DETERMINATION OFTHE CRYSTALLINITY IN DIFFERENT TYPE POLY (OXYETHYLENE-STYRENE)BLOCK COPOLYMERS BY X-RAY DIFFRACTION METHOD

By means of the intensity theory of X-ray scattering and the two-phase concept of high polymer, the basic formula of the crystaUinity in block copolymers has been proposed after the corrections of atomic, temperature, absorption, Lorentz and polarization factor. Application of this method to different type poly (oxyethylene-styrene)block copolymers and the same type block copolymers with different EO contents indicates that the crystallinity in poly (oxyethylene-styrene ) block copolymers increases with the increase of the EO content and decreases in the order: PEO-PS-PEO>PEO-PS>PS-PEO-PS.

Residual stress measurement of coarse-grain aluminum alloy using X-ray diffraction method

When measuring residual stress of coarse-grain aluminum alloy using X-ray diffraction method, the diffraction profile shows two peaks and position of measured 20 will be changed, which lead to an inaccurate measurement result. Hence, in this paper, some methods were employed to improve the measurement accuracy. During the measuring process, different parameters （diameter of irradiated area, Ψ-oscillation range and exposure time） were selected and profile peak shift method was utilized. Moreover, when the 20 of profiles was determined, different calculation methods were used to calculate the residual stress. The results show that diameter of irradiated area and Ψ-oscillation range have significant influence on the measuring result. For stress value calculated directly from the test equipment, cross correlation method is more accurate than the absolute peak. Furthermore, another two calculation methods of slope with 2θ- sin^2Ψ and ε- sin^2Ψwere used to calculate the stress based on parameters （2θ, ε） obtained from cross correlation method. It is concluded that 2θ - sin^2Ψ method can further improve the measurement accuracy.

Microstructures and micromechanical behaviors of high -entropy alloys investigated by synchrotron X-ray and neutron diffraction techniques: A review

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.

Intensity correlation properties of x-ray beams split with Laue diffraction

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.

Tracking the phase transformation and microstructural evolution of Sn anode using operando synchrotron X-ray energy-dispersive diffraction and X-ray tomography

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.

STRUCTURE DETERMINATION OF KANGLEMEISU A BY X-RAY DIFFRACTION METHOD

Kanglemeisu A (C50H63O19N·CH3OH) is the product of an actinomyces species from a soil sample gathered in China. Kanglemeisu A belongs to the triclinic system, space group P1,unit cell:a=12.760（3）, b=10.287（2）, c=9.926（2） , α=88.39（2）,β=78.64（2）, γ=89.14（2）. RANTAN direct method is used to solve the structure.The final discrepancy factor is R=0.0689, after atom coordinates and temperature factors have been refined with full matrix least squares.The structure skeleton consists of four parts, the naphthalene nucleus connected to the 5-membered ring, a 17-membered ring connected to C2, a dimethyl butane diacid extended out from C20, β-D-3,4-OO’ methylenedigitoxose passing through an oxygen bridge O6 and linked to C27 of ansa ring.

Thermal expansivity of geikielite and ilmenite utilizing in-situ synchrotron X-ray diffraction at high temperature

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).

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.

The determination of the crystal struoure of tetra-potassium uranyl tricarbonate by powder X-ray diffraction method

A uranyl compound, K_4UO_2(CO_3)_3 has been characterized by powder X-ray diffraction method. M. W.=606.46, monoclinic, C2/c (No. 15), a=1.0240(7), b=0.9198(4), c=1.2222(12)nm, β=95.12(4)°,V=1.1466(5)nm^3, Z=4, D_m=3.468g/cm^3, D_c=3.513g/cm~, λ(Cu Kα_1)=O.1540598nm, T=298K. The structure was solved by heavy atom method and Fourier synthesis, and refined by full- matrix least-squares method to R=0.1185 for 275 reflections. The uranium (Ⅵ) atom is in an eight-coordinate distorted hexagonal-bipyramidal environment with creasy fan shape. The linear uranyl group approaches to perpendicular to the equatorial plane in which three carbonate groups are chelated. U(Ⅵ) has two linear oxygen atoms closer to it (U-O=0.1767 (5) nm) than six other neighbours (U-O ranging from 0.2516 to 0.2568nm). The distances between carbon atoms and uncoordinated oxygen atoms are 0.122 (1) and 0.123(1) nm, which are distinctly different from those between carbon and coordinated oxygen atoms (mean 0.134(6) nm). This fact reveals the non-eq- uivalence of one oxygen atom to the other two in each carbonate. In K_4UO_2(CO_3)_3, the O-O dis- tance for the adjacent carbonate groups is 0.2794(4)nm approaching to the sum of Van der Waals radii of two oxygen atoms. The K-O distances vary between 0.2667 and 0.3131nm, and each anion is immediately surrounded by six potassium ions, only four of which can be considered to belong to the same structural formula unit, and they are symmetrically located above and below the equatorial plane.

MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

Influence of Replacement Level of Coal-series Kaolin on Hydration of Ordinary Portland Cement by X-ray Diffraction/Rietveld Method

The influence of replacement level of calcined coal-series kaolin(CCK) on hydration of ordinary Portland cement(OPC) was studied by X-ray diffraction(XRD)/Rietveld method. X-ray diffraction/Rietveld method was used to quantify the crystalline phase composition of the hydrated samples. Additionally, the morphology of hydrated samples was observed by scanning electron microscopy(SEM). The results showed that, calcium hydroxide(CH), ettringite(AFt) and amorphous phase content in hydrated samples decreased as the replacement level of CCK increased, while AFm and str?tlingite increased, which was caused by the combination of dilute, physical and pozzolanic effects. The hydration of anhydrous cement phases was accelerated by physical effect but hindered by the retardation effect of CCK. The role of each effects was discussed in detail to analyze the mechanism of OPC hydration with CCK addition. The SEM images showed that the shortening of AFt at 1 day and the denser texture at 28 days was observed with CCK addition, which was caused by the physical and pozzolanic effects, respectively.

Correlation between crystal structure and mechanical performance of Cr-implanted 300M high-strength steel using X-ray diffraction method

In order to study the influence of crystal structure change due to implantation dose on the hardness and wear performance of 300M high-strength steel,samples were surface modified by Cr implantation with dosages of 5.0 × 10^16,1.5 × 10^17 and 3.0 × 10^17 ions/cm^2.X-ray diffraction method,which was already applied in studies on the microstructure of deformed and heat-treated materials,was used to study the crystal structure of the implanted steel,and the results were corrected with the hardness and wear performance.The solid solution strengthening effect and microstructure vary with increase in implantation dose.Owing to strong solid solution hardening of Cr,small average crystallite size and high dislocation density,the hardness and wear resistance of implanted steel with dose of 5.0 × 10^16 ions/cm^2 were found to be the highest compared with other samples.Moreover,although the crystal lite size of the implanted sample with dose of 3 × 10^17 ions/cm^2 was similar to that of substrate and the dislocation density was lower than that of the substrate,its higher hardness and lower specific wear rate were due to the solid solution hardening and perhaps Cr clusters reinforcement.

In situ X-ray diffraction and thermal analysis of LiNi0.8Co0.15Al0.05O2 synthesized via co-precipitation method

LiNi0.9Co0.15Al0.05O2 （NCA） material is successfully synthesized with a modified co-precipitation method,in which NH3,H2O and EDTA are used as two chelating agents. The obtained LiNi0.9Co0.15Al0.05O2 materialhas well-defined layered structure and uniform element distribution, which reveals an enhanced electro-chemical performance with a capacity retention of 97.9% after 100 cycles at 0.2 C, and reduced thermalrunaway from the isothermal calorimetry test. In situ X-ray diffraction （XRD） was employed to capturethe structural changes during the charge-discharge process. The reversible evolutions of lattice parame-ters （a, b, c, and V） further verify the structural stability.

Fitting Full X-Ray Diffraction Patterns for Quantitative Analysis: A Method for Readily Quantifying Crystalline and Disordered Phases

Fitting of full X-ray diffraction patterns is an effective method for quantifying abundances during X-ray diffraction (XRD) analyses. The method is based on the principal that the observed diffraction pattern is the sum of the individual phases that compose the sample. By adding an internal standard (usually corundum) to both the observed patterns and to those for individual pure phases (standards), all patterns can all be normalized to an equivalent intensity based on the internal standard intensity. Using least-squares refinement, the individual phase proportions are varied until an optimal match is reached. As the fitting of full patterns uses the entire pattern, including background, disordered and amorphous phases are explicitly considered as individual phases, with their individual intensity profiles or “amorphous humps” included in the refinement. The method can be applied not only to samples that contain well-ordered materials, but it is particularly well suited for samples containing amorphous and/or disordered materials. In cases with extremely disordered materials where no crystal structure is available for Rietveld refinement or there is no unique intensity area that can be measured for a traditional RIR analysis, full-pattern fitting may be the best or only way to readily obtain quantitative results. This approach is also applicable in cases where there are several coexisting highly disordered phases. As all phases are considered as discrete individual components, abundances are not constrained to sum to 100%.

AN INCREMENTAL METHOD OF X-RAY DIFFRACTION QUANTITATIVE PHASE ANALYSIS OF SAMPLESCONTAINING AMORPHOUS MATERIAL

A new method for quantitative X-ray diffraction phase analysis of a powder misture has been developed according to Popovic's doping method. The weight fraction of amorphous material in the analysed sample is obtained. For a multicomponent system in which (n-2) pure phases are added into an n-phase compnent sample and theweight fractions of all n phases can be determined by the method. The test results of confirmation agree well with the theory.

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.

The Method of Testing for Asbestos in Electronic and Electric Products through Polarizing Microscope and X-Ray Diffraction

Asbestos is widely applied in such sectors as manufacturing automobiles, tractors, chemical industrial equipment, and electric equipment. Asbestos fiber is harmful to human health. Therefore, the technology of testing for asbestos in products is especially important. At present, in our country’s national specifications, there is no determination method or specification that is applicable to the asbestos in electronic and electric products. In this article, the components of asbestos in electronic and electric products are identified using the method of combining polarizing microscope with X-ray diffractometer. This method is simple, fast, highly reliable, and suitable to be widely adopted.

Determination of Residuals Stresses Induced by the Autofrettage Treatment by the X-Rays Diffraction Method

Some meaningful advances have been made these last years to value precise and reliable way the residual stresses experimentally created by the autofrettage. The autofrettage process is used widely to introduce residual stresses into thick walled tubes;traditionally residual stresses have been measured using the Sachs method destructive or non-destructive methods. In this paper we describe the application of the X-rays diffraction;this technique permits to justify the presence of the compressive tangential residual stresses, and to value their distribution after two different autofrettage internal pressures loading. The results show that there is a large difference in the residual stresses find in the different autofrettege pressure. One can see the influence of the autofrettage’s pressure quantity on residual stresses created in the thickness of the test tubes.

A Hybrid Angular/Energy Dispersive Method to Improve Some Characteristics of Laboratory X-Ray Diffraction

The Energy Dispersive X-ray Diffraction, generally referred as EDXD, has shown to be a valid alternative to the conventional Angular Dispersive X-ray Diffraction, the ADXD. EDXD exhibits several advantages to its AD counterpart, mainly related to the properties of the polychromatic X-ray beam utilized for diffracting, such as higher signal intensities, a wider accessible region of the reciprocal space, a greater transparency of samples, and a parallel data collection of the q-points in the diffraction pattern acquisition. However, the main drawback of poly-chromaticity lays in the fact that the quantities that modulate the scattered intensity in a diffraction measurement depend on the energy. These quantities are the primary X-ray beam spectrum, polarization, and X-ray absorption, the last producing by far the most critical effect because it rapidly changes as a function of energy. Therefore, a detailed knowledge of the energy dependence of all these quantities is required in EDXD in order to process the data correctly and prevent systematic errors. The difficulty in handling the energy-dependent factors complicates the experimental procedure and may make the measurements unreliable. In the present paper, a hybrid method between the ED and AD X-ray Diffraction is proposed to maintain the advantages of the polychromatic nature of the radiation utilized in EDXD, while preventing the problems produced by the energy-dependent quantities.

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.