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.

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.;

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.

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.

[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.

The PM2.5 capture of poly (lactic acid)/nano MOFs eletrospinning membrane with hydrophilic surface

NASA Astrophysics Data System (ADS)

Wang, Yating; Dai, Xiu; Li, Xu; Wang, Xinlong

2018-03-01

In this article, metal organic frameworks (MOFs) material is introduced in the poly (lactic acid) (PLA) by electrospinning to fabricate the nanocomposite membrane. The acrylic acid (AA) is grafted onto the membrane under UV light. The prepared membrane is studied by scanning electron microscopy (SEM), x-ray diffraction (XRD), thermogravimetry (TG), contact angle test and tensile strength test. The SEM image and XRD indicate that nano MOFs particles adhere to the membrane. Contact angle test shows that grafting AA on the composite fiber membrane improves its hydrophilicity effectively. TG analyses show that the particulate matter (PM) capture capacity of PLA membrane with 2 wt% ZIF-8 content is 22%, which rises to 37% after grafting.

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.

[Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

PubMed

Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

2014-12-01

Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

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

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.

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

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.

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.

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.

[NIR and XRD analysis of drill-hole samples from Zhamuaobao iron-graphite deposit, Inner Mongolia].

PubMed

Li, Ying-kui; Cao, Jian-jin; Wu, Zheng-quan; Dai, Dong-le; Lin, Zu-xu

2015-01-01

The author analyzed the 4202 drill-hole samples from Zhamuaobao iron-graphite deposit by using near infrared spectroscopy(NIR) and X-ray diffraction(XRD) measuring and testing techniques, and then compared and summarized the results of two kinds of testing technology. The results indicate that some difference of the mineral composition exists among different layers, the lithology from upper to deeper is the clay gravel layer of tertiary and quaternary, mudstone, mica quartz schist, quartz actinolite scarn, skarnization marble, iron ore deposits, graphite deposits and mica quartz schist. The petrogenesis in different depth also shows difference, which may indicate the geological characteristic to some extent. The samples had mainly undergone such processes as oxidization, carbonation, chloritization and skarn alteration. The research results can not only improve the geological feature of the mining area, but also have great importance in ore exploration, mining, mineral processing and so on. What's more, as XRD can provide preliminary information about the mineral composition, NIR can make further judgement on the existence of the minerals. The research integrated the advantages of both NIR and XRD measuring and testing techniques, put forward a method with two kinds of modern testing technology combined with each other, which may improve the accuracy of the mineral composition identification. In the meantime, the NIR will be more wildly used in geography on the basis of mineral spectroscopy.

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

Sign reversal of transformation entropy change in Co{sub 2}Cr(Ga,Si) shape memory alloys

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

Xu, Xiao, E-mail: xu@material.tohoku.ac.jp; Omori, Toshihiro; Kainuma, Ryosuke

2015-11-02

In situ X-ray diffraction (XRD) measurements and compression tests were performed on Co{sub 2}Cr(Ga,Si) shape memory alloys. The reentrant martensitic transformation behavior was directly observed during the in situ XRD measurements. The high-temperature parent phase and low-temperature reentrant parent phase were found to have a continuous temperature dependence of lattice parameter, therefore suggesting that they are the same phase in nature. Moreover, compression tests were performed on a parent-phase single crystal sample; an evolution from normal to inverse temperature dependence of critical stress for martensitic transformation was directly observed. Based on the Clausius-Clapeyron analysis, a sign reversal of entropy changemore » can be expected on the same alloy.« less

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.

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.

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

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.;

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

In vitro toxicity test of nano-sized magnesium oxide synthesized via solid-phase transformation

NASA Astrophysics Data System (ADS)

Zheng, Jun; Zhou, Wei

2018-04-01

Nano-sized magnesium oxide (MgO) has been a promising potential material for biomedical pharmaceuticals. In the present investigation, MgO nanoparticles synthesized through in-situ solid-phase transformation based on the previous work (nano-Mg(OH)2 prepared by precipitation technique) using magnesium nitrate and sodium hydroxide. The phase structure and morphology of the MgO nanoparticles are characterized by X-ray powder diffraction (XRD), selected area electronic diffraction (SAED) and transmission electron microscopy (TEM) respectively. In vitro hemolysis tests are adopted to evaluate the toxicity of the synthesized nano-MgO. The results evident that nano-MgO with lower concentration is slightly hemolytic, and with concentration increasing nano-MgO exhibit dose-responsive hemolysis.

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

FT-IR and Zeta potential measurements on TiO nanoparticles

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

Singh, Jaiveer; Rathore, Ravi; Kaurav, Netram, E-mail: netramkaurav@yahoo.co.uk

2016-05-23

In the present investigation, ultrafine TiO particles have been synthesized successfully by thermal decomposition method. The sample was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. As-synthesized TiO nanoparticles have a cubic structure as characterized by power X-ray diffraction (XRD), which shows that TiO nanoparticles have narrow size distribution with particle size 11.5 nm. FTIR data shows a strong peak at 1300 cm{sup −1}, assignable to the Ti-O stretching vibrations mode.

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.

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

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

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.

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.

Microstructure and properties of ceramic coatings prepared by micro-arc oxidation on 7075 aluminum alloy

NASA Astrophysics Data System (ADS)

Cao, G. P.; Song, R. G.

2018-02-01

Micro-arc oxidation (MAO) ceramic coatings were prepared in silicate-based electrolyte on 7075 aluminum alloy. The effects of current density on microstructure and properties of the MAO coatings were studied by scanning electron microscopy (SEM), stereoscopic microscopy, x-ray diffraction (XRD), electrochemical tests as well as tribological and wear tests. The results showed that the current density plays an important role in affecting the quality of the MAO coatings. XRD results showed that the α-Al2O3 phase first increased then decreased with increasing the current density, which matched well with the micro-hardness test and the wearing test results. On the other hand, the coalescent strength measurements revealed that the coating prepared at the current density of 12 A dm-2 is of the highest adhesion force. The potentiodynamic polarization test proved that the coating obtained under 10 A dm-2 exhibits the best corrosion resistance, which is directly related to the morphology of coating.

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.

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.

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

Synthesis and toxicity test of magnetic nanoparticle via biocompatible microemulsion system as template for application in targeted drug delivery

NASA Astrophysics Data System (ADS)

Kader, Razinah Abdul; Rose, Laili Che; Suhaimi, Hamdan; Manickam, Mariessa Soosai

2017-09-01

This work reports the preparation of magnetic nanoparticles (FeNPs) using biocompatible W/O microemulsion for biomedical applications. W/O microemulsion was formed using decane as oil phase, water, tween 80 as non-ionic surfactant and hexanol as organic solvent. The synthesized FeNPs were characterised by using Fourier Transform Infrared Resonance Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD). The FTIR showed that Fe-O bond exist on 581cm-1 having strong magnetic strength whereas SEM showed the morphology surface of magnetic nanoparticles (FeNPs). Furthermore, analysis of XRD pattern magnetic nanoparticles (FeNPs) reveals a cubic iron oxide phase with good crystallize structure. Furthermore, toxicity test on human liver cells proved that it is 70% safe on human and proved to be a safety nanomedicine.

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.

Effect of Cu content on wear resistance and mechanical behavior of Ti-Cu binary alloys

NASA Astrophysics Data System (ADS)

Yu, Feifei; Wang, Hefeng; Yuan, Guozheng; Shu, Xuefeng

2017-04-01

Arc melting with nonconsumable tungsten electrode and water-cooled copper crucible was used to fabricate Ti-Cu binary alloys with different Cu contents in an argon atmosphere. The compositions and phase structures of the fabricated alloys were investigated by glow discharge optical emission spectroscopy (GDOES) and X-ray diffraction (XRD). Nanoindentation tests through continuous stiffness measurement were then performed at room temperature to analyze the mechanical behaviors of the alloys. Results indicated that the composition of each Ti-Cu binary alloy was Ti(100- x) Cu x ( x = 43, 60, 69, and 74 at.%). The XRD analysis results showed that the alloys were composed of different phases, indicating that different Cu contents led to the variations in alloy hardness. The wear tests results revealed that elemental Cu positively affects the wear resistance properties of the Ti-Cu alloys. Nanoindentation testing results showed that the moduli of the Ti-Cu alloys were minimally changed at increasing Cu content, whereas their hardness evidently increased according to the wear test results.

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.

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

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.

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.

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

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

Yttria catalyzed microstructural modifications in oxide dispersion strengthened V-4Cr-4Ti alloys synthesized by field assisted sintering technique

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran; Verma, Shailendra Kumar; Dash, Biswaranjan; Agrawal, Priyanka; Subramanian, Karthikeyan

2017-08-01

The present work deals with synthesis, characterisation and elevated temperature mechanical property evaluation of V-4Cr-4Ti and oxide (yttria = 0.3, 0.6 and 0.9 at%) dispersion strengthened V-4Cr-4Ti alloy processed by mechanical alloying and field-assisted sintering, under optimal conditions. Microstructural parameters of both powder and sintered samples were deduced by X-ray diffraction (XRD) and further confirmed with high resolution transmission electron microscopy. Powder diffraction and electron microscopy study show that ball milling of starting elemental powders (V-4Cr-4Ti) with and without yttria addition has resulted in single phase α-V (V-4Cr-4Ti) alloy. Wherein, XRD and electron microscopy images of sintered samples have revealed phase separation (viz., Cr-V and Ti-V) and domain size reduction, with yttria addition. The reasons behind phase separation and domain size reduction with yttria addition during sintering are extensively discussed. Microhardness and high temperature compression tests were done on sintered samples. Yttria addition (0.3 and 0.6 at.%) increases the elevated temperature compressive strength and strain hardening exponent of α-V alloys. High temperature compression test of 0.9 at% yttria dispersed α-V alloy reveals a glassy behaviour.

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

Characterization of magnetic material in the mound-building termite Macrotermes gilvus in Southeast Asia

NASA Astrophysics Data System (ADS)

Esa, Mohammad Faris Mohammad; Rahim, Faszly; Hassan, Ibrahim Haji; Hanifah, Sharina Abu

2015-09-01

Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties of specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.

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

Esa, Mohammad Faris Mohammad; Hassan, Ibrahim Haji; Rahim, Faszly

Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties ofmore » specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.« less

Processing and Characterization of Fe-Mn-Cu-Sn-C Alloys Prepared by Ball Milling and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Bączek, Elżbieta; Konstanty, Janusz; Romański, Andrzej; Podsiadło, Marcin; Cyboroń, Jolanta

2018-03-01

In this work, Fe-Mn-Cu-Sn-C alloys were prepared by means of powder metallurgy (PM). Powder mixtures were ball-milled for 8, 30 and 120 h and densified to < 1% porosity using spark plasma sintering (SPS) at 900 °C and 35 MPa. After consolidation, all samples of the Fe alloys were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), hardness and flexural strength tests. Resistance to abrasive wear was evaluated in both three-body abrasion and two-body abrasion tests. The SEM observations revealed an evident dependence of grain size and microstructural homogeneity on milling time. The XRD analysis showed a marked increase in austenite content in the as-sintered specimens with milling time. Although the proportion of deformation-induced martensite was small, the strengthening effect of abrasion on the subsurface layer of the investigated alloys was clearly indicated by Knoop hardness measurements.

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.

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.

Layered P2-Na 2/3 Co 1/2 Ti 1/2 O 2 as a high-performance cathode material for sodium-ion batteries

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

Sabi, Noha; Doubaji, Siham; Hashimoto, Kazuki

Layered oxides are regarded as promising cathode materials for sodium-ion batteries. We present Na2/3Co1/2Ti1/2O2 as a potential new cathode material for sodium-ion batteries. The crystal features and morphology of the pristine powder were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cathode material is evaluated in galvanostatic charge-discharge and galvanostatic intermittent titration tests, as well as ex-situ X-ray diffraction analysis. Synthesized by a high-temperature solid state reaction, Na2/3Co1/2Ti1/2O2 crystallizes in P2-type structure with P6(3)/mmc space group. The material presents reversible electrochemical behavior and delivers a specific discharge capacity of 100 mAh g(-1) when tested in Na halfmore » cells between 2.0 and 4.2 V (vs. Na+/Na), with capacity retention of 98% after 50 cycles. Furthermore, the electrochemical cycling of this titanium-containing material evidenced a reduction of the potential jumps recorded in the NaxCoO2 parent phase, revealing a positive impact of Ti substitution for Co. The ex-situ XRD measurements confirmed the reversibility and stability of the material. No structural changes were observed in the XRD patterns, and the P2-type structure was stable during the charge/discharge process between 2.0 and 4.2 V vs. Na+/Na. These outcomes will contribute to the progress of developing low cost electrode materials for sodium-ion batteries. (C) 2017 Elsevier B.V. All rights reserved.« less

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.

Analyses of Failure Mechanisms and Residual Stresses in Graphite/Polyimide Composites Subjected to Shear Dominated Biaxial Loads

NASA Technical Reports Server (NTRS)

Kumosa, M.; Predecki, P. K.; Armentrout, D.; Benedikt, B.; Rupnowski, P.; Gentz, M.; Kumosa, L.; Sutter, J. K.

2002-01-01

This research contributes to the understanding of macro- and micro-failure mechanisms in woven fabric polyimide matrix composites based on medium and high modulus graphite fibers tested under biaxial, shear dominated stress conditions over a temperature range of -50 C to 315 C. The goal of this research is also to provide a testing methodology for determining residual stress distributions in unidirectional, cross/ply and fabric graphite/polyimide composites using the concept of embedded metallic inclusions and X-ray diffraction (XRD) measurements.

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.

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.

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.

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.

Characteristics of Volcanic Soils in Landslide during the 2016 Kumamoto Earthquake, Japan

NASA Astrophysics Data System (ADS)

Hazarika, H.; Fukuoka, H.; Kokusho, T.; Sumartini, O.; Bhoopendra, D.

2017-12-01

There were many seismic subsidence, debris flows, landslides and slope failures, which occurred in Aso area due to the 2016 Kumamoto earthquake, Japan. This research aims to determine the failure mechanism of many mild slopes, and elucidate the strength characteristics of volcanic soils collected from the sites. A series of undrained static and cyclic triaxial tests, ring shear tests and direct shear tests were performed. Also, for further understanding of volcanic soils' material strength, X-ray powder diffraction analysis (XRD), X-ray fluorescence analysis (XRF), and Scanning electron microscope analysis (SEM) were performed. In this paper, preliminary results of the experimental testing program are discussed.

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.

Sol-gel derived porous bioactive nanocomposites: Synthesis and in vitro bioactivity

NASA Astrophysics Data System (ADS)

Shankhwar, Nisha; Kothiyal, G. P.; Srinivasan, A.

2013-06-01

Porous bioactive composites consisting of SiO2-CaO-Na2O-P2O5 bioactive glass-ceramic and synthetic water soluble polymer Polyvinylpyrrolidone [PVP (C6H9NO)n, MW˜40000 g/mol] have been synthesized by sol-gel route. As-prepared polymeric composites were characterized by X-ray diffraction (XRD) technique. Two major bone mineral phases, viz., hydroxyapatite [Ca10(PO4)6(OH)2] and wollastonite [calcium silicate (CaSiO3)] have been identified in the XRD patterns of the composites. Presence of these bone minerals indicates the bioactive nature of the composites. In vitro bioactivity tests confirm bioactivity in the porous composites. The flexibility offered by these bioactive polymer composites is advantageous for its application as implant material.

Lignin-based Biochar/graphene Oxide Composites as Supercapacitor Electrode Materials

NASA Astrophysics Data System (ADS)

Cai, Z.; Jiang, C.; Xiao, X. F.; Zhang, Y. S.; Liang, L.

2018-05-01

The lignin-based biochar/graphene composites were effectively obtained via an easy and rapid co-precipitation method. The chemical structure, microstructure, electrochemical properties of lignin/graphene oxide composites before and after carbonization were investigated by Fourier transformation infrared spectrum (FTIR), Scanning electron microscope (SEM), x-ray diffraction (XRD) and cyclic voltammetry (CV). FTIR results confirmed that the oxygen-containing groups of lignin, GO and their composites were partly removed after 800 °C carbonization and GO had a positive impact on the formation of graphitic structure for lignin. XRD results showed that lignin could completely block the restacking of GO sheets. The electrochemical test presented that lignin/graphene oxide composites exhibited a typical CV curve and the specific capacitance reached ∼103F/g at a scan rate of 20mv/s.

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

NASA Astrophysics Data System (ADS)

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

2013-05-01

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

Preparation and antibacterial effect of silver hydroxyapatite/titania nanocomposite thin film on titanium

NASA Astrophysics Data System (ADS)

Mo, Anchun; Liao, Juan; Xu, Wei; Xian, Suqin; Li, Yubao; Bai, Shi

2008-11-01

The composite which contains Ag + and nanosized hydroxyapatite with TiO 2 was deposited onto titanium by dipping method. The morphology, chemical components and structures of the thin film were characterized by XRD, scanning electronic microscope (SEM) and energy dispersive X-ray analysis (EDX). Staphylococcus aureus and Escherichia coli were utilized to test the antibacterial effect. XRD results demonstrated that the films have characteristic diffraction peaks of pure HA. EDX results showed that the deposited films consisted of Ca, P, Ti, O and Ag, all of which distribute uniformly. With regard to the antibacterial effect, 98% of S. aureus and more than 99% of E. coli were killed after 24 h incubation and pictures of SEM showed obviously fewer cells on the surface with coating.

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.

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

NASA Astrophysics Data System (ADS)

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

2015-07-01

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

Synthesis and characterization of magnesium aluminate (MgAl2O4) spinel (MAS) thin films

NASA Astrophysics Data System (ADS)

Ahmad, Syed Muhammad; Hussain, Tousif; Ahmad, Riaz; Siddiqui, Jamil; Ali, Dilawar

2018-01-01

In a quest to identify more economic routes for synthesis of magnesium aluminate (MgAl2O4) spinel (MAS) thin films, dense plasma focus device was used with multiple plasma focus shots. Structural, bonding between composite films, surface morphological, compositional and hardness properties of MAS thin films were investigated by using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive x-rays (EDX) analysis and Vickers micro hardness test respectively. In XRD graph, the presence of MgAl2O4 diffraction peaks in crystallographic orientations (222), (400) and (622) pointed out the successful formation of polycrystalline thin films of MgAl2O4 with face centered cubic structure. The FTIR spectrums showed a major common transmittance band at 697.95 cm-1 which belongs to MgAl2O4. SEM micrographs illustrated a mesh type, granular and multi layers microstructures with significant melting effects. EDX spectrum confirmed the existence of magnesium, oxygen and aluminum in MAS films. A common increasing behavior in micro-hardness of composite MgAl2O4 films by increasing number of plasma focus shots was found.

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

A Study on Factors Affecting Strength of Solidified Peat through XRD and FESEM Analysis

NASA Astrophysics Data System (ADS)

Rahman, J. A.; Napia, A. M. A.; Nazri, M. A. A.; Mohamed, R. M. S. R.; Al-Geethi, A. S.

2018-04-01

Peat is soft soil that often causes multiple problems to construction. Peat has low shear strength and high deformation characteristics. Thus, peat soil needs to be stabilized or treated. Study on peat stabilization has been conducted for decades with various admixtures and mixing formulations. This project intends to provide an overview of the solidification of peat soil and the factors that affecting the strength of solidified peat soil. Three types of peats which are fabric, hemic and sapric were used in this study to understand the differences on the effect. The understanding of the factors affecting strength of solidified peat in this study is limited to XRD and FESEM analysis only. Peat samples were collected at Pontian, Johor and Parit Raja, Johor. Peat soil was solidified using fly ash, bottom ash and Portland cement with two mixing formulation following literature review. The solidified peat were cured for 7 days, 14 days, 28 days and 56 days. All samples were tested using Unconfined Compressive Strength Test (UCS), X-ray diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM). The compressive strength test of solidified peat had shown consistently increase of sheer strength, qu for Mixing 1 while decrease of its compressive strength value for Mixing 2. All samples were tested and compared for each curing days. Through XRD, it is found that all solidified peat are dominated with pargasite and richterite. The highest qu is Fabric Mixing 1(FM1) with the value of 105.94 kPa. This sample were proven contain pargasite. Samples with high qu were observed to be having fly ash and bottom ash bound together with the help of pargasite. Sample with decreasing strength showed less amount of pargasite in it. In can be concluded that XRD and FESEM findings are in line with UCS values.

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.

Growth and properties of benzil doped benzimidazole (BMZ) single crystals

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

Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Crystal Growth and Crystallography Section, National Physical Laboratory, Krishnan Marg, New Delhi 110 012; Sukumar, M.

2010-09-15

In the present work, we have made an attempt to study the effect of benzil doping on the properties of benzimidazole single crystals. For this purpose we have grown pure and benzil doped benzimidazole single crystals by vertical Bridgman technique. The grown crystals were characterized by various characterization techniques. The presence of dopants confirmed by powder X-ray diffraction (XRD). Crystalline perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD). The transmittance, electrical property and mechanical strength have been analysed using UV-vis-NIR spectroscopic, dielectric and Vicker's hardness studies. The relative second harmonic generation efficiency of pure andmore » doped benzimidazole crystals measured using Kurtz powder test.« less

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

NASA Astrophysics Data System (ADS)

Joshi, Prathmesh

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

Mechanical properties of MEMS materials: reliability investigations by mechanical- and HRXRD-characterization related to environmental testing

NASA Astrophysics Data System (ADS)

Bandi, T.; Shea, H.; Neels, A.

2014-06-01

The performance and aging of MEMS often rely on the stability of the mechanical properties over time and under harsh conditions. An overview is given on methods to investigate small variations of the mechanical properties of structural MEMS materials by functional characterization, high-resolution x-ray diffraction methods (HR-XRD) and environmental testing. The measurement of the dynamical properties of micro-resonators is a powerful method for the investigation of elasticity variations in structures relevant to microtechnology. X-ray diffraction techniques are used to analyze residual strains and deformations with high accuracy and in a non-destructive manner at surfaces and in buried micro-structures. The influence of elevated temperatures and radiation damage on the performance of resonant microstructures with a focus on quartz and single crystal silicon is discussed and illustrated with examples including work done in our laboratories at CSEM and EPFL.

Effect of deep cryogenic treatment on the formation of nano-sized carbides and the wear behavior of D2 tool steel

NASA Astrophysics Data System (ADS)

Amini, Kamran; Akhbarizadeh, Amin; Javadpour, Sirus

2012-09-01

The effect of deep cryogenic treatment on the microstructure, hardness, and wear behavior of D2 tool steel was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), hardness test, pin-on-disk wear test, and the reciprocating pin-on-flat wear test. The results show that deep cryogenic treatment eliminates retained austenite, makes a better carbide distribution, and increases the carbide content. Furthermore, some new nano-sized carbides form during the deep cryogenic treatment, thereby increasing the hardness and improving the wear behavior of the samples.

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...

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.

[Study on chemical compositions and crystallinity changes of bamboo treated with gamma rays].

PubMed

Sun, Feng-Bo; Jiang, Ze-hui; Fei, Ben-hua; Lu, Fang; Yu, Zi-xuan; Chang, Xiang-zhen

2011-07-01

The structures and qualities of main chemical compositions in cell wall of bamboo treated with gamma rays were tested by nuclear magnetic resonance spectrometer (NMR) and X-ray Diffraction (XRD). The result indicated that the bamboo crystallinity increased at the beginning of irradiation process, while the crystallinity reduced when the irradiation dose was raised to about 100 kGy. During the whole irradiation process, hemicellulose degraded, and with the irradiation doses increased the non-phenolic lignin changed to the phenolic.

Templated synthesis of nanoporous titania/nanocarbon composites

NASA Astrophysics Data System (ADS)

Mistry, Jayur

Hexagonally patterned (honeycomb structured) nano-porous titania finds distinct applications in the field of material science, electronics, and catalysis. The preparation of titania/nanocarbon composites was carried out using titanium iso-propoxide precursor and a viscous surfactant templated system arranged into nanoscopic channels of water and iso-octane. Nanocarbon was introduced into the titania pores, as it was dispersed into the water (used to increase the W0), while making templets. Prepared titania/nanocarbon composites were analyzed under scanning electron microscopy (SEM), transmission electron microscope (TEM), and X-ray diffraction (XRD) after a specific heat treatment. SEM and TEM allows us to see the morphology of the hexagonally patterned templates and XRD shows the change in the crystallinity of the titania after the heat treatment. Further tests are run with the Solartron™ CellTest potentiostat syste, which, allows us to study the electrical properties of the nanocomposites. The composites synthesized have wide applications in number of fields, including energy, sensors and electronics.

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.

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

Yudoyono, Gatut, E-mail: gyudoyono@physics.its.ac.id; Zharvan, Vicran; Ichzan, Nur

Titanium dioxide (titania) nanoparticle were synthesized by coprecipitation process of titanium trichloride (TiCl{sub 3}) in aqueous medium, with NH{sub 4}OH as pH regulator. The pH solution was varied during the synthesis process between pH 3-8.4, and all samples were calcined temperature at 400°C for 3 hours. Characteristics and properties of the TiO{sub 2} powder were investigated using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM). XRD results show that the single-phase rutile formed when the pH is less than 5, anatase single phase formed began pH 8, and the pH of the solution between 5-8 formed mixed phase rutile-anatase-brookite, rutile-brookite ormore » anatase-brookite. Methylene Blue (MB) photodegradation test were performed in order to evaluate photocatalytic activity. Nanoparticles TiO{sub 2} rutile, anatase phase, and mixed phase rutile-brookite, anatase-brookite used to test the photocatalytic activity by measuring the absorbance spectrum photodegradation using UV-Vis spectrometer. The test results showed that the mixture phase of rutile-brookite provide the greatest photodegradation than other phases.« less

Metallurgical characterization of experimental Ag-based soldering alloys.

PubMed

Ntasi, Argyro; Al Jabbari, Youssef S; Silikas, Nick; Al Taweel, Sara M; Zinelis, Spiros

2014-10-01

To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627-762 °C for AgGa and 631-756 °C for AgGaSn. The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys.

Metallurgical characterization of experimental Ag-based soldering alloys

PubMed Central

Ntasi, Argyro; Al Jabbari, Youssef S.; Silikas, Nick; Al Taweel, Sara M.; Zinelis, Spiros

2014-01-01

Aim To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Materials and methods Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Results Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627–762 °C for AgGa and 631–756 °C for AgGaSn. Conclusion The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys. PMID:25382945

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…

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

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

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

2016-08-15

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

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.

Synthesis and characterization of barium hexaferrite with manganese (Mn) doping material as anti-radar

NASA Astrophysics Data System (ADS)

Susilawati, Doyan, Aris; Khalilurrahman

2017-01-01

Have been successfully synthesized barium powder doping Manganese hexaferrite with the expected potential as anti-radar material. Synthesis was done by using the co-precipitation method, the variation of the variable x concentrations used were 0; 0.2; 0.4; and 0.6 and calcined at temperatures of 400, 600 and 800°C. Characterization powders of hexaferrite have used XRD (X-Ray Diffraction), SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), LCR (inductance, capacitance, and resistance) meter, and VSM (Vibrating Sample Magnetometer). The higher the concentration and temperature of calcinations given affect the color of the powder. The test results using XRD indicates that it has formed barium hexaferrite phase with a hexagonal crystal structure. Tests using SEM showed that all the constituent elements barium powder hexaferrite by doping Manganese powders have been spread evenly. XRD test results were confirmed by a test using a TEM showing the crystal structure and the powder was sized nano particles. The results from the LCR meter showed that the barium powder hexaferrite by doping Manganese that has been synthesized classified in semiconductor materials. The result from VSM showed that the value of coercivity magnetic powder doped barium hexaferrite Manganese is smaller when compared with barium hexaferrite without doping and belong to the soft magnetic. Based on the results of the synthesis and characterization, we can conclude that the barium powder heksaferrite by doping Manganese potential as a material anti-radar.

Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

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

Measurement of fatigue accumulation in high-strength steels by microstructural examination

NASA Astrophysics Data System (ADS)

Nakagawa, Y. G.; Yoshizawa, H.; Lapides, M. E.

1990-07-01

Fatigue test bars fabricated from an SA508 class 3 low-carbon steel plate were cyclically deformed at 300 °C (constant low-cycle fatigue, total strain range Δɛ = 0.78 pct and 0.48 pct) to crack initiation (100 pct cumulative damage, CD) and to the factors 75, 50, and 25 pct CD. The test bars were cut perpendicular to the stress axis at the center of the gage length. The X-ray diffraction line-broadening (XRD) was performed on the cross sections created by the cuts. Thin foils (˜0.1-μm thick) were prepared from each cross section and used for the transmission electron microscope (TEM) and selected area diffraction (SAD) study. The half-value line breadth change measured by the XRD increased with the CD increase up to 50 pct, beyond which a significant reduction was observed for the 75 and 100 pct CD sample regardless of the incident X-ray beam angle. By the TEM, the undamaged material (0 pct CD) was characterized by high-angle boundaries, small carbide precipitates, and dislocation cell networks in grains. These characteristics did not show any appreciable changes in all of the samples with fatigue damage of the respective levels. Micro-orientation changes of the dislocation cells studied by the SAD of the foils and a statistical data analysis clearly demonstrated that the mean orientation difference in the cells and its standard deviation increased gradually as the CD increased.

Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

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

Uvarov, Vladimir, E-mail: vladimiru@savion.huji.ac.il; Popov, Inna

2013-11-15

Crystallite size values were determined by X-ray diffraction methods for 183 powder samples. The tested size range was from a few to about several hundred nanometers. Crystallite size was calculated with direct use of the Scherrer equation, the Williamson–Hall method and the Rietveld procedure via the application of a series of commercial and free software. The results were statistically treated to estimate the significance of the difference in size resulting from these methods. We also estimated effect of acquisition conditions (Bragg–Brentano, parallel-beam geometry, step size, counting time) and data processing on the calculated crystallite size values. On the basis ofmore » the obtained results it is possible to conclude that direct use of the Scherrer equation, Williamson–Hall method and the Rietveld refinement employed by a series of software (EVA, PCW and TOPAS respectively) yield very close results for crystallite sizes less than 60 nm for parallel beam geometry and less than 100 nm for Bragg–Brentano geometry. However, we found that despite the fact that the differences between the crystallite sizes, which were calculated by various methods, are small by absolute values, they are statistically significant in some cases. The values of crystallite size determined from XRD were compared with those obtained by imaging in a transmission (TEM) and scanning electron microscopes (SEM). It was found that there was a good correlation in size only for crystallites smaller than 50 – 60 nm. Highlights: • The crystallite sizes for 183 nanopowders were calculated using different XRD methods • Obtained results were subject to statistical treatment • Results obtained with Bragg-Brentano and parallel beam geometries were compared • Influence of conditions of XRD pattern acquisition on results was estimated • Calculated by XRD crystallite sizes were compared with same obtained by TEM and SEM.« less

Preparation and Compatibility Evaluation of Polypropylene/High Density Polyethylene Polyblends

PubMed Central

Lin, Jia-Horng; Pan, Yi-Jun; Liu, Chi-Fan; Huang, Chien-Lin; Hsieh, Chien-Teng; Chen, Chih-Kuang; Lin, Zheng-Ian; Lou, Ching-Wen

2015-01-01

This study proposes melt-blending polypropylene (PP) and high density polyethylene (HDPE) that have a similar melt flow index (MFI) to form PP/HDPE polyblends. The influence of the content of HDPE on the properties and compatibility of polyblends is examined by using a tensile test, flexural test, Izod impact test, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), polarized light microscopy (PLM), and X-ray diffraction (XRD). The SEM results show that PP and HDPE are incompatible polymers with PP being a continuous phase and HDPE being a dispersed phase. The FTIR results show that the combination of HDPE does not influence the chemical structure of PP, indicating that the polyblends are made of a physical blending. The DSC and XRD results show that PP and HDPE are not compatible, and the combination of HDPE is not correlated with the crystalline structure and stability of PP. The PLM results show that the combination of HDPE causes stacking and incompatibility between HDPE and PP spherulites, and PP thus has incomplete spherulite morphology and a smaller spherulite size. However, according to mechanical property test results, the combination of HDPE improves the impact strength of PP. PMID:28793750

Preparation and Compatibility Evaluation of Polypropylene/High Density Polyethylene Polyblends.

PubMed

Lin, Jia-Horng; Pan, Yi-Jun; Liu, Chi-Fan; Huang, Chien-Lin; Hsieh, Chien-Teng; Chen, Chih-Kuang; Lin, Zheng-Ian; Lou, Ching-Wen

2015-12-17

This study proposes melt-blending polypropylene (PP) and high density polyethylene (HDPE) that have a similar melt flow index (MFI) to form PP/HDPE polyblends. The influence of the content of HDPE on the properties and compatibility of polyblends is examined by using a tensile test, flexural test, Izod impact test, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), polarized light microscopy (PLM), and X-ray diffraction (XRD). The SEM results show that PP and HDPE are incompatible polymers with PP being a continuous phase and HDPE being a dispersed phase. The FTIR results show that the combination of HDPE does not influence the chemical structure of PP, indicating that the polyblends are made of a physical blending. The DSC and XRD results show that PP and HDPE are not compatible, and the combination of HDPE is not correlated with the crystalline structure and stability of PP. The PLM results show that the combination of HDPE causes stacking and incompatibility between HDPE and PP spherulites, and PP thus has incomplete spherulite morphology and a smaller spherulite size. However, according to mechanical property test results, the combination of HDPE improves the impact strength of PP.

Investigation on mechanical behavior and material characteristics of various weight composition of SiCp reinforced aluminium metal matrix composite

NASA Astrophysics Data System (ADS)

Pichumani, Sivachidambaram; Srinivasan, Raghuraman; Ramamoorthi, Venkatraman

2018-02-01

Aluminium - silicon carbide (Al - SiC) metal matrix composite is produced with following wt % of SiC reinforcement (4%, 8% & 12%) using stir casting method. Mechanical testing such as micro hardness, tensile testing and bend testing were performed. Characterizations, namely micro structure, X-ray diffraction (XRD) analysis, inductive coupled plasma - optical emission spectroscopy (ICP-OES) and scanning electron microscopy (SEM) analysis, were carried out on Al - SiC composites. The presence of SiC on Al - SiC composite is confirmed through XRD technique and microstructure. The percentage of SiC was confirmed through ICP-OES technique. Increase in weight percentage of SiC tends to increase micro hardness, ultimate strength & yield strength but it reduces the bend strength and elongation (%) of the material. SEM factrography of tensile tested fractured samples of Al - 8% SiC & Al - 12% SiC showed fine dimples on fractured surface & coarse dimples fractured surface respectively. This showed significant fracture differences between Al - 8% SiC & Al - 12% SiC. From the above experiment, Al - 8% SiC had good micro hardness, ultimate strength & yield strength without significant loss in elongation (%) & bend strength.

Mechanical properties and XRD of Nafion modified by 2-hydroxyethylammonium ionic liquids

NASA Astrophysics Data System (ADS)

Garaev, V.; Pavlovica, S.; Reinholds, I.; Vaivars, G.

2013-12-01

In this work, the Nafion 112 membrane impregnated with 2-hydroxyethylammonium carboxylate ionic liquids have been investigated. The used ionic liquids were 2-hydroxyethylammonium formate [HEA]F, acetate [HEA]A and lactate [HEA]L. Prepared composite membranes Nafion/ionic liquid are characterized by mechanical testing, such as tensile test and creep test. It is found that ionic liquids decrease elastic modulus and creep compliance, but do not have significant effect on the tensile strength. Also, composite membranes were studied by wide angle X-ray diffraction. All ionic liquids shift the peak maximum to the lower angle. In this work, only biodegradable ionic liquids were used for composite preparation.

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

Structural, optical, mechanical and dielectric studies of pure and doped L-Prolinium trichloroacetate single crystals.

PubMed

Renuka, N; Ramesh Babu, R; Vijayan, N; Vasanthakumar, Geetha; Krishna, Anuj; Ramamurthi, K

2015-02-25

In the present work, pure and metal substituted L-Prolinium trichloroacetate (LPTCA) single crystals were grown by slow evaporation method. The grown crystals were subjected to single crystal X-ray diffraction (XRD), powder X-ray diffraction, FTIR, UV-Visible-NIR, hardness, photoluminescence and dielectric studies. The dopant concentration in the crystals was measured by inductively coupled plasma (ICP) analysis. Single crystal X-ray diffraction studies of the pure and metal substituted LPTCA revealed that the grown crystals belong to the trigonal system. Ni(2+) and Co(2+) doping slightly altered the lattice parameters of LPTCA without affecting the basic structure of the crystal. FTIR spectral analysis confirms the presence of various functional groups in the grown crystals. The mechanical behavior of pure and doped crystals was analyzed by Vickers's microhardness test. The optical transmittance, dielectric and photoluminescence properties of the pure and doped crystals were analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Neoteric environmental detoxification of organic pollutants and pathogenic microbes via green synthesized ZnO nanoparticles.

PubMed

Jaffri, Shaan Bibi; Ahmad, Khuram Shahzad

2018-06-13

Present study has for the first time reported Prunus cerasifera leaf extract mediated zinc oxide nanoparticles in a green and one pot synthetic mode without utilization of any chemical reducing agents. Synthesized nanoparticles were analyzed by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), fourier transmission infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). UV-Vis peak was detected at 380 nm due to surface plasmon resonance (SPR). Variety of biomolecules were revealed by FTIR involved in reduction cum stabilization of zinc oxide nanoparticles. Wurtzite hexagonal geometry with an average crystallite size of 12 nm was obtained from XRD diffraction pattern. SEM exhibited size ranges of 80-100 nm and 60- 100 nm for 200 ℃ and 600 ℃ calcination temperatures. Synthesized nanoparticles were used as bio-cleaning photocatalysts against organic pollutants i.e. bromocresol green, bromophenol blue, methyl red and methyl blue, which yielded pseudo first order reaction kinetics (R 2 = 0.98, 0.92, 0.92, 0.90 respectively). Pollutants expressed higher degradation percentages in less than 14 min in direct solar irradiance. Moreover, synthesized nanoparticles were tested against resistant microbes i.e. Aspergillus niger, Aspergillus flavus, Aspergillus fumigatus, Aspergillus terreus, Penicillium chrysogenum, Fusarium solani, Lasiodiplodia theobromae, Xanthomonas axonopodis pv. citri and Psuedomonas syringae for development of new generation of antimicrobial agents.

Structural and optical properties of nanostructured nickel

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

Singh, J., E-mail: jaiveer24singh@gmail.com; Pandey, J.; Gupta, R.

2016-05-06

Metal nanoparticles are attractive because of their special structure and better optical properties. Nickel nanoparticles (Ni-Np) have been synthesized successfully by thermal decomposition method in the presence of trioctyl phosphine (TOP) and oleylamine (OAm). The samples were characterized by X-ray diffraction (XRD), Zetapotential measurement and Fourier transforms infrared (FTIR) spectroscopy. The size of Ni nanoparticles can be readily tuned from 13.86 nm. As-synthesized Ni nanoparticles have hexagonal closed pack (hcp) cubic structure as characterized by power X-ray diffraction (XRD) prepared at 280°C. The possible formation mechanism has also been phenomenological proposed for as synthesized Ni-Np. The value of Zeta potential wasmore » found 12.25 mV.« less

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.

Laser-induced breakdown spectroscopy is a reliable method for urinary stone analysis

PubMed Central

Mutlu, Nazım; Çiftçi, Seyfettin; Gülecen, Turgay; Öztoprak, Belgin Genç; Demir, Arif

2016-01-01

Objective We compared laser-induced breakdown spectroscopy (LIBS) with the traditionally used and recommended X-ray diffraction technique (XRD) for urinary stone analysis. Material and methods In total, 65 patients with urinary calculi were enrolled in this prospective study. Stones were obtained after surgical or extracorporeal shockwave lithotripsy procedures. All stones were divided into two equal pieces. One sample was analyzed by XRD and the other by LIBS. The results were compared by the kappa (κ) and Spearman’s correlation coefficient (rho) tests. Results Using LIBS, 95 components were identified from 65 stones, while XRD identified 88 components. LIBS identified 40 stones with a single pure component, 20 stones with two different components, and 5 stones with three components. XRD demonstrated 42 stones with a single component, 22 stones with two different components, and only 1 stone with three different components. There was a strong relationship in the detection of stone types between LIBS and XRD for stones components (Spearman rho, 0.866; p<0.001). There was excellent agreement between the two techniques among 38 patients with pure stones (κ index, 0.910; Spearman rho, 0.916; p<0.001). Conclusion Our study indicates that LIBS is a valid and reliable technique for determining urinary stone composition. Moreover, it is a simple, low-cost, and nondestructive technique. LIBS can be safely used in routine daily practice if our results are supported by studies with larger numbers of patients. PMID:27011877

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.

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

NASA Astrophysics Data System (ADS)

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

2012-06-01

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

Study of chloride ion transport of composite by using cement and starch as a binder

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

Armynah, Bidayatul; Halide, Halmar; Zahrawani,

This study presents the chemical bonding and the structural properties of composites from accelerator chloride test migration (ACTM). The volume fractions between binder (cement and starch) and charcoal in composites are 20:80 and 60:40. The effect of the binder to the chemical composition, chemical bonding, and structural properties before and after chloride ion passing through the composites was determined by X-ray fluorescence (XRF), by Fourier transform infra-red (FTIR), and x-ray diffraction (XRD), respectively. From the XRD data, XRF data, and the FTIR data shows the amount of chemical composition, the type of binding, and the structure of composites are dependingmore » on the type of binder. The amount of chloride migration using starch as binder is higher than that of cement as a binder due to the density effects.« less

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

NASA Astrophysics Data System (ADS)

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

2013-09-01

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

Structural, thermal and rheological characterization of modified Dalbergia sissoo gum--A medicinal gum.

PubMed

Munir, Hira; Shahid, Muhammad; Anjum, Fozia; Mudgil, Deepak

2016-03-01

Dalbergia sissoo gum was purified by ethanol precipitation. The purified gum was modified and hydrolyzed. Gum was modified by performing polyacrylamide grafting and carboxymethylation methods. The hydrolysis was carried out by using mannanase, barium hydroxide and trifluoroacetic acid. The modified and hydrolyzed gums were characterized using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The decrease in viscosity was studied by performing the flow test. The modified and hydrolyzed gums were thermally stable as compared to crude gum. There was increase in crystallinity after modification and hydrolysis, determined through XRD. FTIR analysis exhibits no major transformation of functional group, only there was change in the intensity of transmittance. It is concluded that the modified and hydrolyzed gum can be used for pharmaceutical and food industry. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural and magnetic properties of chromium doped zinc ferrite

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

Sebastian, Rintu Mary; Thankachan, Smitha; Xavier, Sheena

2014-01-28

Zinc chromium ferrites with chemical formula ZnCr{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by Sol - Gel technique. The structural as well as magnetic properties of the synthesized samples have been studied and reported here. The structural characterizations of the samples were analyzed by using X – Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The single phase spinel cubic structure of all the prepared samples was tested by XRD and FTIR. The particle size was observed to decrease from 18.636 nm to 6.125more » nm by chromium doping and induced a tensile strain in all the zinc chromium mixed ferrites. The magnetic properties of few samples (x = 0.0, 0.4, 1.0) were investigated using Vibrating Sample Magnetometer (VSM)« less

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

Chang, L. L.; Wang, Y. D.; Ren, Y.

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

[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

Surface modification of 17-4PH stainless steel by DC plasma nitriding and titanium nitride film duplex treatment

NASA Astrophysics Data System (ADS)

Qi, F.; Leng, Y. X.; Huang, N.; Bai, B.; Zhang, P. Ch.

2007-04-01

17-4PH stainless steel was modified by direct current (DC) plasma nitriding and titanium nitride film duplex treatment in this study. The microstructure, wear resistance and corrosion resistance were characterized by X-ray diffraction (XRD), pin-on-disk tribological test and polarization experiment. The results revealed that the DC plasma nitriding pretreatment was in favor of improving properties of titanium nitride film. The corrosion resistance and wear resistance of duplex treatment specimen was more superior to that of only coated titanium nitride film.

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

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.

[The spectrum studies of structure characteristics in magma contact metamorphic coal].

PubMed

Wu, Dun; Sun, Ruo-Yu; Liu, Gui-Jian; Yuan, Zi-Jiao

2013-10-01

The structural parameters evolution of coal due to the influence of intrusions of hot magma was investigated and analyzed. X-ray diffraction and laser confocal microscope Raman spectroscopy were used to test and analyze 4 coal samples undergoing varying contact-metamorphism by igneous magmas in borehole No. 13-4 of Zhuji coal mine, Huainan coalfield. The result showed that coal XRD spectrum showed higher background intensity, with the 26 degrees and 42 degrees nearby apparent graphite diffraction peak. Two significant vibration peaks of coal Raman spectra were observed in the 1 000-2 000 cm(-1) frequency range: broad "D" peak at 1 328-1 369 cm(-1) and sharp "G" peak at 1 564-1 599 cm(-1). With the influence of magma intrusion, the relationship between coal structural parameters and coal ranks was excellent.

Investigating the Effects of Pin Tool Design on Friction Stir Welded Ti-6Al-4V

NASA Technical Reports Server (NTRS)

Rubisoff, H. A.; Querin, J. A.; Schneider, Judy A.; Magee, D.

2009-01-01

Friction stir welding (FSWing), a solid state joining technique, uses a non-consumable rotating pin tool to thermomechanically join materials. Heating of the weldment caused by friction and deformation is a function of the interaction between the pin tool and the work piece. Therefore, the geometry of the pin tool is in part responsible for the resulting microstructure and mechanical properties. In this study microwave sintered tungsten carbide (WC) pin tools with tapers and flats were used to FSW Ti-6Al-4V. Transverse sections of welds were mechanically tested, and the microstructure was characterized using optical microscopy (OM) and scanning election microscopy (SEM). X-ray diffraction (XRD) and electron back-scatter diffraction (EBSD) were used to characterize the texture within the welds produced from the different pin tool designs.

Synthesis, characterization and bioactivity of a calcium-phosphate glass-ceramics obtained by the sol-gel processing method.

PubMed

Jmal, Nouha; Bouaziz, Jamel

2017-02-01

In this work, a calcium-phosphate glass-ceramics was successfully obtained by heat treatment of a mixture of 26.52 in wt.% of fluorapatite (Fap) and 73.48 in wt.% of 77S (77 SiO 2 14 CaO9 P 2 O 5 in wt.%) gel. The calcium phosphate-glass-ceramics was prepared by sol-gel process with tetraethyl orthosilicate (TEOS), triethyl phosphate (TEP), calcium nitrate and fluorapatite. The synthesized powders were characterized by some commonly used tools such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), 31 P magic angle spinning nuclear magnetic resonance (MAS-NMR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and thin-film X-ray diffraction (TF-XRD). The obtained results seemed to confirm the nucleation and growth of hydroxyapatite (Hap) nano-phase in the glass. Moreover, an in-vitro evaluation of the glass-ceramic was performed. In addition, to assess its bioactive capacity, it was soaked in simulated body fluid (SBF) at different time intervals. The SEM, EDS and TF-XRD analyses showed the deposition of hydroxyapatite on the surface of the specimens after three days of immersion in SBF solution. The mechanical properties of the obtained material such as rupture strength, Vickers hardness and elastic modulus were measured. In addition, the friction coefficient of calcium phosphate-glass-ceramics was tested. The values of the composite of rupture strength (24MPa), Vickers hardness (214Hv), Young's modulus (52.3GPa), shear modulus (19GPa) and friction coefficient (0.327) were obtained. This glass-ceramics can have useful applications in dental prostheses. Indeed, this material may have promising applications for implants because of its content of fluorine, the effective protector against dental caries. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Preparation and Characterization of Polyurethanes with Cross-Linked Siloxane in the Side Chain by Sol-Gel Reactions

PubMed Central

Zhao, Hui; Hao, Tong-Hui; Hu, Guo-Hua; Shi, Dean; Huang, Da; Jiang, Tao; Zhang, Qun-Chao

2017-01-01

A series of novel polyurethanes containing cross-linked siloxane in the side chain (SPU) were successfully synthesized through a sol-gel process. The SPU was composed of 0%–20% N-(n-butyl)-3-aminopropyltriethoxysilane (HDI-T) modified hexamethylene diisocynate homopolymer. The effects of HDI-T content on both the structure and properties of SPU were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), mechanical properties tests, gel content test, water contact angle measurement and water absorption test. FT-IR, XPS and XRD results confirmed the successful incorporation of HDI-T onto polyurethanes and the formation of Si–O–Si. The surface roughness and the Si content of SPU enhanced with the increase of HDI-T content. Both crystallization and melting temperature shifted to a lower point after the incorporation of HDI-T. The hydrophobicity, tensile strength, Young’s modulus and pencil hardness overall increased with the increasing of HDI-T content, whereas the thermal stability and the elongation at break of SPU slightly decreased. PMID:28772607

Milestone Report - M3FT-15OR03120215 - Recommend HIP Conditions for AgZ

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

Bruffey, Stephanie H.; Jubin, Robert Thomas

2015-09-18

The purpose of this study was to continue research to determine if HIPing could directly convert I-Ag 0Z into a suitable waste form. Fiscal year (FY) 2015 work completed studies of Phase IIA, IIB, and IIC samples. Product consistency testing (PCT) of Phase IIA samples resulted in iodine release below detection limit for six of twelve samples. This is promising and indicates that a durable waste form may be produced through HIPing even if transformation of the zeolite to a distinct mineral phase does not occur. From PCT results of Phase IIA samples, it was determined that future pressing shouldmore » be conducted at a temperature of 900°C. Phase IIC testing continued production of samples to examine the effects of multiple source materials, compositional variations, and an expanded temperature range. The density of each sample was determined and x-ray diffraction (XRD) patterns were obtained. In all cases, there was nothing in the XRD analyses to indicate the creation of any AgI-containing silicon phase; the samples were found to be largely amorphous.« less

Microstructure Characterization and Wear-Resistant Properties Evaluation of an Intermetallic Composite in Ni-Mo-Si System.

PubMed

Huang, Boyuan; Song, Chunyan; Liu, Yang; Gui, Yongliang

2017-02-04

Intermetallic compounds have been studied for their potential application as structural wear materials or coatings on engineering steels. In the present work, a newly designed intermetallic composite in a Ni-Mo-Si system was fabricated by arc-melting process with commercially pure metal powders as starting materials. The chemical composition of this intermetallic composite is 45Ni-40Mo-15Si (at %), selected according to the ternary alloy diagram. The microstructure was characterized using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive spectroscopy (EDS), and the wear-resistant properties at room temperature were evaluated under different wear test conditions. Microstructure characterization showed that the composite has a dense and uniform microstructure. XRD results showed that the intermetallic composite is constituted by a binary intermetallic compound NiMo and a ternary Mo₂Ni₃Si metal silicide phase. Wear test results indicated that the intermetallic composite has an excellent wear-resistance at room-temperature, which is attributed to the high hardness and strong atomic bonding of constituent phases NiMo and Mo₂Ni₃Si.

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.;

In-Vitro Corrosion Studies of Bioabsorbable Alloys

NASA Astrophysics Data System (ADS)

Gill, P.; Munroe, N.

Magnesium alloys have inspired a significant amount of attention from researchers all over the world for cardiovascular and orthopedic applications due to their light weight, mechanical integrity and degradation behavior. In this investigation, cast manufactured binary, ternary and quaternary magnesium alloys were studied for their degradation behavior by potentiodynamic polarization tests in phosphate buffer saline solution (PBS) and PBS containing amino acids (cysteine, C and tryptophan, W) at 37 °C. Electrochemical impedance spectroscopy (EIS) tests were performed to determine the charge transfer resistance and immersion tests were performed to assess corrosion rate and hydrogen evolution from the alloys. Furthermore, the surface morphology and surface chemistry of the alloys were observed by scanning electron microscopy (SEM) and X-ray diffraction (XRD).

[Effects of magnetron sputtered ZrN on the bonding strength of titanium porcelain].

PubMed

Zhou, Shu; Zhang, Wen-yan; Guang, Han-bing; Xia, Yang; Zhang, Fei-min

2009-04-01

To investigate the effect of magnetron sputtered ZrN on the bonding strength between a low-fusing porcelain (Ti/Vita titankeramik system) and commercially pure cast titanium. Sixteen specimens were randomly assigned to test group and control group (n=8). The control group received no surface treated. Magnetron sputtered ZrN film was deposited on the surface of specimens in the test group. Then the sixteen titanium-porcelain specimens were prepared in a rectangular shape and went through three-point bending test on a universal test machine. The bond strength of Ti/porcelain was recorded. The phase composition of the specimens was analyzed using X-ray diffraction (XRD). The interface at titanium and porcelain and the titanium surface after debonding were observed with a scanning electron microscopy (SEM) and analyzed using energy depressive spectrum (EDS). New phase of ZrN was found with XRD in the test group. Statistical analysis showed higher bond strength following ZrN surface treatment in the test group [(45.991+/-0.648) MPa] than that in the control group [(29.483+/-1.007) MPa] (P=0.000). Bonded ceramic could be observed in test group, the amount of bonded ceramic was more than that in the control group. No obvious bonded ceramic in control group was found. Magnetron sputtered ZrN can improve bond strength of Ti/Vita titankeramik system significantly.

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.

The effect of porosity on the mechanical properties of porous titanium scaffolds: comparative study on experimental and analytical values

NASA Astrophysics Data System (ADS)

Khodaei, Mohammad; Fathi, Mohammadhossein; Meratian, Mahmood; Savabi, Omid

2018-05-01

Reducing the elastic modulus and also improving biological fixation to the bone is possible by using porous scaffolds. In the present study, porous titanium scaffolds containing different porosities were fabricated using the space holder method. Pore distribution, formed phases and mechanical properties of titanium scaffolds were studied by Scanning Electron Microscope (SEM), x-ray diffraction (XRD) and cold compression test. Then the results of compression test were compared to the Gibson-Ashby model. Both experimentally measured and analytically calculated elastic modulus of porous titanium scaffolds decreased by porosity increment. The compliance between experimentally measured and analytically calculated elastic modulus of titanium scaffolds are also increased by porosity increment.

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.

Application of vibrational spectroscopy, thermal analyses and X-ray diffraction in the rapid evaluation of the stability in solid-state of ranitidine, famotidine and cimetidine.

PubMed

Jamrógiewicz, Marzena; Ciesielski, Aleksander

2015-03-25

This paper reports the study on applicability of Fourier transform infrared (FTIR), near-infrared (NIR) and Raman spectroscopy, differential scanning calorimetry (DSC) and X-ray diffraction (XRD) for the estimation of the chemical stability and photostability of histamine H2-receptor antagonist substances. Ranitidine hydrochloride (RAN), famotidine (FAM) and cimetidine (CIM) were tested and differences in sensitivity were measured via soft independence modeling of class analogies (Simca) model. The low values of variations for FAM and CIM and high variations obtained for RAN using FTIR and NIR techniques indicated that these methods were suitable and applicable to classify the degradation of RAN. Examined methods are recommendable in the first technological stage of drug production, and the preclinical and clinical development of pharmaceuticals or their quality control. Copyright © 2015 Elsevier B.V. All rights reserved.

Low temperature synthesis of hexagonal ZnO nanorods and their hydrogen sensing properties

NASA Astrophysics Data System (ADS)

Qurashi, Ahsanulhaq; Faiz, M.; Tabet, N.; Alam, Mir Waqas

2011-08-01

The growth of hexagonal ZnO nanorods was demonstrated by low temperature chemical synthesis approach. X-ray diffraction (XRD) analysis revealed a wurtzite hexagonal structure of the ZnO nanorods. The optical properties were measured by UV-vis spectrophotometer at room temperature. X-ray photoelectron spectroscopy (XPS) confirmed high purity of the ZnO nanorods. The hydrogen sensor made of the ZnO nanorods showed reversible response. The hydrogen gas tests were carried out in presence of ambient air and the influence of operation temperature on the hydrogen gas sensing property of ZnO nanorods was also investigated.

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

PubMed

Tankhiwale, Rasika; Bajpai, S K

2012-02-01

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

Preparation and drug release behavior of temperature-responsive mesoporous carbons

NASA Astrophysics Data System (ADS)

Wang, Xiufang; Liu, Ping; Tian, Yong

2011-06-01

A temperature-responsive composite based on poly (N-isopropylacrylamide) (PNIPAAm) and ordered mesoporous carbons (OMCs) has been successfully prepared by a simple wetness impregnation technique. The structures and properties of the composite were characterized by infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 sorption, thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). The results showed that the inclusion of PNIPAAm had not greatly changed the basic ordered pore structure of the OMCs. Ibuprofen (IBU) was selected as model drug, and in vitro test of IBU release exhibited a temperature-responsive controlled release delivery.

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.

Synthesis of PDLLA/PLLA-bentonite nanocomposite through sonication

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

Sitompul, Johnner, E-mail: sitompul@che.itb.ac.id; Setyawan, Daru, E-mail: daru.setyawan@gmail.com; Kim, Daniel Young Joon, E-mail: daniel.kim12321@gmail.com

2016-04-19

This paper concerns the synthesis of poly(D,L-lactic acid)/poly(L-lactic acid) bentonite nanocomposites. Poly (D,L-lactic acid) (PDLLA) was synthesized using lactic acid through the ZnO-catalyzed direct polycondensation method at vacuum pressure and poly(L-lactic acid) (PLLA) was synthesized with L-lactide by ring-opening polymerization method. The PDLLA/PLLA-bentonite nanocomposite films were synthesized using the solvent casting method. The nanoclay, bentonite, was prepared using the solution-intercalation method by dissolving the nanoparticles into chloroform before sonication. In this study, PDLLA/PLLA-bentonite nanocomposite films were produced using variable amounts of nanoclay and sonication times during the mixing of PDLLA/PLLA and bentonite. The properties of the PDLLA/PLLA nanocomposites were thenmore » characterized using the X-ray Diffraction (XRD), Universal Testing Machine (UTM), Water Vapor Permeability (WVP) tests, and the enzymatic biodegradability test. The XRD test was used to measure the intercalation of nanoclay layers in the PDLLA/PLLA matrix and the PDLLA/PLLA-bentonite intercalated nanocomposite films. It was found through these various tests that adding bentonite to the PDLLA/PLLA increases tensile strength to 56.76 MP. Furthermore, the biodegradability increases as well as the barrier properties of the polymers The different sonication time used during the mixing of the polymer solution with bentonite also affected the properties of the PDLLA/PLLA-bentonite nanocomposite films.« less

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.

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.

A green approach to prepare silver nanoparticles loaded gum acacia/poly(acrylate) hydrogels.

PubMed

Bajpai, S K; Kumari, Mamta

2015-09-01

In this work, gum acacia (GA)/poly(sodium acrylate) semi-interpenetrating polymer networks (Semi-IPN) have been fabricated via free radical initiated aqueous polymerization of monomer sodium acrylate (SA) in the presence of dissolved Gum acacia (GA), using N,N'-methylenebisacrylamide (MB) as cross-linker and potassium persulphate (KPS) as initiator. The semi-IPNs, synthesized, were characterized by various techniques such as X-ray diffraction (XRD), thermo gravimetric analysis (TGA) and Fourier transform infrared (FTIR) spectroscopy. The dynamic water uptake behavior of semi-IPNs was investigated and the data were interpreted by various kinetic models. The equilibrium swelling data were used to evaluate various network parameters. The semi-IPNs were used as template for the in situ preparation of silver nanoparticles using extract of Syzygium aromaticum (clove). The formation of silver nanoparticles was confirmed by surface plasmon resonance (SPR), XRD and transmission electron microscopy (TEM). Finally, the antibacterial activity of GA/poly(SA)/silver nanocomposites was tested against E. coli. Copyright © 2015 Elsevier B.V. All rights reserved.

Laser additive manufacturing bulk graphene-copper nanocomposites.

PubMed

Hu, Zengrong; Chen, Feng; Lin, Dong; Nian, Qiong; Parandoush, Pedram; Zhu, Xing; Shao, Zhuqiang; Cheng, Gary J

2017-11-03

The exceptional mechanical properties of graphene make it an ideal nanofiller for reinforcing metal matrix composites (MMCs). In this work, graphene-copper (Gr-Cu) nanocomposites have been fabricated by a laser additive manufacturing process. Transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy were utilized to characterize the fabricated nanocomposites. The XRD, Raman spectroscopy, energy dispersive spectroscopy and TEM results demonstrated the feasibility of laser additive manufacturing of Gr-Cu nanocomposites. The microstructures were characterized by high resolution TEM and the results further revealed the interface between the copper matrix and graphene. With the addition of graphene, the mechanical properties of the composites were enhanced significantly. Nanoindentation tests showed that the average modulus value and hardness of the composites were 118.9 GPa and 3 GPa respectively; 17.6% and 50% increases were achieved compared with pure copper, respectively. This work demonstrates a new way to manufacture graphene copper nanocomposites with ultra-strong mechanical properties and provides alternatives for applications in electrical and thermal conductors.

Effect of testosterone incorporation on cell proliferation and differentiation for polymer-bioceramic composites.

PubMed

da Costa, Kelen Jorge Rodrigues; Passos, Joel J; Gomes, Alinne D M; Sinisterra, Rubén D; Lanza, Célia R M; Cortés, Maria Esperanza

2012-11-01

In the current study, we characterized the polycaprolactone (PCL), poly(lactic acid-co-glycolic acid) (PLGA), and biphasic calcium phosphate (BCP) composites coated with testosterone propionate (T) using Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (XRD). Osteoblastic cells were seeded with PCL/BCP, PCL/BCP/T, PLGA/PCL/BCP and PLGA/PCL/BCP/T scaffolds, and cell viability, proliferation, differentiation and adhesion were analyzed. The results of physic-chemical experiments showed no displacements or suppression of bands in the FTIR spectra of scaffolds. The XRD patterns of the scaffolds showed an amorphous profile. The osteoblastic cells viability and proliferation increased in the presence of composites with testosterone over 72 h, and were significantly greater when PLGA/PCL/BCP/T scaffold was tested against PCL/BCP/T. Furthermore alkaline phosphatase production was significantly greater in the same group. In conclusion, the PLGA/PCL/BCP scaffold with testosterone could be a promising option for bone tissue applications due to its biocompatibility and its stimulatory effect on cell proliferation.

Time dependent rise and decay of photocurrent in zinc oxide nanoparticles in ambient and vacuum medium

NASA Astrophysics Data System (ADS)

C, Rajkumar; Srivastava, Rajneesh K.

2018-05-01

Zinc oxide (ZnO) nanoparticle has been synthesized by cost effective Co-precipitation method and studied its photo-response activity. The synthesized ZnO nanomaterial was characterized by using various analytical techniques such as x-ray diffraction (XRD), UV–visible spectroscopy, FTIR spectroscopy, photoluminescence (PL) spectroscopy, and Scanning Electron Microscopy (SEM). From the XRD results, it is confirmed that synthesized ZnO nanomaterial possess hexagonal wurtzite phase structure with an average crystallite size of ∼16–17 nm. The UV-Visible absorption spectrum shows that it has blue shift compared to their bulk counterparts. Photoluminescence spectra of ZnO nanoparticles have a strong violet band at 423 nm and three weak bands at 485 nm (blue), 506 nm (green), and 529 nm (green). The presence of hydroxyl group was confirmed by FTIR. The photo-response analysis was studied by the time-dependent rise and decay photocurrent of ZnO nanoparticle was tested in the air as well as vacuum medium.

Study on structure and morphology (Boehmeria nivea) in the irregular and regular parts of the fiber after biodegumming

NASA Astrophysics Data System (ADS)

Wulandari, A. P.; Septarini, D.; Zainuddin, A.

2017-05-01

Ramie is a natural fiber that is very potential to be developed in Indonesia. Decorticated-fiber which has been known as china grass produce different structures irregular part but shows a long straight section in the middle. This study aims to determine differences in chemical components, morphology and microstructure of two different parties after biodegumming process. China grass has been processed to remove gum using pectinolytic fungus. The microstructure of the treated was further tested by Fourier Transform InfraRed (FTIR), X-Ray Diffraction (XRD), and Scanning Electron Microscope (SEM). The FTIR study indicated that during the biodegumming process, chemical bonding of non-cellulose components most removed by the activity of pectinase from the fungus. XRD analysis reflects an increase in the crystallinity of the fiber after biodegumming. Scanning electron microscopy (SEM) was used to confirm a reduction in the size of the fiber after biodegumming either in the irregular and regular part of the fiber after biodegumming.

Preliminary Geological Findings on the BP-1 Simulant

NASA Technical Reports Server (NTRS)

Stoeser, D. B.; Rickman, D. L.; Wilson, S.

2010-01-01

A waste material from an aggregate producing quarry has been used to make an inexpensive lunar simulant called BP-1. The feedstock is the Black Point lava flow in northern Arizona. Although this is part of the San Francisco volcanic field, which is also the source of the JSC-1 series feedstock, BP-1 and JSC-1 are distinct. Chemically, the Black Point flow is an amygdaloidal nepheline-bearing basalt. The amygdules are filled with secondary minerals containing opaline silica, calcium carbonate, and ferric iron minerals. X-ray diffraction (XRD) detected approximately 3% quartz, which is in line with tests done by the Kennedy Space Center Industrial Hygiene Office. Users of this material should use appropriate protective equipment. XRD also showed the presence of significant halite and some bassanite. Both are interpreted to be evaporative residues due to recycling of wash water at the quarry. The size distribution of BP-1 may be superior to some other simulants for some applications.

Synthesis, characterization and antimicrobial activity of dextran stabilized silver nanoparticles in aqueous medium.

PubMed

Bankura, K P; Maity, D; Mollick, M M R; Mondal, D; Bhowmick, B; Bain, M K; Chakraborty, A; Sarkar, J; Acharya, K; Chattopadhyay, D

2012-08-01

A simple one-step rapid synthetic route is described for the preparation of silver nanoparticles by reduction of silver nitrate (AgNO3) using aqueous dextran solution which acts as both reducing and capping agent. The formation of silver nanoparticles is assured by characterization with UV-vis spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The absorbance of the silver nanoparticles is observed at 423 nm. The AFM image clearly shows the surface morphology of the well-dispersed silver nanoparticles with size range of 10-60 nm. TEM images show that the nanoparticles are spherical in shape with ∼5-10 nm dimensions. The crystallinity of Ag nanoparticles is assured by XRD analysis. The antimicrobial activity of as synthesized silver nanoparticles is tested against the bacteria, Bacillus subtilis, Bacillus cereus, Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa. The bacterial growth is inhibited by gradual reduction of the concentration of the silver nanoparticles. Copyright © 2012 Elsevier Ltd. All rights reserved.

Laser additive manufacturing bulk graphene-copper nanocomposites

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Chen, Feng; Lin, Dong; Nian, Qiong; Parandoush, Pedram; Zhu, Xing; Shao, Zhuqiang; Cheng, Gary J.

2017-11-01

The exceptional mechanical properties of graphene make it an ideal nanofiller for reinforcing metal matrix composites (MMCs). In this work, graphene-copper (Gr-Cu) nanocomposites have been fabricated by a laser additive manufacturing process. Transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy were utilized to characterize the fabricated nanocomposites. The XRD, Raman spectroscopy, energy dispersive spectroscopy and TEM results demonstrated the feasibility of laser additive manufacturing of Gr-Cu nanocomposites. The microstructures were characterized by high resolution TEM and the results further revealed the interface between the copper matrix and graphene. With the addition of graphene, the mechanical properties of the composites were enhanced significantly. Nanoindentation tests showed that the average modulus value and hardness of the composites were 118.9 GPa and 3 GPa respectively; 17.6% and 50% increases were achieved compared with pure copper, respectively. This work demonstrates a new way to manufacture graphene copper nanocomposites with ultra-strong mechanical properties and provides alternatives for applications in electrical and thermal conductors.

Microstructure and Mechanical Behavior of Microwave Sintered Cu50Ti50 Amorphous Alloy Reinforced Al Metal Matrix Composites

NASA Astrophysics Data System (ADS)

Reddy, M. Penchal; Ubaid, F.; Shakoor, R. A.; Mohamed, A. M. A.

2018-06-01

In the present work, Al metal matrix composites reinforced with Cu-based (Cu50Ti50) amorphous alloy particles synthesized by ball milling followed by a microwave sintering process were studied. The amorphous powders of Cu50Ti50 produced by ball milling were used to reinforce the aluminum matrix. They were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and compression testing. The analysis of XRD patterns of the samples containing 5 vol.%, 10 vol.% and 15 vol.% Cu50Ti50 indicates the presence of Al and Cu50Ti50 peaks. SEM images of the sintered composites show the uniform distribution of reinforced particles within the matrix. Mechanical properties of the composites were found to increase with an increasing volume fraction of Cu50Ti50 reinforcement particles. The hardness and compressive strength were enhanced to 89 Hv and 449 MPa, respectively, for the Al-15 vol.% Cu50Ti50 composites.

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

NASA Astrophysics Data System (ADS)

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

2015-06-01

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

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.

Alternative High-Performance Ceramic Waste Forms

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

Sundaram, S. K.

This final report (M5NU-12-NY-AU # 0202-0410) summarizes the results of the project titled “Alternative High-Performance Ceramic Waste Forms,” funded in FY12 by the Nuclear Energy University Program (NEUP Project # 12-3809) being led by Alfred University in collaboration with Savannah River National Laboratory (SRNL). The overall focus of the project is to advance fundamental understanding of crystalline ceramic waste forms and to demonstrate their viability as alternative waste forms to borosilicate glasses. We processed single- and multiphase hollandite waste forms based on simulated waste streams compositions provided by SRNL based on the advanced fuel cycle initiative (AFCI) aqueous separation process developed in the Fuel Cycle Research and Development (FCR&D). For multiphase simulated waste forms, oxide and carbonate precursors were mixed together via ball milling with deionized water using zirconia media in a polyethylene jar for 2 h. The slurry was dried overnight and then separated from the media. The blended powders were then subjected to melting or spark plasma sintering (SPS) processes. Microstructural evolution and phase assemblages of these samples were studied using x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion analysis of x-rays (EDAX), wavelength dispersive spectrometry (WDS), transmission electron spectroscopy (TEM), selective area x-ray diffraction (SAXD), and electron backscatter diffraction (EBSD). These results showed that the processing methods have significant effect on the microstructure and thus the performance of these waste forms. The Ce substitution into zirconolite and pyrochlore materials was investigated using a combination of experimental (in situ XRD and x-ray absorption near edge structure (XANES)) and modeling techniques to study these single phases independently. In zirconolite materials, a transition from the 2M to the 4M polymorph was observed with increasing Ce content. The resulting powders were consolidated via SPS. Ce was reduced to the trivalent oxidation state and the zirconolite was converted into undesirable perovskite. The zirconolite polymorphs found in the synthesized powders were recovered after a post-SPS heat treatment in air. These results demonstrated the potential of processing in controlling the phase assemblage in these waste forms. Hollandites with Cr 3+ trivalent cations were identified as potential hosts for Cs immobilization and are being investigated for Cs retention properties. Series of compositions Ba 1.15-xCs 2xCr 2.3Ti 5.7O 16, with increasing Cs loadings, were prepared by sol-gel process and characterized for structural parameters. Structural characterization was performed by a combination of powder XRD and neutron powder diffraction. Phase pure hollandite adapting monoclinic symmetry (I2/m) was observed for 0 ≤ x ≤ 0.55. These results were used to develop a new structural model to interpret Cs immobilization in these hollandites. Performance of these waste forms were evaluated for chemical durability and radiation resistance. Product consistency testing (PCT) and vapor hydration testing (VHT) were used for testing of chemical durability. Radiation resistance was tested using He + ions to simulatemore » $$\\alpha$$ particles and heavy ions such as Au 3+ to simulate a recoil. These results showed that these waste forms were chemically durable. The waste forms also amorphized to various degrees on exposure to simulated radiation.« less

XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

USGS Publications Warehouse

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

1997-01-01

The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good agreement with estimates of the mean thickness of fundamental particles obtained both from TEM measurements and from fixed cations content, up to a mean value of 20 layers. Correction for instrumental broadening under the conditions employed here is unnecessary for this range of thicknesses.

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

Electrochemical oxidation of sulfites by DWCNTs, MWCNTs, higher fullerenes and manganese

NASA Astrophysics Data System (ADS)

Uzun, Dzhamal; Pchelarov, George; Dimitrov, Ognian; Vassilev, Sasho; Obretenov, Willi; Petrov, Konstantin

2018-03-01

Different electrocatalysts were tested for oxidation of sulfites to sulfates, namely, manganese thin films deposited on fullerenes and carbon nanotubes. The results presented clearly show that electrodes containing HFs (higher fullerenes), DWCNTs (double-wall carbon nanotubes) and manganese acetate are effective catalysts in S/O2 fuel cells. HFs and DWCNTs have high catalytic activity and can be employed as standalone catalysts. Manganese was deposited on DWCNTs, HFs and fullerenes C60/C70 by a thermal process. The electrocatalysts were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The electrochemical testing was carried out by plotting the E/V polarization curve. The polarization curves of the electrodes composed of pristine DWCNTs showed the lowest overpotentials.

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

NASA Astrophysics Data System (ADS)

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

2015-03-01

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

Autogenous teeth used for bone grafting: a comparison with traditional grafting materials.

PubMed

Kim, Young-Kyun; Kim, Su-Gwan; Yun, Pil-Young; Yeo, In-Sung; Jin, Seung-Chan; Oh, Ji-Su; Kim, Heung-Joong; Yu, Sun-Kyoung; Lee, Sook-Young; Kim, Jae-Sung; Um, In-Woong; Jeong, Mi-Ae; Kim, Gyung-Wook

2014-01-01

This study evaluated the surface structures and physicochemical characteristics of a novel autogenous tooth bone graft material currently in clinical use. The material's surface structure was compared with a variety of other bone graft materials via scanning electron microscope (SEM). The crystalline structure of the autogenous tooth bone graft material from the crown (AutoBT crown) and root (AutoBT root), xenograft (BioOss), alloplastic material (MBCP), allograft (ICB), and autogenous mandibular cortical bone were compared using x-ray diffraction (XRD) analysis. The solubility of each material was measured with the Ca/P dissolution test. The results of the SEM analysis showed that the pattern associated with AutoBT was similar to that from autogenous cortical bones. In the XRD analysis, AutoBT root and allograft showed a low crystalline structure similar to that of autogenous cortical bones. In the CaP dissolution test, the amount of calcium and phosphorus dissolution in AutoBT was significant from the beginning, while displaying a pattern similar to that of autogenous cortical bones. In conclusion, autogenous tooth bone graft materials can be considered to have physicochemical characteristics similar to those of autogenous bones. Copyright © 2014 Elsevier Inc. All rights reserved.

Uncovering the local inelastic interactions during manufacture of ductile cast iron: How the substructure of the graphite particles can induce residual stress concentrations in the matrix

NASA Astrophysics Data System (ADS)

Andriollo, Tito; Hellström, Kristina; Sonne, Mads Rostgaard; Thorborg, Jesper; Tiedje, Niels; Hattel, Jesper

2018-02-01

Recent X-ray diffraction (XRD) measurements have revealed that plastic deformation and a residual elastic strain field can be present around the graphite particles in ductile cast iron after manufacturing, probably due to some local mismatch in thermal contraction. However, as only one component of the elastic strain tensor could be obtained from the XRD data, the shape and magnitude of the associated residual stress field have remained unknown. To compensate for this and to provide theoretical insight into this unexplored topic, a combined experimental-numerical approach is presented in this paper. First, a material equivalent to the ductile cast iron matrix is manufactured and subjected to dilatometric and high-temperature tensile tests. Subsequently, a two-scale hierarchical top-down model is devised, calibrated on the basis of the collected data and used to simulate the interaction between the graphite particles and the matrix during manufacturing of the industrial part considered in the XRD study. The model indicates that, besides the viscoplastic deformation of the matrix, the effect of the inelastic deformation of the graphite has to be considered to explain the magnitude of the XRD strain. Moreover, the model shows that the large elastic strain perturbations recorded with XRD close to the graphite-matrix interface are not artifacts due to e.g. sharp gradients in chemical composition, but correspond to residual stress concentrations induced by the conical sectors forming the internal structure of the graphite particles. In contrast to common belief, these results thus suggest that ductile cast iron parts cannot be considered, in general, as stress-free at the microstructural scale.

Surfactant-free bio-synthesised Tio2 nanorods from Turbinaria conoides-a study on photocatalytic and anti-bacterial activity

NASA Astrophysics Data System (ADS)

Subhapriya, S.; Gomathipriya, P.

2018-06-01

In this study, Titania nanorods were synthesised from aqueous extract of Turbinaria conoides (brown seaweeds) (TiO2NRs-TC) under surfactant free medium. The photocatalytic activity of the synthesised nanorods was tested towards the photocatalytic decolourization using simulated dye wastewater containing Navy Blue HER (NBHER). The synthesised Titania nanorods were characterized by using x-ray diffraction (XRD), UV–visible spectroscopy (UV–vis), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrophotometer (EDS) and Transmission Electron Microscopy (TEM). XRD pattern confirms the anatase phase formation and HR-SEM micrograph shows the presence of rod like structure with the size of about 50 nm. TEM analysis proves the rod like structure with a size of 45–50 nm which was in agreement with the XRD analysis and HR-SEM images. EDS and XDS confirmed the formation of Titania nanoparticles. The formation of TiO2NRs-TC has a beneficial influence on the dye Navy blue HER photodegradation. TiO2-TC nano rods also show superior photocatalytic ability in hydrogen generation (2.1 mmol/h‑1g‑1). The antibacterial activity of the synthesised nanoparticles was examined using disc diffusion method which showed diverse susceptibility of microorganisms to the Titania nanoparticles.

Synthesis and Characterization of Chukanovite, Fe2CO3(OH)2(s): An Elusive Ferrous Iron Carbonate Hydroxide Mineral

NASA Astrophysics Data System (ADS)

Jang, J. J. H.; Kim, S.; Burton, H.; Knox, J.; Marrs, C.; Sisk-Scott, C.

2017-12-01

The long-term effectiveness of an underground waste repository relies on understanding the chemical reaction products between intrusive brine and the reactive media in the repository. One such component of the stored media, iron, forms mineral precipitates in brine through anoxic corrosion. Chukanovite, Fe2CO3(OH)2(s), could be one of the precipitates and not much is known regarding its formation and thermodynamic stability. Thus, we have investigated eight mixtures of FeCl2 and NaHCO3 with NaOH for the synthesis of chukanovite in an anoxic glovebox. X-ray diffraction (XRD) scans of ten-month aged samples showed the paragenesis of three ferrous iron minerals in all tested conditions; siderite (FeCO3(s)), ferrous iron hydroxide (Fe(OH)2(s)), and chukanovite. Chukanovite was present alongside the two other minerals in between the pH values of 6 and 11. Comparison of relative intensities of major XRD peak heights of three minerals illustrated that the highest phase purity of chukanovite was achieved when the solution pH was approximately 9. XRD and solubility analysis will be performed periodically to determine when the experiments in the eight conditions reach steady state. Solid samples will be further characterized using Mossbauer and Raman spectroscopy.

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

PubMed

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

2014-09-01

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

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.

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

Effect of high-pressure torsion on the microstructural evolution and mechanical properties of an Fe-10Ni-7Mn (wt. %) lath martensitic steel

NASA Astrophysics Data System (ADS)

Kalahroudi, Faezeh Javadzadeh; Koohdar, Hamidreza; Jafarian, Hamidreza; Nili-Ahmadabadi, Mahmoud; Huang, Yi; Langdon, Terence. G.

2018-01-01

The high-pressure torsion (HPT) process is a severe plastic deformation (SPD) technique which imposes exceptionally high strains to produce extremely small grain sizes in bulk materials. In this paper, the HPT process was carried out on an Fe-10Ni-7Mn (wt.%) martensitic steel up to 20 revolutions at a rotation speed of 1 rpm under a pressure of 6.0 GPa at room temperature. The effects of the HPT process on the microstructure evolution and mechanical properties of the alloy were investigated by X-ray diffraction (XRD) analysis, electron backscatter diffraction (EBSD), micro-hardness measurement and conventional tensile testing. The XRD analysis revealed no changes in the detected phases after deformation. A significant refinement in grain size from 200 µm in the initial microstructure to around 230 nm after HPT was observed by EBSD. Although based on a rigid body assumption the imposed strain is linearly proportional to the distance from the center in HPT-processed disks, after 20 revolutions a uniform micro-hardness increment up to 650 Hv was achieved. Moreover, the tensile strength of the alloy increased from ˜800 MPa in the solution annealed condition to about 2300 MPa after the HPT process with a total tensile strain of 4%. Experimental results indicated that the HPT process leads to improvement of the tensile strength with a reasonable ductility due to the significant refinement of the microstructure.

Studies of tin-transition metal-carbon and tin-cobalt-transition metal-carbon negative electrode materials prepared by mechanical attrition

NASA Astrophysics Data System (ADS)

Ferguson, P. P.; Martine, M. L.; George, A. E.; Dahn, J. R.

Samples of Sn 30TM 30C 40 and of Sn 30Co 15TM 15C 40, with TM = 3d transition metals, were prepared by vertical-axis attritor milling. The structure and performance of these samples were studied by X-ray diffraction (XRD) and by electrochemical testing. The XRD patterns of Sn 30TM 30C 40 show an amorphous-like diffraction pattern only for the sample with TM = Co. The other prepared samples show broadened Bragg peaks of their main starting material, along with an amorphous-like background, even after 32 h of milling. Samples with TM = Co and TM = Ni show stable differential capacity versus potential plots and stable cycling for at least 100 cycles with reversible capacities of 425 and 250 mAh g -1, respectively. All samples prepared with 15 at.% Co show good capacity retention for at least 100 cycles ranging from 270 mAh g -1 for samples with TM = Ni to 500 mAh g -1 for samples with TM = Ti. The differential capacity versus potential plots for all the prepared Sn 30Co 15TM 15C 40 samples show similar structure to that of Sn 30Co 30C 40 except when TM = Cu. This shows the possibility of preparing tin-based negative electrode materials using a combination of cobalt and TM, especially if one looks to reduce the cobalt content.

Effect of Gallium Doping on the Characteristic Properties of Polycrystalline Cadmium Telluride Thin Film

NASA Astrophysics Data System (ADS)

Ojo, A. A.; Dharmadasa, I. M.

2017-08-01

Ga-doped CdTe polycrystalline thin films were successfully electrodeposited on glass/fluorine doped tin oxide substrates from aqueous electrolytes containing cadmium nitrate (Cd(NO3)2·4H2O) and tellurium oxide (TeO2). The effects of different Ga-doping concentrations on the CdTe:Ga coupled with different post-growth treatments were studied by analysing the structural, optical, morphological and electronic properties of the deposited layers using x-ray diffraction (XRD), ultraviolet-visible spectrophotometry, scanning electron microscopy, photoelectrochemical cell measurement and direct-current conductivity test respectively. XRD results show diminishing (111)C CdTe peak above 20 ppm Ga-doping and the appearance of (301)M GaTe diffraction above 50 ppm Ga-doping indicating the formation of two phases; CdTe and GaTe. Although, reductions in the absorption edge slopes were observed above 20 ppm Ga-doping for the as-deposited CdTe:Ga layer, no obvious influence on the energy gap of CdTe films with Ga-doping were detected. Morphologically, reductions in grain size were observed at 50 ppm Ga-doping and above with high pinhole density within the layer. For the as-deposited CdTe:Ga layers, conduction type change from n- to p- were observed at 50 ppm, while the n-type conductivity were retained after post-growth treatment. Highest conductivity was observed at 20 ppm Ga-doping of CdTe. These results are systematically reported in this paper.

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

PubMed

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

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

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

Al-Hazeem, Nabeel Z., E-mail: nabeelnano333@gmail.com; Ministry of Education, the General Directorate for Educational Anbar; Ahmed, Naser M.

In this work, we fabricated nanorods by applying an electric potential on poly (ethylene oxide) (PEO) and polyaniline (PANI) as a polymeric solution by electrospinning method. Testing was conducted on the samples by field emission scanning Electron microscope (FE-SEM), X-ray diffraction (XRD) and Photoluminescence. And the results showed the emergence of nanorods in the sample within glass substrate. Diameters of nanorods have ranged between (52.78-122.40)nm And a length of between (1.15 – 1.32)μm. The emergence of so the results are for the first time, never before was the fabrication of nanorods for polymers using the same method used in thismore » research.« less

Comparison of Antimicrobial Properties of Nano Quinolone with its Microscale Effects

NASA Astrophysics Data System (ADS)

Behbahani, G. Rezaie; Sadr, M. Hossaini; Nabipour, H.; Behbahani, H. Rezaei; Vahedpour, M.; Barzegar, L.

2013-06-01

Nano nalidixic acid was prepared by ultrasonic method in carbon tetrachloride. Nano nalidixic acid (quinolone antibiotic) was characterized by X-ray diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscope (SEM). The antibacterial activities of nano nalidixic acid were tested against microorganisms and compared with the microscale drug. The results show that nano nalidixic acid has good inhibitory properties against two Gram-positive species, Staphylococcus aureus and Bacillus subtilis. Nano nalidixic acid also showed good antifungal activity against Candida albicans. Nano nalidixic acid can be injected into the human body as a decontaminating agent to prevent the growth of harmful microorganisms more effectively than the micro-sized drug.

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.

Laboratory Testing of Silica Sol Grout in Coal Measure Mudstones.

PubMed

Pan, Dongjiang; Zhang, Nong; Xie, Zhengzheng; Feng, Xiaowei; Kong, Yong

2016-11-22

The effectiveness of silica sol grout on mudstones is reported in this paper. Using X-ray diffraction (XRD), the study investigates how the silica sol grout modifies mudstone mineralogy. Micropore sizes and mechanical properties of the mudstone before and after grouting with four different materials were determined with a surface area/porosity analyser and by uniaxial compression. Tests show that, after grouting, up to 50% of the mesopore volumes can be filled with grout, the dominant pore diameter decreases from 100 nm to 10 nm, and the sealing capacity is increased. Uniaxial compression tests of silica sol grouted samples shows that their elastic modulus is 21%-38% and their uniaxial compressive strength is 16%-54% of the non-grouted samples. Peak strain, however, is greater by 150%-270%. After grouting, the sample failure mode changes from brittle to ductile. This paper provides an experimental test of anti-seepage and strengthening properties of silica sol.

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

NASA Technical Reports Server (NTRS)

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

1996-01-01

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

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.

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

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...

Facile synthesis of hollow Co3O4 microspheres and its use as a rapid responsive CL sensor of combustible gases.

PubMed

Teng, Fei; Yao, Wenqing; Zheng, Youfei; Ma, Yutao; Xu, Tongguang; Gao, Guizhi; Liang, Shuhui; Teng, Yang; Zhu, Yongfa

2008-09-15

The hollow Co(3)O(4) microspheres (HCMs) were prepared by the carbonaceous templates, which did not need the surface pretreatment. The chemiluminescence (CL) and catalytic properties for CO oxidation over these hollow samples were evaluated. The samples were characterized by scanning electron microscopy (SEM), energy disperse spectra (EDS), transmission electron microscopy (TEM), selected area electron diffraction (ED), X-ray diffraction (XRD), temperature-programmed desorption (TPD) and N(2) adsorption. The influences of filter' band length, flow rate of gas, test temperature, and particle structure on CL intensities were mainly investigated. It was found that compared with the solid Co(3)O(4) particles (SCPs), HCMs had a stronger CL intensity, which was ascribed to its hollow structure; and that CL properties of the catalysts were well correlated with their reaction activities. Moreover, HCMs were used to fabricate a highly sensitive gas detector, which is a rapid and effective method for the selection of catalysts or the detection of environmental deleterious gases.

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering

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

Yuan, Xueming; Duan, Yonghao; He, Lilin

A systematic study was done to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110 °C for 3 h at biomass loadings of 5, 10, 15, 20 and 25 wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ~25 to 625 Å, enabling assessment of contributions of pores with different sizes to increased porositymore » after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role.« less

Tungsten tetraboride, an inexpensive superhard material

PubMed Central

Mohammadi, Reza; Lech, Andrew T.; Xie, Miao; Weaver, Beth E.; Yeung, Michael T.; Tolbert, Sarah H.; Kaner, Richard B.

2011-01-01

Tungsten tetraboride (WB4) is an interesting candidate as a less expensive member of the growing group of superhard transition metal borides. WB4 was successfully synthesized by arc melting from the elements. Characterization using powder X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDX) indicates that the as-synthesized material is phase pure. The zero-pressure bulk modulus, as measured by high-pressure X-ray diffraction for WB4, is 339 GPa. Mechanical testing using microindentation gives a Vickers hardness of 43.3 ± 2.9 GPa under an applied load of 0.49 N. Various ratios of rhenium were added to WB4 in an attempt to increase hardness. With the addition of 1 at.% Re, the Vickers hardness increased to approximately 50 GPa at 0.49 N. Powders of tungsten tetraboride with and without 1 at.% Re addition are thermally stable up to approximately 400 °C in air as measured by thermal gravimetric analysis. PMID:21690363

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering.

PubMed

Yuan, Xueming; Duan, Yonghao; He, Lilin; Singh, Seema; Simmons, Blake; Cheng, Gang

2017-05-01

A systematic study was performed to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110°C for 3h at biomass loadings of 5, 10, 15, 20 and 25wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ∼25 to 625Å, enabling assessment of contributions of pores with different sizes to increased porosity after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Improvement of Strength-Toughness-Hardness Balance in Large Cross-Section 718H Pre-Hardened Mold Steel

PubMed Central

Liu, Hanghang; Fu, Paixian; Liu, Hongwei; Li, Dianzhong

2018-01-01

The strength-toughness combination and hardness uniformity in large cross-section 718H pre-hardened mold steel from a 20 ton ingot were investigated with three different heat treatments for industrial applications. The different microstructures, including tempered martensite, lower bainite, and retained austenite, were obtained at equivalent hardness. The microstructures were characterized by using metallographic observations, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and electron back-scattered diffraction (EBSD). The mechanical properties were compared by tensile, Charpy U-notch impact and hardness uniformity tests at room temperature. The results showed that the test steels after normalizing-quenching-tempering (N-QT) possessed the best strength-toughness combination and hardness uniformity compared with the conventional quenched-tempered (QT) steel. In addition, the test steel after austempering-tempering (A-T) demonstrated the worse hardness uniformity and lower yield strength while possessing relatively higher elongation (17%) compared with the samples after N-QT (14.5%) treatments. The better ductility of A-T steel mainly depended on the amount and morphology of retained austenite and thermal/deformation-induced twined martensite. This work elucidates the mechanisms of microstructure evolution during heat treatments and will highly improve the strength-toughness-hardness trade-off in large cross-section steels. PMID:29642642

Degradation of bisphenol A in water by the heterogeneous photo-Fenton.

PubMed

Jiang, Chuanrui; Xu, Zhencheng; Guo, Qingwei; Zhuo, Qiongfang

2014-01-01

Bisphenol A (BPA) is a kind of a controversial endocrine disruptor, and is ubiquitous in environment. The degradation of BPA with the heterogeneous photo-Fenton system was demonstrated in this study. The Fe-Y molecular sieve catalyst was prepared with the ion exchange method, and it was characterized by X-ray radiation diffraction (XRD). The effects ofpH, initial concentration of H2O2, initial BPA concentration, and irradiation intensity on the degradation of BPA were investigated. The service life and iron solubility of catalyst were also tested. XRD test shows that the major phase of the Fe-Y catalyst was Fe2O3. The method of heterogeneous photo-Fenton with Fe-Y catalyst was superior to photolysis, photo-oxidation with only hydrogen, heterogeneous Fenton, and homogeneous photo-Fenton approaches. pH value had no obvious effects on BPA degradation over the range of 2.2-7.2. The initial concentration of H2O2 had an optimal value of 20 x 10(-4) mol/L. The decrease in initial concentration of BPA was favourable for degradation. The intensity of ultraviolet irradiation has no obvious effect on the BPA removal. The stability tests indicated that the Fe-Y catalyst can be reused and iron solubility concentration ranged from NA to 0.0062 mg/L. Based on the results, the heterogeneous photo-Fenton treatment is the available method for the degradation of BPA.

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.

Polyimide Nanocomposites Prepared from High-Temperature, Reduced Charge Organoclays

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Ladislaw, J. S.; Smith, J. G., Jr.; Connell, J. W.

2003-01-01

Montmorillonite clays modified with the dihydrochloride salt of 1,3-bis(3-aminophenoxy)benzene (APB) were used in the preparation of polyimide/organoclay hybrid films. Organoclays with varying surface charge based upon APB were prepared and examined for their dispersion behavior in the polymer matrix. High molecular weight poly(amide acid) solutions were prepared in the presence of the organoclays. Films were cast and subsequently heated to 300C to cause imidization. The resulting nanocomposite films, containing 3 wt% of organoclay, were characterized by transmission electron microscopy and X-ray diffraction. The clay's cation exchange capacity (CEC) played a key role in determining the extent of dispersion in the polyimide matrix. Considerable dispersion was observed in some of the nanocomposite films. The most effective organoclay was found to have a CEC of 0.70 meq/g. Nanocomposite films prepared with 3-8 wt% of this organoclay were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin-film tensile testing. High levels of clay dispersion could be achieved even at the higher clay loadings. Results from mechanical testing revealed that while the moduli of the nanocomposites increased with increasing clay loadings, both strength and elongation decreased.

Chitosan/graphene oxide biocomposite film from pencil rod

NASA Astrophysics Data System (ADS)

Gea, S.; Sari, J. N.; Bulan, R.; Piliang, A.; Amaturrahim, S. A.; Hutapea, Y. A.

2018-03-01

Graphene Oxide (GO) has been succesfully synthesized using Hummber method from graphite powder of pencil rod. The excellent solubility of graphene oxide (GO)in water imparts its feasibilty as new filler for reinforcement hydrophilic biopolymers. In this research, the biocomposite film was fabricated from chitosan/graphene oxide. The characteristics of graphene oxide were investigated using Fourier Transform Infrared (FT-IR) and X-ray Diffraction (XRD). The results of the XRD showed graphene structur in 2θ, appeared at 9.0715°with interlayer spacing was about 9.74063Å. Preparation films with several variations of chitosan/graphene oxide was done by casting method and characterized by mechanical and morphological analysis. The mechanical properties of the tensile test in the film show that the film CS/GO (85: 15)% has the optimum Young’s modulus size of 2.9 GPa compared to other variations of CS / GO film. Morphological analysis film CS/GO (85:15)% by Scanning Electron Microscopy (SEM), the obtained biocomposites film showed fine dispersion of GO in the CS matrix and could mix each other homogeneously.

Tribological and corrosion behaviour of electroless Ni-B coating possessing a blackberry like structure

NASA Astrophysics Data System (ADS)

Bülbül, Ferhat; Altun, Hikmet; Küçük, Özkan; Ezirmik, Vefa

2012-08-01

This study aims to evaluate the tribological and corrosion properties of the electroless Ni-B coating deposited on AISI 304 stainless steels. The microstructure of the coating was characterized using x-ray diffraction (XRD) and scanning electron microscopy-energy dispersive spectrometry (SEM-EDS). XRD analysis revealed that the prepared coating possessed an amorphous character. SEM-EDS investigation also indicated that a non-stoichiometric Ni-B coating was deposited with a columnar growth mechanism on the stainless steel substrate and the morphology of the growth surface was blackberry-like. The hardness and tribological properties were characterized by microhardness and a pin-on-disc wear test. The electroless Ni-B coated sample had a higher degree of hardness, a lower friction coefficient and a lower wear rate than the uncoated substrate. The electrochemical potentiodynamic polarization method was used to evaluate the corrosion resistance of the coating. The electroless Ni-B coating offered cathodic protection on the substrate by acting as a sacrificial anode although it was electrochemically more reactive than the stainless steel substrate.

Structure and colossal dielectric permittivity of Ca2TiCrO6 ceramics

NASA Astrophysics Data System (ADS)

Yan-Qing, Tan; Meng, Yan; Yong-Mei, Hao

2013-01-01

A colossal permittivity ceramic material, Ca2TiCrO6, was successfully synthesized by the conventional solid-state reaction, and was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray photoemission spectroscopy (XPS) and x-ray diffraction (XRD). Rietveld refinement of XRD data indicated that the material crystallized in orthorhombic structure with space group pbnm. SEM displayed Ca2TiCrO6 ceramic grains packed uniformly with the size range 5-20 µm. XPS analyses indicated that elemental chromium and titanium of the material were in mixed valence. The corresponding dielectric property was tested in the frequency range 1 kHz-1 MHz and the temperature range 213-453 K, and the ceramics exhibited a relaxation-like dielectric behaviour. Importantly, the permittivity of Ca2TiCrO6 could reach 80 000 at 298 K (100 Hz) and was maintained at 40 000 up to 398 K at 1 MHz, which could be attributed to the ion disorder and mixed valence of Cr3+/Cr6+ and Ti3+/Ti4+.

Synergistic effect on the visible light activity of Ti3+ doped TiO2 nanorods/boron doped graphene composite

PubMed Central

Xing, Mingyang; Li, Xiao; Zhang, Jinlong

2014-01-01

TiO2/graphene (TiO2-x/GR) composites, which are Ti3+ self-doped TiO2 nanorods decorated on boron doped graphene sheets, were synthesized via a simple one-step hydrothermal method using low-cost NaBH4 as both a reducing agent and a boron dopant on graphene. The resulting TiO2 nanorods were about 200 nm in length with exposed (100) and (010) facets. The samples were characterized by X-ray diffraction (XRD), UV-visible diffuse reflectance spectroscopy, X-band electron paramagnetic resonance (EPR), X-ray photoelectron spectra (XPS), transmission electron microscope (TEM), Raman, and Fourier-transform infrared spectroscopy (FTIR). The XRD results suggest that the prepared samples have an anatase crystalline structure. All of the composites tested exhibited improved photocatalytic activities as measured by the degradation of methylene blue and phenol under visible light irradiation. This improvement was attributed to the synergistic effect of Ti3+ self-doping on TiO2 nanorods and boron doping on graphene. PMID:24974890

In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

NASA Astrophysics Data System (ADS)

Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

2018-01-01

The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

Study of the presence of fluorine in the recycled fractions during carbothermal treatment of EAF dust.

PubMed

Menad, N; Ayala, J N; Garcia-Carcedo, Fernando; Ruiz-Ayúcar, E; Hernández, A

2003-01-01

Carbothermal treatment tests of electric arc furnace dusts (EAFD) using the Waelz kiln process were carried out in pilot-scale for the production of zinc oxide. The association of halides in the EAFD, and the recycled products, such as zinc oxide fumes and high-grade iron contents fractions were examined by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. XRD reveals the presence of chlorine and fluorine in the dusts in the form of KCl, NaCl and CaF2. An ultra-pure fraction of zinc was obtained after the Double Leaching Waelz Oxide (DLWO) process was performed on the zinc oxide fumes. The halide contents were reduced to approximately 100 ppm Cl and 700 ppm F. The rest of these elements are in the form of CaF2. About 65% F is volatilised as lead and zinc fluorides, 15% is expected in the magnetic fractions and 20% in non-magnetic fractions as CaF2 and MnF2, respectively.

Studies on Magnetron Sputtered ZnO-Ag Films: Adhesion Activity of S. aureus

NASA Astrophysics Data System (ADS)

Geetha, S. R.; Dhivya, P.; Raj, P. Deepak; Sridharan, M.; Princy, S. Adline

Zinc oxide (ZnO) thin films have been deposited onto thoroughly cleaned stainless steel (AISI SS 304) substrates by reactive direct current (dc) magnetron sputtering and the films were doped with silver (Ag). The prepared thin films were analyzed using X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM) to investigate the structural and morphological properties. The thickness values of the films were in the range of 194 to 256nm. XRD results revealed that the films were crystalline with preferred (002) orientation. Grain size values of pure ZnO films were found to be 19.82-23.72nm. On introducing Ag into ZnO film, the micro-structural properties varied. Adhesion test was carried out with Staphylococcus aureus (S. aureus) in order to know the adherence property of the deposited films. Colony formation units (CFU) were counted manually and bacterial adhesion inhibition (BAI) was calculated. We observed a decrease in the CFU on doping Ag in the ZnO films. BAI of the film deposited at - 100 V substrate bias was found to be increased on Ag doping from 69 to 88%.

Influence of Casting Section Thickness on Fatigue Strength of Austempered Ductile Iron

NASA Astrophysics Data System (ADS)

Olawale, J. O.; Ibitoye, S. A.

2017-10-01

The influence of casting section thickness on fatigue strength of austempered ductile iron was investigated in this study. ASTM A536 65-45-12 grade of ductile iron was produced, machined into round samples of 10, 15, 20 and 25 mm diameter, austenitized at a temperature of 820 °C, quenched into an austempering temperature (TA) of 300 and 375 °C and allowed to be isothermally transformed at these temperatures for a fixed period of 2 h. From the samples, fatigue test specimens were machined to conform to ASTM E-466. Scanning electron microscopy (SEM) and x-ray diffraction (XRD) methods were used to characterize microstructural morphology and phase distribution of heat-treated samples. The fatigue strength decreases as the section thickness increases. The SEM image and XRD patterns show a matrix of acicular ferrite and carbon-stabilized austenite with ferrite coarsening and volume fraction of austenite reducing as the section thickness increases. The study concluded that the higher the value of carbon-stabilized austenite the higher the fatigue strength while it decreases as the ausferrite structure becomes coarse.

Apatite layer growth on glassy Zr48Cu36Al8Ag8 sputtered titanium for potential biomedical applications

NASA Astrophysics Data System (ADS)

Thanka Rajan, S.; Karthika, M.; Bendavid, Avi; Subramanian, B.

2016-04-01

The bioactivity of magnetron sputtered thin film metallic glasses (TFMGs) of Zr48Cu36Al8Ag8 (at.%) on titanium substrates was tested for bio implant applications. The structural and elemental compositions of TFMGs were analyzed by XRD, XPS and EDAX. X-ray diffraction analysis displayed a broad hump around the incident angle of 30-50°, suggesting that the coatings possess a glassy structure. An in situ crystal growth of hydroxyapatite was observed by soaking the sputtered specimen in simulated body fluid (SBF). The nucleation and growth of a calcium phosphate (Ca-P) bone-like hydroxyapatite on Zr48Cu36Al8Ag8 (at.%) TFMG from SBF was investigated by using XRD, AFM and SEM. The presence of calcium and phosphorus elements was confirmed by EDAX and XPS. In vitro electrochemical corrosion studies indicated that the Zr-based TFMG coating sustain in the stimulated body-fluid (SBF), exhibiting superior corrosion resistance with a lower corrosion penetration rate and electrochemical stability than the bare crystalline titanium substrate.

Kyllinga brevifolia mediated greener silver nanoparticles

NASA Astrophysics Data System (ADS)

Isa, Norain; Bakhari, Nor Aziyah; Sarijo, Siti Halimah; Aziz, Azizan; Lockman, Zainovia

2017-12-01

Kyllinga brevifolia extract (KBE) was studied in this research as capping as well as reducing agent for the synthesis of greener plant mediated silver nanoparticles. This research was conducted in order to identify the compounds in the KBE that probable to work as reductant for the synthesis of Kyllinga brevifolia-mediated silver nanoparticles (AgNPs). Screening test such as Thin Layer Chromatography (TLC), Fourier Transform Infra-Red (FTIR), Carlo Erba Elemental analysis and Gas Chromatography-Mass Spectroscopy (GCMS) were used in identifying the natural compounds in KBE. The as-prepared AgNPs were characterized by UV-vis spectroscopy (UV-vis), Transmission Electron Microscope (TEM) and X-ray Diffraction (XRD). The TEM images showed that the as-synthesized silver have quasi-spherical particles are distributed uniformly with a narrow distribution from 5 nm to 40 nm. The XRD results demonstrated that the obtained AgNPs were face centre-cubic (FCC) structure. The catalytic activity of AgNPs on reduction of methylene blue (MB) using sodium borohydride (SB) was analyzed using UV-vis spectroscopy. This study showed that the efficacy of mediated AgNPs in catalysing the reduction of MB.

Non-Metal Doped Titania Photocatalysts for the Degradation of Neonicotinoid Insecticides Under Visible Light Irradiation.

PubMed

Joseph, Amala Infant Joice; Thiripuranthagan, Sivakumar

2018-05-01

Recombination of e-/h+ pair, the major issue of any titania based photocatalytic material, is addressed here by doping non-metals such as C, N, B, F into the lattice of nano TiO2. The as-synthesised catalysts were characterized by using various instrumental techniques such as X-ray diffraction (XRD), UV-Diffuse reflectance spectroscopy (UV-DRS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Nanosize of titania was confirmed by both XRD and TEM studies. Visible light inactivity of TiO2 is overcome by C, N, B, F doped titania catalysts in the degradation of neonicotinoid type insecticides namely imidacloprid (IMI) and thiamethoxam (TMX). The degradation efficiencies of the catalysts under different irradiations namely UV, visible and solar were compared. Among the catalysts, CNBF/TiO2 degraded IMI completely at 150, 240 and 330 min whereas TMX has been degraded completely at 210, 270 and 420 min under UV, solar and visible irradiations respectively. The recyclability test of CNBF/TiO2 confirmed its stability towards photocatalytic reaction.

Corrosion Resistance of a Sand Particle-Modified Enamel Coating Applied to Smooth Steel Bars

PubMed Central

Tang, Fujian; Chen, Genda; Brow, Richard K.; Koenigstein, Michael L.

2014-01-01

The protective performance of a sand particle-modified enamel coating on reinforcing steel bars was evaluated in 3.5 wt% NaCl solution by electrochemical impedance spectroscopy (EIS). Seven percentages of sand particles by weight were investigated: 0%, 5%, 10%, 20%, 30%, 50% and 70%. The phase composition of the enamel coating and sand particles were determined with the X-ray diffraction (XRD) technique. The surface and cross-sectional morphologies of the sand particle-modified enamel coating were characterized using scanning electron microscopy (SEM). XRD tests revealed three phases of sand particles: SiO2, CaCO3 and MgCO3. SEM images demonstrated that the enamel coating wetted well with the sand particles. However, a weak enamel coating zone was formed around the sand particles due to concentrated air bubbles, leading to micro-cracks as hydrogen gas pressure builds up and exceeds the tensile strength of the weak zone. As a result, the addition of sand particles into the enamel coating reduced both the coating and corrosion resistances. PMID:28788203

A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

NASA Astrophysics Data System (ADS)

Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

2013-11-01

A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

Boosted surface acidity in TiO2 and Al2O3-TiO2 nanotubes as catalytic supports

NASA Astrophysics Data System (ADS)

Camposeco, R.; Castillo, S.; Mejía-Centeno, Isidro; Navarrete, J.; Nava, N.

2015-11-01

In this study, titanate nanotubes (NT) and titanate nanotubes with alumina (NT-Al) were studied as solid acid catalytic supports to show the relationship between the kind of acidity and catalytic activity. The supports were characterized by XRD, TEM, FTIR, XPS, and tested in the SCR-NO with NH3. It was found that the amount of Brönsted acid sites was maintained and the Lewis acid sites were significantly affected by the addition of alumina (1, 3, 5 and 10 wt.%); such acidity was higher than that of the titanate nanotubes (NT) by two-fold. To confirm the formation of titanate nanotubes and titanate nanotubes with alumina, transmission electron microscopy (TEM) was used. X-ray diffraction (XRD) revealed the formation of the H2Ti4O9·H2O phase. All NT and NT-Al supports presented catalytic activity to remove NO with NH3 under lean conditions, confirming the presence of an important amount of Brönsted and Lewis acid sites in both NT and NT-Al supports.

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

Kanel, S. R.; Clement, T. P.; Barnett, M. O.

Synthetic nano-scale hydroxyapatite (NHA) was prepared and characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods. The XRD data confirmed that the crystalline structure and chemical composition of NHA correspond to Ca 5 OH(PO 4 ) 3 . The SEM data confirmed the size of NHA to be less than 50 nm. A two-dimensional physical model packed with saturated porous media was used to study the transport characteristics of NHA under constant flow conditions. The data show that the transport patterns of NHA were almost identical to tracer transport patterns. This result indicates that the NHA material can movemore » with water like a tracer, and its movement was neither retarded nor influenced by any physicochemical interactions and/or density effects. We have also tested the reactivity of NHA with 1 mg/L hexavalent uranium (U(VI)) and found that complete removal of U(VI) is possible using 0.5 g/L NHA at pH 5 to 6. Our results demonstrate that NHA has the potential to be injected as a dilute slurry for in situ treatment of U(VI)-contaminated groundwater systems.« less

Phase transition of AISI type 304L stainless steel induced by severe plastic deformation via cryo-rolling

NASA Astrophysics Data System (ADS)

Shit, Gopinath; Bhaskar, Pragna; Ningshen, S.; Dasgupta, A.; Mudali, U. Kamachi; Bhaduri, A. Kumar

2017-05-01

The phase transition induced by Severe Plastic Deformation (SPD) was confirmed in metastable AISI type 304L austenitic stainless steel (SS). SPD via cryo-rolling in liquid nitrogen (L-N2) temperature is the adopted route for correlating the phase transition and corrosion resistance. The thickness of the annealed AISI type 304L SS at 1050°C sheet was reduced step by step from 15% to 50% of its initial thickness. The phase changes and phase transformation are qualitatively analyzed by X-Ray Diffraction (XRD) method. During the process, the XRD of each Cryo-Rolled and annealed sample was analyzed and different phases and phase transitions are measured. The investigated AISI type 304L SS by SPD reveals a microstructure of γ-austenite; α'-marternsite and ɛ-martensite formation depending on the percentage of cryo-rolling. The Vickers hardness (HV) of the samples is also measured. The corrosion rate of the annealed sheet and cryo rolled sample was estimated in boiling nitric acid as per ASTM A-262 practice-C test.

Determination of layer-charge characteristics of smectites

USGS Publications Warehouse

Christidis, G.E.; Eberl, D.D.

2003-01-01

A new method for calculation of layer charge and charge distribution of smectites is proposed. The method is based on comparisons between X-ray diffraction (XRD) patterns of K-saturated, ethylene glycol-solvated, oriented samples and calculated XRD patterns for three-component, mixed-layer systems. For the calculated patterns it is assumed that the measured patterns can be modeled as random interstratifications of fully expanding 17.1 Å layers, partially expanding 13.5 Å layers and non-expanding 9.98 Å layers. The technique was tested using 29 well characterized smectites. According to their XRD patterns, smectites were classified as group 1 (low-charge smectites) and group 2 (high-charge smectites). The boundary between the two groups is at a layer charge of −0.46 equivalents per half unit-cell. Low-charge smectites are dominated by 17.1 Å layers, whereas high-charge smectites contain only 20% fully expandable layers on average. Smectite properties and industrial applications may be dictated by the proportion of 17.1 Å layers present. Non-expanding layers may control the behavior of smectites during weathering, facilitating the formation of illite layers after subsequent cycles of wetting and drying. The precision of the method is better than 3.5% at a layer charge of −0.50; therefore the method should be useful for basic research and for industrial purposes.

High-resolution Measurement of Contact Ion-pair Structures in Aqueous RbCl Solutions from the Simultaneous Corefinement of their Rb and Cl K-edge XAFS and XRD Spectra

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

Pham, Van-Thai; Fulton, John L.

2016-06-21

In concentrated solutions of aqueous RbCl, all of the Rb+ and Cl- ions exist as contact ion pairs. This full structural assessment is derived from the refinement of three independent experimental measurements: the Rb and Cl K-edge x-ray absorption fine structure (XAFS) and the x-ray diffraction spectra (XRD). This simultaneous refinement of the XAFS and XRD data provides high accuracy since each method probes the structure of different local regions about the ions with high sensitivity. At high RbCl concentration (6 m (mol/kg )) the solution is dominated by Rb+ - Cl- contact ion pairs yielding an average of 1.5more » pairs at an Rb-Cl distance of 3.24 Å. Upon formation of these ion pairs, approximately 1.1 waters molecules are displaced from the Rb+ and 1.4 water molecules from Cl-. The hydration shells about both the cation and anion are also determined. These results greatly improve the understanding of monovalent ions and provide a basis for testing the Rb+-Cl- interaction potentials used in molecular dynamics (MD) simulation. This research was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Biosciences.« less

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

PubMed Central

Shi, Xinchang

2017-01-01

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

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.

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.

Green synthesis of silver nanoparticles using methanolic root extracts of Diospyros paniculata and their antimicrobial activities.

PubMed

Rao, N Hanumanta; N, Lakshmidevi; Pammi, S V N; Kollu, Pratap; S, Ganapaty; P, Lakshmi

2016-05-01

Since the discovery and subsequent widespread use of antibiotics, a variety of bacterial species of human and animal origin have developed numerous mechanisms that render bacteria resistant to some, and in certain cases to nearly all antibiotics, thereby limiting the treatment options and compromising effective therapy. In the present study, the green synthesis of nanoparticles is carried out by the reduction of silver acetate in the presence of crude methanolic root extracts of Diospyros paniculata, a member of family Ebenaceae. The UV-Vis absorption spectrum of the biologically reduced reaction mixture showed the surface plasmon peak at 428 nm, a characteristic peak of silver nanoparticles. X-ray diffraction (XRD) analysis confirmed the face-centered cubic crystalline structure of metallic silver. The average diameter of Ag NPs is about 17 nm from Transmission Electron Microscopy (TEM) which is in good agreement with the average crystallite size (19 nm) calculated from XRD analysis. Further the study has been extended to the antimicrobial activity against test pathogenic Gram (+), Gram (-) bacterial and fungal strains. The biologically synthesized silver nanoparticles showed promising activity against all the tested pathogenic strains and the activity has been enhanced with the increased dose levels. Copyright © 2016 Elsevier B.V. All rights reserved.

Growth and characterization of novel organic 3-Hydroxy Benzaldehyde-N-methyl 4 Stilbazolium Tosylate crystals for NLO applications.

PubMed

Jagannathan, K; Umarani, P; Ratchagar, V; Ramesh, V; Kalainathan, S

2016-01-15

The 3-Hydroxy Benzaldehyde-N-methyl 4-Stilbazolium Tosylate (3- HBST) is a new organic NLO crystal and it is a new derivative in stilbazolium tosylate family. In this work we have synthesized 3-HBST and the single crystal was grown by conventional slow cooling method. The structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction (XRD) technique and it is exhibiting good crystalline nature which is observed from the powder XRD. In order to check the crystalline quality the rocking curve was recorded using multi crystal X-ray diffractometer. The functional groups were identified from both FTIR and NMR spectral analyses. The π-π* and n-π* optical transition energy levels were estimated from the absorption peaks. The NLO property was confirmed by measuring relative SHG efficiency by Kurtz powder test; it shows 24 times higher SHG efficiency than that of urea. In order to test the mechanical stability the Vickers and Knoop micro hardness measurement were carried out and found that the micro hardness number decreases with increasing load. The melting point was determined from Differential Scanning Colorimetry (DSC). Copyright © 2015 Elsevier B.V. All rights reserved.

PdRu/C catalysts for ethanol oxidation in anion-exchange membrane direct ethanol fuel cells

NASA Astrophysics Data System (ADS)

Ma, Liang; He, Hui; Hsu, Andrew; Chen, Rongrong

2013-11-01

Carbon supported PdRu catalysts with various Pd:Ru atomic ratios were synthesized by impregnation method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), electrochemical half-cell tests, and the anion-exchange membrane direct ethanol fuel cell (AEM-DEFC) tests. XRD results suggest that the PdRu metal exists on carbon support in an alloy form. TEM study shows that the bimetallic PdRu/C catalysts have slightly smaller average particle size than the single metal Pd/C catalyst. Lower onset potential and peak potential and much higher steady state current for ethanol oxidation in alkaline media were observed on the bimetallic catalysts (PdxRuy/C) than on the Pd/C, while the activity for ethanol oxidation on the pure Ru/C was not noticeable. By using Pd/C anode catalysts and MnO2 cathode catalysts, AEM-DEFCs free from the expensive Pt catalyst were assembled. The AEM DEFC using the bimetallic Pd3Ru/C anode catalyst showed a peak power density as high as 176 mW cm-2 at 80 °C, about 1.8 times higher than that using the single metal Pd/C catalyst. The role of Ru for enhancing the EOR activity of Pd/C catalysts is discussed.

Preparation and Characterization of Liquisolid Compacts for Improved Dissolution of Telmisartan

PubMed Central

Narra, Nataraj; Rama Rao, Tadikonda

2014-01-01

The objective of the present work was to obtain pH independent and improved dissolution profile for a poorly soluble drug, telmisartan using liquisolid compacts. Liquisolid compacts were prepared using Transcutol HP as vehicle, Avicel PH102 as carrier, and Aerosil 200 as a coating material. The formulations were evaluated for drug excipient interactions, change in crystallinity of drug, flow properties, and general quality control tests of tablets using Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), X-ray diffraction (XRD), angle of repose, and various pharmacopoeial tests. In vitro dissolution studies were performed at three pH conditions (1.2, 4.5 and 7.4). Stability studies were performed at 40°C and 75% RH for three months. The formulation was found to comply with Indian pharmacopoeial limits for tablets. FTIR studies confirmed no interaction between drug and excipients. XRD and DSC studies indicate change/reduction in crystallinity of drug. Dissolution media were selected based on the solubility studies. The optimized formulation showed pH independent release profile with significant improvement (P < 0.005) in dissolution compared to plain drug and conventional marketed formulation. No significant difference was seen in the tablet properties, and drug release profile after storage for 3 months. PMID:25371826

High pressure infiltration sintering behavior of WC-Co alloys

NASA Astrophysics Data System (ADS)

Fan, Xiaoqin; He, Duanwei; Wang, Pei; Li, Dong; Liu, Yinjuan; Ma, Dejiang; Du, Yanchun; Gao, Shangpan; Kou, Zili

2016-10-01

In this paper, two average tungsten carbide particle sizes of 2, 0.5 μm are placed respectively, in contact with a WC-16Co substrate, pressed at the pressure of 4.5-5.5 GPa, and heated to temperatures ranging from 1350°C to 1500°C in a large-volume cubic press. During the process Co was forced out of the WC-16Co substrate into the compressed powder. The resulting infiltrated samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), Vickers hardness and cutting performance tests. The results of XRD confirmed that the sintered bulks have WC and Co phases. The scanning electron microscopy (SEM) analysis reveals that the WC grains in well-sintered alloys are round in shape and cobalt with lower content is uniformly dispersed in the WC grain boundaries. The sintered sub-micron WC-Co alloy with a cobalt content of 3.8 wt% exhibits a prominent combination of high hardness value of 23.1 GPa and a large fracture toughness value of 8.6 MPa m½. The high-speed cutting tests indicating its cutting performance is significantly superior to the commercial YG6X (WC-6 wt%Co with WC grain size of 0.5 μm).

Efficient visible-light photocatalytic degradation of sulfadiazine sodium with hierarchical Bi₇O₉I₃under solar irradiation.

PubMed

Xu, MengMeng; Zhao, YaLei; Yan, QiShe

2015-01-01

Bi₇O₉I₃, a kind of visible-light-responsive photocatalyst, with hierarchical micro/nano-architecture was successfully synthesized by oil-bath heating method, with ethylene glycol as solvent, and applied to degrade sulfonamide antibiotics. The as-prepared product was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-visible diffuse reflection spectra and scanning electron microscopy (SEM). XRD and XPS tests confirmed that the product was indeed Bi₇O₉I₃. The result of SEM observation shows that the as-synthesized Bi₇O₉I₃ consists of a large number of micro-sheets with parallel rectangle structure. The optical test exhibited strong photoabsorption in visible light irradiation, with 617 nm of absorption edges. Moreover, the difference in the photocatalytic efficiency of as-prepared Bi₇O₉I₃ at different seasons of a whole year was investigated in this study. The chemical oxygen demand removal efficiency and concentration of NO(3)(-) and SO(4)(2-) of solution after reaction were also researched to confirm whether degradation of the pollutant was complete; the results indicated a high mineralization capacity of Bi₇O₉I₃. The as-synthesized Bi₇O₉I₃exhibits an excellent oxidizing capacity of sulfadiazine sodium and favorable stability during the photocatalytic reaction.

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

Metallurgical and electrochemical characterization of contemporary silver-based soldering alloys.

PubMed

Ntasi, Argyro; Al Jabbari, Youssef; Mueller, Wolf Dieter; Eliades, George; Zinelis, Spiros

2014-05-01

To investigate the microstructure, hardness, and electrochemical behavior of four contemporary Ag-based soldering alloys used for manufacturing orthodontic appliances. The Ag-based alloys tested were Dentaurum Universal Silver Solder (DEN), Orthodontic Solders (LEO), Ortho Dental Universal Solder (NOB), and Silver Solder (ORT). Five disk-shaped specimens were produced for each alloy, and after metallographic preparation their microstructural features, elemental composition, and hardness were determined by scanning electron microscopy with energy-dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD) analysis, and Vickers hardness testing. The electrochemical properties were evaluated by anodic potentiodynamic scanning in 0.9% NaCl and Ringer's solutions. Hardness, corrosion current (Icorr), and corrosion potential (Ecorr) were statistically analyzed by one-way analysis of variance and Tukey test (α=.05). EDX analysis showed that all materials belong to the Ag-Zn-Cu ternary system. Three different mean atomic contrast phases were identified for LEO and ORT and two for DEN and NOB. According to XRD analysis, all materials consisted of Ag-rich and Cu-rich face-centered cubic phases. Hardness testing classified the materials in descending order as follows: DEN, 155±3; NOB, 149±3; ORT, 141±4; and LEO, 136±8. Significant differences were found for Icorr of NOB in Ringer's solution and Ecorr of DEN in 0.9% NaCl solution. Ag-based soldering alloys demonstrate great diversity in their elemental composition, phase size and distribution, hardness, and electrochemical properties. These differences may anticipate variations in their clinical performance.

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.

Removal of copper (II) ion from aqueous solution using zeolite Y synthesized from rice husk ash: Equilibrium and kinetic study

NASA Astrophysics Data System (ADS)

Tuyen, Nguyen Thi Kim; Nhan, Do Nguyen Thanh; Nhat, Trieu Thi; An, Ngo Thanh; Long, Nguyen Quang

2017-09-01

Zeolite Y was synthesized from silica of rice-husk ash using hydrothermal process. The crystalline structure FAU of zeolite Y was characterized by X-ray diffraction (XRD). Surface's area of the catalyst was determined by physic-adsorption method using BET model. The zeolite was examined for possibility of Cu2+ adsorbent by an ion-exchange mechanism. Various adsorption isotherm models, such as Langmuir, Freundlich and Dubinin-Radushkevich were tested for equilibrium study. The integration method was applied to find out the possible kinetic equation of the Cu2+ adsorption on the zeolite Y which obtained from cheap and locally available rice husk ash.

A facile sol-gel strategy for the scalable synthesis of CuFe2O4 nanoparticles with enhanced infrared radiation property: Influence of the synthesis conditions

NASA Astrophysics Data System (ADS)

Hou, Haili; Xu, Guoyue; Tan, Shujuan; Zhu, Yongmei

2017-09-01

CuFe2O4 particles were successfully engineered by a facile sol-gel method. The synthesized products were characterized physically by X-ray diffraction (XRD), scanning electron microscopy (SEM). Besides, the effects of the sintering temperature and the molar ration of citric acid/the total metal cations (CA/MC) on their infrared radiant properties were investigated at the wavelength of 3-5 μm. The highest infrared emission value ca. 0.911 was obtained when the test temperature was conducted at 800 °C, indicating its potential application in infrared heating, infrared coating and drying fields.

Dye adsorption into transition metal-doped zinc oxide nanoparticles supported on natural zeolites to solve wastewater issue

NASA Astrophysics Data System (ADS)

Indra Pratiwi, Margaretha; Afifah, Nur; Saleh, Rosari

2017-03-01

In this work, Fe-doped zinc oxide/natural zeolite (Fe:ZnO/NZ) nanocomposites were prepared using the co-precipitation method with various NZ amounts. The nanocomposites were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis and thermogravimetric analysis (TGA). The nanocomposites were used to remove methylene blue (MB) dye from an aqueous solution. The effect of various NZ amounts and initial MB concentration were tested. The Pseudo-first-order and pseudo-second-order kinetic models were used to explain the adsorption mechanism. The Langmuir and the Freundlich isotherm models were used to fit the adsorption isotherms of the nanocomposites.

Single-Source Molecular Precursor for Synthesis of CdS Nanoparticles and Nanoflowers

NASA Astrophysics Data System (ADS)

Salavati-Niasari, Masoud; Sobhani, Azam

2012-04-01

CdS Semiconductor nanostructures were synthesized by using two different methods. Using triphenylphosphine (C18H15P) and oleylamine (C18H37N) as surfactant, CdS semiconductor nanocrystals with a size ranging from 30 to 90 nm can be synthesized by thermal decomposition of precursor [bis(thiosemicarbazide)cadmium(II)]. CdS nanoflowers were synthesized via hydrothermal decomposition of [bis(thiosemicarbazide) cadmium(II)] without any surfactant. X-ray diffraction (XRD) patterns confirm that the resulting samples were a pure hexagonal phase of CdS. The optical property test indicates that the absorption peak of the samples shifts towards short wavelength, and the blue shift phenomenon might be ascribed to the quantum effect.

[Topography structure and flocculation mechanism of polymeric phosphate ferric sulfate (PPFS)].

PubMed

Zheng, Huai-li; Zhang, Hui-qin; Jiang, Shao-jie; Li, Fang; Jiao, Shi-jun; Fang, Hui-li

2011-05-01

Characteristics of polymeric phosphate ferric sulfate (PPFS) were investigated using FTIR (Fourier transform infrared spectrometer), XRD (X-ray diffraction) and SEM (scanning electron microscope) in the present study. The formed PPFS structure and morphology were stereo meshwork, which was clustered and close to coral reef, synthesis of high charge density, bioactive polyhydroxy and mixed polynuclear complex PPFS. The results showed that charge neutralization of PPFS had not played a decisive role in the coagulation beaker test and the zeta potential proved that PPFS was largely affected by bridging and netting sweep. Therefore, the coagulation mechanisms of PPFS were mainly composed of charge neutralization, adsorption bridging and netting sweep mechanisms.

Catalytic dehydration of ethanol using transition metal oxide catalysts.

PubMed

Zaki, T

2005-04-15

The aim of this work is to study catalytic ethanol dehydration using different prepared catalysts, which include Fe(2)O(3), Mn(2)O(3), and calcined physical mixtures of both ferric and manganese oxides with alumina and/or silica gel. The physicochemical properties of these catalysts were investigated via X-ray powder diffraction (XRD), acidity measurement, and nitrogen adsorption-desorption at -196 degrees C. The catalytic activities of such catalysts were tested through conversion of ethanol at 200-500 degrees C using a catalytic flow system operated under atmospheric pressure. The results obtained indicated that the dehydration reaction on the catalyst relies on surface acidity, whereas the ethylene production selectivity depends on the catalyst chemical constituents.

Controlled release of Doxycycline from gum acacia/poly(sodium acrylate) microparticles for oral drug delivery.

PubMed

Bajpai, S K; Jadaun, Mamta; Bajpai, M; Jyotishi, Pooja; Shah, Farhan Ferooz; Tiwari, Seema

2017-11-01

In the present work, Doxycycline loaded gum acacia (GA)/poly(sodium acrylate) (SA) hydrogels were prepared for the oral drug delivery of model drug Doxycycline. The hydrogels were characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR) scanning electron microscopy (SEM) and Zeta potential. The dynamic release of Doxycycline was investigated in the physiological fluids at 37°C. Various kinetic models such as Power function model, Schott model and Higuchi model were applied to interpret the release data. Schott model was found to be most fitted. The Doxycycline loaded hydrogels were tested for their antibacterial action against E. coli. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterisation of titania/hydroxyapatite composite coatings obtained by sol-gel process.

PubMed

Milella, E; Cosentino, F; Licciulli, A; Massaro, C

2001-06-01

In the present work a titania network encapsulating a hydroxyapatite particulate phase is proposed as a bioceramic composite coating. The coating on a titanium substrate was produced starting from a sol containing a mixture of titania colloidal particles and hydroxyapatite submicron particles using the dip-coating technique. The microstructure, the morphology and the surface chemical composition of the coating were characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. Adhesion tests were also performed. These analyses showed that the obtained coating was chemically clean, homogeneous, rough, porous, with a low thickness and well-defined phase composition as well as a good adhesion to the substrate.

Paleoenvironmental Interpretation of drill core from Tugen Hills, Kenya through X-ray Diffraction

NASA Astrophysics Data System (ADS)

Minkara, K. E.; Rabideaux, N. M.; Deocampo, D.; Kingston, J.; Cohen, A. S.

2016-12-01

Paleoenvironmental reconstruction in regions of significant archeological and paleontological discoveries can be used to help better understand early hominin history in relation to environmental changes. Using X-ray diffraction (XRD) analysis of lacustrine sediments obtained from core material recovered during the Hominin Sites and Paleolakes Drilling Project (HSPDP) campaign at the Tugen Hills drilling site in central Kenya we can reconstruct a high-resolution record of paleoclimate and tectonics from the lake sediments during the Plio-Pleistocene. XRD analysis enables us to identify the mineralogical trends from the 227m core, which can be employed to understand the geochemical evolution of the basin. We want to test whether 23-kyr precessional cyclicity is the primary driver of environmental change at Lake Baringo, and how that change influenced vertebrate and hominin evolution. Our goals are to understand how the paleolake geochemically evolved over time and how the mineralogical characteristics are related to climate change. Preliminary results indicate discrete zones of carbonate and zeolite mineral occurrence, suggesting possible paleoclimate indicators of humidity versus aridity. Geochemical and sedimentological analysis will be required to distinguish primary lacustrine carbonate versus secondary or pedogenic carbonate, which does not carry a lacustrine signal. Quartz-rich intervals and diatomaceous sequences are distinct from zeolitic zones, suggesting variable salinities. Furthermore, hkl reflections of clay-rich bulk samples suggest varying relative abundances of kaolinite and smectite. As we extract clay fractions and analyze the clay mineralogy in further detail, this ratio may provide an indicator of paleoweathering intensity within the basin.

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

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

Selvaraj, Mahalakshmi; Department of Material Science, School of Chemistry, Madurai Kamaraj University, Tamilnadu Madurai-625 021; Venkatachalapathy, V.

2015-11-15

Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO{sub 3}) nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C) employing barium dichloride (BaCl{sub 2}) and titanium tetrachloride (TiCl{sub 4}) as precursors and sodium hydroxide (NaOH) as mineralizer for synthesis of BaTiO{sub 3} nanopowders. The as-prepared BaTiO{sub 3} powders were investigated for structural characteristics using x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phasemore » directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula). SEM and TEM analysis verified that the BaTiO{sub 3} nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED) shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric) phases of undoped BaTiO{sub 3} nanopowders can be stabilized by the sol-hydrothermal method.« less

Hydration behaviors of calcium silicate-based biomaterials.

PubMed

Lee, Yuan-Ling; Wang, Wen-Hsi; Lin, Feng-Huie; Lin, Chun-Pin

2017-06-01

Calcium silicate (CS)-based biomaterials, such as mineral trioxide aggregate (MTA), have become the most popular and convincing material used in restorative endodontic treatments. However, the commercially available CS-based biomaterials all contain different minor additives, which may affect their hydration behaviors and material properties. The purpose of this study was to evaluate the hydration behavior of CS-based biomaterials with/without minor additives. A novel CS-based biomaterial with a simplified composition, without mineral oxides as minor additives, was produced. The characteristics of this biomaterial during hydration were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectrometry. The hydration behaviors of commercially available gray and white MTAs with mineral oxide as minor additives were also evaluated for reference. For all three test materials, the XRD analysis revealed similar diffraction patterns after hydration, but MTAs presented a significant decrease in the intensities of Bi 2 O 3 -related peaks. SEM results demonstrated similar porous microstructures with some hexagonal and facetted crystals on the outer surfaces. In addition, compared to CS with a simplified composition, the FTIR plot indicated that hydrated MTAs with mineral oxides were better for the polymerization of calcium silicate hydrate (CSH), presenting Si-O band shifting to higher wave numbers, and contained more water crystals within CSH, presenting sharper bands for O-H bending. Mineral oxides might not result in significant changes in the crystal phases or microstructures during the hydration of CS-based biomaterials, but these compounds affected the hydration behavior at the molecular level. Copyright © 2016. Published by Elsevier B.V.

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

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.

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.

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

NASA Astrophysics Data System (ADS)

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

2016-03-01

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

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 ...

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.

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

Laboratory Testing of Silica Sol Grout in Coal Measure Mudstones

PubMed Central

Pan, Dongjiang; Zhang, Nong; Xie, Zhengzheng; Feng, Xiaowei; Kong, Yong

2016-01-01

The effectiveness of silica sol grout on mudstones is reported in this paper. Using X-ray diffraction (XRD), the study investigates how the silica sol grout modifies mudstone mineralogy. Micropore sizes and mechanical properties of the mudstone before and after grouting with four different materials were determined with a surface area/porosity analyser and by uniaxial compression. Tests show that, after grouting, up to 50% of the mesopore volumes can be filled with grout, the dominant pore diameter decreases from 100 nm to 10 nm, and the sealing capacity is increased. Uniaxial compression tests of silica sol grouted samples shows that their elastic modulus is 21%–38% and their uniaxial compressive strength is 16%–54% of the non-grouted samples. Peak strain, however, is greater by 150%–270%. After grouting, the sample failure mode changes from brittle to ductile. This paper provides an experimental test of anti-seepage and strengthening properties of silica sol. PMID:28774061

Novel Blend for Producing Porous Chitosan-Based Films Suitable for Biomedical Applications

PubMed Central

Nady, Norhan; Kandil, Sherif H.

2018-01-01

In this work, a chitosan–gelatin–ferulic acid blend was used in different ratios for preparing novel films that can be used in biomedical applications. Both acetic and formic acid were tested as solvents for the chitosan–gelatin–ferulic acid blend. Glycerol was tested as a plasticizer. The thickness, mechanical strength, static water contact angle and water uptake of the prepared films were determined. Also, the prepared films were characterized using different analysis techniques such as Fourier transform infrared spectroscopy (FT-IR) analysis, X-ray diffraction (XRD), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Acetic acid produced continuous compact surfaces that are not recommended for testing in biomedical applications. The plasticized chitosan–gelatin–ferulic acid blend, using formic acid solvent, produced novel hexagonal porous films with a pore size of around 10–14 µm. This blend is recommended for preparing films (scaffolds) for testing in biomedical applications as it has the advantage of a decreased thickness. PMID:29301357

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.

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.

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.

Austenite-martensite transformation in electrodeposited Fe70Pd30 NWs: a step towards making bio-nano-actuators tested on in vivo systems

NASA Astrophysics Data System (ADS)

Zuzek Rozman, K.; Pecko, D.; Trafela, S.; Samardzija, Z.; Spreitzer, M.; Jaglicic, Z.; Nadrah, P.; Zorko, M.; Bele, M.; Tisler, T.; Pintar, A.; Sturm, S.; Kostevsek, N.

2018-03-01

Fe69±3Pd31±3 nanowires (NWs) with lengths of a few microns and diameters of 200 nm were synthesized via template-assisted pulsed electrodeposition into alumina-based templates. The as-deposited Fe69±3Pd31±3 NWs exhibited α-Fe (bcc-solid solution of Fe, Pd) nanocrystalline structure as seen from the x-ray diffraction (XRD), that got confirmed by transmission electron microscopy (TEM) with some larger grains up 50 nm observed. Annealing of the as-deposited Fe69±3Pd31±3 NWs at 1173 K/45 min was followed by quenching in ice water and resulted in a transformation to the fcc crystal structure (XRD) with grain sizes up to 200 nm (TEM). To induce the austenite-to-martensite, i.e., fcc-to-fct phase transformation the fcc Fe69±3Pd31±3 NWs were cooled to 73 K. The XRD showed the disappearance of the (200) fcc reflection (at room temperature) and the appearance of the (200) fct reflection (at 73 K), confirming the fcc-to-fct transformation took place. The magnetic measurements revealed that the fcc Fe69±3Pd31±3 NWs measured at low temperatures (50 K) had a larger coercivity than at room temperature, which suggests the fct phase was present in the undercooled state, exhibiting a larger magnetocrystalline anisotropy than the fcc phase present at room temperature. As part of our interest in magnetic-shape-memory actuators, the as-deposited Fe69±3Pd31±3 NWs were tested for toxicity on zebrafish. In vivo tests showed no acute lethal or sub-lethal effects, which implies that the Fe69±3Pd31±3 NWs have the potential to be used as nano-actuators in biomedical applications.

Residual Stress Induced Mechanical Property Enhancement in Steel Encapsulated Light Metal Matrix Composites

NASA Astrophysics Data System (ADS)

Fudger, Sean James

Macro hybridized systems consisting of steel encapsulated light metal matrix composites (MMCs) were produced with the goal of creating a low cost/light weight composite system with enhanced mechanical properties. MMCs are frequently incorporated into advanced material systems due to their tailorable material properties. However, they often have insufficient ductility for many structural applications. The macro hybridized systems take advantage of the high strength, modulus, and damage tolerance of steels and high specific stiffness and low density of MMCs while mitigating the high density of steels and the poor ductility of MMCs. Furthermore, a coefficient of thermal expansion (CTE) mismatch induced residual compressive stress method is utilized as a means of improving the ductility of the MMCs and overall efficiency of the macro hybridized systems. Systems consisting of an A36, 304 stainless steel, or NitronicRTM 50 stainless steel shell filled with an Al-SiC, Al-Al2O3, or Mg-B4C MMC are evaluated in this work. Upon cooling from processing temperatures, residual strains are generated due to a CTE mismatch between each of the phases. The resulting systems offer higher specific properties and a more structurally efficient system can be attained. Mechanical testing was performed and improvements in yield stress, ultimate tensile stress, and ductility were observed. However, the combination of these dissimilar materials often results in the formation of intermetallic compounds. In certain loading situations, these typically brittle intermetallic layers can result in degraded performance. X-ray Diffraction (XRD), X-ray Energy Dispersive Spectroscopy (EDS), and Electron Backscatter Diffraction (EBSD) are utilized to characterize the intermetallic layer formation at the interface between the steel and MMC. As the residual stress condition in each phase has a large impact on the mechanical property improvement, accurate quantification of these strains/stresses is paramount. X-ray Diffraction Residual Stress Analysis (XRD-RSA) or Neutron diffraction was performed on numerous systems in multiple steel shell thickness variations. The analysis shows variation in the measured strain and stress results due to outer steel thickness, difference in CTE between materials, and relative position within the composite. Improvements in mechanical properties, namely ductility and yield stress, are a direct result of these measured strains.

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.

Corrosion resistance and in-vitro bioactivity of BaO containing Na2O-CaO-P2O5 phosphate glass-ceramic coating prepared on 316 L, duplex stainless steel 2205 and Ti6Al4V

NASA Astrophysics Data System (ADS)

Edathazhe, Akhila B.; Shashikala, H. D.

2018-03-01

The phosphate glass with composition 11Na2O-15BaO-29CaO-45P2O5 was coated on biomedical implant materials such as stainless steel 316 L, duplex stainless steel (DSS) 2205 and Ti6Al4V alloy by thermal enamelling method. The structural properties and composition of glass coated substrates were studied by x-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy dispersive x-ray spectroscopy (EDS) analysis. The coatings were partially crystalline in nature with porous structure and pore size varied from micro to nanometer range. The polarization curve was obtained for uncoated and coated substrates from electrochemical corrosion test which was conducted at 37 °C in Hank’s balanced salt solution (HBSS). The corrosion resistance of 316 L substrate increased after coating, whereas it decreased in case of DSS 2205 and Ti6Al4V. The XRD and SEM/EDS studies indicated the bioactive hydroxyapatite (HAp) layer formation on all the coated surfaces after electrochemical corrosion test, which improved the corrosion resistance. The observed electrochemical corrosion behavior can be explained based on protective HAp layer formation, composition and diffusion of ions on glass coated surfaces. The in-vitro bioactivity test was carried out at 37 °C in HBS solution for 14 days under static conditions for uncoated and coated substrates. pH and ion release rate measurements from the coated samples were conducted to substantiate the electrochemical corrosion test. The lower ion release rates of Na+ and Ca2+ from coated 316 L supported its higher electrochemical corrosion resistance among coated samples. Among the uncoated substrates, DSS showed higher electrochemical corrosion resistance. Amorphous calcium-phosphate (ACP) layer formation on all the coated substrates after in-vitro bioactivity test was confirmed by XRD, SEM/EDS and ion release measurements. The present work is a comparative study of corrosion resistance and bioactivity of glass coated and uncoated biomedical implants such as 316 L, DSS and Ti6Al4V.

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.

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.

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.

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...

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

[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

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.

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.

An effective approach to study the biocompatibility of Fe3O4 nanoparticles, graphene and their nanohybrid composite

NASA Astrophysics Data System (ADS)

Singh, Ashwani Kumar; Singh, Pallavi; Verma, Rajiv Kumar; Yadav, Suresh; Singh, Kedar; Srivastava, Amit

2018-02-01

The present manuscript describes a simple, facile and effective solvothermal route to synthesize Fe3O4 nanoparticles (Fe3O4 NPs), reduced graphene oxide nanosheets (rGO NSs) and Fe3O4/reduced graphene oxide nanohybrid composite (Fe3O4/rGO nanohybrid composite) and subsequently examines their comparative biocompatibilities. The as-obtained Fe3O4 NPs, rGO NSs and Fe3O4/rGO nanohybrid composite have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The XRD studies and scanning electron microscope confirmed the proper phase formation and the surface morphology of the as-synthesized products, respectively. The Raman spectra of Fe3O4 NPs show the strongest peak at 673 cm-1 which can be assigned to A1g peak of bare Fe3O4 NPs and it complements the XRD studies. Furthermore, the increment in the I D/I G ratio in the Fe3O4/rGO nanohybrid composite suggests the creation of defects in graphene sheets due to strain caused by Fe3O4 NPs. The biocompatibility of these samples has been tested using Lung cancer cell line H1299 through MTT assay. The MTT assay reveals that the nanohybrid composite endows more biocompatible and effectiveness than rGO NSs and Fe3O4 NPs individually, as anti-proliferative agent for cancer treatment.

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

PubMed

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

2013-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

Influence of ammonium hydroxide solution on LiMn2O4 nanostructures prepared by modified chemical bath method

NASA Astrophysics Data System (ADS)

Koao, Lehlohonolo F.; Motloung, Setumo V.; Motaung, Tshwafo E.; Kebede, Mesfin A.

2018-04-01

LiMn2O4 (LMO) powders were prepared by modified chemical bath deposition (CBD) method by varying ammonium hydroxide solution (AHS). The volume of the AHS was varied from 5 to 120 mL in order to determine the optimum volume that is needed for preparation of LMO powders. The effect of AHS volume on the structure, morphology, and electrochemical properties of LMO powders was investigated. The X-ray diffraction (XRD) patterns of the LMO powders correspond to the cubic spinel LMO phase. It was found that the XRD peaks increased in intensity with increasing volume of the AHS up to 20 mL. The estimated average grain sizes calculated using the XRD patterns were found to be in the order of 66 ± 1 nm. It was observed that the estimated average grain sizes increased up to 20 mL of AHS. The scanning electron microscopy (SEM) results revealed that the AHS volume does not influence the surface morphology of the prepared nano-powders. Elemental energy dispersive (EDS) analysis mapping conducted on the samples revealed homogeneous distribution of Mn and O for the sample synthesized with 120 mL of AHS. The UV-Vis spectra showed a red shift with an increase in AHS up 20 mL. The cyclic voltammetry and galvanostatic charge/discharge cycle testing confirmed that 20 mL of AHS has superior lithium ion kinetics and electrochemical performance.

Evaluation of local anesthetic effects of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles in Male Swiss mice.

PubMed

Jiang, Qiliang; Yu, Shashuang; Li, Xingwang; Ma, Chuangen; Li, Aixiang

2018-01-01

A simple approach for the synthesis of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles (IL-AgNPs) was reported in this work. The shape, size and surface morphology of the Lidocaine-Ibuprofen ionic liquid stabilized AgNPs were characterized by using spectroscopic and microscopic techniques such as Ultraviolet-visible spectroscopy (UV-Visible), X-ray diffraction (XRD) analysis, Selected area electron diffraction (SAED), Transmission electron microscopy (TEM). TEM analysis showed the formation of 20-30nm size of IL-AgNPs with very clear lattice fringes. SAED pattern confirmed the highly crystalline nature of fabricated IL stabilized AgNPs. EDS results confirmed the formation of nanosilver. The fabricated IL-AgNPs were studied for their local anesthetic effect in rats. The results of local anesthetic effect showed that the time for onset of action by IL-AgNPs is 10min, which is significantly higher than that for EMLA. Further, tactile test results confirmed the stronger and faster local anesthetic effect of IL-AgNPs when compared to that of EMLA. Copyright © 2017. Published by Elsevier B.V.

Characterization of biocomposites of sheep hydroxyapatite (SHA)/shellac/sugar as bone filler material

NASA Astrophysics Data System (ADS)

Triyono, Joko; Rizha, Yushak; Triyono, Teguh

2018-04-01

The use of biomaterials in orthopedics is increasing. This led to the growth of innovations in the field of medicine, one of them is the development of biomaterials. Study of Sheep Hydroxyapatite (SHA)/shellac/sugar biocomposite characterization was to determine the phase of the material, porosity, hardness and compressive strength of them. This research was conducted to develop new types of biomaterials that can be used as bone filler material. The analysis that used in this research was dry methods. The results showed that observation of XRD (X-Ray Diffraction) shows the pattern of diffraction 2θ: 31.6472°, 32.7753°, 32.0723°, The highest hardness of SHA/shellac/sugar ratio was 70:30% (7.38±0.1395 VHN) and the lowest at 50:50% (4.91±0.37 VHN). The highest Diametral Tensile Strength (DTS) test was 70:30% (5.43±1.395 MPa) and the lowest at 50:50% (3.10±0.26 MPa). SEM observations are performed to see the material porosity.

Strain softening during tension in cold drawn Cu–Ag alloys

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

Chang, L.L., E-mail: lilichang@sdu.edu.cn; Wen, S.; Li, S.L.

2015-10-15

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed tomore » be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.« less

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

NASA Astrophysics Data System (ADS)

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

2009-01-01

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

TiO₂ sol-gel for formaldehyde photodegradation using polymeric support: photocatalysis efficiency versus material stability.

PubMed

Curcio, Monique S; Oliveira, Michel P; Waldman, Walter R; Sánchez, Benigno; Canela, Maria Cristina

2015-01-01

Photocatalysts supported on polymers are not frequently used in heterogeneous photocatalysis because of problems such as wettability and stability that affect photocatalysis conditions. In this work, we used polypropylene as support for TiO2 sol-gel to evaluate its stability and efficiency under UV radiation. We also tested the effect of the thermo-pressing PP/TiO2 system on the photocatalytic efficiency and stability under UV radiation. The films were characterized by scanning electron microscopy (SEM), UV-Vis spectroscopy and X-ray diffraction (XRD). The SEM micrographs showed that the films of TiO2 sol-gel onto PP has approximately 1.0-μm thick and regular surface and the generation of polypropylene nanowires on hot-pressed samples. XRD showed the formation of TiO2 anatase on the surface of the films made by dip-coating. All photocatalysts were tested in decontaminating air-containing gaseous formaldehyde (70 ppmv) presenting degradation of the target compound to the limit of detection. The photocatalysts showed no deactivation during the entire period tested (30 h), and its reuse after washing showed better photocatalytic performance than on first use. The photocatalyst showed the best results were tested for 360 h with no observed deactivation. Aging studies showed that the film of TiO2 causes different effects on the photostability of composites, with stabilizing effect when exposed to most energetic UVC radiation (λmax = 254 nm) and degradative effects when exposed to UVA radiation (λmax = 365 nm).

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.

Synthesis and Characterization of a New Co-Crystal Explosive with High Energy and Good Sensitivity

NASA Astrophysics Data System (ADS)

Gao, Han; Jiang, Wei; Liu, Jie; Hao, Gazi; Xiao, Lei; Ke, Xiang; Chen, Teng

2017-10-01

A new energetic co-crystal consisting of one of the most powerful explosive molecules 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and the military explosive cyclotrimethylenetrinitramine (RDX) was prepared with a simple solvent evaporation method. Scanning electron microscopy (SEM) revealed the morphology of the bar-shaped product, which differed greatly from the morphology of the individual components. Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction spectrum (XRD), and differential scanning calorimetry (DSC) proved the formation of the co-crystal at the molecular level. The result of mechanical sensitivity test indicated the sensitivity was effectively reduced compared to raw CL-20. Finally, a possible crystallization mechanism was discussed.

The influence of chemical surface modification of kenaf fiber using hydrogen peroxide on the mechanical properties of biodegradable kenaf fiber/poly(lactic acid) composites.

PubMed

Razak, Nur Inani Abdul; Ibrahim, Nor Azowa; Zainuddin, Norhazlin; Rayung, Marwah; Saad, Wan Zuhainis

2014-03-07

Bleaching treatment of kenaf fiber was performed in alkaline medium containing hydrogen peroxide solution maintained at pH 11 and 80 °C for 60 min. The bleached kenaf fiber was analyzed using Fourier Transform Infrared (FTIR) and X-ray Diffraction (XRD) analysis. The bleached kenaf fiber was then compounded with poly-(lactic acid) (PLA) via a melt blending method. The mechanical (tensile, flexural and impact) performance of the product was tested. The fiber treatment improved the mechanical properties of PLA/bleached kenaf fiber composites. Scanning electron micrograph (SEM) morphological analysis showed improvement of the interfacial adhesion between the fiber surface and polymer matrix.

The synthesis of biocompatible and SERS-active gold nanoparticles using chitosan.

PubMed

Potara, Monica; Maniu, Dana; Astilean, Simion

2009-08-05

In this study we present a clean, nontoxic, environmentally friendly synthesis procedure to generate a large variety of gold nanoparticles (GNPs) by using chitosan, a biocompatible, biodegradable, natural polymer, as reducing and stabilizing agent. The formation of gold-chitosan nanocomposites was characterized by UV-vis absorption spectroscopy, transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy. The results show that the reaction temperature plays a crucial role in controlling the size, shape and crystalline structure of GNPs. In addition, it is demonstrated that chitosan can perform as a scaffold for the assembly of GNPs, which were successfully applied as substrate for surface-enhanced Raman scattering (SERS). To test the SERS activity, a relevant biological molecule--tryptophan--was adopted as the analyte.

Evaluation the pozzolanic reactivity of sonochemically fabricated nano natural pozzolan.

PubMed

Askarinejad, Azadeh; Pourkhorshidi, Ali Reza; Parhizkar, Tayebeh

2012-01-01

Natural pozzolans are appropriate supplementary cementitious materials in cement and concrete industry. A simple sonochemical method was developed to synthesize nanostructures of natural pozzolan. Chemical composition, crystallinity, morphology and reactivity of the natural pozzolan samples were compared before and after the sonochemical process, by using powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Thermal Gravimetry and Differential Thermal Analysis (TG/DTA). Compressive strength tests were performed to evaluate the properties of blended cements incorporating nano natural pozzolan. Under optimized conditions, the nano natural pozzolans showed a superior reactivity as compared with the bulk natural pozzolan. Also higher compressive strength was obtained for the cement specimen incorporating nano natural pozzolan. Copyright © 2011 Elsevier Ltd. All rights reserved.

Effect of Gold on the Corrosion Behavior of an Electroless Nickel/Immersion Gold Surface Finish

NASA Astrophysics Data System (ADS)

Bui, Q. V.; Nam, N. D.; Yoon, J. W.; Choi, D. H.; Kar, A.; Kim, J. G.; Jung, S. B.

2011-09-01

The performance of surface finishes as a function of the pH of the utilized plating solution was evaluated by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in 3.5 wt.% NaCl solution. In addition, the surface finishes were examined by x-ray diffraction (XRD), and the contact angle of the liquid/solid interface was recorded. NiP films on copper substrates with gold coatings exhibited their highest coating performance at pH 5. This was attributed to the films having the highest protective efficiency and charge transfer resistance, lowest porosity value, and highest contact angle among those examined as a result of the strongly preferred Au(111) orientation and the improved surface wettability.

Mössbauer study of iron-based perovskite-type materials as potential catalysts for ethyl acetate oxidation

NASA Astrophysics Data System (ADS)

Paneva, D.; Dimitrov, M.; Velinov, N.; Kolev, H.; Kozhukharov, V.; Tsoncheva, T.; Mitov, I.

2010-03-01

La-Sr-Fe perovskite-type oxides were prepared by the nitrate-citrate method. The basic object of this study is layered Ruddlesden-Popper phase LaSr3Fe3O10. The phase composition and structural properties of the obtained materials are investigated by Mössbauer spectroscopy, X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS) and temperature programmed reduction (TPR). The preliminary catalytic tests show a high potential of these materials for volatile organic compounds (VOCs) elimination as they possess high conversion ability and selectivity to total oxidation of ethyl acetate. Catalytic performance of LaSr3Fe3O10 is depended on the stability of structure and Fe4+-oxidation state.

Fabrication and characterization of bioactive glass-ceramic using soda-lime-silica waste glass.

PubMed

Abbasi, Mojtaba; Hashemi, Babak

2014-04-01

Soda-lime-silica waste glass was used to synthesize a bioactive glass-ceramic through solid-state reactions. In comparison with the conventional route, that is, the melt-quenching and subsequent heat treatment, the present work is an economical technique. Structural and thermal properties of the samples were examined by X-ray diffraction (XRD) and differential thermal analysis (DTA). The in vitro test was utilized to assess the bioactivity level of the samples by Hanks' solution as simulated body fluid (SBF). Bioactivity assessment by atomic absorption spectroscopy (AAS) and scanning electron microscopy (SEM) was revealed that the samples with smaller amount of crystalline phase had a higher level of bioactivity. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of silver nanoparticles loaded graphene oxide nanosheets for antibacterial activity

NASA Astrophysics Data System (ADS)

T, T. T., Vi; Lue, S. J.

2016-11-01

A simple, facile method to fabricate successfully silver nanoparticle (AgNPs) decorated on graphene oxide (GO) layers via grafted thiol groups. Samples were prepared with different concentrations of AgNO3. Resulting AgNPs were quasi-spherical in shape and attached on the layers of GO. Physical properties were confirmed by X-ray diffraction (XRD), zeta potential, dynamic light scattering (DLS), Fourier transform infrared (FTIR) spectra, thermogravimetric analyzer (TGA), transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM). Antimicrobial test was effectively showed using MRSA (Staphylococcus areus). The GO-Ag NPs with appropriate Ag NPs content of 0.2 M AgNO3 exhibited the strongest antibacterial activity at 48.77% inhibition after 4 hours incubation.

Pt nanoparticle-reduced graphene oxide nanohybrid for proton exchange membrane fuel cells.

PubMed

Park, Dae-Hwan; Jeon, Yukwon; Ok, Jinhee; Park, Jooil; Yoon, Seong-Ho; Choy, Jin-Ho; Shul, Yong-Gun

2012-07-01

A platinum nanoparticle-reduced graphene oxide (Pt-RGO) nanohybrid for proton exchange membrane fuel cell (PEMFC) application was successfully prepared. The Pt nanoparticles (Pt NPs) were deposited onto chemically converted graphene nanosheets via ethylene glycol (EG) reduction. According to the powder X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) analysis, the face-centered cubic Pt NPs (3-5 nm in diameter) were homogeneously dispersed on the RGO nanosheets. The electrochemically active surface area and PEMFC power density of the Pt-RGO nanohybrid were determined to be 33.26 m2/g and 480 mW/cm2 (maximum values), respectively, at 75 degrees C and at a relative humidity (RH) of 100% in a single-cell test experiment.

Second harmonic generation and crystal growth of new chalcone derivatives

NASA Astrophysics Data System (ADS)

Patil, P. S.; Dharmaprakash, S. M.; Ramakrishna, K.; Fun, Hoong-Kun; Sai Santosh Kumar, R.; Narayana Rao, D.

2007-05-01

We report on the synthesis, crystal structure and optical characterization of chalcone derivatives developed for second-order nonlinear optics. The investigation of a series of five chalcone derivatives with the second harmonic generation powder test according to Kurtz and Perry revealed that these chalcones show efficient second-order nonlinear activity. Among them, high-quality single crystals of 3-Br-4'-methoxychalcone (3BMC) were grown by solvent evaporation solution growth technique. Grown crystals were characterized by X-ray powder diffraction (XRD), laser damage threshold, UV-vis-NIR and refractive index measurement studies. Infrared spectroscopy, thermogravimetric analysis and differential thermal analysis measurements were performed to study the molecular vibration and thermal behavior of 3BMC crystal. Thermal analysis does not show any structural phase transition.

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

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

Fatimah, Is

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

Synthesis of Zeolite-X from Bottom Ash for H2 Adsorption

NASA Astrophysics Data System (ADS)

Kurniawan, R. Y.; Romadiansyah, T. Q.; Tsamarah, A. D.; Widiastuti, N.

2018-01-01

Zeolite-X was synthesized from bottom ash power plant waste using fusion method on air atmosphere. The fused product dissolved in demineralized water and aluminate solution was added to adjust the SiO2/Al2O3 molar ratio gel prior hydrothermal process. The synthesis results were characterized using X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Fourier Transform Infrared (FTIR). The results showed that the zeolite-X has a high crystallinity with octahedral particle. The pure-form zeolite-X then was characterized and tested for H2 gas adsorption by gravimetric method to determine the H2 gas adsorption capacity of zeolite-X from bottom ash and it was compared to synthetic zeolite-X.

The Bulk Nanocrystalline zn Produced by Mechanical Attrition

NASA Astrophysics Data System (ADS)

Zhu, X. K.; Zhao, K. Y.; Li, C. J.; Tao, J. M.; Chan, T. L.; Koch, C. C.

The purpose of experiment was to produce bulk nanocrystalline Zn by mechanical attrition. The bulk nanocrystalline Zn produced by mechanical attrition was studied. The microstructural evolution during cryomilling and subsequent room temperature milling was characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD). In this paper, Nanocrystalline Zn was produced by insitu consolidation of Zn elemental powder using mechanical attrition at liquid nitrogen and room temperature. For the samples studied, the longest elongation of 65% and highest stress of 200 MPa is obtained in nanocrystalline Zn during tensile testing at the condition of strain rate (10-3 sec-1) and 20°C which is equal to 0.43 Tm (Tm is the melting temperature of pure Zn).

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

PubMed

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

2017-10-31

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

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

High performance field emission of silicon carbide nanowires and their applications in flexible field emission displays

NASA Astrophysics Data System (ADS)

Cui, Yunkang; Chen, Jing; Di, Yunsong; Zhang, Xiaobing; Lei, Wei

2017-12-01

In this paper, a facile method to fabricate the flexible field emission devices (FEDs) based on SiC nanostructure emitters by a thermal evaporation method has been demonstrated. The composition characteristics of SiC nanowires was characterized by X-ray diffraction (XRD), selected area electron diffraction (SAED) and energy dispersive X-ray spectrometer (EDX), while the morphology was revealed by field emission scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). The results showed that the SiC nanowires grew along the [111] direction with the diameter of ˜110 nm and length of˜30 μm. The flexible FEDs have been fabricated by transferring and screen-printing the SiC nanowires onto the flexible substrates exhibited excellent field emission properties, such as the low turn-on field (˜0.95 V/μm) and threshold field (˜3.26 V/μm), and the high field enhancement factor (β=4670). It is worth noting the current density degradation can be controlled lower than 2% per hour during the stability tests. In addition, the flexible FEDs based on SiC nanowire emitters exhibit uniform bright emission modes under bending test conditions. As a result, this strategy is very useful for its potential application in the commercial flexible FEDs.

Improved microstructure of cement-based composites through the addition of rock wool particles

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

Lin, Wei-Ting; Institute of Nuclear Energy Research, Atomic Energy Council, Taoyuan 32546, Taiwan; Cheng, An, E-mail: ancheng@niu.edu.tw

2013-10-15

Rock wool is an inorganic fibrous substance produced by steam blasting and cooling molten glass. As with other industrial by-products, rock wool particles can be used as cementitious materials or ultra fine fillers in cement-based composites. This study investigated the microstructure of mortar specimens produced with cement-based composites that include various forms of rock wool particles. It conducted compressive strength testing, rapid chloride penetration tests, X-ray diffraction analysis, thermo-gravimetric analysis, and scanning electronic microscopy to evaluate the macro- and micro-properties of the cement-based composites. Test results indicate that inclusion of rock wool particles in composites improved compressive strength and reducedmore » chloride ion penetration at the age of 91 days due to the reduction of calcium hydroxide content. Microscopic analysis confirms that the use of rock wool particles contributed to the formation of a denser, more compact microstructure within the hardened paste. In addition, X-ray diffraction analysis shows few changes in formation of pozzolanic reaction products and no new hydrations are formed with incorporating rock wool particles. - Highlights: • We report the microstructural characterization of cement-based composites. • Different mixes produced with various rock wool particles have been tested. • The influence of different mixes on macro and micro properties has been discussed. • The macro properties are included compressive strength and permeability. • XRD and SEM observations confirm the pozzolanic reaction in the resulting pastes.« less

Green synthesis of gold nanoparticles using a cheap Sphaeranthus indicus extract: Impact on plant cells and the aquatic crustacean Artemia nauplii.

PubMed

Balalakshmi, Chinnasamy; Gopinath, Kasi; Govindarajan, Marimuthu; Lokesh, Ravi; Arumugam, Ayyakannu; Alharbi, Naiyf S; Kadaikunnan, Shine; Khaled, Jamal M; Benelli, Giovanni

2017-08-01

The impact of green-fabricated gold nanoparticles on plant cells and non-target aquatic species is scarcely studied. In this research, we reported an environment friendly technique for the synthesis of gold nanoparticles (Au NPs) using the Sphaeranthus indicus leaf extract. The formation of the metal NPs was characterized by UV-Visible and FT-IR spectroscopy, XRD, SEM and TEM analyses. The UV-Visible spectra of Au NPs showed a surface plasmon resonance peak at 531nm. FT-IR analysis indicated functional bio-molecules associated with Au NPs formation. The crystalline nature of Au nanoparticles was confirmed by their XRD diffraction pattern. TEM revealed the spherical shape with a mean particle size of 25nm. Au NPs was tested at 0, 1, 3, 5, 7 and 10% doses in mitotic cell division assays, pollen germination experiments, and in vivo toxicity trials against the aquatic crustacean Artemia nauplii. Au NPs did not show any toxic effects on plant cells and aquatic invertebrates. Notably, Au NPs promoted mitotic cell division in Allium cepa root tip cells and germination of Gloriosa superba pollen grains. Au NPs showed no mortality on A. nauplii, all the tested animals showed 100% survivability. Therefore, these Au NPs have potential applications in the development of pollen germination media and plant tissue culture. Copyright © 2017 Elsevier B.V. All rights reserved.

Titanium-35niobium alloy as a potential material for biomedical implants: In vitro study.

PubMed

de Andrade, Dennia Perez; de Vasconcellos, Luana Marotta Reis; Carvalho, Isabel Chaves Silva; Forte, Lilibeth Ferraz de Brito Penna; de Souza Santos, Evelyn Luzia; Prado, Renata Falchete do; Santos, Dalcy Roberto Dos; Cairo, Carlos Alberto Alves; Carvalho, Yasmin Rodarte

2015-11-01

Research on new titanium alloys and different surface topographies aims to improve osseointegration. The objective of this study is to analyze the behavior of osteogenic cells cultivated on porous and dense samples of titanium-niobium alloys, and to compare them with the behavior of such type of cells on commercial pure titanium. Samples prepared using powder metallurgy were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and metallographic and profilometer analyses. Osteogenic cells from newborn rat calvaria were plated over different groups: dense or porous samples composed of Ti or Ti-35niobium (Nb). Cell adhesion, cell proliferation, MTT assay, cell morphology, protein total content, alkaline phosphatase activity, and mineralization nodules were assessed. Results from XRD and EDS analysis confirmed the presence of Ti and Nb in the test alloy. Metallographic analysis revealed interconnected pores, with pore size ranging from 138 to 150μm. The profilometer analysis detected the greatest rugosity within the dense alloy samples. In vitro tests revealed similar biocompatibility between Ti-35Nb and Ti; furthermore, it was possible to verify that the association of porous surface topography and the Ti-35Nb alloy positively influenced mineralized matrix formation. We propose that the Ti-35Nb alloy with porous topography constitutes a biocompatible material with great potential for use in biomedical implants. Copyright © 2015 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-02-01

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

Studies on the synthesis, spectral, optical and thermal properties of l-Valine Zinc Sulphate: an organic inorganic hybrid nonlinear optical crystal.

PubMed

Puhal Raj, A; Ramachandra Raja, C

2012-11-01

Nonlinear optical (NLO) organic inorganic hybrid l-Valine Zinc Sulphate (LVZS) was synthesized and single crystals were obtained from saturated aqueous solution by slow evaporation method at 36°C using a constant temperature bath (CTB) with an accuracy of ±0.01°C. This crystal is reported with its characterization by single crystal and powder XRD, FTIR, UV-Vis-NIR, TG/DTA analysis and SHG test. Single crystal XRD study reveals that LVZS crystallizes in monoclinic system with the lattice constants a=9.969(3) Å, b=7.238(3) Å, c=24.334(9) Å and cell volume is 1736.00Å(3). Sharp peaks observed in powder X-ray diffraction studies confirm the high degree of crystallinity of grown crystal. The incorporation of sulphate ion with l-valine is confirmed by FTIR spectrum in LVZS crystal(.) A remarkable increase in optical transparency has been observed in LVZS when compared to l-valine and zinc sulphate heptahydrate Thermal properties of LVZS have been reported by using TG/DTA analysis. Kurtz powder second harmonic generation (SHG) test confirms NLO property of the crystal and SHG efficiency of LVZS was found to be 1.34 times more than pure l-valine. Copyright © 2012 Elsevier B.V. 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.

Investigating the structure and biocompatibility of niobium and titanium oxides as coatings for orthopedic metallic implants.

PubMed

Pradhan, D; Wren, A W; Misture, S T; Mellott, N P

2016-01-01

Applying sol gel based coatings to orthopedic metallic implant materials can significantly improve their properties and lifespan in vivo. For this work, niobium (Nb2O5) and titanium (TiO2) oxides were prepared via solution processing in order to determine the effect of atomic arrangement (amorphous/crystalline) on bioactivity. Thermal evaluation on the synthesized materials identified an endotherm for Nb2O5 at 75 °C with 40% weight loss below 400 °C, and minimal weight loss between 400 and 850 °C. Regarding TiO2 an endotherm was present at 92 °C with 25% weight loss below 400 °C, and 4% between 400 and 850 °C. Phase evolution was determined using High Temperature X-ray Diffraction (HT-XRD) where amorphous-Nb2O5 (450 °C), hexagonal-Nb2O5 (525 °C), orthorhombic-Nb2O5 (650 °C), amorphous-TiO2 (275 °C) and tetragonal TiO2 (500 °C) structures were produced. Simulated body fluid (SBF) testing was conducted over 1, 7 and 30 days and resulted in positive chemical and morphological changes for crystalline Nb2O5 (525 °C) and TiO2 (500 °C) after 30 days of incubation. Rod-like CaP deposits were observed on the surfaces using Scanning Electron Microscopy (FE-SEM) and Grazing Incidence-X-ray Diffraction (GI-XRD) shows that the deposits were X-ray amorphous. Cell viability was higher with the TiO2 (122%) samples when compared to the growing cell population while Nb2O5 samples exhibited a range of viability (64-105%), partially dependent on materials atomic structure. Copyright © 2015 Elsevier B.V. All rights reserved.

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