利用X-射线衍射仪评价防膨剂效果的实验方法

以水化膨胀能力最强的钠蒙脱石为研究对象,利用X′PertPro粉晶X-射线衍射仪测试蒙脱石(001)晶面间距的原理,探索性地建立了使用X-射线衍射仪直接、快速评价防膨剂防膨效果的方法和实验流程。系统总结了钠蒙脱石在去离子水、有机防膨剂、无机防膨剂中的(001)晶面间距变化情况。研究表明,蒙脱石(001)晶面间距的变化能够直观的反应防膨剂的防膨效果。并且采取了先抑后膨、先膨后抑的方法对防膨剂的稳定性、持续性进行了评价,拓宽了评价防膨剂的性能参数。

草酸钙结石不同层面的扫描电镜能谱和X线衍射分析

目的:分析草酸钙结石不同层面的化学成分,探讨其形成机制。方法:结合扫描电镜能谱分析(SEM-EDS)和X线衍射(XRD)定性、定量分析24例完整草酸钙结石样本不同层面的化学成分。结果:所有结石均为草酸钙混合结石,均含有磷酸钙成分。SEM-EDS显示结石核心、中间、外周的元素含量C(27.97%、30.83%、33.73%)、Ca(12.05%、9.36%、8.95%)、P(3.28%、2.34%、1.67%)差异存在显著性(P<0.05)。XRD显示核心区域含有草酸钙和磷酸钙晶体,外层区域仅含有草酸钙晶体。结论:联合运用SEM-EDS和XRD对结石的不同层面进行成分分析,能够较为准确地检测结石的组分和物相。草酸钙混合结石可能起始于磷酸钙晶体的聚集,草酸钙晶体在此基础上沉积生长可能是结石逐渐增大的原因。

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.

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.

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.

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.

Analysis of surface orange peel of aluminum-alloy automobile sheet by using of EBSD and X-ray diffraction

The formation cause of orange peel of aluminum-alloy automotive sheet after tensile deformation was analysed by using X-ray diffraction and electron back-scattered diffraction(EBSD).The test results showed that formation cause of surface orange peel after tensile deformation related to product texture and nonuniform deformation during the tensile process.The grain size has significant effect on deformation uniform and texture formation.Coarse grains were easy to produce nonuniform deformation and texture,which would produce surface orange peel after tensile deformation.

Structure of the organic crystallite unit in coal as determined by X-ray diffraction

X-ray diffraction （XRD） was used to study the structure of the organic crystallite unit （La, Lo doo2） in coals collected from Henan and Shanxi Provinces. XRD patterns of coal were collected in a step-scan mode （0.1 °/step） over an angular range of 2-90° （20）, allowing 8 s at each step. The structure of the crystallite unit was determined from the Scherrer equation and peak parameters deduced from whole pattern fitting. The results show that the structure of the crystallite unit in coal is mainly controlled by the coal rank. As the coal rank increases the average diameter of a coal crystallite unit （La） increases, the interlayer spacing （doo2） decreases slightly, and the average height of a coal crystallite unit （Lc） increases at first but then decreases. A new diffraction peak from the crystallite unit in coal was found at a low scattering angle in the XRD pattern （2-10~）. This suggests a structure with an inter-layer spacing from 1.9 to 2.8 nm exists in coal crystallites.

Characterization of Average Molecular Structure of Heavy Oil Fractions by ~1H Nuclear Magnetic Resonance and X-ray Diffraction

The chemical structure of heavy oil fractions obtained by liquid-solid adsorption chromatography was character-ized by 1 H nuclear magnetic resonance and X-ray diffraction.The molecular weight and molecular formula of asphaltene molecules were estimated by combining 1 H nuclear magnetic resonance and X-ray diffraction analyses,and were also ob-tained from vapor pressure osmometry and elemental analysis.Heteroatoms,such as S,N,and O atoms,were considered in the construction of average molecular structure of heavy oils.Two important structural parameters were proposed,including the number of alkyl chain substituents to aromatic rings and the number of total rings with heteroatoms.Ultimately,the av-erage molecular structures of polycyclic aromatics,heavy resins and asphaltene molecules were constructed.The number of α-,β-,γ-,and aromatic hydrogen atoms of the constructed average molecular structures fits well with the number of hydro-gen atoms derived from the experimental spectral data.

X-ray peak profile analysis of dislocation type,density and crystallite size distribution in cold deformed Pb-Ca-Sn alloys

The density,nature of the dislocations and distribution of the domain sizes in cold-deformed Pb-Ca-Sn solid solution were determined by X-ray diffraction profile analysis.The dislocation densities are of the order of 1010 cm-2.The strain broadening of diffraction profiles was accounted for by dislocation contrast factor.The coherent domain size was determined by the recently developed PM2K software package.Assuming that the domain size distribution is log-normal,the distribution function（median μ and variance σ） was calculated from the size parameters determined from X-ray diffraction profile analysis.

Structural Analysis of Hydroxamate Reagents by X-Ray Diffraction

Axis House manufactures and supplies alkyl hydroxamate reagent of various carbon chain lengths for application in flotation of oxide copper and other minerals. As a part of reagent performance improvement, the structural factors of hydroxamate are examined by various analytical tools in particular with X-ray diffraction of single crystals. In a recent publication, the structures of n-octyl hydroxamic acid and its corresponding potassium salt are presented with findings of hydroxamic functional group geometric preference, H-bonding, keto-enol tautomerisation, acid-salt aggregation and alignment of carbon chain. In this paper, an example of branched alkyl hydroxamate3,5,5-trimethyl hexyl hydroxamate. hydroxamate is presented and compared with the result of linear alkyl

Preparation, crystallization and preliminary X-ray diffraction analysis of PH1948, predicted RNA methyltransferase from Pyrococcus horikoshii

RNA methyltransferase is responsible for transferring methyl and resulting in methylation on the bases or ribose ring of RNA, which existed widely but mostly remains an open question. A recombinant protein PH1948 predicting RNA methyl- transferase from Pyrococcus horikoshii OT3 has been crystallized. The crystals of selenomethionyl PH1948 belong to space group C2, with unit-cell parameters a=207.0 ?, b=43.1 ?, c=118.2 ?, β=92.1°, and diffract X-rays to 2.2 ? resolution. The VM value was determined to be 2.8 ?3/Da, indicating the presence of four protein molecules in the asymmetric unit.

Evaluation method of coal rank based on X-ray diffraction analysis an example from SE Qinshui Basin

Based on analysis on X-ray diffraction, the metamorphic grade of coal in southeast Qinshui Basin was discussed, and a precise evaluation of coal rank through XRD analysis was made, in addition, the correlation of coal rank and vitrinite reflectance （Ro） was compared. XRD spectra of coal shows （002）-band and γ-band, and based on fitting calculation and multi-peak separation methods, the values of 2θ002 and 2θγ can be obtained, as well as corresponding intensities I002 and Iγ, consequently the coal rank can be quantized as the ratio of I002 and Iγ, that is coal rank=I002/Iγ. The research shows that the values of θ002 and θγ increase with the metamorphic grade, and a very good linear positive correlation exists between calculated Coal Rank and Ro.

Magnetostrictive distortion in Pr_(0.15)Tb_xDy_(0.85-x)Fe_2 polycrystals by X-ray diffraction

The ingots of Pr0.15TbxDy0.85-xFe2 （x=0.10-0.85） series compounds with a single phase were prepared -by a arc melting method. The X-ray diffraction patterns were measured using a Philips X’pert MPD X-ray diffractometer with a non-ambient sample stage at different temperatures, the magnetostrictive distortion in (Pr0.15TbxDy0.85-xFe2) polycrystals was investigated by X-ray diffraction patterns and the magnetostriction coefficient λ111 was calculated. The results show -when the temperature is raised above the spin reorientation temperature region, a splitting appears in the reflection （440）; the λ111 increase with the increasing of Tb content for (Pr0.15TbxDy0.85-xFe2) polycrystals and the full width at half maximum （FWHM） of the reflection （440） increases gradually with the increasing of Tb content. Moreover, as the FWHM of the reflection （440） decreases gradually with the increasing of temperature, the λ111 decreases slightly with the increasing of temperature at the temperature region of 223-373K for Pr0.15Tb0.3Dy0.55Fe2 alloy.

Getting and X-Ray Diffraction Analysis of the Uranium Catalyst SAPO-U, Nd, Sb, Bi on the Basis of Natural Zeolite Deposits Chankanayskoe

To study the physical and chemical properties of uranium catalyst by impregnation and calcination us was first obtained uranium catalyst SAPO-U, Nd, Sb, Bi. The method of X-ray structure has been studied of the uranium catalyst SAPO-U, Nd, Sb, Bi.

Obtaining and Reviewing X-ray Diffraction Analysis of the Uranium Catalyst SAPO-U, W, V Based on Natural Zeolite Chankanayskoe Deposits for the Oxidation of S02 to S03

We first obtained by impregnating the zeolite with salts U, W and V and examined the X-ray uranium catalyst SAPO-U, W, V based on natural zeolite Chankanayskogoe deposits for the oxidation of SO2 to SO3.

Simulation of X-ray Diffraction Line Broadening Caused by Stress Gradients and Determination of Stress Distribution by Fourier Analysis

Different physical, mechanical and chemical processes, such as： ion implantation, oxidation, nitridation and others create on the surface of materials residual stress state, characterized by high level and strong gradient. X-ray diffraction method widely used for stress measurements has some difficulties in interpretation of experimental data, when the depth of X-ray penetration is compared with thickness of surface layer where inhomogeneous stress distribution is localized. Early it has been shown by authors that diffraction line broadening occurs when analyzed surface is characterized by strong gradient. The interest to study the diffraction line broadening is connected to the possibility of obtaining information about parameters of surface stress distribution. In the present paper the convolution and deconvolution concepts of Fourier analysis were applied to study X ray diffraction line broadening caused by surface stress gradients. Developed methodology allows determining of stress distribution in superficial layers of materials.

Photoluminescence and X-ray Diffraction of Distributed Bragg Reflector

Spectral and structural characteristics of distributed Bragg reflector (DBR) in vertical-cavity surface-emitting lasers were studied with photoluminescence and double-crystal X-ray diffraction measurement.The expected high quality epitaxial DBR structure was verified.In the X-ray double-crystal rocking curves of DBR the zeroth-order peak,the first and second order satellite peaks were measured.Splitting of diffraction peak appeared in the rocking curves was analyzed.The effects of introduced deep energy levels on the structural perfection and optical properties were discussed.