Soapnut extract mediated synthesis of nanoscale cobalt substituted NdFeB ferromagnetic materials and their characterization

NASA Astrophysics Data System (ADS)

Rao, G. V. S. Jayapala; Prasad, T. N. V. K. V.; Shameer, Syed; Rao, M. Purnachandra

2018-04-01

Neodymium iron boron (NdFeB) permanent magnets have high energy product with suitable magnetic and physical properties for an array of applications including power generation and motors. However, synthetic routes of NdFeB permanent magnets involve critical procedures with high energy and needs scientific skills. Herein, we report on soapnut extract mediated synthesis of nanoscale cobalt substituted NdFeB (Co-NdFeB) permanent magnetic powders (Nd: 15%, Fe: 77.5%, B: 7.5% and Co with molar ratios: 0.5, 1, 1.5 and 2). A 10 ml of 10% soapnut extract was added to 90 ml of respective chemical composition and heated to 60 °C for 30 min and aged for 24 h. The dried powder was sintered at 500 °C for 1 h. The characterization of the prepared nanoscale Co-NdFeB magnetic powders was done using the techniques such as Dynamic Light Scattering (DLS for size and zeta potential measurements), X-ray diffraction (XRD) for structural determination, Scanning electron microscopy (SEM) with energy dispersion spectroscopy (EDS) for surface morphological and elemental analysis, Fourier transform infrared spectroscopy (FT-IR) for the identification of functional groups associated and hysteresis loop studies to quantify the magnetization. The results revealed that particles were in irregular and tubular shaped and highly stable (Zeta potential: -44.4 mV) with measured size <100 nm. XRD micrographs revealed a tetragonal crystal structure and FTIR showed predominant N-H and O-H stretching indicates the involvement of these functional groups in the reduction and stabilization process of Co-NdFeB magnetic powders. Hysteresis studies signify the effect of an increase in Co concentration.

Skin delivery of epigallocatechin-3-gallate (EGCG) and hyaluronic acid loaded nano-transfersomes for antioxidant and anti-aging effects in UV radiation induced skin damage.

PubMed

Avadhani, Kiran S; Manikkath, Jyothsna; Tiwari, Mradul; Chandrasekhar, Misra; Godavarthi, Ashok; Vidya, Shimoga M; Hariharapura, Raghu C; Kalthur, Guruprasad; Udupa, Nayanabhirama; Mutalik, Srinivas

2017-11-01

The present work attempts to develop and statistically optimize transfersomes containing EGCG and hyaluronic acid to synergize the UV radiation-protective ability of both compounds, along with imparting antioxidant and anti-aging effects. Transfersomes were prepared by thin film hydration technique, using soy phosphatidylcholine and sodium cholate, combined with high-pressure homogenization. They were characterized with respect to size, polydispersity index, zeta potential, morphology, entrapment efficiency, Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), in vitro antioxidant activity and ex vivo skin permeation studies. Cell viability, lipid peroxidation, intracellular ROS levels and expression of MMPs (2 and 9) were determined in human keratinocyte cell lines (HaCaT). The composition of the transfersomes was statistically optimized by Design of Experiments using Box-Behnken design with four factors at three levels. The optimized transfersome formulation showed vesicle size, polydispersity index and zeta potential of 101.2 ± 6.0 nm, 0.245 ± 0.069 and -44.8 ± 5.24 mV, respectively. FTIR and DSC showed no interaction between EGCG and the selected excipients. XRD results revealed no form conversion of EGCG in its transfersomal form. The optimized transfersomes were found to increase the cell viability and reduce the lipid peroxidation, intracellular ROS and expression of MMPs in HaCaT cells. The optimized transfersomal formulation of EGCG and HA exhibited considerably higher skin permeation and deposition of EGCG than that observed with plain EGCG. The results underline the potential application of the developed transfersomes in sunscreen cream/lotions for improvement of UV radiation-protection along with deriving antioxidant and anti-aging effects.

Adsorption of dodecylamine hydrochloride on graphene oxide in water

NASA Astrophysics Data System (ADS)

Chen, Peng; Li, Hongqiang; Song, Shaoxian; Weng, Xiaoqing; He, Dongsheng; Zhao, Yunliang

Cationic surfactants in water are difficult to be degraded, leading to serious water pollution. In this work, graphene oxide (GO) was used as an adsorbent for removing Dodecylamine Hydrochloride (DACl), a representative cationic surfactant. X-ray diffraction (XRD), FT-IR spectroscopy and atomic force microscope (AFM) were used to characterize the prepared GO. The adsorption of DACl on GO have been investigated through measurements of adsorption capacity, zeta potential, FTIR, and X-ray photoelectron spectroscopy (XPS). The experimental results have shown that the adsorption kinetics could be described as a rate-limiting pseudo second-order process, and the adsorption isotherm agreed well with the Freundlich model. GO was a good adsorbent for DACl removal, compared with coal fly ash and powdered activated carbon. The adsorption process was endothermic, and could be attributed to electrostatic interaction and hydrogen bonding between DACl and GO.

Synthesis and characterization of polyethylene glycol mediated silver nanoparticles by the green method.

PubMed

Shameli, Kamyar; Ahmad, Mansor Bin; Jazayeri, Seyed Davoud; Sedaghat, Sajjad; Shabanzadeh, Parvaneh; Jahangirian, Hossein; Mahdavi, Mahnaz; Abdollahi, Yadollah

2012-01-01

The roles of green chemistry in nanotechnology and nanoscience fields are very significant in the synthesis of diverse nanomaterials. Herein, we report a green chemistry method for synthesized colloidal silver nanoparticles (Ag NPs) in polymeric media. The colloidal Ag NPs were synthesized in an aqueous solution using silver nitrate, polyethylene glycol (PEG), and β-D-glucose as a silver precursor, stabilizer, and reducing agent, respectively. The properties of synthesized colloidal Ag NPs were studied at different reaction times. The ultraviolet-visible spectra were in excellent agreement with the obtained nanostructure studies performed by transmission electron microscopy (TEM) and their size distributions. The Ag NPs were characterized by utilizing X-ray diffraction (XRD), zeta potential measurements and Fourier transform infrared (FT-IR). The use of green chemistry reagents, such as glucose, provides green and economic features to this work.

Preparation and characterization of bee venom-loaded PLGA particles for sustained release.

PubMed

Park, Min-Ho; Jun, Hye-Suk; Jeon, Jong-Woon; Park, Jin-Kyu; Lee, Bong-Joo; Suh, Guk-Hyun; Park, Jeong-Sook; Cho, Cheong-Weon

2016-12-14

Bee venom-loaded poly(lactic-co-glycolic acid) (PLGA) particles were prepared by double emulsion-solvent evaporation, and characterized for a sustained-release system. Factors such as the type of organic solvent, the amount of bee venom and PLGA, the type of PLGA, the type of polyvinyl alcohol, and the emulsification method were considered. Physicochemical properties, including the encapsulation efficiency, drug loading, particle size, zeta-potential and surface morphology were examined by Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and X-ray diffraction (XRD). The size of the bee venom-loaded PLGA particles was 500 nm (measured using sonication). Zeta-potentials of the bee venom-loaded PLGA particles were negative owing to the PLGA. FT-IR results demonstrated that the bee venom was completely encapsulated in the PLGA particles, indicated by the disappearance of the amine and amide peaks. In addition, sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis indicated that the bee venom in the bee venom-loaded PLGA particles was intact. In vitro release of the bee venom from the bee venom-loaded PLGA particles showed a sustained-release profile over 1 month. Bee venom-loaded PLGA particles can help improve patients' quality of life by reducing the number of injections required.

Low-Temperature Synthesis of Anatase TiO2 Nanoparticles with Tunable Surface Charges for Enhancing Photocatalytic Activity

PubMed Central

Li, Ye; Qin, Zhenping; Guo, Hongxia; Yang, Hanxiao; Zhang, Guojun; Ji, Shulan; Zeng, Tingying

2014-01-01

In this work, the positively or negatively charged anatase TiO2 nanoparticles were synthesized via a low temperature precipitation-peptization process (LTPPP) in the presence of poly(ethyleneimine) (PEI) and poly(sodium4- styrenesulfonate) (PSS). X-ray diffraction (XRD) pattern and high-resolution transmission electron microscope (HRTEM) confirmed the anatase crystalline phase. The charges of the prepared TiO2, PEI-TiO2 and PSS-TiO2 nanoparticles were investigated by zeta potentials. The results showed that the zeta potentials of PEI-TiO2 nanoparticles can be tuned from +39.47 mV to +95.46 mV, and that of PSS-TiO2 nanoparticles can be adjusted from −56.63 mV to −119.32 mV. In comparison with TiO2, PSS-TiO2 exhibited dramatic adsorption and degradation of dye molecules, while the PEI modified TiO2 nanoparticles showed lower photocatalytic activity. The photocatalytic performances of these charged nanoparticles were elucidated by the results of UV-vis diffuse reflectance spectra (DRS) and the photoluminescence (PL) spectra, which indicated that the PSS-TiO2 nanoparticles showed a lower recombination rate of electron-hole pairs than TiO2 and PEI-TiO2. PMID:25506839

Competitive adsorption of Pb2+, Cu2+, and Cd2+ ions on microporous titanosilicate ETS-10.

PubMed

Lv, Lu; Hor, Mei Peng; Su, Fabing; Zhao, X S

2005-07-01

In the present study, the competitive adsorption characteristics of binary and ternary heavy metal ions Pb2+, Cu2+, and Cd2+ on microporous titanosilicate ETS-10 were investigated in batch systems. Pure microporous titanosilicate ETS-10 was synthesized with P25 as the Ti source and characterized by the techniques of X-ray diffraction (XRD), field emission-scanning electron microscope (FESEM), nitrogen adsorption, and zeta-potential. Equilibrium and kinetic adsorption data showed that ETS-10 displays a high selectivity toward one metal in a two-component or a three-component system with an affinity order of Pb2+ > Cd2+ > Cu2+. The equilibrium behaviors of heavy metals species with stronger affinity toward ETS-10 can be described by the Langmuir equation while the adsorption kinetics of the metals can be well fitted to a pseudo-second-order (PSO) model.

Synthesis and characterization of a novel mucoadhesive derivative of xyloglucan.

PubMed

Madgulkar, Ashwini R; Bhalekar, Mangesh R; Asgaonkar, Kalyani D; Dikpati, Amrita A

2016-01-01

A novel polymer in the form of a thiolated derivative of natural tamarind seed polysaccharide or xyloglucan was synthesized and its chacteristics as a mucoadhesive polymer were studied as a part of the study undertaken herein. The synthetic route followed involves a two-step reaction mechanism of firstly oxidizing xyloglucan and then further conjugating it with l-cysteine to form thiolated xyloglucan or thiomer via imine linkage. The thiomer thus formed was characterized using various analytical techniques as differential scanning calorimetry (DSC), X-ray diffraction analysis (XRD), and nuclear magnetic resonance (NMR). Ellman's method was used to determine the numbers of thiol groups/g of thiolated xyloglucan. Zeta potential measurements were carried out for thiolated xyloglucan. Viscosities of the formulated xyloglucan and thiolated xyloglucan gels were comparatively evaluated along with the evaluation of mucoadhesive properties of the gels using ex vivo bioadhesion study employing freshly excised sheep intestinal mucosa. Copyright © 2015 Elsevier Ltd. All rights reserved.

Green synthesis of colloidal copper oxide nanoparticles using Carica papaya and its application in photocatalytic dye degradation

NASA Astrophysics Data System (ADS)

Sankar, Renu; Manikandan, Perumal; Malarvizhi, Viswanathan; Fathima, Tajudeennasrin; Shivashangari, Kanchi Subramanian; Ravikumar, Vilwanathan

2014-03-01

Copper oxide (CuO) nanoparticles were synthesized by treating 5 mM cupric sulphate with Carica papaya leaves extract. The kinetics of the reaction was studied using UV-visible spectrophotometry. An intense surface Plasmon resonance between 250-300 nm in the UV-vis spectrum clearly reveals the formation of copper oxide nanoparticles. The results of scanning electron microscopy (SEM) and dynamic light scattering (DLS) exhibited that the green synthesized copper oxide nanoparticles are rod in shape and having a mean particle size of 140 nm, further negative zeta potential disclose its stability at -28.9 mV. The Fourier-transform infrared (FTIR) spectroscopy results examined the occurrence of bioactive functional groups required for the reduction of copper ions. X-ray diffraction (XRD) spectra confirmed the copper oxide nanoparticles crystalline nature. Furthermore, colloidal copper oxide nanoparticles effectively degrade the Coomassie brilliant blue R-250 dye beneath the sunlight.

Amine-functionalized magnetic mesoporous silica nanoparticles for DNA separation

NASA Astrophysics Data System (ADS)

Sheng, Wei; Wei, Wei; Li, Junjian; Qi, Xiaoliang; Zuo, Gancheng; Chen, Qi; Pan, Xihao; Dong, Wei

2016-11-01

We report a modified approach for the functionalized magnetic mesoporous silica nanoparticles (MMSN) using polymer microspheres incorporated with magnetic nanoparticles in the presence of cetyltrimethylammonium bromide (CTAB) and the core-shell magnetic silica nanoparticles (MSN). These particles were functionalized with amino groups via the addition of aminosilane directly to the particle sol. We then evaluate their DNA separation abilities and find the capacity of DNA binding significantly increased (210.22 μg/mg) compared with normal magnetic silica spheres (138.44 μg/mg) by using an ultraviolet and visible spectrophotometer (UV). The morphologies, magnetic properties, particle size, pore size, core-shell structure and Zeta potential are characterized by Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM), Powder X-ray diffraction (XRD), and dynamic light scattering (DLS). This work demonstrates that our MMSN own an excellent potential application in bioseparation and drug delivery.

Controllable biosynthesis of gold nanoparticles from a Eucommia ulmoides bark aqueous extract

NASA Astrophysics Data System (ADS)

Guo, Mingxia; Li, Wei; Yang, Feng; Liu, Huihong

2015-05-01

The present work reports the green synthesis of gold nanoparticles (AuNPs) by water extract of Eucommia ulmoides (E. ulmoides) bark. The effects of various parameters such as the concentration of reactants, pH of the reaction mixture, temperature and the time of incubation were explored to the controlled formation of gold nanoparticles. The characterization through high resolution-transmission electron microscopic (HRTEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) infer that the as-synthesized AuNPs were spherical in shape with a face cubic crystal (FCC) structure. The results from zeta potential and dynamic light scattering (DLS) suggest the good stability and narrow size distribution of the AuNPs. This method for synthesis of AuNPs is simple, economic, nontoxic and efficient. The as-synthesized AuNPs show excellent catalytic activity for the catalytic reducing decoloration of model compounds of azo-dye: reactive yellow 179 and Congo red.

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.

Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

PubMed Central

Predoi, Daniela; Iconaru, Simona Liliana; Deniaud, Aurélien; Chevallet, Mireille; Michaud-Soret, Isabelle; Buton, Nicolas; Prodan, Alina Mihaela

2017-01-01

The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn:HAp) (0.01 < xZn < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn:HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10−xZnx(PO4)6(OH), with 0.01 ≤ xZn ≤ 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out. PMID:28772589

Zeta potential and Raman studies of PVP capped Bi2S3 nanoparticles synthesized by polyol method

NASA Astrophysics Data System (ADS)

Tarachand, Sathe, Vasant G.; Okram, Gunadhor S.

2018-05-01

Here we report the synthesis and characterisation of polyvinylpyrrolidone (PVP) capped Bi2S3 nanoparticles via one step catalyst-free polyol method. Raman spectroscopy, dynamic light scattering and zeta potential analysis were performed on it. Rietveld refinement of powder XRD of PVP capped samples confirmed the formation of single phase orthorhombic Bi2S3 for all PVP capped samples. The presence of eight obvious Raman modes further confirmed the formation of stoichiometric Bi2S3. Dynamic light scattering (DLS) studies show a clear increase in hydrodynamic diameter for samples made with increasing PVP concentration. Particle size obtained from DLS and XRD (using Scherrer's formula) combine with change in full width half maxima of Raman modes collectively suggest overall improvement in crystallinity and quality of product on introducing PVP. In zeta potential (ζ) measurement, steric hindrance of carbon chains plays very crucial role and a systematic reduction of ζ value is observed for samples made with decreasing PVP concentration. An isoelectric point is obtained for sample made with low PVP (1g). Present results are likely to open a window for its medical and catalytic applications.

Green engineering of biomolecule-coated metallic silver nanoparticles and their potential cytotoxic activity against cancer cell lines

NASA Astrophysics Data System (ADS)

Prasannaraj, Govindaraj; Venkatachalam, Perumal

2017-06-01

This report describes the synthesis of metallic silver nanoparticles (AgNPs) using extracts of four medicinal plants (Aegle marmelos (A. marmelos), Alstonia scholaris (A. scholaris), Andrographis paniculata (A. paniculata) and Centella asiatica (C. asiatica)). The bio-conjugates were characterized by UV-visible spectroscopy, scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), Fourier transform infrared spectrometry (FTIR), x-ray diffraction (XRD) and zeta potential. This analysis confirmed that UV-Vis spectral peaks at 375 nm, 380 nm, 420 nm and 380 nm are corresponding to A. marmelos, A. scholaris, A. paniculata and C. asiatica mediated AgNPs, respectively. SEM images revealed that all the obtained four AgNPs are predominantly spherical, fibres and rectangle in shape with an average size of 36-97 nm. SEM-EDS and XRD analysis confirmed the presence of elemental AgNPs in crystalline form for all the four nanoparticle samples. The phytochemicals of various medicinal plant extracts with different functional groups were responsible for reduction of Ag+ to AgNPs, which act as capping and stabilizing agent. Among four types of AgNPs tested for anticancer activity, the Ap mediated AgNPs had shown enhanced activity against HepG2 cells (27.01 µg ml-1) and PC3 cells (32.15 µg ml-1).

Chamomile flower extract-directed CuO nanoparticle formation for its antioxidant and DNA cleavage properties.

PubMed

Duman, Fatih; Ocsoy, Ismail; Kup, Fatma Ozturk

2016-03-01

In this study, we report the synthesis of copper oxide nanoparticles (CuO NPs) using a medicinal plant (Matricaria chamomilla) flower extract as both reducing and capping agent and investigate their antioxidant activity and interaction with plasmid DNA (pBR322).The CuO NPs were characterized using Uv-Vis spectroscopy, FT-IR (Fourier transform infrared spectroscopy), DLS (dynamic light scattering), XRD (X-ray diffraction), EDX (energy-dispersive X-ray) spectroscopy and SEM (scanning electron microscopy). The CuO NPs exhibited nearly mono-distributed and spherical shapes with diameters of 140 nm size. UV-Vis absorption spectrum of CuO NPs gave a broad peak around 285 and 320 nm. The existence of functional groups on the surface of CuO NPs was characterized with FT-IR analysis. XRD pattern showed that the NPs are in the form of a face-centered cubic crystal. Zeta potential value was measured as -20 mV due to the presence of negatively charged functional groups in plant extract. Additionally, we demonstrated concentration-dependent antioxidant activity of CuO NPs and their interaction with plasmid DNA. We assumed that the CuO NPs both cleave and break DNA double helix structure. Copyright © 2015 Elsevier B.V. All rights reserved.

Fungus-mediated synthesis of gold nanoparticles and standardization of parameters for its biosynthesis.

PubMed

Tidke, Pritish R; Gupta, Indarchand; Gade, Aniket K; Rai, Mahendra

2014-12-01

We report the extracellular biosynthesis of gold nanoparticles (AuNPs) using a fungus Fusarium acuminatum. Mycosynthesis of Au-NPs was carried out by challenging the fungal cells filtrate with HAuCl 4 solution (1 mM), as nanoparticles synthesizing enzyme secrete extracellularly by the fungi. The AuNPs were characterized with the help of UV-Visible spectrophotometer, Fourier Transform Infrared spectroscopy, Zeta Potential, X-ray diffraction (XRD) and Transmission electron microscopy (TEM). We observed absorbance peak in between 520 nm-550 nm corresponding to the surface plasmon absorbance of the gold nanoparticles. The nanoparticles synthesized in the present investigation were found to be capped by proteins. XRD results showed that the distinctive formation of crystalline gold nanoparticles in the solution. The spherical and polydispersed AuNPs in the range 8 to 28 nm with average size of 17 nm were observed by TEM analysis. We also standardized the parameters like the effect of pH, temperature and salt concentration on the biosynthesis of gold nanoparticles. It was found that acidic pH, 1 mM salt concentration and 37 (°)C temperature were found to be optimum for the synthesis of Au-NPs. Therefore, the present study introduces the easy, better and cheaper method for biosynthesis of AuNPs.

Nano-graphene oxide carboxylation for efficient bioconjugation applications: a quantitative optimization approach

NASA Astrophysics Data System (ADS)

Imani, Rana; Emami, Shahriar Hojjati; Faghihi, Shahab

2015-02-01

A method for carboxylation of graphene oxide (GO) with chloroacetic acid that precisely optimizes and controls the efficacy of the process for bioconjugation applications is proposed. Quantification of COOH groups on nano-graphene oxide sheets (NGOS) is performed by novel colorimetric methylene blue (MB) assay. The GO is synthesized and carboxylated by chloroacetic acid treatment under strong basic condition. The size and morphology of the as-prepared NGOS are characterized by scanning electron microscopy, transmission electron microscopy (TEM), and atomic force microscopy (AFM). The effect of acid to base molar ratio on the physical, chemical, and morphological properties of NGOS is analyzed by Fourier-transformed infrared spectrometry (FTIR), UV-Vis spectroscopy, X-ray diffraction (XRD), AFM, and zeta potential. For evaluation of bioconjugation efficacy, the synthesized nano-carriers with different carboxylation ratios are functionalized by octaarginine peptide sequence (R8) as a biomolecule model containing amine groups. The quantification of attached R8 peptides to graphene nano-sheets' surface is performed with a colorimetric-based assay which includes the application of 2,4,6-Trinitrobenzene sulfonic acid (TNBS). The results show that the thickness and lateral size of nano-sheets are dramatically decreased to 0.8 nm and 50-100 nm after carboxylation process, respectively. X-ray analysis shows the nano-sheets interlaying space is affected by the alteration of chloroacetic acid to base ratio. The MB assay reveals that the COOH groups on the surface of NGOS are maximized at the acid to base ratio of 2 which is confirmed by FTIR, XRD, and zeta potential. The TNBS assay also shows that bioconjugation of the optimized carboxylated NGOS sample with octaarginine peptide is 2.5 times more efficient compared to bare NGOS. The present work provides evidence that treatment of GO by chloroacetic acid under an optimized condition would create a functionalized high surface area nano-substrate which can be used for subsequent efficient bioconjugation applications.

Preliminary X-ray crystallographic analysis of glutathione transferase zeta 1 (GSTZ1a-1a)

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

Boone, Christopher D.; Zhong, Guo; Smeltz, Marci

2014-01-21

Crystals of glutathione transferase zeta 1 were grown and shown to diffract X-rays to 3.1 Å resolution. They belonged to space group P1, with unit-cell parameters a = 42.0, b = 49.6, c = 54.6 Å, α = 82.9, β = 69.9, γ = 73.4°.

Green synthesis of colloidal copper oxide nanoparticles using Carica papaya and its application in photocatalytic dye degradation.

PubMed

Sankar, Renu; Manikandan, Perumal; Malarvizhi, Viswanathan; Fathima, Tajudeennasrin; Shivashangari, Kanchi Subramanian; Ravikumar, Vilwanathan

2014-01-01

Copper oxide (CuO) nanoparticles were synthesized by treating 5 mM cupric sulphate with Carica papaya leaves extract. The kinetics of the reaction was studied using UV-visible spectrophotometry. An intense surface Plasmon resonance between 250-300 nm in the UV-vis spectrum clearly reveals the formation of copper oxide nanoparticles. The results of scanning electron microscopy (SEM) and dynamic light scattering (DLS) exhibited that the green synthesized copper oxide nanoparticles are rod in shape and having a mean particle size of 140 nm, further negative zeta potential disclose its stability at -28.9 mV. The Fourier-transform infrared (FTIR) spectroscopy results examined the occurrence of bioactive functional groups required for the reduction of copper ions. X-ray diffraction (XRD) spectra confirmed the copper oxide nanoparticles crystalline nature. Furthermore, colloidal copper oxide nanoparticles effectively degrade the Coomassie brilliant blue R-250 dye beneath the sunlight. Copyright © 2013 Elsevier B.V. All rights reserved.

Green synthesis of silver nanoparticles by waste tea extract and degradation of organic dye in the absence and presence of H2O2

NASA Astrophysics Data System (ADS)

Qing, Weixia; Chen, Kui; Wang, Yong; Liu, Xiuhua; Lu, Minghua

2017-11-01

The silver nanoparticles (AgNPs) had been successfully synthesized by using an aqueous extract of waste tea as a stabilizing and reducing agent. The green synthesized AgNPs were characterized by ultraviolet visible (UV-vis) spectroscopy, Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and zeta potential. The work focused on the degradation of methylene blue (MB) and ethyl violet (EV) in aqueous solution with AgNPs as catalyst in the absence and presence of H2O2. The AgNPs exhibit fast, efficient and stable catalytic activity in the degradation of cationic organic dyes, but it is no catalytic degradation of anionic organic dyes at room temperature. The kinetics of dyes degradation with AgNPs follows the pseudo-second-order model. Meanwhile, the AgNPs also show better antimicrobial activity against pathogenic bacteria. The formed highly catalytic active AgNPs can be used as catalyst in industries and water purification.

Preparation and physico-chemical characterization of β-cyclodextrin incorporated chitosan biosorbent beads with potential environmental applications

NASA Astrophysics Data System (ADS)

Munim, Somayyah Abdul; Tahir Saddique, Muhammad; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan

2018-06-01

Biosorption is one of the most efficient and feasible methods for eliminating noxious wastes from the aqueous systems. The use of non-hazardous, low-cost and biodegradable chitosan as a biosorbent is of significant importance in the above context. Present study was aimed to develop a β-cyclodextrin (β-CD) incorporated chitosan biosorbent in the form of beads. The prepared biosorbent beads were characterized using scanning electron microscopy (SEM), Fourier transform infrared (FTIR), x-ray diffraction (XRD) analysis, and thermo gravimetric analysis (TGA). The values of point of zero charge (PZC) of chitosan and β-CD incorporated chitosan beads were determined in the presence of an electrolyte by means of different methods including mass titration, salt addition and zeta potential ones. The SEM images exhibited roughened and porous morphologies which could enhance the adsorption of metal ions. The values of PZC of chitosan and β-CD incorporated chitosan biosorbent beads were found to be 6.38 and 7.12, respectively.

Triton X-100 functionalized Fe3O4 nanoparticles for biomedical applications

NASA Astrophysics Data System (ADS)

Gawali, Santosh L.; Madan, Devendra P.; Barick, K. C.; Somani, R.; Hassan, P. A.

2018-04-01

We report the preparation of Triton X-100 functionalized Fe3O4 nanoparticles (TXMNPs) and investigated their potential application in hyperthermia therapy. The formation of highly crystalline, spinel-structured Fe3O4 nanoparticles of average size of about 10 nm was evident from X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses. Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), UV-visible spectroscopy and zeta-potential measurements suggest the successful functionalization of nanoparticles with TX-100. These TXMNPs exhibit good colloidal stabilization in aqueous medium and show protein resistance characteristic in physiological medium. They showed excellent heating efficacy under AC magnetic field (AMF) with specific absorption rate (SAR) values of 146 and 260 W/g of Fe for 1.25 and 0.625 mg/ml of Fe, respectively at an applied AMF of 507 Oe and frequency of 300 kHz. Thus, these nanoparticles can be used as effective thermoseed for hyperthermia treatment of cancer.

Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

USDA-ARS?s Scientific Manuscript database

Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

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

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

Hepatoprotective effect of engineered silver nanoparticles coated bioactive compounds against diethylnitrosamine induced hepatocarcinogenesis in experimental mice.

PubMed

Prasannaraj, Govindaraj; Venkatachalam, Perumal

2017-02-01

Nanoparticle based drug delivery can rapidly improves the therapeutic potential of anti-cancer agents. The present study focused to evaluate the hepatoprotective activity of silver nanoparticles (AgNPs) synthesized using aqueous extracts of Andrographis paniculata leaves (ApAgNPs) and Semecarpus anacardium nuts (SaAgNPs) against diethylnitrosamine (DEN) induced liver cancer in mice model. The physico-chemical properties of synthesized AgNPs were characterized by Fourier transform infrared (FTIR) spectroscopy, Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), X-ray Diffraction (XRD), Energy Dispersive X-ray (EDX) spectrum, Zeta potential and Dynamic Light Scattering (DLS) analysis. The surface plasmon resonance (SPR) absorption spectrum revealed a strong peak at 420nm for both SaAgNPs and ApAgNPs. FTIR results exhibited the presence of possible functional groups in the synthesized AgNPs. TEM analysis determined the hexagonal, and spherical shape of the synthesized silver nanoparticles. The XRD and SAED pattern confirmed the crystalline nature and crystalline size of the AgNPs. EDX result clearly showed strong silver signals in the range between 2 and 4keV. Zeta potential measurements indicated a sharp peak at -3.93 and -13.8mV for ApAgNPs and SaAgNPs, respectively. DLS measurement expressed the particle size distribution was 70 and 60nm for ApAgNPs and SaAgNPs, respectively. DEN (20mg/kg b.wt.) was subjected to induce liver cancer in mice for 8weeks and treated with biosynthesized silver nanoparticles. Interestingly, ApAgNPs and SaAgNPs treated DEN induced animal groups show a decreased level of aspartate amino transferase (AST), alanine amino transferase (ALT), serum glutamate oxaloacetate transaminase (SGOT), serum glutamate pyruvate transaminase (SGPT) activity and elevated level of catalase (CAT), glutathione peroxidase (GPx), glutathione S-transferase (GST) and superoxide dismutase (SOD) activity over untreated DEN control animals group. Histopathological investigation reveals decreased fat accumulation, appearance of binucleated cells in nanoparticle treated animals and showed mere normal cells induced by DEN. Argyrophilic nucleolar organiser region (AgNORs) had a significant decrease in number of acidic proteins and mast cells assay showed decrease of metachromatic cells in nanoparticles treated animal groups over control. Present results strongly suggest that biomolecule coated silver nanoparticles exposure showed potential hepatoprotective effect against DEN induced liver cancer and could be used as an effective anticancer nanodrug. Copyright © 2017. Published by Elsevier B.V.

Monodispersed spherical shaped selenium nanoparticles (SeNPs) synthesized by Bacillus subtilis and its toxicity evaluation in zebrafish embryos

NASA Astrophysics Data System (ADS)

Chandramohan, Subburaman; Sundar, Krishnan; Muthukumaran, Azhaguchamy

2018-02-01

Selenium is one of the essential elements involved in antioxidative and antiinflammatory effects in human body. By naturally, selenium ions are metabolised and converted into nano selenium. Now a days there is an increasing attention on applications of nanoparticles in therapeutic field. In the present study Bacillus subtilis was used to convert sodium selenite to SeNPs. The synthesized SeNPs were characterized by Fourier Transform Infrared Spectroscopy (FTIR), X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) coupled with Energy Dispersive X ray spectroscopy (EDX). The presence of SeNPs was confirmed by the formation of red colour. The bands were sharp with broad absorption peaks at 3562 cm-1 and 1678-1 cm in FTIR which showed that the bacterial proteins were responsible for the reduction of sodium selenite to SeNPs. The average size of the SeNPs was 334 nm and were spherical in shape with uniform distribution. The XRD data confirmed that SeNPs were of amorphous in nature. The zeta potential of SeNPs was negative in charge which indicated high stability. In the present study zebrafish embryos were used to study the toxicity of SeNPs and the results showed that the concentration beyond 10 μg ml-1 leads to toxic effects in embryos/hatchlings. The lesser concentration of SeNPs can be useful in various biomedical applications.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise.

PubMed

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R; Thorogood, Gordon; Nelwamondo, Aubrey N; Ntsoane, Tshepo P; Roberts, Sarah K; Holliday, Kiel S

2018-01-01

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Effect of Humic Acids and pesticides on Agricultural Soil Structure and Stability and Its Implication on Soil Quality

NASA Astrophysics Data System (ADS)

Gaonkar, O. D.; Nambi, I. M.; G, S. K.

2016-12-01

The functional and morphological aspects of soil structure determine the soil quality. The dispersion of colloidal soil particles, especially the clay fraction and rupture of soil aggregates, both of which play an important role in soil structure development, lead to degradation of soil quality. The main objective of this work was to determine the effect of behaviour of soil colloids on the agricultural soil structure and quality. The effect of commercial humic acid, organophosphate pesticides and soil natural organic matter on the electrical and structural properties of the soil colloids was also studied. Agricultural soil, belonging to the sandy loam texture class from northern part of India was considered in this study. In order to understand the changes in the soil quality in the presence and absence of humic acids, the soil fabric and structure was analyzed by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy (SEM). Electrical properties of natural soil colloids in aqueous suspensions were assessed by zeta potential measurements at varying pH values with and without the presence of humic acids and pesticides. The influence of natural organic matter was analyzed by oxidizing the natural soil organic matter with hydrogen peroxide. The zeta potential of the soil colloids was found to be negative in the pH range studied. The results indicated that hydrogen peroxide treatment lead to deflocculation of colloidal soil particles. In addition, the humic acids undergoes effective adsorption onto the soil surface imparting more negative zeta potential to the colloidal soil particles. The soil hydrophilicity decreased in the presence of humic acids which was confirmed by surface free energy determination. Thus, it can be concluded that the presence of humic acids altered the soil fabric and structure, thereby affecting the soil quality. This study assumes significance in understanding the soil aggregation and the interactions at soil solid-liquid interface.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

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

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE PAGES

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; ...

2018-01-24

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Synthesis of zinc sulfide nanoparticles and their incorporation into poly(hydroxybutyrate) matrix in the formation of a novel nanocomposite

NASA Astrophysics Data System (ADS)

Riaz, Shahina; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan; Jan, Tariq

2018-05-01

In the present study, zinc sulfide (ZnS) nanoparticles (NPs) were successfully synthesized through a modified chemical precipitation protocol and then mediated into poly(hydroxybutyrate) (PHB) matrix to get ZnS/PHB nanocomposite. Mean diameter and zeta potential of ZnS NPs, as determined using dynamic light scattering technique (DLS), were observed to be 53 nm and ‑89 mV, respectively. The structural investigations performed using x-ray diffraction (XRD) technique depicted the phase purity of ZnS NPs exhibiting cubic crystal structure. Fourier transform infrared (FTIR) spectroscopic analysis was conducted to identify the presence or absence of bonding vibrational modes on the surface of synthesized single phase ZnS NPs. The FTIR analysis confirmed the metal to sulphur bond formation by showing the characteristic band at 1123 cm‑1. The UV–vis absorption spectra of ZnS NPs confirmed the synthesis of particles in nanoscale regime showing a λ max of 302 nm. These NPs were then successfully incorporated into PHB matrix to synthesize ZnS/PHB nanocomposite. The synthesis of nanocomposite was confirmed by EDX analysis. The chemical bonding and structural properties of ZnS/PHB nanocomposite were determined by FTIR and XRD analysis, respectively. The FTIR analysis confirmed the synthesis of ZnS/PHB nanocomposite. Moreover, XRD analysis showed that structure of nanocomposite was completely controlled by ZnS NPs as pure PHB exhibited orthorhombic crystal structure while the nanocomposite demonstrated cubic crystal structure of ZnS. Thermal properties of nanocomposite were studied through thermogravimetric analysis revealing that the incorporation of ZnS NPs into PHB matrix lead to enhance heat resistance properties of PHB.

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.;

Design and evaluation of acrylate polymeric carriers for fabrication of pH-sensitive microparticles.

PubMed

Arya, Amit; Majumdar, Dipak K; Pathak, Dharam Pal; Sharma, Anil K; Ray, Alok R

2017-02-01

Colon-targeted microparticles loaded with a model anti-inflammatory drug were fabricated using especially designed acrylic acid-butyl methacrylate copolymers. Microparticles were prepared by oil-in-oil solvent evaporation method using Span 80 as emulsifier. Microparticles were found to be spherical in shape, hemocompatible and anionic with zeta potential of -27.4 and -29.0 mV. Entrapment of drug in the microparticles was confirmed by Fourier transform infrared (FTIR) spectroscopy. However, X-ray diffraction (XRD) and differential scanning calorimetry (DSC) revealed amorphous nature of microparticles due to the dilution effect of amorphous polymer. The microparticles released less than 5% drug at pH 1.2, while more than 90% of the drug load was released at pH 7.4. This suggested the colon targeting nature of the formulations. In experimentally developed colitis in Wistar rats, the microparticle formulation showed significant reduction (p < .05) in the disease activity score (disease symptoms), the colon-to-body weight ratio (tissue edema) and the myeloperoxidase, tumor necrosis factor (TNF)-α and interleukin (IL)-1β activities.

Bioleaching of a low-grade nickel-copper sulfide by mixture of four thermophiles.

PubMed

Li, Shuzhen; Zhong, Hui; Hu, Yuehua; Zhao, Jiancun; He, Zhiguo; Gu, Guohua

2014-02-01

This study investigated thermophilic bioleaching of a low grade nickel-copper sulfide using mixture of four acidophilic thermophiles. Effects of 0.2g/L l-cysteine on the bioleaching process were further evaluated. It aimed at offering new alternatives for enhancing metal recoveries from nickel-copper sulfide. Results showed a recovery of 80.4% nickel and 68.2% copper in 16-day bioleaching without l-cysteine; while 83.7% nickel and 81.4% copper were recovered in the presence of l-cysteine. Moreover, nickel recovery was always higher than copper recovery. l-Cysteine was found contributing to lower pH value, faster microbial growth, higher Oxidation-Reduction Potential (ORP), higher zeta potential and absorbing on the sulfide surfaces through amino, carboxyl and sulfhydryl groups. X-ray Diffraction (XRD) patterns of leached residues showed generation of S, jarosite and ammoniojarosite. Denaturing Gradient Gel Electrophoresis (DGGE) results revealed that l-cysteine could have variant impacts on different microorganisms and changed the microbial community composition dramatically during nickel-copper sulfide bioleaching. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and characterization of biotin modified cholesteryl pullulan as a novel anticancer drug carrier.

PubMed

Yang, Wenzhi; Wang, Miaomiao; Ma, Lilan; Li, Haiying; Huang, Le

2014-01-01

A series of biotin modified cholesteryl pullulan (Bio-CHSP) conjugates with different degrees of substitution (DS) of biotin moiety were synthesized and characterized by Fourier transform infrared (FT-IR), proton nuclear magnetic resonance ((1)H NMR) and X-ray diffraction (XRD). Bio-CHSP conjugates were amphiphilic in nature and their self-aggregation behavior in aqueous media was evaluated by the fluorescence probe technique. Bio-CHSP self-aggregated nanoparticles (Bio-CHSP NPs) were prepared and analyzed by dynamic light scattering (DLS), zeta potential and transmission electron microscopy (TEM) technologies. These novel nanoparticles were almost spherical in shape, and their size, ranging from 178.8 to 100.0 nm. The safety of Bio-CHSP NPs was studied through single dose toxicity test in mice, and the result showed that Bio-CHSP NPs were well tolerated at the intravenous dose of 200 mg/kg in mice. Moreover, as a model anticancer drug, mitoxantrone loaded Bio-CHSP NPs were also prepared and characterized in this study. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effect of surfactant concentration in the electrolyte on the tribological properties of nickel-tungsten carbide composite coatings produced by pulse electro co-deposition

NASA Astrophysics Data System (ADS)

Kartal, Muhammet; Uysal, Mehmet; Gul, Harun; Alp, Ahmet; Akbulut, Hatem

2015-11-01

A nickel plating bath containing WC particles was used to obtain hard and wear-resistant particle reinforced Ni/WC MMCs on steel surfaces for anti-wear applications. Copper substrates were used for electro co-deposition of Ni matrix/WC with the particle size of <1 μm tungsten carbide reinforcements. The influence of surfactant (sodium dodecyl sulfate, SDS) concentration on particle distribution, microhardness and wear resistance of composite coatings has been studied. The nickel films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The effects of the surfactant on the zeta potential, co-deposition and distribution of WC particles in the nickel matrix, as well as the tribological properties of composite coatings were also investigated. The tribological behaviors of the electrodeposited WC composite coatings sliding against M50 steel ball (Ø 10 mm) were examined on a CSM Instrument. All friction and wear tests were performed without lubrication at room temperature and in the ambient air (relative humidity 55-65%).

Gold nanoparticle incorporated polymer/bioactive glass composite for controlled drug delivery application.

PubMed

Jayalekshmi, A C; Sharma, Chandra P

2015-02-01

The present study discusses the development of a biodegradable polymer encapsulated-nanogold incorporated-bioactive glass composite (AuPBG) by a low-temperature method. The composite was analyzed by atomic force microscopy (AFM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetry (TG), fluorescence and dissolution analysis. The composite exhibited aggregation behaviour in solid and solution states and exhibited negative zeta potential (-13.3 ± 1.4 mV). The composite exhibited fast degradation starting from the 5(th) day onwards in phosphate buffered saline (PBS) for a period of 14 days. The composite showed fluorescence quenching effect at pH 7 and the fluorescence recovered at pH 5. The composite has been found to be suitable for the release of doxorubicin at high rates at acidic pH (∼ 5) which is the intracellular pH of tumour cells. The drug loading ratio is also high and it exhibited a controlled release for a period of 8 days in PBS. The system serves as a promising material for targeted drug delivery applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of SLS: APG mixed surfactant systems as carrier for solid dispersion.

PubMed

Patel, Ashok R; Joshi, Vishal Y

2008-01-01

The present investigation aims at studying the effect of mixed surfactant system of sodium lauryl sulphate (SLS) and alkyl polyglucosides (C(10)APG, C(12)APG and C(12/14)APG) on dissolution rate enhancement of poorly water soluble drug. Aceclofenac--a non-steroidal anti-inflammatory agent was used as a model drug as it has limited water solubility. The influence of the surfactant concentration in various blends on dissolution rate of Solid Dispersion (SD), prepared using solution method with ethanol as the solvent was studied and the advantage of mixed surfactant systems over the individual surfactants was illustrated by differences in the in-vitro dissolution profiles of SD. Physico chemical evaluation (critical micellar concentration, zeta potential and beta-parameter calculations) was carried out to study the mixed surfactant systems. Solid mixtures were characterized by Infrared spectroscopy (FT-IR); X-ray diffraction studies (XRD) and scanning electron microscopy (SEM). It was seen that the dissolution rate of aceclofenac from SD increased with the increase in the APG proportion relative to SLS with the optimum ratio of 0.2 SLS:0.8 APG showing the best effect in all cases. Results obtained from physico-chemical evaluation (the decrease in the value of critical micelle concentration and higher negative value of beta-parameters) suggested the existence of synergism between surfactants blends. The observed results in the dissolution rate enhancement could be attributed to the drug--surfactant interactions as evident from FT-IR, SEM and XRD results.

Development of subcutaneous sustained release nanoparticles encapsulating low molecular weight heparin

PubMed Central

Jogala, Satheesh; Rachamalla, Shyam Sunder; Aukunuru, Jithan

2015-01-01

The objective of the present research work was to prepare and evaluate sustained release subcutaneous (s.c.) nanoparticles of low molecular weight heparin (LMWH). The nanoparticles were prepared by water–in-oil in-water (w/o/w) emulsion and evaporation method using different grades of polylactide co-glycolide (50:50, 85:15), and different concentrations of polyvinyl alcohol (0.1%, 0.5%, 1%) aqueous solution as surfactant. The fabricated nanoparticles were evaluated for size, shape, zeta potential, encapsulation efficiency, in vitro drug release, and in vivo biological activity (anti-factor Xa activity) using the standard kit. The drug and excipient compatibility was analyzed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and X-ray diffraction (XRD) studies. The formation of nanoparticles was confirmed by scanning electron microscopy; nanoparticles were spherical in shape. The size of prepared nanoparticles was found between 195 nm and 251 nm. The encapsulation efficiency of the nanoparticles was found between 46% and 70%. In vitro drug, release was about 16–38% for 10 days. In vivo drug, release shows the sustained release of drug for 10 days in rats. FTIR studies indicated that there was no loss in chemical integrity of the drug upon fabrication into nanoparticles. DSC and XRD results demonstrated that the drug was changed from the crystalline form to the amorphous form in the formulation during the fabrication process. The results of this study revealed that the s.c. nanoparticles were suitable candidates for sustained delivery of LMWH. PMID:25878975

Improved physicochemical characteristics of felodipine solid dispersion particles by supercritical anti-solvent precipitation process.

PubMed

Won, Dong-Han; Kim, Min-Soo; Lee, Sibeum; Park, Jeong-Sook; Hwang, Sung-Joo

2005-09-14

Solid dispersions of felodipine were formulated with HPMC and surfactants by the conventional solvent evaporation (CSE) and supercritical anti-solvent precipitation (SAS) methods. The solid dispersion particles were characterized by particle size, zeta potential, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), solubility and dissolution studies. The effects of the drug/polymer ratio and surfactants on the solubility of felodipine were also studied. The mean particle size of the solid dispersions was 200-250 nm; these had a relatively regular spherical shape with a narrow size distribution. The particle size of the solid dispersions from the CSE method increased at 1 h after dispersed in distilled water. However, the particle sizes of solid dispersions from the SAS process were maintained for 6 h due to the increased solubility of felodipine. The physical state of felodipine changed from crystalline to amorphous during the CSE and SAS processes, confirmed by DSC/XRD data. The equilibrium solubility of the felodipine solid dispersion prepared by the SAS process was 1.5-20 microg/ml, while the maximum solubility was 35-110 microg/ml. Moreover, the solubility of felodipine increased with decreasing drug/polymer ratio or increasing HCO-60 content. The solid dispersions from the SAS process showed a high dissolution rate of over 90% within 2 h. The SAS process system may be used to enhance solubility or to produce oral dosage forms with high dissolution rate.

Method of Generating X-Ray Diffraction Data for Integral Detection of Twin Defects in Super-Hetero-Epitaxial Materials

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor); Elliott, James R. (Inventor)

2009-01-01

A method provides X-ray diffraction (XRD) data suitable for integral detection of a twin defect in a strained or lattice-matched epitaxial material made from components having crystal structures having symme try belonging to different space groups. The material is mounted in a n X-ray diffraction (XRD) system. In one embodiment, the XRD system's goniometer angle Omega is set equal to (Theta(sub B)-Beta) where The ta(sub B) is a Bragg angle for a designated crystal plane of the allo y that is disposed at a non-perpendicular orientation with respect to the {111) crystal plane, and Beta is the angle between the designate d crystal plane and a { 111 } crystal plane of one of the epitaxial components. The XRD system's detector angle is set equal to (Theta(su b B)+Beta). The material can be rotated through an angle of azimuthal rotation Phi about the axis aligned with the material. Using the det ector, the intensity of the X-ray diffraction is recorded at least at the angle at which the twin defect occurs.

Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

PubMed

Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

2012-08-01

Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.

Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

NASA Technical Reports Server (NTRS)

Blake, David F.; DeVincenzi, D. (Technical Monitor)

1999-01-01

The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

PubMed

Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

2011-01-01

Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

Green synthesis of gold nanoparticles using Citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) aqueous extract and its characterization.

PubMed

Sujitha, Mohanan V; Kannan, Soundarapandian

2013-02-01

This study reports the biological synthesis of gold nanoparticles by the reduction of HAuCl(4) by using citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) juice extract as the reducing and stabilizing agent. A various shape and size of gold nanoparticles were formed when the ratio of the reactants were altered with respect to 1.0mM chloroauric acid solution. The gold nanoparticles obtained were characterized by UV-visible spectra, transmission electron microscopy (TEM) and X-ray diffraction (XRD). TEM studies showed the particles to be of various shapes and sizes and particle size ranges from 15 to 80 nm. Selected-area electron diffraction (SAED) pattern confirmed fcc phase and crystallinity of the particles. The X-ray diffraction analysis revealed the distinctive facets (111, 200, 220 and 222 planes) of gold nanoparticles. Dynamic light scattering (DLS) studies revealed that the average size for colloid gp(3) of C. limon, C. reticulata and C. sinensis are 32.2 nm, 43.4 nm and 56.7 nm respectively. The DLS graph showed that the particles size was larger and more polydispersed compared to the one observed by TEM due to the fact that the measured size also includes the bio-organic compounds enveloping the core of the Au NPs. Zeta potential value for gold nanoparticles obtained from colloid gp(3) of C. limon, C. reticulata and C. sinensis are -45.9, -37.9 and -31.4 respectively indicating the stability of the synthesized nanoparticles. Herein we propose a novel, previously unexploited method for the biological syntheses of polymorphic gold nanoparticles with potent biological applications. Copyright © 2012 Elsevier B.V. All rights reserved.

Cadmium-free aqueous synthesis of ZnSe and ZnSe@ZnS core-shell quantum dots and their differential bioanalyte sensing potential

NASA Astrophysics Data System (ADS)

Mir, Irshad Ahmad; Rawat, Kamla; Bohidar, H. B.

2016-10-01

Herein we report a facile and cadmium-free approach to prepare water-soluble fluorescent ZnSe@ZnS core-shell quantum dots (QDs), using thioglycolic acid (TGA) ligand as a stabilizer and thiourea as a sulfur source. The optical properties and morphology of the obtained core-shell QDs were characterized by UV-vis and fluorescence spectroscopy, transmission electron microscopy (TEM), energy-dispersive x-ray analysis (EDX), x-ray diffraction (XRD), electrophoresis and dynamic light scattering (DLS) techniques. TEM analysis, and electrophoresis data showed that ZnSe core had an average size of 3.60 ± 0.12 nm and zeta potential of -38 mV; and for ZnSe@ZnS QDs, the mean size was 4.80 ± 0.20 nm and zeta potential was -45 mV. Compared to the core ZnSe QDs, the quantum yield of these core-shell structures was higher (13% versus 32%). These were interacted with five common bioanalytes such as, ascorbic acid, citric acid, oxalic acid, glucose and cholesterol which revealed fluorescence quenching due to concentration dependent binding of analytes to the core only, and core-shell QDs. The binding pattern followed the sequence: cholesterol < glucose < ascorbic acid < oxalic acid < citric acid for ZnSe, and cholesterol < glucose < oxalic acid < ascorbic acid < citric acid for core-shell QDs. Thus, enhanced binding was noticed for the analyte citric acid which may facilitate development of a fluorescence-based sensor based on the ZnSe core-only quantum dot platform. Further, the hydrophilic core-shell structure may find use in cell imaging applications.

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

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

2001-01-01

X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

Roosevelt Hot Springs, Utah FORGE X-Ray Diffraction Data

DOE Data Explorer

Nash, Greg; Jones, Clay

2018-02-07

This dataset contains X-ray diffraction (XRD) data taken from wells and outcrops as part of the DOE GTO supported Utah FORGE project located near Roosevelt Hot Springs. It contains an Excel spreadsheet with the XRD data, a text file with sample site names, types, and locations in UTM, Zone 12, NAD83 coordinates, and a GIS shapefile of the sample locations with attributes.

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

NASA Technical Reports Server (NTRS)

Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

2015-01-01

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

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

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.« less

Synthesis, cytotoxicity, and hydroxyapatite formation in 27-Tris-SBF for sol-gel based CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses

NASA Astrophysics Data System (ADS)

Kaur, Gurbinder; Pickrell, G.; Kimsawatde, G.; Homa, D.; Allbee, H. A.; Sriranganathan, N.

2014-03-01

CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses were prepared via an optimized sol-gel method. The current investigation was focused on producing novel zinc based calcium phosphoborosilicate glasses and to evaluate their mechanical, rheological, and biocompatible properties. The morphology and composition of these glasses were studied using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The particle size, mechanical and flexural strength was also determined. Furthermore, the zeta potential of all the glasses were determined to estimate their flocculation tendency. The thermal analysis and weight loss measurements were carried out using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) respectively. For assessing the in-vitro bioactive character of synthesized glasses, the ability for apatite formation on their surface upon their immersion in simulated body fluid (SBF) was checked using SEM and pH measurements. MTS assay cytotoxicity assay and live-dead cell viability test were conducted on J774A.1 cells murine macrophage cells for different glass concentrations.

Water-dispersible hydroxyapatite nanoparticles synthesized in aqueous solution containing grape seed extract

NASA Astrophysics Data System (ADS)

Zhou, Ruchao; Si, Shaoxiong; Zhang, Qiyi

2012-02-01

A novel and effective method for the preparation of water-dispersible nano-hydroxyapatite (nHAp) particles was reported. nHAp was prepared in the presence of grape seed polyphenol (GSP) solution with different concentrations. Chemical precipitation method was adopted to produce pure nHAp and modified nHAp (nHAp-GSP) at 60 °C for 2 h. The chemical nature of the products was detected by Fourier transform infrared spectroscopy (FTIR) and thermal gravimetric analysis (TGA). Moreover, the crystal structure and morphology of particles was confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results indicated that the spherical nHAp particles with a diameter of 20-50 nm could be synthesized at 60 °C. The zeta potential values of pure nHAp and nHAp-GSP are -0.36 mV and -26.1 mV respectively. According to the sedimentary time, the colloidal stability of nHAp-GSP in water could be improved dramatically with the increase of GSP content and the particles tended to exist as dispersive nanoparticles without aggregation. All the results indicated that GSP exhibited strong binding to nHAp and enhanced the colloidal stability of nHAp particles.

Fabrication of magnetic water-soluble hyperbranched polyol functionalized graphene oxide for high-efficiency water remediation

PubMed Central

Hu, Lihua; Li, Yan; Zhang, Xuefei; Wang, Yaoguang; Cui, Limei; Wei, Qin; Ma, Hongmin; Yan, Liangguo; Du, Bin

2016-01-01

Magnetic water-soluble hyperbranched polyol functionalized graphene oxide nanocomposite (MWHPO-GO) was successfully prepared and applied to water remediation in this paper. MWHPO-GO was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), magnetization curve, zeta potential, scanning electron microscope (SEM) and transmission electron microscope (TEM) analyses. MWHPO-GO exhibited excellent adsorption performance for the removal of synthetic dyes (methylene blue (MB) and methyl violet (MV)) and heavy metal (Pb(II)). Moreover, MWHPO-GO could be simply recovered from water with magnetic separation. The pseudo-second order equation and the Langmuir model exhibited good correlation with the adsorption kinetic and isotherm data, respectively, for these three pollutants. The thermodynamic results (ΔG < 0, ΔH < 0, ΔS < 0) implied that the adsorption process of MB, MV and Pb(II) was feasible, exothermic and spontaneous in nature. A possible adsorption mechanism has been proposed where π-π stacking interactions, H-bonding interaction and electrostatic attraction dominated the adsorption of MB/MV and chelation and electrostatic attraction dominated the adsorption of Pb(II). In addition, the excellent reproducibility endowed MWHPO-GO with the potential for application in water remediation. PMID:27354318

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

Arul, K. Thanigai; Kolanthai, Elayaraja; Manikandan, E.

Highlights: • Rapid technique to synthesize nanorods of magnesium ion incorporated hydroxyapatite. • Enhanced electrical and mechanical properties. • Improved photoluminescence and wettability on magnesium incorporation. • Increased in vitro bioactivity. - Abstract: Nanocrystalline hydroxyapatite (HAp-Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2,} 35 nm) and magnesium (Mg{sup 2+}) ion incorporated HAp were synthesized by microwave technique. XRD (X-ray diffraction), FTIR (Fourier transform infrared spectroscopy), FE-HRTEM (Field emission high resolution transmission electron microscopy), DLS (dynamic light scattering), EDXRF (energy dispersive X-ray fluorescence spectrometry), microhardness, permittivity and alternating current (ac) conductivity, besides the PL (photoluminescence), wettability and in vitro bioactivity of the samples weremore » analysed. EDXRF revealed the Mg{sup 2+} ion incorporation in HAp. The Mg{sup 2+} ion incorporation did not alter the phase but drastically reduced the crystallite size and particle size respectively by 48% and 32%. There was enhanced microhardness (24%) at low level (<13%) and decreased zeta potential of Mg{sup 2+} ion incorporation. The permittivity, ac conductivity, PL, wettability and in vitro bioactivity were enhanced on Mg{sup 2+} ion incorporation. These properties enable them to be a promising candidate for wound healing, bone replacement applications and also as a biosensor.« less

Adsorption of ferrous ions onto montmorillonites

NASA Astrophysics Data System (ADS)

Qin, Dawei; Niu, Xia; Qiao, Min; Liu, Gang; Li, Hongxin; Meng, Zhenxiao

2015-04-01

The adsorption of Fe (II) onto montmorillonites was investigated through initial concentration, contact time, pH and temperature. During the whole adsorption process, the ascorbic acid (Vitamin C) was added as a kind of antioxidant, at the same time, deionized water (after boiling) and nitrogen protection were also used to avoid oxidation. The Fe2+/Fetotal ratio of the iron exists in the Fe-montmorillonites was found more than 95%. Two kinetic models, including pseudo-first-order and pseudo-second-order model, were used to analyze the adsorption process of Fe (II) on montmorillonites. The results of our study showed that adsorption process fitted with pseudo-second-order well. Adsorption isotherms showed that Langmuir model was better than Freundlich model. The thermodynamic parameters ΔG0 and ΔH0 were 3.696 kJ/mol and 6.689 kJ/mol (we just gave the values at 298 K), respectively. The positive values at different temperatures showed that the adsorption process was non-spontaneous and endothermic. The characteristics of materials were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Surface area and porosity analyzer, Thermogravimetric analysis (TGA), Differential scanning calorimeter (DSC) and Zeta potential distribution.

High-pressure homogenization associated hydrothermal process of palygorskite for enhanced adsorption of Methylene blue

NASA Astrophysics Data System (ADS)

Zhang, Zhifang; Wang, Wenbo; Wang, Aiqin

2015-02-01

Palygorskite (PAL) was modified by a high-pressure homogenization assisted hydrothermal process. The effects of modification on the morphology, structure and physicochemical properties of PAL were systematically investigated by Field-emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FTIR), Brunauer-Emmett-Teller (BET) analysis, X-ray diffraction (XRD) and Zeta potential analysis techniques, and the adsorption properties were systematically evaluated using Methylene blue (MB) as the model dye. The results revealed that the crystal bundles were disaggregated and the PAL nanorods became more even after treated via associated high-pressure homogenization and hydrothermal process, and the crystal bundles were dispersed as nanorods. The intrinsic crystal structure of PAL was remained after hydrothermal treatment, and the pore size calculated by the BET method was increased. The adsorption properties of PAL for MB were evidently improved (from 119 mg/g to 171 mg/g) after modification, and the dispersion of PAL before hydrothermal reaction is favorable to the adsorption. The desorption evaluation confirms that the modified PAL has stronger affinity with MB, which is benefit to fabricate a stable organic-inorganic hybrid pigment.

Synthesis, cytotoxicity, and hydroxyapatite formation in 27-Tris-SBF for sol-gel based CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses.

PubMed

Kaur, Gurbinder; Pickrell, G; Kimsawatde, G; Homa, D; Allbee, H A; Sriranganathan, N

2014-03-18

CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses were prepared via an optimized sol-gel method. The current investigation was focused on producing novel zinc based calcium phosphoborosilicate glasses and to evaluate their mechanical, rheological, and biocompatible properties. The morphology and composition of these glasses were studied using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The particle size, mechanical and flexural strength was also determined. Furthermore, the zeta potential of all the glasses were determined to estimate their flocculation tendency. The thermal analysis and weight loss measurements were carried out using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) respectively. For assessing the in-vitro bioactive character of synthesized glasses, the ability for apatite formation on their surface upon their immersion in simulated body fluid (SBF) was checked using SEM and pH measurements. MTS assay cytotoxicity assay and live-dead cell viability test were conducted on J774A.1 cells murine macrophage cells for different glass concentrations.

Synthesis, cytotoxicity, and hydroxyapatite formation in 27-Tris-SBF for sol-gel based CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses

PubMed Central

Kaur, Gurbinder; Pickrell, G.; Kimsawatde, G.; Homa, D.; Allbee, H. A.; Sriranganathan, N.

2014-01-01

CaO-P2O5-SiO2-B2O3-ZnO bioactive glasses were prepared via an optimized sol–gel method. The current investigation was focused on producing novel zinc based calcium phosphoborosilicate glasses and to evaluate their mechanical, rheological, and biocompatible properties. The morphology and composition of these glasses were studied using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The particle size, mechanical and flexural strength was also determined. Furthermore, the zeta potential of all the glasses were determined to estimate their flocculation tendency. The thermal analysis and weight loss measurements were carried out using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) respectively. For assessing the in-vitro bioactive character of synthesized glasses, the ability for apatite formation on their surface upon their immersion in simulated body fluid (SBF) was checked using SEM and pH measurements. MTS assay cytotoxicity assay and live-dead cell viability test were conducted on J774A.1 cells murine macrophage cells for different glass concentrations. PMID:24637634

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders.

PubMed

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng

2017-09-21

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.

Structural characteristics of mixed oxides MOx/SiO2 affecting photocatalytic decomposition of methylene blue

NASA Astrophysics Data System (ADS)

Gun'ko, V. M.; Blitz, J. P.; Bandaranayake, B.; Pakhlov, E. M.; Zarko, V. I.; Sulym, I. Ya.; Kulyk, K. S.; Galaburda, M. V.; Bogatyrev, V. M.; Oranska, O. I.; Borysenko, M. V.; Leboda, R.; Skubiszewska-Zięba, J.; Janush, W.

2012-06-01

A series of photocatalysts based on silica (nanoparticulate) supported titania, ceria, and ceria/zirconia were synthesized and characterized by a variety of techniques including surface area measurements, X-ray diffraction, Fourier transform infrared spectroscopy, zeta potential, surface charge density, and photocatalytic behavior toward methylene blue decomposition. Thermal treatment at 600 °C increases the anatase content of the titania based catalysts detected by XRD. Changes in the infrared spectra before and after thermal treatment indicate that at low temperature there are more tbnd Sisbnd Osbnd Titbnd bonds than at high temperature. As these bonds break upon heating the SiO2 and TiO2 separate, allowing the TiO2 anatase phase to form. This results in an increased catalytic activity for the thermally treated samples. Nearly all titania based samples exhibit a negative surface charge density at pH 7 (initial pH of photocatalytic studies) which aids adsorption of methylene blue. The crystallinity of ceria and ceria/zirconia based catalysts are in some cases limited, and in others non-existent. Even though the energy band gap (Eg) can be lower for these catalysts than for the titania based catalysts, their photocatalytic properties are inferior.

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

In situ X-ray diffraction analysis of (CF x) n batteries: signal extraction by multivariate analysis

DOE PAGES

Rodriguez, Mark A.; Keenan, Michael R.; Nagasubramanian, Ganesan

2007-11-10

In this study, (CF x) n cathode reaction during discharge has been investigated using in situ X-ray diffraction (XRD). Mathematical treatment of the in situ XRD data set was performed using multivariate curve resolution with alternating least squares (MCR–ALS), a technique of multivariate analysis. MCR–ALS analysis successfully separated the relatively weak XRD signal intensity due to the chemical reaction from the other inert cell component signals. The resulting dynamic reaction component revealed the loss of (CF x) n cathode signal together with the simultaneous appearance of LiF by-product intensity. Careful examination of the XRD data set revealed an additional dynamicmore » component which may be associated with the formation of an intermediate compound during the discharge process.« less

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

NASA Astrophysics Data System (ADS)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data.

PubMed

Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed

2012-11-01

New crystallographic tools were developed to access a more precise description of the spin-dependent electron density of magnetic crystals. The method combines experimental information coming from high-resolution X-ray diffraction (XRD) and polarized neutron diffraction (PND) in a unified model. A new algorithm that allows for a simultaneous refinement of the charge- and spin-density parameters against XRD and PND data is described. The resulting software MOLLYNX is based on the well known Hansen-Coppens multipolar model, and makes it possible to differentiate the electron spins. This algorithm is validated and demonstrated with a molecular crystal formed by a bimetallic chain, MnCu(pba)(H(2)O)(3)·2H(2)O, for which XRD and PND data are available. The joint refinement provides a more detailed description of the spin density than the refinement from PND data alone.

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.

In-situ XRD vs ex-situ vacuum annealing of tantalum oxynitride thin films: Assessments on the structural evolution

NASA Astrophysics Data System (ADS)

Cunha, L.; Apreutesei, M.; Moura, C.; Alves, E.; Barradas, N. P.; Cristea, D.

2018-04-01

The purpose of this work is to discuss the main structural characteristics of a group of tantalum oxynitride (TaNxOy) thin films, with different compositions, prepared by magnetron sputtering, and to interpret and compare the structural changes, by X-ray diffraction (XRD), when the samples are vacuum annealed under two different conditions: i) annealing, followed by ex-situ XRD: one sample of each deposition run was annealed at a different temperature, until a maximum of 800 °C, and the XRD patterns were obtained, at room temperature, after each annealing process; ii) annealing with in-situ XRD: the diffraction patterns are obtained, at certain temperatures, during the annealing process, using always the same sample. In-situ XRD annealing could be an interesting process to perform annealing, and analysing the evolution of the structure with the temperature, when compared to the classical process. A higher structural stability was observed in some of the samples, particularly on those with highest oxygen content, but also on the sample with non-metal (O + N) to metal (Ta) ratio around 0.5.

Synthesis of highly stable silver nanoparticles through a novel green method using Mirabillis jalapa for antibacterial, nonlinear optical applications

NASA Astrophysics Data System (ADS)

Pugazhendhi, S.; Palanisamy, P. K.; Jayavel, R.

2018-05-01

Green synthesis techniques are developing as more simplistic and eco-friendly approach for the synthesis of metal nanoparticles compared to chemical reduction methods. Herein we report Synthesis of highly stable silver nanoparticles using Mirabillis jalapa seed extract as a reducing and capping agent. The as-prepared silver nanoparticles were characterized by UV-vis spectroscopy (UV-vis) to confirm the formation of silver nanoparticles by its characteristic surface plasmon resonance peak observed at 420 nm. The Powder X-ray diffraction (P-XRD) revealed the structure and crystalline nature of synthesized silver nanoparticles, The Fourier transform infra-red spectroscopic (FT-IR) revealed the presence of the biomolecules in the extract that acted as reducing as well stabilizing agent. The high resolution transmission electron microscopic (HRTEM) images divulged that the synthesized silver nanoparticles were spherical in shape and poly dispersed. The energy dispersive X-ray diffraction (EDX) profile revealed the elements present in the as-synthesized colloidal silver nanoparticles and its percentages. The Zeta potential measured for silver nanoparticles evidenced that the prepared silver nanoparticles owned high stability in room temperature itself. The as-synthesized silver nanoparticles (AgNPs) in colloidal form were showed good antimicrobial effects and it's were found to exhibit third order optical nonlinearity as studied by Z-scan technique using 532 nm Nd:YAG (SHG) CW laser beam (COHERENT-Compass 215 M-50 diode pumped) output as source. The negative nonlinearity observed was well utilized for the study of optical limiting behavior of the silver nanoparticles.

Green and rapid synthesis of silver nanoparticles using Borago officinalis leaf extract: anticancer and antibacterial activities.

PubMed

Singh, Hina; Du, Juan; Yi, Tae-Hoo

2017-11-01

This study highlights the facile, reliable, cost effective, and ecofriendly synthesis of silver nanoparticles (AgNPs) using Borago officinalis leaves extract efficiently. The biosynthesis of AgNPs was verified by UV-Vis spectrum which showed the surface plasmon resonance (SPR) band at 422 nm. Transmission electron microscope (TEM) analysis revealed that the particles were spherical, hexagonal, and irregular in shape and had size ranging from 30 to 80 nm. The energy dispersive X-ray spectroscopy (EDX) and elemental mapping have displayed the purity and maximum distribution of silver in the AgNPs. The crystalline nature of AgNPs had been identified using X-ray diffraction (XRD) and selected area diffraction pattern (SAED). The particle size analysis revealed that the Z-average diameter of the AgNPs was 50.86 nm with polydispersity index (PDI) 0.136. Zeta potential analysis displayed the colloidal stability of AgNPs. This work also showed the efficacy of AgNPs against lung cancer cell lines (A549) and cervical cancer cell line (HeLa), in vitro. The AgNPs showed cytotoxicity to the A549 and HeLa cancer cell line at the concentrations 5 and 2 μg/ml. The AgNPs were also explored for the antibacterial activity including biofilm inhibition against pathogenic bacteria. The B. officinalis leaves extract can be used efficiently for green synthesis AgNPs. The biosynthesized AgNPs demonstrated potentials as anticancer and antibacterial agents. This work provides helpful insight into the development of new anticancer and antimicrobial agents.

Effect of iron doping on structural and microstructural properties of nanocrystalline ZnSnO3 thin films prepared by spray pyrolysis techniques

NASA Astrophysics Data System (ADS)

Pathan, Idris G.; Suryawanshi, Dinesh N.; Bari, Anil R.; Patil, Lalchand A.

2018-05-01

This work presents the effect of iron doping having different volume ratios (1 ml, 2.5 ml and 5 ml) on the structural, microstructural and electrical properties of zinc stannate thin films, prepared by spray pyrolysis method. These properties were characterized with X-ray diffraction (XRD) and Transmission Electron Microscope (TEM). In our study, XRD pattern indicates that ZnSnO3 has a perovskite phase with face exposed hexahedron structure. The electron diffraction fringes observed are in consistent with the peak observed in XRD patterns. Moreover the sensor reported in our study is cost-effective, user friendly and easy to fabricate.

Pole Figure Explorer v. 1.8

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

Van Benthem, Mark H.

2016-05-04

This software is employed for 3D visualization of X-ray diffraction (XRD) data with functionality for slicing, reorienting, isolating and plotting of 2D color contour maps and 3D renderings of large datasets. The program makes use of the multidimensionality of textured XRD data where diffracted intensity is not constant over a given set of angular positions (as dictated by the three defined dimensional angles of phi, chi, and two-theta). Datasets are rendered in 3D with intensity as a scaler which is represented as a rainbow color scale. A GUI interface and scrolling tools along with interactive function via the mouse allowmore » for fast manipulation of these large datasets so as to perform detailed analysis of diffraction results with full dimensionality of the diffraction space.« less

Solid state synthesis of starch-capped silver nanoparticles.

PubMed

Hebeish, A; Shaheen, Th I; El-Naggar, Mehrez E

2016-06-01

The present research addresses the establishment of a technique which is solely devoted to environmentally friendly one-pot green synthesis of dry highly stable powdered silver nanoparticles (AgNPs) using starch as both reductant and stabilizing agent in the presence of sodium hydroxide. It is believed that the sodium hydroxide can improve the reduction potential of starch. Thus when the alkali treated starch is submitted to addition of silver nitrate (AgNO3), the alkali treated starch induces the well-established dual role of starch; reduction of silver ions (Ag(+)) to AgNPs and capping the as-formed AgNPs to prevent them from further growth and agglomeration. Beside assessment of AgNPs formation, structural and morphological characteristics of AgNPs are investigated by making use of UV-vis spectroscopy, transmission electron microscopy (TEM), dynamic light scattering (DLS), zeta potential, FT-IR and X-ray diffraction (XRD) analysis. Research outputs signify (a) the absorbance around 410-420nm in the UV-vis spectra of AgNPs appears most, probably owing to the presence of nanosized silver particles and the intensity of this peak increases by increasing AgNO3 concentration; (b) that highly stable AgNPs with well-dispersed particle are successfully prepared using the present research-based innovation; (c) that the size of AgNPs does not exceed 30nm with sphere-like morphology even at the highest Ag(+) concentration employed during synthesis operation; (d) that the XRD and FT-IR confirm the successful preparation of pure AgNPs without noticeable impurities; (d) and that the one-pot synthesis of powdered AgNPs in large scale is clean and easily operated and easily transportation which may be applied as per demands of industries such as textile and painting industry. Copyright © 2016. Published by Elsevier B.V.

Nanoethosomal formulation of gammaoryzanol for skin-aging protection and wrinkle improvement: a histopathological study.

PubMed

Heydari, Saman; Ghanbarzadeh, Saeed; Anoush, Behzad; Ranjkesh, Mohammadreza; Javadzadeh, Yousef; Kouhsoltani, Maryam; Hamishehkar, Hamed

2017-07-01

Free radical scavengers and antioxidants, with the main focus on enhanced targeting to the skin layers, can provide protection against skin ageing. The aim of the present study was to prepare nanoethosomal formulation of gammaoryzanol (GO), a water insoluble antioxidant, for its dermal delivery to prevent skin aging. Nanoethosomal formulation was prepared by a modified ethanol injection method and characterized by using laser light scattering, scanning electronic microscope (SEM) and X-ray diffraction (XRD) techniques. The effects of formulation parameters on nanoparticle size, encapsulation efficiency percent (EE%) and loading capacity percent (LC%) were investigated. Antioxidant activity of GO-loaded formulation was investigated in vitro using normal African green monkey kidney fibroblast cells (Vero). The effect of control and GO-loaded nanoethosomal formulation on superoxide dismutase (SOD) and malondialdehyde (MDA) content of rat skin was also probed. Furthermore, the effect of GO-loaded nanoethosomes on skin wrinkle improvement was studied by dermoscopic and histological examination on healthy humans and UV-irradiated rats, respectively. The optimized nanoethosomal formulation showed promising characteristics including narrow size distribution 0.17 ± 0.02, mean diameter of 98.9 ± 0.05 nm, EE% of 97.12 ± 3.62%, LC% of 13.87 ± 1.36% and zeta potential value of -15.1 ± 0.9 mV. The XRD results confirmed uniform drug dispersion in the nanoethosomes structure. In vitro and in vivo antioxidant studies confirmed the superior antioxidant effect of GO-loaded nanoethosomal formulation compared with control groups (blank nanoethosomes and GO suspension). Nanoethosomes was a promising carrier for dermal delivery of GO and consequently had superior anti-aging effect.

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

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.;

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

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

2004-01-01

Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

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.

Modeling and measurements of XRD spectra of extended solids under high pressure

NASA Astrophysics Data System (ADS)

Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

2017-06-01

We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

Structural Characterization and Antifungal Studies of Zinc-Doped Hydroxyapatite Coatings.

PubMed

Iconaru, Simona Liliana; Prodan, Alina Mihaela; Buton, Nicolas; Predoi, Daniela

2017-04-09

The present study is focused on the synthesis, characterization and antifungal evaluation of zinc-doped hydroxyapatite (Zn:HAp) coatings. The Zn:HAp coatings were deposited on a pure Si (Zn:HAp_Si) and Ti (Zn:HAp_Ti) substrate by a sol-gel dip coating method using a zinc-doped hydroxyapatite nanogel. The nature of the crystal phase was determined by X-ray diffraction (XRD). The crystalline phase of the prepared Zn:HAp composite was assigned to hexagonal hydroxyapatite in the P6 3/m space group. The colloidal properties of the resulting Zn:HAp (x Zn = 0.1) nanogel were analyzed by Dynamic Light Scattering (DLS) and zeta potential. Scanning Electron Microscopy (SEM) was used to investigate the morphology of the zinc-doped hydroxyapatite (Zn:HAp) nanogel composite and Zn:HAp coatings. The elements Ca, P, O and Zn were found in the Zn:HAp composite. According to the EDX results, the degree of Zn substitution in the structure of Zn:HAp composite was 1.67 wt%. Moreover, the antifungal activity of Zn:HAp_Si and Zn:HAp_Ti against Candida albicans ( C. albicans ) was evaluated. A decrease in the number of surviving cells was not observed under dark conditions, whereas under daylight and UV light illumination a major decrease in the number of surviving cells was observed.

Comparative assessment of toxicity of ZnO and amine-functionalized ZnO nanorods toward Daphnia magna in acute and chronic multigenerational tests.

PubMed

Gonçalves, Renata Amanda; de Oliveira Franco Rossetto, Ana Letícia; Nogueira, Diego José; Vicentini, Denice Schulz; Matias, William Gerson

2018-04-01

Zinc oxide nanomaterials (ZnO NM) have been used in a large number of applications due to their interesting physicochemical properties. However, the increasing use of ZnO NM has led to concerns regarding their environmental impacts. In this study, the acute and chronic toxicity of ZnO nanorods (NR) bare (ZnONR) and amine-functionalized (ZnONR@AF) toward the freshwater microcrustacean Daphnia magna was evaluated. The ZnO NR were characterized by transmission electron microscopy (TEM), X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and the zeta potential and hydrodynamic diameter (HD). The acute EC50 (48h) values for D. magna revealed that the ZnONR@AF were more toxic than the ZnONR. The generation of reactive oxygen species (ROS) was observed in both NM. Regarding the chronic toxicity, the ZnONR@AF were again found to be more toxic than the ZnONR toward D. magna. An effect on longevity was observed for ZnONR, while ZnONR@AF affected the reproduction, growth and longevity. In the multigenerational recovery test, we observed that maternal exposure can affect the offspring even when these organisms are not directly exposed to the ZnO NR. Copyright © 2018 Elsevier B.V. All rights reserved.

High ink absorption performance of inkjet printing based on SiO2@Al13 core-shell composites

NASA Astrophysics Data System (ADS)

Chen, YiFan; Jiang, Bo; Liu, Li; Du, Yunzhe; Zhang, Tong; Zhao, LiWei; Huang, YuDong

2018-04-01

The increasing growth of the inkjet market makes the inkjet printing more necessary. A composite material based on core-shell structure has been developed and applied to prepare inkjet printing layer. In this contribution, the ink printing record layers based on SiO2@Al13 core-shell composite was elaborated. The prepared core-shell composite materials were characterized by X-ray photoelectron spectroscopy (XPS), zeta potential, X-ray diffraction (XRD), scanning electron microscopy (SEM). The results proved the presence of electrostatic adsorption between SiO2 molecules and Al13 molecules with the formation of the well-dispersed system. In addition, based on the adsorption and the liquid permeability analysis, SiO2@Al13 ink printing record layer achieved a relatively high ink uptake (2.5 gmm-1) and permeability (87%), respectively. The smoothness and glossiness of SiO2@Al13 record layers were higher than SiO2 record layers. The core-shell structure facilitated the dispersion of the silica, thereby improved its ink absorption performance and made the clear printed image. Thus, the proposed procedure based on SiO2@Al13 core-shell structure of dye particles could be applied as a promising strategy for inkjet printing.

Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

PubMed

Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

2018-06-01

This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders

PubMed Central

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong

2017-01-01

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH4)2C2O4·H2O and Na2CO3) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7–10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na2CO3 precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed. PMID:28934147

Manipulation of partially oriented hydroxyapatite building blocks to form flowerlike bundles without acid-base regulation.

PubMed

Wen, Zhenliang; Wang, Zihao; Chen, Jingdi; Zhong, Shengnan; Hu, Yimin; Wang, Jianhua; Zhang, Qiqing

2016-06-01

The application of hydroxyapatite (HAP) in different fields depends greatly on its morphology, composition and structure. Besides, the main inorganic building blocks of human bones and teeth are also HAP. Therefore, accurate shape and aggregation control and of hydroxyapatite particles will be of great interest. Herein, oriented bundles of flowerlike HAP nanorods were successfully prepared through hydrothermal treatment without acid-base regulation, with the mono-alkyl phosphate (MAP) and sodium citrate as surfactant and chelating agent, respectively. The prepared samples were characterized by the X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and zeta potential, the pH value and conductivity value of suspension were characterized by pH meter and conductivity measurement. The results showed that the MAP and citrate play an important role in assembly of HAP nanorods without acid-base regulation. Citrate calcium complex could decompose slowly and release citrate ions at hydrothermal conditions. Besides, the further decomposition of citrate ions could release aconitic acid as the reaction time prolongs. Moreover, the possible scheme for the formation process was discussed in detail. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of nanocellulose from Imperata brasiliensis grass using Taguchi method.

PubMed

Benini, Kelly Cristina Coelho de Carvalho; Voorwald, Herman Jacobus Cornelis; Cioffi, Maria Odila Hilário; Rezende, Mirabel Cerqueira; Arantes, Valdeir

2018-07-15

Cellulose nanoparticles (CNs) were prepared by acid hydrolysis of the cellulose pulp extracted from the Brazilian satintail (Imperata Brasiliensis) plant using a conventional and a total chlorine free method. Initially, a statistical design of experiment was carried out using Taguchi orthogonal array to study the hydrolysis parameters, and the main properties (crystallinity, thermal stability, morphology, and sizes) of the nanocellulose. X-ray diffraction (XRD), fourier-transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy (FE-SEM), dynamic light scattering (DLS), zeta potential and thermogravimetric analysis (TGA) were carried out to characterize the physical-chemical properties of the CNs obtained. Cellulose nanoparticles with diameter ranging from 10 to 60 nm and length between 150 and 250 nm were successfully obtained at sulfuric acid concentration of 64% (m/m), temperature 35 °C, reaction time 75 min, and a 1:20 (g/mL) pulp-to-solution ratio. Under this condition, the Imperata Brasiliensis CNs showed good stability in suspension, crystallinity index of 65%, and a cellulose degradation temperature of about 117 °C. Considering that these properties are similar to those of nanocelluloses from other lignocellulosics feedstocks, Imperata grass seems also to be a suitable source for nanocellulose production. Copyright © 2018 Elsevier Ltd. All rights reserved.

Evaluation of antibacterial efficacy of phyto fabricated silver nanoparticles using Mukia scabrella (Musumusukkai) against drug resistance nosocomial gram negative bacterial pathogens.

PubMed

Prabakar, Kandasamy; Sivalingam, Periyasamy; Mohamed Rabeek, Siyed Ibrahim; Muthuselvam, Manickam; Devarajan, Naresh; Arjunan, Annavi; Karthick, Rajamanickam; Suresh, Micky Maray; Wembonyama, John Pote

2013-04-01

Given the fact in the limitation of the therapeutic options for emerging multidrug resistance gram-negative bacteria (MDR-GNB) of respiratory tract infections, the present study was focused on green synthesis of antimicrobial silver nanoparticles (AgNPs) using leaf extract of Mukia scabrella. An obvious color change to brown color and surface plasmon resonance by UV-visible spectroscopy (UV-vis) indicated a well observable peak at 440 nm confirming the synthesis of AgNPs. Fourier transform infra-red spectroscopy (FTIR) analysis indicates protein as possible capping agents. Energy dispersive X-ray (EDAX) spectroscopy results showed major signal for elemental silver. X-ray diffraction (XRD) analysis indicates the formation of metallic silver nanomaterials. Transmission electron microscopic (TEM) study showed the nanoparticles in the size range of 18-21 nm with spherical shape. Zeta potential analysis showed -21.7 mV characteristic for stable AgNPs. The biosynthesized AgNPs exhibited significant antimicrobial activity against MDR-GNB nosocomial pathogens of Acinetobacter sp., Klebsiella pneumoniae and Pseudomonas aeruginosa. Results from the current study suggested that M. scabrella material could be exploited for the fabrication of AgNPs with potential therapeutic applications in nanomedicine especially for nosocomial bacterial infections. Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation of PEO/Clay Nanocomposites Using Organoclay Produced via Micellar Adsorption of CTAB

PubMed Central

Gürses, Ahmet; Ejder-Korucu, Mehtap; Doğar, Çetin

2012-01-01

The aim of this study was the preparation of polyethylene oxide (PEO)/clay nanocomposites using organoclay produced via micellar adsorption of cethyltrimethyl ammonium bromide (CTAB) and their characterisation by X-ray diffraction (XRD), and Fourier transform infrared (FT-IR) spectra, and the investigation of certain mechanical properties of the composites. The results show that the basal distance between the layers increased with the increasing CTAB/clay ratio as parallel with the zeta potential values of particles. By considering the aggregation number of CTAB micelles and interlayer distances of organo-clay, it could be suggested that the predominant micelle geometry at lower CTAB/clay ratios is an ellipsoidal oblate, whereas, at higher CTAB/clay ratios, sphere-ellipsoid transition occurs. The increasing tendency of the exfoliation degree with an increase in clay content may be attributed to easier diffusion of PEO chains to interlayer regions. FT-IR spectra show that the intensity of Si-O stretching vibrations of the organoclays (1050 cm−1) increased, especially in the ratios of 1.0 g/g clay and 1.5 g/g clay with the increasing CTAB content. It was observed that the mechanical properties of the composites are dependent on both the CTAB/clay ratios and clay content of the composites. PMID:23365515

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

2004-01-01

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

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.

Concave Urinary Crystallines: Direct Evidence of Calcium Oxalate Crystals Dissolution by Citrate In Vivo

PubMed Central

Shang, Yun-Feng; Xu, Meng; Zhang, Guang-Na; Ouyang, Jian-Ming

2013-01-01

The changes in urinary crystal properties in patients with calcium oxalate (CaOx) calculi after oral administration of potassium citrate (K3cit) were investigated via atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray powder diffractometry (XRD), and zeta potential analyzer. The AFM and SEM results showed that the surface of urinary crystals became concave, the edges and corners of crystals became blunt, the average size of urinary crystallines decreased significantly, and aggregation of urinary crystals was reduced. These changes were attributed to the significant increase in concentration of excreted citrate to 492 ± 118 mg/L after K3cit intake from 289 ± 83 mg/L before K3cit intake. After the amount of urinary citrate was increased, it complexed with Ca2+ ions on urinary crystals, which dissolved these crystals. Thus, the appearance of concave urinary crystals was a direct evidence of CaOx dissolution by citrate in vivo. The XRD results showed that the quantities and species of urinary crystals decreased after K3cit intake. The mechanism of inhibition of formation of CaOx stones by K3cit was possibly due to the complexation of Ca2+ with citrate, increase in urine pH, concentration of urinary inhibitor glycosaminoglycans (GAGs), and the absolute value of zeta potential after K3cit intake. PMID:24363634

Development and characterization of parenteral nanoemulsions containing thalidomide.

PubMed

Araújo, F A; Kelmann, R G; Araújo, B V; Finatto, R B; Teixeira, H F; Koester, L S

2011-02-14

This study reports the development of nanoemulsions intended for intravenous administration of thalidomide (THD). The formulations were prepared by spontaneous emulsification method and optimized with respect to thalidomide (0.01-0.05%, w/w), and hydrophilic emulsifier (polysorbate 80; 0.5-4.0%, w/w) content. The formulations were evaluated concerning physical appearance and drug crystallization; droplet size; zeta potential and drug assay. Only the formulation containing 0.01% THD and 0.5% polysorbate kept its properties in a satisfactory range over the evaluated period (60 days), i.e. droplet size around 200nm, drug content around 95% and zeta potential around -30mV. The transmission electron microscopy revealed emulsion droplets almost spherical in shape confirming the results obtained by photon correlation spectroscopy. Drug crystallization observed for higher content (THD 0.05%, w/w) nanoemulsions was investigated. The crystals observed at optical microscopy presented a different crystal habit compared to that of the raw material used. It was speculated whether the kind of THD polymorph employed could influence nanoemulsion formulation. Formulations were prepared with either one of THD polymorphs (β- or α-) and crystals were characterized by fourier transformed infrared spectroscopy (FTIR) and X-ray diffraction (XRD). It was observed that regardless of the polymorph employed (β- or α-), drug crystallization occurs in the α-form. THD solubility in oils was not influenced by the polymorphic form. In addition, the in vitro dissolution profile of the selected formulation (THD 0.01%, w/w; polysorbate 0.5%, w/w) was assessed by bulk-equilibrium reverse dialysis sac technique and demonstrated a release profile similar to that of a THD acetonitrile solution, with around 95% THD being dissolved within 4h. Finally, a pharmacokinetic simulation of an intravenous infusion of 250mL of the selected nanoemulsion suggests that the parenteral administration of a dose as low as 25mg might lead to therapeutic plasma concentrations of thalidomide. Copyright © 2010 Elsevier B.V. All rights reserved.

Bacillus thuringiensis coated zinc oxide nanoparticle and its biopesticidal effects on the pulse beetle, Callosobruchus maculatus.

PubMed

Malaikozhundan, Balasubramanian; Vaseeharan, Baskaralingam; Vijayakumar, Sekar; Thangaraj, Merlin P

2017-09-01

Insect pests belonging to the genus Callosobruchus are the major cause of damage to stored pulse crops. Recently, nanotechnology has emerged as a promising tool for pest control. In the present study, we report for the first time the synthesis and biological evaluation of Bacillus thuringiensis coated zinc oxide nanoparticles (Bt-ZnO NPs) on the pulse beetle, Callosobruchus maculatus. The biologically synthesized Bt-ZnO NPs were extensively characterized using UV-Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and Zeta potential. The bio-physical characterization revealed that the Bt-ZnO NPs has a hexagonal wurtzite structures with an average particle size of 20nm. In addition, zeta potential measurement demonstrated that the Bt-ZnO NPs are negatively charged (-12.7mV) and are moderately stable. The biopesticidal effect of Bt-ZnO NPs was tested against the pulse beetle, C. maculatus. Treatment with Bt-ZnO NPs reduced the fecundity (eggs laid) and hatchability of C. maculatus in a dose-dependent manner. A significant delay in the larval, pupal and total development period of C. maculatus was observed after treatment with Bt-ZnO NPs at 25μg/mL. Furthermore, Bt-ZnO NPs are highly effective in the control of C. maculatus and caused 100% mortality at 25μg/mL. The LC 50 value was estimated to be 10.71μg/mL. In addition, treatment with Bt-ZnO NPs decreased the mid-gut α-amylase, cysteine protease, α-glucosidase and glutathione S-transferase (GST) activity in C. maculatus. Our results suggest that Bt-ZnO NPs are effective against C. maculatus and could be used as nanobiopesticides in the control of stored grain insect pests in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

Final Report for X-ray Diffraction Sample Preparation Method Development

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

Ely, T. M.; Meznarich, H. K.; Valero, T.

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Metastable and equilibrium phase formation in sputter-deposited Ti/Al multilayer thin films

NASA Astrophysics Data System (ADS)

Lucadamo, G.; Barmak, K.; Lavoie, C.; Cabral, C., Jr.; Michaelsen, C.

2002-06-01

The sequence and kinetics of metastable and equilibrium phase formation in sputter deposited multilayer thin films was investigated by combining in situ synchrotron x-ray diffraction (XRD) with ex situ electron diffraction and differential scanning calorimetry (DSC). The sequence included both cubic and tetragonal modifications of the equilibrium TiAl3 crystal structure. Values for the formation activation energies of the various phases in the sequence were determined using the XRD and DSC data obtained here, as well as activation energy data reported in the literature.

An X-ray diffraction method for semiquantitative mineralogical analysis of Chilean nitrate ore

USGS Publications Warehouse

Jackson, J.C.; Ericksent, G.E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

An x-ray diffraction method for semiquantitative mineralogical analysis of chilean nitrate ore

USGS Publications Warehouse

John, C.; George, J.; Ericksen, E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

Nanostructured mesoporous silica: influence of the preparation conditions on the physical-surface properties for efficient organic dye uptake

NASA Astrophysics Data System (ADS)

Morsi, Rania E.; Mohamed, Rasha S.

2018-03-01

A series of ordered mesoporous silica such as MCM-41, SBA-3 and SBA-15, in addition to silica micro- (SM) and nano- (SN) mesoporous particles, were prepared. The preparation conditions were found to greatly influence the physical-surface properties including morphological structure, porosity, particle size, aggregate average size, surface area, pore size, pore volume and zeta potential of the prepared silica, while the chemical structure, predicted from FT-IR spectra, and the diffraction patterns, predicted from wide-angle X-ray diffraction spectra, were identical. Surface areas of approximately 1500, 1027, 600, 552 and 317 m2 g-1, pore volumes of 0.93, 0.56, 0.82, 0.72 and 0.5 cm3 g-1, radii of 2.48, 2.2, 5.66, 6.6 and 8.98 nm, average aggregate sizes of 56, 65.4, 220.9, 73, 61.1 and 261 nm and zeta potential values of -32.8, -46.1, -26.3, -31.4 and -25.9 mV were obtained for MCM-41, SBA-3, SBA-15, SN and SM, respectively. Methylene blue dye uptake capacity of the prepared silica types was investigated using the batch technique and, in addition, the most effective material was further studied by the column flow system. The kinetics and isotherms of the uptake process were studied. The morphological structure, surface area, pore radius and zeta potential values were the most correlated factors.

Nanostructured mesoporous silica: influence of the preparation conditions on the physical-surface properties for efficient organic dye uptake.

PubMed

Morsi, Rania E; Mohamed, Rasha S

2018-03-01

A series of ordered mesoporous silica such as MCM-41, SBA-3 and SBA-15, in addition to silica micro- (SM) and nano- (SN) mesoporous particles, were prepared. The preparation conditions were found to greatly influence the physical-surface properties including morphological structure, porosity, particle size, aggregate average size, surface area, pore size, pore volume and zeta potential of the prepared silica, while the chemical structure, predicted from FT-IR spectra, and the diffraction patterns, predicted from wide-angle X-ray diffraction spectra, were identical. Surface areas of approximately 1500, 1027, 600, 552 and 317 m 2  g -1 , pore volumes of 0.93, 0.56, 0.82, 0.72 and 0.5 cm 3  g -1 , radii of 2.48, 2.2, 5.66, 6.6 and 8.98 nm, average aggregate sizes of 56, 65.4, 220.9, 73, 61.1 and 261 nm and zeta potential values of -32.8, -46.1, -26.3, -31.4 and -25.9 mV were obtained for MCM-41, SBA-3, SBA-15, SN and SM, respectively. Methylene blue dye uptake capacity of the prepared silica types was investigated using the batch technique and, in addition, the most effective material was further studied by the column flow system. The kinetics and isotherms of the uptake process were studied. The morphological structure, surface area, pore radius and zeta potential values were the most correlated factors.

X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

NASA Astrophysics Data System (ADS)

Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

2017-05-01

Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

Structural properties and electrochemistry of α-LiFeO2

NASA Astrophysics Data System (ADS)

Abdel-Ghany, A. E.; Mauger, A.; Groult, H.; Zaghib, K.; Julien, C. M.

2012-01-01

In this work, we study the physico-chemistry and electrochemistry of lithium ferrite synthesized by solid-state reaction. Characterization included X-ray diffraction (XRD), scanning electronic microscopy (SEM), Raman scattering (RS), Fourier transform infrared spectroscopy (FTIR), and SQUID magnetometry. XRD peaks gradually sharpen with increasing firing temperature; all the diffraction peaks can be indexed to the cubic α-LiFeO2 phase (Fm3m space group) with the refined cell parameter a = 4.155 Å. RS and FTIR spectra show the vibrational modes due to covalent Fe-O bonds and the Li-cage mode at low-frequency. The electrochemical properties of Li/LiFeO2 are revisited along with the post-mortem analysis of the positive electrode material using XRD and Raman experiments.

Ostwald ripening and interparticle-diffraction effects for illite crystals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.

1988-01-01

The Warren-Averbach method, an X-ray diffraction (XRD) method used to measure mean particle thickness and particle-thickness distribution, is used to restudy sericite from the Silverton caldera. Apparent particle-thickness distributions indicate that the clays may have undergone Ostwald ripening and that this process has modified the K-Ar ages of the samples. The mechanism of Ostwald ripening can account for many of the features found for the hydrothermal alteration of illite. Expandabilities measured by the XRD peak-position method for illite/smectites (I/S) from various locations are smaller than expandabilities measured by transmission electron microscopy (TEM) and by the Warren-Averbach (W-A) method. This disparity is interpreted as being related to the presence of nonswelling basal surfaces that form the ends of stacks of illite particles (short-stack effect), stacks that, according to the theory of interparticle diffraction, diffract as coherent X-ray scattering domains. -from Authors

Structural changes in shock compressed silicon observed using time-resolved x-ray diffraction at the Dynamic Compression Sector

NASA Astrophysics Data System (ADS)

Turneaure, Stefan; Zdanowicz, E.; Sinclair, N.; Graber, T.; Gupta, Y. M.

2015-06-01

Structural changes in shock compressed silicon were observed directly using time-resolved x-ray diffraction (XRD) measurements at the Dynamic Compression Sector at the Advanced Photon Source. The silicon samples were impacted by polycarbonate impactors accelerated to velocities greater than 5 km/s using a two-stage light gas gun resulting in impact stresses of about 25 GPa. The 23.5 keV synchrotron x-ray beam passed through the polycarbonate impactor, the silicon sample, and an x-ray window (polycarbonate or LiF) at an angle of 30 degrees relative to the impact plane. Four XRD frames (~ 100 ps snapshots) were obtained with 153.4 ns between frames near the time of impact. The XRD measurements indicate that in the peak shocked state, the silicon samples completely transformed to a high-pressure phase. XRD results for both shocked polycrystalline silicon and single crystal silicon will be presented and compared. Work supported by DOE/NNSA.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

PubMed

Chung, Frank H

2017-05-01

For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

A Curved Image-Plate Detector System for High-Resolution Synchrotron X-ray Diffraction

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

Sarin, P.; Haggerty, R; Yoon, W

2009-01-01

The developed curved image plate (CIP) is a one-dimensional detector which simultaneously records high-resolution X-ray diffraction (XRD) patterns over a 38.7 2{theta} range. In addition, an on-site reader enables rapid extraction, transfer and storage of X-ray intensity information in {le}30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X-ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate,more » regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X-ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high-temperature XRD.« less

Simple X-ray diffraction algorithm for direct determination of cotton crystallinity

USDA-ARS?s Scientific Manuscript database

Traditionally, XRD had been used to study the crystalline structure of cotton celluloses. Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI), in its present state, XRD measurement can only provide a qualitative or semi-quantitative assessme...

PyXRD v0.6.7: a free and open-source program to quantify disordered phyllosilicates using multi-specimen X-ray diffraction profile fitting

NASA Astrophysics Data System (ADS)

Dumon, M.; Van Ranst, E.

2016-01-01

This paper presents a free and open-source program called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The validity of the program was checked by comparing its output with Sybilla v2.2.2, which shares the same mathematical formalism. The novelty of this program is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. PyXRD thus allows for modelling multiple specimens side by side, and this approach speeds up the manual refinement process significantly. To check the hypothesis that this multi-specimen set-up - as it effectively reduces the number of parameters and increases the number of observations - can also improve automatic parameter refinements, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for one refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups, which do not contain enough information to discern all minerals present (e.g. patterns of heated samples). Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

Measurement of fundamental illite particle thicknesses by X-ray diffraction using PVP-10 intercalation

USGS Publications Warehouse

Eberl, D.D.; Nüesch, R.; Šucha, Vladimír; Tsipursky, S.

1998-01-01

The thicknesses of fundamental illite particles that compose mixed-layer illite-smectite (I-S) crystals can be measured by X-ray diffraction (XRD) peak broadening techniques (Bertaut-Warren-Averbach [BWA] method and integral peak-width method) if the effects of swelling and XRD background noise are eliminated from XRD patterns of the clays. Swelling is eliminated by intercalating Na-saturated I-S with polyvinylpyrrolidone having a molecular weight of 10,000 (PVP-10). Background is minimized by using polished metallic silicon wafers cut perpendicular to (100) as a substrate for XRD specimens, and by using a single-crystal monochromator. XRD measurements of PVP-intercalated diagenetic, hydrothermal and low-grade metamorphic I-S indicate that there are at least 2 types of crystallite thickness distribution shapes for illite fundamental particles, lognormal and asymptotic; that measurements of mean fundamental illite particle thicknesses made by various techniques (Bertant-Warren-Averbach, integral peak width, fixed cation content, and transmission electron microscopy [TEM]) give comparable results; and that strain (small differences in layer thicknesses) generally has a Gaussian distribution in the log-normal-type illites, but is often absent in the asymptotic-type illites.

Application of graphene oxide-poly (vinyl alcohol) polymer nanocomposite for memory devices

NASA Astrophysics Data System (ADS)

Kaushal, Jyoti; Kaur, Ravneet; Sharma, Jadab; Tripathi, S. K.

2018-05-01

Significant attention has been gained by polymer nanocomposites because of their possible demands in future electronic memory devices. In the present work, device based on Graphene Oxide (GO) and polyvinyl alcohol (PVA) has been made and examined for the memory device application. The prepared Graphene oxide (GO) and GO-PVA nanocomposite (NC) has been characterized by X-ray Diffraction (XRD). GO nanosheets show the diffraction peak at 2θ = 11.60° and the interlayer spacing of 0.761 nm. The XRD of GO-PVA NC shows the diffraction peak at 2θ =18.56°. The fabricated device shows bipolar switching behavior having ON/OFF current ratio ˜102. The Write-Read-Erase-Read (WRER) cycles test shows that the Al/GO-PVA/Ag device has good stability and repeatability.

Thermal behaviour and microanalysis of coal subbituminus

NASA Astrophysics Data System (ADS)

Heriyanti; Prendika, W.; Ashyar, R.; Sutrisno

2018-04-01

Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRD) is used to study the thermal behaviour of sub-bituminous coal. The DSC experiment was performed in air atmosphere up to 125 °C at a heating rate of 25 °C min1. The DSC curve showed that the distinct transitional stages in the coal samples studied. Thermal heating temperature intervals, peak and dissociation energy of the coal samples were also determined. The XRD analysis was used to evaluate the diffraction pattern and crystal structure of the compounds in the coal sample at various temperatures (25-350 °C). The XRD analysis of various temperatures obtained compounds from the coal sample, dominated by quartz (SiO2) and corundum (Al2O3). The increase in temperature of the thermal treatment showed a better crystal formation.

Synthesis and structural characterization of polyaniline/cobalt chloride composites

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

Asha, E-mail: arana5752@gmail.com; Goyal, Sneh Lata; Kishore, Nawal

2016-05-23

Polyaniline (PANI) and PANI /cobalt chloride composites were synthesized by in situ chemical oxidative polymerization of aniline with CoCl{sub 2}.6H{sub 2}O using ammonium peroxidisulphate as an oxidant. These composites were characterized by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). The XRD study reveals that both PANI and composites are amorphous. The XRD and SEM results confirm the presence of cobalt chloride in the composites.

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

L-arginine modified magnetic nanoparticles: green synthesis and characterization

NASA Astrophysics Data System (ADS)

Bagherpour, A. R.; Kashanian, F.; Seyyed Ebrahimi, S. A.; Habibi-Rezaei, M.

2018-02-01

In recent years, there has been considerable interest in Arg which is a unique, nontoxic, and biocompatible biomolecule since it can be utilized as an agent for the functionalization and subsequent stabilization of MNPs against oxidation and aggregation, during or after a synthesis procedure. Our studies demonstrate that Arg has great impacts on MNPs with the decreasing size of the particle. Also, saturation magnetization and electrostatic interactions of RMNPs have a direct impact on biological molecules such as proteins and nucleic acids. By controlling the concentration of Arg, it is possible to accurately control the above-mentioned characteristics, which are useful tools for applications such as connecting to antibodies, catalysis, drug loading, and modification of MNP stability. In the current study, three RMNPs with different Arg densities, i.e. 0.42, 1.62, and 2.29 μg per mg were successfully synthesized through a simple co-precipitation method (named p 0.5, p 1, and p 1.5, respectively) and verified by colorimetric determination. Also, the as-synthesized RMNP powders were characterized by XRD, SEM/EDAX, FTIR, VSM, and zeta potential analysis. The presence of a magnetic core was proved by XRD, FTIR, and EDAX. Colorimetric analysis showed the existence of Arg in the synthesized samples. According to the zeta potential and VSM results, increasing the cap of Arg on the MNP surface leads to an increase in the surface charge and decrease in the magnetization of the RMNPs, respectively.

Nanostructured mesoporous silica: influence of the preparation conditions on the physical-surface properties for efficient organic dye uptake

PubMed Central

Mohamed, Rasha S.

2018-01-01

A series of ordered mesoporous silica such as MCM-41, SBA-3 and SBA-15, in addition to silica micro- (SM) and nano- (SN) mesoporous particles, were prepared. The preparation conditions were found to greatly influence the physical-surface properties including morphological structure, porosity, particle size, aggregate average size, surface area, pore size, pore volume and zeta potential of the prepared silica, while the chemical structure, predicted from FT-IR spectra, and the diffraction patterns, predicted from wide-angle X-ray diffraction spectra, were identical. Surface areas of approximately 1500, 1027, 600, 552 and 317 m2 g−1, pore volumes of 0.93, 0.56, 0.82, 0.72 and 0.5 cm3 g−1, radii of 2.48, 2.2, 5.66, 6.6 and 8.98 nm, average aggregate sizes of 56, 65.4, 220.9, 73, 61.1 and 261 nm and zeta potential values of −32.8, −46.1, −26.3, −31.4 and −25.9 mV were obtained for MCM-41, SBA-3, SBA-15, SN and SM, respectively. Methylene blue dye uptake capacity of the prepared silica types was investigated using the batch technique and, in addition, the most effective material was further studied by the column flow system. The kinetics and isotherms of the uptake process were studied. The morphological structure, surface area, pore radius and zeta potential values were the most correlated factors. PMID:29657800

The Effect of Compaction Force on the Transition to Hydrate of Anhydrous Aripiprazole.

PubMed

Togo, Taichiro; Taniguchi, Toshiya; Nakata, Yoshitaka

2018-01-01

Aripiprazole (APZ) is used to treat schizophrenia and is administered as a tablet containing the anhydrous form of APZ. In this study, the effect of compaction force on the crystal form transition was investigated. The crystalline state was observed by X-ray diffraction (XRD). APZ Anhydrous Form II was compacted into tablets. The XRD intensity of anhydrous APZ became lower with higher compressive force. The degree of crystallinity decreased with the compaction force. The powder and the compacted tablets of anhydrous APZ were stored for one week under 60°C and 75% relative humidity. The powder showed no crystal form transition after storage. For the tablets, however, XRD peaks of APZ hydrate were observed after storage. The tablets compacted with higher force showed the higher XRD diffraction intensity of hydrate form. We concluded that the crystallinity reduction of APZ Anhydrous Form II by compaction caused and accelerated the transition to hydrate under high temperature and humidity conditions. In order to manufacture crystallographically stable tablets containing anhydrous APZ, it is important to prevent this crystallinity reduction during compaction.

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.

X-Ray Diffraction of different samples of Swarna Makshika Bhasma.

PubMed

Gupta, Ramesh Kumar; Lakshmi, Vijay; Jha, Chandra Bhushan

2015-01-01

Shodhana and Marana are a series of complex procedures that identify the undesirable effects of heavy metals/minerals and convert them into absorbable and assimilable forms. Study on the analytical levels is essential to evaluate the structural and chemical changes that take place during and after following such procedures as described in major classical texts to understand the mystery behind these processes. X-Ray Diffraction (XRD) helps to identify and characterize minerals/metals and fix up the particular characteristics pattern of prepared Bhasma. To evaluate the chemical changes in Swarna Makshika Bhasma prepared by using different media and methods. In this study, raw Swarna Makshika, purified Swarna Makshika and four types of Swarna Makshika Bhasma prepared by using different media and methods were analyzed by XRD study. XRD study of different samples revealed strongest peaks of iron oxide in Bhasma. Other phases of Cu2O, FeS2, Cu2S, FeSO4, etc., were also identified in many of the samples. XRD study revealed that Swarna Makshika Bhasma prepared by Kupipakwa method is better, convenient, and can save time.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

PubMed Central

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

2013-01-01

Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

Simultaneous femtosecond X-ray spectroscopy and diffraction of photosystem II at room temperature.

PubMed

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; Difiore, Dörte; Milathianaki, Despina; Fry, Alan R; Miahnahri, Alan; Schafer, Donald W; Messerschmidt, Marc; Seibert, M Marvin; Koglin, Jason E; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J; Grosse-Kunstleve, Ralf W; Zwart, Petrus H; White, William E; Glatzel, Pieter; Adams, Paul D; Bogan, Michael J; Williams, Garth J; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K; Yachandra, Vittal K; Bergmann, Uwe; Yano, Junko

2013-04-26

Intense femtosecond x-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous x-ray diffraction (XRD) and x-ray emission spectroscopy (XES) of microcrystals of photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD-XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation-sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies.

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Characterization of mineral phases of agricultural soil samples of Colombian coffee using Mössbauer spectroscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Rodríguez, Humberto Bustos; Lozano, Dagoberto Oyola; Martínez, Yebrayl Antonio Rojas; Pinilla, Marlene Rivera; Alcázar, German Antonio Pérez

2012-03-01

Soil chemical analysis, X-ray diffraction (XRD) and Mössbauer spectrometry (MS) of 57Fe were used to characterize mineral phases of samples taken from the productive layer (horizon A) of agricultural coffee soil from Tolima (Colombia). Chemical analysis shows the chemical and textural parameters of samples from two different regions of Tolima, i.e., Ibagué and Santa Isabel. By XRD phases like illite (I), andesine (A) and quartz (Q) in both samples were identified. The quantity of these phases is different for the two samples. The MS spectra taken at room temperature were adjusted by using five doublets, three of them associated to Fe + 3 type sites and the other two to Fe + 2 type sites. According to their isomer shift and quadrupole splitting the presence of phases like illite (detected by DRX), nontronite and biotite (not detected by XRD) can be postulated.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

On-the-fly segmentation approaches for x-ray diffraction datasets for metallic glasses

DOE PAGES

Ren, Fang; Williams, Travis; Hattrick-Simpers, Jason; ...

2017-08-30

Investment in brighter sources and larger detectors has resulted in an explosive rise in the data collected at synchrotron facilities. Currently, human experts extract scientific information from these data, but they cannot keep pace with the rate of data collection. Here, we present three on-the-fly approaches—attribute extraction, nearest-neighbor distance, and cluster analysis—to quickly segment x-ray diffraction (XRD) data into groups with similar XRD profiles. An expert can then analyze representative spectra from each group in detail with much reduced time, but without loss of scientific insights. As a result, on-the-fly segmentation would, therefore, result in accelerated scientific productivity.

Sand sources and transport pathways for the San Francisco Bay coastal system, based on X-ray diffraction mineralogy

USGS Publications Warehouse

Hein, James R.; Mizell, Kira; Barnard, Patrick L.; Barnard, P.L.; Jaffee, B.E.; Schoellhamer, D.H.

2013-01-01

The mineralogical compositions of 119 samples collected from throughout the San Francisco Bay coastal system, including bayfloor and seafloor, area beaches, cliff outcrops, and major drainages, were determined using X-ray diffraction (XRD). Comparison of the mineral concentrations and application of statistical cluster analysis of XRD spectra allowed for the determination of provenances and transport pathways. The use of XRD mineral identifications provides semi-quantitative compositions needed for comparisons of beach and offshore sands with potential cliff and river sources, but the innovative cluster analysis of XRD diffraction spectra provides a unique visualization of how groups of samples within the San Francisco Bay coastal system are related so that sand-sized sediment transport pathways can be inferred. The main vector for sediment transport as defined by the XRD analysis is from San Francisco Bay to the outer coast, where the sand then accumulates on the ebb tidal delta and also moves alongshore. This mineralogical link defines a critical pathway because large volumes of sediment have been removed from the Bay over the last century via channel dredging, aggregate mining, and borrow pit mining, with comparable volumes of erosion from the ebb tidal delta over the same period, in addition to high rates of shoreline retreat along the adjacent, open-coast beaches. Therefore, while previously only a temporal relationship was established, the transport pathway defined by mineralogical and geochemical tracers support the link between anthropogenic activities in the Bay and widespread erosion outside the Bay. The XRD results also establish the regional and local importance of sediment derived from cliff erosion, as well as both proximal and distal fluvial sources. This research is an important contribution to a broader provenance study aimed at identifying the driving forces for widespread geomorphic change in a heavily urbanized coastal-estuarine system.

Magnetic liposomes for colorectal cancer cells therapy by high-frequency magnetic field treatment

NASA Astrophysics Data System (ADS)

Hardiansyah, Andri; Huang, Li-Ying; Yang, Ming-Chien; Liu, Ting-Yu; Tsai, Sung-Chen; Yang, Chih-Yung; Kuo, Chih-Yu; Chan, Tzu-Yi; Zou, Hui-Ming; Lian, Wei-Nan; Lin, Chi-Hung

2014-09-01

In this study, we developed the cancer treatment through the combination of chemotherapy and thermotherapy using doxorubicin-loaded magnetic liposomes. The citric acid-coated magnetic nanoparticles (CAMNP, ca. 10 nm) and doxorubicin were encapsulated into the liposome (HSPC/DSPE/cholesterol = 12.5:1:8.25) by rotary evaporation and ultrasonication process. The resultant magnetic liposomes ( ca. 90 to 130 nm) were subject to characterization including transmission electron microscopy (TEM), dynamic light scattering (DLS), X-ray diffraction (XRD), zeta potential, Fourier transform infrared (FTIR) spectrophotometer, and fluorescence microscope. In vitro cytotoxicity of the drug carrier platform was investigated through 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay using L-929 cells, as the mammalian cell model. In vitro cytotoxicity and hyperthermia (inductive heating) studies were evaluated against colorectal cancer (CT-26 cells) with high-frequency magnetic field (HFMF) exposure. MTT assay revealed that these drug carriers exhibited no cytotoxicity against L-929 cells, suggesting excellent biocompatibility. When the magnetic liposomes with 1 μM doxorubicin was used to treat CT-26 cells in combination with HFMF exposure, approximately 56% cells were killed and found to be more effective than either hyperthermia or chemotherapy treatment individually. Therefore, these results show that the synergistic effects between chemotherapy (drug-controlled release) and hyperthermia increase the capability to kill cancer cells.

Investigation on Synthesis, Stability, and Thermal Conductivity Properties of Water-Based SnO2/Reduced Graphene Oxide Nanofluids

PubMed Central

Yu, Xiaofen; Wu, Qibai; Zhang, Haiyan; Zeng, Guoxun; Li, Wenwu; Qian, Yannan; Li, Yang; Yang, Guoqiang; Chen, Muyu

2017-01-01

With the rapid development of industry, heat removal and management is a major concern for any technology. Heat transfer plays a critically important role in many sectors of engineering; nowadays utilizing nanofluids is one of the relatively optimized techniques to enhance heat transfer. In the present work, a facile low-temperature solvothermal method was employed to fabricate the SnO2/reduced graphene oxide (rGO) nanocomposite. X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectroscope (XPS), Raman spectroscopy, and transmission electron microscopy (TEM) have been performed to characterize the SnO2/rGO nanocomposite. Numerous ultrasmall SnO2 nanoparticles with average diameters of 3–5 nm were anchored on the surface of rGO, which contain partial hydrophilic functional groups. Water-based SnO2/rGO nanofluids were prepared with various weight concentrations by using an ultrasonic probe without adding any surfactants. The zeta potential was measured to investigate the stability of the as-prepared nanofluid which exhibited great dispersion stability after quiescence for 60 days. A thermal properties analyzer was employed to measure thermal conductivity of water-based SnO2/rGO nanofluids, and the results showed that the enhancement of thermal conductivity could reach up to 31% at 60 °C under the mass fraction of 0.1 wt %, compared to deionized water. PMID:29280972

Preparation of 1D Hierarchical Material Mesosilica/Pal Composite and Its Performance in the Adsorption of Methyl Orange

PubMed Central

Wu, Mei; Han, Haifeng; Ni, Lingli; Song, Daiyun; Li, Shuang; Hu, Tao; Jiang, Jinlong; Chen, Jing

2018-01-01

This paper highlights the synthesis of a one-dimensional (1D) hierarchical material mesosilica/palygorskite (Pal) composite and evaluates its adsorption performance for anionic dye methyl orange (MO) in comparison with Pal and Mobile crystalline material-41 (MCM-41). The Mesosilica/Pal composite is consisted of mesosilica coated Pal nanorods and prepared through a dual template approach using cetyltrimethyl ammonium bromide (CTAB) and Pal as soft and hard templates, respectively. The composition and structure of the resultant material was characterized by a scanning electron microscope (SEM), transmissionelectron microscopy (TEM), N2 adsorption-desorption analysis, small-angle X-Ray powder diffraction (XRD), and zeta potential measurement. Adsorption experiments were carried out with different absorbents at different contact times and pH levels. Compared with Pal and MCM-41, the mesosilica/Pal composite exhibited the best efficiency for MO adsorption. Its adsorption ratio is as high as 70.4%. Its adsorption equilibrium time is as short as 30 min. Results testify that the MO retention is promoted for the micro-mesoporous hierarchical structure and positive surface charge electrostatic interactions of the mesosilica/Pal composite. The regenerability of the mesosilica/Pal composite absorbent was also assessed. 1D morphology makes it facile to separate from aqueous solutions. It can be effortlessly recovered and reused for up to nine cycles. PMID:29361713

Preparation of 1D Hierarchical Material Mesosilica/Pal Composite and Its Performance in the Adsorption of Methyl Orange.

PubMed

Wu, Mei; Han, Haifeng; Ni, Lingli; Song, Daiyun; Li, Shuang; Hu, Tao; Jiang, Jinlong; Chen, Jing

2018-01-20

This paper highlights the synthesis of a one-dimensional (1D) hierarchical material mesosilica/palygorskite (Pal) composite and evaluates its adsorption performance for anionic dye methyl orange (MO) in comparison with Pal and Mobile crystalline material-41 (MCM-41). The Mesosilica/Pal composite is consisted of mesosilica coated Pal nanorods and prepared through a dual template approach using cetyltrimethyl ammonium bromide (CTAB) and Pal as soft and hard templates, respectively. The composition and structure of the resultant material was characterized by a scanning electron microscope (SEM), transmissionelectron microscopy (TEM), N₂ adsorption-desorption analysis, small-angle X-Ray powder diffraction (XRD), and zeta potential measurement. Adsorption experiments were carried out with different absorbents at different contact times and pH levels. Compared with Pal and MCM-41, the mesosilica/Pal composite exhibited the best efficiency for MO adsorption. Its adsorption ratio is as high as 70.4%. Its adsorption equilibrium time is as short as 30 min. Results testify that the MO retention is promoted for the micro-mesoporous hierarchical structure and positive surface charge electrostatic interactions of the mesosilica/Pal composite. The regenerability of the mesosilica/Pal composite absorbent was also assessed. 1D morphology makes it facile to separate from aqueous solutions. It can be effortlessly recovered and reused for up to nine cycles.

Characterization of the Microstructure of the Compositionally Complex Alloy Al1Mo0.5Nb1Ta0.5Ti1Zr1 (Postprint)

DTIC Science & Technology

2016-05-01

limited to X-ray diffraction ( XRD ) and scanning electron microscopy (SEM). The alloy was reported to contain two bcc phases with similar lattice...it appears that the interface between the two phases is fairly coherent. Interestingly, the XRD study described in [8] suggested that there were two...line-scan shown in (h). 3 Distribution A. Approved for public reledifference in lattice parameter measurements realized in bulk samples ( XRD ) vs

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

Micro-X-ray diffraction assessment of shock stage in enstatite chondrites

NASA Astrophysics Data System (ADS)

Izawa, Matthew R. M.; Flemming, Roberta L.; Banerjee, Neil R.; McCausland, Philip J. A.

2011-05-01

A new method for assessing the shock stage of enstatite chondrites has been developed, using in situ micro-X-ray diffraction (μXRD) to measure the full width at half maximum (FWHMχ) of peak intensity distributed along the direction of the Debye rings, or chi angle (χ), corresponding to individual lattice reflections in two-dimensional XRD patterns. This μXRD technique differs from previous XRD shock characterization methods: it does not require single crystals or powders. In situ μXRD has been applied to polished thin sections and whole-rock meteorite samples. Three frequently observed orthoenstatite reflections were measured: (020), (610), and (131); these were selected as they did not overlap with diffraction lines from other phases. Enstatite chondrites are commonly fine grained, stained or darkened by weathering, shock-induced oxidation, and metal/sulfide inclusions; furthermore, most E chondrites have little olivine or plagioclase. These characteristics inhibit transmitted-light petrography, nevertheless, shock stages have been assigned MacAlpine Hills (MAC) 02837 (EL3) S3, Pecora Escarpment (PCA) 91020 (EL3) S5, MAC 02747 (EL4) S4, Thiel Mountains (TIL) 91714 (EL5) S2, Allan Hills (ALHA) 81021 (EL6) S2, Elephant Moraine (EET) 87746 (EH3) S3, Meteorite Hills (MET) 00783 (EH4) S4, EET 96135 (EH4-5) S2, Lewis Cliff (LEW) 88180 (EH5) S2, Queen Alexandra Range (QUE) 94204 (EH7) S2, LaPaz Icefield (LAP) 02225 (EH impact melt) S1; for the six with published shock stages, there is agreement with the published classification. FWHMχ plotted against petrographic shock stage demonstrates positive linear correlation. FWHMχ ranges corresponding to shock stages were assigned as follows: S1 < 0.7°, S2 = 0.7-1.2°, S3 = 1.2-2.3°, S4 = 2.3-3.5°, S5 > 3.5°, S6—not measured. Slabs of Abee (EH impact-melt breccia), and Northwest Africa (NWA) 2212 (EL6) were examined using μXRD alone; FWHMχ values place both in the S2 range, consistent with literature values. Micro-XRD analysis may be applicable to other shocked orthopyroxene-bearing rocks.

THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

Rapid synthesis of Ti-MCM-41 by microwave-assisted hydrothermal method towards photocatalytic degradation of oxytetracycline.

PubMed

Chen, Hanlin; Peng, Yen-Ping; Chen, Ku-Fan; Lai, Chia-Hsiang; Lin, Yung-Chang

2016-06-01

This study employed microwave-assisted hydrothermal method to synthesize Ti-MCM-41, which are mesoporous materials with a high surface area and excellent photocatalytic ability. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) were employed. The XRD findings showed that Ti-MCM-41 exhibited a peak at 2θ of 2.2°, which was attributed to the hexagonal MCM-41 structure. The BET (Brunauer-Emmett-Teller) results agreed with the TEM findings that Ti-MCM-41 has a pore size of about 3-5nm and a high surface area of 883m(2)/g. FTIR results illustrated the existence of Si-O-Si and Si-O-Ti bonds in Ti-MCM-41. The appearance of Ti 2p peaks in the XPS results confirmed the FTIR findings that the Ti was successfully doped into the MCM-41 structure. Zeta (ζ)-potential results indicated that the iso-electric point (IEP) of Ti-MCM-41 was at about pH3.02. In this study, the photocatalytic degradation of oxytetracycline (OTC) at different pH was investigated under Hg lamp irradiation (wavelength 365nm). The rate constant (K'obs) for OTC degradation was 0.012min(-1) at pH3. Furthermore, TOC (total organic carbon) and high resolution LC-MS (liquid chromatography-mass spectrometry) analyses were conducted to elucidate the possible intermediate products and degradation pathway for OTC. The TOC removal efficiency of OTC degradation was 87.0%, 74.4% and 50.9% at pH3, 7 and 10, respectively. LC-MS analysis results showed that the degradation products from OTC resulted from the removal of functional groups from the OTC ring. Copyright © 2016. Published by Elsevier B.V.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

PubMed

Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

PubMed

Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

2009-09-01

Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

Growth of high quality and large-sized Rb 0.3MoO 3 single crystals by molten salt electrolysis method

NASA Astrophysics Data System (ADS)

Wang, Junfeng; Xiong, Rui; Yi, Fan; Yin, Di; Ke, Manzhu; Li, Changzhen; Liu, Zhengyou; Shi, Jing

2005-05-01

High quality and large-sized Rb 0.3MoO 3 single crystals were synthesized by molten salt electrolysis method. X-ray diffraction (XRD) patterns and rocking curves, as well as the white beam Laue diffraction of X-ray images show the crystals grown by this method have high quality. The lattice constants evaluated from XRD patterns are a0=1.87 nm, b0=0.75 nm, c0=1.00 nm, β=118.83∘. The in situ selected area electron diffraction (SAED) patterns along the [101¯], [11¯1¯] and [103¯] zone axes at room temperature indicate that the Rb 0.3MoO 3 crystal possess perfect C-centered symmetry. Temperature dependence of the resistivity shows this compound undergoes a metal to semiconductor transition at 183 K.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

NASA Astrophysics Data System (ADS)

Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

A novel bio-degradable polymer stabilized Ag/TiO2 nanocomposites and their catalytic activity on reduction of methylene blue under natural sun light.

PubMed

Geetha, D; Kavitha, S; Ramesh, P S

2015-11-01

In the present work we defined a novel method of TiO2 doped silver nanocomposite synthesis and stabilization using bio-degradable polymers viz., chitosan (Cts) and polyethylene glycol (PEG). These polymers are used as reducing agents. The instant formation of AgNPs was analyzed by visual observation and UV-visible spectrophotometer. TiO2 nanoparticles doped at different concentrations viz., 0.03, 0.06 and 0.09mM on PEG/Cts stabilized silver (0.04wt%) were successfully synthesized. This study presents a simple route for the in situ synthesis of both metal and polymer confined within the nanomaterial, producing ternary hybrid inorganic-organic nanomaterials. The results reveal that they have higher photocatalytic efficiencies under natural sun light. The synthesized TiO2 doped Ag nanocomposites (NCs) were characterized by SEM/EDS, TEM, XRD, FTIR and DLS with zeta potential. The stability of Ag/TiO2 nanocomposite is due to the high negative values of zeta potential and capping of constituents present in the biodegradable polymer which is evident from zeta potential and FT-IR studies. The XRD and EDS pattern of synthesized Ag/TiO2 NCs showed their crystalline structure, with face centered cubic geometry oriented in (111) plane. AFM and DLS studies revealed that the diameter of stable Ag/TiO2 NCs was approximately 35nm. Moreover the catalytic activity of synthesize Ag/TiO2 NCs in the reduction of methylene blue was studied by UV-visible spectrophotometer. The synthesized Ag/TiO2 NCs are observed to have a good catalytic activity on the reduction of methylene blue by bio-degradable which is confirmed by the decrease in absorbance maximum value of methylene blue with respect to time using UV-vis spectrophotometer. The significant enhancement in the photocatalytic activity of Ag/TiO2 nanocomposites under sun light irradiation can be ascribed to the effect of noble metal Ag by acting as electron traps in TiO2 band gap. Copyright © 2015. Published by Elsevier Inc.

Structure of chitosan thermosensitive gels containing graphene oxide

NASA Astrophysics Data System (ADS)

Tylman, Michał; Pieklarz, Katarzyna; Owczarz, Piotr; Maniukiewicz, Waldemar; Modrzejewska, Zofia

2018-06-01

The supramolecular hydrogels of chitosan and graphene oxide (GO) have been prepared at temperature of the human body, by controlling the concentration of GO and ratio of chitosan to GO. During the preparation of gels the sodium β-glycerophosphate (Na-β-GP) was used as a neutralizing agent. The structure of obtained gels was determined on the basis of FTIR spectra and XRD diffraction patterns. The results of structural studies have been referenced to gels without graphene oxide. It was found that the gels crystalline structure after the addition of GO does not change. The XRD diffraction patterns are characterized by a number of peaks associated with precipitated NaCl during drying and presence of sodium β-glycerophosphate.

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

Ion beam modification of the structure and properties of hexagonal boron nitride: An infrared and X-ray diffraction study

NASA Astrophysics Data System (ADS)

Aradi, E.; Naidoo, S. R.; Billing, D. G.; Wamwangi, D.; Motochi, I.; Derry, T. E.

2014-07-01

The vibrational mode for the cubic symmetry of boron nitride (BN) has been produced by boron ion implantation of hexagonal boron nitride (h-BN). The optimum fluence at 150 keV was found to be 5 × 1014 ions/cm2. The presence of the c-BN phase was inferred using glancing incidence XRD (GIXRD) and Fourier Transform Infrared Spectroscopy (FTIR). After implantation, Fourier Transform Infrared Spectroscopy indicated a peak at 1092 cm-1 which corresponds to the vibrational mode for nanocrystalline BN (nc-BN). The glancing angle XRD pattern after implantation exhibited c-BN diffraction peaks relative to the implantation depth of 0.4 μm.

Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

Treesearch

Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

2017-01-01

Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

PubMed Central

2013-01-01

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure. PMID:24386493

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.

PubMed

Dudenko, Dmytro V; Williams, P Andrew; Hughes, Colan E; Antzutkin, Oleg N; Velaga, Sitaram P; Brown, Steven P; Harris, Kenneth D M

2013-06-13

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1 H and 13 C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1 H and 13 C chemical shifts for directly bonded 13 C- 1 H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.

Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

ERIC Educational Resources Information Center

Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

2007-01-01

A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

Glass transition in ferroic glass K x (ND4)1-x D2PO4: a complete x-ray diffraction line shape analysis

NASA Astrophysics Data System (ADS)

Ranjan Choudhury, Rajul; Chitra, R.; Jayakrishnan, V. B.

2016-03-01

Quenching of dynamic disorder in glassy systems is termed as the glass transition. Ferroic glasses belong to the class of paracrystalline materials having crystallographic order in-between that of a perfect crystal and amorphous material, a classic example of ferroic glass is the solid solution of ferroelectric deuterated potassium dihydrogen phosphate and antiferroelectric deuterated ammonium dihydrogen phosphate. Lowering temperature of this ferroic glass can lead to a glass transition to a quenched disordered state. The subtle atomic rearrangement that takes place at such a glass transition can be revealed by careful examination of the temperature induced changes occurring in the x-ray powder diffraction (XRD) patterns of these materials. Hence we report here results of a complete diffraction line shape analysis of the XRD patterns recorded at different temperatures from deuterated mixed crystals DK x A1-x DP with mixing concentration x ranging as 0 < x < 1. Changes observed in diffraction peak shapes have been explained on the basis of structural rearrangements induced by changing O-D-O hydrogen bond dynamics in these paracrystals.

In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions

NASA Astrophysics Data System (ADS)

Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F.; van Bokhoven, Jeroen A.

2017-08-01

An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions.

PubMed

Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F; van Bokhoven, Jeroen A

2017-08-01

An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

The effect of nano-TiO2 photocatalysis on the antioxidant activities of Cu, Zn-SOD at physiological pH.

PubMed

Zheng, Wen; Zou, Hai-Feng; Lv, Shao-Wu; Lin, Yan-Hong; Wang, Min; Yan, Fei; Sheng, Ye; Song, Yan-Hua; Chen, Jie; Zheng, Ke-Yan

2017-09-01

Security issues of nanoparticles on biological toxicity and potential environmental risk have attracted more and more attention with the rapid development and wide applications of nanotechnology. In this work, we explored the effect and probable mechanism of nano-TiO 2 on antioxidant activity of copper, zinc superoxide dismutase (Cu, Zn-SOD) under natural light and mixed light at physiological pH. Nano-TiO 2 was prepared by sol-hydrothermal method, and then characterized by X-ray Diffraction (XRD) and Transmission electron micrographs (TEM). The Cu, Zn-SOD was purified by sephadex G75 chromatography and qualitatively analyzed by sodium dodecyl sulfate polypropylene amide gel electrophoresis (SDS-PAGE). The effect and mechanism were elucidated base on Fourier Transform Infrared Spectrometer (FT-IR), Circular Dichroism (CD), zeta potential, and electron spin resonance (ESR) methods. Accompanying the results of FT-IR, CD and zeta potential, it could be concluded that nano-TiO 2 had no effect on the antioxidant activity of Cu, Zn-SOD by comparing the relative activity under natural light at physiological pH. But the relative activity of Cu, Zn-SOD significantly decreased along with the increase of nano-TiO 2 concentration under the mixed light. The results of ESR showed the cause of this phenomenon was the Cu(II) in the active site of Cu, Zn-SOD was reduced to Cu(I) by H 2 O 2 and decreased the content of active Cu, Zn-SOD. The reduction can be inhibited by catalase. Excess O 2 ·- produced by nano-TiO 2 photocatalysis under mixed light accumulated a mass of H 2 O 2 through disproportionation reaction in this experimental condition. The results show that nano-TiO 2 cannot affect the antioxidant activity of Cu, Zn-SOD in daily life. The study on the effect of nano-TiO 2 on Cu, Zn-SOD will provide a valid theory support for biological safety and the toxicological effect mechanism of nanomaterials on enzyme. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrafast visualization of crystallization and grain growth in shock-compressed SiO2

PubMed Central

Gleason, A. E.; Bolme, C. A.; Lee, H. J.; Nagler, B.; Galtier, E.; Milathianaki, D.; Hawreliak, J.; Kraus, R. G.; Eggert, J. H.; Fratanduono, D. E.; Collins, G. W.; Sandberg, R.; Yang, W.; Mao, W. L.

2015-01-01

Pressure- and temperature-induced phase transitions have been studied for more than a century but very little is known about the non-equilibrium processes by which the atoms rearrange. Shock compression generates a nearly instantaneous propagating high-pressure/temperature condition while in situ X-ray diffraction (XRD) probes the time-dependent atomic arrangement. Here we present in situ pump–probe XRD measurements on shock-compressed fused silica, revealing an amorphous to crystalline high-pressure stishovite phase transition. Using the size broadening of the diffraction peaks, the growth of nanocrystalline stishovite grains is resolved on the nanosecond timescale just after shock compression. At applied pressures above 18 GPa the nuclueation of stishovite appears to be kinetically limited to 1.4±0.4 ns. The functional form of this grain growth suggests homogeneous nucleation and attachment as the growth mechanism. These are the first observations of crystalline grain growth in the shock front between low- and high-pressure states via XRD. PMID:26337754

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO4:Dy TL material

NASA Astrophysics Data System (ADS)

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Hamid, Muhammad Azmi Abdul; Dollah, Mohd Taufik

2014-09-01

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO4) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO4 with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO4:Dy was studied using a TLD reader after exposure to gamma ray by Co60 source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

X-ray Diffraction and Rietveld Refinement in Deferrified Clays for Forensic Science.

PubMed

Prandel, Luis V; Melo, Vander de F; Brinatti, André M; Saab, Sérgio da C; Salvador, Fábio A S

2018-01-01

Soil vestiges might provide information about a crime scene. The Rietveld method with X-ray diffraction data (RM-XRD) is a nondestructive technique that makes it possible to characterize minerals present in the soils. Soil clays from the metropolitan region of Curitiba (Brazil) were submitted to DCB treatment and analyzed using XRD with CuK α radiation in the step-scan mode (0.02° 2θ/5 s). The GSAS+EXPGUI software was used for RM refinement. The RM-XRD results, together with the principal component analysis (PCA) (52.6% total variance), showed the kaolinite predominance in most analyzed samples and the highest quartz contents in "site 1." Higher anatase, and gibbsite and muscovite contents influenced discrimination, mainly in "site 3" and "site 1," respectively. These results were enough to discriminate clays of four sites and two horizons using a reduced amount of sample showing that the technique can be applied to the investigation into soil vestiges. © 2017 American Academy of Forensic Sciences.

Role of Ga particulates on the structure and optical properties of Y3(Al,Ga)5O12:Tb thin films prepared by PLD

NASA Astrophysics Data System (ADS)

Yousif, A.; Duvenhage, M. M.; Ntwaeaborwa, O. M.; Swart, H. C.

2018-04-01

Y3(Al,Ga)5O12:Tb thin films (70 nm) have been prepared by pulsed laser deposition on a Si (100) substrate at the substrate temperature of 300 °C. The effect of annealing time on the structural, morphological and luminescence properties of Y3(Al,Ga)5O12:Tb thin films at 800 °C were studied. The crystal structure of the samples was studied by X- ray diffraction (XRD) and showed shifts in the peak positions to lower diffraction angles for the annealed film compared to the XRD peak positions of the commercial Y3(Al,Ga)5O12:Tb powder. A new excitation band different from the original Y3(Al,Ga)5O12:Tb powder was also observed for the annealed films. The shift in the XRD pattern and the new excitation band for the annealed film suggested that the films were enriched with Ga after annealing.

Ultrafast visualization of crystallization and grain growth in shock-compressed SiO 2

DOE PAGES

Gleason, A. E.; Bolme, C. A.; Lee, H. J.; ...

2015-09-04

Pressure- and temperature-induced phase transitions have been studied for more than a century but very little is known about the non-equilibrium processes by which the atoms rearrange. Shock compression generates a nearly instantaneous propagating high-pressure/temperature condition while in situ X-ray diffraction (XRD) probes the time-dependent atomic arrangement. Here we present in situ pump–probe XRD measurements on shock-compressed fused silica, revealing an amorphous to crystalline high-pressure stishovite phase transition. Using the size broadening of the diffraction peaks, the growth of nanocrystalline stishovite grains is resolved on the nanosecond timescale just after shock compression. At applied pressures above 18 GPa the nuclueationmore » of stishovite appears to be kinetically limited to 1.4 ± 0.4 ns. The functional form of this grain growth suggests homogeneous nucleation and attachment as the growth mechanism. As a result, these are the first observations of crystalline grain growth in the shock front between low- and high-pressure states via XRD.« less

Computer Simulations to Study Diffraction Effects of Stacking Faults in Beta-SiC: II. Experimental Verification. 2; Experimental Verification

NASA Technical Reports Server (NTRS)

Pujar, Vijay V.; Cawley, James D.; Levine, S. (Technical Monitor)

2000-01-01

Earlier results from computer simulation studies suggest a correlation between the spatial distribution of stacking errors in the Beta-SiC structure and features observed in X-ray diffraction patterns of the material. Reported here are experimental results obtained from two types of nominally Beta-SiC specimens, which yield distinct XRD data. These samples were analyzed using high resolution transmission electron microscopy (HRTEM) and the stacking error distribution was directly determined. The HRTEM results compare well to those deduced by matching the XRD data with simulated spectra, confirming the hypothesis that the XRD data is indicative not only of the presence and density of stacking errors, but also that it can yield information regarding their distribution. In addition, the stacking error population in both specimens is related to their synthesis conditions and it appears that it is similar to the relation developed by others to explain the formation of the corresponding polytypes.

CdO-NPs; synthesis from 1D new nano Cd coordination polymer, characterization and application as anti-cancer drug for reducing the viability of cancer cells

NASA Astrophysics Data System (ADS)

Afzalian Mend, Behnaz; Delavar, Mahmoud; Darroudi, Majid

2017-04-01

The hexagonal CdO nano-particles (CdO-NPs) was prepared using new nano Cd coordination polymer, [Cd(NO3)(bipy)(pzca)]n (1) as a precursor, through direct calcination process at 500 °C. The precursor (1) was synthesized by sonochemical method. The new nano compound (1) was characterized by IR spectroscopy, elemental analyses, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and thermal gravimetric analyses. The structure of nano coordination polymer was determined by comparing the XRD pattern of nano and single-crystal of compound (1). The nano CdO was characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). In addition, the activity and efficiency of nano CdO as an anti-cancer drug was studied on cancer cells with different concentration. The results shows that the viability of cancer cells reduced above 2 μg/mL of CdO-NPs concentration.

Step-by-step fabrication of a highly oriented crystalline three-dimensional pillared-layer-type metal-organic framework thin film confirmed by synchrotron X-ray diffraction.

PubMed

Otsubo, Kazuya; Haraguchi, Tomoyuki; Sakata, Osami; Fujiwara, Akihiko; Kitagawa, Hiroshi

2012-06-13

Fabrication of a crystalline ordered thin film based on the porous metal-organic frameworks (MOFs) is one of the practical applications of the future functional nanomaterials. Here, we report the creation of a highly oriented three-dimensional (3-D) porous pillared-layer-type MOF thin film on a metal substrate using a step-by-step approach based on liquid-phase epitaxy. Synchrotron X-ray diffraction (XRD) study clearly indicates that the thin film is crystalline and its orientation is highly controlled in both horizontal and vertical directions relative to the substrate. This report provides the first confirmation of details of not only the crystallinity but also the orientation of 3-D MOF thin film using synchrotron XRD. Moreover, we also demonstrate its guest adsorption/desorption behavior by using in situ XRD measurements. The results presented here would promise useful insights for fabrication of MOF-based nanodevices in the future.

MultiLaue: A Technique to Extract d-spacings from Laue XRD

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

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

MultiLaue: A Technique to Extract d-spacings from Laue XRD

DOE PAGES

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi; ...

2016-07-25

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

Using Variable Temperature Powder X-Ray Diffraction to Determine the Thermal Expansion Coefficient of Solid MgO

ERIC Educational Resources Information Center

Corsepius, Nicholas C.; DeVore, Thomas C.; Reisner, Barbara A.; Warnaar, Deborah L.

2007-01-01

A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a…

Laser-induced Multi-energy Processing in Diamond Growth

DTIC Science & Technology

2012-05-01

microscopy (SEM) and energy dispersive X - ray (EDX) measurements, Drs. Yi Liu and Shah Valloppilly from Nebraska Center for Materials and Nanoscience...NCMN) at UNL for help on X - Ray diffraction (XRD) measurements, and Professor Steve W. Martin and Dr. Young Sik Kim from the Department of Material...spectroscopy and X - ray diffraction ................... 62 4.4 Conclusions

Phyto-reduction of graphene oxide using the aqueous extract of Eichhornia crassipes (Mart.) Solms

NASA Astrophysics Data System (ADS)

Firdhouse, M. Jannathul; Lalitha, P.

2014-10-01

The aqueous extract of Eichhornia crassipes was used as reductant to produce graphene from graphene oxide by refluxing method. The complete reduction of graphene oxide was monitored using UV-Vis spectrophotometer. Characterization of graphene was made through FTIR, XRD, and Raman spectroscopy analysis. The stability of graphene was studied by thermal gravimetric analysis and zeta potential measurements. The nature and surface morphology of the synthesized graphene was analyzed by transmission electron microscopy. The production of graphene using phytoextract as reductant emphasizes on the facile method of synthesis and greener nanotechnology.

Carbonation-induced weathering effect on cesium retention of cement paste

NASA Astrophysics Data System (ADS)

Park, S. M.; Jang, J. G.

2018-07-01

Carbonation is inevitable for cement and concrete in repositories over an extended period of time. This study investigated the carbonation-induced weathering effect on cesium retention of cement. Cement paste samples were exposed to accelerated carbonation for different durations to simulate the extent of weathering among samples. The extent of carbonation in cement was characterized by XRD, TG and NMR spectroscopy, while the retention capacity for cesium was investigated by zeta potential measurement and batch adsorption tests. Though carbonation led to decalcification from the binder gel, it negatively charged the surface of cement hydrates and enhanced their cesium adsorption capacity.

Deactivation of Zeolite Catalyst H-ZSM-5 during Conversion of Methanol to Gasoline: Operando Time- and Space-Resolved X-ray Diffraction.

PubMed

Rojo-Gama, Daniel; Mentel, Lukasz; Kalantzopoulos, Georgios N; Pappas, Dimitrios K; Dovgaliuk, Iurii; Olsbye, Unni; Lillerud, Karl Petter; Beato, Pablo; Lundegaard, Lars F; Wragg, David S; Svelle, Stian

2018-03-15

The deactivation of zeolite catalyst H-ZSM-5 by coking during the conversion of methanol to hydrocarbons was monitored by high-energy space- and time-resolved operando X-ray diffraction (XRD) . Space resolution was achieved by continuous scanning along the axial length of a capillary fixed bed reactor with a time resolution of 10 s per scan. Using real structural parameters obtained from XRD, we can track the development of coke at different points in the reactor and link this to a kinetic model to correlate catalyst deactivation with structural changes occurring in the material. The "burning cigar" model of catalyst bed deactivation is directly observed in real time.

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.

Impact of welan gum on tricalcium aluminate-gypsum hydration

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

Ma Lei, E-mail: malei198713@163.com; Zhao Qinglin, E-mail: zhaoqinglin@whut.edu.cn; Yao Chukang

The retarding effect of welan gum on tricalcium aluminate-gypsum hydration, as a partial system of ordinary Portland cement (OPC) hydration, was investigated with several methods. The tricalcium aluminate-gypsum hydration behavior in the presence or absence of welan gum was researched by field emission gun scanning electron microscopy, X-ray diffraction and zeta potential analysis. Meanwhile, we studied the surface electrochemical properties and adsorption characteristics of welan gum by utilizing a zeta potential analyzer and UV-VIS absorption spectrophotometer. By adding welan gum, the morphology change of ettringite and retardation of hydration stages in tricalcium aluminate-gypsum system was observed. Moreover, we detected themore » adsorption behavior and zeta potential inversion of tricalcium aluminate and ettringite, as well as a rapid decrease in the zeta potential of tricalcium aluminate-gypsum system. The reduction on nucleation rate of ettringite and hydration activity of C{sub 3}A was also demonstrated. Thus, through the adsorption effect, welan gum induces a retarding behavior in tricalcium aluminate-gypsum hydration. Highlights: Black-Right-Pointing-Pointer Adsorption characteristics of welan gum on C{sub 3}A and ettringite have been studied. Black-Right-Pointing-Pointer C{sub 3}A-gypsum hydration behavior and the hydration products are examined in L/S = 3. Black-Right-Pointing-Pointer Welan gum retards the process of C{sub 3}A-gypsum hydration. Black-Right-Pointing-Pointer The addition of welan gum changes the nucleation growth of ettringite.« less

Thermal and pH responsive polymer-tethered multifunctional magnetic nanoparticles for targeted delivery of anticancer drug.

PubMed

Sahoo, Banalata; Devi, K Sanjana P; Banerjee, Rakesh; Maiti, Tapas K; Pramanik, Panchanan; Dhara, Dibakar

2013-05-01

Targeted and efficient delivery of therapeutics to tumor cells is one of the key issues in cancer therapy. In the present work, we report a temperature and pH dual responsive core-shell nanoparticles comprising smart polymer shell coated on magnetic nanoparticles as an anticancer drug carrier and cancer cell-specific targeting agent. Magnetite nanoparticles (MNPs), prepared by a simple coprecipitation method, was surface modified by introducing amine groups using 3-aminopropyltriethoxysilane. Dual-responsive poly(N-isopropylacrylamide)-block-poly(acrylic acid) copolymer, synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization, was then attached to the amine-functionalized MNPs via EDC/NHS method. Further, to accomplish cancer-specific targeting properties, folic acid was tethered to the surface of the nanoparticles. Thereafter, rhodamine B isothiocyanate was conjugated to endow fluorescent property to the MNPs required for cellular imaging applications. The nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), thermogravimetric analysis (TGA), zeta potential, vibrating sample magnetometer (VSM), X-ray photoelectron spectroscopy (XPS) measurements, and FTIR, UV-vis spectral analysis. Doxorubicin (DOX), an anticancer drug used for the present study, was loaded into the nanoparticles and its release behavior was subsequently studied. Result showed a sustained release of DOX preferentially at the desired lysosomal pH and temperature condition. The biological activity of the DOX-loaded MNPs was studied by MTT assay, fluorescence microscopy, and apoptosis. Intracellular-uptake studies revealed preferential uptake of these nanoparticles into cancer cells (HeLa cells) compared to normal fibroblast cells (L929 cells). The in vitro apoptosis study revealed that the DOX-loaded nanoparticles caused significant death to the HeLa cells. These nanoparticles were capable of target specific release of the loaded drug in response to pH and temperature and hence may serve as a potential drug carrier for in vivo applications.

Statistical Nature of Atomic Disorder in Irradiated Crystals.

PubMed

Boulle, A; Debelle, A

2016-06-17

Atomic disorder in irradiated materials is investigated by means of x-ray diffraction, using cubic SiC single crystals as a model material. It is shown that, besides the determination of depth-resolved strain and damage profiles, x-ray diffraction can be efficiently used to determine the probability density function (PDF) of the atomic displacements within the crystal. This task is achieved by analyzing the diffraction-order dependence of the damage profiles. We thereby demonstrate that atomic displacements undergo Lévy flights, with a displacement PDF exhibiting heavy tails [with a tail index in the γ=0.73-0.37 range, i.e., far from the commonly assumed Gaussian case (γ=2)]. It is further demonstrated that these heavy tails are crucial to account for the amorphization kinetics in SiC. From the retrieved displacement PDFs we introduce a dimensionless parameter f_{D}^{XRD} to quantify the disordering. f_{D}^{XRD} is found to be consistent with both independent measurements using ion channeling and with molecular dynamics calculations.

[Identification of Dens Draconis and Os Draconis by XRD method].

PubMed

Chen, Guang-Yun; Wu, Qi-Nan; Shen, Bei; Chen, Rong

2012-04-01

To establish an XRD method for evaluating the quality of Os Draconis and Dens Draconis and applying in judgement of the counterfeit. Dens Draconis, Os Draconis and the counterfeit of Os Draconis were analyzed by XRD. Their diffraction patterns were clustered analysis and evaluated their similarity degree. Established the analytical method of Dens Draconis and Os Draconis basing the features fingerprint information of the 10 common peaks by XRD pattern. Obtained the XRD pattern of the counterfeit of Os Draconis. The similarity degree of separate sources of Dens Draconis was high,while the similarity degree of separate sources of Os Draconis was significant different from each other. This method can be used for identification and evaluation of Os Draconis and Dens Draconis. It also can be used for identification the counterfeit of Os Draconis effectively.

Development of Thin Films as Potential Structural Cathodes to Enable Multifunctional Energy-Storage Structural Composite Batteries for the U.S. Army’s Future Force

DTIC Science & Technology

2011-09-01

glancing angle X - ray diffraction (GAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and electrochemical...Emission SEM FWHM full width at half maximum GAXRD glancing angle X - ray diffraction H3COCH2CH2OH 2-methoxyethanol LiMn2O4 lithium manganese oxide...were characterized by scanning electron microscopy (SEM), X - ray diffraction (XRD), and atomic force microscopy (AFM). In addition,

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Synthesis, characterization and adsorption properties of microcrystalline cellulose based nanogel for dyes and heavy metals removal.

PubMed

El-Naggar, Mehrez E; Radwan, Emad K; El-Wakeel, Shaimaa T; Kafafy, Hany; Gad-Allah, Tarek A; El-Kalliny, Amer S; Shaheen, Tharwat I

2018-07-01

Recently, naturally occurring biopolymers have attracted the attention as potential adsorbents for the removal of water contaminants. In this work, we present the development of microcrystalline cellulose (MCC)-based nanogel grafted with acrylamide and acrylic acid in the presence of methylene bisacrylamide and potassium persulphate as a crosslinking agent and initiator, respectively. World-class facilities such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), surface analysis, field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HR-TEM) and zeta sizer were used to characterize the synthesized MCC based nanogel. The prepared nanogel was applied to remove reactive red 195 (RR195) dye and Cd (II) from aqueous medium at different operational conditions. The adsorption experiments showed that the feed concentration of monomers has a significant effect on the removal of RR195 which peaked (93% removal) after 10min of contact time at pH2 and a dose of 1.5g/L. On contrary, the feed concentration has insignificant effect on the removal of Cd (II) which peaked (97% removal) after 30min of contact time at pH6 and a dose of 0.5g/L. The adsorption equilibrium data of RR195 and Cd (II) was best described by Freundlich and Langmuir, respectively. Conclusively, the prepared MCC based nanogels were proved as promising adsorbents for the removal of organic pollutants as well as heavy metals. Copyright © 2018 Elsevier B.V. All rights reserved.

Evaluation of tetraethoxysilane (TEOS) sol-gel coatings, modified with green synthesized zinc oxide nanoparticles for combating microfouling.

PubMed

Krupa, A Nithya Deva; Vimala, R

2016-04-01

Green synthesis of zinc oxide nanoparticles (ZnO-NPs) is gaining importance as an eco-friendly alternative to conventional methods due to its enormous applications. The present work reports the synthesis of ZnO-NPs using the endosperm of Cocos nucifera (coconut water) and the bio-molecules responsible for nanoparticle formation have been identified. The synthesized nanoparticles were characterized using UV-Visible spectroscopy (UV-Vis), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Zeta potential measurement. The results obtained reveal that the synthesized nanoparticles are moderately stable with the size ranging from 20 to 80 nm. The bactericidal effect of the nanoparticles was proved by well diffusion assay and determination of minimum inhibitory concentration (MIC) against marine biofilm forming bacteria. Further the green synthesized ZnO-NPs were doped with TEOS sol-gels (TESGs) in order to assess their antimicrofouling capability. Different volumes of liquid sol-gels were coated on to 96-well microtitre plate and cured under various conditions. The optimum curing conditions were found to be temperature 60 °C, time 72 h and volume 200 μl. Antiadhesion test of the undoped (SG) and ZnO-NP doped TEOS sol-gel (ZNSG) coatings were evaluated using marine biofilm forming bacteria. ZNSG coatings exhibited highest biofilm inhibition (89.2%) represented by lowest OD value against Pseudomonasotitidis strain NV1. Copyright © 2016 Elsevier B.V. All rights reserved.

Research on magnetic separation for complex nickel deep removal and magnetic seed recycling.

PubMed

Qiu, Yiqin; Xiao, Xiao; Ye, Ziwei; Guan, Zhijie; Sun, Shuiyu; Ren, Jie; Yan, Pingfan

2017-04-01

This study investigated the deep removal of complex nickel from simulated wastewater using magnetic separation and magnetic seed recycling. Nano-magnetite (Fe 3 O 4 ) was used as the magnetic seed. The flocculant applied was N,N-bis-(dithiocarboxy) ethanediamine (EDTC), a highly efficient heavy metal chelating agent included in dithiocarbamate (DTC). Important investigated parameters included hydraulic retention time, magnetic seed dosage, and magnetic field strength. The study also explored the magnetic flocculation mechanism involved in the reaction. The result indicated that the residual Ni concentration was reduced to less than 0.1 mg/L from the initial concentration of 50 mg/L under optimal conditions. Magnetic seed recovery reached 76.42% after a 3-h stirring period; recycled magnetic seeds were analyzed using scanning electron microscope (SEM) and X-ray diffraction (XRD). The zeta potential results illustrated that magnetic seeds firmly combined with flocs when the pH ranged from 6.5 to 7.5 due to the electrostatic attraction. When the pH was less than 7, magnetic seeds and EDTC were also combined due to electrostatic attraction. Particle size did affect microfloc size; it decreased microfloc size and increased floc volume through magnetic seed loading. The effective binding sites between flocs and magnetic seeds increased when adding the magnetic seeds. This led the majority of magnetic flocs to be integrated with the magnetic seeds, which served as a nucleus to enhance the flocculation property and ultimately improve the nickel complex removal rate.

Theoretical and experimental adsorption studies of sulfamethoxazole and ketoprofen on synthesized ionic liquids modified CNTs.

PubMed

Lawal, Isiaka A; Lawal, Monsurat M; Akpotu, Samson O; Azeez, Mayowa A; Ndungu, Patrick; Moodley, Brenda

2018-06-18

The adsorption of sulfamethoxazole (SMZ) and ketoprofen (KET) using carbon nanotubes (CNTs) and CNTs modified with ionic liquids (ILs) was investigated. Two ionic liquids (1-benzyl, 3-hexyl imidazolium, IL1 and 1-benzyl, 3-decahexyl imidazolium, IL2) were synthesized, and characterized by nuclear magnetic resonance ( 1 H and 13 C NMR) and high resolution-mass spectrometry (HR-MS). CNTs and modified CNTs were characterized using FT-IR, X-ray diffraction (XRD), surface area and porosity analysis, thermal gravimetric analysis (TGA), Zeta potential, Raman and scanning electron microscopy (SEM). Kinetics, isotherm and computational studies were carried out to determine the efficiency and adsorption mechanism of SMZ and KET on modified CNTs. A density functional theory (DFT) method was applied to shed more light on the interactions between the pharmaceutical compounds and the adsorbents at the molecular level. The effects of adsorbent dosage, concentration, solution pH, energetics and contact time of SMZ and KET on the adsorption process were investigated. The adsorption of SMZ and KET on CNTs and modified CNTs were pH dependent, and adsorption was best described by pseudo-second-order kinetics and the Freundlich adsorption isotherm. Ionic liquid modified CNTs showed improved adsorption capacities compared to the unmodified ones for both SMZ and KET, which is in line with the computational results showing performance order; CNT+KET/SMZ < CNT-ILs+SMZ < CNT-ILs+KET. Copyright © 2018 Elsevier Inc. All rights reserved.

Magnetic Fe3O4@V2O5/rGO nanocomposite as a recyclable photocatalyst for dye molecules degradation under direct sunlight irradiation.

PubMed

Boruah, Purna K; Szunerits, Sabine; Boukherroub, Rabah; Das, Manash R

2018-01-01

Reduced graphene oxide nanosheets decorated with Fe 3 O 4 and V 2 O 5 nanoparticles as a magnetically recoverable nanocomposite (Fe 3 O 4 @V 2 O 5 /rGO) was synthesized by a simple solution chemistry approach. The synthesized nanocomposite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM), Fourier transform infrared (FTIR), fluorescence, and zeta potential measurements. The narrow band gap and different band gap energies of Fe 3 O 4 and V 2 O 5 proved to be suitable for the absorption of visible light in the solar spectrum. The Fe 3 O 4 @V 2 O 5 /rGO displayed indeed excellent photocatalytic activity towards the degradation of harmful cationic Bismarck Brown (BB) as well as anionic Acid Orange 7 (AO) dyes under direct sunlight irradiation. The photocatalytic activity of the Fe 3 O 4 @V 2 O 5 /rGO is influenced by solution pH, catalyst loading, initial dye concentration and the presence of different inorganic ions (NH 4 + , Na + , Mg 2+ , Ca 2+, SO 4 2- , Br - , NO 3 - , Cl - , HCO 3 - ). This study provides a new scientific knowledge on the sunlight driven photocatalytic degradation of dye molecules using novel mixed metal oxide/rGO nanocomposite photocatalyst. Copyright © 2017 Elsevier Ltd. All rights reserved.

The first X-ray diffraction measurements on Mars.

PubMed

Bish, David; Blake, David; Vaniman, David; Sarrazin, Philippe; Bristow, Thomas; Achilles, Cherie; Dera, Przemyslaw; Chipera, Steve; Crisp, Joy; Downs, R T; Farmer, Jack; Gailhanou, Marc; Ming, Doug; Morookian, John Michael; Morris, Richard; Morrison, Shaunna; Rampe, Elizabeth; Treiman, Allan; Yen, Albert

2014-11-01

The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component.

Identification of a deleterious phase in photocatalyst based on Cd1 - xZnxS/Zn(OH)2 by simulated XRD patterns.

PubMed

Cherepanova, Svetlana; Markovskaya, Dina; Kozlova, Ekaterina

2017-06-01

The X-ray diffraction (XRD) pattern of a deleterious phase in the photocatalyst based on Cd 1 - x Zn x S/Zn(OH) 2 contains two relatively intense asymmetric peaks with d-spacings of 2.72 and 1.56 Å. Very small diffraction peaks with interplanar distances of (d) ≃ 8.01, 5.40, 4.09, 3.15, 2.49 and 1.35 Å are characteristic of this phase but not always observed. To identify this phase, the XRD patterns for sheet-like hydroxide β-Zn(OH) 2 and sheet-like hydrozincite Zn 5 (CO 3 ) 2 (OH) 6 as well as for turbostratic hydrozincite were simulated. It is shown that the XRD pattern calculated on the basis of the last model gives the best correspondence with experimental data. Distances between layers in the turbostratically disordered hydrozincite fluctuate around d ≃ 8.01 Å. This average layer-to-layer distance is significantly higher than the interlayer distance 6.77 Å in the ordered Zn 5 (CO 3 ) 2 (OH) 6 probably due to a deficiency of CO 3 2- anions, excess OH - and the presence of water molecules in the interlayers. It is shown by variable-temperature XRD and thermogravimetric analysis (TGA) that the nanocrystalline turbostratic nonstoichiometric hydrozincite-like phase is quite thermostable. It decomposes into ZnO in air above 473 K.

In situ 2D diffraction as a tool to characterize ferroelectric and piezoelectric thin films

NASA Astrophysics Data System (ADS)

Khamidy, N. I.; Kovacova, V.; Bernasconi, A.; Le Rhun, G.; Vaxelaire, N.

2017-08-01

In this paper the application of 2D x-ray diffraction (XRD2) as a technique to characterize in situ during electrical cycling the properties of a ferroelectric and piezoelectric thin film is discussed. XRD2 is one type of XRD on which a 2D detector is used instead of a point detector. This technique enables simultaneous recording of many sample information in a much shorter time compared to conventional XRD. The discussion is focused especially on the data processing technique of the huge data acquired. The methodology to calculate an effective piezoelectric coefficient, analyze the phase and texture, and estimate the domain size and shape is described in this paper. This methodology is then applied to a lead zirconate titanate (PZT) thin film at the morphotropic phase boundary (MPB) composition (i.e. Pb[Zr0.52Ti0.48]O3) with a preferred orientation of (1 0 0). The in situ XRD2 characterization was conducted in the European synchrotron radiation facility (ESRF) in Grenoble, France. Since a high-energy beam with vertical resolution as small as 100 nm was used, a cross-sectional scan of the sample was performed over the entire thickness of the film. From these experimental results, a better understanding on the piezoelectricity phenomena in PZT thin film at MPB composition were achieved, providing original feedback between the elaboration processes and functional properties of the film.

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.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

Impact of Pluronic F-68 vs Tween 80 on Fabrication and Evaluation of Acyclovir SLNs for Skin Delivery.

PubMed

Bhupinder, Kaur; Newton, Maria J

2016-01-01

The solid lipid nanoparticles (SLNs) of Acyclovir (ACV) were fabricated with Soya lecithin and Fractionated Coconut oil (medium chain glyceride) as a first time combination. The research was focused on developing ACV-SLN by using high pressure hot-homogenization technique. The ingredients were used in different concentrations and ratios to identify the best formulation design. The tween 80 and Pluronic F-68 were used in various concentrations in formulation design to assess the impact on the fabrication and evaluation of SLNs. The impact of nanotechnology gain to play a vital role in the topical pharmaceutical products and the related patents will play a significant role in related industries. The SLNs were subjected to various characterization techniques such as XRD, FTIR, Master sizer analysis and zeta potential. The mean particle size was determined by master sizer and zeta sizer. Transmission electron microscopy (TEM) was used as a tool to analyze the morphology and other features. The zeta potential and drug entrapment efficiency (EE%) were also determined for the prepared ACV-SLNs. The efficiency of drug release from prepared formulations was studied by using in vitro study with the utilization of dialysis membrane technique. SLN dispersions exhibited the average size in nano range. SLNs with small particle size found to have predetermined encapsulation efficiency, and relatively high loading capacity and predetermined in vitro drug release profile. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

NASA Astrophysics Data System (ADS)

Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

2011-03-01

FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

XRD measurement of mean thickness, thickness distribution and strain for illite and illite-smectite crystallites by the Bertaut-Warren-Averbach technique

USGS Publications Warehouse

Drits, Victor A.; Eberl, Dennis D.; Środoń, Jan

1998-01-01

A modified version of the Bertaut-Warren-Averbach (BWA) technique (Bertaut 1949, 1950; Warren and Averbach 1950) has been developed to measure coherent scattering domain (CSD) sizes and strains in minerals by analysis of X-ray diffraction (XRD) data. This method is used to measure CSD thickness distributions for calculated and experimental XRD patterns of illites and illite-smectites (I-S). The method almost exactly recovers CSD thickness distributions for calculated illite XRD patterns. Natural I-S samples contain swelling layers that lead to nonperiodic structures in the c* direction and to XRD peaks that are broadened and made asymmetric by mixed layering. Therefore, these peaks cannot be analyzed by the BWA method. These difficulties are overcome by K-saturation and heating prior to X-ray analysis in order to form 10-Å periodic structures. BWA analysis yields the thickness distribution of mixed-layer crystals (coherently diffracting stacks of fundamental illite particles). For most I-S samples, CSD thickness distributions can be approximated by lognormal functions. Mixed-layer crystal mean thickness and expandability then can be used to calculate fundamental illite particle mean thickness. Analyses of the dehydrated, K-saturated samples indicate that basal XRD reflections are broadened by symmetrical strain that may be related to local variations in smectite interlayers caused by dehydration, and that the standard deviation of the strain increases regularly with expandability. The 001 and 002 reflections are affected only slightly by this strain and therefore are suited for CSD thickness analysis. Mean mixed-layer crystal thicknesses for dehydrated I-S measured by the BWA method are very close to those measured by an integral peak width method.

Structural and optical characterization of bismuth sulphide nanorods

NASA Astrophysics Data System (ADS)

Shah, N. M.; Poria, K. C.

2017-05-01

In this work Bismuth sulfide (Bi2S3) nanorods with a high order of crystallinity is synthesized via hydrothermal method from aqueous solution of Bismuth Nitrate Pentahydrate and elemental Sulphur using Triethanolamine (TEA) as capping agent. The microstructures of Bi2S3 nanorods were investigated by X-ray diffraction (XRD) analysis. The positions and relative intensities of all the peaks in XRD pattern are in good agreement with those of the orthorhombic crystal structure of Bi2S3. TEM images shows that synthesized Bi2S3 has morphology of nanorods while selected area electron diffraction pattern indicates single crystalline nature. The analysis of diffuse reflectance (DR) spectrum of as synthesized Bi2S3 using Kubelka - Munk theory suggests direct energy band gap of 1.5 eV.

Synthesis and structural properties of Ba(1-x)LaxTiO3 perovskite nanoparticles fabricated by solvothermal synthesis route

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Elupula, Ravinder; Molugu, Sudheer; Shipman, Josh; Chrisey, Douglas B.

2017-05-01

We report the successful synthesis and structural characterization of barium lanthanum titanate Ba(1-x)LaxTiO3 (x=0.003,0.006,0.010) nanoparticles. The colloidal nanoparticles were prepared with high yield by a solvothermal method at temperatures as low as 150°C for 24h. The as-prepared nanopowders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. The XRD studies revealed pseudo-cubic crystalline structure, with no impurity phases at room temperature. However ferroelectric tetragonal modes were clearly observed using Raman spectroscopy measurements. From TEM measurements, uniformly sized BLT nanoparticles were observed. Selected area diffraction TEM images revealed polycrystalline perovskite ring patterns, identified as corresponding to the tetragonal phase.

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO{sub 4}:Dy TL material

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

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Dollah, Mohd Taufik

2014-09-03

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO{sub 4}) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO{sub 4} with average crystallite size of 74 nm with orthorhombic crystal system. Themore » TL behavior of produced CaSO{sub 4}:Dy was studied using a TLD reader after exposure to gamma ray by Co{sup 60} source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.« less

Mössbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

NASA Astrophysics Data System (ADS)

Constantinescu, Serban Grigore; Udubasa, Sorin S.; Udubasa, Gheorghe; Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel

2012-03-01

The complementary investigation techniques, Mössbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MÖSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Mössbauer technique.

Characterization of Sb-doped Bi(2)UO(6) solid solutions by X-ray diffraction and X-ray absorption spectroscopy.

PubMed

Misra, N L; Yadav, A K; Dhara, Sangita; Mishra, S K; Phatak, Rohan; Poswal, A K; Jha, S N; Sinha, A K; Bhattacharyya, D

2013-01-01

The preparation and characterization of Sb-doped Bi(2)UO(6) solid solutions, in a limited composition range, is reported for the first time. The solid solutions were prepared by solid-state reactions of Bi(2)O(3), Sb(2)O(3) and U(3)O(8) in the required stoichiometry. The reaction products were characterized by X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) measurements at the Bi and U L(3) edges. The XRD patterns indicate the precipitation of additional phases in the samples when Sb doping exceeds 4 at%. The chemical shifts of the Bi absorption edges in the samples, determined from the XANES spectra, show a systematic variation only up to 4 at% of Sb doping and support the results of XRD measurements. These observations are further supported by the local structure parameters obtained by analysis of the EXAFS spectra. The local structure of U is found to remain unchanged upon Sb doping indicating that Sb(+3) ions replace Bi(+3) during the doping of Bi(2)UO(6) by Sb.

Detecting Nanophase Weathering Products with CheMin: Reference Intensity Ratios of Allophane, Aluminosilicate Gel, and Ferrihydrite

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Bish, D. L.; Chipera, S. J.; Morris, R. V.; Achilles, C. N.; Ming, D W.; Blake, D. F.; Anderson, R. C.; Bristow, T. F.; Crisp, A.;

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Effect of solvent on the synthesis of SnO{sub 2} nanoparticles

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

Kumar, Virender; Singh, Karamjit; Singh, Kulwinder

Tin oxide (SnO{sub 2}) nanoparticles have been synthesized by co-precipitation method. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD) and Ultraviolet-Visible spectroscopy (UV-VIS). XRD analysis confirmed the formation of single phase of SnO{sub 2} nanoparticles. It has been found that solvents played important role in controlling the crystallite size of SnO{sub 2} nanoparticles. The XRD analysis showed well crystallized tetragonal SnO{sub 2} nanoparticles. The crystallite size of SnO{sub 2} nanoparticles varies with the solvent. Tauc plot showed that optical band gap was also tailored by controlling the solvent during synthesis.

High temperature XRD of Cu2.1Zn0.9SnSe4

NASA Astrophysics Data System (ADS)

Chetty, Raju; Mallik, Ramesh Chandra

2014-04-01

Quaternary compound with chemical composition Cu2.1Zn0.9SnSe4 is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

NASA Astrophysics Data System (ADS)

Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

2016-11-01

Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2 θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2 θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in Roman-Egyptian paintings as "encaustic" and in form of emulsion (modified wax), can be detected and, based on the shape of the peaks, these two ways of applying the wax can be distinguished from one another.

Organic Photonics: Toward a New Generation of Thin Film Photovoltaics and Lasers

DTIC Science & Technology

2011-03-07

plane. 39 Both electron and x - ray diffraction confirm the existence of crystalline domains of CuPc and C60. Crystalline domain sizes range from 5...nanocrystalline domains indicated by white curves that locate the domain boundaries. Scale bar=5 nm. b, X - ray diffraction pattern of an OVPD grown A... ray diffraction (XRD) and atomic force microscopy (AFM), as shown in Fig. 8. A cross-sectional TEM image of [CuPc(6.1nm)/C60(6.1nm)]10 is shown in

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

Shivananda, C. S.; Rao, B. Lakshmeesha; Madhukumar, R.

In this work silk fibroin/pullulan blend films have been prepared by solution casting method. The blend films were examined for structural, and thermal properties using X-ray diffraction (XRD), thermogravimatric (TGA) and differential scanning calorimetry (DSC) analysis. The XRD results indicate that with the introduction of pullulan, the interaction between SF and pullulan in the blend films induced the conformation transition of SF films and amorphous phase increases with increasing pullulan ratio. The thermal properties of the blend films were improved significantly in the blend films.

Electric-field responsive contrast agent based on liquid crystals and magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Mair, Lamar O.; Martinez-Miranda, Luz J.; Kurihara, Lynn K.; Nacev, Aleksandar; Hilaman, Ryan; Chowdhury, Sagar; Jafari, Sahar; Ijanaten, Said; da Silva, Claudian; Baker-McKee, James; Stepanov, Pavel Y.; Weinberg, Irving N.

2018-05-01

The properties of liquid crystal-magnetic nanoparticle composites have potential for sensing in the body. We study the response of a liquid crystal-magnetic nanoparticle (LC-MNP) composite to applied potentials of hundreds of volts per meter. Measuring samples using X-ray diffraction (XRD) and imaging composites using magnetic resonance imaging (MRI), we demonstrate that electric potentials applied across centimeter scale LC-MNP composite samples can be detected using XRD and MRI techniques.

Compression Freezing Kinetics of Water to Ice VII

DOE PAGES

Gleason, A. E.; Bolme, C. A.; Galtier, E.; ...

2017-07-11

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Coupling Graphene Sheets with Magnetic Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

sheets obtained from three different synthetic methods: (i) electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) [8], (ii...Figure 8d, the characteristic lattice fringes of ɤ-Fe2O3 nanoparticles in graphene sheet is shown. Typical X-ray diffraction ( XRD ) patterns of the HOPG ...pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG , exfoliated graphene, PyDop1

Compression Freezing Kinetics of Water to Ice VII

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

Gleason, A. E.; Bolme, C. A.; Galtier, E.

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Understanding Two Different Structures in the Dark Stable State of the Oxygen‐Evolving Complex of Photosystem II: Applicability of the Jahn–Teller Deformation Formula

PubMed Central

Shoji, Mitsuo; Isobe, Hiroshi; Tanaka, Ayako; Fukushima, Yoshimasa; Kawakami, Keisuke; Umena, Yasufumi; Kamiya, Nobuo; Nakajima, Takahito

2017-01-01

Abstract Tanaka et al. (J. Am. Chem. Soc., 2017, 139, 1718) recently reported the three‐dimensional (3D) structure of the oxygen evolving complex (OEC) of photosystem II (PSII) by X‐ray diffraction (XRD) using extremely low X‐ray doses of 0.03 and 0.12 MGy. They observed two different 3D structures of the CaMn4O5 cluster with different hydrogen‐bonding interactions in the S1 state of OEC keeping the surrounding polypeptide frameworks of PSII the same. Our Jahn–Teller (JT) deformation formula based on large‐scale quantum mechanics/molecular mechanics (QM/MM) was applied for these low‐dose XRD structures, elucidating important roles of JT effects of the MnIII ion for subtle geometric distortions of the CaMn4O5 cluster in OEC of PSII. The JT deformation formula revealed the similarity between the low‐dose XRD and damage‐free serial femtosecond X‐ray diffraction (SFX) structures of the CaMn4O5 cluster in the dark stable state. The extremely low‐dose XRD structures were not damaged by X‐ray irradiation. Implications of the present results are discussed in relation to recent SFX results and a blue print for the design of artificial photocatalysts for water oxidation. PMID:29577075

XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

PubMed

Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

2013-12-01

The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

Evolution of the substructure of a novel 12% Cr steel under creep conditions

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

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

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

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ~10 3–10 4-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering andmore » analysis of phenylalanine hydroxylase fromChromobacterium violaceumcPAH,Trichinella spiralisdeubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied.« less

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

PubMed

Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

2015-07-01

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

Supercritical carbon dioxide treatment as a method for polymorph preparation of deoxycholic acid.

PubMed

Tozuka, Yuichi; Kawada, Dai; Oguchi, Toshio; Yamamoto, Keiji

2003-09-16

A new polymorph of deoxycholic acid (DCA) was formed by using a supercritical carbon dioxide treatment. Deoxycholic acid crystals were stored in a pressure vessel purged with carbon dioxide at 12MPa, 60 degrees C for definite intervals. After storage for 1h in supercritical carbon dioxide (SC-CO2), new X-ray diffraction (XRD) peaks, not found in the bulk DCA crystal, were observed at 2theta = 7.4 degrees, 9.7 degrees and 14.0 degrees. The intensities of the new diffraction peaks increased with an increase in storage time, whereas the intensities of the diffraction peaks due to bulk DCA crystal decreased. On the DSC curves, the crystals obtained showed an exothermic peak at around 155 degrees C followed by the melting peak of bulk DCA crystal at 175 degrees C. By the temperature-controlled powder XRD measurement, the crystals obtained were found to be a metastable form of DCA. The polymorphs of DCA have not been reported; therefore, the SC-CO2 treatment would be a peculiar method to obtain a DCA polymorph.

Electrochemical reactions in fluoride-ion batteries: mechanistic insights from pair distribution function analysis

DOE PAGES

Grenier, Antonin; Porras-Gutierrez, Ana-Gabriela; Groult, Henri; ...

2017-07-05

Detailed analysis of electrochemical reactions occurring in rechargeable Fluoride-Ion Batteries (FIBs) is provided by means of synchrotron X-ray diffraction (XRD) and Pair Distribution Function (PDF) analysis.

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

NASA Astrophysics Data System (ADS)

Stan, Manuela; Popa, Adriana; Toloman, Dana; Silipas, Teofil-Danut; Vodnar, Dan Cristian; Katona, Gabriel

2015-12-01

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn2+ ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes and oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.

Phase Compositions of Self Reinforcement Al2O3/CaAl12O19 Composite using X-ray Diffraction Data and Rietveld Technique

NASA Astrophysics Data System (ADS)

Asmi, D.; Low, I. M.; O'Connor, B.

2008-03-01

The analysis of x-ray diffraction (XRD) patterns by the Rietveld technique was tested to the quantitatively phase compositions of self reinforcement Al2O3/CaAl12O19 composite. Room-temperature XRD patterns revealed that α-Al2O3 was the only phase presence in the CA0 sample, whereas the α-Al2O3 and CaAl12O19 phases were found for CA5, CA15, CA30, and CA50 samples. The peak intensity of CA6 in the self reinforcement Al2O3/CaAl12O19 composites increased in proportion with increase in CaAl12O19 content in contrast to α-Al2O3. The diffraction patterns for CA100 sample shows minor traces of α-Al2O3 even in relatively low peak intensity. It is suggesting that the in-situ reaction sintering of raw materials were not react completely to form 100 wt% CaAl12O19 at temperature 1650 °C. Quantitative phase compositions of self reinforcement Al2O3/CaAl12O19 composites by Rietveld analysis with XRD data has been well demonstrated. The results showed that the GOF values are relatively low and the fluctuation in the difference plots shows a reasonable fit between the observed and the calculated plot.

Kinetics and structural changes of Li-rich layered oxide 0.5Li2MnO3·0.5LiNi(0.292)Co(0.375)Mn(0.333)O2 material investigated by a novel technique combining in situ XRD and a multipotential step.

PubMed

Shen, Chong-Heng; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Wang, Qin; Su, Hang; Fu, Fang; Zheng, Xiao-Mei

2014-08-13

Li-rich layered oxide 0.5Li2MnO3·0.5LiNi0.292Co0.375Mn0.333O2 was prepared by an aqueous solution-evaporation route. X-ray powder diffraction (XRD) showed that the as-synthesized material was a solid solution consisting of layered α-NaFeO2-type LiMO2 (M = Ni, Co, Mn) and monoclinic Li2MnO3. The superlattice spots in the selected area electron diffraction pattern indicated the ordering of lithium ions with transition metal (TM) ions in TM layers in this Li-rich layered oxide. Electrochemical performance testing showed that the as-synthesized material could deliver an initial discharge capacity of 267.7 mAh/g, with a capacity retention of 88.5% after 33 cycles. A new combination technique, multipotential step in situ XRD (MPS in situ XRD) measurement, was applied for the first time to investigate the Li-rich layered oxide. Using this approach, the relationships between kinetics and structural variations can be obtained simutaneously. In situ XRD results showed that the c parameter decreased from 3.70 to 4.30 V and increased from 4.30 to 4.70 V, whereas the a parameter underwent a decrease above 4.30 V during the first charge process. Below 3.90 V during the first discharge process, a slight decrease in the c parameter was found along with an increase in the a parameter. During the first charge process, the value of the coefficient of diffusion for lithium ions (DLi+) decreased to its mininum at 4.55 V, which might be associated with Ni(2+) migration, as indicated by both Ni occupancy in 3b sites (Ni3b%) in the Li(+) layers and complicated chemical reactions. Remarkably, a lattice distortion might occur within the local domain in the host stucture during the first discharge process, indicated by a slight splitting of the (003) diffraction peak at 3.20 V.

Multi-level diffractive optics for single laser exposure fabrication of telecom-band diamond-like 3-dimensional photonic crystals.

PubMed

Chanda, Debashis; Abolghasemi, Ladan E; Haque, Moez; Ng, Mi Li; Herman, Peter R

2008-09-29

We present a novel multi-level diffractive optical element for diffractive optic near-field lithography based fabrication of large-area diamond-like photonic crystal structure in a single laser exposure step. A multi-level single-surface phase element was laser fabricated on a thin polymer film by two-photon polymerization. A quarter-period phase shift was designed into the phase elements to generate a 3D periodic intensity distribution of double basis diamond-like structure. Finite difference time domain calculation of near-field diffraction patterns and associated isointensity surfaces are corroborated by definitive demonstration of a diamond-like woodpile structure formed inside thick photoresist. A large number of layers provided a strong stopband in the telecom band that matched predictions of numerical band calculation. SEM and spectral observations indicate good structural uniformity over large exposure area that promises 3D photonic crystal devices with high optical quality for a wide range of motif shapes and symmetries. Optical sensing is demonstrated by spectral shifts of the Gamma-Zeta stopband under liquid emersion.

High-Temperature, Perhaps Silicic, Volcanism on Mars Evidenced by Tridymite Detection in High-SiO2 Sedimentary Rock at Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Morris, R. V.; Vaniman, D. T.; Blake, D. F.; Gellert, R.; Chipera, S. J.; Rampe, E. B.; Ming, D. W.; Morrison, S. M.; Downs, R. T.; Treiman, A. H.;

Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

High temperature XRD of Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4}

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

Chetty, Raju, E-mail: rcmallik@physics.iisc.ernet.in; Mallik, Ramesh Chandra, E-mail: rcmallik@physics.iisc.ernet.in

2014-04-24

Quaternary compound with chemical composition Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4} is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

Structural analysis of emerging ferrite: Doped nickel zinc ferrite

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

Kumar, Rajinder; Kumar, Hitanshu; Singh, Ragini Raj

2015-08-28

Ni{sub 0.6-x}Zn{sub 0.4}Co{sub x}Fe{sub 2}O{sub 4} (x = 0, 0.033, 0.264) nanoparticles were synthesized by sol-gel method and annealed at 900°C. Structural properties of all prepared samples were examined with X-ray diffraction (XRD). The partial formation of hematite (α-Fe{sub 2}O{sub 3}) secondary phase with spinel phase cubic structure of undoped and cobalt doped nickel zinc ferrite was found by XRD peaks. The variation in crystallite size and other structural parameters with cobalt doping has been calculated for most prominent peak (113) of XRD and has been explained on the basis of cations ionic radii difference.

Cooperative use of VCD and XRD for the determination of tetrahydrobenzoisoquinolines absolute configuration: a reliable proof of memory of chirality and retention of configuration in enediyne rearrangements.

PubMed

Mondal, Shovan; Naubron, Jean-Valère; Campolo, Damien; Giorgi, Michel; Bertrand, Michéle P; Nechab, Malek

2013-12-01

The absolute configurations (AC) of azaheterocylic compounds resulting from the cascade rearrangement of enediynes involving only light atoms were unambiguously assigned by the joint use of vibrational circular dichroism (VCD) and copper radiation single crystal X-ray diffraction (XRD). These AC determinations proved that the rearrangements of enediynes proceeded with memory of chirality and retention of configuration. © 2013 Wiley Periodicals, Inc.

Laser sintered thin layer graphene and cubic boron nitride reinforced nickel matrix nanocomposites

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Tong, Guoquan

2015-10-01

Laser sintered thin layer graphene (Gr)-cubic boron nitride (CBN)-Ni nanocomposites were fabricated on AISI 4140 plate substrate. The composites fabricating process, composites microstructure and mechanical properties were studied. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy were employed to study the micro structures and composition of the composites. XRD and Raman tests proved that graphene and CBN were dispersed in the nanocomposites. Nanoindentation test results indicate the significant improvements were achieved in the composites mechanical properties.

Classification of crystal structure using a convolutional neural network

PubMed Central

Park, Woon Bae; Chung, Jiyong; Sohn, Keemin; Pyo, Myoungho

2017-01-01

A deep machine-learning technique based on a convolutional neural network (CNN) is introduced. It has been used for the classification of powder X-ray diffraction (XRD) patterns in terms of crystal system, extinction group and space group. About 150 000 powder XRD patterns were collected and used as input for the CNN with no handcrafted engineering involved, and thereby an appropriate CNN architecture was obtained that allowed determination of the crystal system, extinction group and space group. In sharp contrast with the traditional use of powder XRD pattern analysis, the CNN never treats powder XRD patterns as a deconvoluted and discrete peak position or as intensity data, but instead the XRD patterns are regarded as nothing but a pattern similar to a picture. The CNN interprets features that humans cannot recognize in a powder XRD pattern. As a result, accuracy levels of 81.14, 83.83 and 94.99% were achieved for the space-group, extinction-group and crystal-system classifications, respectively. The well trained CNN was then used for symmetry identification of unknown novel inorganic compounds. PMID:28875035

Classification of crystal structure using a convolutional neural network.

PubMed

Park, Woon Bae; Chung, Jiyong; Jung, Jaeyoung; Sohn, Keemin; Singh, Satendra Pal; Pyo, Myoungho; Shin, Namsoo; Sohn, Kee-Sun

2017-07-01

A deep machine-learning technique based on a convolutional neural network (CNN) is introduced. It has been used for the classification of powder X-ray diffraction (XRD) patterns in terms of crystal system, extinction group and space group. About 150 000 powder XRD patterns were collected and used as input for the CNN with no handcrafted engineering involved, and thereby an appropriate CNN architecture was obtained that allowed determination of the crystal system, extinction group and space group. In sharp contrast with the traditional use of powder XRD pattern analysis, the CNN never treats powder XRD patterns as a deconvoluted and discrete peak position or as intensity data, but instead the XRD patterns are regarded as nothing but a pattern similar to a picture. The CNN interprets features that humans cannot recognize in a powder XRD pattern. As a result, accuracy levels of 81.14, 83.83 and 94.99% were achieved for the space-group, extinction-group and crystal-system classifications, respectively. The well trained CNN was then used for symmetry identification of unknown novel inorganic compounds.

Tensile stress effect on epitaxial BiFeO 3 thin film grown on KTaO 3

DOE PAGES

Bae, In-Tae; Ichinose, Tomohiro; Han, Myung-Geun; ...

2018-01-17

Comprehensive crystal structural study is performed for BiFeO 3 (BFO) film grown on KTaO 3 (KTO) substrate using transmission electron microscopy (TEM) and x-ray diffraction (XRD). Nano beam electron diffraction (NBED) combined with structure factor calculation and high resolution TEM images clearly reveal that the crystal structure within BFO thin film is rhombohedral BFO, i.e., bulk BFO phase. Epitaxial relationship found by NBED indicates the BFO film grows in a manner that minimizes lattice mismatch with KTO. It further suggests BFO film is under slight biaxial tensile stress (~0.35%) along in-plane direction. XRD reveals BFO lattice is under compressive stressmore » (~1.6%), along out-of-plane direction as a result of the biaxial tensile stress applied along in-plane direction. This leads to Poisson’s ratio of ~0.68. In addition, we demonstrate (1) why hexagonal notation rather than pseudocubic one is required for accurate BFO phase evaluation and (2) a new XRD method that shows how rhombohedral BFO can readily be identified among other phases by measuring a rhombohedral specific Bragg’s peak.« less

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.

XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

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

Borodi, G.; Pascuta, P.; Dan, V.

2013-11-13

X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd{sub 2}O{sub 3}){sub x}⋅(B{sub 2}O{sub 3}){sub (60−x)}⋅(ZnO){sub 40} glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB{sub 4}O{sub 7}, Zn{sub 4}O(B{sub 6}O{sub 12}), Zn{sub 3}(BO{sub 3}){sub 2} and GdBO{sub 3}. From the XRD data, the average unit-cell parameter and themore » quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO{sub 3}, BO{sub 4} and ZnO{sub 4} are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.« less

Tensile stress effect on epitaxial BiFeO 3 thin film grown on KTaO 3

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

Bae, In-Tae; Ichinose, Tomohiro; Han, Myung-Geun

Comprehensive crystal structural study is performed for BiFeO 3 (BFO) film grown on KTaO 3 (KTO) substrate using transmission electron microscopy (TEM) and x-ray diffraction (XRD). Nano beam electron diffraction (NBED) combined with structure factor calculation and high resolution TEM images clearly reveal that the crystal structure within BFO thin film is rhombohedral BFO, i.e., bulk BFO phase. Epitaxial relationship found by NBED indicates the BFO film grows in a manner that minimizes lattice mismatch with KTO. It further suggests BFO film is under slight biaxial tensile stress (~0.35%) along in-plane direction. XRD reveals BFO lattice is under compressive stressmore » (~1.6%), along out-of-plane direction as a result of the biaxial tensile stress applied along in-plane direction. This leads to Poisson’s ratio of ~0.68. In addition, we demonstrate (1) why hexagonal notation rather than pseudocubic one is required for accurate BFO phase evaluation and (2) a new XRD method that shows how rhombohedral BFO can readily be identified among other phases by measuring a rhombohedral specific Bragg’s peak.« less

Preparation and physical properties of polycrystalline (Bi1-xPbx)2Sr2Ca2Cu3Oy high T c superconductors

NASA Astrophysics Data System (ADS)

Awan, M. S.; Maqsood, M.; Mirza, S. A.; Yousaf, M.; Maqsood, A.

1995-02-01

(Bi1-xPbx:)2Sr2Ca2Cu3Oy ( x = 0.3) high critical transition temperature ( T c) superconductors are synthesized by the solid-state reaction method in polycrystalline form. X-ray diffraction (XRD) studies, direct current (dc) electrical resistivity measurements, scanning electron microscopic (SEM) studies, critical current density measurements, and zero-field alternating current (ac) susceptibility measurements are performed to investigate the physical changes, structural changes, and magnetic behavior of the superconducting samples. X-ray diffraction studies show that a high T c phase exists with orthorhombic symmetry in the specimen. According to the XRD data, the lattice parameters of the high T c phase were determined as a = 0.537(1) nm, b = 0.539(1) nm, and c = 3.70(1) nm. The compound exhibits a superconducting transition at 106 ±1 K for zero resistance. The ac susceptibility measurements in zero field confirm the dc electrical resistivity results; hence both support the XRD results. The particle size and structural changes as a function of the cold-pressing and aging effect are also reported.

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.

Stable Dispersions of Covalently Tethered Polymer Improved Graphene Oxide Nanoconjugates as an Effective Vector for siRNA Delivery.

PubMed

Yadav, Nisha; Kumar, Naveen; Prasad, Peeyush; Shirbhate, Shivani; Sehrawat, Seema; Lochab, Bimlesh

2018-05-02

Conjugates of poly(amidoamine) (PAMAM) with modified graphene oxide (GO) are attractive nonviral vectors for gene-based cancer therapeutics. GO protects siRNA from enzymatic cleavage and showed reasonable transfection efficiency along with simultaneous benefits of low cost and large scale production. PAMAM is highly effective in siRNA delivery but suffers from high toxicity with poor in vivo efficacy. Co-reaction of GO and PAMAM led to aggregation and more importantly, have detrimental effect on stability of dispersion at physiological pH preventing their exploration at clinical level. In the current work, we have designed, synthesized, characterized and explored a new type of hybrid vector (GPD), using GO synthesized via improved method which was covalently tethered with poly(ethylene glycol) (PEG) and PAMAM. The existence of covalent linkage, relative structural changes and properties of GPD is well supported by Fourier transform infrared (FTIR), UV-visible (UV-vis), Raman, X-ray photoelectron (XPS), elemental analysis, powder X-ray diffraction (XRD), thermogravimetry analysis (TGA), dynamic light scattering (DLS), and zeta potential. Scanning electron microscopy (SEM), and transmission electron microscopy (TEM) of GPD showed longitudinally aligned columnar self-assembled ∼10 nm thick polymeric nanoarchitectures onto the GO surface accounting to an average size reduction to ∼20 nm. GPD revealed an outstanding stability in both phosphate buffer saline (PBS) and serum containing cell medium. The binding efficiency of EPAC1 siRNA to GPD was supported by gel retardation assay, DLS, zeta potential and photoluminescence (PL) studies. A lower cytotoxicity with enhanced cellular uptake and homogeneous intracellular distribution of GPD/siRNA complex is confirmed by imaging studies. GPD exhibited a higher transfection efficiency with remarkable inhibition of cell migration and lower invasion than PAMAM and Lipofectamine 2000 suggesting its role in prevention of breast cancer progression and metastasis. A significant reduction in the expression of the specific protein against which siRNA was delivered is revealed by Western blot assay. Furthermore, a pH-triggered release of siRNA from the GPD/siRNA complex was studied to provide a mechanistic insight toward unloading of siRNA from the vector. Current strategy is a way forward for designing effective therapeutic vectors for gene-based antitumor therapy.

The Interactions Between Three Typical PPCPs and LDH

PubMed Central

Li, Erwei; Liao, Libing; Lv, Guocheng; Li, Zhaohui; Yang, Chengxue; Lu, Yanan

2018-01-01

With a layered structure, layered double hydroxide (LDH) has potential applications in remediation of anionic contaminants, which has been a hot topic for recent years. In this study, a Cl type Mg-Al hydrotalcite (Cl-LDH) was prepared by a co-precipitation method. The adsorption process of three pharmaceuticals and personal care products (PPCPs) [tetracycline (TC), diclofenac sodium (DF), chloramphenicol (CAP)] by Cl-LDH was investigated by X-ray diffraction (XRD), Zeta potential, dynamic light scattering (DLS), BET, Fourier transform infrared (FTIR) spectroscopy, and molecular dynamics simulation. The results showed that the adsorption equilibrium of TC and DF could be reached in 120 min, and the maximum adsorption capacity of the TC and DF were 1.85 and 0.95 mmol/g, respectively. The isothermal adsorption model of TC was fitted with the Freundlich adsorption model, and the isothermal adsorption model of DF was fitted with the Langmuir adsorption model. The adsorption dynamics of TC and DF followed the pseudo-second-order model. The adsorption mechanisms of the three PPCPs into Cl-LDH were different based on the experimental results and molecular dynamics simulation. The TC adsorption on Cl-LDH was accompanied by the electrostatic interactions between the negative charge of TC and the positive charge of Cl-LDH. The uptake of DF was attributed to anion exchange and electrostatic interaction. Cl-LDH does not adsorb CAP due to no electrostatic interaction. The molecular dynamic simulation further confirmed different configurations of three selected PPCPs, which were ultimately responsible for the uptake of PPCPs on Cl-LDH. PMID:29556493

Quantitative Characterization of Magnetic Mobility of Nanoparticle in Solution-Based Condition.

PubMed

Rodoplu, Didem; Boyaci, Ismail H; Bozkurt, Akif G; Eksi, Haslet; Zengin, Adem; Tamer, Ugur; Aydogan, Nihal; Ozcan, Sadan; Tugcu-Demiröz, Fatmanur

2015-01-01

Magnetic nanoparticles are considered as the ideal substrate to selectively isolate target molecules or organisms from sample solutions in a wide variety of applications including bioassays, bioimaging and environmental chemistry. The broad array of these applications in fields requires the accurate magnetic characterization of nanoparticles for a variety of solution based-conditions. Because the freshly synthesized magnetic nanoparticles demonstrated a perfect magnetization value in solid form, they exhibited a different magnetic behavior in solution. Here, we present simple quantitative method for the measurement of magnetic mobility of nanoparticles in solution-based condition. Magnetic mobility of the nanoparticles was quantified with initial mobility of the particles using UV-vis absorbance spectroscopy in water, ethanol and MES buffer. We demonstrated the efficacy of this method through a systematic characterization of four different core-shell structures magnetic nanoparticles over three different surface modifications. The solid nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD) and saturation magnetization (Ms). The surfaces of the nanoparticles were functionalized with 11-mercaptoundecanoic acid and bovine serum albumin BSA was selected as biomaterial. The effect of the surface modification and solution media on the stability of the nanoparticles was monitored by zeta potentials and hydrodynamic diameters of the nanoparticles. Results obtained from the mobility experiments indicate that the initial mobility was altered with solution media, surface functionalization, size and shape of the magnetic nanoparticle. The proposed method easily determines the interactions between the magnetic nanoparticles and their surrounding biological media, the magnetophoretic responsiveness of nanoparticles and the initial mobilities of the nanoparticles.

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.

Antibacterial efficacy of silver nanoparticles and ethyl acetate's metabolites of the potent halophilic (marine) bacterium, Bacillus cereus A30 on multidrug resistant bacteria.

PubMed

Arul, Dhayalan; Balasubramani, Govindasamy; Balasubramanian, Velramar; Natarajan, Thillainathan; Perumal, Pachiappan

2017-10-01

Bacteria are generally responsible for the prevalence of several diseases and pathogenic bacteria are showing increasing resistance to different antibacterials. During the present study an extremophilic bacterium-A30 isolated from the marine waters was characterized and evaluated against four multi-drug resistant (MDR) pathogens, viz; Methicillin-resistant Staphylococcus aureus (MRSA), Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa. The sensitivity pattern of the selected pathogens was tested with 31 antibiotics. Among the 47 marine microbial extracts tested on 4-MDR pathogens viz: Methicillin-resistant Staphylococcus aureus (MRSA), E. coli, K. pneumoniae and P. aeruginosa, only our strain A30 strain exhibited highest efficacy. This strain was subsequently subjected to 16S rDNA sequencing which confirmed its allocation as Bacillus cereus. Silver nanoparticle (AgNPs) synthesis and ethyl acetate extraction were performed using the supernatant of B. cereus. The synthesized AgNPs were characterized by UV-Visible, Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), Field emission-scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX), and Zeta potential analyses. The presence of functional groups and 13 bioactive components in the ethyl acetate extract were analyzed using FT-IR and gas chromatography-mass spectrometry (GC-MS). The synthesized of AgNPs and the ethyl acetate extract showed preponderant activity against P. aeruginosa and MRSA, respectively. The effects of AgNPs were significant when compared to ethyl acetate extract. Therefore, the halophilic bacterium, B. cereus mediated AgNPs could provide antibacterial applications in the biomedical industries.

A quantitative X-ray diffraction inventory of the tephra and volcanic glass inputs into the Holocene marine sediment archives off Iceland: A contribution to V.A.S.T.

USGS Publications Warehouse

Andrews, John T.; Kristjansdottir, Greta B.; Eberl, Dennis D.; Jennings, Anne E.

2013-01-01

This paper re-evaluates how well quantitative x-ray diffraction (qXRD) can be used as an exploratory method of the weight percentage (wt%) of volcaniclastic sediment, and to identify tephra events in marine cores. In the widely used RockJock v6 software programme, qXRD tephra and glass standards include the rhyodacite White River tephra (Alaska), a rhyolitic tephra (Hekla-4) and the basaltic Saksunarvatn tephra. Experiments of adding known wt% of tephra to felsic bedrock samples indicated that additions ≥10 wt% are accurately detected, but reliable estimates of lesser amounts are masked by amorphous material produced by milling. Volcaniclastic inputs range between 20 and 50 wt%. Primary tephra events are identified as peaks in residual qXRD glass wt% from fourth-order polynomial fits. In cores where tephras have been identified by shard counts in the > 150 µm fraction, there is a positive correlation (validation) with peaks in the wt% glass estimated by qXRD. Geochemistry of tephra shards confirms the presence of several Hekla-sourced tephras in cores B997-317PC1 and -319PC2 on the northern Iceland shelf. In core B997-338 (north-west Iceland), there are two rhyolitic tephras separated by ca. 100 cm with uncorrected radiocarbon dates on articulated shells of around 13 000 yr B.P. These tephras may be correlatives of the Borrobol and Penifiler tephras found in Scotland. The number of Holocene tephra events per 1000 yr was estimated from qXRD on 16 cores and showed a bimodal distribution with an increased number of events in both the late and early Holocene.

Revisiting the hydration structure of aqueous Na +

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

Galib, M.; Baer, M. D.; Skinner, L. B.

In this paper, a combination of theory, X-ray diffraction (XRD) and extended x-ray absorption fine structure (EXAFS) are used to probe the hydration structure of aqueous Na +. The high spatial resolution of the XRD measurements corresponds to Qmax = 24 Å –1 while the first-reported Na K-edge EXAFS measurements have a spatial resolution corresponding to 2k = Qmax = 16 Å –1. Both provide an accurate measure of the shape and position of the first peak in the Na–O pair distribution function, g NaO(r). The measured Na–O distances of 2.384 ± 0.003 Å (XRD) and 2.37 ± 0.024 Åmore » (EXAFS) are in excellent agreement. These measurements show a much shorter Na–O distance than generally reported in the experimental literature (Na–O avg ~ 2.44 Å) although the current measurements are in agreement with recent neutron diffraction measurements. The measured Na–O coordination number from XRD is 5.5 ± 0.3. The measured structure is compared with both classical and first-principles density functional theory (DFT) simulations. Both of the DFT-based methods, revPBE and BLYP, predict a Na–O distance that is too long by about 0.05 Å with respect to the experimental data (EXAFS and XRD). The inclusion of dispersion interactions (–D3 and –D2) significantly worsens the agreement with experiment by further increasing the Na–O distance by 0.07 Å. In contrast, the use of a classical Na–O Lennard-Jones potential with SPC/E water accurately predicts the Na–O distance as 2.39 Å although the Na–O peak is over-structured with respect to experiment.« less

Revisiting the hydration structure of aqueous Na +

DOE PAGES

Galib, M.; Baer, M. D.; Skinner, L. B.; ...

2017-02-27

In this paper, a combination of theory, X-ray diffraction (XRD) and extended x-ray absorption fine structure (EXAFS) are used to probe the hydration structure of aqueous Na +. The high spatial resolution of the XRD measurements corresponds to Qmax = 24 Å –1 while the first-reported Na K-edge EXAFS measurements have a spatial resolution corresponding to 2k = Qmax = 16 Å –1. Both provide an accurate measure of the shape and position of the first peak in the Na–O pair distribution function, g NaO(r). The measured Na–O distances of 2.384 ± 0.003 Å (XRD) and 2.37 ± 0.024 Åmore » (EXAFS) are in excellent agreement. These measurements show a much shorter Na–O distance than generally reported in the experimental literature (Na–O avg ~ 2.44 Å) although the current measurements are in agreement with recent neutron diffraction measurements. The measured Na–O coordination number from XRD is 5.5 ± 0.3. The measured structure is compared with both classical and first-principles density functional theory (DFT) simulations. Both of the DFT-based methods, revPBE and BLYP, predict a Na–O distance that is too long by about 0.05 Å with respect to the experimental data (EXAFS and XRD). The inclusion of dispersion interactions (–D3 and –D2) significantly worsens the agreement with experiment by further increasing the Na–O distance by 0.07 Å. In contrast, the use of a classical Na–O Lennard-Jones potential with SPC/E water accurately predicts the Na–O distance as 2.39 Å although the Na–O peak is over-structured with respect to experiment.« less

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

Zhang, Baozhuo; Young, Marcus L.

Many technological applications of austenitic shape memory alloys (SMAs) involve cyclical mechanical loading and unloading in order to take advantage of pseudoelasticity. In this paper, we investigated the effect of mechanical bending of pseudoelastic NiTi SMA wires using high-energy synchrotron radiation X-ray diffraction (SR-XRD). Differential scanning calorimetry was performed to identify the phase transformation temperatures. Scanning electron microscopy images show that micro-cracks in compressive regions of the wire propagate with increasing bend angle, while tensile regions tend not to exhibit crack propagation. SR-XRD patterns were analyzed to study the phase transformation and investigate micromechanical properties. By observing the various diffraction peaks such as the austenite (200) and the martensite (more » $${\\bar 1}12$$), ($${\\bar 1}03$$), ($${\\bar 1}11$$), and (101) planes, intensities and residual strain values exhibit strong anisotropy, depending upon whether the sample is in compression or tension during bending.« less

Study of Initial Stages of Ball-Milling of Cu Powder Using X-ray Diffraction

NASA Astrophysics Data System (ADS)

Gayathri, N.; Mukherjee, Paramita

2018-04-01

The initial stage of size refinement of Cu powder is studied using detailed X-ray diffraction (XRD) analysis to understand the mechanism of formation of nanomaterials during the ball-milling process. The study was restricted to samples obtained for milling time up to 240 min to understand the deformation mechanism at the early stages of ball milling. Various model based approaches for the analysis of the XRD were used to study the evolution of the microstructural parameters such as domain size and microstrain along the different crystallographic planes. It was seen that the domain size saturates at a low value along the (311) plane whereas the size along the (220) and (200) plane is still higher. The r.m.s microstrain showed a non-monotonic change along the different crystallographic directions up to the milling time of 240 min.

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

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

Stan, Manuela, E-mail: manuela.stan@itim-cj.ro; Popa, Adriana; Toloman, Dana

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn{sup 2+} ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes andmore » oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.« less

Body-centered orthorhombic C 16 : A novel topological node-line semimetal

DOE PAGES

Wang, Jian -Tao; Weng, Hongming; Nie, Simin; ...

2016-05-11

We identify by ab initio calculations a novel topological semimetal carbon phase in all-sp 2 bonding networks with a 16-atom body-centered orthorhombic unit cell, termed bco-C 16. Total-energy calculations show that bco-C 16 is comparable to solid fcc-C 60 in energetic stability, and phonon and molecular dynamics simulations confirm its dynamical stability. This all-sp 2 carbon allotrope can be regarded as a three-dimensional modification of graphite, and its simulated x-ray diffraction (XRD) pattern matches well a previously unexplained diffraction peak in measured XRD spectra of detonation and chimney soot, indicating its presence in the specimen. Electronic band structure calculations revealmore » that bco-C 16 is a topological node-line semimetal with a single nodal ring. Lastly, these findings establish a novel carbon phase with intriguing structural and electronic properties of fundamental significance and practical interest.« less

Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

NASA Astrophysics Data System (ADS)

Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

2003-10-01

The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

A photodiode based on PbS nanocrystallites for FYTRONIX solar panel automatic tracking controller

NASA Astrophysics Data System (ADS)

Wageh, S.; Farooq, W. A.; Tataroğlu, A.; Dere, A.; Al-Sehemi, Abdullah G.; Al-Ghamdi, Ahmed A.; Yakuphanoglu, F.

2017-12-01

The structural, optical and photoelectrical properties of the fabricated Al/PbS/p-Si/Al photodiode based on PbS nanocrystallites were investigated. The PbS nanocrystallites were characterized by X-ray diffraction (XRD), UV-VIS-NIR, Infrared and Raman spectroscopy. The XRD diffraction peaks show that the prepared PbS nanostructure is in high crystalline state. Various electrical parameters of the prepared photodiode were analyzed from the electrical characteristics based on I-V and C-V-G. The photodiode has a high rectification ratio of 5.85×104 at dark and ±4 V. Moreover, The photocurrent results indicate a strong photovoltaic behavior. The frequency dependence of capacitance and conductance characteristics was attributed to depletion region behavior of the photodiode. The diode was used to control solar panel power automatic tracking controller in dual axis. The fabricated photodiode works as a photosensor to control Solar tracking systems.

Thin single-crystalline Bi2(Te1-xSex)3 ternary nanosheets synthesized by a solvothermal technique

NASA Astrophysics Data System (ADS)

Guo, Jing; Jian, Jikang; Zhang, Zhihua; Wu, Rong; Li, Jin; Sun, Yanfei

2016-01-01

Bi2(Te1-xSex)3 ternary nanosheets have been successfully synthesized through a facile solvothermal technique using diethylenetriamine as solvent, where x can vary from 0 to 1. X-ray diffraction (XRD) and Scanning electron microscopy (SEM) indicate that the as-synthesized Bi2(Te1-xSex)3 samples are nanosheets with rhombohedral structure, and the thickness of the nanosheets can be as thin as several nanometers. High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) reveal that the nanosheets are single crystalline with a rhombohedral structure. Energy disperse spectroscopy (EDS) and XRD analysis by Vegard's law confirm that the ternary Bi2(Te1-xSex)3 nanosheets have been obtained here. The growth of the nanosheets is discussed based on an amine-based molecular template mechanism that has been employed to synthesize some other metal chalcogenides.

Sodium storage mechanisms of bismuth in sodium ion batteries: An operando X-ray diffraction study

NASA Astrophysics Data System (ADS)

Gao, Hui; Ma, Wensheng; Yang, Wanfeng; Wang, Jiawei; Niu, Jiazheng; Luo, Fakui; Peng, Zhangquan; Zhang, Zhonghua

2018-03-01

Understanding the sodium (Na) chemistry is crucial for development of high-performance sodium ion batteries (SIBs). Nanostructured bismuth (Bi) has shown great potentials as an anode in SIBs, however, the Na storage mechanisms of Bi are still unclear. Herein, the operando X-ray diffraction (XRD) technique was utilized to probe the Na storage mechanisms of three Bi anodes (sputtered Bi film, nanoporous Bi and commercial Bi). Despite different morphologies and sizes, all the Bi anodes follow the same two-step reversible alloying/dealloying mechanisms (Bi ↔ NaBi ↔ Na3Bi) during the discharge/charge processes, associated with two voltage plateaus. As for the intercalation/deintercalation mechanism proposed for nanostructured Bi anodes in SIBs, we rationalize the reason why only the Bi phase is detected in the discharged/charged samples under ex-situ XRD conditions through addressing the stability issue of the Na-Bi system (NaBi and Na3Bi).

Disruption of crystalline structure of Sn3.5Ag induced by electric current

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

Huang, Han-Chie; Lin, Kwang-Lung, E-mail: matkllin@mail.ncku.edu.tw; Wu, Albert T.

2016-03-21

This study presented the disruption of the Sn and Ag{sub 3}Sn lattice structures of Sn3.5Ag solder induced by electric current at 5–7 × 10{sup 3} A/cm{sup 2} with a high resolution transmission electron microscope investigation and electron diffraction analysis. The electric current stressing induced a high degree of strain on the alloy, as estimated from the X-ray diffraction (XRD) peak shift of the current stressed specimen. The XRD peak intensity of the Sn matrix and the Ag{sub 3}Sn intermetallic compound diminished to nearly undetectable after 2 h of current stressing. The electric current stressing gave rise to a high dislocation density ofmore » up to 10{sup 17}/m{sup 2}. The grain morphology of the Sn matrix became invisible after prolonged current stressing as a result of the coalescence of dislocations.« less

X-ray diffraction study of low-temperature phase transformations in nickel-titanium orthodontic wires.

PubMed

Iijima, M; Brantley, W A; Guo, W H; Clark, W A T; Yuasa, T; Mizoguchi, I

2008-11-01

Employ conventional X-ray diffraction (XRD) to analyze three clinically important nickel-titanium orthodontic wire alloys over a range of temperatures between 25 and -110 degrees C, for comparison with previous results from temperature-modulated differential scanning calorimetry (TMDSC) studies. The archwires selected were 35 degrees C Copper Ni-Ti (Ormco), Neo Sentalloy (GAC International), and Nitinol SE (3M Unitek). Neo Sentalloy, which exhibits superelastic behavior, is marketed as having shape memory in the oral environment, and Nitinol SE and 35 degrees C Copper Ni-Ti also exhibit superelastic behavior. All archwires had dimensions of 0.016in.x0.022in. (0.41 mm x 0.56 mm). Straight segments cut with a water-cooled diamond saw were placed side-by-side to yield a 1 cm x 1cm test sample of each wire product for XRD analysis (Rint-Ultima(+), Rigaku) over a 2theta range from 30 degrees to 130 degrees and at successive temperatures of 25, -110, -60, -20, 0 and 25 degrees C. The phases revealed by XRD at the different analysis temperatures were in good agreement with those found in previous TMDSC studies of transformations in these alloys, in particular verifying the presence of R-phase at 25 degrees C. Precise comparisons are not possible because of the approximate nature of the transformation temperatures determined by TMDSC and the preferred crystallographic orientation present in the wires. New XRD peaks appear to result from low-temperature transformation in martensite, which a recent transmission electron microscopy (TEM) study has shown to arise from twinning. While XRD is a useful technique to study phases in nickel-titanium orthodontic wires and their transformations as a function of temperature, optimum insight is obtained when XRD analyses are combined with complementary TMDSC and TEM study of the wires.

Tetramethylene glycol mediated hydrothermal synthesis of defect-rich SnO2 nanoparticles for fast adsorption and degradation of MB dye

NASA Astrophysics Data System (ADS)

Rani, Barkha; Jadhao, Charushila Vasant; Sahu, Niroj Kumar

2018-04-01

Defect-rich pristine tin oxide nanoparticles (SnO2 NPs) with high colloidal stability have been synthesized by tetramethylene glycol (TMG) mediated hydrothermal process and characterized by XRD, TEM, Zeta Potential, PL spectroscopy and porosity measurement techniques. XRD result suggests the formation of rutile phase of SnO2 with average crystallite size of 2.65 nm. TMG act as a structure directing agent assist in the formation of network like structure of SnO2 NPs as confirmed from TEM. Significant blue shifts in the UV absorption spectrum as that of the bulk and defect bands in the PL spectrum are observed. The nanomaterial possesses very high surface area of 263.102 m2/g and large pore volume. The above properties strongly influence the photocatalytic degradation of methylene blue dye. Very fast adsorption and 96% degradation (under UV irradiation) has been achieved when 10 ppm methylene blue solutions is catalysed by 20 mg SnO2 NPs which pave the way for potential environmental application.

XRD and mineralogical analysis of gypsum dunes at White Sands National Monument, New Mexico and applications to gypsum detection on Mars

NASA Astrophysics Data System (ADS)

Lafuente, B.; Bishop, J. L.; Fenton, L. K.; King, S. J.; Blake, D.; Sarrazin, P.; Downs, R.; Horgan, B. H.

2013-12-01

A field portable X-ray Diffraction (XRD) instrument was used at White Sands National Monument to perform in-situ measurements followed by laboratory analyses of the gypsum-rich dunes and to determine its modal mineralogy. The field instrument is a Terra XRD (Olympus NDT) based on the technology of the CheMin (Chemistry and Mineralogy) instrument onboard the Mars Science Laboratory (MSL) rover Curiosity which is providing the mineralogical and chemical composition of scooped soil samples and drilled rock powders collected at Gale Crater [1]. Using Terra at White Sands will contribute to 'ground truth' for gypsum-bearing environments on Mars. Together with data provided by VNIR spectra [2], this study clarifies our understanding of the origin and history of gypsum-rich sand dunes discovered near the northern polar region of Mars [3]. The results obtained from the field analyses performed by XRD and VNIR spectroscopy in four dunes at White Sands revealed the presence of quartz and dolomite. Their relative abundance has been estimated using the Reference Intensity Ratio (RIR) method. For this study, particulate samples of pure natural gypsum, quartz and dolomite were used to prepare calibration mixtures of gypsum-quartz and gypsum-dolomite with the 90-150μm size fractions. All single phases and mixtures were analyzed by XRD and RIR factors were calculated. Using this method, the relative abundance of quartz and dolomite has been estimated from the data collected in the field. Quartz appears to be present in low amounts (2-5 wt.%) while dolomite is present at percentages up to 80 wt.%. Samples from four dunes were collected and prepared for subsequent XRD analysis in the lab to estimate their composition and illustrate the changes in mineralogy with respect to location and grain size. Gypsum-dolomite mixtures: The dolomite XRD pattern is dominated by an intense diffraction peak at 2θ≈36 deg. which overlaps a peak of gypsum, This makes low concentrations of dolomite difficult to quantify in mixtures with high concentration of gypsum. Dolomite has been detected in some locations at dune 3 as high as 80 wt.%. Gypsum-quartz mixtures: The intensity of the main diffraction peak of quartz at 2θ≈31 deg. decreases progressively with the decrease of the amount of quartz in the mixtures. Samples from dune 1 and 2 show quartz abundance at 5.6 and 2.6 wt.% respectively . [1] Blake et al. Space Sci. Rev. (2012). doi:10.1007/s11214-012-9905-1. [2] King et al. (2013) AGU, submitted. [3] Langevin et al. (2005). Science 307, 1584-1586.

The effect of doped zinc on the structural properties of nano-crystalline (Se0.8Te0.2)100-xZnx

NASA Astrophysics Data System (ADS)

Kumar, Arun; Singh, Harkawal; Gill, P. S.; Goyal, Navdeep

2016-05-01

The effect of metallic zinc (Zn) on the structural properties of (Se0.8Te0.2)1-XZnX (x=0, 2, 6, 8, 10) samples analyzed by X-ray Diffraction (XRD). The presence of sharp peaks in XRD patterns confirmed the crystalline nature of the samples and is indexed in orthorhombic crystal structure. XRD studies predicts that the average particle size of all the samples are about 46.29 nm, which is less than 100 nm and hence have strong tendency of agglomeration. Williamson-Hall plot method was used to evaluate the lattice strain. The dislocation density and no. of unit cells of the samples were calculated which show the inverse relation with each other. Morphology index derived from FWHM of XRD data explains the direct relationship with the particle size.

DISTRIBUTION SYSTEM SOLIDS - A RESEARCH APPROACH

EPA Science Inventory

The U.S. EPA's AWBERC research facility is equipped with capabilities to analyze a variety of solids in support many Laboratory-wide research studies. Techniques available on site include X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microsco...

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.

In-field X-ray and neutron diffraction studies of re-entrant charge-ordering and field induced metastability in La0.175Pr0.45Ca0.375MnO3-δ

NASA Astrophysics Data System (ADS)

Sharma, Shivani; Shahee, Aga; Yadav, Poonam; da Silva, Ivan; Lalla, N. P.

2017-11-01

Low-temperature high-magnetic field (2 K, 8 T) (LTHM) powder X-ray diffraction (XRD) and time of flight powder neutron diffraction (NPD), low-temperature transmission electron microscopic (TEM), and resistivity and magnetization measurements have been carried out to investigate the re-entrant charge ordering (CO), field induced structural phase transitions, and metastability in phase-separated La0.175Pr0.45Ca0.375MnO3-δ (LPCMO). Low-temperature TEM and XRD studies reveal that on cooling under zero-field, paramagnetic Pnma phase transforms to P21/m CO antiferromagnetic (AFM) insulating phase below ˜233 K. Unlike reported literature, no structural signature of CO AFM P21/m to ferromagnetic (FM) Pnma phase-transition during cooling down to 2 K under zero-field was observed. However, the CO phase was found to undergo a re-entrant transition at ˜40 K. Neutron diffraction studies revealed a pseudo CE type spin arrangement of the observed CO phase. The low-temperature resistance, while cooled under zero-field, shows insulator to metal like transition below ˜105 K with minima at ˜25 K. On application of field, the CO P21/m phase was found to undergo field-induced transition to FM Pnma phase, which shows irreversibility on field removal below ˜40 K. Zero-field warming XRD and NPD studies reveal that field-induced FM Pnma phase is a metastable phase, which arise due to the arrest of kinetics of the first-order phase transition of FM Pnma to CO-AFM P21/m phase, below 40 K. Thus, a strong magneto-structural coupling is observed for this system. A field-temperature (H-T) phase-diagram has been constructed based on the LTHM-XRD, which matches very nicely with the reported H-T phase-diagram constructed based on magnetic measurements. Due to the occurrence of gradual growth of the re-entrant CO phase and the absence of a clear structural signature of phase-separation of CO-AFM P21/m and FM Pnma phases, the H-T minima in the phase-diagram of the present LPCMO sample has been attributed to the strengthening of AFM interaction during re-entrant CO transition and not to glass like "dynamic to frozen" transition.

Thermoluminescence and X-ray diffraction studies on sliced ancient porcelain samples

NASA Astrophysics Data System (ADS)

Leung, P. L.; Yang, B.

1999-09-01

The thermal activation characteristics (TACs) of the sensitivity of the '110°C' peak in 14 sliced ancient Chinese porcelain samples are studied. Comparing with the TACs of natural quartz and synthetic mullite, the relation between the TACs and the composition of the sample is discussed with reference to the X-ray diffraction (XRD) spectra. It is suggested that in some cases, contribution of the porcelain components other than quartz to the TACs is not negligible.

Test and Delivery of the Chemin Mineralogical Instrument for Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Blake, D. F.; Vaniman, D.; Anderson, R.; Bish, D.; Chipera, S.; Chemtob, S.; Crisp, J.; DesMarais, D. J.; Downs, R.; Feldman, S.;

Deposition of dual-layer coating on Ti6Al4V

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

Synthesis and characterization of nanostructured titanium carbide for fuel cell applications

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

Singh, Paviter; Singh, Harwinder; Singh, Bikramjeet

2016-04-13

Titanium carbide (TiC) nanoparticles have been successfully synthesized by carbo-thermic reaction of titanium and acetone at 800 °C. This method is relatively low temperature synthesis route. It can be used for large scale production of TiC. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA) techniques. XRD analysis confirmed the formation of single phase TiC. XRD analysis confirmed that the particles are spherical in shape with an average particle size of 13 nm. DTA analysis shows that the phase is stable upto 900 °C and the material can be used formore » high temperature applications.« less

Role of low-temperature AlGaN interlayers in thick GaN on silicon by metalorganic vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Fritze, S.; Drechsel, P.; Stauss, P.; Rode, P.; Markurt, T.; Schulz, T.; Albrecht, M.; Bläsing, J.; Dadgar, A.; Krost, A.

2012-06-01

Thin AlGaN interlayers have been grown into a thick GaN stack on Si substrates to compensate tensile thermal stress and significantly improve the structural perfection of the GaN. In particular, thicker interlayers reduce the density in a-type dislocations as concluded from x-ray diffraction (XRD) measurements. Beyond an interlayer thickness of 28 nm plastic substrate deformation occurs. For a thick GaN stack, the first two interlayers serve as strain engineering layers to obtain a crack-free GaN structure, while a third strongly reduces the XRD ω-(0002)-FWHM. The vertical strain and quality profile determined by several XRD methods demonstrates the individual impact of each interlayer.

Structural investigations in helium charged titanium films using grazing incidence XRD and EXAFS spectroscopy

NASA Astrophysics Data System (ADS)

Wan, Chubin; Zhou, Xiaosong; Wang, Yuting; Li, Shina; Ju, Xin; Peng, Shuming

2014-01-01

The crystal structure and local atomic arrangements surrounding Ti atoms were determined for He-charged hexagonal close-packed (hcp) Ti films and measured at glancing angles by synchrotron radiation X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS) spectroscopy, respectively. The charged specimens were prepared by direct current magnetron sputtering with a He/Ar mixture. He atoms with a relatively medium concentration (He/Ti atomic ratio as high as 17 at.%) were incorporated evenly in the deposited films. XRD results showed the changes in the peak intensities in Ti films with different He contents. EXAFS Fourier Transform analysis indicated that the average Ti-Ti distance decreased significantly, and proved the existence of phase transition.

Study of structural and magnetic properties of cobalt ferrite nanoparticles sintered at different temperature

NASA Astrophysics Data System (ADS)

Kumari, Mukesh; Bhatnagar, Mukesh Chander

2018-05-01

Cobalt ferrite (CFO) has been synthesized in the form of nanoparticles (NPs) through sol-gel auto-combustion method. The prepared NPs of CFO were sintered for four hours at various temperatures from 300°C to 900°C. The physical properties of the sintered samples have been optimized using X-ray diffraction (XRD), Raman spectroscopy and physical properties measurement system (PPMS). The XRD and Raman studies have confirmed the cubic spinel phase formation of CFO NPs. XRD results showed that as we increase the sintering temperature the crystallite size of particles increases. Whereas the magnetic studies revealed that the saturation magnetization (MS) increases while the coercivity (HC) of nanoparticles decreases with increase of sintering temperature.

Single phase Pb0.7Bi0.3Fe0.65Nb0.35O3 multiferroic: Neutron diffraction, impedance and modulus studies

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshpande, S. K.; Angadi, Basavaraj

2018-04-01

The Pb0.7Bi0.3Fe0.65Nb0.35O3 (PBFNO) multiferroic solid solution was synthesized by using single step solid state reaction method. Single phase formation was confirmed through room temperature (RT) X Ray Diffraction (XRD) and Neutron Diffraction (ND). Rietveld refinement was used to perform the structural analysis using FullProf Suite program. RT XRD and ND patterns well fitted with monoclinic structure (Cm space group) and cell parameters from the ND data are found to be a = 5.6474(4) Å, b = 5.6415(3) Å, c = 3.9992(3) Å and β = 89.95(2)°. ND data at RT exhibits G-type antiferromagnetic structure. The electrical properties (impedance and modulus) of PBFNO were studied as a function of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K) by Impedance spectroscopy technique. Impedance and modulus spectroscopy studies confirm the contribution to the conductivity is from grains only and the relaxation is of non-Debye type. The PBFNO sample exhibits negative temperature coefficient of resistance (NTCR) behaviour. PBFNO is found be a potential candidate for RT applications.

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.

Developing high-transmittance heterojunction diodes based on NiO/TZO bilayer thin films

PubMed Central

2013-01-01

In this study, radio frequency magnetron sputtering was used to deposit nickel oxide thin films (NiO, deposition power of 100 W) and titanium-doped zinc oxide thin films (TZO, varying deposition powers) on glass substrates to form p(NiO)-n(TZO) heterojunction diodes with high transmittance. The structural, optical, and electrical properties of the TZO and NiO thin films and NiO/TZO heterojunction devices were investigated with scanning electron microscopy, X-ray diffraction (XRD) patterns, UV-visible spectroscopy, Hall effect analysis, and current-voltage (I-V) analysis. XRD analysis showed that only the (111) diffraction peak of NiO and the (002) and (004) diffraction peaks of TZO were observable in the NiO/TZO heterojunction devices, indicating that the TZO thin films showed a good c-axis orientation perpendicular to the glass substrates. When the sputtering deposition power for the TZO thin films was 100, 125, and 150 W, the I-V characteristics confirmed that a p-n junction characteristic was successfully formed in the NiO/TZO heterojunction devices. We show that the NiO/TZO heterojunction diode was dominated by the space-charge limited current theory. PMID:23634999

Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline

PubMed Central

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.

2013-01-01

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294

Structural and thermal properties of silk fibroin - Silver nanoparticles composite films

NASA Astrophysics Data System (ADS)

Shivananda, C. S.; Rao B, B. Lakshmeesha; Shetty, G. Rajesh; Sangappa, Y.

2018-05-01

In this work, silk fibroin-silver nanoparticles (SF-AgNPs) composite films have been prepared by simple solution casting method. The composite films were examined for structural and thermal properties using X-ray diffraction (XRD), thermogravimatric (TGA) and differential scanning calorimetry (DSC) analysis. The XRD results showed that with the introduction of AgNPs in the silk fibroin matrix the amorphous nature of the silk fibroin decreases with increasing nanoparticles concentration. The silk fibroin films possess good thermal stability with the presence of AgNPs.

Structural, thermal, optical, and photoacoustic study of nanocrystalline Bi{sub 2}Te{sub 3} produced by mechanical alloying

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

Souza, S. M.; Triches, D. M.; Poffo, C. M.

2011-01-01

Nanocrystalline Bi{sub 2}Te{sub 3} was produced by mechanical alloying and its properties were investigated by differential scanning calorimetry (DSC) x-ray diffraction (XRD), Raman spectroscopy (RS), and photoacoustic spectroscopy (PAS). Combining the XRD and RS results, the volume fraction of the interfacial component in as-milled and annealed samples was estimated. The PAS results suggest that the contribution of the interfacial component to the thermal diffusivity of nanostructured Bi{sub 2}Te{sub 3} is very significant.

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

PubMed

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

2014-04-24

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

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

of highly oriented pyrolytic graphite ( HOPG ) flake. Two electrode system containing platinum as counter electrode and HOPG as working electrode is... XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3 and PyDop1-ɤ-Fe2O3-graphene are given in Figure 1e. HOPG show a very sharp diffraction...atoms arranged in hexagonal pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG

Structural and optical properties of electrospun MoO3 nanowires

NASA Astrophysics Data System (ADS)

Das, Arnab Kumar; Modak, Rajkumar; Srinivasan, Ananthakrishnan

2018-05-01

Nanofibers of polyvinyl alcohol (PVA) containing ammonium molybdate were prepared by a combination of sol-gel and electrospinning techniques. Heat treatment of the as-spun composite nanofibers at 500 °C yielded MoO3 nanowires with a diameter of ˜180 nm. The product was characterized by X-ray diffraction (XRD), scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. XRD and Raman spectra of the heat nanowires clearly show the formation of orthorhombic single phase MoO3 structure without any impurity phases.

Synthesis and Properties of Ortho-Nitro-Fe Complex

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

Mishra, A.; Mishra, Niyati; Sharma, R.

2011-07-15

Ortho-Nitro-Fe complex (Transition metal complex) has synthesized by chemical route method and properties of made complex has characterized by X-Ray diffraction (XRD), Moessbauer spectroscopy, Fourier transformation infra-red spectroscopy (FTIR) and X-Ray photoelectron spectroscopy (XPS). XRD analysis shows that sample is crystalline in nature and having particle size in the range of few nano meters. Moessbauer spectroscopy at room temperature shows the oxidation state of Iron (central metal ion) after complaxasion. FTIR spectra of the complex confirms the coordination of metal ion with ligand.

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

Rifaximin - Chitosan Nanoparticles for Inflammatory Bowel Disease (IBD).

PubMed

Kumar, Jatinder; Newton, Amaldoss M J

2017-01-01

Inflammatory Bowel Disease (IBD) cannot be controlled easily and the recurrence is the most challenging issue for the physicians. There are various controlled and colon targeted drug delivery systems available for the treatment with limited success rate. Nanoparticles prepared by using the colon targeted polymers such as chitosan may improve the IBD due to their smaller size, unique physico chemical properties and targeting potential. The aim of this investigation was designed to formulate and develop a colon targeted polysaccharide nanoparticles of rifaximin (RFX) by using linear polysaccharide chitosan, for the improvement of rifaximin solubility, overall therapeutic efficacy and colon targeting. The research was focused on developing RFX nanoparticles for the treatment of Inflammatory Bowel Disease (IBD) by ionic gelation method. Nanoparticles were subjected to various characterization techniques such as XRD, FTIR and mean particle size (MPS) by Master Sizer and Zeta Sizer. Transmission Electron Microscopy (TEM), drug entrapment efficiency and zeta potential are also determined for the developed formulations. The efficiency of drug release from prepared formulation was studied in vitro by using a dialysis bag diffusion technique in the buffer condition mimicking stomach, intestine and colonic pH conditions. The prepared nanoparticles demonstrated the size in the nano range. The drug release profile was controlled in the upper GI tract and the maximum amount of drug was released in the colonic conditions. The prepared nanoparticles significantly improved the solubility of rifaximin. The zeta potential of the best chitosan preparation was found to be 37.79, which confirms the stability of prepared nanosuspension. Nanoparticles with small particle size found to have high encapsulation efficiency and relatively high loading capacity and predetermined in vitro release profile. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

IVABRADINE LOADED SOLID LIPID MICROPARTICLES: FORMULATION, CHARACTERIZATION AND OPTIMIZATION BY CENTRAL COMPOSITE ROTATABLE DESIGN.

PubMed

Hanif, Muhammad; Khan, Hafeez Ullah; Afzal, Samina; Sher, Muhammad

2017-01-01

The current research focused on improvement of oral bioavailability and decrease in dosing frequency of ivabradine (Iva) in order to enhance patient compliance by formulating novel sustained release Iva loaded solid lipid microparticles (SLMs) with the help of melt emulsification technique. SLMs formulations were designed with the help of three level central composite rotatable design (CCRD) to study the impact of independent variables like lipid concentration, surfactant concentration and stirring speed on responses - percentage yield (Y,) and entrapment efficiency (Y2). Compatibility between the drug and bees wax (BW) was checked by conducting Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRD). SLMs were further evaluated for rheological behavior, zeta potential, particle size and for morphology by scanning'electron microscope (SEM). The release of drug from SLMs was conducted by USP type-Il apparatus at pH 1.2, pH 6.8 and data were analyzed by different kinetic models like zero order, first order, Higuchi model, Korsmeyer-Peppas and Hixon-Crowell models. The rheo- logical studies approved the good flow behavior of SLMs and spherical smooth surface of SLMs was observed from SEM. DSC, FTIR and XRD studies concluded the lack of any possible interaction between formulation components. The size-of SLMs ranged from 300 to 500 pm and zeta potential study showed the presence of higher negative charge (-30 to -52 mV). Response Y, varied from 53 to 90% and response Y2 ranged from 29 to 78% indicating the effect of formulation variables. The obtained outcomes were analyzed by second order polynomial equation and suggested quadratic model was also validated. SLMs released Iva from 54 to 90% at pH 6.8 and was significantly (p 0.05) affected by BW concentration. The release mechanism followed the zero order and Korsmeyer-Peppas (n 0.85) kinetic models suggesting slow erosion along with diffusion mechanism for Iva release.

High-pressure phase transition in silicon carbide under shock loading using ultrafast x-ray diffraction

NASA Astrophysics Data System (ADS)

Tracy, S. J.; Smith, R. F.; Wicks, J. K.; Fratanduono, D. E.; Gleason, A. E.; Bolme, C.; Speziale, S.; Appel, K.; Prakapenka, V. B.; Fernandez Panella, A.; Lee, H. J.; MacKinnon, A.; Eggert, J.; Duffy, T. S.

2017-12-01

The behavior of silicon carbide (SiC) under shock loading was investigated through a series of time-resolved pump-probe x-ray diffraction (XRD) measurements. SiC is found at impact sites and has been put forward as a possible constituent in the proposed class of extra-solar planets known as carbon planets. Previous studies have used wave profile measurements to identify a phase transition under shock loading near 1 Mbar, but crystal structure information was not obtained. We have carried out an in situ XRD study of shock-compressed SiC using the Matter in Extreme Conditions instrument of the Linac Coherent Light Source. The femtosecond time resolution of the x-ray free electron laser allows for the determination of time-dependent atomic arrangements during shock loading and release. Two high-powered lasers were used to generate ablation-driven compression waves in the samples. Time scans were performed using the same drive conditions and nominally identical targets. For each shot in a scan, XRD data was collected at a different probe time after the shock had entered the SiC. Probe times extended up to 40 ns after release. Scans were carried out for peak pressures of 120 and 185 GPa. Our results demonstrate that SiC transforms directly from the ambient tetrahedrally-coordinated phase to the octahedral B1 structure on the nanosecond timescale of laser-drive experiments and reverts to the tetrahedrally coordinated ambient phase within nanoseconds of release. The data collected at 120 GPa exhibit diffraction peaks from both compressed ambient phase and transformed B1 phase, while the data at 185 GPa show a complete transformation to the B1 phase. Densities determined from XRD peaks are in agreement with an extrapolation of previous continuum data as well as theoretical predictions. Additionally, a high degree of texture was retained in both the high-pressure phase as well as on back transformation. Two-dimensional fits to the XRD data reveal details of the orientational relationships between the low- and high-pressure phases that can be interpreted to provide information about transformation pathways between tetrahedral and octahedral coordination structures. We acknowledge support for this work from SLAC National Accelerator Laboratory, Lawrence Livermore National Laboratory, and Los Alamos National Laboratory.

Microwave assisted scalable synthesis of titanium ferrite nanomaterials

NASA Astrophysics Data System (ADS)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.

Two-dimensional X-ray diffraction and transmission electron microscopy study on the effect of magnetron sputtering atmosphere on GaN/SiC interface and gallium nitride thin film crystal structure

NASA Astrophysics Data System (ADS)

Shen, Huaxiang; Zhu, Guo-Zhen; Botton, Gianluigi A.; Kitai, Adrian

2015-03-01

The growth mechanisms of high quality GaN thin films on 6H-SiC by sputtering were investigated by X-ray diffraction (XRD) and scanning transmission electron microscopy (STEM). The XRD θ-2θ scans show that high quality ( 0002 ) oriented GaN was deposited on 6H-SiC by reactive magnetron sputtering. Pole figures obtained by 2D-XRD clarify that GaN thin films are dominated by ( 0002 ) oriented wurtzite GaN and { 111 } oriented zinc-blende GaN. A thin amorphous silicon oxide layer on SiC surfaces observed by STEM plays a critical role in terms of the orientation information transfer from the substrate to the GaN epilayer. The addition of H2 into Ar and/or N2 during sputtering can reduce the thickness of the amorphous layer. Moreover, adding 5% H2 into Ar can facilitate a phase transformation from amorphous to crystalline in the silicon oxide layer and eliminate the unwanted { 3 3 ¯ 02 } orientation in the GaN thin film. Fiber texture GaN thin films can be grown by adding 10% H2 into N2 due to the complex reaction between H2 and N2.

X-ray diffraction investigation of amorphous calcium phosphate and hydroxyapatite under ultra-high hydrostatic pressure

NASA Astrophysics Data System (ADS)

Lam, Elisa; Gu, Qinfen; Swedlund, Peter J.; Marchesseau, Sylvie; Hemar, Yacine

2015-11-01

The changes in the crystal structures of synthetically prepared amorphous calcium phosphate (ACP) and hydroxyapatite (HAP) in water (1:1 mass ratio) were studied by synchrotron X-ray diffraction (XRD) under ultra-high hydrostatic pressures as high as 2.34 GPa for ACP and 4 GPa for HAP. At ambient pressure, the XRD patterns of the ACP and HAP samples in capillary tubes and their environmental scanning electron micrographs indicated amorphous and crystalline characteristics for ACP and HAP, respectively. At pressures greater than 0.25 GPa, an additional broad peak was observed in the XRD pattern of the ACP phase, indicating a partial phase transition from an amorphous phase to a new high-pressure amorphous phase. The peak areas and positions of the ACP phase, as obtained through fitting of the experimental data, indicated that the ACP exhibited increased pseudo-crystalline behavior at pressures greater than 0.96 GPa. Conversely, no structural changes were observed for the HAP phase up to the highest applied pressure of 4 GPa. For HAP, a unit-cell reduction during compression was evidenced by a reduction in both refined lattice parameters a and c. Both ACP and HAP reverted to their original structures when the pressure was fully released to ambient pressure.

Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

PubMed

Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

2010-04-01

Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

The Influence of Growth Temperature on Sb Incorporation in InAsSb, and the Temperature-dependent Impact of Bi Surfactants

DTIC Science & Technology

2014-01-01

resolution X - ray diffraction (XRD) were collected for all samples, and reciprocal space maps (RSMs) were collected from selected samples. The complete data...exposure. The lines represent the model fit. 19 13 Figure 1. Triple axis x - ray diffraction from the bi-layered InAsSb structures grown on GaSb at...Applied Physics, Structural properties of bismuth‐bearing semiconductor alloys, 63 (1988) 107. 18 12 Figure Captions Figure 1. Triple axis x - ray

Effects of Peripheral Architecture on the Properties of Aryl Polyhedral Oligomeric Silsesquioxanes

DTIC Science & Technology

2012-07-26

POSS) molecules are described. These POSS materials were synthesized in our laboratory and characterized by single-crystal and powder X - ray diffraction ...powder X - ray diffraction (XRD), where applicable. 1H, 13C, and 29Si NMR spectra were obtained on Bruker 300 and 400 MHz spectrometers using 5 mm o.d...degree of cage ordering during precipitation. Referring back to Figure 14, strong X - ray scattering peaks in the spectra for 1 in the d- spacing range

Structural and spectroscopic study of mechanically synthesized SnO2 nanostructures

NASA Astrophysics Data System (ADS)

Vij, Ankush; Kumar, Ravi

2016-05-01

We report the single step synthesis of SnO2 nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO2 nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A1g Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Analysis of x-ray diffraction pattern and complex plane impedance plot of polypyrrole/titanium dioxide nanocomposite: A simulation study

NASA Astrophysics Data System (ADS)

Ravikiran, Y. T.; Vijaya Kumari, S. C.

2013-06-01

To innovate the properties of Polypyrrole/Titanium dioxide (PPy/TiO2) nanocomposite further, it has been synthesized by chemical polymerization technique. The nanostructure and monoclinic phase of the prepared composite have been confirmed by simulating the X-ray diffraction pattern (XRD). Also, complex plane impedance plot of the composite has been simulated to find equivalent resistance capacitance circuit (RC circuit) and numerical values of R and C have been predicted.

[Study on bamboo treated with gamma rays by X-ray diffraction].

PubMed

Sun, Feng-Bo; Fei, Ben-Hua; Jiang, Ze-Hui; Yu, Zi-Xuan; Tian, Gen-Lin; Yang, Quan-Wen

2011-06-01

The microfibril angle and crystallinity of bamboo treated with gamma rays were tested by X-ray diffraction (XRD). The result indicated that crystallinity in bamboo increased when irradiation dose was less than 100 kGy, while the irradiation dose was raised to about 100 kGy, crystallinity in bamboo reduced. But during the whole irradiation process, the influence on microfibril angle was not obvious, so it was not the dominant factors on variation in physical-mechanical properties of bamboo during the process of irradiation.

Semi-insulating GaN Substrates for High-frequency Device Fabrication

DTIC Science & Technology

2008-06-18

of the undoped and iron-doped samples were probed by X-ray diffraction (XRD) measurements using a Philips X’pert MRD triple axis diffracted beam system...diode laser. The light emitted by the samples was dispersed by a Princeton/Acton Trivista 557 triple spectrometer fit with an LN2 cool OMA V InGaAs... point out that the relative intensity of all these bands decreases with increasing of the iron doping. This observation is consistent with the change in

Applications of High Throughput (Combinatorial) Methodologies to Electronic, Magnetic, Optical, and Energy-Related Materials

DTIC Science & Technology

2013-06-17

of the films without having to fabricate capacitors. In addition, the use of X - ray diffraction (XRD) analysis enabled Chikyow et al.40 to identify an...effects of Al doping and annealing on the thermal stabil- ity of the Y2O3/Si gate stack were studied by X - ray photoemission spectroscopy (XPS) and X - ray ...the major diffraction features in the phase distribution. For a given structural phase, the X - ray peak intensity allows one to track the compositional

Hydrothermal synthesis of tungsten doped tin dioxide nanocrystals

NASA Astrophysics Data System (ADS)

Zhou, Cailong; Li, Yufeng; Chen, Yiwen; Lin, Jing

2018-01-01

Tungsten doped tin dioxide (WTO) nanocrystals were synthesized through a one-step hydrothermal method. The structure, composition and morphology of WTO nanocrystals were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, UV-vis diffuse reflectance spectra, zeta potential analysis and high-resolution transmission electron microscopy. Results show that the as-prepared WTO nanocrystals were rutile-type structure with the size near 13 nm. Compared with the undoped tin dioxide nanocrystals, the WTO nanocrystals possessed better dispersity in ethanol phase and formed transparent sol.

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

Phosphate Remediation and Recovery using Iron Oxide-based Adsorbents

EPA Science Inventory

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

Effects of Plastizers on the Structure and Properties of Starch-Clay Nanocomposites

USDA-ARS?s Scientific Manuscript database

Biodegradable nanocomposites were successfully fabricated from corn starch and montmorillonite (MMT) nanoclays by melt extrusion processing. The structure and morphology of the nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and film propertie...

Preparation and In Vitro/Ex Vivo Evaluation of Moxifloxacin-Loaded PLGA Nanosuspensions for Ophthalmic Application.

PubMed

Mudgil, Meetali; Pawar, Pravin K

2013-01-01

The aim of the present investigation was to prepare a colloidal ophthalmic formulation to improve the residence time of moxifloxacin. Moxifloxacin-loaded poly(dl-lactide-co-glycolide) (PLGA) nanosuspensions were prepared by using the solvent evaporation technique. The nanosuspensions were characterised physically by using different techniques like particle size, zeta potential, FTIR, DSC, and XRD analysis. In vitro and ex vivo studies of nanosuspensions were carried out using a modified USP dissolution apparatus and all-glass Franz diffusion cells, respectively. The antibacterial activities of the nanosuspension and marketed formulations were performed against S. aureus and P. aeroginosa. The moxifloxacin-loaded PLGA nanosuspensions showed uniform particle size, ranging between 164-490 nm with negative zeta potential for all batches. The percentage entrapment efficiency of the drug-loaded nano-suspension was found to be between 84.09 to 92.05%. In vitro drug release studies suggest that all of the formulations showed extended drug release profiles and follow Korsemeyer-Peppas release kinetics. In vitro corneal permeability was found to be comparable with that of the marketed formulation across isolated goat cornea, indicating the suitability of the nanosuspension formulation in the ophthalmic delivery of moxifloxacin. The optimised nano-suspension was found to be more active against S. aureus and P. aeruginosa compared to the marketed eye drops.

Evolved Gas Analysis and X-Ray Diffraction of Carbonate Samples from the 2009 Arctic Mars Analog Svalbard Expedition: Implications for Mineralogical Inferences from the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

McAdam, A. C.; Mahaffy, P. R.; Blake, D. F.; Ming, D. W.; Franz, H. B.; Eigenbrode, J. L.; Steele, A.

2010-01-01

The 2009 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return (MSR). AMASE-related research comprises both analyses conducted during the expedition and further analyses of collected samples using laboratory facilities at a variety of institutions. The Sample Analysis at Mars (SAM) instrument suite, which will be part of the Analytical Laboratory on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS). An Evolved Gas Analysis Mass Spectrometer (EGA-MS) was used during AMASE to represent part of the capabilities of SAM. The other instrument included in the MSL Analytical Laboratory is CheMin, which uses X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during the AMASE 2009. Here, we discuss the preliminary interpretation of EGA and XRD analyses of selected AMASE carbonate samples and implications for mineralogical interpretations from MSL. Though CheMin will be the primary mineralogical tool on MSL, SAM EGA could be used to support XRD identifications or indicate the presence of volatile-bearing minerals which may be near or below XRD detection limits. Data collected with instruments in the field and in comparable laboratory setups (e.g., the SAM breadboard) will be discussed.

X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Kim, Hyun Jung (Inventor); Skuza, Jonathan R. (Inventor); Lee, Kunik (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor)

2017-01-01

An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

Structural analysis of the industrial grade calcite

NASA Astrophysics Data System (ADS)

Shah, Rajiv P.; Raval, Kamlesh G.

2017-05-01

The chemical, optical and structural characterization of the industrial grade Calcite by EDAX, FT-IR and XRD. EDAX is a widely used technique to analyze the chemical components in a material, FT-IR stands for Fourier Transform Infra-Red, the preferred method of infrared spectroscopy. The resultant spectrum represents the molecular absorption and transmission, creating a molecular fingerprint of the sample, The atomic planes of a crystal cause an incident beam of X-rays to interfere with one another as they leave the crystal. The phenomenon is called X ray diffraction.(XRD). Data analysis of EDAX, FT-IR and XRD has been carried out with help of various instruments and software and find out the results of the these industrial grade materials which are mostly used in ceramics industries

MnFe2O4/CdSe magneto-fluorescent nanocomposite for possible biomedical applications

NASA Astrophysics Data System (ADS)

Chandunika, R. K.; Vijayaraghavan, R.; Sahu, Niroj Kumar

2018-04-01

Acombined superparamagnetic and fluorescent MnFe2O4/CdSe multifunctional nanocompositehas been prepared by suitable surface functionalizationswith citric acid, polyethyleneimine(PEI) and thioglycolic acid (ThA).and the samples were characterized by XRD, FT-IR, TEM, Zeta Potential, VSM, UV-Vis and PL spectroscopy. MnFe2O4 crystalizes with average size of 38.6 nm whereas CdSe with average size of 2.03 nm. In composite, the CdSe quantum dots (QD) are homogeneously distributed in the matrix of porous MnFe2O4 nanoparticles. Thenanocomposites are well dispersed in aqueous solvent and possess significant magnetic and luminescence properties which may be utilised for magnetic resonance imaging and luminescence tagging of biomolecules.

Synthesis and characterization of nanomagnetite particles and their polymer coated forms.

PubMed

Utkan, Guldem Guven; Sayar, Filiz; Batat, Pinar; Ide, Semra; Kriechbaum, Manfred; Pişkin, Erhan

2011-01-15

Superparamagnetic nanoparticles were prepared by coprecipitation of ferrous (Fe(2+)) and ferric (Fe(3+)) aqueous solution by a base. Nanomagnetite particles were coated with poly(St/PEG-EEM/DMAPM) and poly(St/PEG-MA/DMAPM) layer by emulsifier-free emulsion polymerization. Chemical structure of nanoparticles was characterized by both FTIR and (1)H NMR. Particle morphologies were determined by Zeta Sizer, DLS, XRD and SAXS. Structural analysis showed that after polymer coating nanomagnetite particles kept their superparamagnetic property. Besides the synthesized magnetites, polymer coated forms of these particles are more biocompatible, well dispersable and uniform. These properties make them a very strong candidate for bioengineering applications, such as bioseparation, gene transfer. Copyright © 2010 Elsevier Inc. All rights reserved.

Halloysite clay nanotubes for controlled release of protective agents.

PubMed

Abdullayev, Elshad; Lvov, Yuri

2011-11-01

Halloysite is a naturally occurring clay mineral with submicron sized hollow cylindrical morphology. Halloysite morphology, structure and properties were characterized by using SEM, TEM, XRD, FT-IR spectroscopy, surface electrokinetic (zeta) potential and nitrogen adsorption isotherms. Comparison of the halloysite structure with imogolite was also provided. Halloysite toxicological studies revealed that it is environmentally friendly and biocompatible material. Due to its unique tubular shape and availability in thousands of tons halloysite has potential to be applied as nanocontainers for encapsulation of chemically and biologically active agents such as medicines, pharmaceuticals, antiseptics, corrosion inhibitors, antifouling agents, and doped with them plastics producing smart polymeric nanocomposites with improved mechanical strength. Finally possibility to synthesize metal nanorods within the halloysite lumen was demonstrated.

XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less

Use of X-ray diffraction to quantify amorphous supplementary cementitious materials in anhydrous and hydrated blended cements

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

Snellings, R., E-mail: ruben.snellings@epfl.ch; Salze, A.; Scrivener, K.L., E-mail: karen.scrivener@epfl.ch

2014-10-15

The content of individual amorphous supplementary cementitious materials (SCMs) in anhydrous and hydrated blended cements was quantified by the PONKCS [1] X-ray diffraction (XRD) method. The analytical precision and accuracy of the method were assessed through comparison to a series of mixes of known phase composition and of increasing complexity. A 2σ precision smaller than 2–3 wt.% and an accuracy better than 2 wt.% were achieved for SCMs in mixes with quartz, anhydrous Portland cement, and hydrated Portland cement. The extent of reaction of SCMs in hydrating binders measured by XRD was 1) internally consistent as confirmed through the standardmore » addition method and 2) showed a linear correlation to the cumulative heat release as measured independently by isothermal conduction calorimetry. The advantages, limitations and applicability of the method are discussed with reference to existing methods that measure the degree of reaction of SCMs in blended cements.« less

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali silica reaction in concrete structures

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

Dähn, R.; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This particular high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating themore » sample. Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. Furthermore, it is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali–silica reaction in concrete structures

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

Dähn, R., E-mail: rainer.daehn@psi.ch; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating the sample.more » Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. It is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Enhanced model for determining the number of graphene layers and their distribution from X-ray diffraction data

PubMed Central

Ademi, Abdulakim; Grozdanov, Anita; Paunović, Perica; Dimitrov, Aleksandar T

2015-01-01

Summary A model consisting of an equation that includes graphene thickness distribution is used to calculate theoretical 002 X-ray diffraction (XRD) peak intensities. An analysis was performed upon graphene samples produced by two different electrochemical procedures: electrolysis in aqueous electrolyte and electrolysis in molten salts, both using a nonstationary current regime. Herein, the model is enhanced by a partitioning of the corresponding 2θ interval, resulting in significantly improved accuracy of the results. The model curves obtained exhibit excellent fitting to the XRD intensities curves of the studied graphene samples. The employed equation parameters make it possible to calculate the j-layer graphene region coverage of the graphene samples, and hence the number of graphene layers. The results of the thorough analysis are in agreement with the calculated number of graphene layers from Raman spectra C-peak position values and indicate that the graphene samples studied are few-layered. PMID:26665083

STM-electroluminescence from clustered C3N4 nanodomains synthesized via green chemistry process.

PubMed

Andrade, E P; Costa, B B A; Chaves, C R; de Paula, A M; Cury, L A; Malachias, A; Safar, G A M

2018-01-01

A Scanning Tunneling Microscopy/Spectroscopy (STM/STS) and synchrotron X-ray diffraction study on clustered C 3 N 4 nanoparticles (nanoflakes) is conducted on green-chemistry synthesized samples obtained from chitosan through high power sonication. Morphological aspects and the electronic characteristics are investigated. The observed bandgap of the nanoflakes reveals the presence of different phases in the material. Combining STM morphology, STS spectra and X-ray diffraction (XRD) results one finds that the most abundant phase is graphitic C 3 N 4 . A high density of defects is inferred from the XRD measurements. Additionally, STM-electroluminescence (STMEL) is detected in C 3 N 4 nanoflakes deposited on a gold substrate. The tunneling current creates photons that are three times more energetic than the tunneling electrons of the STM sample. We ponder about the two most probable models to explain the observed photon emission energy: either a nonlinear optical phenomenon or a localized state emission. Copyright © 2017 Elsevier B.V. All rights reserved.

Characterization of food additive-potato starch complexes by FTIR and X-ray diffraction.

PubMed

Dankar, Iman; Haddarah, Amira; Omar, Fawaz E L; Pujolà, Montserrat; Sepulcre, Francesc

2018-09-15

Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) techniques were used to study the effect of four food additives, agar, alginate, lecithin and glycerol, at three different concentrations, 0.5, 1 and 1.5%, on the molecular structure of potato puree prepared from commercial potato powder. Vibrational spectra revealed that the amylose-amylopectin skeleton present in the raw potato starch was missing in the potato powder but could be fully recovered upon water addition when the potato puree was prepared. FTIR peaks corresponding to water were clearly present in the potato powder, indicating the important structural role of water molecules in the recovery of the initial molecular conformation. None of the studied puree samples presented a crystalline structure or strong internal order. A comparison of the FTIR and XRD results revealed that the additives exerted some effects, mainly on the long-range order of the starch structure via interacting with and changing -OH and hydrogen bond interactions. Copyright © 2018 Elsevier Ltd. All rights reserved.

Structural and Electronic Properties Study of Colombian Aurifer Soils by Mössbauer Spectroscopy and X-ray Diffraction

NASA Astrophysics Data System (ADS)

Bustos Rodríguez, H.; Rojas Martínez, Y.; Oyola Lozano, D.; Pérez Alcázar, G. A.; Fajardo, M.; Mojica, J.; Molano, Y. J. C.

2005-02-01

In this work a study on gold mineral samples is reported, using optical microscopy, X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The auriferous samples are from the El Diamante mine, located in Guachavez-Nariño (Colombia) and were prepared by means of polished thin sections. The petrography analysis registered the presence, in different percentages that depend on the sample, of pyrite, quartz, arsenopyirite, sphalerite, chalcopyrite and galena. The XRD analysis confirmed these findings through the calculated cell parameters. One typical Rietveld analysis showed the following weight percent of phases: 85.0% quartz, 14.5% pyrite and 0.5% sphalerite. In this sample, MS demonstrated the presence of two types of pyrite whose hyperfine parameters are δ 1 = 0.280 ± 0.002 mm/s and Δ 1 = 0.642 ± 0.002 mm/s, δ 2 = 0.379 ± 0.002 mm/s and Δ 2 = 0.613 ± 0.002 mm/s.

Structural and morphological study on ZnO:Al thin films grown using DC magnetron sputtering

NASA Astrophysics Data System (ADS)

Astuti, B.; Sugianto; Mahmudah, S. N.; Zannah, R.; Putra, N. M. D.; Marwoto, P.; Aryanto, D.; Wibowo, E.

2018-03-01

ZnO doped Al (ZnO:Al ) thin film was deposited on corning glass substrate using DC magnetron sputtering method. Depositon process of the ZnO:Al thin films was kept constant at plasma power, deposition temperature and deposition time are 40 watt, 400°C and 2 hours, respectivelly. Furthermore, for annealing process has been done on the variation of oxygen pressure are 0, 50, and 100 mTorr. X-ray diffraction (XRD), and SEM was used to characterize ZnO:Al thin film was obtained. Based on XRD characterization results of the ZnO:Al thin film shows that deposited thin film has a hexagonal structure with the dominant diffraction peak at according to the orientation of the (002) plane and (101). Finally, the crystal structure of the ZnO:Al thin films that improves with an increasing the oxygen pressure at annealing process up to 100 mTorr and its revealed by narrow FWHM value and also with dense crystal structure.

Facile synthesis of Co3O4 hexagonal plates by flux method

NASA Astrophysics Data System (ADS)

Han, Ji-Long; Meng, Qing-Fen; Gao, Sheng-Li

2018-01-01

Using a novel flux method, a hexagonal plate of Co3O4 was directly synthesized. In this method, CoCl2·6H2O, NaOH, and the cosolvent H3BO3 were heated to 750 °C for 2 h in a corundum crucible. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscope (HRTEM). Furthermore, XRD studies indicated that the product consisted of a cubic phase of Co3O4, and the phase existed in a completely crystalline form. Then, SEM results indicated that these hexagonal plates tiered up and they had diameters in the range of 2-10 μm. According to the results of SAED and HRTEM analyses, the interlayer spacing was about 0.24 nm, which corresponds to the interlayer distance of (3 1 1) crystal plane of cubic Co3O4.

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.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

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.

Matching 4.7-Å XRD Spacing in Amelogenin Nanoribbons and Enamel Matrix

PubMed Central

Sanii, B.; Martinez-Avila, O.; Simpliciano, C.; Zuckermann, R.N.; Habelitz, S.

2014-01-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

PubMed

Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

2014-04-23

In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

Sol-gel derived silica/chitosan/Fe3O4 nanocomposite for direct electrochemistry and hydrogen peroxide biosensing

NASA Astrophysics Data System (ADS)

Satvekar, R. K.; Rohiwal, S. S.; Tiwari, A. P.; Raut, A. V.; Tiwale, B. M.; Pawar, S. H.

2015-01-01

A novel strategy to fabricate hydrogen peroxide third generation biosensor has been developed from sol-gel of silica/chitosan (SC) organic-inorganic hybrid material assimilated with iron oxide magnetic nanoparticles (Fe3O4). The large surface area of Fe3O4 and porous morphology of the SC composite facilitates a high loading of horseradish peroxidase (HRP). Moreover, the entrapped enzyme preserves its conformation and biofunctionality. The fabrication of hydrogen peroxide biosensor has been carried out by drop casting of the SC/F/HRP nanocomposite on glassy carbon electrode (GCE) for study of direct electrochemistry. The x-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) confirms the phase purity and particle size of as-synthesized Fe3O4 nanoparticles, respectively. The nanocomposite was characterized by UV-vis spectroscopy, fluorescence spectroscopy and Fourier transform infrared (FTIR) for the characteristic structure and conformation of enzyme. The surface topographies of the nanocomposite thin films were investigated by scanning electron microscopy (SEM). Dynamic light scattering (DLS) was used to determine the particle size distribution. The electrostatic interactions of the SC composite with Fe3O4 nanoparticles were studied by the zeta potential measurement. Electrochemical impedance spectroscopy (EIS) of the SC/F/HRP/GCE electrode displays Fe3O4 nanoparticles as an excellent candidate for electron transfer. The SC/F/HRP/GCE exhibited a pair of well-defined quasi reversible cyclic voltammetry peaks due to the redox couple of HRP-heme Fe (III)/Fe (II) in pH 7.0 potassium phosphate buffer. The biosensor was employed to detect H2O2 with linear range of 5 μM to 40 μM and detection limit of 5 μM. The sensor displays excellent selectivity, sensitivity, good reproducibility and long term stability.

Bio-synthesis of silver nanoparticles using Potentilla fulgens Wall. ex Hook. and its therapeutic evaluation as anticancer and antimicrobial agent.

PubMed

Mittal, Amit Kumar; Tripathy, Debabrata; Choudhary, Alka; Aili, Pavan Kumar; Chatterjee, Anupam; Singh, Inder Pal; Banerjee, Uttam Chand

2015-08-01

The present study aims to develop an easy and eco-friendly method for the synthesis of silver nanoparticles using extracts from the medicinal plant, Potentilla fulgens and evaluation of its anticancer and antimicrobial properties. The various parts of P. fulgens were screened and the root extract was found to have the highest potential for the synthesis of nanoparticles. The root extracts were able to quickly reduce Ag(+) to Ag(0) and stabilized the nanoparticles. The synthesis of nanoparticles was confirmed by UV-Visible spectrophotometry and further characterized using Zeta sizer, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD). Electron microscopic study showed that the size of the nanoparticle was in the range of 10 to 15 nm and spherical in shape. The studies of phytochemical analysis of nanoparticles indicated that the adsorbed components on the surface of nanoparticles were mainly flavonoid in nature. Furthermore, nanoparticles were evaluated as cytotoxic against various cancer cell lines and 0.2 to 12 μg/mL nanoparticles showed good toxicity. The IC50 value of nanoparticles was found to be 4.91 and 8.23 μg/mL against MCF-7 and U-87 cell lines, respectively. Additionally, the apoptotic effect of synthesized nanoparticles on normal and cancer cells was studied using trypan blue assay and flow-cytometric analysis. The results indicate the synthesized nanoparticle ability to kill cancer cells compared to normal cells. The nanoparticles also exhibited comparable antimicrobial activity against both Gram-positive and Gram-negative bacteria. Copyright © 2015 Elsevier B.V. All rights reserved.

A novel antimicrobial therapy for the control of Aeromonas hydrophila infection in aquaculture using marine polysaccharide coated gold nanoparticle.

PubMed

Vijayakumar, Sekar; Vaseeharan, Baskaralingam; Malaikozhundan, Balasubramanian; Gobi, Narayanan; Ravichandran, Samuthirapandian; Karthi, Sellamuthu; Ashokkumar, Balasubramaniem; Sivakumar, Natesan

2017-09-01

In the present study, we prepared fucoidan coated Au-NPs (Fu-AuNPs), and examined its antimicrobial activity against Aeromonas hydrophila. The green synthesized Fu-AuNPs were bio-physically characterized by Ultraviolet-visible (UV-Vis) spectroscopy, X-ray Diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Higher Transmission Electron Microscopy (HR-TEM), Zeta potential analysis and Energy Dispersive X-ray spectroscopy (EDX). Fu-AuNPs were crystalline in nature, spherical to triangular in shape, with particle size ranging within 10-100 nm. The synthesized Fu-AuNPs at 100 μg mL -1 showed inhibition zone against A. hydrophila (23.2 mm) which is much higher than that of commercial antibiotic chloramphenicol (17.3 mm). The biofilm inhibitory activity of Fu-AuNPs against Gram negative (Aeromonas hydrophila) was higher. Light and confocal laser scanning microscopic observations showed that the Fu-AuNPs at 100 μg mL -1 inhibited the biofilm of A. hydrophila. The cytotoxicity study indicated that Fu-AuNPs were effective in inhibiting the viability of human cervical cancer cells (HeLa) at 100 μg mL -1 . In another experiment, the antibacterial effect of Fu-AuNPs on tilapia, Oreochromis mossambicus were evaluated in vivo. The mortality rate of O. mossambicus infected by A. hydrophila was much higher (90%), whereas, the mortality of O. mossambicus that received Fu-AuNPs followed by challenge with A. hydrophia was reduced to 30%. This study concludes that Fu-AUNPs are effective in the control of A. hydrophila infections in O. mossambicus. Copyright © 2017 Elsevier Ltd. All rights reserved.

A novel polymeric ionic liquid-coated magnetic multiwalled carbon nanotubes for the solid-phase extraction of Cu, Zn-superoxide dismutase.

PubMed

Wen, Qian; Wang, Yuzhi; Xu, Kaijia; Li, Na; Zhang, Hongmei; Yang, Qin

2016-10-05

A novel magnetic adsorbent, benzyl groups functionalized imidazolium-based polymeric ionic liquid (PIL)-coated magnetic multiwalled carbon nanotubes (MWCNTs) (m-MWCNTs@PIL), has been successfully synthesized and applied for the extraction of Cu, Zn-superoxide dismutase (Cu, Zn-SOD). The m-MWCNTs@PIL were characterized by X-ray diffraction (XRD), Fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), vibrating sample magnetometer (VSM) and zeta-potential nanoparticles. In this method, the m-MWCNTs@PIL could interact with Cu, Zn-SOD through hydrogen bonding, π-π and electrostatic interactions. The extraction performance of the m-MWCNTs@PIL in the magnetic solid-phase extraction (MSPE) procedure was investigated, coupled with the determination by UV-vis spectrophotometer. Compared with m-MWCNTs@IL and m-MWCNTs, the m-MWCNTs@PIL exhibited the highest extraction capacity of 29.1 mg/g for Cu, Zn-SOD. The adsorbed Cu, Zn-SOD remained high specific activity after being eluted from m-MWCNTs@PIL by 1 moL/L NaCl solution. Besides, the m-MWCNTs@PIL could be easily recycled and successfully employed in the extraction of Cu, Zn-SOD from real samples. Under the optimal conditions, the precision, repeatability and stability of the proposed method were investigated and the RSDs were 0.29%, 1.68% and 0.54%, respectively. Recoveries were in the range of 82.7-102.3%, with the RSD between 3.47% and 5.35%. On the basis of these results, the developed method has great potential in the extraction of Cu, Zn-SOD or other analytes from biological samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of ionic liquid modified magnetic metal-organic frameworks composites for the solid-phase extraction of α-chymotrypsin.

PubMed

Wei, Xiaoxiao; Wang, Yuzhi; Chen, Jing; Xu, Panli; Zhou, Yigang

2018-05-15

A novel magnetic solid-phase extraction (MSPE) method based on 1-hexyl-3-methyl imidazolium chloride ionic liquid (IL) modified magnetic Fe 3 O 4 nanoparticles, hydroxylated multiwall carbon nanotubes (MWCNTs-OH) and zeolitic imidazolate frameworks (ZIFs) nanocomposites (Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL) were proposed and applied to extract α-chymotrypsin. The magnetic materials were synthesized successfully and characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), thermal gravimetric analysis (TGA), fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometer (VSM) and zeta potentials. Subsequently, the UV-vis spectrophotometer at about 280 nm was utilized to quantitatively analyze the α-chymotrypsin concentration in the supernatant. Furthermore, single factor experiments revealed that the extraction capacity was influenced by initial α-chymotrypsin concentration, ionic strength, extraction time, extraction temperature and pH value. The extraction capacity could reach up to about 635 mg g -1 under the optimized conditions, absolutely higher than that of extraction for Ovalbumin (OVA), Bovine serum albumin (BSA) and Bovine hemoglobin (BHb). In addition, the regeneration studies showed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL particles could be reused several times and kept a high extraction capacity. Besides, the study of enzymatic activity also indicated that the activity of the extracted α-chymotrypsin was well maintained 93% of initial activity. What's more, the proposed method was successfully applied to extract α-chymotrypsin in porcine pancreas crude extract with satisfactory results. All of above conclusions highlight the great potential of the proposed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL-MSPE method in the analysis of biomolecules. Copyright © 2018 Elsevier B.V. All rights reserved.

A novel dianionic amino acid ionic liquid-coated PEG 4000 modified Fe3O4 nanocomposite for the magnetic solid-phase extraction of trypsin.

PubMed

Yang, Qin; Wang, Yuzhi; Zhang, Hongmei; Xu, Kaijia; Wei, Xiaoxiao; Xu, Panli; Zhou, Yigang

2017-11-01

A novel magnetic extractant, PEG 4000 modified Fe 3 O 4 nanomaterial that coated with dianionic amino acid ionic liquid (Fe 3 O 4 @PEG@DAAAIL), was successfully synthesized and characterized. X-ray diffraction (XRD), transmission electron microscope (TEM), vibrating sample magnetometer (VSM), fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA) and zeta potentials were used to confirm that the novel nanocomposite was successfully synthesized. Subsequently, the prepared Fe 3 O 4 @PEG@DAAAIL nanocomposite was used as the extractant for trypsin coupled with magnetic solid-phase extraction (MSPE). The concentrations of trypsin in the supernatant were detected by UV-vis spectrophotometer at 278nm. The extraction ability turned out to be better than the other four kinds of extractants prepared in this work. Furthermore, the influence of a series of factors, such as extraction time and temperature, initial trypsin concentration, the value of pH and ionic strength, was systematically investigated. Under the optimal extraction condition, the extraction capacity for trypsin could reach up to 718.73mg/g, absolutely higher than that of other adsorbents reported. This satisfactory extraction capacity could be maintained unchangeable after at least eight days, and kept over 90% of initial extraction capacity after eight recycles. What's more, the activity of trypsin after extraction retained 92.29% of initial activity, verifying the biocompatibility of the prepared extractant. Finally, the developed Fe 3 O 4 @PEG@DAAAIL-MSPE method was successfully applied to the real sample analysis with satisfactory results. All of above proves the potential value of Fe 3 O 4 @PEG@DAAAIL-MSPE in the analysis of biomass. Copyright © 2017 Elsevier B.V. All rights reserved.

Development and statistical optimization of nefopam hydrochloride loaded nanospheres for neuropathic pain using Box-Behnken design.

PubMed

Sukhbir, S; Yashpal, S; Sandeep, A

2016-09-01

Nefopam hydrochloride (NFH) is a non-opioid centrally acting analgesic drug used to treat chronic condition such as neuropathic pain. In current research, sustained release nefopam hydrochloride loaded nanospheres (NFH-NS) were auspiciously synthesized using binary mixture of eudragit RL 100 and RS 100 with sorbitan monooleate as surfactant by quasi solvent diffusion technique and optimized by 3 5 Box-Behnken designs to evaluate the effects of process and formulation variables. Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetric (DSC) and X-ray diffraction (XRD) affirmed absence of drug-polymer incompatibility and confirmed formation of nanospheres. Desirability function scrutinized by design-expert software for optimized formulation was 0.920. Optimized batch of NFH-NS had mean particle size 328.36 nm ± 2.23, % entrapment efficiency (% EE) 84.97 ± 1.23, % process yield 83.60 ± 1.31 and % drug loading (% DL) 21.41 ± 0.89. Dynamic light scattering (DLS), zeta potential analysis and scanning electron microscopy (SEM) validated size, charge and shape of nanospheres, respectively. In-vitro drug release study revealed biphasic release pattern from optimized nanospheres. Korsmeyer Peppas found excellent kinetics model with release exponent less than 0.45. Chronic constricted injury (CCI) model of optimized NFH-NS in Wistar rats produced significant difference in neuropathic pain behavior ( p  < 0.05) as compared to free NFH over 10 h indicating sustained action. Long term and accelerated stability testing of optimized NFH-NS revealed degradation rate constant 1.695 × 10 -4 and shelf-life 621 days at 25 ± 2 °C/60% ± 5% RH.

The interactions between three typical PPCPs and LDH

NASA Astrophysics Data System (ADS)

Li, Erwei; Liao, Libing; Lv, Guocheng; Li, Zhaohui; Yang, Chengxue; Lu, Yanan

2018-03-01

With a positively charged layered structure, layered double hydroxide has potential applications in remediation of anionic contaminants, which has been a hot topic for recent years. In this study, a Cl type Mg-Al hydrotalcite (Cl-LDH) was prepared by a co-precipitation method. The adsorption process of three pharmaceuticals and personal care products (PPCPs) (tetracycline (TC), diclofenac sodium (DF), chloramphenicol (CAP)) by Cl-LDH was investigated by X-ray diffraction (XRD), Zeta potential, dynamic light scattering (DLS), BET, FT-IR spectroscopy and molecular dynamics simulation. The results showed that the adsorption equilibrium of TC and DF could be reached in 120 min, and the maximum adsorption capacity of the Cl-LDH for TC and DF were 1.85 mmol/g and 0.95 mmol/g, respectively. The adsorption isothermal of TC was fitted with the Freundlich adsorption model, and the adsorption isothermal of DF was fitted with the Langmuir adsorption model. The adsorption dynamics of TC and DF followed the pseudo-second-order model. The adsorption mechanisms of the three PPCPs onto Cl-LDH were different based on the experimental results and molecular dynamics simulation. The TC adsorption on Cl-LDH was mainly driven by the electrostatic interactions between the negative charge of TC and the positive charge of Cl-LDH. The uptake of anionic DF was attributed both to ion exchange of DF for Cl- and the electrostatic interaction between the negatively charged DF and the positively charged structure layer of Cl-LDH. Cl-LDH does not adsorb the neutral CAP due to no electrostatic interaction. The molecular dynamic simulation further confirmed different configurations of the three selected PPCPs in the interlayer of Cl-LDH, which were responsible for the different uptake process of PPCPs on Cl-LDH.

Surface free energy of TiC layers deposited by electrophoretic deposition (EPD)

NASA Astrophysics Data System (ADS)

Gorji, Mohammad Reza; Sanjabi, Sohrab

2018-01-01

In this study porous structure coatings of bare TiC (i.e. 20 nm, 0.7 µm and 5/45 µm) and core-shell structures of TiC/NiP synthesized through electroless plating were deposited by EPD. Room temperature surface free energy (i.e. γs) of TiC and TiC/NiP coatings were determined via measuring contact angles of distilled water and diiodemethane liquids. The effect of Ni-P shell on spreading behavior of pure copper on porous EPD structures was also investigated by high temperature wetting experiments. According to the results existence of a Ni-P layer around the TiC particles has led to roughness (i.e. at least 0.1 µm), and porosity mean length (i.e. at least 1 µm) increase. This might be related to various sizes of TiC agglomerates formed during electroless plating. It has been observed that room temperature γs changed from 44.49 to 54.12 mJ.m-2 as a consequence of particle size enlargement for TiC. The highest and lowest (67.25 and 44.49 mJ.m-2) γs were measured for TiC nanoparticles which showed 1.5 times increase in surface free energy after being plated with Ni-P. It was also observed that plating Ni-P altered non-spreading (θs > 100 o) behavior of TiC to full-spreading ((θs 0o)) which can be useful for preparation of hard coatings by infiltration sintering phenomenon. Zeta potential of EPD suspensions, morphology, phase structure and topography of as-EPD layers were investigated through Zetasizer, field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and atomic force microscopy (AFM) instruments respectively.

Influence of montmorillonites exchange capacity on the basal spacing of cation–anion organo-montmorillonites

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

Sanqin, Wu; Zepeng, Zhang, E-mail: unite508@163.com; Yunhua, Wang

Graphical abstract: This picture shows the distribution of organic modifier (CTAB and SDS) in Mt interlayer and the basal spacing changes of Mt modified by CTAB and SDS. Organic modifier molecule in Mt interlayer is more and more orderly. The basal spacing of Mt is from 1.5 nm to 5 nm as modifier added. - Highlights: • The d{sub 001} of Ca-Mt, R-Na-Mt, Na-Mt modified by CTAB and SDS can reach 5 nm. • It is easier to get cation–anion OMt with greater d{sub 001} if CEC is lower. • The organic molecules distribution in cation–anion OMt was analyzed. •more » The influence mechanism of Ca-Mt CEC on the d{sub 001} was discussed. - Abstract: With cationic and anionic surfactants cetyltrimethylammonium bromide (CTAB) and sodium dodecylsulfonate (SDS) as modifiers, Ca-montmorillonites (Ca-Mt), artificial Na-montmorillonites (R-Na-Mt) and natural Na-montmorillonites (Na-Mt) with different cation exchange capacity (CEC) were modified by solution intercalation method, respectively. Then cation–anion organo-montmorillonites (OMt) were prepared. The influence of CEC on the basal spacing of cation–anion OMt and the influence mechanism were discussed by X-ray diffraction (XRD) and zeta potential testing. The results indicate that the basal spacing of cation–anion OMt is related to CEC. For the same type montmorillonites, the basal spacing of cation–anion OMt decreases with the increase of CEC and it is easier to get cation–anion OMt with greater basal spacing when CEC is lower. Moreover, the CEC of Na-Mt has the greatest influence on the basal spacing of cation–anion OMt.« less

Preparation, characterization and toxicology properties of α- and β-chitosan Maillard reaction products nanoparticles.

PubMed

Zhang, Hongcai; Zhang, Yiwen; Bao, Erjaing; Zhao, Yanyun

2016-08-01

In this study, β-chitosan (CS) Maillard reaction (MR) NPs was prepared to improve the water solubility of CS NPs. The α- and β-CS MR was firstly induced by high intensity ultrasound-assisted (UA) water-bath heating at 80°C for 8h. The α- and β-CS Maillard reaction products (MRPs NPs were then prepared by ionic gelation method between the positively charged primary amino groups of CS and the negatively charged groups of sodium tripolyphosphate (TPP). The α- and β-CS MRPs NPs had particle size of 42.49 and 61.74nm, and Zeta-potential of 27.43 and 35.13mV, respectively. The prepared α- and β-CS MRPs NPs was characterized by transmission electron microscope (TEM), Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and thermogravimetric analysis (TGA)-differential scanning calorimetry (DSC) to verify whether α- and β-CS MRPs has been incorporated into the CS NPs. The α- and β-CS MRPs NPs exhibited no significant difference (p>0.05) in antioxidant activity compared with α- and β-CS MRPs at the same concentration based on reducing power, DPPH radical scavenging activity, and ORAC values. The cytotoxicity test of α- and β-CS MRPs NPs showed good cell viability (70.86-99.16%) of human pulmonary microvascular endothelial cells (HLMVEC) at the concentration range from 0.12 to 1mg/mL, and fluorescein-5-isothiocyanate (FITC)-α- and β-CS MRPs NPs maintained the morphological characteristics of living cells. These results showed that α- and β-CS MRPs NPs can be used as water-soluble antioxidant substances for applications in food and other fields. Copyright © 2016. Published by Elsevier B.V.

Aripiprazole-Loaded Polymeric Micelles: Fabrication, Optimization and Evaluation using Response Surface Method.

PubMed

Patil, Payal Hasmukhlal; Wankhede, Pooja R; Mahajan, H S; Zawar, Laxmikant

2018-01-04

The fundamental objective of current study was to encapsulate Ari-piprazole (ARP) within Pluronic F127 micelles to improve its aqueous solubility. The recent patents on Ar-ipiprazole (JP2013136621) and micelles (WO2016004369A1) facilitated selection of drug and polymer. The drug-laden micelles were fabricated using thin-film hydration technique. Optimization of the micellar formulation was done by using response surface method (RSM). The Pluronic F127 concentration of 150 mg and 75 rpm rotational speed of rotary evaporator were found to be optimized conditions for formulating micelles. The prepared batches were further characterized for PDI (polydispersity index), zeta potential, % DLC (% Drug loading content), % EE (% Entrapment Efficiency) and % drug release study; results of these parameters were found to be 0.228, −4.04 mV and 76.50 % and 18.56 % respectively. It was observed from the In vitro release study that 97.37 ± 1.81 % drug had released from micelles after 20 hrs which were found about thrice as compared to that of pure drug. The optimized ARP micellar for-mulation was characterized using DSC (Differential Scanning Colorimetry), FT-IR (Fourier Trans-formed Infrared Spectroscopy), P-XRD (Powdered X-ray Diffraction Study) and TEM (Transmission Electronic Microscopy) studies. ARP-loaded micelles displayed a hydrodynamic diameter of 170.3 nm and a sphere-shaped morphology as determined by dynamic light scattering as well as TEM study. It is concluded that the prepared polymeric micellar system has an excellent potential to be used as a delivery carrier for Aripiprazole with increased solubility. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

A new magnetic nanodiamond/graphene oxide hybrid (Fe3O4@ND@GO) material for pre-concentration and sensitive determination of sildenafil in alleged herbal aphrodisiacs by HPLC-DAD system.

PubMed

Yilmaz, Erkan; Ulusoy, Halil İbrahim; Demir, Özge; Soylak, Mustafa

2018-05-01

A sensitive analytical methodology was investigated to concentrate and determine of sildenafil citrate (SLC) present at trace level in herbal supplementary products. The proposed method is based on simple and sensitive pre-concentration of SLC by using magnetic solid phase extraction with new developed magnetic nanodiamond/graphene oxide hybrid (Fe 3 O 4 @ND@GO) material as a sorbent. Experimental variables affecting the extraction efficiency of SLC like; pH, sample volume, eluent type and volume, extraction time and amount of adsorbent were studied and optimized in detail. Determination of sildenafil citrate after magnetic solid phase extraction (MSPE) was carried out by HPLC-DAD system. The morphology, composition, and properties of the synthesized hybrid material was characterized by Fourier transform infrared spectrometry (FT-IR), Raman spectrometry (Raman), X-ray diffraction spectrometry (XRD), scanning electron microscopy (SEM), mapping photographs, zeta potential analyzer, and BET surface area analysis. Under optimized conditions, linear range was ranged from 5.00 to 250.00 ng mL -1 with R 2 of 0.9952. The limit of detection (LOD) was 1.49 ng mL -1 and the recoveries at two spiked levels were ranged from 94.0 to 104.1% with the relative standard deviation (RSD) < 7.1% (n = 5). The enhancement factor (EF) was 86.9. The results show that the combination MSPE with HPLC-DAD is a suitable and sensitive method for the determination of SLC in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Swinging Symmetry, Multiple Structural Phase Transitions, and Versatile Physical Properties in RECuGa3 (RE = La-Nd, Sm-Gd).

PubMed

Subbarao, Udumula; Rayaprol, Sudhindra; Dally, Rebecca; Graf, Michael J; Peter, Sebastian C

2016-01-19

The compounds RECuGa3 (RE = La-Nd, Sm-Gd) were synthesized by various techniques. Preliminary X-ray diffraction (XRD) analyses at room temperature suggested that the compounds crystallize in the tetragonal system with either the centrosymmetric space group I4/mmm (BaAl4 type) or the non-centrosymmetric space group I4mm (BaNiSn3 type). Detailed single-crystal XRD, neutron diffraction, and synchrotron XRD studies of selected compounds confirmed the non-centrosymmetric BaNiSn3 structure type at room temperature with space group I4mm. Temperature-dependent single-crystal XRD, powder XRD, and synchrotron beamline measurements showed a structural transition between centro- and non-centrosymmetry followed by a phase transition to the Rb5Hg19 type (space group I4/m) above 400 K and another transition to the Cu3Au structure type (space group Pm3̅m) above 700 K. Combined single-crystal and synchrotron powder XRD studies of PrCuGa3 at high temperatures revealed structural transitions at higher temperatures, highlighting the closeness of the BaNiSn3 structure to other structure types not known to the RECuGa3 family. The crystal structure of RECuGa3 is composed of eight capped hexagonal prism cages [RE4Cu4Ga12] occupying one rare-earth atom in each ring, which are shared through the edge of Cu and Ga atoms along the ab plane, resulting in a three-dimensional network. Resistivity and magnetization measurements demonstrated that all of these compounds undergo magnetic ordering at temperatures between 1.8 and 80 K, apart from the Pr and La compounds: the former remains paramagnetic down to 0.3 K, while superconductivity was observed in the La compound at T = 1 K. It is not clear whether this is intrinsic or due to filamentary Ga present in the sample. The divalent nature of Eu in EuCuGa3 was confirmed by magnetization measurements and X-ray absorption near edge spectroscopy and is further supported by the crystal structure analysis.

Structural characterization of precious-mean quasiperiodic Mo/V single-crystal superlattices grown by dual-target magnetron sputtering

NASA Astrophysics Data System (ADS)

Birch, J.; Severin, M.; Wahlström, U.; Yamamoto, Y.; Radnoczi, G.; Riklund, R.; Sundgren, J.-E.; Wallenberg, L. R.

1990-05-01

A class of quasiperiodic superlattice structures, which can be generated by the concurrent inflation rule A-->AmB and B-->A (where m=positive integer), has been studied both theoretically and experimentally. Given that the ratios between the thicknesses of the two superlattice building blocks, A and B, are chosen to be γ(m)=[m+(m2+4)1/2]/2 (known as the ``precious means''), then the x-ray- and electron-diffraction peak positions are analytically found to be located at the wave vectors q=2πΛ-1r[γ(m)]k, where r and k are integers and Λ is an average superlattice wavelength. The analytically obtained results have been compared to experimental results from single-crystalline Mo/V superlattice structures, generated with m=1, 2, and 3. The superlattices were grown by dual-target dc-magnetron sputtering on MgO(001) substrates kept at 700 °C. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) showed that the analytical model mentioned above predicts the peak positions of the experimental XRD and SAED spectra with a very high accuracy. Furthermore, numerical calculations of the diffraction intensities based on a kinematical model of diffraction showed good agreement with the experimental data for all three cases. In addition to a direct verification of the quasiperiodic modulation, both conventional and high-resolution cross-sectional transmission electron microscopy (XTEM) showed that the superlattices are of high crystalline quality with sharp interfaces. Based on lattice resolution images, the width of the interfaces was determined to be less than two (002) lattice-plane spacings (~=0.31 nm).

X-ray diffraction study of A- plane non-polar InN epilayer grown by MOCVD

NASA Astrophysics Data System (ADS)

Moret, Matthieu; Briot, Olivier; Gil, Bernard

2015-03-01

Strong polarisation-induced electric fields in C-plane oriented nitrides semiconductor layers reduce the performance of devices. Eliminating the polarization fields can be achieved by growing nitrides along non polar direction. We have grown non polar A-plane oriented InN on R-plane (1‾102) nitridated sapphire substrate by MOCVD. We have studied the structural anisotropy observed in these layers by analyzing High Resolution XRay Diffraction rocking curve (RC) experiments as a function of the in-plane beam orientation. A-plane InN epilayer have a unique epitaxial relationship on R-Plane sapphire and show a strong structural anisotropy. Full width at half maximum (FWHM) of the InN(11‾20) XRD RC values are contained between 44 and 81 Arcmin. FWHM is smaller when the diffraction occurs along the [0001] and the largest FWHM values, of the (11‾20) RC, are obtained when the diffraction occurs along the [1‾100] in-plane direction. Atomic Force Microscopy imaging revealed morphologies with well organized crystallites. The grains are structured along a unique crystallographic orientation of InN, leading to larger domains in this direction. This structural anisotropy can be, in first approximation, attributed to the difference in the domain sizes observed. XRD reciprocal space mappings (RSM) were performed in asymmetrical configuration on (13‾40) and (2‾202) diffraction plane. RSM are measured with a beam orientation corresponding to a maximal and a minimal width of the (11‾20) Rocking curves, respectively. A simple theoretical model is exposed to interpret the RSM. We concluded that the dominant contribution to the anisotropy is due to the scattering coherence length anisotropy present in our samples.

Investigation of photoluminescence and dielectric properties of pure and Fe doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmad, Arham S.

2018-05-01

The nanocrystallites of pure and Fe doped Nickel Oxide (NiO) were synthesized by the cost effective co-precipitation method using nickel nitrate as the initial precursor. The synthesized nickel oxide nanoparticles were characterized by X-Ray Diffraction (XRD), Photoluminiscence Spectroscopy (PL), LCR meter. The crystallite size of synthesized pure Nickel Oxide nanoparticles obtained by XRD using Debye Scherer's formula was found to be 21.8nm and the size decreases on increasing the dopant concentration. The optical properties were analyzed by PL and dielectric ones by using LCR meter.

Preparation of Cu-doped nickel oxide thin films and their properties

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

Gowthami, V.; Meenakshi, M.; Anandhan, N.

2014-04-24

Copper doped Nickel oxide film was preferred on glass substrate by simple nebulizer technique keeping the substrate temperature at 350°C and characterized by X-ray diffraction (XRD), Photoluminescence (PL) and Four probe resistivity measurements. XRD studies indicated cubic structure and the crystallites are preferentially oriented along the [111] direction. Interesting results have been obtained from the study of PL spectra. A peak corresponding to 376nm in the emission spectra for 0%, 5% and 10% copper doped samples. The samples show sharp and strong UV emission corresponding to the near band edge emission under excitation of 275nm.

Observation of martensitic transformation in Ni50Mn41Cu4Sn5 Heusler alloy prepared by mechanical alloying

NASA Astrophysics Data System (ADS)

Saini, Dinesh; Singh, Satyavir; Banerjee, M. K.; Sachdev, K.

2017-05-01

Mechanical alloying route has been employed for preparation of a single phase Ni50Mn41Cu4Sn5 (atomic %) Heusler alloy. Use of high energy planetary ball mill enables successful preparation of the same as authenticated by detailed X-ray diffraction (XRD) study. Microstructural study is carried out by optical and scanning electron microscopic techniques. XRD results reveal that increasing milling time leads to reduction in crystallite size and concurrent increase in lattice strain. Microstructural results indicate formation of self-assembled martensite twins.

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

Ren, Fang; Williams, Travis; Hattrick-Simpers, Jason

Investment in brighter sources and larger detectors has resulted in an explosive rise in the data collected at synchrotron facilities. Currently, human experts extract scientific information from these data, but they cannot keep pace with the rate of data collection. Here, we present three on-the-fly approaches—attribute extraction, nearest-neighbor distance, and cluster analysis—to quickly segment x-ray diffraction (XRD) data into groups with similar XRD profiles. An expert can then analyze representative spectra from each group in detail with much reduced time, but without loss of scientific insights. As a result, on-the-fly segmentation would, therefore, result in accelerated scientific productivity.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

Yepes, N.; Orozco, J.; Caamaño, Z.; Mass, J.; Pérez, G.

2014-04-01

Nanostructured Fe50Co50 alloy was prepared by mechanical alloying of Fe and Co powders in a planetary high energy ball milling. The microstructure and structural evolution of the alloy have been investigated as a function of milling time (0 h, 8 h, 20 h and 35 h) by scanning electron microscopy (SEM) and X-Ray diffraction (XRD) characterization techniques. SEM micrographs showed different powder particles morphologies during the mechanical alloying stages. By XRD analysis it could be identified the structural phases of the alloy and the crystallite size was calculated as a function of the milling time.

Structural and electrical study of ZrO{sub 2} nanoparticles modified with surfactants

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

Sidhu, Gaganpreet Kaur; Kumar, Rajesh, E-mail: rajeshbaboria@gmail.com; Tripathi, S. K.

2015-06-24

Zirconia ceramic is one of the most investigated materials for its outstanding mechanical properties and ionic conduction properties, due to its high oxygen ion conduction. In order to achieve novel properties of zirconia nanoparticles, nanoparticles of zirconia are modified by using two different surfactants (SDS and CTAB) were prepared by in-situ method using zirconia/surfactant dispersions. Zirconia nanoparticles with surfactant (SDS or CTAB) were synthesized by hydrothermal method. The structural and optical properties of Zirconia/surfactant nanoparticles were investigated comprehensively by X-Ray diffraction (XRD), and electrical measurements. XRD highlights the crystalline behavior of nanoparticles.

Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

PubMed

Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

2009-01-01

A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

Aspherical-atom modeling of coordination compounds by single-crystal X-ray diffraction allows the correct metal atom to be identified.

PubMed

Dittrich, Birger; Wandtke, Claudia M; Meents, Alke; Pröpper, Kevin; Mondal, Kartik Chandra; Samuel, Prinson P; Amin Sk, Nurul; Singh, Amit Pratap; Roesky, Herbert W; Sidhu, Navdeep

2015-02-02

Single-crystal X-ray diffraction (XRD) is often considered the gold standard in analytical chemistry, as it allows element identification as well as determination of atom connectivity and the solid-state structure of completely unknown samples. Element assignment is based on the number of electrons of an atom, so that a distinction of neighboring heavier elements in the periodic table by XRD is often difficult. A computationally efficient procedure for aspherical-atom least-squares refinement of conventional diffraction data of organometallic compounds is proposed. The iterative procedure is conceptually similar to Hirshfeld-atom refinement (Acta Crystallogr. Sect. A- 2008, 64, 383-393; IUCrJ. 2014, 1,61-79), but it relies on tabulated invariom scattering factors (Acta Crystallogr. Sect. B- 2013, 69, 91-104) and the Hansen/Coppens multipole model; disordered structures can be handled as well. Five linear-coordinate 3d metal complexes, for which the wrong element is found if standard independent-atom model scattering factors are relied upon, are studied, and it is shown that only aspherical-atom scattering factors allow a reliable assignment. The influence of anomalous dispersion in identifying the correct element is investigated and discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Morphology and crystallinity of sisal nanocellulose after sonication

NASA Astrophysics Data System (ADS)

Sosiati, H.; Wijayanti, D. A.; Triyana, K.; Kamiel, B.

2017-09-01

Different preparation methods on the natural fibers resulted in different morphology. However, the relationships between type of natural fibers, preparation methods and the morphology of produced nanocellulose could not be exactly defined. The sisal nanocellulose was presently prepared by alkalization and bleaching followed by sonication to verify changes in the morphology and crystallinity of nanocellulose related to the formation mechanism. The extracted microcellulose was subjected to scanning electron microscopy (SEM) and x-ray diffraction (XRD) analysis. The isolated cellulose nanospheres were examined with respect to morphology by SEM and transmission electron microscopy (TEM) and, to crystallinity by electron diffraction analysis. Bleaching after alkalization made the microfibrils clearly separated from each other to the individual fiber whose width of the single fiber was ranging from 6 to 13 µm. The XRD crystallinity index (CI) of microcellulose gradually increased after the chemical treatments; 83.12% for raw sisal fiber, 88.57% for alkali treated fiber and 94.03% for bleached fibers. The ultrasonic agitation after bleaching that was carried out at 750 Watt, 20 kHz and amplitude of 39% for 2 h produces homogeneous cellulose nanospheres less than 50 nm in diameter with relatively low crystallinity. The electron diffraction analysis confirmed that the low crystallinity of produced nnocellulose is related to the effect of chemical treatment done before sonication.

Compositional and quantitative microtextural characterization of historic paintings by micro-X-ray diffraction and Raman microscopy.

PubMed

Romero-Pastor, Julia; Duran, Adrian; Rodríguez-Navarro, Alejandro Basilio; Van Grieken, René; Cardell, Carolina

2011-11-15

This work shows the benefits of characterizing historic paintings via compositional and microtextural data from micro-X-ray diffraction (μ-XRD) combined with molecular information acquired with Raman microscopy (RM) along depth profiles in paint stratigraphies. The novel approach was applied to identify inorganic and organic components from paintings placed at the 14th century Islamic University-Madrasah Yusufiyya-in Granada (Spain), the only Islamic University still standing from the time of Al-Andalus (Islamic Spain). The use of μ-XRD to obtain quantitative microtextural information of crystalline phases provided by two-dimensional diffraction patterns to recognize pigments nature and manufacture, and decay processes in complex paint cross sections, has not been reported yet. A simple Nasrid (14th century) palette made of gypsum, vermilion, and azurite mixed with glue was identified in polychromed stuccos. Here also a Christian intervention was found via the use of smalt, barite, hematite, Brunswick green and gold; oil was the binding media employed. On mural paintings and wood ceilings, more complex palettes dated to the 19th century were found, made of gypsum, anhydrite, barite, dolomite, calcite, lead white, hematite, minium, synthetic ultramarine blue, and black carbon. The identified binders were glue, egg yolk, and oil.

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

Mohamad, Khairul Anuar; Rusnan, Fara Naila; Seria, Dzulfahmi Mohd Husin

Investigation on the physical characterization and comparison of organic thin film based on a soluble 6,13-bis(triisopropylsilylethynyl) (TIPS) pentacene is reported. Oriented thin-films of pentacene have been successfully deposited by flow-coating method, in which the chloroform solution is sandwiched between a transparent substrate and a slide glass, followed by slow-drawing of the substrate with respect to the slide glass. Molecular orientation of flow-coated TIPS-pentacene is comparable to that of the thermal-evaporated pentacene thin film by the X-ray diffraction (XRD) results. XRD results showed that the morphology of flow-coated soluble pentacene is similar to that of the thermal-evaporated pentacene thin films inmore » series of (00l) diffraction peaks where the (001) diffraction peaks are strongest in the nominally out-of-plane intensity and interplanar spacing located at approximately 2θ = 5.33° (d-spacing, d{sub 001} = 16 Å). Following that, ITO/p-TIPS-pentacene/n-ZnO/Au vertical diode was fabricated. The diode exhibited almost linear characteristics at low voltage with nonlinear characteristics at higher voltage which similar to a pn junction behavior. The results indicated that the TIPS-pentacene semiconductor active thin films can be used as a hole injection layer for fabrication of a vertical organic transistor.« less

Structure-charge relationship - the case of hematite (001)

DOE PAGES

Lutzenkirchen, Johannes; Heberling, Frank; Supljika, Filip; ...

2015-01-16

We present a multidisciplinary study on the hematite (001)–aqueous solution interface, in particular the relationship between surface structure (studied via surface diffraction in a humid atmosphere) and the macroscopic charging (studied via surface- and zeta-potential measurements in electrolyte solutions as a function of pH). Upon aging in water changes in the surface structure are observed, that are accompanied by drastic changes in the zeta-potential. Surprisingly the surface potential is not accordingly affected. We interpret our results by increasing hydration of the surface with time and enhanced reactivity of singly-coordinated hydroxyl groups that cause the isoelectric point of the surface tomore » shift to values that are reminiscent of those typically reported for hematite particles. In its initial stages after preparation the hematite surface is very flat and only weakly hydrated. Our model links the entailing weak water structure with the observed low isoelectric point reminiscent of hydrophobic surfaces. The absence of an aging effect on the surface potential vs. pH curves is interpreted as domination of the surface potential by the doubly coordinated hydroxyls, which are present on both surfaces.« less

X-ray diffraction study of the mineralogy of microinclusions in fibrous diamond

NASA Astrophysics Data System (ADS)

Smith, Evan; Kopylova, Maya; Dubrovinksy, Leonid

2010-05-01

Fibrous diamond, occurring both as cuboids and as coatings over non-fibrous diamond nuclei, is translucent due to the presence of millions of sub-micron-sized mineral and fluid inclusions. Diamond is strong and relatively inert, making it an excellent vessel to preserve trapped materials. These microinclusions represent direct samples of natural diamond-forming mantle fluids, and are critical for our understanding of diamond genesis. Traditionally, infrared spectroscopy, Raman spectroscopy, secondary ion mass spectrometry, electron microprobe, and FIB-TEM techniques have proven to be effective for the study of microinclusions in diamond. The abundance and random orientation of included minerals in fibrous diamond make them amenable to a powder-type X-ray diffraction (XRD) technique. This technique provides an accurate way to identify included minerals. It also has the advantage of analyzing thousands of inclusions simultaneously, rather than analyzing one inclusion at a time, as with common FIB-TEM techniques. XRD provides a bulk analysis, giving a superior measure of relative abundances of included minerals, as well as potentially accounting for small quantities of minerals that might otherwise be overlooked. We studied fibrous cuboid diamonds with microinclusions from the Democratic Republic of Congo (DRC) (23 samples), Brazil (4 samples), Jericho (1 sample), and Wawa conglomerates (9 samples). XRD analysis was performed at the Bayerisches Geoinstitut (BGI), University of Bayreuth, Germany. The unique XRD setup consists of a RIGAKU FR-D high-brilliance source, OSMIC Inc. Confocal Max-Flux optics, and a SMART APEX 4K CCD area detector. Preliminary XRD studies of microinclusions 8 fibrous diamonds from the DRC showed a prevalence of silicates with structural and coordinated H2O. Sheet silicates constituted 9 out of 13 detected minerals, with phlogopite-biotite micas being present in 4 out of 8 samples. Other detected minerals were 2 chlorite minerals, 2 clay phyllosilicates, serpentine, zircon, a hydrous carbonate and an unidentified zeolite. Many of these phases are deuteric, replacing high-T, high-P micas and carbonates that precipitate from the fluid in the diamond stability field. The ongoing XRD study will (1) elucidate the mineralogy of fluid inclusions in diamonds from Wawa, (2) compare XRD analyses to distinguish between diamonds with carbonatitic versus saline fluid compositions, and (3) reveal whether carbonates occur as crystalline phases or as dissolved or amorphous material in fibrous diamond.

Is Tridymite at Gale Crater Evidence for Silicic Volcanism on Mars?

NASA Technical Reports Server (NTRS)

Morris, Richard V.; Vaniman, David T.; Ming, Douglas W.; Graff, Trevor G.; Downs, Robert T.; Fendrich, Kim; Mertzman, Stanley A.

2016-01-01

The X-ray diffraction (XRD) instrument (CheMin) onboard the MSL rover Curiosity detected 17 wt% of the SiO2 polymorph tridymite (relative to bulk sample) for the Buckskin drill sample (73 wt% SiO2) obtained from sedimentary rock in the Murray formation at Gale Crater, Mars. Other detected crystalline materials are plagioclase, sanidine, cristobalite, cation-deficient magnetite, and anhydrite. XRD amorphous material constitutes approx. 60 wt% of bulk sample, and the position of its broad diffraction peak near approx. 26 deg. 2-theta is consistent with opal-A. Tridymite is a lowpressure, high-temperature mineral (approx. 870 to 1670 deg. C) whose XRD-identified occurrence on the Earth is usually associated with silicic (e.g., rhyolitic) volcanism. High SiO2 deposits have been detected at Gale crater by remote sensing from martian orbit and interpreted as opal-A on the basis H2O and Si-OH spectral features. Proposed opal-A formation pathways include precipitation of silica from lake waters and high-SiO2 residues of acid-sulfate leaching. Tridymite is nominally anhydrous and would not exhibit these spectral features. We have chemically and spectrally analyzed rhyolitic samples from New Mexico and Iwodake volcano (Japan). The glassy (by XRD) NM samples have H2O spectral features similar to opal-A. The Iwodake sample, which has been subjected to high-temperature acid sulfate leaching, also has H2O spectral features similar to opal-A. The Iwodake sample has approx. 98 wt% SiO2 and 1% wt% TiO2 (by XRF), tridymite (>80 wt.% of crystalline material without detectable quartz by XRD), and H2O and Si-OH spectral features. These results open the working hypothesis that the opal-A-like high-SiO2 deposits at Gale crater detected from martian orbit are products of alteration associated with silicic volcanism. The presence or absence of tridymite will depend on lava crystallization temperatures (NM) and post crystallization alteration temperatures (Iwodake).

In-plane x-ray diffraction for characterization of monolayer and few-layer transition metal dichalcogenide films

NASA Astrophysics Data System (ADS)

Chubarov, Mikhail; Choudhury, Tanushree H.; Zhang, Xiaotian; Redwing, Joan M.

2018-02-01

There is significant interest in the growth of single crystal monolayer and few-layer films of transition metal dichalcogenides (TMD) and other 2D materials for scientific exploration and potential applications in optics, electronics, sensing, catalysis and others. The characterization of these materials is crucial in determining the properties and hence the applications. The ultra-thin nature of 2D layers presents a challenge to the use of x-ray diffraction (XRD) analysis with conventional Bragg-Brentano geometry in analyzing the crystallinity and epitaxial orientation of 2D films. To circumvent this problem, we demonstrate the use of in-plane XRD employing lab scale equipment which uses a standard Cu x-ray tube for the analysis of the crystallinity of TMD monolayer and few-layer films. The applicability of this technique is demonstrated in several examples for WSe2 and WS2 films grown by chemical vapor deposition on single crystal substrates. In-plane XRD was used to determine the epitaxial relation of WSe2 grown on c-plane sapphire and on SiC with an epitaxial graphene interlayer. The evolution of the crystal structure orientation of WS2 films on sapphire as a function of growth temperature was also examined. Finally, the epitaxial relation of a WS2/WSe2 vertical heterostructure deposited on sapphire substrate was determined. We observed that WSe2 grows epitaxially on both substrates employed in this work under all conditions studied while WS2 exhibits various preferred orientations on sapphire substrate which are temperature dependent. In contrast to the sapphire substrate, WS2 deposited on WSe2 exhibits only one preferred orientation which may provide a route to better control the orientation and crystal quality of WS2. In the case of epitaxial graphene on SiC, no graphene-related peaks were observed in in-plane XRD while its presence was confirmed using Raman spectroscopy. This demonstrates the limitation of the in-plane XRD technique for characterizing low electron density materials.

Structural and spectroscopic study of mechanically synthesized SnO{sub 2} nanostructures

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

Vij, Ankush, E-mail: vij-anx@yahoo.com; Kumar, Ravi; Presently at Beant College of Engineering and Technology, Gurdaspur-143521

2016-05-23

We report the single step synthesis of SnO{sub 2} nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO{sub 2} nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A{sub 1g} Raman mode towards lower wave number, which is correlated with the nanostructure formation.

In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

PubMed

Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

2017-06-12

The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

A study of tantalum pentoxide Ta 2O 5 structures up to 28 GPa

DOE PAGES

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

2017-05-02

In this study, tantalum pentoxide Ta 2O 5 with the orthorhombic L-Ta 2O 5 structure has been experimentally studied up to 28.3 GPa (at ambient temperature) using synchrotron angle-dispersive powder X-ray diffraction (XRD). The ambient pressure phase remains stable up to 25 GPa where with increased pressure a crystalline to amorphous phase transition occurs. A detailed equation of state (EOS), including pressure dependent lattice parameters, is reported. The results of this study were compared with a previous high-pressure XRD study by Li et al. A clear discrepancy between the ambient-pressure crystal structures and, consequently, the reported EOSs between the twomore » studies was revealed. Finally, he origin of this discrepancy is attributed to two different crystal structures used to index the XRD patterns.« less

Adsorption of vitamin E on mesoporous titania nanocrystals

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

Shih, C.J., E-mail: cjshih@kmu.edu.tw; Lin, C.T.; Wu, S.M.

2010-07-15

Tri-block nonionic surfactant and titanium chloride were used as starting materials for the synthesis of mesoporous titania nanocrystallite powders. The main objective of the present study was to examine the synthesis of mesoporous titania nanocrystals and the adsorption of vitamin E on those nanocrystals using X-ray diffraction (XRD), transmission electron microscopy, and nitrogen adsorption and desorption isotherms. When the calcination temperature was increased to 300 {sup o}C, the reflection peaks in the XRD pattern indicated the presence of an anatase phase. The crystallinity of the nanocrystallites increased from 80% to 98.6% with increasing calcination temperature from 465 {sup o}C tomore » 500 {sup o}C. The N{sub 2} adsorption data and XRD data taken after vitamin E adsorption revealed that the vitamin E molecules were adsorbed in the mesopores of the titania nanocrystals.« less

Effects of Gold Salt Speciation and Structure of Human and Bovine Serum Albumin on the Synthesis and Stability of Gold Nanostructures

NASA Astrophysics Data System (ADS)

Miranda, Érica; Tofanello, Aryane; Brito, Adrianne; Lopes, David; Giacomelli, Fernando; Albuquerque, Lindomar; Costa, Fanny; Ferreira, Fabio; Araujo-Chaves, Juliana; de Castro, Carlos; Nantes, Iseli

2016-03-01

The present study aimed to investigate the influence of albumin structure and gold speciation on the synthesis of gold nanoparticles (GNPs). The strategy of synthesis was the addition of HAuCl4 solutions at different pH values (3-12) to solutions of human and bovine serum albumins (HSA and BSA) at the same corresponding pH values. Different pH values influence the GNP synthesis due to gold speciation. Besides the inherent effect of pH on the native structure of albumins, the use N-ethylmaleimide (NEM)-treated and heat-denaturated forms of HSA and BSA provided additional insights about the influence of protein structure, net charge, and thiol group approachability on the GNP synthesis. NEM treatment, heating, and the extreme values of pH promoted loss of the native albumin structure. The formation of GNPs indicated by the appearance of surface plasmon resonance (SPR) bands became detectable from fifteen days of the synthesis processes that were carried out with native, NEM-treated and heat-denaturated forms of HSA and BSA, exclusively at pH 6 and 7. After two months of incubation, SPR band was also detected for all synthesis carried out at pH 8.0. The mean values of the hydrodynamic radius (RH) were 24 and 34 nm for GNPs synthesized with native HSA and BSA, respectively. X-ray diffraction (XRD) revealed crystallites of 13 nm. RH, XRD, and zeta potential values were consistent with GNP capping by the albumins. However, the GNPs produced with NEM-treated and heat-denaturated albumins exhibited loss of protein capping by lowering the ionic strength. This result suggests a significant contribution of non-electrostatic interactions of albumins with the GNP surface, in these conditions. The denaturation of proteins exposes hydrophobic groups to the solvent, and these groups could interact with the gold surface. In these conditions, the thiol blockage or oxidation, the latter probably favored upon heating, impaired the formation of a stable capping by thiol coordination with the gold surface. Therefore, the cysteine side chain of albumins is important for the colloidal stabilization of GNPs rather than as the reducing agent for the synthesis. Despite the presence of more reactive gold species at more acidic pH values, i.e., below

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour

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

Narayanan, Kannan Badri; Sakthivel, Natarajan, E-mail: puns2005@gmail.com

2011-10-15

Highlights: {yields} Synthesis of AgNPs using the leaf extract of Coleus amboinicus L. was described. {yields} UV-vis absorption spectra showed the formation of isotrophic AgNPs at 437 nm in 6 h. {yields} XRD analysis showed intense peaks corresponding to fcc structure of AgNPs. {yields} HR-TEM analysis revealed the formation of stable anisotrophic and isotrophic AgNPs. -- Abstract: In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmissionmore » electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Johnson, David K; Lee, Christopher; Dazen, Kevin

2015-07-04

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Lee, Christopher M; Dazen, Kevin; Kafle, Kabindra

2015-01-01

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Dynamic XRD, Shock and Static Compression of CaF2

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew; Smith, Jesse; Sinogeikin, Stanislav

2017-06-01

The high-pressure behavior of CaF2 is probed with x-ray diffraction (XRD) combined with both dynamic compression, using a two-stage light gas gun, and static compression, using diamond anvil cells. We use XRD to follow the unfolding of a shock-driven, fluorite to cotunnite phase transition, on the timescale of nanoseconds. The dynamic behavior of CaF2 under shock loading is contrasted with that under static compression. This work leverages experimental capabilities at the Advanced Photon Source: dynamic XRD and shock experiments at the Dynamic Compression Sector, as well as XRD and static compression in diamond anvil cell at the High-Pressure Collaborative Access Team. These experiments and cross-platform comparisons, open the door to an unprecedented understanding of equations of state and phase transitions at the microstructural level and at different time scales and will ultimately improve our capability to simulate the behavior of materials at extreme conditions. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Simulation study of an X-ray diffraction system for breast tumor detection

NASA Astrophysics Data System (ADS)

Marticke, F.; Montémont, G.; Paulus, C.; Michel, O.; Mars, J. I.; Verger, L.

2017-09-01

X-ray diffraction (XRD) is a powerful technique used to determine the molecular structure of biological tissues. In breast tissues for example, the scattering signatures of dense fibroglandular tissue and carcinoma have been shown to be significantly different. In this study, XRD was used as a second control level when conventional mammography results were unclear, for instance because of overly high breast density. A system optimized for this issue, called multifocal XRD, was developed combining energy dispersive spectral information at different scattering angles. This system allows depth-imaging in one go but needs an x,y-direction scan to image the region conventional mammography identified as suspect. The scan-time for about 10 cm3 with an incident flux of about 4 . 8 ṡ 107 photons per second would be around 2 s. For this study, breast phantoms with and without cancerous nodule were simulated to assess the separation power of the method and to determine the radiation dose required to obtain nearly ideal separation. For tumors situated in the center of the breast, the required dose was only about 0.3 mGy, even for breasts with high density. The tumor position was shown to have a low impact on detectability provided it remained in a zone where the system was sufficiently sensitive. The influence of incident spectrum maximum energy was also studied. The required dose remained very low with any of the incident spectra tested. Finally, an image slice was reconstructed in the x-direction and showed that the system can detect the presence of a small tumor (4 mm). Hence, XRD is a very promising tool to reduce the number of unnecessary invasive breast biopsies.

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.

Remediation of uranium-contaminated groundwater by sorption onto hydoxyapatite derived from catfish bones

USDA-ARS?s Scientific Manuscript database

Hydroxyapatite was prepared from catfish bones, called catfish hydroxyapatite (CFHA), by mechanical and chemical treatment methods and was characterized by x-ray diffraction (X-RD) and scanning electron microscope (SEM) techniques to confirm the presence of hydroxyapatite. The ability of CFHA to rem...

Assessing the Potential for Bioremediation through Formation and Fate of Metal Rich Granules in the Terrestrial Environment

DTIC Science & Technology

2011-05-01

laboratory ► biochemistry and analytical laboratories BUILDING STRONG® Impacts of Lead (Pb) • Most common metal contaminant on US Army small arms...Diffraction (XRD): Crystalline phase identification through fingerprinting Tungsten and Calcium in Snail Shell W Identificati on of Selenium and

SORPTION OF LEAD ON A RUTHENIUM COMPOUND: A MACROSCOPIC AND MICROSCOPIC STUDY

EPA Science Inventory

The objective of this study was to elucidate the sorption mechanism of Pb on the high-affinity ruthenium compound with time at pH 6 employing batch methods and X-ray absorption fine structure (XAFS) and X-ray diffraction (XRD) spectroscopies. For the spectroscopic studies, Pb so...

Simple Analysis of Historical Lime Mortars

ERIC Educational Resources Information Center

Pires, Joa~o

2015-01-01

A laboratory experiment is described in which a simple characterization of a historical lime mortar is made by the determination of its approximate composition by a gravimetric method. Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) are also used for the qualitative characterization of the lime mortar components. These…

Structural transformation of biochar black carbon by C60 superstructure: Environmental implications

USDA-ARS?s Scientific Manuscript database

Aqueous fullerene C60 nanoparticles (nC60) are frequently considered within the environmental engineering community as the aggregate of 60-carbon molecules. This study employed transmission electron microscopy (TEM) and x-ray diffraction (XRD) to demonstrate that nC60 formed via prolonged stirring ...

Carnosine-graphene oxide conjugates decorated with hydroxyapatite as promising nanocarrier for ICG loading with enhanced antibacterial effects in photodynamic therapy against Streptococcus mutans.

PubMed

Gholibegloo, Elham; Karbasi, Ashkan; Pourhajibagher, Maryam; Chiniforush, Nasim; Ramazani, Ali; Akbari, Tayebeh; Bahador, Abbas; Khoobi, Mehdi

2018-04-01

Antimicrobial photodynamic therapy (aPDT) has been emerged as a noninvasive strategy to remove bacterial contaminants such as S. mutans from the tooth surface. Photosensitizer (PS), like indocyanine green (ICG), plays a key role in this technique which mainly suffers from the poor stability and concentration-dependent aggregation. An appropriate nanocarrier (NC) with enhanced antibacterial effects could overcome these limitations and improve the efficiency of ICG as a PS. In this study, various ICG-loaded NCs including graphene oxide (GO), GO-carnosine (Car) and GO-Car/Hydroxyapatite (HAp) were synthesized and characterized by Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Filed Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS), Zeta Potential and Ultraviolet-Visible spectrometry (UV-Vis). The colony forming unit and crystal violet assays were performed to evaluate the antimicrobial and anti-biofilm properties of PSs against S. mutans. The quantitative real-time PCR approach was also applied to determine the expression ratio of the gtfB gene in S. mutans. The zeta potential analysis and UV-Vis spectrometry indicated successful loading of ICG onto/into NCs. GO-Car/HAp showed highest amount of ICG loading (57.52%) and also highest aqueous stability after one week (94%). UV-Vis spectrometry analyses disclosed a red shift from 780 to 800 nm for the characteristic peak of ICG-loaded NCs. In the lack of aPDT, GO-Car@ICG showed the highest decrease in bacterial survival (86.4%) which indicated that Car could significantly promote the antibacterial effect of GO. GO@ICG, GO-Car@ICG and GO-Car/HAp@ICG mediated aPDT, dramatically declined the count of S. mutans strains to 91.2%, 95.5% and 93.2%, respectively (P < 0.05). The GO@ICG, GO-Car@ICG, GO-Car/HAp@ICG significantly suppressed the S. mutans biofilm formation by 51.4%, 63.8%, and 56.8%, respectively (P < 0.05). The expression of gtfB gene was considerably reduced to 6.0, 9.0 and 7.9-fold after aPDT in the presence of GO@ICG, GO-Car@ICG, GO-Car/HAp@ICG, respectively (P < 0.05). It could be concluded that the multi-functionalized GO as a novel nanocarrier could significantly enhance the ICG loading, stability, and improve its inhibitory effects as a photosensitizer in aPDT against S. mutans. These findings might provide opportunity for efficient treatment of local dental infections. Copyright © 2018 Elsevier B.V. All rights reserved.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Research on the Treatment of Wastewater by Waste Ceramic Adsorption

NASA Astrophysics Data System (ADS)

He, Lingfeng; Zhang, Yongli; Shi, Liang

2018-03-01

The process of preparing porous ceramic with waste porcelain powder as aggregate was researched. The affect of assimilate time on cuprum removal efficiency in wastewater containing copper was investigated. The results show the water copper removal rate increased along with the augment of assimilate time, and the assimilate time is suitable for 35 min; XRD characterizations show the porous ceramic catalyst before and after calcination in active components of X ray diffraction peak position almost had no changes, and the diffraction intensity slightly changed with calcination and absorption, and diffraction peaks became sharper, and its crystallinity was improved. Baking leads to the growth of crystal particles, and the performance of porous ceramics is stable before and after adsorption.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

One-step synthesis of magnetic chitosan for controlled release of 5-hydroxytryptophan

NASA Astrophysics Data System (ADS)

Santos Menegucci, Jucély dos; Santos, Mac-Kedson Medeiros Salviano; Dias, Diego Juscelino Santos; Chaker, Juliano Alexandre; Sousa, Marcelo Henrique

2015-04-01

In this work, nanoparticles of chitosan embedded with 25% (w/w) of iron oxide magnetic nanoparticles (magnetite/maghemite) with narrow size-distribution and with a loading efficiency of about 80% for 5-hydroxytryptophan (5-HTP), which is a chemical precursor in the biosynthesis of important neurotransmitters as serotonin, were synthesized with an initial mass ratio of 5-HTP/magnetic chitosan=1.2, using homogeneous precipitation by urea decomposition, in an efficient one-step procedure. Characterization of morphology, structure and surface were performed by XRD, TEM, FTIR, TGA, magnetization and zeta potential measurements, while drug loading and drug releasing were investigated using UV-vis spectroscopy. Kinetic drug release experiments under different pH conditions revealed a pH-sensitivecontrolled-release system, ruled by polymer swelling and/or particle dissolution.

Preparation of well-adhered γ-Al 2O 3 washcoat on metallic wire mesh monoliths by electrophoretic deposition

NASA Astrophysics Data System (ADS)

Sun, Hong; Quan, Xie; Chen, Shuo; Zhao, Huimin; Zhao, Yazhi

2007-01-01

Washcoat deposited on metallic wire mesh monoliths was prepared using γ-alumina powders by electrophoretic deposition under a relatively low electric voltage. The microstructure, phase structure and adhesion of washcoat were investigated by SEM, XRD, ultrasonic vibration and thermal shock. The results showed that the loading and adhesion of washcoat were affected obviously by the properties of suspension, such as the zeta potential and the amount of adding binders. A small quantity of aluminum isopropoxide could promote the cohesive affinity of washcoat in thermal shock. The adhesion of washcoat in ultrasonic vibration could be reinforced by increasing calcined temperature and adding a certain aluminum particles. It was also found that the washcoat immersed metal nitrate has excellent vibration-resistant ability.

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

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

Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon

2016-10-18

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffractionmore » data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.« less

Structure and luminescence properties of Tb3+-doped Lu3Al5O12 films prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Wang, Jian; Shen, Siqing; Xie, Jianjun; Shi, Ying; Ai, Fei

2011-02-01

Tb3+-doped Lu3Al5O12(hereinafter referred to as LuAG:Tb) films were successfully prepared by Pechini sol-gel process and spin-coating technique on carefully cleaned (111) silicon wafer. The microstructure and optical properties of the LuAG:Tb films were studied by X-ray diffraction (XRD), atomic force microscopy(AFM), as well as photoluminescence (PL) spectra. The XRD results showed that the precursor films started to crystallize at about 900°C. All as-calcined LuAG:Tb films showed the Tb3+ characteristic emission bands.

Structure and luminescence properties of Tb3+-doped Lu3Al5O12 films prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Wang, Jian; Shen, Siqing; Xie, Jianjun; Shi, Ying; Ai, Fei

2010-10-01

Tb3+-doped Lu3Al5O12(hereinafter referred to as LuAG:Tb) films were successfully prepared by Pechini sol-gel process and spin-coating technique on carefully cleaned (111) silicon wafer. The microstructure and optical properties of the LuAG:Tb films were studied by X-ray diffraction (XRD), atomic force microscopy(AFM), as well as photoluminescence (PL) spectra. The XRD results showed that the precursor films started to crystallize at about 900°C. All as-calcined LuAG:Tb films showed the Tb3+ characteristic emission bands.

Green synthesis of silver nanoparticles using tannins

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

Synthesis, structure and temperature dependent luminescence of Eu3+ doped hydroxyapatite

NASA Astrophysics Data System (ADS)

Luo, Xiaobing; Luo, Xiaoxia; Wang, Hongwei; Deng, Yue; Yang, Peixin; Tian, Yili

2018-01-01

A series of Eu3+ substituted hydroxyapatite (HA) were prepared by co-precipitation reactions. The phase, fluorescence and temperature dependent luminescence of the phosphors were investigated by X-ray diffraction (XRD) and photoluminescence (PL). It is found that the doped Eu3+ ions have entered the hexagonal lattice with no obvious secondary phase were detected by XRD. The 5D0 → 7F0 transition was clearly split into two even at room temperature. The predominate 573 nm peak illustrates Eu3+ ions occupy more Ca(II) sites. The temperature dependent luminescent results show HA:xEu might be applied as one potential optical thermometry material.

Cadmium effect on structural properties of Cu{sub 2}Zn{sub 1-x}Cd{sub x}SnS{sub 4} quinternary alloys nanostructures

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

Ibraheam, A. S.; Al-Douri, Y., E-mail: yaldouri@yahoo.com; Hashim, U.

The study report novel sensing plat of extended quinternart materials, Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures were fabricated onto oxidized silicon substrate by sol-gel method and characterized were synthesized by X-ray diffraction (XRD). The XRD peaks were shifted towered the lower angle side with increasing cadmium content. The practical size average of the Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures between 34.55 to 63.30 nm.

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

In search of the elusive IrB 2: Can mechanochemistry help?

DOE PAGES

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina; ...

2015-10-20

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

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.

In search of the elusive IrB 2: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

Polymethacrylic acid as a new precursor of CuO nanoparticles

NASA Astrophysics Data System (ADS)

Hosny, Nasser Mohammed; Zoromba, Mohamed Shafick

2012-11-01

Polymethacrylic acid and its copper complexes have been synthesized and characterized. These complexes have been used as precursors to produce CuO nanoparticles by thermal decomposition in air. The stages of decompositions and the calcination temperature of the precursors have been determined from thermal analyses (TGA). The obtained CuO nanoparticles have been characterized by X-ray diffraction (XRD), scanning tunneling microscopy (STM) and transmission electron microscopy (TEM). XRD showed a monoclinic structure with particle size 8-20 nm for the synthesized copper oxide nanoparticles. These nanoparticles are catalytically active in decomposing hydrogen peroxide and a mechanism of decomposition has been suggested.

Interplay of structural, optical and magnetic properties in Gd doped CeO{sub 2}

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

Soni, S.; Dalela, S., E-mail: sdphysics@rediffmail.com; Kumar, Sudish

In this research wok systematic investigation on the synthesis, characterization, optical and magnetic properties of Ce{sub 1-x}Gd{sub x}O{sub 2} (where x=0.02, 0.04, 0.06, and 0.10) synthesized using the Solid-state method. Structural, Optical and Magnetic properties of the samples were investigated by X-ray diffraction (XRD), UV-VIS-NIR spectroscopy and VSM. Fluorite structure is confirmed from the XRD measurement on Gd doped CeO{sub 2} samples. Magnetic studies showed that the Gd doped polycrystalline samples display room temperature ferromagnetism and the ferromagnetic ordering strengthens with the Gd concentration.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

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

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Preparation and In Vitro/Ex Vivo Evaluation of Moxifloxacin-Loaded PLGA Nanosuspensions for Ophthalmic Application

PubMed Central

Mudgil, Meetali; Pawar, Pravin K.

2013-01-01

The aim of the present investigation was to prepare a colloidal ophthalmic formulation to improve the residence time of moxifloxacin. Moxifloxacin-loaded poly(dl-lactide-co-glycolide) (PLGA) nanosuspensions were prepared by using the solvent evaporation technique. The nanosuspensions were characterised physically by using different techniques like particle size, zeta potential, FTIR, DSC, and XRD analysis. In vitro and ex vivo studies of nanosuspensions were carried out using a modified USP dissolution apparatus and all-glass Franz diffusion cells, respectively. The antibacterial activities of the nanosuspension and marketed formulations were performed against S. aureus and P. aeroginosa. The moxifloxacin-loaded PLGA nanosuspensions showed uniform particle size, ranging between 164–490 nm with negative zeta potential for all batches. The percentage entrapment efficiency of the drug-loaded nano-suspension was found to be between 84.09 to 92.05%. In vitro drug release studies suggest that all of the formulations showed extended drug release profiles and follow Korsemeyer-Peppas release kinetics. In vitro corneal permeability was found to be comparable with that of the marketed formulation across isolated goat cornea, indicating the suitability of the nanosuspension formulation in the ophthalmic delivery of moxifloxacin. The optimised nano-suspension was found to be more active against S. aureus and P. aeruginosa compared to the marketed eye drops. PMID:23833723

Novel lectin-modified poly(ethylene-co-vinyl acetate) mucoadhesive nanoparticles of carvedilol: preparation and in vitro optimization using a two-level factorial design.

PubMed

Varshosaz, Jaleh; Moazen, Ellaheh

2014-08-01

Carvedilol used in cardiovascular diseases has systemic bioavailability of 25-35%. The objective of this study was production of lectin-modified poly(ethylene-co-vinyl acetate) (PEVA) as mucoadhesive nanoparticles to enhance low oral bioavailability of carvedilol. Nanoparticles were prepared by the emulsification-solvent evaporation method using a two-level factorial design. The studied variables included the vinyl acetate content of the polymer, drug and polymer content. Surface modification of PEVA nanoparticles with lectin was carried out by the adsorption method and coupling efficiency was determined using the Bradford assay. Mucoadhesion of nanoparticles was studied on mucin. The particle size, polydispersity index, zeta potential, drug loading and drug release from nanoparticles were studied. The morphology of nanoparticles and crystalline status of the entrapped drug were studied by SEM, DSC and XRD tests, respectively. Results showed the most effective factor on particle size and zeta potential was the interaction of polymer and drug content while, drug loading efficiency and mucoadhesion were more affected by the interaction of polymer type and drug content. Drug concentration was the most effective variable on the drug release rate. The drug was in amorphous state in nanoparticles. The optimum nanoparticles obtained by 45 mg of copolymer contained 12% vinyl acetate/4.3 ml of organic phase and drug concentration of 37.5 wt% of polymer.

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Asymmetric flavone-based liquid crystals: synthesis and properties

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

Timmons, Daren J.; Jordan, Abraham J.; Kirchon, Angelo A.

2017-02-01

A series of flavones (n-F) substituted at the 4', and 6 positions was prepared, characterised by NMR (1H,13C), HRMS, and studied for liquid crystal properties. The 4'-alkoxy,6-methoxyflavones (4-F–16-F) exhibit varying ranges of nematic and smectic A phases as evidenced by polarised optical microscopy and differential scanning calorimetry (DSC). As the tail length is increased, the smectic phase becomes more prevalent. Smectic phases for (8-F–16-F) were further analysed by powder X-ray diffraction (XRD), and the rate of structural transformations was explored by combined DSC/XRD studies. Flavonol 6-F–OH was also prepared but no mesogenic behaviour was observed. The molecular structures of 6-Fmore » and 6-F–OH were determined by single-crystal XRD and help to explain the differences in material properties. Additionally, fluorescence and electrochemical studies were conducted on solutions of n-F.« less

Stability of fluorite-type La 2Ce 2O 7 under extreme conditions

DOE PAGES

Zhang, F. X.; Tracy, C. L.; Lang, M.; ...

2016-03-03

Here, the structural stability of fluorite-type La 2Ce 2O 7 was studied at pressure up to ~40 GPa and under hydrothermal conditions (~1 GPa, 350 °C), respectively, using synchrotron x-ray diffraction (XRD) and Raman scattering measurements. XRD measurements indicated that fluorite-type La 2Ce 2O 7 is not stable at pressures greater than 22.6 GPa and slowly transforms to a high-pressure phase. The high-pressure phase is not stable and changes back to the fluorite-type structure when pressure is released. The La 2Ce 2O 7 fluorite is also not stable under hydrothermal conditions and begins to react with water at 200~250 °C.more » Both Raman and XRD results suggest that lanthanum hydroxide La(OH) 3 and La 3+-doped CeO 2 fluorite are the dominant products after hydrothermal treatment.« less

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.

XRD, SEM and infrared study into the intercalation of sodium hexadecyl sulfate (SHS) into hydrocalumite.

PubMed

Zhang, Ping; Wang, Tianqi; Zhang, Longlong; Wu, Daishe; Frost, Ray L

2015-12-05

Hydrocalumite (CaAl-LDH-Cl) interacted with a natural anionic surfactant, sodium hexadecyl sulfate (SHS), was performed using an intercalation method. To understand the intercalation behavior and characterize the resulting products, powder X-ray diffraction (XRD), scan electron microscopy (SEM) and mid-infrared (MIR) spectroscopy combined with near-infrared (NIR) spectroscopy technique were used. The XRD analysis indicated that SHS was intercalated into CaAl-LDH-Cl successfully, resulting in an expansion of the interlayer (from 0.78 nm to 2.74 nm). The bands of C-H stretching vibrations of SHS were observed in the near-infrared spectra, which indicated that the resulting products were indeed CaAl-LDH-SHS. In addition, the bands of water stretching vibrations and OH groups shifted to higher wavenumbers when SHS was intercalated into CaAl-LDH-Cl interlayer space. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Improving the Mechanical Performance and Thermal Stability of a PVA-Clay Nanocomposite by Electron Beam Irradiation

NASA Astrophysics Data System (ADS)

Shokuhi Rad, A.; Ebrahimi, D.

2017-07-01

The effects of electron beam irradiation and presence of clay on the mechanical properties and thermal stability of montmorillonite clay-modified polyvinyl alcohol nanocomposites were studied. By using the X-ray diffraction (XRD) and transmission electron microscopy (TEM), the microstructure of the nanocomposites was investigated. The results obtained from TEM and XRD tests showed that montmorillonite clay nanoparticles were located in the polyvinyl alcohol phase. The XRD analysis confirmed the formation of an exfoliated structure in nanocomposites samples. Increasing the amount of clay to 20 wt.% increased the tensile strength and modulus of the nanocomposite. Irradiation up to an absorbed dose of 100 kGy increased its mechanical properties and thermal stability, but at higher irradiation levels, the mechanical strength and thermal stability declined. The sample with 20 wt.% of the nanofiller, exposed to 100 kGy, showed the highest mechanical strength and thermal stability.

Classification-free threat detection based on material-science-informed clustering

NASA Astrophysics Data System (ADS)

Yuan, Siyang; Wolter, Scott D.; Greenberg, Joel A.

2017-05-01

X-ray diffraction (XRD) is well-known for yielding composition and structural information about a material. However, in some applications (such as threat detection in aviation security), the properties of a material are more relevant to the task than is a detailed material characterization. Furthermore, the requirement that one first identify a material before determining its class may be difficult or even impossible for a sufficiently large pool of potentially present materials. We therefore seek to learn relevant composition-structure-property relationships between materials to enable material-identification-free classification. We use an expert-informed, data-driven approach operating on a library of XRD spectra from a broad array of stream of commerce materials. We investigate unsupervised learning techniques in order to learn about naturally emergent groupings, and apply supervised learning techniques to determine how well XRD features can be used to separate user-specified classes in the presence of different types and degrees of signal degradation.

Influence of supercritical CO(2) pressurization on the phase behavior of mixed cholesteryl esters.

PubMed

Huang, Zhen; Feng, Mei; Su, Junfeng; Guo, Yuhua; Liu, Tie-Yan; Chiew, Yee C

2010-09-15

Evidences indicating the presence of phase transformations in the mixed cholesteryl benzoate (CBE) and cholesteryl butyrate (CBU) under the supercritical CO(2) pressurization, by means of differential scanning calorimetry (DSC) and X-ray diffraction (XRD), are presented in this work. These include (1) the DSC heating curve of pure CBU; (2) the DSC heating curves of CBU/CBE mixtures; (3) the XRD spectra of pure CBU; (4) the XRD spectra of CBU/CBE mixtures; (5) CBU and CBE are miscible in either solid phase or liquid phase over the whole composition range. As a result of the presence of these phase transformations induced by pressurization, it could be deduced that a solid solution of the CBU/CBE mixture might have formed at the interfaces under supercritical conditions, subsequently influencing their dissolving behaviors in supercritical CO(2). Copyright 2010 Elsevier B.V. All rights reserved.

A new approach for the recovery of precious metals from solution and from leachates derived from electronic scrap.

PubMed

Macaskie, L E; Creamer, N J; Essa, A M M; Brown, N L

2007-03-01

A new approach is described for the recovery of precious metals (PMs: Au, Pd and Ag) with >99% efficiency from aqueous solution utilising biogas produced during the aerobic growth of Klebsiella pneumoniae. Gold was recovered from electronic scrap leachate ( approximately 95%) by this method, with some selectivity against Cu. The recovered PM solids all contained metal and sulphur as determined by energy dispersive X-ray microanalysis (EDX). X-ray powder diffraction analysis (XRD) showed no crystalline metal sulphur compounds but a crystalline palladium amine was recorded. Silver was recovered as a sulphide (found by EDX), carbonate and oxide (found by XRD). EDX analysis of the Au-precipitate showed mainly gold and sulphur, with some metallic Au(0) detected by XRD. The gold compound was shock-sensitive; upon grinding it detonated to leave a sooty black deposit.

Effects of uniformities of deposition of respirable particles on filters on determining their quartz contents by using the direct on-filter X-ray diffraction (DOF XRD) method.

PubMed

Chen, Ching-Hwa; Tsaia, Perng-Jy; Lai, Chane-Yu; Peng, Ya-Lian; Soo, Jhy-Charm; Chen, Cheng-Yao; Shih, Tung-Sheng

2010-04-15

In this study, field samplings were conducted in three workplaces of a foundry plant, including the molding, demolding, and bead blasting, respectively. Three respirable aerosol samplers (including a 25-mm aluminum cyclone, nylon cyclone, and IOSH cyclone) were used side-by-side to collect samples from each selected workplace. For each collected sample, the uniformity of the deposition of respirable dusts on the filter was measured and its free silica content was determined by both the DOF XRD method and NIOSH 7500 XRD method (i.e., the reference method). A same trend in measured uniformities can be found in all selected workplaces: 25-mm aluminum cyclone>nylon cyclone>IOSH cyclone. Even for samples collected by the sampler with the highest uniformity (i.e., 25-mm aluminum cyclone), the use of the DOF XRD method would lead to the measured free silica concentrations 1.15-2.89 times in magnitude higher than that of the reference method. A new filter holder should be developed with the minimum uniformity comparable to that of NIOSH 7500 XRD method (=0.78) in the future. The use of conversion factors for correcting quartz concentrations obtained from the DOF XRD method based on the measured uniformities could be suitable for the foundry industry at this stage. 2009 Elsevier B.V. All rights reserved.

Magnetic and dielectric properties of Ca-substituted BiFeO3 nanoferrites by the sol-gel method.

PubMed

Lin, Jinpei; Guo, Zeping; Li, Mei; Lin, Qing; Huang, Kangling; He, Yun

2018-01-01

A multiferroic material can simultaneously show two or more basic magnetic properties, including ferromagnetism, antiferromagnetism, and ferroelectricity. BiFeO 3 is a multiferroic material with a rhombohedral distorted perovskite structure. Doping can reduce the volatility of Bi and greatly improve the magnetoelectric properties of BiFeO 3 . To investigate the influence of the doping content we used the following analytical methods: X-ray powder diffraction (XRD), scanning electron microscopy (SEM), microwave network analysis (PNA-N5244A), and the Superconducting Quantum Interference Device (Quantum Design MPMS) test. With the increase of Ca 2+ concentration in the solution, the grain size of Bi 1- x Ca x FeO 3 becomes smaller, showing the role of Ca 2+ ions as the dopant for fine grains. The calcination temperatures are the major causes for the saturated magnetization. The residual magnetization ( M r ) and the coercive force ( H c ) decrease linearly with the increase of x value, and due to the effect of Ca 2+ substitution at Bi 3+ sites, which causes the valence change of Fe and/or the oxygen vacancies. The XRD result indicates that the diffraction peak emerges with the increase of Ca 2+ and the main diffraction peak achieves a high angle. The best calcining temperature is 600 °C, and the morphology is very dependent on the calcining temperature.

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

X-Ray Diffraction Profile Analysis for Characterizing Isothermal Aging Behavior of M250 Grade Maraging Steel

NASA Astrophysics Data System (ADS)

Mahadevan, S.; Jayakumar, T.; Rao, B. P. C.; Kumar, Anish; Rajkumar, K. V.; Raj, Baldev

2008-08-01

X-ray diffraction (XRD) studies were carried out to characterize aging behavior of M250 grade maraging steel samples subjected to isothermal aging at 755 K for varying durations of 0.25, 1, 3, 10, 40, 70, and 100 hours. Earlier studies had shown typical features of precipitation hardening, wherein the hardness increased to a peak value due to precipitation of intermetallics and decreased upon further aging (overaging) due to reversion of martensite to austenite. Intermetallic precipitates, while coherent, are expected to increase the microstrain in the matrix. Hence, an attempt has been made in the present study to understand the microstructural changes in these samples using XRD line profile analysis. The anisotropic broadening with diffraction angle observed in the simple Williamson Hall (WH) plot has been addressed using the modified WH (mWH) approach, which takes into account the contrast caused by dislocations on line profiles, leading to new scaling factors in the WH plot. The normalized mean square strain and crystallite size estimated from mWH have been used to infer early precipitation and to characterize aging behavior. The normalized mean square strain has been used to determine the Avrami exponent in the Johnson Mehl Avrami (JMA) equation, which deals with the kinetics of precipitation. The Avrami exponent thus determined has matched well with values found by other methods, as reported in literature.

Effect of Annealing Temperature on Structural and Optical Properties of Sol-Gel-Derived ZnO Thin Films

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Vilarinho, Paula M.; Singh, Arun

2018-04-01

Nanocrystalline ZnO thin films were deposited on glass substrate via sol-gel dip-coating technique then annealed at 300°C, 400°C, and 500°C for 1 h. Their optical, structural, and morphological properties were studied using ultraviolet-visible (UV-Vis) spectrophotometry, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). XRD diffraction revealed that the crystalline nature of the thin films increased with increasing annealing temperature. The c-axis orientation improved, and the grain size increased, as indicated by increased intensity of the (002) plane peak at 2θ = 34.42° corresponding to hexagonal ZnO crystal. The average crystallite size of the thin films ranged from 13 nm to 23 nm. Increasing the annealing temperature resulted in larger crystallite size and higher crystallinity with increased surface roughness. The grain size according to SEM analysis was in good agreement with the x-ray diffraction data. The optical bandgap of the thin films narrowed with increasing annealing temperature, lying in the range of 3.14 eV to 3.02 eV. The transmission of the thin films was as high as 94% within the visible region. The thickness of the thin films was 400 nm, as measured by ellipsometry, after annealing at the different temperatures of 300°C, 400°C, and 500°C.

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.

Effect of Synthesis Parameter on Crystal Structures and Magnetic Properties of Magnesium Nickel Ferrite (Mg0.5Ni0.5Fe2O4) Nanoparticles

NASA Astrophysics Data System (ADS)

Maulia, R.; Putra, R. A.; Suharyadi, E.

2017-05-01

Mg0.5Ni0.5Fe2O4 nanoparticles have been successfully synthesized by using co-precipitation method and varying the synthesis parameter, i.e. synthesis temperature and NaOH concentration. X-ray Diffraction (XRD) pattern showed that nanoparticles have cubic spinel structures with an additional phase of γ-Fe2O3 and particle size varies within the range of 4.3 - 6.7 nm. This variation is due to the effect of various synthesis parameters. Transmission Electron Microscopy (TEM) image showed that the nanoparticles exhibited agglomeration. The observed diffraction ring from selected area electron diffraction showed that the sample was polycrystalline and confirmed the peak appearing in XRD. The coercivities showed an increasing trend with an increase in particle size from 44.7 Oe to 49.6 Oe for variation of NaOH concentration, and a decreasing trend with an increase in particle size from 46.8 to 45.1 Oe for variation of synthesis temperature. The maximum magnetization showed an increasing trend with an increase in the ferrite phase from 3.7 emu/g to 5.4 emu/g possessed in the sample with variations on NaOH concentration. The maximum magnetization for the sample with variations on synthesis temperature varied from 4.4 emu/g to 5.7 emu/g due to its crystal structures.

Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

PubMed

Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

2014-09-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. © International & American Associations for Dental Research.

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.

A new formulation of curcumin using poly (lactic-co-glycolic acid)—polyethylene glycol diblock copolymer as carrier material

NASA Astrophysics Data System (ADS)

Phuong Tuyen Dao, Thi; Hoai Nguyen, To; To, Van Vinh; Ho, Thanh Ha; Nguyen, Tuan Anh; Chien Dang, Mau

2014-09-01

The aim of this study is to fabricate a nanoparticle formulation of curcumin using a relatively new vehicle as the matrix polymer: poly(lactic-co-glycolic acid) (PLGA)- polyethylene glycol (PEG) diblock copolymer, and to investigate the effects of the various processing parameters on the characteristics of nanoparticles (NPs). We successfully synthesized the matrix polymer of PLGA-PEG by conjugation of PLGA copolymer with a carboxylate end group to a heterobifunctional amine-PEG-methoxy using N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as conjugation crosslinkers. The composition of the formed product (PLGA-PEG) was characterized with 500 MHz 1H nuclear magnetic resonance (NMR). The conjugation of PLGA-PEG was confirmed using Fourier transform infrared (FTIR) spectrum study. This diblock copolymer was then used to prepare the curcumin-loaded NPs through nanoprecipitation technique. With this method, we found that the size distribution depends on the type of solvent, the concentration of polymer and the concentration of surfactant. The particle size and size distribution were measured by dynamic light scattering (DLS). Transmission electron microscope (TEM) and scanning electron microscope (SEM) were used to confirm the size, structure and morphology of the successfully prepared NPs. All of our results showed that they are spherical and quite homologous with mean diameter around of 100-300 nm. Further, we evaluated encapsulation efficiency and some characteristics of NPs through high performance liquid chromatography (HPLC) analyses, zeta-potential measurements and x-ray diffraction studies. The HPLC analyses were performed to determine the amount of curcumin entrapped in NPs. The zeta-potential measurements confirmed the stability of NPs and the successful encapsulation of curcumin within NPs and the x-ray diffraction patterns showed the disordered-crystalline phase of curcumin inside the polymeric matrix.

Studies on rock characteristics and timing of creep at selected landslide sites in Taiwan

Treesearch

Cheng-Yi Lee

2000-01-01

A study was conducted to investigate the causes of and rock characteristics at three landslide sites in the Tesngwen Reservoir watershed of southern Taiwan. Research methods used included the petrographic microscope, X-ray diffraction (XRD), scanning electron microscope (SEM), inductively coupled plasma spectroscope (ICP), constant head permeameter in triaxial...

Characterization of liquefied wood residues from different liquefaction conditions

Treesearch

Hui Pan; Todd f. Shupe; Chung-Yun Hse

2007-01-01

The amount of wood residue is used as a measurement of the extent of wood liquefaction. Characterization of the residue from wood liquefaction provides a new approach to understand some fundamental aspects of the liquefaction reaction. Residues were characterized by wet chemical analyses, Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and...

Properties of a porous Ti-6Al-4V implant with a low stiffness for biomedical application.

PubMed

Li, X; Wang, C-T; Zhang, W-G; Li, Y-C

2009-02-01

Porous Ti-6Al-4V alloy was fabricated using the electron beam melting (EBM) process. The phases of the as-received powder and fabricated samples were characterized using X-ray diffraction (XRD) analysis. The XRD peaks of both diffraction patterns agree well, which indicated that the EBM process has not changed the composition of Ti-6Al-4V. The fabricated samples exhibited a Vickers microhardness value of around 428 HV. The compression and three-point bending tests were performed to evaluate the mechanical properties of the porous Ti-6Al-4V implant with a porosity of around 60 per cent. The compressive yield strength, Young's modulus, and ultimate compressive strength were 194.6 MPa, 4.25 GPa, and 222.6 MPa respectively. The bending stiffness and bending strength were 3.7 GPa and 126.3 MPa respectively. These results demonstrated that the porous Ti-6Al-4V implant with a low stiffness and high porosity could be a promising biomaterial for biomedical applications.

Photometric study of single-shot energy-dispersive x-ray diffraction at a laser plasma facility

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

Hoidn, O. R.; Seidler, G. T., E-mail: seidler@uw.edu

The low repetition rates and possible shot-to-shot variations in laser-plasma studies place a high value on single-shot diagnostics. For example, white-beam scattering methods based on broadband backlighter x-ray sources are used to determine changes in the structure of laser-shocked crystalline materials by the evolution of coincidences of reciprocal lattice vectors and kinematically allowed momentum transfers. Here, we demonstrate that white-beam techniques can be extended to strongly disordered dense plasma and warm dense matter systems where reciprocal space is only weakly structured and spectroscopic detection is consequently needed to determine the static structure factor and thus, the ion-ion radial distribution function.more » Specifically, we report a photometric study of energy-dispersive x-ray diffraction (ED-XRD) for structural measurement of high energy density systems at large-scale laser facilities such as OMEGA and the National Ignition Facility. We find that structural information can be obtained in single-shot ED-XRD experiments using established backlighter and spectrometer technologies.« less

Current-voltage characteristics of n-AlMgZnO/p-GaN junction diodes

NASA Astrophysics Data System (ADS)

Hsueh, Kuang-Po; Cheng, Po-Wei; Cheng, Yi-Chang; Sheu, Jinn-Kong; Yeh, Yu-Hsiang; Chiu, Hsien-Chin; Wang, Hsiang-Chun

2013-03-01

This study investigates the temperature dependence of the current-voltage (I-V) characteristics of Al-doped MgxZn1-xO/p-GaN junction diodes. Specifically, this study reports the deposition of n-type Al-doped MgxZn1-xO (AMZO) films on p-GaN using a radio-frequency (RF) magnetron sputtering system followed by annealing at 700, 800, 900, and 1000 °C in a nitrogen ambient for 60 seconds, respectively. The AMZO/GaN films were thereafter analyzed using Hall measurement and the x-ray diffraction (XRD) patterns. The XRD results show that the diffraction angles of the annealed AMZO films remain the same as that of GaN without shifting. The n-AMZO/p-GaN diode with 900 °C annealing had the lowest leakage current in forward and reverse bias. However, the leakage current of the diodes did not change significantly with an increase in annealing temperatures. These findings show that the n-AMZO/p-GaN junction diode is feasible for GaN-based heterojunction bipolar transistors (HBTs) and UV light-emitting diodes (LEDs).

Electroless Nickel Deposition for Front Side Metallization of Silicon Solar Cells

PubMed Central

Hsieh, Shu Huei; Hsieh, Jhong Min; Chen, Wen Jauh; Chuang, Chia Chih

2017-01-01

In this work, nickel thin films were deposited on texture silicon by electroless plated deposition. The electroless-deposited Ni layers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectroscopy (EDS), X-ray diffraction analysis (XRD), and sheet resistance measurement. The results indicate that the dominant phase was Ni2Si and NiSi in samples annealed at 300–800 °C. Sheet resistance values were found to correlate well with the surface morphology obtained by SEM and the results of XRD diffraction. The Cu/Ni contact system was used to fabricate solar cells by using two different activating baths. The open circuit voltage (Voc) of the Cu/Ni samples, before and after annealing, was measured under air mass (AM) 1.5 conditions to determine solar cell properties. The results show that open circuit voltage of a solar cell can be enhanced when the activation solution incorporated hydrofluoric acid (HF). This is mainly attributed to the native silicon oxide layer that can be decreased and/or removed by HF with the corresponding reduction of series resistance. PMID:28805724

Synthesis of nano-forsterite powder by making use of natural silica sand

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

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less

In-situ investigation of stress-induced martensitic transformation in Ti–Nb binary alloys with low Young's modulus [In-situ high-energy X-ray diffraction investigation on stress-induced martensitic transformation in Ti-Nb binary alloys

DOE PAGES

Chang, L. L.; Wang, Y. D.; Ren, Y.

2015-11-04

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated priormore » to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.« less

[Effects of annealing temperature on the structure and optical properties of ZnMgO films prepared by atom layer deposition].

PubMed

Sun, Dong-Xiao; Li, Jin-Hua; Fang, Xuan; Chen, Xin-Ying; Fang, Fang; Chu, Xue-Ying; Wei, Zhi-Peng; Wang, Xiao-Hua

2014-07-01

In the present paper, we report the research on the effects of annealing temperature on the crystal quality and optical properties of ZnMgO films deposited by atom layer deposition(ALD). ZnMgO films were prepared on quartz substrates by ALD and then some of the samples were treated in air ambient at different annealing temperature. The effects of annealing temperature on the crystal quality and optical properties of ZnMgO films were characterized by X-ray diffraction (XRD), photoluminescence (PL) and ultraviolet-visible (UV-Vis) absorption spectra. The XRD results showed that the crystal quality of ZnMgO films was significantly improved when the annealing temperature was 600 degrees C, meanwhile the intensity of(100) diffraction peak was the strongest. Combination of PL and UV-Vis absorption measurements showed that it can strongly promote the Mg content increasing in ZnMgO films and increase the band gap of films. So the results illustrate that suitable annealing temperature can effectively improve the crystal quality and optical properties of ZnMgO films.

Ni@Fe2O3 heterodimers: controlled synthesis and magnetically recyclable catalytic application for dehalogenation reactions

NASA Astrophysics Data System (ADS)

Nakhjavan, Bahar; Tahir, Muhammad Nawaz; Natalio, Filipe; Panthöfer, Martin; Gao, Haitao; Dietzsch, Michael; Andre, Rute; Gasi, Teuta; Ksenofontov, Vadim; Branscheid, Robert; Kolb, Ute; Tremel, Wolfgang

2012-07-01

Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants.Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr12121b

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

FTIR spectroscopic, thermal and XRD characterization of hydroxyapatite from new natural sources

NASA Astrophysics Data System (ADS)

Shaltout, Abdallah A.; Allam, Moussa A.; Moharram, Mohamed A.

2011-12-01

The inorganic constituents of 5 different plants (leaves and stalks) were investigated by using Fourier transformer infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal analysis including thermal gravimetric analysis (TGA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). These plants are Catha edulis (Khat), basil, mint, green tea and trifolium. The absorption bands of carbonate ions CO 32- was exhibited at 1446 cm -1, and the phosphate ions PO 43- was assigned at 1105 and 1035 cm -1. At high temperatures (600, 700 and 600 °C) further absorption bands of the phosphate ions PO 43- was assigned at the frequencies 572, 617, 962, 1043 and 1110 cm -1 and the vibrational absorption band of the carbonate ions CO 32- was assigned at 871, 1416 and 1461 cm -1. X-ray diffraction and thermal analysis confirm the obtained results of FITR. Results showed that the main inorganic constituents of C. edulis and basil leaves are hydroxyapatite whereas the hydroxyapatite content in the other plant samples is less than that in case of C. edulis and basil plant leaves.

Compaction and sintering behaviors of a Nd-Fe-B permanent magnet alloy

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

Chin, T.; Hung, M.; Tsai, D.

1988-11-15

Extensive x-ray diffraction (XRD) and magnetic measurements were done on Nd/sub 15/ Fe/sub 77/ B/sub 8/ magnet alloy green compacts after cold isostatic pressing following a pulsed 2-T field (CIP) and die-pressing under a static 1.2-T perpendicular field (DP1) or parallel field (DP2), and on those after sintering. An alignment factor F, through the calculation of the integrated diffraction intensity ratio of the XRD patterns, was adopted as the effectiveness of magnetic alignment. At the green compact state, DP1 has the best alignment while CIP the worst. However, after sintering the alignment factor was such that CIP>DPI>DP2, the same ordermore » as the magnetic properties. Three mechanisms were proposed for the evolution of the alignment factor at different stages of sintering, i.e., that both the appearance of a liquid phase at low temperatures and preferred grain growth at high temperatures enhance F, while recrystallization at intermediate temperatures deteriorates F. CIP results in less-defect green compact, hence less recrystallization, leading to better resultant alignment« less

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Luminescence study of ZnSe/PVA (polyvinyl alcohol) composite film

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

Lahariya, Vikas

The ZnSe nanocrystals have been prepared into poly vinyl alcohol(PVA) polymer matrix on glass using ZnCl2 and Na2SeSO3 as zinc and selenium source respectively. Poly vinyl Alcohol (PVA) used as polymer matrix cum capping agent due to their high viscosity and water solubility. It is transparent for visible region and prevents Se- ions to photo oxidation. The ZnSe/PVA composite film was deposited on glass substrate. The film was characterized by X Ray Diffraction (XRD) and UV-Visible absorption Spectroscopy and Photoluminescence. The X Ray Diffraction (XRD) study confirms the nanometer size (10 nm) particle formation within PVA matrix with cubic zinc blendmore » crystal structure. The UV-Visible Absorption spectrum of ZnSe/PVA composite film shown blue shift in absorption edge indicating increased band gap due to quantum confinement. The calculated energy band gap from the absorption edge using Tauc relation is 3.4 eV. From the Photoluminescence study a broad peak at 435 nm has been observed in violet blue region due to recombination of surface states.« less

Crystallographic texture and earing behavior analysis for different second cold reductions of double-reduction tinplate

NASA Astrophysics Data System (ADS)

Liao, Lu-hai; Zheng, Xiao-fei; Kang, Yong-lin; Liu, Wei; Yan, Yan; Mo, Zhi-ying

2018-06-01

Since the production of tinplate with non-earing properties is difficult, especially when it is produced via the double-reduction process, the optimal degree of second cold reduction is particularly important for achieving desirable drawing properties. The evolution of texture and the earing propensity of double-reduction tinplate with different extents of second reduction were investigated in this study. Optical microscopy and scanning electron microscopy were used to observe the changes in the microstructure at various extents of reduction. Two common testing methods, X-ray diffraction (XRD) and electron backscatter diffraction, were used to investigate the texture of the specimens, which revealed the effects of deformation percentage on the final texture development and the change in the grain boundary. The earing rate was determined via earing tests involving measurement of the height of any ear. The results obtained from both XRD analyses and earing tests revealed the same ideal value for the second cold reduction on the basis of the relationship between crystallographic texture and the degree of earing.

Resonant x-ray diffraction revealing chemical disorder in sputtered L10 FeNi on Si(0 0 1)

NASA Astrophysics Data System (ADS)

Frisk, Andreas; Lindgren, Bengt; Pappas, Spiridon D.; Johansson, Erik; Andersson, Gabriella

2016-10-01

In the search for new rare earth free permanent magnetic materials, FeNi with a L10 structure is a possible candidate. We have synthesized the phase in the thin film form by sputtering onto HF-etched Si(0 0 1) substrates. Monatomic layers of Fe and Ni were alternately deposited on a Cu buffer layer, all of which grew epitaxially on the Si substrates. A good crystal structure and epitaxial relationship was confirmed by in-house x-ray diffraction (XRD). The chemical order, which to some part is the origin of an uniaxial magnetic anisotropy, was measured by resonant XRD. The 0 0 1 superlattice reflection was split in two symmetrically spaced peaks due to a composition modulation of the Fe and Ni layers. Furthermore the influence of roughness induced chemical anti-phase domains on the RXRD pattern is exemplified. A smaller than expected magnetic uniaxial anisotropy energy was obtained, which is partly due to the composition modulations, but the major reason is concluded to be the Cu buffer surface roughness.

Resonant x-ray diffraction revealing chemical disorder in sputtered L10 FeNi on Si(0 0 1).

PubMed

Frisk, Andreas; Lindgren, Bengt; Pappas, Spiridon D; Johansson, Erik; Andersson, Gabriella

2016-10-12

In the search for new rare earth free permanent magnetic materials, FeNi with a L10 structure is a possible candidate. We have synthesized the phase in the thin film form by sputtering onto HF-etched Si(0 0 1) substrates. Monatomic layers of Fe and Ni were alternately deposited on a Cu buffer layer, all of which grew epitaxially on the Si substrates. A good crystal structure and epitaxial relationship was confirmed by in-house x-ray diffraction (XRD). The chemical order, which to some part is the origin of an uniaxial magnetic anisotropy, was measured by resonant XRD. The 0 0 1 superlattice reflection was split in two symmetrically spaced peaks due to a composition modulation of the Fe and Ni layers. Furthermore the influence of roughness induced chemical anti-phase domains on the RXRD pattern is exemplified. A smaller than expected magnetic uniaxial anisotropy energy was obtained, which is partly due to the composition modulations, but the major reason is concluded to be the Cu buffer surface roughness.

Ultrathin Cr added Ru film as a seedless Cu diffusion barrier for advanced Cu interconnects

NASA Astrophysics Data System (ADS)

Hsu, Kuo-Chung; Perng, Dung-Ching; Yeh, Jia-Bin; Wang, Yi-Chun

2012-07-01

A 5 nm thick Cr added Ru film has been extensively investigated as a seedless Cu diffusion barrier. High-resolution transmission electron microscopy micrograph, X-ray diffraction (XRD) pattern and Fourier transform-electron diffraction pattern reveal that a Cr contained Ru (RuCr) film has a glassy microstructure and is an amorphous-like film. XRD patterns and sheet resistance data show that the RuCr film is stable up to 650 °C, which is approximately a 200 °C improvement in thermal stability as compared to that of the pure Ru film. X-ray photoelectron spectroscopy depth profiles show that the RuCr film can successfully block Cu diffusion, even after a 30-min 650 °C annealing. The leakage current of the Cu/5 nm RuCr/porous SiOCH/Si stacked structure is about two orders of magnitude lower than that of a pristine Ru sample for electric field below 1 MV/cm. The RuCr film can be a promising Cu diffusion barrier for advanced Cu metallization.

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders.

PubMed

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-08-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

Surfactant Mediated Growth of Co on MgO(111)

NASA Astrophysics Data System (ADS)

Johnson-Steigelman, H. Trevor; Parihar, Somendra S.; Lyman, Paul F.

2010-03-01

Monolayer films of Co were deposited using an electrostatic electron-beam evaporator on single-crystal MgO(111)- √3 x√3 R 30^o substrates held at room temperature, with subsequent annealing of temperatures 400 C to 800 C. These films were characterized using low-energy electron diffraction (LEED), x-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and x-ray diffraction (XRD). After short anneals of 400 C, AFM, LEED, and XPS suggest that islanding has occurred at the surface. XPS and XRD indicate the presence of elemental Co. 1-2 ML films of Ag were examined as a potential surfactant to aid in the growth of smooth Co films. Despite the fact that Ag itself formed islands, it was found that the presence of Ag did have a surfactant effect upon the thin-film growth of Co on Ag/MgO(111)- √3 x√3 R 30^o. Co islands were still present, but much more smooth than islands formed without Ag. XPS and AFM suggest strongly that Ag floated to the top of these samples at temperatures above 400 ^oC.

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.

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

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

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

Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis.

PubMed

Habibi, Neda

2015-02-05

The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the NCH3 functional group about 2850cm(-1) is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Green synthesis of gold and silver nanoparticles using Hibiscus rosa sinensis

NASA Astrophysics Data System (ADS)

Philip, Daizy

2010-03-01

Biological synthesis of gold and silver nanoparticles of various shapes using the leaf extract of Hibiscus rosa sinensis is reported. This is a simple, cost-effective, stable for long time and reproducible aqueous room temperature synthesis method to obtain a self-assembly of Au and Ag nanoparticles. The size and shape of Au nanoparticles are modulated by varying the ratio of metal salt and extract in the reaction medium. Variation of pH of the reaction medium gives silver nanoparticles of different shapes. The nanoparticles obtained are characterized by UV-vis, transmission electron microscopy (TEM), X-ray diffraction (XRD) and FTIR spectroscopy. Crystalline nature of the nanoparticles in the fcc structure are confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes, bright circular spots in the selected area electron diffraction (SAED) and clear lattice fringes in the high-resolution TEM image. From FTIR spectra it is found that the Au nanoparticles are bound to amine groups and the Ag nanoparticles to carboxylate ion groups.

X-ray diffraction and TGA kinetic analyses for chemical looping combustion applications.

PubMed

Tijani, Mansour Mohammedramadan; Aqsha, Aqsha; Mahinpey, Nader

2018-04-01

Synthesis and characterization of supported metal-based oxygen carriers were carried out to provide information related to the use of oxygen carriers for chemical looping combustion processes. The Cu, Co, Fe, Ni metals supported with Al 2 O 3 , CeO 2 , TiO 2 , ZrO 2 were prepared using the wetness impregnation technique. Then, the X-ray Diffraction (XRD) characterization of oxidized and reduced samples was obtained and presented. The kinetic analysis using Thermogravimetric analyzer (TGA) of the synthesized samples was conducted. The kinetics of reduction reaction of all samples were estimated and explained.

Structural properties of alkaline sodium lead fluoride borate glasses incorporated with Praseodymium ion

NASA Astrophysics Data System (ADS)

Lenkennavar, Susheela K.; Madhu, A.; Eraiah, B.; Kokila, M. K.

2018-05-01

The effect of different alkaline and Pr ions on the density and structure of Na2O-PbO-MO-B2O3 (M represents Ba/Ca/Sr) has been investigated using X-ray diffraction (XRD), infrared spectrophotometer (FTIR). The amorphous phase has been identified based on X-ray diffraction analysis. The Praseodymium oxide plays the role as a glass-modifier and influences on BO3↔BO4 conversion. The same effect is also observed in density and molar volume variation due to non bridging oxygen's (NBO) created when BO3 units are converted.

Structural analysis of aluminium substituted nickel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh, H. S.; Sangwa, Neha

2018-05-01

Aluminium substituted nickel ferrite nanoparticles were synthesized by High Energy Ball milling (HEBM) of the mixture of α-NiO, α-Al2O3 and α-Fe2O3 followed by annealing at 1000˚C. X-ray diffraction (XRD) and Energy dispersive spectroscopy analysis (EDS) characterization was done for Aluminium substituted nickel ferrite. The structural analysis reveals the formation of the single phase compound. The average grain size was estimated by X-ray diffraction technique ranges from 30 to 10 nm with the increasing concentration of Aluminium. EDS spectra conforms the homogeneous mixing and purity of ferrite.

Nano modification of NZVI with an aquatic plant Azolla filiculoides to remove Pb(II) and Hg(II) from water: Aging time and mechanism study.

PubMed

Arshadi, M; Abdolmaleki, M K; Mousavinia, F; Foroughifard, S; Karimzadeh, A

2017-01-15

This paper reports the preparation and stabilization of nano zero valent iron (NZVI) on a modified aquatic plant, Azolla filiculoides, and investigates its potential for the adsorption/reduction of Pb(II) and Hg(II) ions from aqueous media even after six months of storage in the lab condition. XRD, TEM and zeta potential results demonstrated that the Azolla-NaOH could be a good stabilizer of aged NZVI (six months) and the green support suppressed the oxidation and aggregation of immobilized NZVI. Kinetic and equilibrium models for lead and mercury ions uptake were developed by considering the effect of the initial Pb(II) and Hg(II) concentrations, contact time, adsorbent dosage, initial pH and effect of temperature. The contact time to obtain equilibrium for maximum uptake by Azolla-OH-NZVI was 20min. The removal of toxic metal ions has been monitored in terms of pseudo-first- and -second-order kinetics, and the Freundlich and Langmuir isotherms models have also been utilized to the equilibrium uptake results. The uptake kinetics followed the mechanism of the pseudo-second-order equation for all systems studied, confirming chemical sorption as the rate-limiting step of adsorption mechanisms and not involving a mass transfer in solution. The thermodynamic results confirmed that the uptake of Pb(II) and Hg(II) ions were feasible, spontaneous and endothermic at 25-80°C. XRD and zeta potential data displayed the existence of Pb(0) and Hg(0) on the Azolla-OH-NZVI surface. The nanobioadsorbent revealed high recyclability due to its reasonable uptake efficiency after 7th adsorption-desorption cycles. The proposed nano biocomposite could also be utilized to uptake Pb(II) and Hg(II) ions from the real water (Anzali lagoon water). However, coated NZVI with Azolla filiculoides as a green and environmentally friendly support suppressed rapid oxidation and aggregation of the immobilized NZVI, therefore vastly enhancing the probability of environmental transport and reducing the sedimentation and potential for toxicity. Copyright © 2016 Elsevier Inc. All rights reserved.

Sound velocity measurements of dhcp-FeHx up to 70 GPa using inelastic X-ray scattering: Implications for the abundance of hydrogen in the Earth's core

NASA Astrophysics Data System (ADS)

Shibazaki, Y.; Ohtani, E.; Fukui, H.; Sakai, T.; Kamada, S.; Baron, A. Q.; Nishitani, N.; Hirao, N.; Takemura, K.

2011-12-01

The Earth's interior has been directly investigated by seismic wave propagation and normal mode oscillation. In particular, the distributions of density and sound velocity are available to study the Earth's core (e.g. PREM). The inner core, which is solid state, is approximately 3 % less dense than pure iron (a core density deficit), and it is considered that the core consists of iron and light elements, such as hydrogen, carbon, oxygen, silicon, and sulfur. In this work, in order to constrain the abundance of hydrogen in the Earth's core by matching the density and sound velocity of FeHx to those of PREM, we determined the compressional sound velocity of iron hydride at high pressure using inelastic X-ray scattering (IXS). The IXS experiments and in situ X-ray diffraction (XRD) experiments were conducted up to 70 GPa and room temperature. High-pressure conditions were generated using a symmetric diamond anvil cell (DAC) with tungsten gaskets. Hydrogen initially pressurized to 0.18 GPa was loaded to the sample chamber. The IXS experiments were performed at BL35XU of the SPring-8 facility in Japan. The XRD experiments at high pressure were carried out by the angle dispersive method at BL10XU of the SPring-8 facility in Japan. The each XRD pattern of FeHx was collected after each IXS measurement in order to obtain directly the density of FeHx. Over the range of pressure studied, the diffraction lines of double-hexagonal close-packed (dhcp)-FeHx were observed and there were no diffraction lines of iron. We show that FeHx follows Birch's law for Vp above 37 GPa, namely a linear dependence between velocity and density. The estimated Vp, extrapolated to core conditions, is compared with PREM. Our results provide that the Earth's inner core could contain about 0.2 wt% hydrogen.

MUDMASTER: A Program for Calculating Crystalline Size Distributions and Strain from the Shapes of X-Ray Diffraction Peaks

USGS Publications Warehouse

Eberl, D.D.; Drits, V.A.; Środoń, Jan; Nüesch, R.

1996-01-01

Particle size may strongly influence the physical and chemical properties of a substance (e.g. its rheology, surface area, cation exchange capacity, solubility, etc.), and its measurement in rocks may yield geological information about ancient environments (sediment provenance, degree of metamorphism, degree of weathering, current directions, distance to shore, etc.). Therefore mineralogists, geologists, chemists, soil scientists, and others who deal with clay-size material would like to have a convenient method for measuring particle size distributions. Nano-size crystals generally are too fine to be measured by light microscopy. Laser scattering methods give only average particle sizes; therefore particle size can not be measured in a particular crystallographic direction. Also, the particles measured by laser techniques may be composed of several different minerals, and may be agglomerations of individual crystals. Measurement by electron and atomic force microscopy is tedious, expensive, and time consuming. It is difficult to measure more than a few hundred particles per sample by these methods. This many measurements, often taking several days of intensive effort, may yield an accurate mean size for a sample, but may be too few to determine an accurate distribution of sizes. Measurement of size distributions by X-ray diffraction (XRD) solves these shortcomings. An X-ray scan of a sample occurs automatically, taking a few minutes to a few hours. The resulting XRD peaks average diffraction effects from billions of individual nano-size crystals. The size that is measured by XRD may be related to the size of the individual crystals of the mineral in the sample, rather than to the size of particles formed from the agglomeration of these crystals. Therefore one can determine the size of a particular mineral in a mixture of minerals, and the sizes in a particular crystallographic direction of that mineral.

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

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

Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.

2014-01-01

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrationalmore » and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.« less

Morphology and thermal studies of zinc sulfide and cadmium sulfide nanoparticles in polyvinyl alcohol matrix

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2016-09-01

Zn(II) and Cd(II) metal complexes of 1-cyano-1-carboethoxyethylene-2,2-dithiolato-κS,S'-bis(N,N-dimethylthiourea-κS) have been synthesized and characterized with analytical and spectroscopic techniques. The complexes were thermolysed in hexadecylamine at 200 °C to prepare ZnS and CdS nanoparticles. The nanoparticles were characterized with scanning electron microscope (SEM), transmission electron microscope (TEM), and powder X-ray diffraction (p-XRD). TEM images showed spherically shaped nanoparticles, whose sizes are in the range 4.33-7.21 nm for ZnS and 4.95-7.7 nm CdS respectively and XRD confirmed cubic crystalline phases for the nanoparticles. The optical band gap energy evaluated from the absorption spectra are 2.88 eV (430 nm) and 2.81 eV (440 nm) for the ZnS and CdS nanoparticles respectively. The as-prepared metal sulfide nanoparticles were further incorporated into polyvinyl alcohol (PVA) to give ZnS/PVA and CdS/PVA composites. The polymer nanocomposites were studied to investigate their morphology and thermal properties relative to the pure PVA. XRD diffractions indicated that the crystalline phases of the nanoparticles and the sizes in PVA matrices remained unaltered. Infra-red spectra studies revealed interactions between the PVA and the metal sulfide nanoparticles and TGA studies show that the ZnS/PVA and CdS/PVA nanocomposites exhibit better thermal stability than the pure PVA.

Ion-pairing in aqueous CaCl 2 and RbBr solutions. Simultaneous structural refinement of XAFS and XRD data

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

Pham, Thai V.; Fulton, John L.

2013-01-22

We present a new methodology involving the simultaneous refinement of both x-ray absorption and x-ray diffraction spectra (X-ray Absorption/Diffraction Structural Refinement,XADSR), to study hydration and ion pair structure of CaCl 2 and RbBr salts in concentrated aqueous solutions. The XADSR analysis includes the XAFS spectra analysis of both the cation and anion as a probe of their short-range structure with an XRD spectral analysis as a probe of the global structural. Together they deliver a comprehensive picture of the cation and anion hydration, the contact ion pair (CIP) structure and the solvent-separated ion pair (SSIP) structure. XADSR analysis of 6.0more » m aqueous CaCl 2 reveals that there are an insignificant number of Ca 2+-Cl- CIP’s, but there are approximately 3.4 SSIP’s separated by about 4.99 Å. In contrast XADSR analysis of aqueous RbBr yields about 0.7 pair CIP at a bond length 3.51 Å. The present work demonstrates a new approach for a direct co-refinement of XRD and XAFS spectra in a simple and reliable fashion, opening new opportunities for analysis in various disordered and crystalline systems. This work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences and Biosciences. Pacific Northwest National Laboratory (PNNL) is operated for the U.S. Department of Energy by Battelle.« less

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.

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury

PubMed Central

Li, Cen; Yang, Hongxia; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao

2016-01-01

Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

PubMed

Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

2016-01-01

Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

Fabrication, characterization and bioevaluation of silibinin loaded chitosan nanoparticles.

PubMed

Pooja, Deep; Babu Bikkina, Dileep J; Kulhari, Hitesh; Nikhila, Nalla; Chinde, Srinivas; Raghavendra, Y M; Sreedhar, B; Tiwari, Ashok K

2014-08-01

Silibinin is reported to possess multiple biological activities. However, its hydrophobic nature limits its bioavailability compromising in vivo biological activities. Nanoparticles-based delivery of such molecules has emerged as new technique to resolve these issues. Bio-degradable, compatible and adhesive nature of chitosan has recently attracted its suitability as a carrier for biologically active molecules. This study presents fabrication and characterization of chitosan-tripolyphosphate based encapsulation of silibinin. Various preparations of silibinin encapsulated chitosan-tripolyphosphate nanoparticles were studied for particle size, morphology, zeta-potential, and encapsulation efficiencies. Preparations were also evaluated for cytotoxic activities in vitro. The optimized silibinin loaded chitosan nanoparticles were of 263.7±4.1nm in particle size with zeta potential 37.4±1.57mV. Nanoparticles showed high silibinin encapsulation efficiencies (82.94±1.82%). No chemical interactions between silibinin and chitosan were observed in FTIR analysis. Powder X-ray diffraction analysis revealed transformed physical state of silibinin after encapsulation. Surface morphology and thermal behaviour were determined using TEM and DSC analysis. Encapsulated silibinin displayed increased dissolution and better cytotoxicity against human prostate cancer cells (DU145) than silibinin alone. Copyright © 2014 Elsevier B.V. All rights reserved.

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

Activation-induced proteolysis of cytoplasmic domain of zeta in T cell receptors and Fc receptors.

PubMed

Taupin, J L; Anderson, P

1994-12-01

The CD3-T cell receptor (TCR) complex on T cells and the Fc gamma receptor type III (Fc gamma RIII)-zeta-gamma complex on natural killer cells are functionally analogous activation receptors that associate with a family of disulfide-linked dimers composed of the related subunits zeta and gamma. Immunochemical analysis of receptor complexes separated on two-dimensional diagonal gels allowed the identification of a previously uncharacterized zeta-p14 heterodimer. zeta-p14 is a component of both CD3-TCR and Fc gamma RIII-zeta-gamma. Peptide mapping analysis shows that p14 is structurally related to zeta, suggesting that it is either: (i) derived from zeta proteolytically or (ii) the product of an alternatively spliced mRNA. The observation that COS cells transformed with a cDNA encoding zeta express zeta-p14 supports the former possibility. The expression of CD3-TCR complexes including zeta-p14 increases following activation with phorbol 12-myristate 13-acetate or concanavalin A, suggesting that proteolysis of zeta may contribute to receptor modulation or desensitization.

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

Synthesis of platinum nanoparticles using seaweed Padina gymnospora and their catalytic activity as PVP/PtNPs nanocomposite towards biological applications.

PubMed

Ramkumar, V Sri; Pugazhendhi, A; Prakash, S; Ahila, N K; Vinoj, G; Selvam, S; Kumar, G; Kannapiran, E; Rajendran, R Babu

2017-08-01

In the recent years, synthesis of nanomaterials using seaweeds and their diverse applications is escalating research in modern era. Among the noble metals, platinum nanoparticles (PtNPs) are of great importance owing to their catalytic property and less toxicity. The significance of this work is a simple one-step synthesis of PtNPs using aqueous extract of Indian brown seaweed Padina gymnospora and their catalytic activity with a polymer Polyvinylpyrrolidone (PVP) as PVP/PtNPs nanocomposite towards antimicrobial, haemolytic, cytotoxic (Artemia salina) and antioxidant properties. Fourier Transform Infrared (FT-IR) spectrum results showed diversified functional groups (biomoeities such as carbohydrates and proteins) present in the seaweed extract is responsible for the reduction of platinum ions (Pt + ) to PtNPs. The seaweed mediated PtNPs was characterized by UV-vis spectrophotometer, X-ray diffraction (XRD) pattern, Field Emission Scanning Electron Microscopy (FESEM) equipped with Energy Dispersive X-ray (EDX) spectroscopy and High Resolution Transmission Electron Microscopy (HRTEM) analysis. The synthesized PtNPs was found to be truncated octahedral in shape with the range of 5-50nm. Crystalline nature of the nanoparticles was evidenced by Selected Area Electron Diffraction (SAED) pattern with bright circular spots corresponding to (111), (200), (220) and (311) Bragg's reflection planes. The size of the PtNPs was further evidenced by Dynamic Light Scattering (DLS) analysis and it is originate to be stable at -22.5mV through Zeta Potential (ZP) analysis. The present study shows that the catalytic behavior of PtNPs as polymer/metal nanocomposite (PVP/PtNPs) preparation for an antibacterial activity against seven disease causing pathogenic bacterial strains with the maximum activity against Escherichia coli (15.6mm) followed by Lactococcus lactis (14.8mm) and Klebsiella pneumoniae (14.4mm). But no haemolytic activity was seen at their effective bactericidal concentration, whereas increase in the haeomyltic activity was seen only in higher concentrations (600, 900 and 1200μgmL -1 ). On the other hand, PVP/PtNPs nanocomposite has shown cytotoxic activity at 100±4μgmL -1 (LC 50 ) against Artemia salina nauplii. Furthermore, PVP/PtNPs nanocomposite showed an enhanced scavenging activity against 2,2-diphenyl-1-picrylhydrazyl (DPPH), superoxide, nitric oxide and hydroxyl radicals. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Generation of drugs coated iron nanoparticles through high energy ball milling

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

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

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

Structural and chemical ordering of Heusler C o x M n y G e z epitaxial films on Ge (111): Quantitative study using traditional and anomalous x-ray diffraction techniques

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

Collins, B. A.; Chu, Y. S.; He, L.

2015-12-01

Epitaxial films of CoxMnyGez grown on Ge (111) substrates by molecular-beam-epitaxy techniques have been investigated as a continuous function of composition using combinatorial synchrotron x-ray diffraction (XRD) and x-ray fluorescence (XRF) spectroscopy techniques. A high-resolution ternary epitaxial phase diagram is obtained, revealing a small number of structural phases stabilized over large compositional regions. Ordering of the constituent elements in the compositional region near the full Heusler alloy Co2MnGe has been examined in detail using both traditional XRD and a new multiple-edge anomalous diffraction (MEAD) technique. Multiple-edge anomalous diffraction involves analyzing the energy dependence of multiple reflections across each constituent absorptionmore » edge in order to detect and quantify the elemental distribution of occupation in specific lattice sites. Results of this paper show that structural and chemical ordering are very sensitive to the Co : Mn atomic ratio, such that the ordering is the highest at an atomic ratio of 2 but significantly reduced even a few percent off this ratio. The in-plane lattice is nearly coherent with that of the Ge substrate, while the approximately 2% lattice mismatch is accommodated by the out-of-plane tetragonal strain. The quantitative MEAD analysis further reveals no detectable amount (< 0.5%) of Co-Mn site swapping, but instead high levels (26%) of Mn-Ge site swapping. Increasing Ge concentration above the Heusler stoichiometry (Co0.5Mn0.25Ge0.25) is shown to correlate with increased lattice vacancies, antisites, and stacking faults, but reduced lattice relaxation. The highest degree of chemical ordering is observed off the Heusler stoichiometry with a Ge enrichment of 5 at.%.« less

Quantification of local strain distributions in nanoscale strained SiGe FinFET structures

NASA Astrophysics Data System (ADS)

Mochizuki, Shogo; Murray, Conal E.; Madan, Anita; Pinto, Teresa; Wang, Yun-Yu; Li, Juntao; Weng, Weihao; Jagannathan, Hemanth; Imai, Yasuhiko; Kimura, Shigeru; Takeuchi, Shotaro; Sakai, Akira

2017-10-01

Strain within nanoscale strained SiGe FinFET structures has been investigated using a combination of X-ray diffraction and transmission electron microscopy-based nanobeam diffraction (NBD) techniques to reveal the evolution of the stress state within the FinFETs. Reciprocal space maps collected using high-resolution X-ray diffraction exhibited distinct features corresponding to the SiGe fin width, pitch, and lattice deformation and were analyzed to quantify the state of stress within the fins. Although the majority of the SiGe fin volume exhibited a uniaxial stress state due to elastic relaxation of the transverse in-plane stress, NBD measurements confirmed a small interaction region near the SOI interface that is mechanically constrained by the underlying substrate. We have quantitatively characterized the evolution of the fin stress state from biaxial to uniaxial as a function of fin aspect ratio and Ge fraction and confirmed that the fins obey elastic deformation based on a model that depends on the relative difference between the equilibrium Si and SiGe lattice constants and relative fraction of in-plane stress transverse to the SiGe fins. Spatially resolved, nanobeam X-ray diffraction measurements conducted near the SiGe fin edge indicate the presence of additional elastic relaxation from a uniaxial stress state to a fully relaxed state at the fin edge. Mapping of the lattice deformation within 500 nm of this fin edge by NBD revealed large gradients, particularly at the top corner of the fin. The values of the volume averaged lattice deformation obtained by nanoXRD and NBD are qualitatively consistent. Furthermore, the modulation of strain at the fin edge obtained by quantitative analysis of the nanoXRD results agrees with the lattice deformation profile obtained by NBD.

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.

OMVPE Growth of Quaternary (Al,Ga,In)N for UV Optoelectronics (title change from A)

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

HAN,JUNG; FIGIEL,JEFFREY J.; PETERSEN,GARY A.

We report the growth and characterization of quaternary AlGaInN. A combination of photoluminescence (PL), high-resolution x-ray diffraction (XRD), and Rutherford backscattering spectrometry (RBS) characterizations enables us to explore the contours of constant PL peak energy and lattice parameter as functions of the quaternary compositions. The observation of room temperature PL emission at 351nm (with 20% Al and 5% In) renders initial evidence that the quaternary could be used to provide confinement for GaInN (and possibly GaN). AlGaInN/GrdnN MQW heterostructures have been grown; both XRD and PL measurements suggest the possibility of incorporating this quaternary into optoelectronic devices.

Synthesis of kaolinite-filled EPDM rubber composites by solution intercalation: structural characterization and studies on mechanical properties

NASA Astrophysics Data System (ADS)

Ginil Mon, S.; Jaya Vinse Ruban, Y.; Vetha Roy, D.

2011-09-01

In the large field of nanotechnology, polymer matrix-based nanocomposites have become a prominent area of current research and development. Exfoliated clay-based nanocomposites have dominated the polymer world with excellent characteristics. EPDM rubber composites have been synthesized by solution-intercalation using the easily available kaolinite as filler. The composite structure has been elucidated by X-ray diffraction (XRD), Fourier transform IR, and scanning electron microscope studies. The molecular level dispersion of clay layers has been verified by the disappearance of basal XRD peak of kaolinite in the EPDM/kaolinite composites. The mechanical properties showed significant improvement of EPDM/kaolinite composites with respect to neat EPDM.

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.

Single step synthesis of nanostructured boron nitride for boron neutron capture therapy

NASA Astrophysics Data System (ADS)

Singh, Bikramjeet; Singh, Paviter; Kumar, Manjeet; Thakur, Anup; Kumar, Akshay

2015-05-01

Nanostructured Boron Nitride (BN) has been successfully synthesized by carbo-thermic reduction of Boric Acid (H3BO3). This method is a relatively low temperature synthesis route and it can be used for large scale production of nanostructured BN. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA). XRD analysis confirmed the formation of single phase nanostructured Boron Nitride. SEM analysis showed that the particles are spherical in shape. DTA analysis showed that the phase is stable upto 900 °C and the material can be used for high temperature applications as well boron neutron capture therapy (BNCT).

The photoluminescent properties of Y2O3:Bi3+, Eu3+, Dy3+ phosphors for white-light-emitting diodes.

PubMed

Han, Xiumei; Feng, Xu; Qi, Xiwei; Wang, Xiaoqiang; Li, Mingya

2014-05-01

Bi3+, Eu3+, Dy3+ activated Y2O3 phosphors were prepared through the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, and photoluminescence (PL) spectra were used to characterize the resulting phosphors. The XRD patterns show the refined crystal structure of Y2O3. The energy transfer processes of Bi(3+)-Eu3+ occurred in the host lattices. The thermal stability of Y2O3:Bi3+, Eu3+, Dy3+ phosphors was studied. Under short wavelength UV excitation, the phosphors show excellent characteristic red, blue, and yellow emission with medium intensity.

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

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

Winterrose, M.; Lucas, M; Yue, A

Synchrotron x-ray diffraction (XRD) measurements, nuclear forward scattering (NFS) measurements, and density functional theory (DFT) calculations were performed on L12-ordered Pd3Fe. Measurements were performed at 300 K at pressures up to 33 GPa, and at 7 GPa at temperatures up to 650 K. The NFS revealed a collapse of the 57Fe magnetic moment between 8.9 and 12.3 GPa at 300 K, coinciding with a transition in bulk modulus found by XRD. Heating the sample under a pressure of 7 GPa showed negligible thermal expansion from 300 to 523 K, demonstrating Invar behavior. Zero-temperature DFT calculations identified a ferromagnetic ground statemore » and showed several antiferromagnetic states had comparable energies at pressures above 20 GPa.« less

The Synthesis and Photoluminescent Properties of CaMoO₄:Eu³⁺ Nanocrystals by a Soft Chemical Route.

PubMed

Li, Fuhai; Yu, Lixin; Sun, Jiaju; Li, Songchu; Wei, Shuilin

2017-04-01

In this paper, the CaMoO4:Eu3+ phosphors were prepared by a simple hydrothermal method assisted by the citric acid as the surfactant, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and fluorescent spectrophotometry. The results of XRD show that the as-prepared samples are single phase. The process of the Ostwald ripening is controlled by the content of the citric acid in the hydrothermal reaction. The pH value of the precursor affects the shift of the charge transition band (CTB) in the excitation spectra. The reaction condition can strongly affect the luminescent intensity of the samples.

Nano sized La2Co2O6 double perovskite synthesized by sol gel method

NASA Astrophysics Data System (ADS)

Solanki, Neha; Lodhi, Pavitra Devi; Choudhary, K. K.; Kaurav, Netram

2018-05-01

We report here the synthesis of double perovskite La2Co2O6 (LCO) compound by a sol gel route method. The double perovskite structure of LCO system was confirmed via X-ray diffraction (XRD) analysis. Further, the lattice parameter, unit cell volume and bond length were refined by means of rietveld analysis using the full proof software. Debye Scherer formula was used to determine the particle size. The compound crystallized in triclinic structure with space group P-1 in ambient condition. We also obtained Raman modes from XRD spectra of poly-crystalline LCO sample. These results were interpreted for the observation of phonon excitations in this compound.

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

Structural, optical and dielectric properties of pure and chromium (Cr) doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmed, Arham S.

2018-05-01

The pure and Cr doped nickel oxide (NiO) nanoparticles have been synthesized by cost effective co-precipitation method having nickel nitrate as initial precursor. The synthesized samples were characterized by X-Ray diffraction (XRD), UV-Visible Spectroscopy(UV-Vis) and LCR meter for structural, optical and dielectric properties respectively. The crystallite size of pure nickel oxide nanoparticles characterized by XRD using Debye Scherer's formula was found to be 21.7nm and the same decreases on increasing Cr concentration whereas optical and dielectric properties were analyzed by UV-Vis and LCR meter respectively. The energy band gaps were determined by UV-Vis using Tauc relation.

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

PubMed Central

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

Fabrication of high-k dielectric Calcium Copper Titanate (CCTO) target by solid state route

NASA Astrophysics Data System (ADS)

Tripathy, N.; Das, K. C.; Ghosh, S. P.; Bose, G.; Kar, J. P.

2016-02-01

CaCu3Ti4O12 (CCTO) ceramic pellet of 10mm diameter has been synthesized by adopting solid state route. The structural and morphological characterization of the ceramics sample was carried out by X-ray diffraction (XRD) and scanning electron microscope (SEM), respectively. XRD pattern revealed the CCTO phase formation, where as SEM micrograph shows the sample consisting of well defined grain and grain boundaries. The room temperature dielectric constant of the sample was found to be ∼ 5000 at 1kHz. After successful preparation of CCTO pellet, a 2 inch diameter CCTO sputtering target is also fabricated in order to deposit CCTO thin films for microelectronic applications.

Rietveld refinement and FTIR analysis of bulk ceramic Co3-xMnxO4 compositions

NASA Astrophysics Data System (ADS)

Meena, P. L.; Kumar, Ravi; Sreenivas, K.

2013-02-01

Co3-xMnxO4 (x = 0.0, 0.6, 1.2) prepared by solid state reaction method and characterized by powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Lattice parameters (a), oxygen parameter (u), and ionic radii of cations have been determined through Rietveld analysis. Both a and u parameters are related to expansion of octahedral site as Mn content in Co3O4. Analysis of XRD data show that Mn (x ≤ 1.2) is accommodated at the octahedral site, while retaining the cubic spinel structure. FTIR results also confirm the same and signify strong interactions due to overlapping of Co and Mn octahedra.

Comparison of different bonding techniques for efficient strain transfer using piezoelectric actuators

NASA Astrophysics Data System (ADS)

Ziss, Dorian; Martín-Sánchez, Javier; Lettner, Thomas; Halilovic, Alma; Trevisi, Giovanna; Trotta, Rinaldo; Rastelli, Armando; Stangl, Julian

2017-04-01

In this paper, strain transfer efficiencies from a single crystalline piezoelectric lead magnesium niobate-lead titanate substrate to a GaAs semiconductor membrane bonded on top are investigated using state-of-the-art x-ray diffraction (XRD) techniques and finite-element-method (FEM) simulations. Two different bonding techniques are studied, namely, gold-thermo-compression and polymer-based SU8 bonding. Our results show a much higher strain-transfer for the "soft" SU8 bonding in comparison to the "hard" bonding via gold-thermo-compression. A comparison between the XRD results and FEM simulations allows us to explain this unexpected result with the presence of complex interface structures between the different layers.

Comparison of different bonding techniques for efficient strain transfer using piezoelectric actuators

PubMed Central

Ziss, Dorian; Martín-Sánchez, Javier; Lettner, Thomas; Halilovic, Alma; Trevisi, Giovanna; Trotta, Rinaldo; Rastelli, Armando; Stangl, Julian

2017-01-01

In this paper, strain transfer efficiencies from a single crystalline piezoelectric lead magnesium niobate-lead titanate substrate to a GaAs semiconductor membrane bonded on top are investigated using state-of-the-art x-ray diffraction (XRD) techniques and finite-element-method (FEM) simulations. Two different bonding techniques are studied, namely, gold-thermo-compression and polymer-based SU8 bonding. Our results show a much higher strain-transfer for the “soft” SU8 bonding in comparison to the “hard” bonding via gold-thermo-compression. A comparison between the XRD results and FEM simulations allows us to explain this unexpected result with the presence of complex interface structures between the different layers. PMID:28522879

Comparison of different bonding techniques for efficient strain transfer using piezoelectric actuators.

PubMed

Ziss, Dorian; Martín-Sánchez, Javier; Lettner, Thomas; Halilovic, Alma; Trevisi, Giovanna; Trotta, Rinaldo; Rastelli, Armando; Stangl, Julian

2017-04-01

In this paper, strain transfer efficiencies from a single crystalline piezoelectric lead magnesium niobate-lead titanate substrate to a GaAs semiconductor membrane bonded on top are investigated using state-of-the-art x-ray diffraction (XRD) techniques and finite-element-method (FEM) simulations. Two different bonding techniques are studied, namely, gold-thermo-compression and polymer-based SU8 bonding. Our results show a much higher strain-transfer for the "soft" SU8 bonding in comparison to the "hard" bonding via gold-thermo-compression. A comparison between the XRD results and FEM simulations allows us to explain this unexpected result with the presence of complex interface structures between the different layers.

DSC and Raman studies of silver borotellurite glasses

NASA Astrophysics Data System (ADS)

Kaur, Amandeep; Khanna, Atul; Gonzàlez, Fernando

2016-05-01

Silver borotellurite glasses of composition: xAg2O-yB2O3-(100-x-y)TeO2 (x=20-mol%, y = 0, 10, 20 and 30-mol%) were prepared and characterized by density, X-ray diffraction (XRD), differential scanning calorimetry, and Raman spectroscopy. XRD confirmed the amorphous structure of all samples. Density of glasses decreases while the glass transition temperature increases with increase in B2O3 content from 10 to 30-mol%. Raman study shows that coordination number of Te with oxygen decreases steadily from 3.42 to 3.18 on adding B2O3 due to the transformation of TeO4 into TeO3 units.

Ellipsometric study of Si(0.5)Ge(0.5)/Si strained-layer superlattices

NASA Technical Reports Server (NTRS)

Sieg, R. M.; Alterovitz, S. A.; Croke, E. T.; Harrell, M. J.

1993-01-01

An ellipsometric study of two Si(0.5)Ge(0.5)/Si strained-layer super lattices grown by MBE at low temperature (500 C) is presented, and results are compared with x ray diffraction (XRD) estimates. Excellent agreement is obtained between target values, XRD, and ellipsometry when one of two available Si(x)Ge(1-x) databases is used. It is shown that ellipsometry can be used to nondestructively determine the number of superlattice periods, layer thicknesses, Si(x)Ge(1-x) composition, and oxide thickness without resorting to additional sources of information. It was also noted that we do not observe any strain effect on the E(sub 1) critical point.

Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

NASA Astrophysics Data System (ADS)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

Synthesis and Characterization of YVO4-Based Phosphor Doped with Eu3+ Ions for Display Devices

NASA Astrophysics Data System (ADS)

Thakur, Shashi; Gathania, Arvind K.

2015-10-01

YVO4:Eu nanophosphor has been synthesized by the sol-gel method. Samples were characterized by x-ray diffraction (XRD), energy-dispersive x-ray spectroscopy, Fourier-transform infrared spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, photoluminescence, and Raman spectroscopy. The XRD profile confirms the tetragonal phase of the Eu3+-doped YVO4 nanophosphor. The efficiency of the prepared phosphor was analyzed by means of its emission spectral profile. We also observed rich red emission from the prepared phosphor on excitation by an ultraviolet source. The calculated Commission International de l'Éclairage coordinates reveal excellent color purity efficiency. Such luminescent powder is useful as red phosphor in display device applications.

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

Shetty, G. Rajesha; Kumar, R. Madhu; Rao, B. Lakshmeesha

In this work, the structural and mechanical stability of silk fibroin/Hydroxypropylmethyl cellulose (SF-HPMC) blend films were characterized by X-ray diffraction (XRD) and Universal Testing Machine (UTM). The results indicate that with the introduction of HPMC, the interactions between SF and HPMC results in improved crystallite size and increase in mechanical properties. The blend film obtained is more flexible compared to pure SF film.

The pyrolysis characteristics of moso bamboo

Treesearch

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

2012-01-01

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

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

Tripathi, S., E-mail: shilpatr3@gmail.com; Shripathi, T.; Tripathi, J.

The results are reported on solution cast PMMA-PCTFE blend films characterized using x-ray diffraction and FTIR. The nanocrystalline nature of PMMA is still seen in the blends, however, the bond modifications are clearly observed. The addition of PCTFE results in the modification in structural properties, as reflected in the XRD and FTIR spectra showing modifications in bonding as a function of PCTFE percentage.

Nanomechanical study of amorphous and polycrystalline ALD HfO2 thin films

Treesearch

K. Tapily; J.E. Jakes; D. Gu; H. Baumgart; A.A. Elmustafa

2011-01-01

Thin films of hafnium oxide (HfO2) were deposited by atomic layer deposition (ALD). The structural properties of the deposited films were characterised by transmission electron microscopy (TEM) and X-ray diffraction (XRD). We investigated the effect of phase transformations induced by thermal treatments on the mechanical properties of ALD HfO

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

Ultrafine particles derived from mineral processing: A case study of the Pb-Zn sulfide ore with emphasis on lead-bearing colloids.

PubMed

Mikhlin, Yuri; Vorobyev, Sergey; Romanchenko, Alexander; Karasev, Sergey; Karacharov, Anton; Zharkov, Sergey

2016-03-01

Although mining and mineral processing industry is a vast source of heavy metal pollutants, the formation and behavior of micrometer- and nanometer-sized particles and their aqueous colloids entered the environment from the technological media has received insufficient attention to date. Here, the yield and characteristics of ultrafine mineral entities produced by routine grinding of the Pb-Zn sulfide ore (Gorevskoe ore deposit, Russia) were studied using laser diffraction analysis (LDA), dynamic light scattering (DLS) and zeta potential measurement, microscopy, X-ray photoelectron spectroscopy, with most attention given to toxic lead species. It was revealed, in particular, that the fraction of particles less that 1 μm in the ground ore typical reaches 0.4 vol. %. The aquatic particles in supernatants were micrometer size aggregates with increased content of zinc, sulfur, calcium as compared with the bulk ore concentrations. The hydrodynamic diameter of the colloidal species decreased with time, with their zeta potentials remaining about -12 mV. The colloids produced from galena were composed of 20-50 nm PbS nanoparticles associated with lead sulfate and thiosulfate, while the surface oxidation products at precipitated galena were largely lead oxyhydroxides. The size and zeta potential of the lead-bearing colloids decreased with time down to about 100 nm and from -15 mV to -30 mV, respectively. And, conversely, lead sulfide nanoparticles were mobilized before the aggregates during redispersion of the precipitates in fresh portions of water. The potential environmental impact of the metal-bearing colloids, which is due to the large-scale production and relative stability, is discussed. Copyright © 2015 Elsevier Ltd. All rights reserved.