A Novel High Temperature Apparatus for in situ Synchrotron X-ray Diffraction Studies of Molten Salt

This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.

Evaluation on residual stresses of silicon-doped CVD diamond films using X-ray diffraction and Raman spectroscopy

The effect of silicon doping on the residual stress of CVD diamond films is examined using both X-ray diffraction (XRD) analysis and Raman spectroscopy measurements. The examined Si-doped diamond films are deposited on WC-Co substrates in a home-made bias-enhanced HFCVD apparatus. Ethyl silicate (Si(OC2H5)4) is dissolved in acetone to obtain various Si/C mole ratio ranging from 0.1% to 1.4% in the reaction gas. Characterizations with SEM and XRD indicate increasing silicon concentration may result in grain size decreasing and diamond [110] texture becoming dominant. The residual stress values of as-deposited Si-doped diamond films are evaluated by both sin2ψ method, which measures the (220) diamond Bragg diffraction peaks using XRD, with ψ-values ranging from 0° to 45°, and Raman spectroscopy, which detects the diamond Raman peak shift from the natural diamond line at 1332 cm-1. The residual stress evolution on the silicon doping level estimated from the above two methods presents rather good agreements, exhibiting that all deposited Si-doped diamond films present compressive stress and the sample with Si/C mole ratio of 0.1% possesses the largest residual stress of ~1.75 GPa (Raman) or ~2.3 GPa (XRD). As the silicon doping level is up further, the residual stress reduces to a relative stable value around 1.3 GPa.

Analysis of electrochemical impedance and XRD spectroscopy for complex self-assembled film on silver

Self-assembled monolayers （SAMs） of （3-mercaptopropy） trimethoxysilane （3-MtrF） chemisorbed on silver surfaces were chemically ＂modified by 1-octadecanethiol to form self-assembled mixed-monolayers （SAMM） and the co-polymer of N-vinylcarbazole and methyl methacrylate ester （to form complex selfassembled film （CSAF））. The oxidation resistance of these barriers on silver surfaces and some influential factors concerned processes were analyzed by electrochemical impedance spectroscopy （EIS） in a 10% NaOH aqueous solution at oxidation potential. X-ray diffraction （XRD） spectroscopy shows that the oxidation occurring on the silver surface may be restrained effectively due to the coating barrier, and CSAF（Ⅱ） is the best one. Studies also reveal that oxide processes of bare silver and a series of modified silver electrodes in a 10% NaOH aqueous solution are of more than two relaxation time constants.

Variation of microfibril angle and its correlation to wood properties in poplars

The microfibril angle of seven poplar clones was determined by using X-ray diffraction technique. Microfibril angle, wood basic density, fiber length, fiber width and cellulose content were assessed for every growth ring at breast height for all sample trees. Significant variation in microfibril angle was observed among growth rings. Mean microfibril angle (MFA) at breast height varied from 7.8?to 28?between growth rings with cambial age and showed a consistent pith-to-bark trend of decline an-gles. Analysis of variance also indicated that there were significant differences in wood basic density, fiber length, fiber width and cellulose content between the growth rings, which had an increasing tendency from pith to bark. Correlations between MFA and examined wood properties were predominantly large and significant negative (?0.01), and the coefficients were -0.660 for cellulose content, -0.586 for fiber length, -0.516 for fiber width and -0.450 for wood basic density, respectively. Regression analysis with linear and curve estimation indicated that a quadratic function showed the largest R2 and the least standard error for describing the relationships between microfibril angle and measured wood properties, and the correlation coefficients were over -0.45 (n=125). The results from this study suggested that microfibril angle would be a good characteristic for improvement in the future breeding program of poplars.

Effects of PVP K30 on Aqueous Solubility and Dissolution Propertiesof Daidzein

AimTo study effects of PVP K30 on the aque ou s solubility and dissolution properties of daidzein. Methods To measure the aqueous solubility and dissolution rates of daidzein in three diffe rent states (within solid dispersions, physical mixtures and as a pure drug) and investigate drug-polymer interactions in the solid state using X-ray powder d iffraction and fourier-transform infrared spectroscopy. Results The negative values of the Gibbs free energy and enthalpy of transfer explaine d the spontaneous transfer of daidzein from phosphate buffer solution (PBS) to a solution of PVP in PBS. X-ray powder diffraction patterns showed that the drug was in the amorphous state (ratio of the drug ∶ PVP<1∶5) when dispers ed i n PVP K30. The infrared spectra indicated there exist interactions between the O H of daidzein and the C=O of PVP K30. Conclusionthe dispersion of daidzein in PVP K30 considerably enhances the solubility and dissolution rat e.

Enhanced Photoelectrochemical Property of Zn Loaded TiO2 Nanotube Arrays Electrode

TiO2 nanotube arrays （TNTs） electrode loaded with Zn nanoparticles was prepared by anodization and the size of Zn nanoparticle loaded on TNTs electrode was controlled by chronoamperometry deposition time. Results of SEM and XRD analysis show that Zn nanoparticles had a diameter of about 15-25 nm when the deposition time was 3-5 s. The UV-Vis diffuse reflectance spectra show the Zn loaded harvest light with 480-780 nm more effectively than the unloaded sample. The photocurrent response of Zn loaded TNTs electrodes were studied, the results showed that TNTs electrodes loaded with Zn nanoparti-cles has 50% increased photocurrent response under high-pressure mercury lamp irradiation compared with unloaded TNTs electrode.

Determination of Structure and Polarity of Si C Single Crystal by X-Ray Diffraction Technique

Structure and polarity of the Si C single crystal have been analyzed with the four- circle X- ray diffraction method by a double- crystal diffractom eter.The hexagonal{ 10 15 } pole figure shows that this Si C sam ple has a6 H modification.The difference between the integrated intensities m easured byω scan in the triple- axis diffraction set- up finds some convincing evidence that the surface is either a Si- terminated face or C- terminated face.The experi- mental ratios of| F( 0 0 0 L) | 2 / | F( 0 0 0 L) | 2 are in good agreem entwith the calculated ones after the dispersion cor- rections to the atomic scattering factors( L=6 ,12 and18,respectively) .Thus,this m easurem ent technique is con- venient for the application of the materials with remarkable surface polarity.

Preparation and Characterization of Solid Dispersions of Silymarin with Polyethylene Glycol 6000

Aim To prepare and characterize solid dispersions of silymarin with the intention of improving their dissolution properties. Methods The solid dispersions were prepared by the fusion method with polyethylene glycol 6000(PEG 6000) as the carrier. Evaluation of the properties of the dispersions was performed using dissolution studies, X ray powder diffraction and Fourier transform infrared (FT IR) spectroscopy. Results The rate of dissolution of silymarin was considerably improved as compared with pure silymarin when formulated in solid dispersions with PEG 6000. The data of the X ray diffraction showed some changes in the parameters of lattice spacing [ d ], peak position and relative intensities. FT IR together with those from X ray diffraction showed the absence of well defined drug polymer interactions. Conclusion The dissolution improvement of poorly soluble silymarin could be illuminated by the changes of the lattice parameters of PEG 6000 and the drug.

Microbially induced deposition of barium phosphates and its ingredient,morphology and size under different pH values

A phosphate-mineralization microbe was used to induce barium phosphates precipitation, and the precipitates with different types were obtained under different pH values. The average crystallite size of the barium phosphates was calculated by particle size distribution curves, and the size of the products was 33.40, 29. 37, 24. 13, 47.76 and 96. 53 μm when the pH values of the mixed solution are 7, 8, 9, 10 and 11, respectively. The results of X-ray diffraction （XRD） show that the structures of the particles controlled by the mixed solution are mainly BaaPO4 when pH 〈 10; the barium phosphates are synthesized by biological deposition which is the mixture of BaHPO4 and Ba5 （PO4）3OH when pH = 10; when pH = 11, the barium phosphates are also the mixtures, which are Ba5 （PO4）3OH and BaNaPO4. The above results indicate that the phosphate-mineralization microbe can produce a certain enzyme which constantly hydrolyzes phosphate monoester in the mixed solution, and then PO4^3- ions are obtained.

X-ray Comparative Analysis of Rhubarb in Different Production Areas of Qinghai

[Objective] The aim of this study was to provide a basis for distinguishing quality of rhubarb in different production areas. [Method ] X-ray diffraction patterns of rhubarbs in different production areas of Qinghai were obtained by X-ray diffraction analysis, and then its similarity analysis was also investigated. [ Result] The content of chemical components in rhubarbs from different production areas had differences, but its diffraction patterns and diffraction peaks had certain fingerprint characteristics. [ Conclusion] X-ray diffraction method is a fast and effective method for identifying rhubarb and other Chinese herbal medicines in different production areas.

Characterization of Ga NAs/ Ga As and Ga In NAs/ Ga As Quantum Wells Grown by Plasma-Assisted Molecular Beam Epitaxy: Effects of Ion Damage

The effects of ion damage on Ga NAs/Ga As and Ga In NAs/Ga As quantum wells ( QWs) grown by plas- ma- assisted molecular beam epitaxy have been investigated. Itis found thation damage is a key factor affecting the quality of Ga NAs and Ga In NAs QWs. Obvious appearance of pendello¨ sung fringes in X- ray diffraction pattern and remarkable im provement in the optical properties of the samples grown with ion removal magnets are observed.By removing nitrogen ions,the PL intensity of the Ga In NAs QW is improved so as to be comparable with that of Ga In As QW. The stronger is the magnetic field,the m ore obvious the PL intensity im provement would be.

Twinning in Low-Temperature MOCVD Grown GaN on (001) GaAs Substrate

GaN buffer layers (thickness ～60nm) grown on GaAs(001) by low-temperature MOCVD are investigated by X-ray diffraction pole figure measurements using synchrotron radiation in order to understand the heteroepitaxial growth features of GaN on GaAs(001) substrates.In addition to the epitaxially aligned crystallites,their corresponding twins of the first and the second order are found in the X-ray diffraction pole figures.Moreover,{111} φ scans with χ at 55° reveal the abnormal distribution of Bragg diffractions.The extra intensity maxima in the pole figures shows that the process of twinning plays a dominating role during the growth process.It is suggested that the polarity of {111} facets emerged on (001) surface will affect the growth-twin nucleation at the initial stages of GaN growth on GaAs(001) substrates.It is proposed that twinning is prone to occurring on {111}B,N-terminated facets.

Fabrication and Growth Mechanism of Bamboo-structured Boron Nitride Nanotubes with Thorn-Like Morphology

Bamboo-structured boron nitride （BN） nanotubes with thorn-like morphology were synthe-sized by thermal chemical reaction using amorphous boron powders and NiO nanoparticles as precursors under the flow of NH3 at 1100 oC. The structural and morphological charac-teristics of BN nanotubes were investigated by X-ray diraction and transmission electron microscopy. The results showed that the thorn-like nanostructures attaching to the stems of bamboo-structured BN nanotubes were the hexagonal BN nano akes. Based on the diffu-sion of solid B and vapor B2O2, a possible growth mechanism of these novel thorn-like BN nanotubes was primarily proposed.

Metalorganic Chemical Vapor Deposition of GaNAs Alloy Using Dimethylhydrazine as Nitrogen Precursor

GaNAs alloy is grown by metalorganic chemical vapor deposition (MOCVD) using dimethylhydrazine (DMHy) as the nitrogen precursor.High resolution X ray diffraction (HRXRD) and secondary ion mass spectro metry (SIMS) are combined in determining the nitrogen contents in the samples.Room temperature photoluminescence (RTPL) measurement is also used in characterizing.The influence of different Ga precursors on GaNAs quality is investigated.Samples grown with triethylgallium (TEGa) have better qualities and less impurity contamination than those with trimethylgallium (TMGa).Nitrogen content of 5 688% is achieved with TEGa.The peak wavelength in RTPL measurement is measured to be 1278 5nm.

Visible-Light Activities of Erbium Doped BiVO4 Photocatalysts

Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectra techniques. The activity of the catalyst was determined by oxidative decomposition of methyl orange in aqueous solution under visible-light irradiation. X-ray photoelectron spectroscopy and energy-dispersive X-ray Spectroscopy analysis revealed that the doped Er existed in the form of Er2O3. It also showed that the Er doping can enhance the visible-light absorption abilities of catalysts and their visible-light-driven photocatalytic activities in comparison with those of pure BiVO4.

Effects of Thickness on Properties of ZnO Films Grown on Si by MOCVD

High quality ZnO films are successfully grown on Si（100） substrates by metal-organic chemical vapor deposition at 300℃. The effects of the thickness of the ZnO films on crystal structure, surface morphology,and optical properties are investigated using X-ray diffraction, scanning probe microscopy,and photoluminescence spectra, respectively. It is shown that the ZnO films grown on Si substrates have a highly-preferential C-axis orientation,but it is difficult to obtain the better structural and optical properties of the ZnO films with the increasing of thickness. It is maybe due to that the grain size and the growth model are changed in the growth process.

SnO_2-based solid solutions for CH_4 deep oxidation: Quantifying the lattice capacity of SnO_2 using an X-ray diffraction extrapolation method

A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.

A Reflectron Time-of-Flight Mass Spectrometer with a Nano-Electrospray Ionization Source for Study of Metal Cluster Compounds

An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.

Hot deformation behavior and microstructure evolution of TC4 titanium alloy

The hot deformation behavior of Ti-6Al-4V （TC4） titanium alloy was investigated in the temperature range from 650℃ to 950℃ with the strain rate ranging from 7.7×10^-4 s^-1 to 7.7×10^-2 s^-1. The hot tension test results indicate that the flow stress decreases with increasing the deformation temperature and increases with increasing the strain rate. XRD analysis result reveals that only deformation temperature affects the phase constitution. The microstructure evolution under different deformation conditions was characterized by TEM observation. For the deformation of TC4 alloy, the work-hardening is dominant at low temperature, while the dynamic recovery and dynamic re-crystallization assisted softening is dominant at high temperature.

Characterization of residual stresses and microstructural features in an Inconel 718 forged compressor disc

Residual stress plays an important part in fabricating commercial aero engine Inconel 718 components for their fatigue properties, reliability and durability. Due to the limitation of Chinese neutron diffraction instrument and lack of test practice and specifications, there is little systematic research on the residual stress of forged compressor disc. X-ray diffraction and neutron diffraction methods were used to measure the residual stress of Inconel 718 forged discs at the surface and in the interior, respectively. Scanning electron microscope and transmission electron microscope were used to characterize the microstructural features. The residual stress state at the disc is in near-surface compression, balanced by tension within the disc core. However, the surface residual stress of disc depends more on the rough machining than on the forging process. Also, the dislocation densities increase with decreasing distance to the surfaces of disc, and the residual stress accelerates dislocation generation and dynamic recrystallization.