Operando measurement of lattice deformation profiles of synchrotron radiation monochromator

This study presents a new method for characterizing the thermal lattice deformation of a monochromator with high precision under service conditions and first reports the operando measurements of nanoscale thermal lattice deformation on a double-crystal monochromator at different incident powers.The nanoscale thermal lattice deformation of the monochromator first crystal was obtained by analyzing the intensity of the distorted DuMond diagrams.DuMond diagrams of the 333 diffraction index,sensitive to lattice deformation,were obtained directly using a 2D detector and an analyzer crystal orthogonal to the monochromator.With increasing incident power and power density,the maximum height of the lattice deformation increased from 3.2 to 18.5 nm,and the deformation coefficient of the maximum height increased from 1.1 to 3.2 nm/W.The maximum relative standard deviation was 4.2%,and the maximum standard deviation was 0.1 nm.Based on the measured thermal deformations,the flux saturation phenomenon and critical point for the linear operation of the monochromator were predicted with increasing incident power.This study provides a simple solution to the problem of the lower precision of synchrotron radiation monochromator characterizations compared to simulations.

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction（XRD） in diamond anvil cells（DACs） using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF（Beijing Synchrotron Radiation Facility） and some results are also presented.

Microstructure and strain analysis of GaN epitaxial films using in-plane grazing incidence x-ray diffraction

This paper investigates the major structural parameters, such as crystal quality and strain state of （001）-oriented GaN thin films grown on sapphire substrates by metalorganic chemical vapour deposition, using an in-plane grazing incidence x-ray diffraction technique. The results are analysed and compared with a complementary out-of-plane x- ray diffraction technique. The twist of the GaN mosaic structure is determined through the direct grazing incidence t of （100） reflection which agrees well with the result obtained by extrapolation method. The method for directly determining the in-plane lattice parameters of the GaN layers is also presented. Combined with the biaxial strain model, it derives the lattice parameters corresponding to fully relaxed GaN films. The GaN epilayers show an increasing residual compressive stress with increasing layer thickness when the two dimensional growth stage is established, reaching to a maximum level of-0.89 GPa.

Ultrahard X-ray multifunctional application beamline at the SSRF

The ultrahard X-ray multifunctional application beamline(BL12SW)is a phase-II beamline project at the Shanghai Syn-chrotron Radiation Facility.The primary X-ray techniques used at the beamline are high-energy X-ray diffraction and imaging using white and monochromatic light.The main scientific objectives of ultrahard X-ray beamlines are focused on two research areas.One is the study of the structural properties of Earth’s interior and new materials under extreme high-temperature and high-pressure conditions,and the other is the characterization of materials and processes in near-real service environments.The beamline utilizes a superconducting wiggler as the light source,with two diamond windows and SiC discs to filter out low-energy light(primarily below 30 keV)and a Cu filter assembly to control the thermal load entering the subsequent optical components.The beamline is equipped with dual monochromators.The first was a meridional bending Laue monochromator cooled by liquid nitrogen,achieving a full-energy coverage of 30-162 keV.The second was a sagittal bending Laue monochromator installed in an external building,providing a focused beam in the horizontal direction with an energy range of 60-120 keV.There were four experimental hutches:two large-volume press experimental hutches(LVP1 and LVP2)and two engineering material experimental hutches(ENG1 and ENG2).Each hutch was equipped with various near-real service conditions to satisfy different requirements.For example,LVP1 and LVP2 were equipped with a 200-ton DDIA press and a 2000-ton dual-mode(DDIA and Kawai)press,respectively.ENG1 and ENG2 provide in situ tensile,creep,and fatigue tests as well as high-temperature conditions.Since June 2023,the BL12SW has been in trial operation.It is expected to officially open to users by early 2024.

High-pressure investigations on Piplia Kalan eucrite meteorite using in-situ X-ray diffraction and ^(57)Fe Mssbauer spectroscopic technique up to 16 GPa

We report here high-pressure investigations on Piplia Kalan eucrite-a member of HED （Howardite -Eucrite-Diogenite） family from asteroid 4-Vesta based on synchrotron X-ray diffraction （up to 16 GPa） and ^57Fe Mossbauer spectroscopy （up to 8 GPa）. Dominant with anorthite-rich plagioclase, pigeonite-rich pyroxene and clino-ferrosilite, the sample displayed various phase transitions attaining amorphous character at 16 GPa. These phase transitions of individual components could be explained simultaneously through variations in high-pressure XRD patterns and the Mossbauer parameters. Most prominent P21/c to C2/c transition of pigeonite and ferrosilite was exhibited both as sudden variation in Mossbauer parameters and population inversion of Fe^2＋ in M1 and M2 sites between 2.9 and 3.8 GPa and variation in intensity profile in XRD patterns at 3.56 GPa. Anorthite seemed to respond more to such impact than other components in the sample. Complete amorphization in anorthite which occurred at lower pressure of - 12 GPa implied residual stress experienced due to shock impact. The presence of high pressure （monoclinic） phase of pigeonite and ferrosilite at ambient condition in this eucrite sample confirmed earlier suggestions of an early shock event. This report is an attempt to emphasize the role of anorthite in the determination of the residual stress due to impact process in the parent body thus to understand the behavioral differences amongst HED members.

Evaluation of both composition and strain distributions in InGaN epitaxial film using x-ray diffraction techniques

The composition and stain distributions in the InGaN epitaxial films are jointly measured by employing various x-ray diffraction （XRD） techniques, including out-of-plane XRD at special planes, in-plane grazing incidence XRD, and reciprocal space mapping （RSM）. It is confirmed that the measurement of （204） reflection allows a rapid access to estimate the composition without considering the influence of biaxial strain. The two-dimensional RSM checks composition and degree of strain relaxation jointly, revealing an inhomogeneous strain distribution profile along the growth direction. As the film thickness increases from 100 nm to 450 nm, the strain status of InGaN films gradually transfers from almost fully strained to fully relaxed state and then more In atoms incorporate into the film, while the near-interface region of InGaN films remains pseudomorphic to GaN.

Synchrotron radiation X-ray diffraction in situ study of fine-grained minerals in shock veins of Suizhou meteorite

The synchrotron radiation X-ray diffraction technique developed for in situ study ahigh pressure and temperature has also been used to investigate microscopic mineral inclusionsin ultrahigh-pressure metamorphic rocks and deep-mantle samples. Present study added twomore examples of successful utilization of synchrotron radiation X-ray diffraction technique for insitu investigations of fine-grained (0.5―30 μm in size) minerals in very thin shock melt veins othe Suizhou meteorite: ( i ) X-ray diffraction measurement of extremely small-sized vein matrixminerals, and (ii) identification of the micron-sized new mineral tuite embedded in the vein matrixIt has been revealed that the fine-grained vein matrix consists of well crystallized garnet, kamacite and troilite, and the powder diffraction pattern consisting of 17 lines with d-values, intensities( I ), relative intensities (I/Io) and Miller indices, as well as the cell parameters for the new mineratuite has also been successfully obtained. The result of present investigations has enriched thecontent of dynamic high-pressure mineralogy and that of Earth’s mantle geochemistry.

Establishment of Energy Dispersive X-ray Diffraction Experimental System With Synchrotron Radiation Under High Pressure

Because the interactions between molecules and atoms in mediums can be dramatically changed by compression, high pressure studies on materials can provide much information on fundamental properties including phase transition and

Phase Evolution and Thermal Expansion Behavior of aγ′Precipitated Ni-Based Superalloy by Synchrotron X-Ray Diffraction

The phase evolution and thermal expansion behavior in superalloy during heating play an essential role in controlling the size and distribution of precipitates,as well as optimizing thermomechanical properties.Synchrotron X-ray diffraction is able to go through the interior of sample and can be carried out with in situ environment,and thus,it can obtain more statistics information in real time comparing with traditional methods,such as electron and optical microscopies.In this study,in situ heating synchrotron X-ray diffraction was carried out to study the phase evolution in a typicalγ′phase precipitation strengthened Ni-based superalloy,Waspaloy,from 29 to 1050°C.Theγ′,γ,M_(23)C_(6)and M C phases,including their lattice parameters,misfits,dissolution behavior and thermal expansion coefficients,were mainly investigated.Theγ′phase and M_(23)C_(6)carbides appeared obvious dissolution during heating and re-precipitated when the temperature dropped to room temperature.Combining with the microscopy results,we can indicate that the dissolution of M_(23)C_(6)leads to the growth of grain andγ′phase cannot be completely dissolved for the short holding time above the solution temperature.Besides,the coefficients of thermal expansions of all the phases are calculated and fitted as polynomials.

Hard X-ray focusing resolution and efficiency test with a thickness correction multilayer Laue lens

The multilayer Laue lens(MLL) is a diffractive focusing optical element which can focus hard X-rays down to the nanometer scale. In this study, a WSi_(2)/Si multilayer structure consisting of 1736 layers, with a 7.2-nm-thick outermost layer and a total thickness of 17 μm, is prepared by DC magnetron sputtering. Regarding the thin film growth rate calibration, we correct the long-term growth rate drift from 2 to 0.6%, as measured by the grazing incidence X-ray reflectivity(GIXRR). A one-dimensional line focusing resolution of 64 nm was achieved,while the diffraction efficiency was 38% of the-1 order of the MLL Shanghai Synchrotron Radiation Facility(SSRF) with the BL15U beamline.

Recent Progress of Synchrotron X-Ray Imaging and Diffraction on the Solidification and Deformation Behavior of Metallic Materials

Characterizing the microstructure and deformation mechanism associated with the performances and properties of metallic materials is of great importance in understanding the microstructure-property relationship.The past few decades have witnessed the rapid development of characterization techniques from optical microscopy to electron microscopy,although these conventional methods are generally limited to the sample surface because of the intrinsic opaque nature of metallic materials.Advanced synchrotron radiation(SR)facilities can produce X-rays with strong penetrability and high spatiotemporal resolution,and thereby enabling the non-destructive visualization of full-field structural information in three dimensions.Tremendous endeavors were devoted to the 3 rd generation SR over the past three decades,in which X-ray beams have been focused down to 100 nm.In this paper,recent progresses on SR-related characterization technologies were reviewed,with particular emphases on the fundamentals of synchrotron X-ray imaging and synchrotron X-ray diffraction,as well as their applications in the in situ observations of material preparation(e.g.,in situ dendrite growth during solidification)and service under extreme environment(e.g.,in situ mechanics).Future innovations toward next-generation SR and newly emerging SRbased technologies such as dark-field X-ray microscopy and Bragg coherent X-ray diffraction imaging were also advocated.

Influence of Cryorolling on the Precipitation of Cu–Ni–Si Alloys: An In Situ X-ray Diffraction Study

The effect of cryorolling on the precipitation process of deformed Cu-Ni-Si alloys was investigated through in situ synchrotron X-ray diffraction technique. The results demonstrate that the precipitation process is significantly accelerated by cryorolling. Cryorolling produces higher dislocation density, which provides more heterogeneous nucleation sites for Ni2Si precipitates, hence promotes precipitation. In the early stage of aging, the enhanced nucleation of precipitates accelerates the depletion of supersaturation, and finer precipitates are obtained. In addition, recrystallization is promoted as a result of high stored energy in the cryorolled Cu-Ni-Si alloys, which facilitates the formation of discontinuous precipitation in the late stage of aging.

X-ray diffraction enhanced imaging study of intraocular tumors in human beings

Diffraction enhanced imaging （DEI） with edge enhancement is suitable for the observation of weakly absorbing objects. The potential ability of the DEI was explored for displaying the microanatomy and pathology of human eyeball in this work. The images of surgical specimens from malignant intraocular tumor of hospitalized patients were taken using the hard X-rays from the topography station of Beamline 4W1A at Beijing Synchrotron Radiation Facility （BSRF）. The obtained radiographic images were analyzed in correlation with those of pathology. The results show that the anatomic and pathologic details of intraocular tumors in human beings can be observed clearly by DEI for the first time, with good visualization of the microscopic details of eyeball ring such as sclera, choroids and other details of intraocular organelles. And the best resolution of DEI images reaches up to the magnitude of several tens of μm. The results suggest that it is capable of exhibiting clearly the details of intraocular tumor using DEI method.

Synchrotron radiation study on structure of Sb 5-doped Si

The impurity-doping in semiconductors is the way to control their electroinc andphoto-electronic properties. The distribution and amount of the dopant affect their physi-cal properties. The development of the molecular beam epitaxy (MBE) and other epitaxytechniques has attracted full atttention to new semiconductor materials, such assuperlattices. Recently, δ-doped semiconductors, which can reduce the scattering ofimpurity in two-dimensional electron (hole) systems, have been showing promisingpotentials for scientific researches and techmological applications.

Beam test of a one-dimensional position sensitive chamber on synchrotron radiation

A one-dimensional single-wire chamber was developed to provide high position resolution for powder diffraction experiments with synchrotron radiation. A diffraction test using the sample of SiO2 has been accomplished at 1W2B laboratory of Beijing Synchrotron Radiation Source. The data of the beam test were analyzed and some diffraction angles were obtained. The experimental results were in good agreement with standard data from ICDD powder diffraction file. The precision of diffraction angles was 1% to 4.7%. Most of the relative errors between measured values of diffraction angles and existing data were less than 1%. As for the detector, the best position resolution in the test was 138 p.m （a value） with an X-ray tube. Finally, discussions of the results were given. The major factor that affected the precision of measurement was deviation from the flat structure of the detector. The effect was analyzed and the conclusion was reached that it would be the optimal measurement scheme when the distance between the powder sample and detector was from 400 mm to 600 mm.

High resolution X-ray diffraction investigation of epitaxially grown SrTiO_3 thin films by laser-MBE

SrTiO3 thin films are epitaxially grown on DyScO3, LaAlO3 substrates with/without buffer layers of DyScO3 and SrRuO3 using laser-MBE. X-ray diffraction methods, such as high resolution X-ray diffraction, grazing incident X-ray diffraction, and reciprocal space mapping are used to investigate the lattice structure, dislocation density, in-plane lattice strain distribution along film thickness. From the measurement results, the effects of substrate on film lattice quality and microstructure are discussed.

ZnO/α-Al_2O_3界面结构的掠入射X射线衍射研究

采用脉冲激光沉积(PLD)技术,以α-Al2O3(001)为衬底,在不同衬底温度下制备ZnO薄膜。利用X射线衍射(XRD)和同步辐射掠入射X射线衍射(GID)研究了薄膜的结晶性能和薄膜与衬底的界面结构。实验结果表明,在衬底温度较低(450℃)时,ZnO薄膜主要受衬底拉应力的作用,使界面处a方向的晶格常数增大;而在衬底温度较高(750℃)时,ZnO薄膜主要受衬底压应力的作用,使界面处a方向的晶格常数减小;在优化的衬底温度(650℃)下,ZnO薄膜受到的衬底应力较小,结晶性最好。且ZnO薄膜垂直方向的晶格排列要比面内的晶格排列更有序。

湿度环境下钙钛矿太阳能电池薄膜微结构演化的同步辐射原位实时研究

环境湿度对有机-无机杂化钙钛矿薄膜太阳能电池稳定性有着相当重要的影响,在湿度环境下原位实时观测钙钛矿薄膜微结构的演化有助于揭示湿度导致的器件性能衰减的微观机理.本文基于上海光源X射线衍射线站,建立了一套湿度可调可控的原位X射线衍射实验装置用以实时观测湿度环境下钙钛矿薄膜的微结构演化.在相对湿度为60%±2%的环境中,采用原位同步辐射掠入射X射线衍射发现在钙钛矿薄膜暴露在湿度环境的最初阶段,其(110)衍射峰附近逐渐出现了中间相结构,应该是来源于部分钙钛矿晶体结构的逐渐分解所形成的钙钛矿多相结构;同时,紫外可见吸收光谱实验表明,经环境湿度处理后的薄膜吸收有所降低,尤其是在约770 nm处吸收台阶发生蓝移,在一定程度上反映出钙钛矿晶体结构的减少或结晶性变弱;扫描电子显微镜结果进一步显示,湿度实验后薄膜形貌的均匀性明显变差,覆盖率降低、孔洞变大及晶界变明显;采用环境湿度实验前后的钙钛矿薄膜上制备的太阳能电池J-V性能测试结果显示,器件的填充因子和光电转换效率均由于环境湿度处理降低了30%以上.因此,同步辐射原位实验观测清晰地揭示了器件性能与钙钛矿薄膜形貌以及微结构演化的密切关联,为理解有机-无机杂化的钙钛矿薄膜的降解微观机理提供了实验依据和指导.

ZnO/Si(111)界面结构的同步辐射掠入射X射线衍射研究

在不同的衬底温度下,用脉冲激光沉积(PLD)方法制备了c轴高度取向的ZnO薄膜.采用同步辐射掠入射X射线衍射(GID)技术研究了ZnO薄膜与Si(111)衬底的界面结构.GID结果表明:不管衬底温度是500℃还是300℃,在无氧气氛下用PLD方法制备的ZnO外延膜均处于压应力状态,且随着X射线探测深度的增加,应力增大.结合常规X射线衍射技术,计算了薄膜内的双轴应力;给出了样品的泊松比和c/a值,得出两样品均接近理想的六方密堆积结构,偏离标准的ZnO值.综合各方面实验结果,说明衬底温度控制在500℃时生长的ZnO薄膜具有较好的晶体质量.

NSRL衍射和散射站的性能及在材料科学中的典型应用

介绍了国家同步辐射实验室二期工程X射线衍射和散射光束线实验站的建设与主要设备.利用设备采用X射线反射法,在不破坏样品的情况下得到了Si/C多层膜的结构信息;通过对标准Si粉末样品的FWHM测试表明该站可进行粉末全谱扫描;利用X射线掠入射衍射技术分析了ZnO薄膜的生长条件与结构的关系;采用X射线散斑方法直接观测了弛豫铁电体内部的纳米空间尺度的电极化团簇的空间时间构造.