptake have prompted efforts to investigate the oil absorption and distribution in fried starchy foods. In the present study, attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, together with a chloroform-methanol method, was used to analyze the external and internal oil contents in fried starchy samples. The micromorphology of fried starchy samples was further investigated using scanning electron microscope (SEM), polarized light microscope (PLM) and confocal laser scanning microscopy (CLSM). The results indicated that large amounts of oil were absorbed in or within waxy maize starch, but the majority of oil was located near the surface layer of the starch granules. After defatting, the internal oil was thoroughly removed, while a small amount of external oil remained. As evidenced by the changes of the crystalline characteristics with the help of X-ray diffraction (XRD), the interaction between starch and lipids on the surface was confirmed to form V-type complex compounds during frying at high moisture. Copyright © 2017 Elsevier Ltd. All rights reserved.

Bioleaching of two different genetic types of chalcopyrite and their comparative mineralogical assessment.

PubMed

Deng, Sha; Gu, Guohua; Ji, Jing; Xu, Baoke

2018-02-01

The bioleaching of two different genetic types of chalcopyrite by the moderate thermophile Sulfobacillus thermosulfidooxidans was investigated by leaching behaviors elucidation and their comparative mineralogical assessment. The leaching experiment showed that the skarn-type chalcopyrite (STC) revealed a much faster leaching rate with 33.34% copper extracted finally, while only 23.53% copper was bioleached for the porphyry-type chalcopyrite (PTC). The mineralogical properties were analyzed by XRD, SEM, XPS, and Fermi energy calculation. XRD indicated that the unit cell volume of STC was a little larger than that of PTC. SEM indicated that the surface of STC had more steps and ridges. XPS spectra showed that Cu(I) was the dominant species of copper on the surfaces of the two chalcopyrite samples, and STC had much more copper with lower Cu 2p 3/2 binding energy. Additionally, the Fermi energy of STC was much higher than that of PTC. These mineralogical differences were in good agreement with the bioleaching behaviors of chalcopyrite. This study will provide some new information for evaluating the oxidation kinetics of chalcopyrite.

Phase separation in SiGe nanocrystals embedded in SiO{sub 2} matrix during high temperature annealing

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

Mogaddam, N. A. P.; Turan, R.; Alagoz, A. S.

2008-12-15

SiGe nanocrystals have been formed in SiO{sub 2} matrix by cosputtering Si, Ge, and SiO{sub 2} independently on Si substrate. Effects of the annealing time and temperature on structural and compositional properties are studied by transmission electron microscopy, x-ray diffraction (XRD), and Raman spectroscopy measurements. It is observed that Ge-rich Si{sub (1-x)}Ge{sub x} nanocrystals do not hold their compositional uniformity when annealed at high temperatures for enough long time. A segregation process leading to separation of Ge and Si atoms from each other takes place. This process has been evidenced by a double peak formation in the XRD and Ramanmore » spectra. We attributed this phase separation to the differences in atomic size, surface energy, and surface diffusion disparity between Si and Ge atoms leading to the formation of nonhomogenous structure consist of a Si-rich SiGe core covered by a Ge-rich SiGe shell. This experimental observation is consistent with the result of reported theoretical and simulation methods.« less

Spectral masking of goethite in abandoned mine drainage systems: implications for Mars

USGS Publications Warehouse

Cull, Selby; Cravotta, Charles A.; Klinges, Julia Grace; Weeks, Chloe

2014-01-01

Remote sensing studies of the surface of Mars use visible- to near-infrared (VNIR) spectroscopy to identify hydrated and hydroxylated minerals, which can be used to constrain past environmental conditions on the surface of Mars. However, due to differences in optical properties, some hydrated phases can mask others in VNIR spectra, complicating environmental interpretations. Here, we examine the role of masking in VNIR spectra of natural precipitates of ferrihydrite, schwertmannite, and goethite from abandoned mine drainage (AMD) systems in southeastern Pennsylvania. Mixtures of ferrihydrite, schwertmannite, and goethite were identified in four AMD sites by using X-ray diffractometry (XRD), and their XRD patterns compared to their VNIR spectra. We find that both ferrihydrite and schwertmannite can mask goethite in VNIR spectra of natural AMD precipitates. These findings suggest that care should be taken in interpreting environments on Mars where ferrihydrite, schwertmannite, or goethite are found, as the former two may be masking the latter. Additionally, our findings suggest that outcrops on Mars with both goethite and ferrihydrite/schwertmannite VNIR signatures may have high relative abundances of goethite, or the goethite may exist in a coarsely crystalline phase.

Effect of surfactant types and their concentration on the structural characteristics of nanoclay

NASA Astrophysics Data System (ADS)

Zawrah, M. F.; Khattab, R. M.; Saad, E. M.; Gado, R. A.

2014-03-01

A series of organo-modified nanoclays was synthesized using three different surfactants having different alkyl chain lengths and concentrations [0.5-5.0 cation exchange capacity (CEC)]. These surfactants were Ethanolamine (EA), Cetyltrimethylammoniumbromide (CTAB) and Tetraoctadecylammoniumbromide (TO). The obtained modified nanoclays were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM) and compared with unmodified nanoclay. The results of XRD analysis indicated that the basal d-spacing has increased with increasing alkyl chain length and surfactant concentration. From the obtained microstructures of these organo-modified nanoclays, the mechanism of surfactant adsorption was proposed. At relatively low loading of surfactant, most of surfactant entered the spacing by an ion-exchange mechanism and is adsorbed onto the interlayer cation sites. When the concentration of the surfactant exceeds the CEC of clay, the surfactant molecules then adhere to the surface adsorbed surfactant. Some surfactants entered the interlayers, whereas the others were attached to the clay surface. When the concentration of surfactant increased further beyond 2.0 CEC, the surfactants might occupy the inter-particle space within the house-of-cards aggregate structure.

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

Graphene/Ruthenium Active Species Aerogel as Electrode for Supercapacitor Applications.

PubMed

Gigot, Arnaud; Fontana, Marco; Pirri, Candido Fabrizio; Rivolo, Paola

2017-12-30

Ruthenium active species containing Ruthenium Sulphide (RuS₂) is synthesized together with a self-assembled reduced graphene oxide (RGO) aerogel by a one-pot hydrothermal synthesis. Ruthenium Chloride and L-Cysteine are used as reactants. The hydrothermal synthesis of the innovative hybrid material occurs at 180 °C for 12 h, by using water as solvent. The structure and morphology of the hybrid material are fully characterized by Raman, XRD, XPS, FESEM and TEM. The XRD and diffraction pattern obtained by TEM display an amorphous nanostructure of RuS₂ on RGO crystallized flakes. The specific capacitance measured in planar configuration in 1 M NaCl electrolyte at 5 mV s -1 is 238 F g -1 . This supercapacitor electrode also exhibits perfect cyclic stability without loss of the specific capacitance after 15,000 cycles. In summary, the RGO/Ruthenium active species hybrid material demonstrates remarkable properties for use as active material for supercapacitor applications.

Impact of natural organic matter coatings on the microbial reduction of iron oxides

NASA Astrophysics Data System (ADS)

Poggenburg, Christine; Mikutta, Robert; Schippers, Axel; Dohrmann, Reiner; Guggenberger, Georg

2018-03-01

Iron (Fe) oxyhydroxides are important constituents of the soil mineral phase known to stabilize organic matter (OM) under oxic conditions. In an anoxic milieu, however, these Fe-organic associations are exposed to microbial reduction, releasing OM into soil solution. At present, only few studies have addressed the influence of adsorbed natural OM (NOM) on the reductive dissolution of Fe oxyhydroxides. This study therefore examined the impact of both the composition and concentration of adsorbed NOM on microbial Fe reduction with regard to (i) electron shuttling, (ii) complexation of Fe(II,III), (iii) surface site coverage and/or pore blockage, and (iv) aggregation. Adsorption complexes with varying carbon loadings were synthesized using different Fe oxyhydroxides (ferrihydrite, lepidocrocite, goethite, hematite, magnetite) and NOM of different origin (extracellular polymeric substances from Bacillus subtilis, OM extracted from soil Oi and Oa horizons). The adsorption complexes were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), N2 gas adsorption, electrophoretic mobility and particle size measurements, and OM desorption. Incubation experiments under anaerobic conditions were conducted for 16 days comparing two different strains of dissimilatory Fe(III)-reducing bacteria (Shewanella putrefaciens, Geobacter metallireducens). Mineral transformation during reduction was assessed via XRD and FTIR. Microbial reduction of the pure Fe oxyhydroxides was controlled by the specific surface area (SSA) and solubility of the minerals. For Shewanella putrefaciens, the Fe reduction of adsorption complexes strongly correlated with the concentration of potentially usable electron-shuttling molecules for NOM concentrations <2 mg C L-1, whereas for Geobacter metallireducens, Fe reduction depended on the particle size and thus aggregation of the adsorption complexes. These diverging results suggest that the influence of NOM on the stability of Fe-organic associations in soils cannot easily be assessed without considering the composition of the microbial soil community.

Anti-bacteria activity of carbon nanotubes grown on trimetallic catalyst

NASA Astrophysics Data System (ADS)

Ibrahim, S. O.; Abdulkareem, A. S.; Isah, K. U.; Ahmadu, U.; Bankole, M. T.; Kariim, I.

2018-06-01

Trimetallic catalyst was prepared using wet impregnation method to produce carbon nanotubes (CNTs) through the method of catalytic chemical vapor deposition (CCVD). Characterization of the developed catalyst and CNTs were carried out using thermogravimetric analysis (TGA), x-ray diffraction (XRD), specific surface area Brunauer-Emmett-Teller (BET), Fourier-transform infrared spectroscopy (FTIR), high-resolution scanning electron microscopy (HRSEM)/energy dispersive x-ray spectroscopy (EDS) and high-resolution transmission electron microscopy (HRTEM)/selected area electron diffraction (SAED). The BET and TGA analysis indicated that the catalyst has a high surface area and is thermally stable. The FTIR of the developed catalyst shows notable functional group with presence of unbound water. The HRSEM of the catalyst revealed agglomerated, homogeneous and porous particles while the HRSEM/HRTEM of the produced CNTs gave the formation of long strand of multiwalled carbon nanotubes (MWCNTs), and homogeneous crystalline fringe like structure with irregular diameter. EDS revealed the dominance of carbon in the elemental composition. XRD/SAED patterns of the catalyst suggest high dispersion of the metallic particles in the catalyst mixture while that of the CNTs confirmed that the produced MWCNTs were highly graphitized and crystalline in nature with little structural defects. The anti-bacteria activity of the produced MWCNTs on Klebsiella pneumoneae, Escherichia coli, and Pseudomonas aeruginosa was also carried out. It was observed that the produced MWCNTs have an inhibitory property on bacteria; Escherichia coli and Klebsiella pneumoneae from zero day ( and ) through to twelfth day (Nil count) respectively. It has no effect on Pseudomonas aeruginosa with too numerous to count at zero-sixth day, but a breakdown in its growth at ninth-twelfth day (). This study implied that MWCNTs with varying diameter and well-ordered nano-structure can be produced from catalyst via CCVD method, and it can be recommended that the MWCNTs can be used to treat infected media contaminated with Klebsiella pneumoneae, Escherichia coli, and Pseudomonas aeruginosa.

Mercury Retention and Accumulation by Plants at the Abandoned New Idria Mine Site - a Preliminary micro-XRF and micro-XRD Study

NASA Astrophysics Data System (ADS)

Siebner, H.; Webb, S. M.; Brown, G. E.

2008-12-01

Due to its high toxicity and increasing levels in ecosystems, Hg pollution has become a serious global problem. A lot of research has been conducted with regard to Hg biogeochemical cycles in aquatic systems. Much less is known about terrestrial Hg-cycles in general and in plants specifically. Plants play an important role in these cycles; they are known to be an important sink for both atmospheric and soil Hg, the vegetative cover significantly influences soil erosion and migration of contaminants into aquatic systems. However, the processes involved in the interactions of Hg with plants and plants products are poorly studied. Information concerning the interaction of Hg in plants at the molecular level is sparse. The present study is intended to provide new information on Hg retention, translocation, and accumulation in plants associated with mercury mine wastes in central California. We present here preliminary results of Hg distribution in root and leave samples, taken from different plant species, which have adapted to the hostile environment at the New Idria site. Samples were taken at two locations that differ in water acidity and flooding regime. The distribution of Hg appears to be affected by plant species, growing conditions, and development stage. Micro-XRF images of root sections show that Hg is mainly associated with Fe plaque at the outer surfaces and epidermis, but is distributed differently in roots of the two plants. Micro-XRD showed evidence for mineralogical changes in the plaque through the sections. Mercury in leaves was found to be highly diffuse in its distribution, and is not associated with Fe-rich particles attached to the outer surface of the leaf. This finding implies that Hg is assimilated in the leaf tissue. Further examination of Fe plaque characteristics and associated Hg, as well as Hg speciation in the different organs of these plants, is being conducted in our lab.

A facile method to modify bentonite nanoclay with silane

NASA Astrophysics Data System (ADS)

Abeywardena, Sujani B. Y.; Perera, Srimala; Nalin de Silva, K. M.; Tissera, Nadeeka P.

2017-07-01

Immobilization of smectite clay onto a desirable surface has received much attention, since its nanospace can be utilized for many applications in material science. Here, we present an efficient method to functionalize surface of bentonite nanoclay (BNC) through the grafting of 3-aminotriethoxysilane (APTES). Infrared spectroscopy and elemental analysis confirmed the presence of organic chains and amine groups in modified nanoclay. XRD analysis confirmed grafting of APTES on the surface of bentonite nanoclay without intercalation. The accomplishment of the surface modification was quantitatively proved by TGA analysis. Modified BNC can covalently couple with different material surfaces, allowing its nanospace to be utilized for intercalation of cations, bio-molecules, and polymeric materials, to be used in advanced military aerospace, pharmaceuticals, and many other commercial applications.

Amorphous V-O-C composite nanofibers electrospun from solution precursors as binder- and conductive additive-free electrodes for supercapacitors with outstanding performance

NASA Astrophysics Data System (ADS)

Chen, Xia; Zhao, Bote; Cai, Yong; Tadé, Moses O.; Shao, Zongping

2013-11-01

Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well-dispersed in the carbon nanofibers, free from the formation of an aggregated crystalline phase, even in the case of V20. A specific surface area of 587.9 m2 g-1 was reached for V10 after calcination, which is approximately twice that of the vanadium-free carbon nanofibers (V0, 300.9 m2 g-1). To perform as an electrode for supercapacitors in an aqueous electrolyte, the V10 film delivered a specific capacitance of 463 F g-1 at 1 A g-1. V10 was also able to retain a specific capacitance of 380 F g-1, even at a current density of 10 A g-1. Additionally, very stable cycling stability was achieved, maintaining an outstanding specific capacitance of 400 F g-1 at 5 A g-1 after charge-discharge cycling 5000 times. Thus, V-O-C composite nanofibers are highly attractive electrode materials for flexible, high-power, thin film energy storage devices and applications.Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well-dispersed in the carbon nanofibers, free from the formation of an aggregated crystalline phase, even in the case of V20. A specific surface area of 587.9 m2 g-1 was reached for V10 after calcination, which is approximately twice that of the vanadium-free carbon nanofibers (V0, 300.9 m2 g-1). To perform as an electrode for supercapacitors in an aqueous electrolyte, the V10 film delivered a specific capacitance of 463 F g-1 at 1 A g-1. V10 was also able to retain a specific capacitance of 380 F g-1, even at a current density of 10 A g-1. Additionally, very stable cycling stability was achieved, maintaining an outstanding specific capacitance of 400 F g-1 at 5 A g-1 after charge-discharge cycling 5000 times. Thus, V-O-C composite nanofibers are highly attractive electrode materials for flexible, high-power, thin film energy storage devices and applications. Electronic supplementary information (ESI) available: FE-SEM image. See DOI: 10.1039/c3nr04484j

Mechanisms of uranium interactions with hydroxyapatite: Implications for groundwater remediation

USGS Publications Warehouse

Fuller, C.C.; Bargar, J.R.; Davis, J.A.; Piana, M.J.

2002-01-01

The speciation of U(VI) sorbed to synthetic hydroxyapatite was investigated using a combination of U LIII-edge XAS, synchrotron XRD, batch uptake measurements, and SEM-EDS. The mechanisms of U(VI) removal by apatite were determined in order to evaluate the feasibility of apatitebased in-situ permeable reactive barriers (PRBs). In batch U(VI) uptake experiments with synthetic hydroxyapatite (HA), near complete removal of dissolved uranium (>99.5%) to <0.05 ??M was observed over a range of total U(VI) concentrations up to equimolar of the total P in the suspension. XRD and XAS analyses of U(VI)-reacted HA at sorbed concentrations ???4700 ppm U(VI) suggested that uranium(VI) phosphate, hydroxide, and carbonate solids were not present at these concentrations. Fits to EXAFS spectra indicate the presence of Ca neighbors at 3.81 A??. U-Ca separation, suggesting that U(VI) adsorbs to the HA surfaces as an inner-sphere complex. Uranium(VI) phosphate solid phases were not detected in HA with 4700 ppm sorbed U(VI) by backscatter SEM or EDS, in agreement with the surface complexation process. In contrast, U(VI) speciation in samples that exceeded 7000 ppm sorbed U(VI) included a crystalline uranium(VI) phosphate solid phase, identified as chernikovite by XRD. At these higher concentrations, a secondary, uranium(VI) phosphate solid was detected by SEM-EDS, consistent with chernikovite precipitation. Autunite formation occurred at total U:P molar ratios ???0.2. Our findings provide a basis for evaluating U(VI) sorption mechanisms by commercially available natural apatites for use in development of PRBs for groundwater U(VI) remediation.

Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

PubMed

Morgan, Dane V; Macy, Don; Stevens, Gerald

2008-11-01

A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35 ns pulse. The characteristic K(alpha) lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5 degrees . A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device camera through a coherent fiber-optic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1 mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic aluminum lattice with no phase transformation.

The effect of surface treatments on dental zirconia: An analysis of biaxial flexural strength, surface roughness and phase transformation.

PubMed

Botelho, Michael G; Dangay, Sachin; Shih, Kaimin; Lam, Walter Y H

2018-05-26

This study investigates the effect of selected surface finishing techniques on the biaxial flexural strength, surface roughness and phase transformation of a zirconia dental restorative material. Fully-sintered zirconia discs (⌀19.5 mm × 0.85 mm) were treated on one side with a single or a combination of the following treatments: diamond and/or tungsten-carbide burs without water coolant in an air-turbine handpiece, air-particle abrasion, rubber-point polishing in a contra-angle handpiece, or no treatment (control). Biaxial flexural strength (BFS) (eleven groups, n = 10) was determined using a universal testing machine and surface roughness (thirteen groups, n = 6) was assessed using a profilometer. Results were analysed using one-way ANOVA and Student-Newman-Keuls Post-hoc test (α = 0.05) with Bonferroni correction. Specimens were observed under scanning electron microscopy (SEM) and x-ray diffraction (XRD) for their microstructure and crystalline phases respectively. Grinding with diamond burs did not weaken zirconia (p > 0.0045) but produced rougher surfaces than the control group (p < 0.0038). Tungsten-carbide burs smoothened diamond ground specimens (p < 0.0038) for both grits of diamond. Specimens ground by tungsten-carbide burs have significantly reduced mean BFS (p < 0.0045) by up to two-thirds and SEM revealed fine surface cracks. Air-particle abrasion restored the mean BFS of tungsten-carbide ground specimens to control levels (p > 0.0045) and surface cracks were not observed. Phase transformation was not detected by XRD. Dental zirconia ground dry with tungsten-carbide burs has a significantly reduced BFS and a smooth but defective surface. These defects may be removed and BFS restored by air-particle abrasion. The use of tungsten-carbide burs for grinding dental zirconia should be cautioned. Diamond grinding does not weaken zirconia but requires further polishing. Copyright © 2018 Elsevier Ltd. All rights reserved.

Coherent 3D nanostructure of γ-Al{sub 2}O{sub 3}: Simulation of whole X-ray powder diffraction pattern

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

Pakharukova, V.P., E-mail: verapakh@catalysis.ru; Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk; Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090

2017-02-15

The structure and nanostructure features of nanocrystalline γ-Al{sub 2}O{sub 3} obtained by dehydration of boehmite with anisotropic platelet-shaped particles were investigated. The original models of 3D coherent nanostructure of γ-Al{sub 2}O{sub 3} were constructed. The models of nanostructured γ-Al{sub 2}O{sub 3} particles were first confirmed by a direct simulation of powder X–Ray diffraction (XRD) patterns using the Debye Scattering Equation (DSE) with assistance of high-resolution transmission electron microscopy (HRTEM) study. The average crystal structure of γ-Al{sub 2}O{sub 3} was shown to be tetragonally distorted. The experimental results revealed that thin γ-Al{sub 2}O{sub 3} platelets were heterogeneous on a nanometer scalemore » and nanometer-sized building blocks were separated by partially coherent interfaces. The XRD simulation results showed that a specific packing of the primary crystalline blocks in the nanostructured γ-Al{sub 2}O{sub 3} particles with formation of planar defects on (001), (100), and (101) planes nicely accounted for pronounced diffuse scattering, anisotropic peak broadening and peak shifts in the experimental XRD pattern. The identified planar defects in cation sublattice seem to be described as filling cation non-spinel sites in existing crystallographic models of γ-Al{sub 2}O{sub 3} structure. The overall findings provided an insight into the complex nanostructure, which is intrinsic to the metastable γ-Al{sub 2}O{sub 3} oxide. - Highlights: • Thin plate-like crystallites of γ-Al{sub 2}O{sub 3} were obtained. • Models of 3D coherent nanostructure of γ-Al{sub 2}O{sub 3} were constructed. • Models were verified by simulating XRD patterns using the Debye Scattering Equation. • Specific broadening of XRD peaks was explained in terms of planar defects. • Primary crystalline blocks in γ-Al{sub 2}O{sub 3} are separated by partially coherent interfaces.« less

Micro and sub-micron surface structuring of AZ31 by laser re-melting and dimpling

NASA Astrophysics Data System (ADS)

Furlan, Valentina; Demir, Ali Gökhan; Previtali, Barbara

2015-12-01

In this work, the use of ns-pulsed fibre laser for surface structuring of AZ31 Mg alloy is investigated. Surface re-melting was employed to change surface morphology, especially in terms of surface roughness. Dimpling by percussion microdrilling was investigated to control the hole geometry.. With surface remelting mono-directional and homogeneous surfaces were obtained with Fl<500 J/cm2. Above 500 J/cm2 particle generation was observed, which induced sub-micron structure growth with nano-fibrous features. Moreover, surface roughness could be controlled below the initial value and much higher. With dimpling, transformation from gentle to strong ablation was observed at F0=10.3 J/cm2. XRD analysis was employed to link oxide growth to the surface morphology. Tensile tests were carried out to assess the damage on the mechanical properties after surface structuring.

Sodium Hydroxide Activated Nanoporous Carbons Based on Lapsi Seed Stone.

PubMed

Joshi, Sahira; Shrestha, Lok Kumar; Kamachi, Yuichiro; Yamauchi, Yusuke; Pradhananga, Mandira Adhikari; Pokhrel, Bhadra Prasad; Ariga, Katsuhiko; Pradhananga, Raja Ram

2015-02-01

Nanoporous activated carbons (ACs) were prepared from Lapsi (Choerospondias axillaris) seed powder by chemical activation with sodium hydroxide (NaOH) at different NaOH impregnation ratios. The prepared ACs were characterized by Fourier transform-infrared (FTIR) spectroscopy, Raman scattering, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Semi-quantitative information on the surface properties was obtained by estimating iodine number. FTIR spectra showed the presence of oxygenated functional groups such as hydroxyl, carbonyl, and carboxyl in the prepared ACs. Raman scattering showed clear D and G bands in the spectra. The intensity ratio of G and D band peak intensity was ca. 1.39 at lowest NaOH and Lapsi seed powder ratio 0.25:1 showing high graphitic degree. This ratio decreased with increase in the NaOH impregnation ratio and reached minimum ca. 0.94 (comparable with commercial AC) at NaOH and Lapsi seed powder ratio 1:1 demonstrating that higher NaOH impregnation reduces the graphitic structure of the carbon. XRD patterns showed two broad peaks at diffraction angles of approximately 25 and 43 degrees indicating the amorphous structure. Surface properties of the ACs (BET surface area, pore volume, and pore size distributions) were evaluated by nitrogen adsorption-desorption isotherm. Our ACs showed strong methylene blue adsorption property (maximum methylene blue is ca. 200 mg/g). Judging from the iodine number and methylene blue values, structure, and surface areas, it can be concluded that NaOH impregnation ratio is one of the key parameters to tune the surface properties of Lapsi seed stone-based activated carbons.

Evolution of catalytic activity of Au-Ag bimetallic nanoparticles on mesoporous support for CO oxidation.

PubMed

Wang, Ai-Qin; Chang, Chun-Ming; Mou, Chung-Yuan

2005-10-13

We report a novel Au-Ag alloy catalyst supported on mesoporous aluminosilicate Au-Ag@MCM prepared by a one-pot synthesis procedure, which is very active for low-temperature CO oxidation. The activity was highly dependent on the hydrogen pretreatment conditions. Reduction at 550-650 degrees C led to high activity at room temperature, whereas as-synthesized or calcined samples did not show any activity at the same temperature. Using various characterization techniques, such as XRD, UV-vis, XPS, and EXAFS, we elucidated the structure and surface composition change during calcination and the reduction process. The XRD patterns show that particle size increased only during the calcination process on those Ag-containing samples. XPS and EXAFS data demonstrate that calcination led to complete phase segregation of the Au-Ag alloy and the catalyst surface is greatly enriched with AgBr after the calcination process. However, subsequent reduction treatment removed Br- completely and the Au-Ag alloy was formed again. The surface composition of the reduced Au-Ag@MCM (nominal Au/Ag = 3/1) was more enriched with Ag, with the surface Au/Ag ratio being 0.75. ESR spectra show that superoxides are formed on the surface of the catalyst and its intensity change correlates well with the trend of catalytic activity. A DFT calculation shows that CO and O2 coadsorption on neighboring sites on the Au-Ag alloy was stronger than that on either Au or Ag. The strong synergism in the coadsorption of CO and O2 on the Au-Ag nanoparticle can thus explain the observed synergetic effect in catalysis.

XRD and SEM study of alumina silicate porcelain insulator

NASA Astrophysics Data System (ADS)

Duddi, Dharmender; Singh, G. P.; Kalra, Swati; Shekhawat, M. S.; Tak, S. K.

2018-05-01

Higher strength electrical porcelain is a requirement of industry. This will be achieved by a specific composition of raw materials, which is consisted of clays and feldspars. Water absorption, particle size and insulating properties are of special interest now a day. China clay, Ball clay and Quartz are widely used by ceramic industries in Bikaner district of Rajasthan. Sample for present study were prepared by mixing of above clay, feldspar with MnO2, then shrinkage is observed. Bar shaped samples were prepared and heated up to a temperature of about 1185° C to observe shrinkage. For phase study of XRD and SEM are observed.

Titanium hydride and hydrogen concentration in acid-etched commercially pure titanium and titanium alloy implants: a comparative analysis of five implant systems.

PubMed

Szmukler-Moncler, S; Bischof, M; Nedir, R; Ermrich, M

2010-09-01

Acid etching is a popular method to texture the surface of dental implants. During etching, the titanium oxide protective layer is dissolved and small native hydrogen ions diffuse into the unprotected implant surface. They enrich the implant surface with hydrogen and precipitate into titanium hydride (TiH). The aim of this study was to measure the concentration of TiH at the implant surface and the total concentration of Hydrogen at five commercially available implant systems, made of either commercially pure (cp) titanium or titanium alloy. X-Ray diffraction (XRD) was conducted on each implant system to determine the compounds present at the implant surface. Following a TiH(2)/Ti calibration curve, the concentration of TiH was determined. Concentration of hydrogen in the implants was measured by the inert gas fusion thermal conductivity/infrared detection method. XRD data showed that TiH was present on all cp titanium implants but not on the alloyed implants. TiH concentration varied between 5% and 37%. Hydrogen concentration varied between 43 and 108 ppm, no difference in uptake was found between the cp titanium and alloyed implants. Low solubility of hydrogen in alpha-titanium is responsible for precipitation into TiH. Stronger etching conditions led to higher concentration of TiH2-x. High solubility of hydrogen in the beta-phase of the alloy is preventing hydrogen from precipitating into TiH. All implants, even those lacking TiH at the surface, were enriched with hydrogen. In all implants, hydrogen concentration was within the normative limit of 130 ppm.

Bioactivity and biocompatibility of hydroxyapatite-based bioceramic coatings on zirconium by plasma electrolytic oxidation.

PubMed

Aktuğ, Salim Levent; Durdu, Salih; Yalçın, Emine; Çavuşoğlu, Kültigin; Usta, Metin

2017-02-01

In the present work, hydroxyapatite (HAP)-based plasma electrolytic oxide (PEO) coatings were produced on zirconium at different current densities in a solution containing calcium acetate and β-calcium glycerophosphate by a single step. The phase structure, surface morphology, functional groups, thickness and roughness of the coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), eddy current method and surface profilometer, respectively. The phases of cubic-zirconia, calcium zirconate and HAP were detected by XRD. The amount of HAP and calcium zirconate increased with increasing current density. The surface of the coatings was very porous and rough. Moreover, bioactivity and biocompatibility of the coatings were analyzed in vitro immersion simulated body fluid (SBF) and MTT (3-(4,5-dimethyl thiazol-2yl)-2,5-diphenyl tetrazolium bromide) assay, hemolysis assay and bacterial formation. The apatite-forming ability of the coatings was evaluated after immersion in SBF up to 28days. After immersion, the bioactivity of HAP-based coatings on zirconium was greater than the ones of uncoated zirconium and zirconium oxide-based surface. The bioactivity of PEO surface on zirconium was significantly improved under SBF conditions. The bacterial adhesion of the coatings decreased with increasing current density. The bacterial adhesion of the coating produced at 0.370A/cm 2 was minimum compared to uncoated zirconium coated at 0.260 and 0.292A/cm 2 . The hemocompatibility of HAP-based surfaces was improved by PEO. The cell attachment and proliferation of the PEO coatings were better than the one of uncoated zirconium according to MTT assay results. Copyright © 2016 Elsevier B.V. All rights reserved.

Apatite grown in niobium by two-step plasma electrolytic oxidation.

PubMed

Pereira, Bruno Leandro; Lepienski, Carlos Maurício; Mazzaro, Irineu; Kuromoto, Neide Kazue

2017-08-01

Plasma electrolytic oxidation (PEO) of niobium plates were done electrochemically in two steps with electrolytes containing phosphorous and calcium being observed the formation of crystalline apatite. All samples were submitted to a first step of PEO using an electrolyte containing phosphate ions. The second oxidization step was made using three different electrolytes. Some samples were oxidized by PEO in electrolyte containing calcium, while in other samples it was used two mixtures of phosphoric acid and calcium acetate monohydrate solutions. Three different surface layers were obtained. The morphology and chemical composition of the films were analyzed by scanning electronic microscopy (SEM), and energy dispersive spectroscopy (EDS) respectively. It was observed that all samples submitted to two-step oxidation shown porous surface and a calcium and phosphorus rich layer. Average surface roughness (Ra) was measured by a profilometer remaining in the sub-micrometric range. The contact angle by sessile drop technique, using 1μL of distilled water was performed with an optical goniometer. It was verified a higher hydrophilicity in all surfaces compared to the polished niobium. Orthorhombic Nb 2 O 5 was identified by XRD in the oxide layer. Crystalline apatite was identified by XRD in surfaces after the second oxidation made with the Ca-rich electrolyte and a mixture of an electrolyte richer in Ca compared to P. These results indicate that a two-step oxidized niobium surface present great features for applications in the osseointegration processes: favorable chemical composition that increase the biocompatibility, the formation of crystalline niobium pentoxide (orthorhombic), high hydrophilicity and formation of crystalline calcium phosphate (apatite) under adequate electrolyte composition. Copyright © 2016 Elsevier B.V. All rights reserved.

Impact of Plasma Surface Treatment on Bamboo Charcoal/silver Nanocomposite

NASA Astrophysics Data System (ADS)

Vignesh, K.; Vijayalakshmi, K. A.; Karthikeyan, N.

2016-10-01

Bamboo charcoal (BC) accompanied silver (Ag) nanocomposite is synthesized through sol-gel method. The produced BC/Ag nanocomposite was surface modified by air and oxygen plasma treatments. Silver ions (Ag+) will serve to improve the antibacterial activity as well as the surface area of BC. Plasma treatment has improved the surface functional groups, crystalline intensity and antibacterial activity of the prepared nanocomposite. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) studies show that Ag nanoparticles have good agreement with BC and the particle size has a mean diameter of 20-40nm. We observe the carboxyl functional groups in Fourier transform infrared spectroscopy (FTIR) after the oxygen plasma treatment. Moreover surface area and adsorption were analyzed by using the Brunauer, Emmett and Teller (BET) surface area (SBET) and UV-Vis spectroscopy.

Quantitative XRD analysis of {110} twin density in biotic aragonites.

PubMed

Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

2012-12-01

{110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

Comparing two tetraalkylammonium ionic liquids. II. Phase transitions

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

Lima, Thamires A.; Paschoal, Vitor H.; Faria, Luiz F. O.

Phase transitions of the ionic liquids n-butyl-trimethylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1114}][NTf{sub 2}], and methyl-tributylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1444}][NTf{sub 2}], were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) measurements, and Raman spectroscopy. XRD and Raman spectra were obtained as a function of temperature at atmospheric pressure, and also under high pressure at room temperature using a diamond anvil cell (DAC). [N{sub 1444}][NTf{sub 2}] experiences glass transition at low temperature, whereas [N{sub 1114}][NTf{sub 2}] crystallizes or not depending on the cooling rate. Both the ionic liquids exhibit glass transition under high pressure. XRD and low-frequency Raman spectra provide a consistent physical picturemore » of structural ordering-disordering accompanying the thermal events of crystallization, glass transition, cold crystallization, pre-melting, and melting. Raman spectra in the high-frequency range of some specific cation and anion normal modes reveal conformational changes of the molecular structures along phase transitions.« less

Magnetic composites from minerals: study of the iron phases in clay and diatomite using Mössbauer spectroscopy, magnetic measurements and XRD

NASA Astrophysics Data System (ADS)

Cabrera, M.; Maciel, J. C.; Quispe-Marcatoma, J.; Pandey, B.; Neri, D. F. M.; Soria, F.; Baggio-Saitovitch, E.; de Carvalho, L. B.

2014-01-01

Magnetic particles as matrix for enzyme immobilization have been used and due to the enzymatic derivative can be easily removed from the reaction mixture by a magnetic field. This work presents a study about the synthesis and characterization of iron phases into magnetic montmorillonite clay (mMMT) and magnetic diatomaceous earth (mDE) by 57Fe Mössbauer spectroscopy (MS), magnetic measurements and X-ray diffraction (XRD). Also these magnetic materials were assessed as matrices for the immobilization of invertase via covalent binding. Mössbauer spectra of the magnetic composites performed at 4.2 K showed a mixture of magnetite and maghemite about equal proportion in the mMMT, and a pure magnetite phase in the sample mDE. These results were verified using XRD. The residual specific activity of the immobilized invertase on mMMT and mDE were 83 % and 92.5 %, respectively. Thus, both magnetic composites showed to be promising matrices for covalent immobilization of invertase.

Magnetic transition in Y-site doped multiferroic YMnO{sub 3}

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

Thakur, Rajesh K., E-mail: thakur.rajesh2009@gmail.com; Thakur, Rasna, E-mail: rasnathakur@yahoo.com; Gaur, N. K., E-mail: srl-nkgaur@yahoo.co.in

2016-05-06

We have synthesized polycrystalline hexagonal Y{sub 1-x}Sr{sub x}MnO{sub 3} (x=0.02, 0.1) compounds by using conventional solid state reaction method. The detailed structural investigations are carried out by using XRD studies which reveals the single phase formation of the reported compounds with hexagonal structure and space group P6{sub 3}cm (JCPDS: 25-1079). Further the XRD data of reported compounds were analyzed by RIETVELD (FULLPROFF) method which shows the decrease in the lattice parameter with increasing concentration of divalent strontium to Y-site. The observed pointed kinks in the specific heat study are indicative of the probable coupling in between the electric and magneticmore » orders in this class of materials. The reported systematic specific heat studies shows that the antiferromagnetic (AFM) transition temperature (T{sub N}) shifts to higher value with increasing concentration of Sr{sup 2+} ion in the YMnO{sub 3} compound which is attributed to the enhanced lattice contribution to the specific heat in the this compound. The present compound shows the independence of specific heat and magnetic transition temperature with applied magnetic field of 8T and 12T.« less

Influence of incubation temperature on biofilm formation and corrosion of carbon steel by Serratia marcescens

NASA Astrophysics Data System (ADS)

Harimawan, Ardiyan; Devianto, Hary; Kurniawan, Ignatius Chandra; Utomo, Josephine Christine

2017-01-01

Microbial induced corrosion (MIC) or biocorrosion is one type of corrosion, directly or indirectly influenced by microbial activities, by forming biofilm and adhering on the metal surface. When forming biofilm, the microorganisms can produce extracellular products which influence the cathodic and anodic reactions on metal surfaces. This will result in electrochemical changes in the interface between the biofilm and the metal surface, leading to corrosion and deterioration of the metal. MIC might be caused by various types of microorganism which leads to different corrosion mechanism and reaction kinetics. Furthermore, this process will also be influenced by various environmental conditions, such as pH and temperature. This research is aimed to determine the effect of incubation temperature on corrosion of carbon steel caused by Serratia marcescens in a mixture solution of synthetic seawater with Luria Bertani medium with a ratio of 4:1. The incubation was performed for 19 days with incubation temperature of 30, 37, and 50°C. The analyses of biofilm were conducted by total plate count (TPC), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Biofilm was found to be evenly growth on the surface and increasing with increasing incubation temperature. It consists of functional group of alcohol, alkane, amine, nitro, sulfate, carboxylic acid, and polysulfide. The analyses of the corrosion were conducted by gravimetric and X-ray diffraction (XRD). Higher incubation temperature was found to increase the corrosion rate. However, the corrosion products were not detected by XRD analysis.

The role of S(II) and Pb(II) in xanthate flotation of smithsonite: Surface properties and mechanism

NASA Astrophysics Data System (ADS)

Jia, Kai; Feng, Qiming; Zhang, Guofan; Ji, Wanying; Zhang, Wukai; Yang, Bingqian

2018-06-01

Smithsonite is a readily dissolvable carbonate mineral that is naturally hydrophilic, making recovery of this ore by flotation difficult. The flotation results showed that conditioning with only sodium sulfide (Na2S) did not successfully allow the smithsonite samples to float, whereas treatment with a combination of S(II), Pb(II) and xanthate (with Na2S as the sulfurizing reagent, lead ions (Pb(II)) as the activator, and xanthate as the collector) improved the flotation of smithsonite, achieving a mass recovery of 95.8%. A combination of analytical techniques, including X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS), in conjunction with depth profiling, was used to investigate the chemical nature of the sulfur and lead species on the smithsonite surface. For S(II)-conditioned smithsonite, a layer of ZnS formed on the smithsonite (ZnCO3) substrates; this newly formed ZnS coating was amorphous or poorly crystallized. For smithsonite samples conditioned with S(II) and Pb(II), the microstructures and the phase constituents, obtained by AFM and XRD analyses, confirmed the formation of the PbS species with a cubic galena structure on the surface. XPS depth profiling showed that the PbS layer was 18-nm thick, which corresponds to 30 PbS molecular layers. This study presents direct evidence that the coating of the activation product, PbS, on the smithsonite surface was similar to a relatively thick galena layer, which led to successful flotation.

Functional characteristics, wettability properties and cytotoxic effect of starch film incorporated with multi-walled and hydroxylated multi-walled carbon nanotubes.

PubMed

Shahbazi, Mahdiyar; Rajabzadeh, Ghadir; Sotoodeh, Shahnaz

2017-11-01

Two types of multi-walled carbon nanotubes (CNT and CNT-OH) at different levels (0.1-0.9wt%) were introduced into starch matrix in order to modify its functional properties. The optimum concentration of each nanotube was selected based on the results of water solubility, water permeability and mechanical experiments. The physico-mechanical data showed that CNT up to 0.7wt% led to a notable increase in water resistance, water barrier property and tensile strength, whilst regarding CNT-OH, these improvements found at 0.9wt%. Therefore, effects of optimized level of each nanotube on the starch film were evaluated by XRD, surface hydrophobicity, wettability and surface energy tests. XRD revealed that the position of starch characteristic peak shifted to higher degree after nanotubes introducing. The hydrophobic character of the film was greatly increased with incorporation of nanoparticles, as evidenced by increased contact angle with greatest value regarding CNT-OH. Moreover, CNT-OH notably decreased the surface free energy of the starch film. Finally, the conformity of both nanocomposites with actual food regulations on biodegradable materials was tested by cytotoxicity assay to evaluate the possibility of application in food packaging sector. Both nanocomposite films had potential of cytotoxic effects, since they could increase cytoplasmic lactate dehydrogenase release from L-929 fibroblast cells in contact with their surface. Copyright © 2017 Elsevier B.V. All rights reserved.

Arsenate adsorption mechanisms at the allophane - Water interface

USGS Publications Warehouse

Arai, Y.; Sparks, D.L.; Davis, J.A.

2005-01-01

We investigated arsenate (As(V)) reactivity and surface speciation on amorphous aluminosilicate mineral (synthetic allophane) surfaces using batch adsorption experiments, powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The adsorption isotherm experiments indicated that As(V) uptake increased with increasing [As(V)]0 from 50 to 1000 ??M (i.e., Langmuir type adsorption isotherm) and that the total As adsorption slightly decreased with increasing NaCl concentrations from 0.01 to 0.1 M. Arsenate adsorption was initially (0-10 h) rapid followed by a slow continuum uptake, and the adsorption processes reached the steady state after 720 h. X-ray absorption spectroscopic analyses suggest that As(V) predominantly forms bidentate binuclear surface species on aluminum octahedral structures, and these species are stable up to 11 months. Solubility calculations and powder XRD analyses indicate no evidence of crystalline AI-As(V) precipitates in the experimental systems. Overall, macroscopic and spectroscopic evidence suggest that the As(V) adsorption mechanisms at the allophane-water interface are attributable to ligand exchange reactions between As(V) and surface-coordinated water molecules and hydroxyl and silicate ions. The research findings imply that dissolved tetrahedral oxyanions (e.g., H2PO42- and H2AsO42-) are readily retained on amorphous aluminosilicate minerals in aquifer and soils at near neutral pH. The innersphere adsorption mechanisms might be important in controlling dissolved arsenate and phosphate in amorphous aluminosilicate-rich low-temperature geochemical environments. ?? 2005 American Chemical Society.

Dendritic Ag-Fe nanocrystalline alloy synthesized by pulsed electrodeposition and its characterization

NASA Astrophysics Data System (ADS)

Santhi, Kalavathy; Revathy, T. A.; Narayanan, V.; Stephen, A.

2014-10-01

Synthesis of dendrite shaped Ag-Fe alloy nanomaterial by pulsed electrodeposition route was investigated. The alloy samples were deposited at different current densities from electrolytes of different compositions to study the influence of current density and bath composition on metal contents in the alloy, which was determined by ICP-OES analysis. The XRD studies were carried out to determine the structure of these samples. Magnetic characterization at room temperature and during heating was carried out to understand their magnetic behaviour and to confirm the inferences drawn from the XRD results. The XPS spectra proved the presence of Fe and Ag in the metallic form in the alloy samples. The FESEM and TEM micrographs were taken to view the surface morphology of the nanosized particles.

Characterization of 17-4PH stainless steel powders produced by supersonic gas atomization

NASA Astrophysics Data System (ADS)

Zhao, Xin-Ming; Xu, Jun; Zhu, Xue-Xin; Zhang, Shao-Ming; Zhao, Wen-Dong; Yuan, Guo-Liang

2012-01-01

17-4PH stainless steel powders were prepared using a supersonic nozzle in a close-coupled gas atomization system. The characteristics of powder particles were carried out by means of a laser particle size analyzer, scanning electron microscopy (SEM), and the X-ray diffraction (XRD) technique. The results show that the mass median particle diameter is about 19.15 μm. Three main types of surface microstructures are observed in the powders: well-developed dendrite, cellular, and cellular dendrite structure. The XRD measurements show that, as the particle size decreases, the amount of fcc phase gradually decreases and that of bcc phase increases. The cooling rate is inversely related to the particle size, i.e., it decreases with an increase in particle size.

Preparation and antibacterial effect of silver hydroxyapatite/titania nanocomposite thin film on titanium

NASA Astrophysics Data System (ADS)

Mo, Anchun; Liao, Juan; Xu, Wei; Xian, Suqin; Li, Yubao; Bai, Shi

2008-11-01

The composite which contains Ag + and nanosized hydroxyapatite with TiO 2 was deposited onto titanium by dipping method. The morphology, chemical components and structures of the thin film were characterized by XRD, scanning electronic microscope (SEM) and energy dispersive X-ray analysis (EDX). Staphylococcus aureus and Escherichia coli were utilized to test the antibacterial effect. XRD results demonstrated that the films have characteristic diffraction peaks of pure HA. EDX results showed that the deposited films consisted of Ca, P, Ti, O and Ag, all of which distribute uniformly. With regard to the antibacterial effect, 98% of S. aureus and more than 99% of E. coli were killed after 24 h incubation and pictures of SEM showed obviously fewer cells on the surface with coating.

The new insight into the structure-activity relation of Pd/CeO2-ZrO2-Nd2O3 catalysts by Raman, in situ DRIFTS and XRD Rietveld analysis.

PubMed

Yang, X; Yang, L; Lin, J; Zhou, R

2016-01-28

Pd/CeO2-ZrO2-Nd2O3 (CZN) catalysts with different CeO2/ZrO2 molar ratios were synthesized and have been characterized by multiple techniques, e.g. XRD in combination with Rietveld refinement, UV-Raman, XPS and in situ DRIFTS. The XRD pattern of CZN with CeO2/ZrO2 molar ratios ≥1/2 can be indexed satisfactorily to the fluorite structure with a space group Fm3̄m, while the XRD patterns of CZ12 only display diffraction peaks of the tetragonal phase (S.G. P42/nmc). Nd addition can effectively stabilize the cubic structure of the CZN support and increase the enrichment of defect sites on the surface, which may be related to the better catalytic activity of Pd/CZN12 catalysts compared with Pd/CZ12. The presence of moderate ZrO2 can increase the concentration of O* active species, leading to accelerate the formation of nitrate species and thus enhance the catalytic activity of NOx and HC elimination. The Pd-dispersion decreases with the increasing Zr content, leading to the decreased CO catalytic activity, especially for the aged catalysts. The change regularity of the OSC value is almost the same with the in situ dynamic operational window, demonstrating that the in situ dynamic operational window is basically affected by the OSC value.

Superhydrophobic alumina surface based on stearic acid modification

NASA Astrophysics Data System (ADS)

Feng, Libang; Zhang, Hongxia; Mao, Pengzhi; Wang, Yanping; Ge, Yang

2011-02-01

A novel superhydrophobic alumina surface is fabricated by grafting stearic acid layer onto the porous and roughened aluminum film. The chemical and phase structure, morphology, and the chemical state of the atoms at the superhydrophobic surface were investigated by techniques as FTIR, XRD, FE-SEM, and XPS, respectively. Results show that a super water-repellent surface with a contact angle of 154.2° is generated. The superhydrophobic alumina surface takes on an uneven flowerlike structure with many nanometer-scale hollows distribute in the nipple-shaped protrusions, and which is composed of boehmite crystal and γ-Al2O3. Furthermore, the roughened and porous alumina surface is coated with a layer of hydrophobic alkyl chains which come from stearic acid molecules. Therefore, both the roughened structure and the hydrophobic layer endue the alumina surface with the superhydrophobic behavior.

VERUCLAY – a new type of photo-adsorbent active in the visible light range: modification of montmorillonite surface with organic surfactant

EPA Science Inventory

Montmorillonite K10 was treated with VeruSOL-3, a biodegradable and food-grade surfactant mixture of coconut oil, castor oil and citrus extracts, to manufacture a benign catalytic adsorbent that is active in the visible light. Veruclay was characterized by SEM, XRD, TGA, UVDRS, a...

Calcination Conditions on the Properties of Porous TiO2 Film

NASA Astrophysics Data System (ADS)

Zhang, Wenjie; Pei, Xiaobei; Bai, Jiawei; He, Hongbo

2014-03-01

Porous TiO2 films were deposited on SiO2 precoated glass-slides by sol-gel method using PEG1000 as template. The strongest XRD diffraction peak at 2θ = 25.3° is attributed to [101] plane of anatase TiO2 in the film. The increases of calcination temperature and time lead to stronger diffraction peak intensity. High transmittance and blue shift of light absorption edge are the properties of the film prepared at high calcination temperature. The average pore size of the films increases with the increasing calcination temperature as the result of TiO2 crystalline particles growing up and aggregation, accompanied with higher specific surface area. Photocatalytic activity of porous TiO2 films increases with the increasing calcination temperature. The light absorption edge of the films slightly moves to longer wavelength region along with the increasing calcination time. The mesoporous film calcinated at 500 °C for 2 h has the highest transmittance, the maximum surface area, and the maximum total pore volume. Consequently, the optimum degradation activity is achieved on the porous TiO2 film calcinated at 500 °C for 2 h.

Quality engineering and control semiannual progress report, November--December 1977 and January--April 1978

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

Carpenter, R.L.

1978-10-10

Determination of ppM concentrations of dibutyl phosphate in aqueous solutions of nitric acid or sodium carbonate is possible after an extraction step with carbon tetrachloride. Ester cleavage of the fatty triglyceride constituents is the principal radiolytic reaction in irradiation of a dolphin-head oil base precision watch oil. Use of a special container and a vacuum-brazing furnace permits the high-temperature dynamic determination of volatile surface contamination from samples of large geometric surface areas. Status of the mass spectrometer development project is discussed. A mass spectroscopy method provided rapid, specific, and quantitative results for environmental monitoring of polychlorinated biphenyl compounds. A sequentialmore » procedure for improved separation of actinides in soil samples was developed. Testing of packings in intimate contact with acid was accomplished by differential thermal analysis. Analysis results obtained on the XRD-6 x-ray unit are discussed for Nb in U-Nb alloys and for Cr and Ne in stainless steels. Correlation coefficients of 0.994 or better resulted for the determinations of Cr, Mn, and Ne in the stainless steel standards employed in the statistical evaluation of the Quanta Metrix x-ray unit.« less

ZnO nanostructures with different morphology for enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Peter, I. John; Praveen, E.; Vignesh, G.; Nithiananthi, P.

2017-12-01

ZnO nanomaterials of different morphologies have been synthesized and the effect of morphology on Photocatalytic activity on natural dye has been investigated. Crystalline size and lattice strain of the synthesized particles are determined by XRD analysis and Williamson-Hall (W-H) method respectively. All other important physical parameters such as strain, stress and energy density values are also calculated using W-H analysis using different models such as uniform deformation model, uniform deformation stress model and uniform deformation energy density model. A shift in the peak of FTIR spectrum of ZnO is observed due to morphology effects. The SEM analysis reveals that the synthesized ZnO nanoparticles appear as flake, rod and dot. ZnO quantum dot exhibits higher photocatalytic activity comparing to the other morphologies. Larger surface area, high adsorption rate, large charge separation and the slow recombination of electrons/holes in ZnO dots establish dots as favorable morphology for good photocatalysis. Among the three, ZnO quantum dot shows three-times enhancement in the kinetic rate constants of photocatalysis. The results confirm that availability of specific (active) surface area, photocatalytic potential and quantum confinement of photo-induced carriers differ with morphology.

Surface molecularly imprinted polymer capped Mn-doped ZnS quantum dots as a phosphorescent nanosensor for detecting patulin in apple juice.

PubMed

Zhang, Wengang; Han, Yong; Chen, Xiumei; Luo, Xueli; Wang, Jianlong; Yue, Tianli; Li, Zhonghong

2017-10-01

A Mn-doped ZnS quantum dots (QDs) based nanosensor for selective phosphorescent determination of patulin (PAT) was synthesized with 6-hydroxynicotinic acid (6-HNA) as dummy template via a surface molecular imprinting sol-gel process. FTIR and XRD indicated the successful graft of molecularly imprinted polymer (MIP) onto crystal QDs. Binding tests revealed that the MIP-QDs presented higher selectivity, adsorption capacity and mass transfer rate than non-imprinted polymers, demonstrating a specific recognition for PAT among competitive mycotoxins and its analogues with the imprinting factor of 2.02. The MIP-QDs could recognize PAT in a linear range of 0.43-6.50μmolL -1 with a detection limit of 0.32μmolL -1 and a correlation coefficient (R 2 ) of 0.9945. Recoveries of 102.9-127.2% with relative standard deviations <4.95% were achieved in apple juice samples which were in good agreement with high-performance liquid chromatography (HPLC) (P>0.05). The results indicated a simple phosphorescent nanosensor for PAT detection in complex matrix. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characteristics of supported nano-TiO2/ZSM-5/silica gel (SNTZS): photocatalytic degradation of phenol.

PubMed

Zainudin, Nor Fauziah; Abdullah, Ahmad Zuhairi; Mohamed, Abdul Rahman

2010-02-15

Photocatalytic degradation of phenol was investigated using the supported nano-TiO(2)/ZSM-5/silica gel (SNTZS) as a photocatalyst in a batch reactor. The prepared photocatalyst was characterized using XRD, TEM, FT-IR and BET surface area analysis. The synthesized photocatalyst composition was developed using nano-TiO(2) as the photoactive component and zeolite (ZSM-5) as the adsorbents, all supported on silica gel using colloidal silica gel binder. The optimum formulation of SNTZS catalyst was observed to be (nano-TiO(2):ZSM-5:silica gel:colloidal silica gel=1:0.6:0.6:1) which giving about 90% degradation of 50mg/L phenol solution in 180 min. The SNTZS exhibited higher photocatalytic activity than that of the commercial Degussa P25 which only gave 67% degradation. Its high photocatalytic activity was due to its large specific surface area (275.7 m(2)/g), small particle size (8.1 nm), high crystalline quality of the synthesized catalyst and low electron-hole pairs recombination rate as ZSM-5 adsorbent was used. The SNTZS photocatalyst synthesized in this study also has been proven to have an excellent adhesion and reusability.

Nickel nanoparticle decorated graphene for highly selective isolation of polyhistidine-tagged proteins

NASA Astrophysics Data System (ADS)

Liu, Jia-Wei; Yang, Ting; Ma, Lin-Yu; Chen, Xu-Wei; Wang, Jian-Hua

2013-12-01

Nickel nanoparticle decorated graphene (GP-Ni) is prepared by one-pot hydrothermal reduction of graphene oxide and nickel cations by hydrazine hydrate in the presence of poly(sodium-p-styrenesulfonate) (PSS). The GP-Ni hybrid is characterized by XRD, TEM, SEM, XPS, Raman and FT-IR spectra, demonstrating the formation of poly-dispersed nickel nanoparticles with an average size of 83 nm attached on the surface of graphene sheets. The GP-Ni hybrid exhibits ferromagnetic behavior with a magnetization saturation of 31.1 emu g-1 at 10 000 Oersted (Oe). The GP-Ni also possesses favorable stability in aqueous medium and rapid magnetic response to an external magnetic field. These make it a novel magnetic adsorbent for the separation/isolation of His6-tagged recombinant proteins from a complex sample matrix (cell lysate). The targeted protein species is captured onto the surface of the GP-Ni hybrid via specific metal affinity force between polyhistidine groups and nickel nanoparticles. The SDS-PAGE assay indicates highly selective separation of His6-tagged Smt A from cell lysate. The GP-Ni hybrid displays favorable performance on the separation/isolation of His6-tagged recombinant proteins with respect to the commercial NTA-Ni2+ column.

PdNP Decoration of Halloysite Lumen via Selective Grafting of Ionic Liquid onto the Aluminol Surfaces and Catalytic Application.

PubMed

Dedzo, Gustave K; Ngnie, Gaëlle; Detellier, Christian

2016-02-01

The synthesis of selectively deposited palladium nanoparticles (PdNPs) inside tubular halloysite lumens is reported. This specific localization was directed by the selective modification of the aluminol surfaces of the clay mineral through stable Al-O-C bonds. An ionic liquid (1-(2-hydroxyethyl)-3-methylimidazolium) was grafted onto halloysite following the guest displacement method (generally used for kaolinite) using halloysite-DMSO preintercalate. The characterization of this clay nanohybrid material (XRD, NMR, TGA) showed characteristics reminiscent of similar materials synthesized from kaolinite. The grafting on halloysite lumens was also effective without using the DMSO preintercalate. The presence of these new functionalities in halloysite directs the synthesis of uniform PdNPs with size ranging between 3 and 6 nm located exclusively in the lumens. This results from the selective adsorption of PdNPs precursors in functionalized lumens through an anion exchange mechanism followed by in situ reduction. In contrast, the unmodified clay mineral displayed nanoparticles both inside and outside the tubes. These catalysts showed significant catalytic activity for the reduction of 4-nitrophenol (4-NP). The most efficient catalysts were recycled up to three times without reducing significantly the catalytic activities.

Controlled release and long-term antibacterial activity of reduced graphene oxide/quaternary ammonium salt nanocomposites prepared by non-covalent modification.

PubMed

Ye, Xiaoli; Feng, Jin; Zhang, Jingxian; Yang, Xiujiang; Liao, Xiaoyan; Shi, Qingshan; Tan, Shaozao

2017-01-01

In order to control the long-term antibacterial property of quaternary ammonium salts, dodecyl dimethyl benzyl ammonium chloride (rGO-1227) and rGO-bromohexadecyl pyridine (rGO-CPB) were self-assembled on surfaces of reduced graphene oxide (rGO) via π-π interactions. The obtained rGO-1227 and rGO-CPB nanocompounds were characterized by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM).The antibacterial activities were evaluated on Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus. Both rGO-CPB and rGO-1227 reduced the cytotoxicity of the pure antimicrobial agents and presented strong antimicrobial properties. Especially, CPB could be loaded efficiently on the surface of rGO via π-π conjugate effect, which resulted in a nanocomposite presenting a long-term antibacterial capability due to the more important quantity of free π electrons compared to that of 1227. When comparing the advantages of both prepared nanocomposites, rGO-CPB displayed a better specific-targeting capability and a longer-term antibacterial property. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation and Characterization of Impregnated Commercial Rice Husks Activated Carbon with Piperazine for Carbon Dioxide (CO2) Capture

NASA Astrophysics Data System (ADS)

Masoum Raman, S. N.; Ismail, N. A.; Jamari, S. S.

2017-06-01

Development of effective materials for carbon dioxide (CO2) capture technology is a fundamental importance to reduce CO2 emissions. This work establishes the addition of amine functional group on the surface of activated carbon to further improve the adsorption capacity of CO2. Rice husks activated carbon were modified using wet impregnation method by introducing piperazine onto the activated carbon surfaces at different concentrations and mixture ratios. These modified activated carbons were characterized by using X-Ray Diffraction (XRD), Brunauer, Emmett and Teller (BET), Fourier Transform Infrared Spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). The results from XRD analysis show the presence of polyethylene butane at diffraction angles of 21.8° and 36.2° for modified activated carbon with increasing intensity corresponding to increase in piperazine concentration. BET results found the surface area and pore volume of non-impregnated activated carbon to be 126.69 m2/g and 0.081 cm3/g respectively, while the modified activated carbons with 4M of piperazine have lower surface area and pore volume which is 6.77 m2/g and 0.015 cm3/g respectively. At 10M concentration, the surface area and pore volume are the lowest which is 4.48 m2/g and 0.0065 cm3/g respectively. These results indicate the piperazine being filled inside the activated carbon pores thus, lowering the surface area and pore volume of the activated carbon. From the FTIR analysis, the presence of peaks at 3312 cm-1 and 1636 cm-1 proved the existence of reaction between carboxyl groups on the activated carbon surfaces with piperazine. The surface morphology of activated carbon can be clearly seen through FESEM analysis. The modified activated carbon contains fewer pores than non-modified activated carbon as the pores have been covered with piperazine.

A novel approach to enhancement of surface properties of CdO films by using surfactant: dextrin

NASA Astrophysics Data System (ADS)

Sahin, Bünyamin; Bayansal, Fatih; Yüksel, Mustafa

2015-12-01

We studied the effect of an organic surfactant, dextrin, concentration on structural, morphological and optical properties of nanostructured CdO films deposited on glass substrates by using an easy and low-cost SILAR method. Microstructures of the nanostructured CdO films were optimized by adjusting dextrin concentration. XRD, SEM and UV-Vis Spectroscopy were used to study phase structure, surface morphology and optical properties of CdO films. Furthermore, effects of dextrin concentration on the surface roughness characteristics of CdO samples were reported. The results showed that the presence of organic surfactant highly affected the physical properties of CdO nanomaterials.

Label-free immunosensor based on hyperbranched polyester for specific detection of α-fetoprotein.

PubMed

Niu, Yanlian; Yang, Tian; Ma, Shangshang; Peng, Fang; Yi, Meihui; Wan, Mimi; Mao, Chun; Shen, Jian

2017-06-15

A novel label-free immunosensor based on hyperbranched polyester nanoparticles with nitrite groups (HBPE-NO 2 ), which were synthesized through a simple one-step chemical reaction, was first developed for specific detection of α-fetoprotein (AFP), the tumor marker for liver cancer. The obtained HBPE-NO 2 nanoparticles (NPs) were characterized by the proton nuclear magnetic resonance spectroscopy ( 1 H NMR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). And the fabricated process of immunosensor was investigated by attenuated total reflection Fourier-transform infrared spectra (ATR-FTIR), static water contact angles, scanning electron microscope (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The electrochemical performances of the AFP immunosensor were studied. Results indicated the prepared HBPE-NO 2 -modified immunosensor showed excellent electrochemical properties and satisfactory accuracy for the detection of AFP of the real clinical samples that attributed to the properties of the HBPE-NO 2 NPs, which had nanosized structure to increase the specific surface area and unique chemical reactivity for loading capacity of protein molecules. Construction of biosensors using the structure and properties of hyperbranched molecules will offer ideal electrode substrates, which provided more possibilities for the design of biosensor. Copyright © 2017 Elsevier B.V. All rights reserved.

X-Ray Diffraction Reference Intensity Ratios of Amorphous and Poorly Crystalline Phases: Implications for CheMin on the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Morris, R. V.; Achilles, C. N.; Chipera, S. J.; Ming, D. W.; Rampe, E. B.

2013-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. Piezoelectric vibration of the cell is used to randomize the sample to reduce preferred orientation effects. Instrument details are provided in [1, 2, 3]. Analyses of rock and soil samples by the Mars Exploration Rovers (MER) show nanophase ferric oxide (npOx) is a significant component of the Martian global soil [4] and is thought to be one of the major contributing phases that the Curiosity rover will encounter if a soil sample is analyzed in Gale Crater. Because of the nature of this material, npOx will likely contribute to an X-ray amorphous or short-order component of a XRD pattern measured by the CheMin instrument.

Radiation-induced changes in electrical conductivity and structure of BaPbO3 after γ-irradiation

NASA Astrophysics Data System (ADS)

Shan, Qing; Cai, Pingkun; Zhang, Xinlei; Li, Jiatong; Chu, Shengnan; Jia, Wenbao

2015-11-01

Several barium plumbate (BaPbO3) solid samples, made from PbO and BaCO3 powder by chemistry liquid-phase coprecipitation, were investigated before and after γ-irradiation. The solid samples were irradiated by a 60Co γ-irradiation source whose dose rate is about 0.7 kGy per hour. The irradiation times were 0, 72, 144, 216, 288 and 360 h. Then, the four-probe method, X-ray diffraction (XRD), scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS) were used to indicate the changes in electrical conductivity and microstructure of BaPbO3 after γ-irradiation. The XRD results indicated that the content of PbO was reduced as the irradiation dose was increased and eventually vanished from the surface of samples. However, there was no new obvious substance phase found from the XRD atlas. It seems that the PbO transformed into nearly amorphous Pb5O8. The conjecture could be proved by the results of annealing experiment and SEM. The XPS results seem to show that the microstructure of BaPbO3 was slightly changed.

Cobalt ferrite nano-composite coated on glass by Doctor Blade method for photo-catalytic degradation of an azo textile dye Reactive Red 4: XRD, FESEM and DRS investigations.

PubMed

Habibi, Mohammad Hossein; Parhizkar, Janan

2015-11-05

Cobalt ferrite nano-composite was prepared by hydrothermal route using cobalt nitrate, iron nitrate and ethylene glycol as chelating agent. The nano-composite was coated on glass by Doctor Blade method and annealed at 300 °C. The structural, optical, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV-visible spectroscopy (UV-Vis DRS). Powder XRD analysis confirmed formation of CoFe2O4 spinel phase. The estimated particle size from FESEM data was 50 nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra was 1.3 eV. Photocatalytic degradation of Reactive Red 4 as an azo textile was investigated in aqueous solution under irradiation showed 68.0% degradation of the dye within 100 min. The experimental enhanced activity compare to pure Fe2O3 can be ascribed to the formation of composite, which was mainly attributable to the transfer of electron and hole to the surface of composite and hinder the electron hole recombination. Copyright © 2015 Elsevier B.V. All rights reserved.

X-ray characterization of indium during melting

NASA Astrophysics Data System (ADS)

Gondi, P.; Montanari, R.; Costanza, G.

During melting of Indium the structure of solid and liquid phases have been investigated by X-ray diffractometry (XRD) in 1-g conditions. At the melting point T M a re-orientation of crystalline grains occurs in the solid phase. The texture change, unusually rapid for a thermally activated process, is attributed to an abnormal increase of vacancy concentration. This explanation is in agreement with the observed shifts of XRD peaks towards lower angles. As a consequence of the texture change, the lattice planes facing the first formed liquid are (002) and (101) planes, i.e. those planes allocating 1st and 2nd neighbours around a given atom with shell radii very close to the mean distance of nearest neighbours in liquid as obtained from the radial distribution function (RDF). Convective motions in the liquid can be eliminated by repeating the same XRD measurements in μ-g. To get the best experimental conditions it is discussed the possibility to use thin oxide films grown on the external surface of samples as containers during melting. This technique was already successfully tested by present investigators in the experiment ES 311 A-B carried out during the mission SPACELAB-1.

Improve electrochemical performance of CeO2 surface modification LiNi0.80Co0.15Al0.05O2 cathode material

NASA Astrophysics Data System (ADS)

Xia, Shubiao; Zhang, Yingjie; Dong, Peng; Zhang, Yannan

2014-06-01

Lithium ion battery cathode material LiNi0.8Co0.15Al0.05O2 cathode has successfully prepared by co-precipitation. CeO2 surface modification has improved LiNi0.80Co0.15Al0.05O2 electrochemical performance use sol-gel method and subsequent heat treatment at 600 °C for 5 h. Different to other conventional coating material, CeO2 coating layer can not only inhibit the reaction of the electrode and the electrolyte, but also can reduce the impedance of electron transfer due to its high conductivity, and inhibit the production of Ni2+ because of its high oxidation. The surface-modified and pristine LiNi0.80Co0.15Al0.05O2 powders are characterized by XRD, SEM, TEM, XPS, CV and DSC. When CeO2 coating is 0.02% (mole ratio), contrast to pristine NCA, the CeO2-coated NCA cathode exhibits no decrease in its initial specific capacity of 184 mAh g -1 (at 0.2 C) and excellent capacity retention (86% of its initial capacity at 1 C) between 2.75 and 4.3 V after 100 cycles. The results indicate that the CeO2 surface treatment should be an effective way to improve cycle properties due to CeO2 inhibit the electrodes and the electrolyte side effects.

Pseudocapacitive performance of electrodeposited porous Co3O4 film on electrophoretically modified graphite electrodes with carbon nanotubes

NASA Astrophysics Data System (ADS)

Kazazi, Mahdi; Sedighi, Ali Reza; Mokhtari, Mohammad Amin

2018-05-01

A facile and efficient two-step procedure was developed for the fabrication of a high-performance and binder-free cobalt oxide-carbon nanotubes (CO/CNT) pseudocapacitive electrode. First, CNTs were deposited on the surface of a chemically activated graphite sheet by cathodic electrophoretic deposition technique from their ethanolic suspension. In the next step, a thin film of cobalt oxide was electrodeposited on the CNTs coated graphite substrate by a galvanostatic method, followed by a thermal treatment in air. The structure and morphology of the prepared cobaltite electrode with and without CNT interlayer were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and nitrogen adsorption-desorption measurement. The results indicated that Co3O4 nanoparticles were uniformly attached on the surface of CNTs, to form a porous-structured CO/CNT composite electrode with a high specific surface area of 144.9 m2 g-1. Owing to the superior electrical conductivity of CNTs, high surface area and open porous structure, and improved integrity of the electrode structure, the composite electrode delivered a high areal capacitance of 4.96F cm-2 at a current density of 2 mA cm-2, a superior rate performance (64.7% capacitance retention from 2 mA cm-2 to 50 mA cm-2), as well as excellent cycling stability (91.8% capacitance retention after 2000 cycles), which are higher than those of the pure cobaltite electrode.

Pyrite Stability Under Venus Surface Conditions

NASA Astrophysics Data System (ADS)

Kohler, E.; Craig, P.; Port, S.; Chevrier, V.; Johnson, N.

2015-12-01

Radar mapping of the surface of Venus shows areas of high reflectivity in the Venusian highlands, increasing to 0.35 ± 0.04 to 0.43 ± 0.05 in the highlands from the planetary average of 0.14 ± 0.03. Iron sulfides, specifically pyrite (FeS2), can explain the observed high reflectivity. However, several studies suggest that pyrite is not stable under Venusian conditions and is destroyed on geologic timescales. To test the stability of pyrite on the Venusian surface, pyrite was heated in the Venus simulation chamber at NASA Goddard Space Flight Center to average Venusian surface conditions, and separately to highland conditions under an atmosphere of pure CO2 and separately under an atmosphere of 96.5% CO2, 3.5% N2 and 150 ppm SO2. After each run, the samples were weighed and analyzed using X-Ray Diffraction (XRD) to identify possible phase changes and determine the stability of pyrite under Venusian surface conditions. Under a pure CO2 atmosphere, the Fe in pyrite oxidizes to form hematite which is more stable at higher temperatures corresponding to the Venusian lowlands. Magnetite is the primary iron oxide that forms at lower temperatures corresponding to the radar-bright highlands. Our experiments also showed that the presence of atmospheric SO2 inhibits the oxidation of pyrite, increasing its stability under Venusian conditions, especially those corresponding to the highlands. This indicates that the relatively high level of SO2 in the Venusian atmosphere is key to the stability of pyrite, making it a possible candidate for the bright radar signal in the Venusian highlands.

Natural fiber templated TiO2 microtubes via a double soaking sol-gel route and their photocatalytic performance

NASA Astrophysics Data System (ADS)

Yang, Li; Li, Xu; Wang, Ziru; Shen, Yun; Liu, Ming

2017-10-01

TiO2 microtubes with a yam-like surface were prepared for the first time through a simple and efficient double soaking sol-gel route by utilizing Platanus acerifolia seed fibers as bio-templates. The physicochemical properties of the samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), Brunauer Emmett Teller (BET) surface analysis and Ultraviolet-visible absorption spectroscopy (UV-vis). The results showed that the obtained TiO2 microtubes had an anatase phase and were composed of a smooth internal wall and a rough yam-like external wall with an average diameter of 24 μm and the wall thickness of 2 μm. The surface area and pore volume of the as-prepared TiO2 microtubes reached 128.271 m2/g and 0.149 cm3/g, respectively. The UV-vis analysis displayed a favorable extension of light absorption capacity of TiO2 microtubes. The synthetic mechanism was preliminarily discussed as well. The moisture in the natural fiber templates facilitated the mild hydrolysis of titanium sol, leaving a prime layer on the surface of the fibers, and subsequently assisted in the successful preparation of TiO2 microtubes with a yam-like surface without requiring specific control of hydrolysis. Photocatalytic experiments indicated that the as-obtained TiO2 microtubes exhibited a higher efficiency than commercial P25 in the degradation of tetracycline hydrochloride.

Mg-Doped Hydroxyapatite/Chitosan Composite Coated 316L Stainless Steel Implants for Biomedical Applications.

PubMed

Sutha, S; Dhineshbabu, N R; Prabhu, M; Rajendran, V

2015-06-01

In this investigation, ultrasonication process was used for the synthesis of magnesium doped nano-hydroxyapatite (MH) (0, 1, 2, and 3 mol% of Mg concentration) particles with controlled size and surface morphology. The size of the prepared MH particles was in the range of 20-100 nm with narrow distribution. Increase in the concentration of Mg reduced the particle size distribution from 60 to 40 nm. On incorporation of Mg in HAp lattice, an increase of 20-66 nm in specific surface area was observed in microporous HAp particles. XRF and XRD patterns reveal that the particles possess stoichiometric composition with reduced crystallinity with respect to the Mg concentration. Surface morphology of MH/chitosan (CTS) coated implant was found to be uniform without any defects. The corrosion rate of the implant decreased with increase in Mg concentration. The in vitro formation of bonelike apatite layer on the surface of the MH/CTS coated implant was observed from simulated body fluid studies. The antimicrobial activity of the MH/CTS composites against gram-positive and gram-negative bacterial strains indicated that increasing Mg concentration enhanced antimicrobial properties. Nanoindentation analysis of apatite coated implant surface reveals that the mechanical property depends on the concentration of magnesium in HAp. From the cytotoxicity analysis against NIH 3T3 fibroblast, it was observed that the Mg incorporated HAp/CTS composite was less toxic than the MHO/CTS composite. From this result, it was concluded that the MH/CTS nanocomposites coated implant is the excellent material for implants.

Growth and microtopographic study of CuInSe{sub 2} single crystals

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

Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P.

2016-05-23

The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

Laser Surface Hardening of Groove Edges

NASA Astrophysics Data System (ADS)

Hussain, A.; Hamdani, A. H.; Akhter, R.; Aslam, M.

2013-06-01

Surface hardening of groove-edges made of 3Cr13 Stainless Steel has been carried out using 500 W CO2 laser with a rectangular beam of 2.5×3 mm2. The processing speed was varied from 150-500 mm/min. It was seen that the hardened depth increases with increase in laser interaction time. A maximum hardened depth of around 1mm was achieved. The microhardness of the transformed zone was 2.5 times the hardness of base metal. The XRD's and microstructural analysis were also reported.

Composition and structure of pyrophoric nickel catalysts according to X-ray diffraction data

NASA Astrophysics Data System (ADS)

Osadchaya, T. Yu.; Afineevskii, A. V.; Prozorov, D. A.; Kochetkov, S. P.; Rumyantsev, R. N.; Lukin, M. V.

2017-01-01

The properties of a nickel catalyst obtained by treatment of nickel-aluminum alloy with sodium hydroxide in the presence of H2O2 and additionally stabilized with increased pressure were studied. Additional stabilization decreased the catalyst activity by 25%, but gave a more distinct picture for an XRD analysis of the active catalyst surface and decreased the time of deactivation of the dehydrated catalyst with air oxygen. The catalyst stabilization was explained by the displacement of water, decrease in the pore size, and surface inhomogeneity.

Surface acid-base properties and hydration/dehydration mechanisms of aluminum (hydr)oxides.

PubMed

Yang, Xiaofang; Sun, Zhongxi; Wang, Dongsheng; Forsling, Willis

2007-04-15

In this paper, surface physiochemical properties of three typical aluminas, gamma-Al(OH)3, gamma-Al2O3, and alpha-Al2O3, were investigated by means of XRD, SEM, TEM, BET surface area, TG/DTA, and potentiometric titration techniques. Based on the titration data, surface protonation and deprotonation constants were determined using the constant capacitance model (CCM). The emphasis of this research was laid on the comparison of the crystal structure, surface hydration/dehydration and acid-base properties of these three typical alumina minerals. The calculation results revealed that the surface acidity of the aluminas is in the order of alpha-Al2O3>gamma-Al(OH)3>gamma-Al2O3 after being hydrated for 1 h. The correlation between the hydration/dehydration mechanisms of alumina and its acid/base properties is discussed.

In vitro characterisation of a sol-gel derived in situ silica-coated silicate and carbonate co-doped hydroxyapatite nanopowder for bone grafting.

PubMed

Latifi, Seyed Mohsen; Fathi, Mohammadhossein; Sharifnabi, Ali; Varshosaz, Jaleh

2017-06-01

Design and synthesis of materials with better properties and performance are essential requirements in the field of biomaterials science that would directly improve patient quality of life. For this purpose, in situ silica-coated silicate and carbonate co-doped hydroxyapatite (Sc/S.C.HA) nanopowder was synthesized via the sol-gel method. Characterisation of the prepared nanopowder was carried out by XRD, FTIR, TEM, SEM, EDX, ICP, zeta potential, acid dissolution test, and cell culture test. The substitution of the silicate and carbonate ions into hydroxyapatite structure was confirmed by FTIR analysis. XRD analysis showed that silica is an amorphous phase, which played a role in covering the surface of the S.C.HA nanoparticles as confirmed by acid dissolution test. Low thickness and low integrity of the amorphous silica surface layer facilitated ions release from S.C.HA nanoparticles into physiological saline solution. Zeta potential of the prepared nanopowder suspended in physiological saline solution was -27.3±0.2mV at pH7.4. This negatively charged surface, due to the presence of amorphous silica layer upon the S.C.HA nanoparticles, not only had an accelerating effect on in vitro biomineralization of apatite, but also had a positive effect on cell attachment. Copyright © 2017 Elsevier B.V. All rights reserved.

Treatments to induce the nucleation and growth of apatite-like layers on polymeric surfaces and foams.

PubMed

Reis, R L; Cunha, A M; Fernandes, M H; Correia, R N

1997-12-01

In this work, a bioactive glass is used as a percusor of calcium-phosphate (Ca-P) film deposition onto several polymer-based materials. Both bioinert (high molecular weight polyethylene, HMWPE), and biodegradable (corn starch-based blends, SEVA-C) polymers, unreinforced or reinforced with hydroxylapatite (HA), were coated by the very simple proposed route. Also polyurethane (PU) foams, with an open-cell structure, were mineralized by the proposed method. In fact, it was possible to induce the growth of the Ca-P films not only at the surface, but also in the bulk of the PU foam. These cellular materials are intended for cancellous bone replacement applications. The morphology of the formed films was strongly dependent on the used substrate, its polar character, and on the presence of HA in its composition, as observed by SEM. Nevertheless, a well defined needly like structure was observed in all samples at high magnifications. The Ca:P ratios of the films were between 1.5 and 1.7, i.e. in the range of tricalcium phosphate-hydroxylapatite. Raman spectroscopy and thin-film x-ray diffraction (XRD) evidenced the formation of mostly amorphous calcium-phosphate films. After scraping the coating from the polymer surface and heat-treating the resulting powder at 1000 degrees C for 1 h, HA and beta-tricalcium phosphate (TCP) typical peaks were found on XRD patterns.

Differentiations of Chitin Content and Surface Morphologies of Chitins Extracted from Male and Female Grasshopper Species

PubMed Central

Kaya, Murat; Lelešius, Evaldas; Nagrockaitė, Radvilė; Sargin, Idris; Arslan, Gulsin; Mol, Abbas; Baran, Talat; Can, Esra; Bitim, Betul

2015-01-01

In this study, we used Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TGA), X-ray diffractometry (XRD), and scanning electron microscopy (SEM) to investigate chitin structure isolated from both sexes of four grasshopper species. FT-IR, EA, XRD, and TGA showed that the chitin was in the alpha form. With respect to gender, two main differences were observed. First, we observed that the quantity of chitin was greater in males than in females and the dry weight of chitin between species ranged from 4.71% to 11.84%. Second, using SEM, we observed that the male chitin surface structure contained 25 – 90nm wide nanofibers and 90 – 250 nm nanopores, while no pores or nanofibers were observed in the chitin surface structure of the majority of females (nanofibers were observed only in M. desertus females). In contrast, the elemental analysis, thermal properties, and crystalline index values for chitin were similar in males and females. Also, we carried out enzymatic digestion of the isolated chitins using commercial chitinase from Streptomyces griseus. We observed that there were no big differences in digestion rate of the chitins from both sexes and commercial chitin. The digestion rates were for grasshoppers’ chitins; 88.45–95.48% and for commercial chitin; 94.95%. PMID:25635814

Effect of thickness on surface morphology, optical and humidity sensing properties of RF magnetron sputtered CCTO thin films

NASA Astrophysics Data System (ADS)

Ahmadipour, Mohsen; Ain, Mohd Fadzil; Ahmad, Zainal Arifin

2016-11-01

In this study, calcium copper titanate (CCTO) thin films were deposited on ITO substrates successfully by radio frequency (RF) magnetron sputtering method in argon atmosphere. The CCTO thin films present a polycrystalline, uniform and porous structure. The surface morphology, optical and humidity sensing properties of the synthesized CCTO thin films have been studied by X-ray diffraction (XRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), UV-vis spectrophotometer and current-voltage (I-V) analysis. XRD and AFM confirmed that the intensity of peaks and pore size of CCTO thin films were enhanced by increasing the thin films. Tauc plot method was adopted to estimate the optical band gaps. The surface structure and energy band gaps of the deposited films were affected by film thickness. Energy band gap of the layers were 3.76 eV, 3.68 eV and 3.5 eV for 200 nm, 400 nm, and 600 nm CCTO thin films layer, respectively. The humidity sensing properties were measured by using direct current (DC) analysis method. The response times were 12 s, 22 s, and 35 s while the recovery times were 500 s, 600 s, and 650 s for 200 nm, 400 nm, and 600 nm CCTO thin films, respectively at humidity range of 30-90% relative humidity (RH).

Graphene oxide coated with porous iron oxide ribbons for 2, 4-Dichlorophenoxyacetic acid (2,4-D) removal.

PubMed

Nethaji, S; Sivasamy, A

2017-04-01

Graphene oxide (GO) was prepared from commercially available graphite powder. Porous iron oxide ribbons were grown on the surface of GO by solvothermal process. The prepared GO-Fe 3 O 4 nanocomposites are characterized by FT-IR, XRD, VSM, SEM, TEM, Raman spectroscopy, surface functionality and zero point charge studies. The morphology of the iron oxide ribbons grown on GO is demonstrated with TEM at various magnifications. The presence of magnetite nanoparticles is evident from XRD peaks and the magnetization value is found to be 37.28emu/g. The ratio of intensity of D-peak to G-peak from Raman spectrum is 0.995. The synthesized Graphene oxide-Fe 3 O 4 nanocomposites (GO-Fe 3 O 4 ) were explored for its surface adsorptive properties by using a model organic compound, 2,4-Dichlorophenoxy acetic acid (2,4-D) from aqueous solution. Batch adsorption studies were performed and the equilibrium data are modelled with Langmuir, Freundlich and Temkin isotherms. The maximum monolayer capacity from Langmuir isotherm is 67.26mg/g. Kinetic studies were also carried out and the studied adsorption process followed pseudo second-order rate equation. Mechanism of the adsorption process is studied by fitting the data with intraparticle diffusion model and Boyd plot. The studied adsorption process is both by film diffusion and intraparticle diffusion. Copyright © 2017 Elsevier Inc. All rights reserved.

In situ soft XAS study on nickel-based layered cathode material at elevated temperatures: A novel approach to study thermal stability

DOE PAGES

Yoon, Won -Sub; Yang, Xiao -Qing; Haas, Otto; ...

2014-10-29

Tracking thermally induced reactions has always been challenging for electrode materials of electrochemical battery systems. Traditionally, a variety of calorimetric techniques and in situ XRD at elevated temperatures has been used to evaluate the thermal stability of electrode materials. These techniques are capable of providing variations in heat capacity, mass and average bulk composition of materials only. Herein, we report investigation of thermal characteristics of Li 0.33Ni 0.8Co 0.15Al 0.05O 2 by using in situ soft XAS measurements in combination with XRD. Fluorescence yield and partial electron yield measurements are used simultaneously to obtain element selective surface and bulk information.more » Fluorescence yield measurements reveal no energy change of the absorption peak and thus no valence state change in the bulk. However, electron yield measurements indicate that NiO-type rock salt structure is formed at the surface at temperatures above 200°C while no evidence for a surface reaction near Co sites in investigated temperature range is found. These results clearly show that in situ soft XAS can give a unique understanding of the role of each element in the structural transformation under thermal abuse offering a useful guidance in developing new battery system with improved safety performance.« less

Electrodeposition of Zn-doped α-nickel hydroxide with flower-like nanostructure for supercapacitors

NASA Astrophysics Data System (ADS)

You, Zheng; Shen, Kui; Wu, Zhicheng; Wang, Xiaofeng; Kong, Xianghua

2012-08-01

Zn-doped α-nickel hydroxide materials with flower-like nanostructures are synthesized by electrochemical deposition method. The samples are characterized by X-ray diffraction (XRD), field emission scanning electron microscope (SEM) and electrochemical measurements. XRD spectra indicate nickel hydroxide doped with Zn is α-Ni(OH)2 with excellent crystallization. The SEM observation shows that the formation of Zn-doped Ni(OH)2 includes two steps: a honeycomb-like film forms on the substrate first, then flower-like particles forms on the films. The nickel hydroxide doped with 5% Zn can maintain a maximum specific capacitance of 860 F g-1, suggesting its potential application in electrochemical capacitors.

Identification of Breast Cancer-Associated Lipids in Scalp Hair

PubMed Central

Mistry, Dharmica A.H.; Haklani, Joseph; French, Peter W.

2012-01-01

A correlation between the presence of breast cancer and a change in the synchrotron-generated X-ray diffraction (XRD) pattern of hair has been reported in several publications by different groups, and on average XRD-based assays detect around 75% of breast cancer patients in blinded studies. To date, the molecular mechanisms leading to this alteration are largely unknown. We have determined that the alteration is likely to be due to the presence of one or more breast cancer-associated phospholipids. Further characterization of these lipids could be used to develop a novel, sensitive and specific screening test for breast cancer, based on hair initially, and potentially extendable to other biological samples. PMID:22872787

Biomass derived hierarchically porous and heteroatom-doped carbons for supercapacitors.

PubMed

Kang, Xiaonan; Zhu, Hui; Wang, Chuanyi; Sun, Kang; Yin, Jiao

2018-01-01

In this research, Rapeseed dregs (RDs), as a byproduct of agriculture (derived from processing of rapeseed for oil production), were originally employed asa new carbonaceous precursor to synthesize hierarchically porous and heteroatom-doped activated carbons (ACs) with the activation of ZnCl 2 at various high temperatures. A variety of measurements have been adopted to systemically characterize the RD-derived ACs. The micro-morphology, pore structures and surface chemistry property were fully investigated by SEM, TEM, XRD, Raman, N 2 adsorption-desorption analysis, XPS and IR, respectively. The RD-derived ACs possess as large specific surface area as up to 1416.966m 2 g -1 and the pore size distribution concentrates on 1-2, 2-5, 5-15 and 25-35nm, indicating their hierarchically porous structures. Furthermore, electrochemical measurements including electrochemical impedance spectroscopy (EIS), galvanostatic charge/discharge (GCD) and cyclic voltammetry (CV) were conducted to estimate RDAC's supercapacitive performance and rate capability. The investigations illustrated that RD derived ACs reached as high specific capacitance as 170.5 and 153.2Fg -1 at a scan rate of 5mVs -1 in 1M H 2 SO 4 and 1M Et 4 NBF 4 /AN, respectively. In addition, the RD-derived ACs demonstrated good long-term cycling stability and more than 90% initial capacity have been retained after 6400 cycles at a large current density of 1Ag -1 . Copyright © 2017 Elsevier Inc. All rights reserved.

N-enriched multilayered porous carbon derived from natural casings for high-performance supercapacitors

NASA Astrophysics Data System (ADS)

Xu, Zongying; Li, Yu; Li, Dandan; Wang, Dawei; Zhao, Jing; Wang, Zhifeng; Banis, Mohammad N.; Hu, Yongfeng; Zhang, Huaihao

2018-06-01

In this study, N-enriched multilayered porous activated carbon (LPAC), using natural casings as precursor, was fabricated by a facile carbonization and subsequent KOH activation procedure. The influence of the mass ratio of KOH to carbonized material on pore-structure and surface element composition of LPACs was investigated by a variety of means, such as SEM, HRTEM, BET, Raman, XRD, XPS and XAS. Owing to the unique multilayered texture and nitrogen (N) and oxygen (O) rich feature of natural casings, the resulting LPACs possess interconnected and developed porous structure with N- and O-enriched functional groups, contributing to larger pseudocapacitance. With the rise of mass ratio, the specific surface area (SSA) and average pore size of LPACs increased. The final materials were endowed with a desirable SSA (3100 m2 g-1) and high N content (6.34 at.%). Meanwhile, N- and O-enriched LPAC-4 exhibited a high specific capacitance (307.5 F g-1 at a current density of 0.5 A g-1 in 6 M KOH aqueous solution), excellent rate performance (63.4% capacitance retention at 20 A g-1) and good cycling stability (7.1% capacitance loss after 5000 cycles). Furthermore, the assembled symmetrical supercapacitor (LPAC-4//LPAC-4) with a wide voltage window of 1.4 V delivered a remarkable energy density of 11.6 Wh kg-1 at a power density of 297 W kg-1. These results suggested that unique LPACs derived from natural casings are a promising material for supercapacitors.

Effect of Gold on the Corrosion Behavior of an Electroless Nickel/Immersion Gold Surface Finish

NASA Astrophysics Data System (ADS)

Bui, Q. V.; Nam, N. D.; Yoon, J. W.; Choi, D. H.; Kar, A.; Kim, J. G.; Jung, S. B.

2011-09-01

The performance of surface finishes as a function of the pH of the utilized plating solution was evaluated by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in 3.5 wt.% NaCl solution. In addition, the surface finishes were examined by x-ray diffraction (XRD), and the contact angle of the liquid/solid interface was recorded. NiP films on copper substrates with gold coatings exhibited their highest coating performance at pH 5. This was attributed to the films having the highest protective efficiency and charge transfer resistance, lowest porosity value, and highest contact angle among those examined as a result of the strongly preferred Au(111) orientation and the improved surface wettability.

Effect of Ultrasonic Surface Treatment on the Transparency and Orientation of Fresnoite Surface Crystallization

NASA Astrophysics Data System (ADS)

Endo, A.; Sakida, S.; Benino, Y.; Nanba, T.

2011-10-01

Surface crystallized glass ceramics with fresnoite (Ba2TiSi2O8) phase were prepared by conventional heat treatment of 30BaO-20TiO2-50SiO2 glass together with ultrasonic surface treatment (UST) technique. The precursor glass was fully crystallized in a bulk form without any cracks, and the optical transparency and crystallographic orientation of the crystalline layers were evaluated by UV-Vis spectroscopy and XRD diffraction analyses, respectively. These properties were both enhanced significantly by applying UST using fresnoite/water suspension before the crystallization process, which is advantage for nonlinear optical applications of bulk glass ceramics. The effects of UST on the crystallization behavior were investigated by applying UST with various conditions.

Surface modification of boron nitride nanosheets by polyelectrolytes via atom transfer radical polymerization

NASA Astrophysics Data System (ADS)

Wu, Yuanpeng; Guo, Meiling; Liu, Guanfei; Xue, Shishan; Xia, Yuanmeng; Liu, Dan; Lei, Weiwei

2018-04-01

In this study, the surface modification of boron nitride nanosheets (BNNSs) with poly 2-acrylamido-2-methyl- propanesulfonate (PAMPS) brushes is achieved through electron transfer atom transfer radical polymerization (ARGET ATRP). BNNSs surface was first modified with α-bromoisobutyryl bromide (BIBB) via hydroxyl groups, then PAMPS brushes were grown on the surface through ARGET ATRP. Polyelectrolyte brushes modified BNNSs were further characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analyses (TGA), x-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The concentraction of water-dispersion of BNNSs have been enhanced significantly by PAMPS and the high water-dispersible functional BNNSs/PAMPS composites are expected to have potential applications in biomedical and thermal management in electronics.

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

NASA Astrophysics Data System (ADS)

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

2012-10-01

In this study, nano-silver (nano-Ag) complexes showing different properties have been synthesized as follows. Polypyrrolidone (PVP)-stabilized silver colloids (NAg), nano-Ag bound to silica (SiO2) (NSS), and nano-Ag bound to a complex of SiO2 and polyaniline (PANI) (NSSPAI) were prepared via γ-irradiation at room temperature. NAg and NSS used PVP as a colloidal stabilizer, while NSSPAI did not use PVP as a colloidal stabilizer. Interesting bonding properties occurred in the nano-Ag complex and anticipated structural changes were clearly shown through a surface analysis of x-ray photoelectron spectroscopy (XPS). The morphologies by field emission-scanning electron microscopy (FE-SEM) analysis showed that nano-Ag complexes have various particle sizes ranging from 10 to 30 nm. NSS (average, 10 nm) and NSSPAI (average, 30 nm) showed a uniformly spherical shape and size, while NAg did not. From the reflection peaks in the x-ray diffraction (XRD) patterns, surface crystallinity of the nano-Ag complexes was indicated to be in the same degree as that of NSSPAI>NSS>NAg. Also, in the contact angle (CA) determination, surface hydrophobicity of NSSPAI was stronger than those of NSS and NAg, relatively. The different nano-Ag complexes prepared by γ-irradiation can be applicable in various industry fields due to the increase in specific property.

Preparation and Characterization of Cu and Ni on Alumina Supports and Their Use in the Synthesis of Low-Temperature Metal-Phthalocyanine Using a Parallel-Plate Reactor

PubMed Central

Sánchez-De la Torre, Fernando; De la Rosa, Javier Rivera; Kharisov, Boris I.; Lucio-Ortiz, Carlos J.

2013-01-01

Ni- and Cu/alumina powders were prepared and characterized by X-ray diffraction (XRD), scanning electronic microscope (SEM), and N2 physisorption isotherms were also determined. The Ni/Al2O3 sample reveled agglomerated (1 μm) of nanoparticles of Ni (30–80 nm) however, NiO particles were also identified, probably for the low temperature during the H2 reduction treatment (350 °C), the Cu/Al2O3 sample presented agglomerates (1–1.5 μm) of nanoparticles (70–150 nm), but only of pure copper. Both surface morphologies were different, but resulted in mesoporous material, with a higher specificity for the Ni sample. The surfaces were used in a new proposal for producing copper and nickel phthalocyanines using a parallel-plate reactor. Phthalonitrile was used and metallic particles were deposited on alumina in ethanol solution with CH3ONa at low temperatures; ≤60 °C. The mass-transfer was evaluated in reaction testing with a recent three-resistance model. The kinetics were studied with a Langmuir-Hinshelwood model. The activation energy and Thiele modulus revealed a slow surface reaction. The nickel sample was the most active, influenced by the NiO morphology and phthalonitrile adsorption. PMID:28788334

A comparison study of the start-up of a MnOx filter for catalytic oxidative removal of ammonium from groundwater and surface water.

PubMed

Cheng, Ya; Li, Ye; Huang, Tinglin; Sun, Yuankui; Shi, Xinxin; Shao, Yuezong

2018-03-01

As an efficient method for ammonium (NH 4 + ) removal, contact catalytic oxidation technology has drawn much attention recently, due to its good low temperature resistance and short start-up period. Two identical filters were employed to compare the process for ammonium removal during the start-up period for ammonium removal in groundwater (Filter-N) and surface water (Filter-S) treatment. Two types of source water (groundwater and surface water) were used as the feed waters for the filtration trials. Although the same initiating method was used, Filter-N exhibited much better ammonium removal performance than Filter-S. The differences in catalytic activity among these two filters were probed using X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and compositional analysis. XRD results indicated that different manganese oxide species were formed in Filter-N and Filter-S. Furthermore, the Mn3p XPS spectra taken on the surface of the filter films revealed that the average manganese valence of the inactive manganese oxide film collected from Filter-S (FS-MnO x ) was higher than in the film collected from Filter-N (FN-MnO x ). Mn(IV) was identified as the predominant oxidation state in FS-MnO x and Mn(III) was identified as the predominant oxidation state in FN-MnO x . The results of compositional analyses suggested that polyaluminum ferric chloride (PAFC) used during the surface water treatment was an important factor in the mineralogy and reactivity of MnO x . This study provides the theoretical basis for promoting the wide application of the technology and has great practical significance. Copyright © 2017. Published by Elsevier B.V.

The observation of the physicochemical change of rock under freeze-thawing experiment: CLSM, XRD and ICP analysis

NASA Astrophysics Data System (ADS)

Choi, J.; Chae, B.; Chon, C.; Jeong, J.

2013-12-01

Abstract : In order to understand the progress of the physical weathering of rock sample, we managed freeze-thawing experiment at temperature of up to 40C from -20C taking into account of South Korea. In this study, the time was held by two hours the temperature of the maximum (40C) and minimum (-20C) and the experiments were carried out at intervals of one hour rising and falling. We have run the experiment about 120 cycle with the cycle of -20C from 40C experiment. We measured the physical properties of rock samples after each 20 cycle has elapsed by using confocal laser scanning microscope (CLSM) and observed changes in roughness of rock samples surface. We also analyzed the mineral of rock sample using the XRD analysis and observing the change in chemical composition of solution used in the experiment by using ICP analysis. Through the above process, we observed physico-chemical changes in the rock sample due to freeze-thaw cycles. To analysis of the line roughness parameter we used set by the 10 vertical and horizontal cross section line on the surface and surface roughness parameter was analyzed by using the area on the surface. Through such a process, while the freeze-thawing experiment is advanced, it was studied how the physical roughness and chemical composition were changed. As a result, it was possible to observe a change in the mineral component of the particular dissolved in the solution and it was able to observe the characteristic changes of the parameters of the roughness of the lines and surfaces.

Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

PubMed

Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

2015-09-21

A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

Ex-Situ Synthesis of Polyvinyl alcohol(PVA)-coated Fe3O4 Nanoparticles by Coprecipitation-Ultrasonication Method

NASA Astrophysics Data System (ADS)

Riva'i, Imam; Oktavia Wulandari, Ika; Sulistyarti, Hermin; Sabarudin, Akhmad

2018-01-01

In this study, the synthesis of Fe3O4 nanoparticles was done with surface modification using PVA with coprecipitation-ultrasonication method. Time variations and PVA concentrations were added to determine the effect on crystallite size and lattice parameters on the synthesis of Fe3O4-PVA nanoparticles. Fe3O4 characterization was done using X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) instruments. FTIR was employed to determine PVA coating on the surface of Fe3O4 nanoparticles. The crystallite size and lattice parameters were analyzed using XRD. From the FTIR data, it is known that the interaction between PVA and Fe3O4 nanoparticles is characterized by Fe-O-C group at 1100 cm-1 region which is characteristic of Fe3O4-PVA nanoparticles, C-H groups of PVA in the range of 2950 cm-1 wave number, C-C of PVA regions of wave number 1405 cm-1, Fe3O4 and Fe3O4-PVA samples are in the range of 565 cm-1. In addition, the variation of ultrasonication time and the addition of PVA concentration have an effect on the crystallite size change and the lattice parameter observed from the XRD data. The use of ultrasonication time will affect the size of the crystallite become smaller and the grating lattice parameters obtained are wider. The effect of addition of PVA showed that higher concentration of PVA resulted in smaller crystallite size and larger lattice parameters. These results indicated that ultrasonication time and addition of PVA concentration greatly affect the characteristics of nanoparticles.

Design and synthesis of hierarchical mesoporous WO3-MnO2 composite nanostructures on carbon cloth for high-performance supercapacitors

NASA Astrophysics Data System (ADS)

Shinde, Pragati A.; Lokhande, Vaibhav C.; Patil, Amar M.; Ji, Taeksoo; Lokhande, Chandrakant D.

2017-12-01

To enhance the energy density and power performance of supercapacitors, the rational design and synthesis of active electrode materials with hierarchical mesoporous structure is highly desired. In the present work, fabrication of high-performance hierarchical mesoporous WO3-MnO2 composite nanostructures on carbon cloth substrate via a facile hydrothermal method is reported. By varying the content of MnO2 in the composite, different WO3-MnO2 composite thin films are obtained. The formation of composite is confirmed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses. The Brunauer-Emmett-Teller (BET) analysis reveals maximum specific surface area of 153 m2 g-1. The optimized WO3-MnO2 composite electrode demonstrates remarkable electrochemical performance with high specific capacitance of 657 F g-1 at a scan rate of 5 mV s-1 and superior longterm cycling stability (92% capacity retention over 2000 CV cycles). Furthermore, symmetric flexible solid-state supercapacitor based on WO3-MnO2 electrodes has been fabricated. The device exhibits good electrochemical performance with maximum specific capacitance of 78 F g-1 at a scan rate of 5 mV s-1 and specific energy of 10.8 Wh kg-1 at a specific power of 0.65 kW kg-1. The improved electrochemical performance could be ascribed to the unique combination of multivalence WO3 and MnO2 nanostructures and synergistic effect between them

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

A novel ultrasound assisted method in synthesis of NZVI particles.

PubMed

Jamei, Mir Roozbeh; Khosravi, Mohamad Reza; Anvaripour, Bagher

2014-01-01

This research is about a novel ultrasound assisted method for synthesis of nano zero valent iron particles (NZVI). The materials were characterized using TEM, FESEM, XRD, BET and acoustic PSA. The effect of ultrasonic power, precursor/reductant concentration (NaBH4, FeSO4·7H2O) and delivery rate of NaBH4 on NZVI characteristics were investigated. Under high ultrasonic power the morphology of nano particles changed from spherical type to plate and needle type. Also, when high precursor/reductant and high ultrasonic power was used the particle size of NZVI decreased. The surface area of NZVI particles synthesized by ultrasonic method was increased when compared by the other method. From the XRD patterns it was found also the crystallinity of particles was poor. Copyright © 2013 Elsevier B.V. All rights reserved.

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Archilles, Cherie; Ming, D. W.; Morris, R. V.; Blake, D. F.

2011-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

Effect of stress, strain and optical properties in vacuum and normal annealed ZnO thin films using RF magnetron sputtering

NASA Astrophysics Data System (ADS)

Kumar, B. Santhosh; Purvaja, K.; Harinee, N.; Venkateswaran, C.

2018-05-01

Zinc oxide thin films have been deposited on quartz substrate using RF magnetron sputtering. The deposited films were subjected to different annealing atmosphere at a fixed temperature of 500 °C for 5h. The X-ray diffraction (XRD) patterns reveals the shift in the peak of both normal annealed and vacuum annealed thin films when compared to as-deposited ZnO film. The crystallite size, intrinsic stress and other parameters were calculated from XRD data. The surface morphology of the obtained films were studied using Atomic force microscopy (AFM). From Uv-Visible spectroscopy, the peak at 374 nm of all the films is characteristics of ZnO. The structural, thermal stability and optical properties of the annealed ZnO films are discussed in detail.

Electrical and thermal properties of Ca and Ni doped barium ferrite

NASA Astrophysics Data System (ADS)

Agrawal, Shraddha; Parveen, Azra; Azam, Ameer

2018-05-01

Ca and Ni doped M type Barium ferrite of the composition ((Ba0.9Ca0.1) (Fe0.8 Ni0.2)12O19) were prepared by the traditional sol gel auto combustion method using citric acid as a fuel. Microstructural analyses were carried out with the help of XRD and SEM. XRD analysis is the evidence of nanometer regime along with crystalline planes of hexagonal structure. It also confirms the hexagonal structure of barium ferrite even with the doping of Ca and Ni. SEM analysis is the signature of the spherical shape and surface morphology of agglomerated form of nano-powders of doped samples. The thermal properties of samples were carried out with the help of TGA. That shows the variation of weight loss of the prepared sample with the temperature.

Synthesis and characterization of 64SiO2-26CaO-5P2O5-5CuO bioactive composition for the growth of hydroxyapatite layer by XRD, Raman and pH studies

NASA Astrophysics Data System (ADS)

Kaur, Pardeep; Singh, K. J.

2016-05-01

Bioactive sample with the nominal composition of 64SiO2-26CaO-5P2O5-5CuO has been prepared in the laboratory by using the sol-gel technique. The bioactivity of the prepared sample has been analyzed by using the Tris Simulated Body Fluid which has also been prepared in the laboratory. XRD and Raman techniques have been employedto probe the formation of hydroxyapatite layer. pH studies has also been undertaken to check the acidic/non-acidic behavior of sample. Growth of hydroxyapatite layer has been observed after one day on the surface of the sample. Moreover, sample has been observed to be non-acidic in nature.

Anisotropically biaxial strain in non-polar (112-0) plane In x Ga1-x N/GaN layers investigated by X-ray reciprocal space mapping.

PubMed

Zhao, Guijuan; Li, Huijie; Wang, Lianshan; Meng, Yulin; Ji, Zesheng; Li, Fangzheng; Wei, Hongyuan; Yang, Shaoyan; Wang, Zhanguo

2017-07-03

In this study, the indium composition x as well as the anisotropically biaxial strain in non-polar a-plane In x Ga 1-x N on GaN is studied by X-ray diffraction (XRD) analysis. In accordance with XRD reciprocal lattice space mapping, with increasing indium composition, the maximum of the In x Ga 1-x N reciprocal lattice points progressively shifts from a fully compressive strained to a fully relaxed position, then to reversed tensile strained. To fully understand the strain in the ternary alloy layers, it is helpful to grow high-quality device structures using a-plane nitrides. As the layer thickness increases, the strain of In x Ga 1-x N layer releases through surface roughening and the 3D growth-mode.

Hydroxyapatite-phosphonoformic acid hybrid compounds prepared by hydrothermal method

NASA Astrophysics Data System (ADS)

Turki, Thouraya; Othmani, Masseoud; Bantignies, Jean-Louis; Bouzouita, Khaled

2014-01-01

Hydroxyapatites were prepared in the presence of different amounts of phosphonoformic acid (PFA) via the hydrothermal method. The obtained powders were characterized through chemical analysis, XRD, IR, 31P MAS-NMR, TEM, and TG-TDA. The XRD showed that the PFA did not affect the apatite composition. Indeed, only a reduction of the crystallite size was noted. After grafting of PFA, the IR spectroscopy revealed the appearance of new bands belonging to HPO42- and carboxylate groups of the apatite and organic moiety, respectively. Moreover, the 31P MAS-NMR spectra exhibited a peak with a low intensity assigned to the terminal phosphonate group of the organic moiety in addition to that of the apatite. Based on these results, a reaction mechanism involving the surface hydroxyl groups (tbnd Casbnd OH) of the apatite and the carboxyl group of the acid was proposed.

Synthesis and toxicity test of magnetic nanoparticle via biocompatible microemulsion system as template for application in targeted drug delivery

NASA Astrophysics Data System (ADS)

Kader, Razinah Abdul; Rose, Laili Che; Suhaimi, Hamdan; Manickam, Mariessa Soosai

2017-09-01

This work reports the preparation of magnetic nanoparticles (FeNPs) using biocompatible W/O microemulsion for biomedical applications. W/O microemulsion was formed using decane as oil phase, water, tween 80 as non-ionic surfactant and hexanol as organic solvent. The synthesized FeNPs were characterised by using Fourier Transform Infrared Resonance Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD). The FTIR showed that Fe-O bond exist on 581cm-1 having strong magnetic strength whereas SEM showed the morphology surface of magnetic nanoparticles (FeNPs). Furthermore, analysis of XRD pattern magnetic nanoparticles (FeNPs) reveals a cubic iron oxide phase with good crystallize structure. Furthermore, toxicity test on human liver cells proved that it is 70% safe on human and proved to be a safety nanomedicine.

Synthesis, characterization and antistructure modeling of Ni nano ferrite

NASA Astrophysics Data System (ADS)

Kane, S. N.; Raghuvanshi, S.; Satalkar, M.; Reddy, V. R.; Deshpande, U. P.; Tatarchuk, T. R.; Mazaleyrat, F.

2018-05-01

We report the role played by cation distribution in determining magnetic properties by comparing dry gel, thermally annealed Ni ferrite prepared by sol-gel auto-combustion technique. X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and Mössbauer spectroscopy were used to characterize the samples. Both XRD and Mössbauer measurements validate the formation of spinel phase with grain diameter 39.13-45.53 nm. First time antistructural modeling for Ni ferrite is reported to get information on active surface centers. Decrease of Debye temperature θD in annealed sample shows enhancement of lattice vibrations. With thermal annealing experimental and Néel magnetic moment (nBe, nBN) increases, suggesting migration of Ni2+ from B to A site with concurrent migration of Fe3+ from A to B site (non-equilibrium cationic distribution), affecting magnetic properties.

Deposition of Metal-Organic Frameworks by Liquid-Phase Epitaxy: The Influence of Substrate Functional Group Density on Film Orientation

PubMed Central

Liu, Jinxuan; Shekhah, Osama; Stammer, Xia; Arslan, Hasan K.; Liu, Bo; Schüpbach, Björn; Terfort, Andreas; Wöll, Christof

2012-01-01

The liquid phase epitaxy (LPE) of the metal-organic framework (MOF) HKUST-1 has been studied for three different COOH-terminated templating organic surfaces prepared by the adsorption of self-assembled monolayers (SAMs) on gold substrates. Three different SAMs were used, mercaptohexadecanoic acid (MHDA), 4’-carboxyterphenyl-4-methanethiol (TPMTA) and 9-carboxy-10-(mercaptomethyl)triptycene (CMMT). The XRD data demonstrate that highly oriented HKUST-1 SURMOFs with an orientation along the (100) direction was obtained on MHDA-SAMs. In the case of the TPMTA-SAM, the quality of the deposited SURMOF films was found to be substantially inferior. Surprisingly, for the CMMT-SAMs, a different growth direction was obtained; XRD data reveal the deposition of highly oriented HKUST-1 SURMOFs grown along the (111) direction.

Copper Oxide Nanograss for Efficient and Stable Photoelectrochemical Hydrogen Production by Water Splitting

NASA Astrophysics Data System (ADS)

Borkar, Rajnikant; Dahake, Rashmi; Rayalu, Sadhana; Bansiwal, Amit

2018-03-01

A biphasic copper oxide thin film of grass-like appendage morphology is synthesized by two-step electro-deposition method and later investigated for photoelectrochemical (PEC) water splitting for hydrogen production. Further, the thin film was characterized by UV-Visible spectroscopy, x-ray diffraction (XRD), Scanning electron microscopy (SEM) and PEC techniques. The XRD analysis confirms formation of biphasic copper oxide phases, and SEM reveals high surface area grass appendage-like morphology. These grass appendage structures exhibit a high cathodic photocurrent of - 1.44 mAcm-2 at an applied bias of - 0.7 (versus Ag/AgCl) resulting in incident to photon current efficiency (IPCE) of ˜ 10% at 400 nm. The improved light harvesting and charge transport properties of grass appendage structured biphasic copper oxides makes it a potential candidate for PEC water splitting for hydrogen production.

Fabrication of mesoporous cerium dioxide films by cathodic electrodeposition.

PubMed

Kim, Young-Soo; Lee, Jin-Kyu; Ahn, Jae-Hoon; Park, Eun-Kyung; Kim, Gil-Pyo; Baeck, Sung-Hyeon

2007-11-01

Mesoporous cerium dioxide (Ceria, CeO2) thin films have been successfully electrodeposited onto ITO-coated glass substrates from an aqueous solution of cerium nitrate using CTAB (Cetyltrimethylammonium Bromide) as a templating agent. The synthesized films underwent detailed characterizations. The crystallinity of synthesized CeO2 film was confirmed by XRD analysis and HR-TEM analysis, and surface morphology was investigated by SEM analysis. The presence of mesoporosity in fabricated films was confirmed by TEM and small angle X-ray analysis. As-synthesized film was observed from XRD analysis and HR-TEM image to have well-crystallized structure of cubic phase CeO2. Transmission electron microscopy and small angle X-ray analysis revealed the presence of uniform mesoporosity with a well-ordered lamellar phase in the CeO2 films electrodeposited with CTAB templating.

La-Sr-Ni-Co-O based perovskite-type solid solutions as catalyst precursors in the CO 2 reforming of methane

NASA Astrophysics Data System (ADS)

Valderrama, Gustavo; Kiennemann, Alain; Goldwasser, Mireya R.

La 1- xSr xNi 0.4Co 0.6O 3 and La 0.8Sr 0.2Ni 1- yCo yO 3 solid solutions with perovskite-type structure were synthesized by the sol-gel resin method and used as catalytic precursors in the dry reforming of methane with CO 2 to syngas, between 873 and 1073 K at atmospheric pressure under continuous flow of reactant gases with CH 4/CO 2 = 1 ratio. These quaternary oxides were characterized by X-ray diffraction (XRD), BET specific surface area and temperature-programmed reduction (TPR) techniques. XRD analyses of the more intense diffraction peaks and cell parameter measurements showed formation of La-Sr-Ni-Co-O solid solutions with La 0.9Sr 0.1CoO 3 and/or La 0.9Sr 0.1NiO 3 as the main crystallographic phases present on the solids depending on the degree of substitution. TPR analyses showed that Sr doping decreases the temperature of reduction via formation of intermediary species producing Ni 0, Co 0 with particle sizes in the range of nanometers over the SrO and La 2O 3 phases. These metallic nano particles highly dispersed in the solid matrix are responsible for the high activity shown during the reaction and avoid carbon formation. The presence of Sr in doping quantities also promotes the secondary reactions of carbon formation and water-gas shift in a very small extension during the dry reforming reaction.

[Removal and Recycle of Phosphor from Water Using Magnetic Core/Shell Structured Fe₃O₄ @ SiO₂Nanoparticles Functionalized with Hydrous Aluminum Oxide].

PubMed

Lai, Li; Xie, Qiang; Fang, Wen-kan; Xing, Ming-chao; Wu, De-yi

2016-04-15

A novel magnetic core/shell structured nano-particle Fe₃O₄@ SiO₂phosphor-removal ahsorbent functionalized with hydrous aluminum oxides (Fe₃O₄@ SiO₂@ Al₂O₃· nH₂O) was synthesized. Fe₃O₄@ SiO₂@ Al₂O₃· nH₂O was characterized by XRD, TEM, VSM and BET nitrogen adsorption experiment. The XRD and TEM results demonstrated the presence of the core/shell structure, with saturated magnetization and specific surface area of 56.00 emu · g⁻¹ and 47.27 m² · g⁻¹, respectively. In batch phosphor adsorption experiment, the Langmuir adsorption maximum capacity was 12.90 mg · g⁻¹ and nearly 96% phosphor could be rapidly removed within a contact time of 40 mm. Adsorption of phosphor on Fe₃O₄@ SiO₂@ Al₂O₃ · nH₂O was highly dependent on pH condition, and the favored pH range was 5-9 in which the phosphor removal rate was above 90%. In the treatment of sewage water, the recommended dosage was 1.25 kg · t⁻¹. In 5 cycles of adsorption-regeneration-desorption experiment, over 90% of the adsorbed phosphor could be desorbed with 1 mol · L⁻¹ NaOH, and Fe₃O₄@ SiO₂@ Al₂O₃· nH₂O could be reused after regeneration by pH adjustment with slightly decreased phosphor removal rate with increasing recycling number, which proved the recyclability of Fe₃O₄@ SiO₂@ Al₂O₃· nH₂O and thereby its potential in recycling of phosphor resources.

Provenance of Holocene sediment on the Chukchi-Alaskan margin based on combined diffuse spectral reflectance and quantitative X-Ray Diffraction analysis

USGS Publications Warehouse

Ortiz, J.D.; Polyak, L.; Grebmeier, J.M.; Darby, D.; Eberl, D.D.; Naidu, S.; Nof, D.

2009-01-01

Sediment clay and silt mineral assemblages provide an excellent means of assessing the provenance of fine-grained Arctic sediment especially when a unique mineral assemblage can be tied to specific source areas. The diffuse spectral reflectance (DSR) first derivative measurements and quantitative X-Ray Diffraction (qXRD) on a high-resolution sediment core from the continental slope north of Alaska constrain the sediment mineralogy. DSR results are augmented by measurements on several adjacent cores and compared to surface sediment samples from the northern Alaskan shelf and slope. Using Principal Component Analysis (PCA), we infer that the three leading DSR modes relate to mixtures of smectite + dolomite, illite + goethite, and chlorite + muscovite. This interpretation is consistent with the down core qXRD results. While the smectite + dolomite, and illite + goethite factors show increased variability down core, the chlorite + muscovite factor had highest positive loadings in the middle Holocene, between ca. 6.0 and 3.6??ka. Because the most likely source of the chlorite + muscovite suite in this vicinity lies in the North Pacific, we argue that the oscillations in chlorite + muscovite values likely reflect an increase in the inflow of Pacific water to the Arctic through the Bering Strait. The time interval of this event is associated in other parts of the globe with a non-linear response of the climate system to the decrease in insolation, which may be related to changes in water exchange between the Pacific and Arctic Ocean. ?? 2009 Elsevier B.V.

Characterization of Serpentine Samples from the Coast Range Ophiolite Microbial Observatory with μ-FTIR and XRD. ­­

NASA Astrophysics Data System (ADS)

Sousa, A.; Cardace, D.

2017-12-01

Serpentinizing systems hold much promise as potentially habitable environments in diverse planetary settings. They involve abundant and simple ingredients (i.e., the mineral olivine, liquid water), support subsurface microbial communities on Earth (Crespo-Medina et al. 2014; Suzuki et al. 2014; Kelley et al. 2005) and are thought to occur elsewhere in our solar system such as Mars (Schulte et al. 2006; Ehlmann et al. 2010)and possibly ocean worlds (Waite et al. 2017; Vance 2009). Although geochemical and microbial data collection continues in serpentinizing systems, the identification and resolution of potential biosignatures in serpentinites are not yet clear. Specifically, the micro-scale mineralogical contexts in which cell fragments or biofilm residues may be formed and preserved is lacking. Here we report preliminary transmission and reflection mode μ-FTIR spectral maps and XRD diffractograms, obtained with instruments relevant to robotic exploration missions (Blake et al. 2012; Igisu et al. 2009; Leroi et al. 2009). Samples analyzed include ultramafic rock and constituent mineral standards (e.g., olivine) and rocks collected from near surface sites associated with the NASA Astrobiology Institute-funded initiative, the Coast Range Ophiolite Microbial Observatory (CROMO), in Lower Lake, CA (Cardace et al. 2013). These new results provide co-registered, complementary data on astrobiologically important rock and mineral phases related to serpentinization (Crespo-Medina et al. 2014; Twing et al. 2017). Future work will leverage this data set in microbial colonization experiments aimed at parsing background organic loads in serpentinites from surficial/fracture-localized modern biofilm signatures.

Electrochemical performance of spinel-type Ni doped ZnCo2O4 mesoporous rods as an electrode for supercapacitors

NASA Astrophysics Data System (ADS)

Kumar, Vijay; Mariappan, C. R.

2018-05-01

The Ni doped ZnCo2O4 mesoporous rods were synthesized via a simple hydrothermal approach. Structural properties of the sample were characterized by means of powder X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA), scanning electron microscope and high-resolution transmission electron microscopy. The surface area of mesoporous rods Zn0.8Ni0.2Co2O4 (MPR=0.2) found to be ˜56 m2g-1 and with pore size of ˜10 nm from N2 absorption isotherm data. The crystal structure with lattice parameter of (MPR=0.2) is found to be 8.138 Å. The average crystallite size is found to be 12 nm from XRD data. TGA study reveals the phase formation temperature of sample is 450 °C. Electron microscopic studies reveal that the mesoporous rods are constituted by a plenty of nanosized crystalline particles. The electrochemical properties of the sample was studied by cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) measurement in three-electrode configuration with 6M KOH as the electrolyte. The specific capacitance (Cs) of (MPR=0.2) used as a working electrode found to be 2021 Fg-1 at a scan rate of 2 mVs-1. Furthermore electrochemical cycling stability of mesoporous rods is examined by GCD with different current densities. It shows maximum Cs of 628.75 Fg-1 at 2.5 Ag-1 and retention is found to be ˜96% of its initial value even after 1000 cycles.

Compositional ratio effect on the surface characteristics of CuZn thin films

NASA Astrophysics Data System (ADS)

Choi, Ahrom; Park, Juyun; Kang, Yujin; Lee, Seokhee; Kang, Yong-Cheol

2018-05-01

CuZn thin films were fabricated by RF co-sputtering method on p-type Si(100) wafer with various RF powers applied on metallic Cu and Zn targets. This paper aimed to determine the morphological, chemical, and electrical properties of the deposited CuZn thin films by utilizing a surface profiler, atomic force microscopy (AFM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), UV photoelectron spectroscopy (UPS), and a 4-point probe. The thickness of the thin films was fixed at 200 ± 8 nm and the roughness of the thin films containing Cu was smaller than pure Zn thin films. XRD studies confirmed that the preferred phase changed, and this tendency is dependent on the ratio of Cu to Zn. AES spectra indicate that the obtained thin films consisted of Cu and Zn. The high resolution XPS spectra indicate that as the content of Cu increased, the intensities of Zn2+ decreased. The work function of CuZn thin films increased from 4.87 to 5.36 eV. The conductivity of CuZn alloy thin films was higher than pure metallic thin films.

Structural and Magnetic Response in Bimetallic Core/Shell Magnetic Nanoparticles

PubMed Central

Nairan, Adeela; Khan, Usman; Iqbal, Munawar; Khan, Maaz; Javed, Khalid; Riaz, Saira; Naseem, Shahzad; Han, Xiufeng

2016-01-01

Bimagnetic monodisperse CoFe2O4/Fe3O4 core/shell nanoparticles have been prepared by solution evaporation route. To demonstrate preferential coating of iron oxide onto the surface of ferrite nanoparticles X-ray diffraction (XRD), High resolution transmission electron microscope (HR-TEM) and Raman spectroscopy have been performed. XRD analysis using Rietveld refinement technique confirms single phase nanoparticles with average seed size of about 18 nm and thickness of shell is 3 nm, which corroborates with transmission electron microscopy (TEM) analysis. Low temperature magnetic hysteresis loops showed interesting behavior. We have observed large coercivity 15.8 kOe at T = 5 K, whereas maximum saturation magnetization (125 emu/g) is attained at T = 100 K for CoFe2O4/Fe3O4 core/shell nanoparticles. Saturation magnetization decreases due to structural distortions at the surface of shell below 100 K. Zero field cooled (ZFC) and Field cooled (FC) plots show that synthesized nanoparticles are ferromagnetic till room temperature and it has been noticed that core/shell sample possess high blocking temperature than Cobalt Ferrite. Results indicate that presence of iron oxide shell significantly increases magnetic parameters as compared to the simple cobalt ferrite. PMID:28335200

Effect of cetyl trimethyl ammonium bromide concentration on structure, morphology and carbon dioxide adsorption capacity of calcium hydroxide based sorbents

NASA Astrophysics Data System (ADS)

Hlaing, Nwe Ni; Vignesh, K.; Sreekantan, Srimala; Pung, Swee-Yong; Hinode, Hirofumi; Kurniawan, Winarto; Othman, Radzali; Thant, Aye Aye; Mohamed, Abdul Rahman; Salim, Chris

2016-02-01

Calcium hydroxide (Ca(OH)2) has been proposed as an important material for industrial, architectural, and environmental applications. In this study, calcium acetate was used as a precursor and cetyl trimethyl ammonium bromide (CTAB) was used as a surfactant to synthesize Ca(OH)2 based adsorbents for carbon dioxide (CO2) capture. The effect of CTAB concentration (0.2-0.8 M) on the structure, morphology and CO2 adsorption performance of Ca(OH)2 was studied in detail. The synthesized samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), BET surfaced area and thermogravimetry-differential thermal analysis (TG-DTA) techniques. The phase purity, crystallite size, Brunauer-Emmett-Teller (BET) surface area and CO2 adsorption performance of Ca(OH)2 precursor adsorbents were significantly increased when the concentration of CTAB was increased. XRD results showed that pure Ca(OH)2 phase was obtained at the CTAB concentration of 0.8 M. TGA results exhibited that 0.8 M of CTAB-assisted Ca(OH)2 precursor adsorbent possessed a residual carbonation conversion of ∼56% after 10 cycles.

Regular square planer bis-(4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione)/copper(II) complex: Trans/cis-DFT isomerization, crystal structure, thermal, solvatochromism, hirshfeld surface and DNA-binding analysis

NASA Astrophysics Data System (ADS)

Hema, M. K.; Karthik, C. S.; Warad, Ismail; Lokanath, N. K.; Zarrouk, Abdelkader; Kumara, Karthik; Pampa, K. J.; Mallu, P.

2018-04-01

Trans-[Cu(O∩O)2] complex, O∩O = 4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione was reported with high potential toward CT-DNA binder. The solved XRD-structure of complex indicated a perfect regular square-planer geometry around the Cu(II) center. The trans/cis-DFT-isomerization calculation supported the XRD seen in reflecting the trans-isomer as the kinetic-favor isomer. The desired complex structure was also characterized by conductivity measurement, CHN-elemental analyses, MS, EDX, SEM, UV-Vis., FT-IR, HAS and TG/DTG. The Solvatochromism behavior of the complex was evaluated using four different polar solvents. MPE and Hirshfeld surface analysis (HSA) come to an agreement that fluoride and thiophene protons atoms are with suitable electro-potential environment to form non-classical H-bonds of type CThsbnd H⋯F. The DNA-binding properties were investigated by viscosity tests and spectrometric titrations, the results revealed the complex as strong calf-thymus DNA binder. High intrinsic-binding constants value ∼1.8 × 105 was collected.

Autogenous teeth used for bone grafting: a comparison with traditional grafting materials.

PubMed

Kim, Young-Kyun; Kim, Su-Gwan; Yun, Pil-Young; Yeo, In-Sung; Jin, Seung-Chan; Oh, Ji-Su; Kim, Heung-Joong; Yu, Sun-Kyoung; Lee, Sook-Young; Kim, Jae-Sung; Um, In-Woong; Jeong, Mi-Ae; Kim, Gyung-Wook

2014-01-01

This study evaluated the surface structures and physicochemical characteristics of a novel autogenous tooth bone graft material currently in clinical use. The material's surface structure was compared with a variety of other bone graft materials via scanning electron microscope (SEM). The crystalline structure of the autogenous tooth bone graft material from the crown (AutoBT crown) and root (AutoBT root), xenograft (BioOss), alloplastic material (MBCP), allograft (ICB), and autogenous mandibular cortical bone were compared using x-ray diffraction (XRD) analysis. The solubility of each material was measured with the Ca/P dissolution test. The results of the SEM analysis showed that the pattern associated with AutoBT was similar to that from autogenous cortical bones. In the XRD analysis, AutoBT root and allograft showed a low crystalline structure similar to that of autogenous cortical bones. In the CaP dissolution test, the amount of calcium and phosphorus dissolution in AutoBT was significant from the beginning, while displaying a pattern similar to that of autogenous cortical bones. In conclusion, autogenous tooth bone graft materials can be considered to have physicochemical characteristics similar to those of autogenous bones. Copyright © 2014 Elsevier Inc. All rights reserved.

Spatial distribution of crystalline corrosion products formed during corrosion of stainless steel in concrete

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

Serdar, Marijana; Meral, Cagla; Kunz, Martin

2015-05-15

The mineralogy and spatial distribution of nano-crystalline corrosion products that form in the steel/concrete interface were characterized using synchrotron X-ray micro-diffraction (μ-XRD). Two types of low-nickel high-chromium reinforcing steels embedded into mortar and exposed to NaCl solution were investigated. Corrosion in the samples was confirmed by electrochemical impedance spectroscopy (EIS). μ-XRD revealed that goethite (α-FeOOH) and akaganeite (β-FeOOH) are the main iron oxide–hydroxides formed during the chloride-induced corrosion of stainless steel in concrete. Goethite is formed closer to the surface of the steel due to the presence of chromium in the steel, while akaganeite is formed further away from themore » surface due to the presence of chloride ions. Detailed microstructural analysis is shown and discussed on one sample of each type of steel. - Highlights: • Synchrotron micro-diffraction used to map the distribution of crystalline phases. • Goethite and akaganeite are the main corrosion products during chloride induced corrosion in mortar. • Layers of goethite and akaganeite are negatively correlated. • EDS showed Cr present in corrosion products identified by SEM.« less

Synergistic effect of indium and gallium co-doping on the properties of RF sputtered ZnO thin films

NASA Astrophysics Data System (ADS)

Shaheera, M.; Girija, K. G.; Kaur, Manmeet; Geetha, V.; Debnath, A. K.; Karri, Malvika; Thota, Manoj Kumar; Vatsa, R. K.; Muthe, K. P.; Gadkari, S. C.

2018-04-01

ZnO thin films were synthesized using RF magnetron sputtering, with simultaneous incorporation of Indium (In) and Gallium (Ga). The structural, optical, chemical composition and surface morphology of the pure and co-doped (IGZO) thin films were characterized by X-Ray diffraction (XRD), UV-visible spectroscopy, Field Emission Scanning Electron Microscopy (FESEM), and Raman spectroscopy. XRD revealed that these films were oriented along c-axis with hexagonal wurtzite structure. The (002) diffraction peak in the co-doped sample was observed at 33.76° with a slight shift towards lower 2θ values as compared to pure ZnO. The surface morphology of the two thin films was observed to differ. For pure ZnO films, round grains were observed and for IGZO thin films round as well as rod type grains were observed. All thin films synthesized show excellent optical properties with more than 90% transmission in the visible region and band gap of the films is observed to decrease with co-doping. The co doping of In and Ga is therefore expected to provide a broad range optical and physical properties of ZnO thin films for a variety of optoelectronic applications.

The Mineralogy of Martian Dust: Design and Analysis Considerations for an X-Ray Diffraction/X-Ray Fluorescence (XRD/XRF) Instrument for Exobiological Studies

NASA Technical Reports Server (NTRS)

Blake, David; Vaniman, David; Bish, David; Morrison, David (Technical Monitor)

1994-01-01

A principal objective of Mars exploration is the search for evidence of past life which may have existed during an earlier clement period of Mars history. We would like to investigate the history of surface water activity (which is a requirement for all known forms of life) by identifying and documenting the distribution of minerals which require water for their formation or distribution. A knowledge of the mineralogy of the present Martian surface would help to identify areas which, due to the early activity of water, might have harbored ancient life. It would be desirable to establish the presence and characterize the distribution of hydrated minerals such as clays, and of minerals which are primarily of sedimentary origin such as carbonates, silica and evaporites. Mineralogy, which is more critical to exobiological exploration than is simple chemical analysis (absent the detection of organics), will remain unknown or will at best be imprecisely constrained unless a technique sensitive to mineral structure such as powder X-ray diffraction (XRD) is employed. Additional information is contained in the original extended abstract.

Characterization of bismuth selenide (Bi2Se3) thin films obtained by evaporating the hydrothermally synthesised nano-particles

NASA Astrophysics Data System (ADS)

Indirajith, R.; Rajalakshmi, M.; Gopalakrishnan, R.; Ramamurthi, K.

2016-03-01

Bismuth selenide (Bi2Se3) was synthesized by hydrothermal method at 200 °C and confirmed by powder X-ray diffraction (XRD) studies. The synthesized material was utilized to deposit bismuth selenide thin films at various substrate temperatures (Room Temperature-RT, 150 °C, 250 °C, 350 °C and 450 °C) by electron beam evaporation technique. XRD study confirmed the polycrystalline nature of the deposited Bi2Se3films. Optical transmittance spectra showed that the deposited (at RT) films acquire relatively high average transmittance of 60%in near infrared region (1500-2500 nm). An indirect allowed optical band gap calculated from the absorption edge for the deposited films is ranging from 0.62 to 0.8 eV. Scanning electron and atomic force microscopy analyses reveal the formation of nano-scale sized particles on the surface and that the nature of surface microstructures is influenced by the substrate temperature. Hall measurements showed improved electrical properties, for the films deposited at 350 °C which possess 2.8 times the mobility and 0.9 times the resistivity of the films deposited at RT.

Investigation on mechanical behavior and material characteristics of various weight composition of SiCp reinforced aluminium metal matrix composite

NASA Astrophysics Data System (ADS)

Pichumani, Sivachidambaram; Srinivasan, Raghuraman; Ramamoorthi, Venkatraman

2018-02-01

Aluminium - silicon carbide (Al - SiC) metal matrix composite is produced with following wt % of SiC reinforcement (4%, 8% & 12%) using stir casting method. Mechanical testing such as micro hardness, tensile testing and bend testing were performed. Characterizations, namely micro structure, X-ray diffraction (XRD) analysis, inductive coupled plasma - optical emission spectroscopy (ICP-OES) and scanning electron microscopy (SEM) analysis, were carried out on Al - SiC composites. The presence of SiC on Al - SiC composite is confirmed through XRD technique and microstructure. The percentage of SiC was confirmed through ICP-OES technique. Increase in weight percentage of SiC tends to increase micro hardness, ultimate strength & yield strength but it reduces the bend strength and elongation (%) of the material. SEM factrography of tensile tested fractured samples of Al - 8% SiC & Al - 12% SiC showed fine dimples on fractured surface & coarse dimples fractured surface respectively. This showed significant fracture differences between Al - 8% SiC & Al - 12% SiC. From the above experiment, Al - 8% SiC had good micro hardness, ultimate strength & yield strength without significant loss in elongation (%) & bend strength.

Textured Pr{sub 2}Fe{sub 14}B flakes with submicron or nanosize thickness prepared by surfactant-assisted ball milling

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

Zuo, Wen-Liang, E-mail: wlzuo@iphy.ac.cn, E-mail: shenbg@aphy.iphy.ac.cn; Liu, Rong-Ming; Zheng, Xin-Qi

2014-05-07

The textured Pr{sub 2}Fe{sub 14}B nanoflakes were produced by surfactant-assisted ball milling (SABM). Single phase tetragonal structure was characterized for the samples before and after SABM by X-ray diffraction (XRD). The thickness and length of the as-milled flakes are mainly in the range of 50–150 nm and 0.5–2 μm, respectively. For the field-aligned Pr{sub 2}Fe{sub 14}B nanoflakes, the out-of-plane texture (the easy magnetization direction (EMD) along the c-axis) is indicated from the increasing (00l) peaks in the XRD patterns. SEM image demonstrates that the EMD is parallel to flaky surface, which is different from the RCo{sub 5} (R = rare earth) system with EMDmore » perpendicular to the surface. We propose a hypothesis that the easy glide planes are related with the area of crystal planes. In addition, a large coercivity H{sub c} = 3.9 kOe is observed in the Pr{sub 2}Fe{sub 14}B flakes with strong texture.« less

Hidroxyapatite Coating on CoCrMo Alloy Titanium Nitride Coated Using Biomimetic Method

NASA Astrophysics Data System (ADS)

Charlena; Sukaryo, S. G.; Fajar, M.

2016-11-01

Bone implants is a way to cure broken bones which is being developed. The implants can be made of metals, ceramics and polymers. Metallic materials commonly used are titanium (Ti), stainless steel, and metal alloys. This study used Co-based alloys, i.e. CoCrMo coated with titanium nitride (TiN) which was then coated on hidroxyapatite (HAp). The HAp coating on the surface of CoCrMo alloy was done by biomimetic methods, first by soaking the metal alloys in simulated body fluid (SBF) solution for 18, 24, and 36 hours. The immersion in the SBF solution produced white coat on the surface of the metal alloy. The layers formed were analyzed by scanning electron microscope (SEM) and characterized by x-ray diffractometer (XRD). Based on the SEM results of 36 hours treatment, the morphology of apatite crystal formed fine grains. According to XRD result, there were HAp peaks at angles 2θ 31.86, 32.25, dan 39.48. However, there were also CaCO3 peaks at angles 2θ 29.46, 36.04, and 46.79. It indicated the pure HAp is not yet formed.

Italian Renaissance and Hispano-Moresque lustre-decorated majolicas: imitation cases of Hispano-Moresque style in central Italy

NASA Astrophysics Data System (ADS)

Padeletti, G.; Fermo, P.

An investigation was carried out on Renaissance lustre-decorated majolica shards, found during excavations made in Umbria (central Italy) and defined by experts, on the ground of the surface decoration, as imitations of the Hispano-Moresque style. A comparison between this particular kind of samples, produced in central Italy, and some Hispano-Moresque lustre shards has been performed. The ceramic bodies as well as the lustred surfaces have been analysed by means of several techniques: inductively coupled plasma optical emission spectrometry, X-ray diffraction (XRD), atomic absorption spectrometry with electrothermal atomisation and scanning electron microscopy. By means of XRD analysis the presence of cosalite (Pb2Bi2S5) has been disclosed in the Italian lustre decorations but was not observed in the Hispano-Moresque ones. A hypothesis has been made, considering bismuth as a discriminating element, between lustres produced in central Italy and the Hispano-Moresque ones. We thought that the Italian artisans were able to manage the use of bismuth. Therefore a recipe, quite similar to the one employed by the Spanish artisans, was used by the Italian ceramists if their aim was to imitate the Hispano-Moresque style.

Deposition of magnesium nitride thin films on stainless steel-304 substrates by using a plasma focus device

NASA Astrophysics Data System (ADS)

Ramezani, Amir Hoshang; Habibi, Maryam; Ghoranneviss, Mahmood

2014-08-01

In this research, for the first time, we synthesize magnesium nitride thin films on 304-type stainless steel substrates using a Mather-type (2 kJ) plasma focus (PF) device. The films of magnesium nitride are coated with different number of focus shots (like 15, 25 and 35) at a distance of 8 cm from the anode tip and at 0° angular position with respect to the anode axis. For investigation of the structural properties and surface morphology of magnesium nitride films, we utilized the X-ray diffractometer (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) analysis, respectively. Also, the elemental composition is characterized by energy-dispersive X-ray (EDX) analysis. Furthermore, Vicker's microhardness is used to study the mechanical properties of the deposited films. The results show that the degree of crystallinity of deposited thin films (from XRD), the average size of particles and surface roughness (from AFM), crystalline growth of structures (from SEM) and the hardness values of the films depend on the number of focus shots. The EDX analysis demonstrates the existence of the elemental composition of magnesium in the deposited samples.

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.

Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

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

Alvarez, Edelio Danguillecourt, E-mail: edelioalvarez42@gmail.com; Laffita, Yodalgis Mosqueda, E-mail: yodalgis@imre.uh.cu; Montoro, Luciano Andrey, E-mail: landrey.montoro@gmail.com

We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer–Emmett–Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m{sup 2} g{sup −1}). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysicalmore » measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10{sup −7} m{sup 2} s{sup −1}) and conductivity (1.1 W m{sup −1} K{sup −1}) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173–293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g{sup −1} was reached. - Graphical abstract: TEM image and electrochemistry behavior of a new graphene oxide-like carbon. - Highlights: • A high disordered graphene oxide-like conducting carbon is reported. • The synthesis was based on palygorskite and sugar cane molasses as precursors. • The disordered conducting carbon is composed of doped- graphene heterogeneous domains. • This material combines a large specific surface area and high electric conductivity. • The thermophysical and electrochemical properties of this material reveal adequate behavior.« less

Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

NASA Astrophysics Data System (ADS)

Alvarez, Edelio Danguillecourt; Laffita, Yodalgis Mosqueda; Montoro, Luciano Andrey; Della Santina Mohallem, Nelcy; Cabrera, Humberto; Pérez, Guillermo Mesa; Frutis, Miguel Aguilar; Cappe, Eduardo Pérez

2017-02-01

We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer-Emmett-Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m2 g-1). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysical measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10-7 m2 s-1) and conductivity (1.1 W m-1 K-1) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173-293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g-1 was reached.