The thermal expansion coefficients of kyanite at ambient pressure have been investigated by an X-ray powder diffraction technique with temperatures up to 1000 ℃. No phase transition was observed in the experimental t...The thermal expansion coefficients of kyanite at ambient pressure have been investigated by an X-ray powder diffraction technique with temperatures up to 1000 ℃. No phase transition was observed in the experimental temperature range. Data for the unit-cell parameters and temperatures were fitted empirically resulting in the following thermal expansion coefficients: αa = 5.8(3) × 10^-5, αb = 5.8 (1)× 10^-5, αc = 5.2(1)× 10^-5, and αv = 7.4(1) × 10^-3 ℃ 1 in good agreement with a recent neutron powder diffraction study. On the other hand, the variation of the unit-cell angles α, β and γ of kyanite with increase in temperature is very complicated, and the agreement among all studies is poor. The thermal expansion data at ambient pressure reported here and the compression data at ambient temperature from the literature suggest that, for the kyanite lattice, the most and least thermally expandable directions correspond to the most and least compressible directions, respectively.展开更多
The crystal structure of [Co(NH3)5Br]Br2 has been determined ab initio from the conventional X-ray powder diffraction data. The approximate structure with all 7 indeyendent non-H atoms was solved by direct methods. Th...The crystal structure of [Co(NH3)5Br]Br2 has been determined ab initio from the conventional X-ray powder diffraction data. The approximate structure with all 7 indeyendent non-H atoms was solved by direct methods. The final orthorhombic unit-cell parameters after Rietveld refinement are: a=13.6927, b=10.7071, c=6.9400A, V=1017.47A3, F30=93(0.0075,43), M20=49, Z=4. Space group is Pnma. The structure agreement factors are: Rp=0.066,Rwp=0.090, RF=0.041, RB=0.042.展开更多
The X-ray powder diffraction data of the compound GdAlSi was studied by means of X-ray diffraction technique and refined by Rietveld method. The compound GdAlSi has tetragonal α-ThSi_2-type structure, space group I4_...The X-ray powder diffraction data of the compound GdAlSi was studied by means of X-ray diffraction technique and refined by Rietveld method. The compound GdAlSi has tetragonal α-ThSi_2-type structure, space group I4_1/amd (No.141), Z=4, the lattice parameters a=041234 (1) nm, c=1.44202(1) nm. The Smith and Snyder figure of merit [5] F_N is F_ 30=2521(36). The R-factors of Rietveld refinement are R_p=0.098 and R_ wp=0.128. The X-ray powder diffraction data are given. The field dependence of the magnetization measured at room temperature and the temperature variation of the inverse magnetic susceptibility of the compound GdAlSi were also presented.展开更多
In cooperation with figure-of-merits the Rietveld analysis can appraise both angular and intensity data of powder diffraction. In this work, X-ray diffraction pattern of Bi4(SiO4)3 was redetermined with intensity figu...In cooperation with figure-of-merits the Rietveld analysis can appraise both angular and intensity data of powder diffraction. In this work, X-ray diffraction pattern of Bi4(SiO4)3 was redetermined with intensity figure-of-merits, which qualify agreement between observed and calculated relative intensities. F30 is 158.90 (0.0059, 32), intensity figure of merit Rint is 8.7, I20(17), 8.0. The values of figure-of-merits show that the data of JCPDS cards are distorted. Both the experimental and calculated peak positions and heights are listed in detail.展开更多
A new method for pattern identification and simulation of X-ray powder diffraction data is described, which can give definite phase composition of the unknown rapidly and correctly. The method is implemented in Micros...A new method for pattern identification and simulation of X-ray powder diffraction data is described, which can give definite phase composition of the unknown rapidly and correctly. The method is implemented in Microsoft Fortran 77 for the IBM PC/XT/AT personal computer or their compatibles.展开更多
The compound GdNiSn has been studied by X-ray powder diffraction technique.The crystal structure and the X-ray diffraction data for this compound at room temperature are reported.The compound GdNiSn is orthorhombic wi...The compound GdNiSn has been studied by X-ray powder diffraction technique.The crystal structure and the X-ray diffraction data for this compound at room temperature are reported.The compound GdNiSn is orthorhombic with lattice parameters a=7.2044(1)A,b=7.6895(6)A,c=4.4772(4)A,space group Pna2_(1) and 4 formula units of GdNiSn in unit cell.The Smith and Snyder figure of index F_(30) for this compound is 35(0.015,59).展开更多
A new compound K6FeNb15O42 was prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The X-ray powder diffraction data of the title compound was measured. K6FeNb15 O42 crystallizes in ...A new compound K6FeNb15O42 was prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The X-ray powder diffraction data of the title compound was measured. K6FeNb15 O42 crystallizes in the hexagonal system with unit cell parameters, a = 9. 1320(4) A ,c = 12. 0670(9) A , and space group P63/mcm (193) , z = 1. The calculated and measured densities are 4. 489 g/cm3 and 4. 485 g. cm3, respectively.展开更多
The 773 K isothermal section of the La-Fe-Sn ternary system was investigated and constructed by X-ray powder diffraction(XRD).The existence of two reported ternary intermetallic compounds,La6Fe13Sn and La3FeSn6,is c...The 773 K isothermal section of the La-Fe-Sn ternary system was investigated and constructed by X-ray powder diffraction(XRD).The existence of two reported ternary intermetallic compounds,La6Fe13Sn and La3FeSn6,is confirmed in this work.Compared with other R-Fe-Sn phase diagrams(R = Pr and Sm),the binary alloys Fe3Sn and Fe5Sn3 are not present.The compound Fe3Sn2 was observed from the XRD pattern of Fe3Sn2 samples,but it is not an equilibrium phase at 773 K and decomposes into Fe and FeSn phases completely for a longer heat treated time.Up to now,the crystal structure data of La2Sn3 has not been reported,so the X-ray pattern of La2Sn3 was only estimated.The phase relationship for this compound was drawn by a dotted line.展开更多
A new compound K6FeNb15O42 u(?) prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The XRD data of the title compound was determined. K6FeNb15O42 crystallizes the hexagonal system w...A new compound K6FeNb15O42 u(?) prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The XRD data of the title compound was determined. K6FeNb15O42 crystallizes the hexagonal system with unit cell parameters a=9. 1320(4) A,c=12. 0670(9) A, and space group P63/mcm(193) , 2=1. The calculated and measured densities are 4. 489 g/ cm3 and 4. 485 g. cm3, respectively.展开更多
CuKβ radiation with a wavelength of λ = 1.3923 ? is recommended for crystal structure determination from X-ray powder diffraction using the Rietfeld method. A highly sensitive image plate detector is able to collect...CuKβ radiation with a wavelength of λ = 1.3923 ? is recommended for crystal structure determination from X-ray powder diffraction using the Rietfeld method. A highly sensitive image plate detector is able to collect enough intensity to record a brilliant X-ray powder pattern in a reasonable time, compared to CuKα1 radiation used today. Especially atomic displacement coefficients could be determined more precisely with the much greater number of reflections recorded. A double-radius Guinier camera attached to a micro-focus rotating anode tube ensures increased brilliance besides high resolution. A simple construction specification is presented to make smart cylindrically bent Ge(111) or Si(111) X-ray monochromators that deliver focused CuKβ radiation. The highly linear response of image plate detectors allows removing of fluorescence radiation simply as background of the pattern. The proposed equipment is a cost-efficient alternative to a liquid gallium-metal-jet X-ray source with maximum power load and a similar wavelength of λ(GaKα1) = 1.34013 ?.展开更多
High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Exten...High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Extensive studies on the deformation mech-anisms of HEAs can guide microstructure control and toughness design,which is vital for understanding and studying state-of-the-art structural materials.Synchrotron X-ray and neutron diffraction are necessary techniques for materials science research,especially for in situ coupling of physical/chemical fields and for resolving macro/microcrystallographic information on materials.Recently,several re-searchers have applied synchrotron X-ray and neutron diffraction methods to study the deformation mechanisms,phase transformations,stress behaviors,and in situ processes of HEAs,such as variable-temperature,high-pressure,and hydrogenation processes.In this review,the principles and development of synchrotron X-ray and neutron diffraction are presented,and their applications in the deformation mechanisms of HEAs are discussed.The factors that influence the deformation mechanisms of HEAs are also outlined.This review fo-cuses on the microstructures and micromechanical behaviors during tension/compression or creep/fatigue deformation and the application of synchrotron X-ray and neutron diffraction methods to the characterization of dislocations,stacking faults,twins,phases,and intergrain/interphase stress changes.Perspectives on future developments of synchrotron X-ray and neutron diffraction and on research directions on the deformation mechanisms of novel metals are discussed.展开更多
Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we i...Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we investigate the intensity correlation between the split x-ray beams by Laue diffraction of stress-free crystal. The analysis based on the dynamical theory of x-ray diffraction indicates that the spatial resolution of diffraction image and transmission image are reduced due to the position shift of the exit beam. In the experimental setup, a stress-free crystal with a thickness of hundredmicrometers-level is used for beam splitting. The crystal is in a non-dispersive configuration equipped with a double-crystal monochromator to ensure that the dimension of the diffraction beam and transmission beam are consistent. A correlation coefficient of 0.92 is achieved experimentally and the high signal-to-noise ratio of the x-ray ghost imaging is anticipated.Results of this paper demonstrate that the developed beam splitter of Laue crystal has the potential in the efficient data acquisition of x-ray ghost imaging.展开更多
オ-ray powder diffraction data and crystal structure of RE compound NdCoGe3 were studied by using X-ray powder diffraction and refined by the Rietveld profile fitting method. The compound has the tetragonal BaNiSn3typ...オ-ray powder diffraction data and crystal structure of RE compound NdCoGe3 were studied by using X-ray powder diffraction and refined by the Rietveld profile fitting method. The compound has the tetragonal BaNiSn3type structure, space group I4mm (No.107) a=0.42961(2) nm, c=098147(4) nm, V=0.018114 nm3, Z=2 and Dx=7.717 g·cm-3. The figure of merit FN for the powder data is F30=623 (0.0107, 45). Structure refinement was performed with 110 reflections and led to Rp=11.78% and Rwp=16.56%.展开更多
Tin(Sn)holds great promise as an anode material for next-generation lithium(Li)ion batteries but suffers from massive volume change and poor cycling performance.To clarify the dynamic chemical and microstructural evol...Tin(Sn)holds great promise as an anode material for next-generation lithium(Li)ion batteries but suffers from massive volume change and poor cycling performance.To clarify the dynamic chemical and microstructural evolution of Sn anode during lithiation and delithiation,synchrotron X-ray energydispersive diffraction and X-ray tomography are simultaneously employed during Li/Sn cell operation.The intermediate Li-Sn alloy phases during de/lithiation are identified,and their dynamic phase transformation is unraveled which is further correlated with the volume variation of the Sn at particle-and electrode-level.Moreover,we find that the Sn particle expansion/shrinkage induced particle displacement is anisotropic:the displacement perpendicular to the electrode surface(z-axis)is more pronounced compared to the directions(x-and y-axis)along the electrode surface.This anisotropic particle displacement leads to an anisotropic volume variation at the electrode level and eventually generates a net electrode expansion towards the separator after cycling,which could be one of the root causes of mechanical detachment and delamination of electrodes during long-term operation.The unraveled chemical evolution of Li-Sn and deep insights into the microstructural evolution of Sn anode provided here could guide future design and engineering of Sn and other alloy anodes for high energy density Li-and Na-ion batteries.展开更多
Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crys...Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form. Unfortunately, it is usually found in a polymorphic mixture with form B. In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FT-IR) and thermal analysis. An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters. The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0- 100% (w/w), good linear relationship, with R2= 0.999, excellent repeatability and precision and low limits of detection (LoD) of 0.15% (w/w) and quantification (LoQ) of 0.5% (w/w). The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method. This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs (forms A and B) quantitatively and control the quality of the bulk drug.展开更多
The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction....The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).展开更多
This research reports the processing of magnesium matrix composites reinforced with silicon carbide(SiC)and aluminium oxide(Al_(2)O_(3))using powder metallurgy technique through high energy milling.Samples of Mg-SiC a...This research reports the processing of magnesium matrix composites reinforced with silicon carbide(SiC)and aluminium oxide(Al_(2)O_(3))using powder metallurgy technique through high energy milling.Samples of Mg-SiC and Mg-Al_(2)O_(3)composites subjected to high energy ball milling for different vol%of secondary particles 20,30 and 40%of SiC and Al_(2)O_(3)are studied by X-Ray diffraction technique.The rietveld method as implemented in the Fullprof program is applied in order to determine the quantities of the resulting crystalline phases and amorphous phases at each stage of the mechanical treatment.Microstructural examination is carried out using Scanning Electron Microscope(SEM).In addition,crystal structural analysis using appropriate size and strain models is performed in order to handle the distinctive anistrophy that is observed in convinced crystallographic directions for the magnesium composite.The results are furnished in terms of crystalline domains size enlargement of the magnesium composites phases upon prolonged milling duration and discussed in the light of up to date views and theories on crystal growth of nanocrystaline materials.The hardness of the composite samples is calculated by Vickers’s Hardness tester.Further,dry sling wear test and corrosion test are performed for the fabricated composites.Composite with 30%secondary particles incorporated magnesium composites exhibits better wear and corrosion resistance than the other composites.展开更多
The isothermal section of the Ho-Ni-Si system at 773 K was constructed by X-ray powder diffraction(XRD)in this work.The system contains sixteen known type structure compounds TiNiSi-type HoNiSi,BaAl4-type HoNi2Si2,CeN...The isothermal section of the Ho-Ni-Si system at 773 K was constructed by X-ray powder diffraction(XRD)in this work.The system contains sixteen known type structure compounds TiNiSi-type HoNiSi,BaAl4-type HoNi2Si2,CeNiSi2-type HoNiSi2,U1Co3Si5-type Ho2Ni3Si5,SmNiGe3-type HoNiSi3,Ce3 Ni6Si2-type Ho3Ni6Si2,ThMn12-type HoNi10Si2,YPd2Si-type HoNi2Si,YNi5Si3-type HoNi5Si3,YNi4Si-type HoNi4Si,Gd3NiSi2-type Ho3NiSi2,YNi6Si6-type HoNi6Si6.AlB2-type Ho2NiSi3,AlB2-type Ho3Ni2Si4,AlB2-type Ho4NiSi7,Gd3Ru4Al12-type Ho8Ni31Si11,and one unknown type structure compound Ho5Ni2Si3.At the same time,one unknown structure new phase Ho37Ni3Si60 was observed.In ternary compounds,Ho2NiSi3 and Ho4NiSi7 have the solid solution phenomena;the solid solution ranges are about Ho33.3Ni18.7-9.7Si-48.0-57.0 and Ho33.Ni-8.3-2.6Si-58.3-64.1,respectively.At the same time,quasi-binary solid solutions were detected at 773 K for Ho2Ni17,HoNi5,Ho2Ni7,HoNi3,HoNi2,HoNi,HoSi.Other binary compounds of the Ho-Ni-Si system do not show any visible solubility.The magnetic property studies show that Ho3NiSi2 compound has two successive magnetic phase transitions in a low field:a spinreorientation transition at TSR=10 K and a second order ferromagnetic(FM)-paramagnetic(PM)transition at Tc=37 K.展开更多
Based on the techniques of sequential extraction and X-ray powder diffraction(XRD) ,the distribution characteristics of phosphorus speciation were investigated in 13 sediment samples from Lake Hongfeng,an important dr...Based on the techniques of sequential extraction and X-ray powder diffraction(XRD) ,the distribution characteristics of phosphorus speciation were investigated in 13 sediment samples from Lake Hongfeng,an important drinking water source for Guiyang with a typical karstic limestone environment.The total phosphorus(TP) concentrations in the sediments ranged from 973.36 to 2334.18 mg/kg with a mean concentration of 1635.87 mg/kg(dry weight) ,and it was evident that the phosphorus level in the sediments was high compared with other eutrophic lakes such as Lake Chaohu and Lake Xihu.The results of the two methods,sequential extraction and XRD,demonstrated the presence of different phosphorus species in the lake sediments.Being compatible with local geophysical characteristics,the results of sequential extraction techniques indicate that the average percentages of dissolved phosphorus(DP) ,aluminum-bound phosphorus(Al-P) ,iron-bound phosphorus(Fe-P) ,calcium-bound phosphorus(Ca-P) and organic phosphorus(OP) in the sediments were 0.40%,7.06%,5.07%,45.48%and 38.49%,respectively.Notably,the concentrations of inorganic phosphorus(IP) were higher than those of OP,and the IP consisted primarily of Ca-P.The high concentrations of Ca-P may temporarily control the release of phosphorus from the sediments because it is a relatively stable,inert and non-bioavailable phosphorus fraction.The results of XRD analysis indicated that,among phosphorus species,AlPO4 was found in all sediment samples at relatively high concentrations.Moreover,the TP concentrations in the sediments were high;thus the release potential and bioavailability of phosphorus in the sediments was important.Further statistical analyses of the results revealed significant correlations between phosphorus species in the sediments with two extractable principal components and four selectable cluster levels allowing interpretation of possible origins of phosphorus loading and transformation mechanisms of phosphorus species.Furthermore,available remediation measures were briefly assessed for the lake while considering its distinct environmental features.展开更多
基金financially supported by the Natural Science Foundation of China(Grant 40872033)the Fundamental Research Funds for the Central Universities(to XL)the Natural Sciences and Engineering Research Council of Canada(to MF)
文摘The thermal expansion coefficients of kyanite at ambient pressure have been investigated by an X-ray powder diffraction technique with temperatures up to 1000 ℃. No phase transition was observed in the experimental temperature range. Data for the unit-cell parameters and temperatures were fitted empirically resulting in the following thermal expansion coefficients: αa = 5.8(3) × 10^-5, αb = 5.8 (1)× 10^-5, αc = 5.2(1)× 10^-5, and αv = 7.4(1) × 10^-3 ℃ 1 in good agreement with a recent neutron powder diffraction study. On the other hand, the variation of the unit-cell angles α, β and γ of kyanite with increase in temperature is very complicated, and the agreement among all studies is poor. The thermal expansion data at ambient pressure reported here and the compression data at ambient temperature from the literature suggest that, for the kyanite lattice, the most and least thermally expandable directions correspond to the most and least compressible directions, respectively.
文摘The crystal structure of [Co(NH3)5Br]Br2 has been determined ab initio from the conventional X-ray powder diffraction data. The approximate structure with all 7 indeyendent non-H atoms was solved by direct methods. The final orthorhombic unit-cell parameters after Rietveld refinement are: a=13.6927, b=10.7071, c=6.9400A, V=1017.47A3, F30=93(0.0075,43), M20=49, Z=4. Space group is Pnma. The structure agreement factors are: Rp=0.066,Rwp=0.090, RF=0.041, RB=0.042.
文摘The X-ray powder diffraction data of the compound GdAlSi was studied by means of X-ray diffraction technique and refined by Rietveld method. The compound GdAlSi has tetragonal α-ThSi_2-type structure, space group I4_1/amd (No.141), Z=4, the lattice parameters a=041234 (1) nm, c=1.44202(1) nm. The Smith and Snyder figure of merit [5] F_N is F_ 30=2521(36). The R-factors of Rietveld refinement are R_p=0.098 and R_ wp=0.128. The X-ray powder diffraction data are given. The field dependence of the magnetization measured at room temperature and the temperature variation of the inverse magnetic susceptibility of the compound GdAlSi were also presented.
文摘In cooperation with figure-of-merits the Rietveld analysis can appraise both angular and intensity data of powder diffraction. In this work, X-ray diffraction pattern of Bi4(SiO4)3 was redetermined with intensity figure-of-merits, which qualify agreement between observed and calculated relative intensities. F30 is 158.90 (0.0059, 32), intensity figure of merit Rint is 8.7, I20(17), 8.0. The values of figure-of-merits show that the data of JCPDS cards are distorted. Both the experimental and calculated peak positions and heights are listed in detail.
文摘A new method for pattern identification and simulation of X-ray powder diffraction data is described, which can give definite phase composition of the unknown rapidly and correctly. The method is implemented in Microsoft Fortran 77 for the IBM PC/XT/AT personal computer or their compatibles.
基金Supported by a Grant-in-Aid from the International Centre for Diffraction Data and the Natural Science Foundation of Guangxi Zhuang Autonomous Region。
文摘The compound GdNiSn has been studied by X-ray powder diffraction technique.The crystal structure and the X-ray diffraction data for this compound at room temperature are reported.The compound GdNiSn is orthorhombic with lattice parameters a=7.2044(1)A,b=7.6895(6)A,c=4.4772(4)A,space group Pna2_(1) and 4 formula units of GdNiSn in unit cell.The Smith and Snyder figure of index F_(30) for this compound is 35(0.015,59).
基金Fund by International Centre for Dlffractlon Data.
文摘A new compound K6FeNb15O42 was prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The X-ray powder diffraction data of the title compound was measured. K6FeNb15 O42 crystallizes in the hexagonal system with unit cell parameters, a = 9. 1320(4) A ,c = 12. 0670(9) A , and space group P63/mcm (193) , z = 1. The calculated and measured densities are 4. 489 g/cm3 and 4. 485 g. cm3, respectively.
文摘The 773 K isothermal section of the La-Fe-Sn ternary system was investigated and constructed by X-ray powder diffraction(XRD).The existence of two reported ternary intermetallic compounds,La6Fe13Sn and La3FeSn6,is confirmed in this work.Compared with other R-Fe-Sn phase diagrams(R = Pr and Sm),the binary alloys Fe3Sn and Fe5Sn3 are not present.The compound Fe3Sn2 was observed from the XRD pattern of Fe3Sn2 samples,but it is not an equilibrium phase at 773 K and decomposes into Fe and FeSn phases completely for a longer heat treated time.Up to now,the crystal structure data of La2Sn3 has not been reported,so the X-ray pattern of La2Sn3 was only estimated.The phase relationship for this compound was drawn by a dotted line.
文摘A new compound K6FeNb15O42 u(?) prepared for the first time by solid state reaction in K2O-Fe2O3-Nb2O5 ternary system. The XRD data of the title compound was determined. K6FeNb15O42 crystallizes the hexagonal system with unit cell parameters a=9. 1320(4) A,c=12. 0670(9) A, and space group P63/mcm(193) , 2=1. The calculated and measured densities are 4. 489 g/ cm3 and 4. 485 g. cm3, respectively.
文摘CuKβ radiation with a wavelength of λ = 1.3923 ? is recommended for crystal structure determination from X-ray powder diffraction using the Rietfeld method. A highly sensitive image plate detector is able to collect enough intensity to record a brilliant X-ray powder pattern in a reasonable time, compared to CuKα1 radiation used today. Especially atomic displacement coefficients could be determined more precisely with the much greater number of reflections recorded. A double-radius Guinier camera attached to a micro-focus rotating anode tube ensures increased brilliance besides high resolution. A simple construction specification is presented to make smart cylindrically bent Ge(111) or Si(111) X-ray monochromators that deliver focused CuKβ radiation. The highly linear response of image plate detectors allows removing of fluorescence radiation simply as background of the pattern. The proposed equipment is a cost-efficient alternative to a liquid gallium-metal-jet X-ray source with maximum power load and a similar wavelength of λ(GaKα1) = 1.34013 ?.
基金supported by the National Natural Science Foundation of China(Nos.52171098 and 51921001)the State Key Laboratory for Advanced Metals and Materials(No.2022Z-02)+1 种基金the National High-level Personnel of Special Support Program(No.ZYZZ2021001)the Fundamental Research Funds for the Central Universities(Nos.FRF-TP-20-03C2 and FRF-BD-20-02B).
文摘High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Extensive studies on the deformation mech-anisms of HEAs can guide microstructure control and toughness design,which is vital for understanding and studying state-of-the-art structural materials.Synchrotron X-ray and neutron diffraction are necessary techniques for materials science research,especially for in situ coupling of physical/chemical fields and for resolving macro/microcrystallographic information on materials.Recently,several re-searchers have applied synchrotron X-ray and neutron diffraction methods to study the deformation mechanisms,phase transformations,stress behaviors,and in situ processes of HEAs,such as variable-temperature,high-pressure,and hydrogenation processes.In this review,the principles and development of synchrotron X-ray and neutron diffraction are presented,and their applications in the deformation mechanisms of HEAs are discussed.The factors that influence the deformation mechanisms of HEAs are also outlined.This review fo-cuses on the microstructures and micromechanical behaviors during tension/compression or creep/fatigue deformation and the application of synchrotron X-ray and neutron diffraction methods to the characterization of dislocations,stacking faults,twins,phases,and intergrain/interphase stress changes.Perspectives on future developments of synchrotron X-ray and neutron diffraction and on research directions on the deformation mechanisms of novel metals are discussed.
基金Project supported by the National Key Research and Development Program of China (Grant Nos.2022YFF0709103,2022YFA1603601,2021YFF0601203,and 2021YFA1600703)the National Natural Science Foundation of China (Grant No.81430087)the Shanghai Pilot Program for Basic Research-Chinese Academy of Sciences,Shanghai Branch (Grant No.JCYJ-SHFY-2021-010)。
文摘Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we investigate the intensity correlation between the split x-ray beams by Laue diffraction of stress-free crystal. The analysis based on the dynamical theory of x-ray diffraction indicates that the spatial resolution of diffraction image and transmission image are reduced due to the position shift of the exit beam. In the experimental setup, a stress-free crystal with a thickness of hundredmicrometers-level is used for beam splitting. The crystal is in a non-dispersive configuration equipped with a double-crystal monochromator to ensure that the dimension of the diffraction beam and transmission beam are consistent. A correlation coefficient of 0.92 is achieved experimentally and the high signal-to-noise ratio of the x-ray ghost imaging is anticipated.Results of this paper demonstrate that the developed beam splitter of Laue crystal has the potential in the efficient data acquisition of x-ray ghost imaging.
文摘オ-ray powder diffraction data and crystal structure of RE compound NdCoGe3 were studied by using X-ray powder diffraction and refined by the Rietveld profile fitting method. The compound has the tetragonal BaNiSn3type structure, space group I4mm (No.107) a=0.42961(2) nm, c=098147(4) nm, V=0.018114 nm3, Z=2 and Dx=7.717 g·cm-3. The figure of merit FN for the powder data is F30=623 (0.0107, 45). Structure refinement was performed with 110 reflections and led to Rp=11.78% and Rwp=16.56%.
基金sponsored by the Helmholtz Association,the China Scholarship Council(CSC)partially funded by the German Research Foundation,DFG(Project No.MA 5039/4-1)。
文摘Tin(Sn)holds great promise as an anode material for next-generation lithium(Li)ion batteries but suffers from massive volume change and poor cycling performance.To clarify the dynamic chemical and microstructural evolution of Sn anode during lithiation and delithiation,synchrotron X-ray energydispersive diffraction and X-ray tomography are simultaneously employed during Li/Sn cell operation.The intermediate Li-Sn alloy phases during de/lithiation are identified,and their dynamic phase transformation is unraveled which is further correlated with the volume variation of the Sn at particle-and electrode-level.Moreover,we find that the Sn particle expansion/shrinkage induced particle displacement is anisotropic:the displacement perpendicular to the electrode surface(z-axis)is more pronounced compared to the directions(x-and y-axis)along the electrode surface.This anisotropic particle displacement leads to an anisotropic volume variation at the electrode level and eventually generates a net electrode expansion towards the separator after cycling,which could be one of the root causes of mechanical detachment and delamination of electrodes during long-term operation.The unraveled chemical evolution of Li-Sn and deep insights into the microstructural evolution of Sn anode provided here could guide future design and engineering of Sn and other alloy anodes for high energy density Li-and Na-ion batteries.
基金supported by the Major Program of Ministry of Science and Technology of China(No:2015ZX09J15104-003002)
文摘Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form. Unfortunately, it is usually found in a polymorphic mixture with form B. In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FT-IR) and thermal analysis. An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters. The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0- 100% (w/w), good linear relationship, with R2= 0.999, excellent repeatability and precision and low limits of detection (LoD) of 0.15% (w/w) and quantification (LoQ) of 0.5% (w/w). The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method. This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs (forms A and B) quantitatively and control the quality of the bulk drug.
基金supported by National Natural Science Foundation of China(U2032118 and 42172048)Guizhou Provincial Science and Technology Projects(QKHPTRCYQK[2023]035 and QKHJC-ZK[2021]ZD042)+1 种基金Hundred Talents Program of the Chinese Academy of SciencesGuizhou Provincial 2020 and 2021 Science and Technology Subsidies(Nos.GZ2020SIG and GZ2021SIG)。
文摘The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).
文摘This research reports the processing of magnesium matrix composites reinforced with silicon carbide(SiC)and aluminium oxide(Al_(2)O_(3))using powder metallurgy technique through high energy milling.Samples of Mg-SiC and Mg-Al_(2)O_(3)composites subjected to high energy ball milling for different vol%of secondary particles 20,30 and 40%of SiC and Al_(2)O_(3)are studied by X-Ray diffraction technique.The rietveld method as implemented in the Fullprof program is applied in order to determine the quantities of the resulting crystalline phases and amorphous phases at each stage of the mechanical treatment.Microstructural examination is carried out using Scanning Electron Microscope(SEM).In addition,crystal structural analysis using appropriate size and strain models is performed in order to handle the distinctive anistrophy that is observed in convinced crystallographic directions for the magnesium composite.The results are furnished in terms of crystalline domains size enlargement of the magnesium composites phases upon prolonged milling duration and discussed in the light of up to date views and theories on crystal growth of nanocrystaline materials.The hardness of the composite samples is calculated by Vickers’s Hardness tester.Further,dry sling wear test and corrosion test are performed for the fabricated composites.Composite with 30%secondary particles incorporated magnesium composites exhibits better wear and corrosion resistance than the other composites.
基金Project supported by the Department of Science and Technology of Sichuan Province in China(2017JY0181)。
文摘The isothermal section of the Ho-Ni-Si system at 773 K was constructed by X-ray powder diffraction(XRD)in this work.The system contains sixteen known type structure compounds TiNiSi-type HoNiSi,BaAl4-type HoNi2Si2,CeNiSi2-type HoNiSi2,U1Co3Si5-type Ho2Ni3Si5,SmNiGe3-type HoNiSi3,Ce3 Ni6Si2-type Ho3Ni6Si2,ThMn12-type HoNi10Si2,YPd2Si-type HoNi2Si,YNi5Si3-type HoNi5Si3,YNi4Si-type HoNi4Si,Gd3NiSi2-type Ho3NiSi2,YNi6Si6-type HoNi6Si6.AlB2-type Ho2NiSi3,AlB2-type Ho3Ni2Si4,AlB2-type Ho4NiSi7,Gd3Ru4Al12-type Ho8Ni31Si11,and one unknown type structure compound Ho5Ni2Si3.At the same time,one unknown structure new phase Ho37Ni3Si60 was observed.In ternary compounds,Ho2NiSi3 and Ho4NiSi7 have the solid solution phenomena;the solid solution ranges are about Ho33.3Ni18.7-9.7Si-48.0-57.0 and Ho33.Ni-8.3-2.6Si-58.3-64.1,respectively.At the same time,quasi-binary solid solutions were detected at 773 K for Ho2Ni17,HoNi5,Ho2Ni7,HoNi3,HoNi2,HoNi,HoSi.Other binary compounds of the Ho-Ni-Si system do not show any visible solubility.The magnetic property studies show that Ho3NiSi2 compound has two successive magnetic phase transitions in a low field:a spinreorientation transition at TSR=10 K and a second order ferromagnetic(FM)-paramagnetic(PM)transition at Tc=37 K.
基金supported by the National Natural Science Foundation of China(20967003)
文摘Based on the techniques of sequential extraction and X-ray powder diffraction(XRD) ,the distribution characteristics of phosphorus speciation were investigated in 13 sediment samples from Lake Hongfeng,an important drinking water source for Guiyang with a typical karstic limestone environment.The total phosphorus(TP) concentrations in the sediments ranged from 973.36 to 2334.18 mg/kg with a mean concentration of 1635.87 mg/kg(dry weight) ,and it was evident that the phosphorus level in the sediments was high compared with other eutrophic lakes such as Lake Chaohu and Lake Xihu.The results of the two methods,sequential extraction and XRD,demonstrated the presence of different phosphorus species in the lake sediments.Being compatible with local geophysical characteristics,the results of sequential extraction techniques indicate that the average percentages of dissolved phosphorus(DP) ,aluminum-bound phosphorus(Al-P) ,iron-bound phosphorus(Fe-P) ,calcium-bound phosphorus(Ca-P) and organic phosphorus(OP) in the sediments were 0.40%,7.06%,5.07%,45.48%and 38.49%,respectively.Notably,the concentrations of inorganic phosphorus(IP) were higher than those of OP,and the IP consisted primarily of Ca-P.The high concentrations of Ca-P may temporarily control the release of phosphorus from the sediments because it is a relatively stable,inert and non-bioavailable phosphorus fraction.The results of XRD analysis indicated that,among phosphorus species,AlPO4 was found in all sediment samples at relatively high concentrations.Moreover,the TP concentrations in the sediments were high;thus the release potential and bioavailability of phosphorus in the sediments was important.Further statistical analyses of the results revealed significant correlations between phosphorus species in the sediments with two extractable principal components and four selectable cluster levels allowing interpretation of possible origins of phosphorus loading and transformation mechanisms of phosphorus species.Furthermore,available remediation measures were briefly assessed for the lake while considering its distinct environmental features.