碲铟汞晶体制备及其热稳定性研究

以高纯Hg、In、Te单质为原料,通过元素直接化合反应合成了碲铟汞(MIT)多晶料,并利用合成的高纯多晶料,在特殊设计的坩埚中,采用垂直Bridgman法通过自发成核方式成功地生长了尺寸为Φ15mm×175mm的MIT单晶体.利用X射线粉末衍射技术对MIT晶体结构及物相进行的分析表明,所获得的晶体是单相的MIT晶体,为缺陷闪锌矿结构,空间群为F43m.采用高分辨X射线衍射仪测量了所生长MIT晶体的摇摆曲线,结果表明所得晶体完整性较好,为高质量的单晶体.对所生长的MIT晶体进行了热分析,发现在MIT晶体中有Hg溢出现象.     

水平温梯冷凝法生长ZnGeP_2单晶

采用高纯(6mol/L)Ge、Zn、P单质为原料,按化学计量比并富P 0.2%配料,通过双温区法合成ZnGeP2多晶粉料,再用水平温梯冷凝法(HGF)生长出尺寸达10mm×20mm×80mm的单晶棒。对单晶进行了X射线衍射、红外透过率、热导率等测试,测试结果表明;单晶完整性好,红外透过率较高;5mm厚晶片(未退火、镀膜)在2～8μm范围内平均透过率可达54%以上;在室温附近(297.34K)热导率为35.89W/(m.K)。     

Pb2MoO5单晶的坩埚下降法生长

本文报道了Pb2MoO5单晶的坩埚下降法生长工艺.按照精确的化学计量比进行配料,应用高温固相反应合成Pb2MoO5多晶料;在晶体生长过程中,控制炉体温度于1050～1070℃,调节固液界面温度梯度为30～40℃/cm,按照0.6～1.0 mm/h的下降速率,通过改进的坩埚下降法生长出透明完整的Pb2MoO5单晶;应用X射线衍射、差热分析、透射光谱等方法进行了单晶基本性质的表征.X射线衍射分析证实该晶体为单斜晶系,DTA/TG曲线表明该晶体在958℃一致熔融,高于此温度熔体组分出现严重挥发,该晶体在可见光波长范围具有良好的光学透过性,其吸收边位于370 nm波长附近.     

Al2-xYxW3O12的合成与热膨胀特性的研究

近零及负热膨胀材料有诸多的潜在应用领域,而具有负热膨胀效应的A2M3O12系列材料在较宽的温度范围,易于通过组份变化调整其热膨胀系数.本文首次使用共沉淀法合成了Al2-xYxw3O12(x=0～2)系列粉体材料.经X射线衍射分析证明Al2W3O12和Y2W3O12能完全固溶形成二元固溶体,采用PowderX软件对Al2-xYxW3O12的晶胞参数进行计算,结果表明室温下随着稀土钇(Y)含量的增加,晶体的晶胞参数与晶胞体积逐渐增加.高温X射线衍射结果表明,随着稀土钇(Y)含量的增加,Al2-xYxW3O12的本征热膨胀系数逐渐由正到负变化.热机械分析(TMA)压缩法测定其宏观热膨胀系数,发现通过调整材料的组成,可以将其热膨胀系数控制为一定的正值、负值或零.但是由于其结构的各向异性,多晶陶瓷内部存在的微裂纹使热膨胀曲线出现较大的滞后环.     

正交结构LiGaS2的合成及表征

为了获得高纯单相LiGaS2多晶原料,采用LiGa与S化合法合成LiGaS2,并与传统的单质直接合成法相对比.利用垂直长石英管作为反应器,采用X射线衍射和Raman光谱对其结构进行表征,同时利用差热–热重分析和紫外光谱对其热性能和光学性能进行研究.研究表明:采用LiGa与S化合法可以获得单相、均一的LiGaS2多晶材料;LiGaS2中的Li–S键平均力常数为fLi-S=16.0 N/m,Ga–S键平均力常数为fGa-S=39.6 N/m;LiGaS2多晶料的熔点为1 020℃,温度低于1 100℃,样品很稳定,没有分解现象;白色样品、黄色样品和灰色样品的紫外吸收边分别为323,435和496 nm.     

双元共掺杂Bi1-xLax(Fe0.95Mn0.05)O3多铁性材料的磁性研究

采用溶胶-凝胶法制备了Bi1-xLax(Fe0.95Mn0.05)O3(x=0,0.10,0.15)多晶样品。X射线衍射实验表明La、Mn离子共掺杂没有改变样品的四方晶格结构。X射线能量色散分析显示样品的化学组分几乎不变。Mn离子掺杂或者是(La、Mn)离子共掺杂,导致铁酸铋材料的磁性增强。X射线吸收精细结构实验表明Mn3+的局域结构的改变是样品磁性增强的原因。     

富锂LiNbO_3∶Fe∶Mg晶体中的X射线折变

从双折率变化测量、吸收光谱和 ESR 谱三个方面研究了富锂 LiNbO_3∶Fe∶Mg、LiNbO_3∶Fe 和纯的LiNbO_3晶体中 X 射线致折射率变化。结果表明 X 射线致折射率变化现象不同于通常的光折变。伴随着 X射线折变的产生,出现了光色效应。X 射线折变后,晶体中 Fe~(2 )含量增加。X 射线折变可能是过量的 Fe~(2 )产生的。     

溅射非晶钴硅薄膜的晶化过程及其分析

利用射频磁控溅射方法制备了具有CoSi2成分的非晶薄膜，对非晶薄膜的晶化过程进行了原位X射线分析。结果显示，溅射态薄膜为非晶态，而自由能一成分曲线说明非晶态合金有较低自由能。在非晶晶化过程中初生相为CoSi相，其形成由有效形成热（EHF）因素和结构因素决定。随加热温度升高，非晶薄膜晶化最终得到晶体CoSi2薄膜。     

X射线衍射在材料结构表征中的应用

扼要介绍了单晶、多晶、表面及薄膜衍射等各种技术在三个层次（多晶聚集态结构、分子与晶体结构和晶体内微结构）的材料结构表征中的应用。还从衍射仪种类、主要组成部件和重要附件三个方面介绍了X射线衍射试验装置。     

PLZT纳米陶瓷粉末的合成及表征

通过溶胶喷雾热解法合成PLZT(10/65/35)陶瓷粉末,通过热分析仪、X射线粉末衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)对样品进行分析。研究表明,前驱体经过900~1 000℃的烧结能得到单一的PLZT晶体;当烧结温度超过1 100℃,PLZT陶瓷发生相变,分解为ZrO_2和Pb_(0.64)La_(0.206)Ti_(0.949)O_(2.846);扫描电镜(SEM)分析表明PLZT粉末样品颗粒饱满、粒径均匀,为纳米晶体;透射电镜(TEM)分析结果表明PLZT晶粒呈现球状,晶粒为多晶结构。     

Transformation of X-ray Server from a set of WWW-accessed programs into WWW-based library for remote calls from X-ray data analysis software

X-ray Server [x-server.gmca.aps.anl.gov] is a public project providing a collection of online software tools for modeling data in the fields of surface X-ray scattering and grazing-incidence X-ray diffraction from thin solid films and multilayers with account for the effects of crystal lattice strains, magnetization and interface roughness. This paper reports on recent developments that are addressing numerous requests to expand the Server access beyond plain web browser sessions and facilitate batch processing, remote fitting and integration of Server programs into users’ data analysis software.     

Implications of stimulated resonant X-ray scattering for spectroscopy,imaging, and diffraction in the regime from soft to hard X-rays

The ultrahigh peak brilliance available at X-ray free-electron lasers opens the possibility to transfer nonlinear spectroscopic techniques from the optical and infrared into the X-ray regime. Here, we present a conceptual treatment of nonlinear X-ray processes with an emphasis on stimulated resonant X-ray scattering as well as a quantitative estimate for the scaling of stimulated X-ray scattering cross sections. These considerations provide the order of magnitude for the required X-ray intensities to experimentally observe stimulated resonant X-ray scattering for photon energies ranging from the extreme ultraviolet to the soft and hard X-ray regimes. At the same time, the regime where stimulated processes can safely be ignored is identified. With this basis, we discuss prospects and implications for spectroscopy, scattering, and imaging experiments at X-ray free-electron lasers.     

The X-ray Quantum Calorimeter Sounding Rocket Experiment: Improvements for the Next Flight

We have developed a new calorimeter array to increase our collecting area by a factor of four. The 6×6 pixel device has a total area of 144 mm², making it one of the largest X-ray microcalorimeter arrays yet constructed. A relatively thin high-z absorber consisting of a 0.7 μm HgTe layer supported on 15 μm high-purity silicon provides good efficiency up to photon energies of 1.5 keV. The heat capacity of this composite is low enough to obtain an energy resolution of ∼6 eV FWHM on the 2 mm×2 mm pixels when operated at a base temperature of 50 mK. The infrared blocking filters have also been improved. Room temperature radiation must be attenuated by about 9 orders of magnitude between 2 μm and 2 cm to avoid having photon shot noise dominate the detectornoise. Accomplishing this while maintaining a high transmission for very soft X-rays that can penetrate only a few μg cm⁻² is a problem common to all soft X-ray calorimeters that observe external targets. We are constructing monolithic silicon two-layer support meshes with a 350 μm pitch front layer on a 5 mm pitch backing layer. These are 98% open and have >95% effective transmission over a 60° field of view, while providing robust support for 38 mm diameter filters consisting of 20 nm of aluminum on 50 nm of polyimide. Five of these filters in series provide the necessary infrared attenuation. Integral deicing heaters are ion implanted in the fine mesh to remove contamination when necessary.      

Exploring nanoscale magnetism in advanced materials with polarized X-rays

Nanoscale magnetism is of paramount scientific interest and high technological relevance. To control magnetization on a nanoscale, both external magnetic fields and spin polarized currents, which generate a spin torque onto the local spin configuration, are being used. Novel ideas of manipulating the spins by electric fields or photons are emerging and benefit from advances in nano-preparation techniques of complex magnetic materials, such as multiferroics, ferromagnetic semiconductors, nanostructures, etc.Advanced analytical tools are needed for their characterization. Polarized soft X-rays using X-ray dichroism effects are used in a variety of spectroscopic and microscopic techniques capable of quantifying in an element, valence and site-sensitive way basic properties of ferro(i)- and antiferromagnetic systems, such as spin and orbital moments, nanoscale spin configurations and spin dynamics with sub-ns time resolution. Future X-ray sources, such as free electron lasers will provide an enormous increase in peak brilliance and open the fs time window to studies of magnetic materials. Thus fundamental magnetic time scales with nanometer spatial resolution can be addressed.This review provides an overview and future opportunities of analytical tools using polarized X-rays by selected examples of current research with advanced magnetic materials.     

Geometrical properties of the X-ray diffraction applied to Laue lenses

An analytical study of the geometrical properties of the X-ray diffraction applied to the case of Laue lenses is reported in this paper. The results of this investigation are analytical equations that describe the point in which a photon is diffracted as a function of the crystal position and of the X-ray source angular coordinates. In addition, the contributions to the lens Point Spread Function of each crystal is described, helping in understanding the optical properties of a Laue lens. The results obtained can be inserted in simulation and image deconvolution softwares for speeding up the calculations.     

Various Optimizations of TES Arrays for X-Ray Astrophysics

We are developing arrays of superconducting transition-edge sensors (TES) for imaging X-ray spectroscopy telescopes such as the XMS on Constellation-X. While our primary focus has been on arrays that meet the XMS requirements (of which, foremost, are an energy resolution of 2.5 eV at 6 keV and a band pass from ∼0.3 keV to 12 keV), we are also beginning to investigate other optimizations that might be used to extend the XMS capabilities. In one of these optimizations, improved resolution below 1 keV is achieved by reducing the heat capacity. These low-energy pixels can be added to an array with broadband response either as a separate array or interspersed, depending on other factors that include telescope design and science requirements. To explore optimizations for higher count rates, we are also optimizing the design and operating temperature of pixels that are coupled to a solid substrate. We present analysis of the preliminary performance of such variations. This research was supported in part by appointments (A.-D. Brown and S.J. Smith) to the NASA Postdoctoral Program at Goddard Space Flight Center, administered by Oak Ridge Associated Universities through a contract with NASA.     

Comparison of back-foil SXRF and EPMA for the elemental characterization of thin coatings

Back-foil scanning X-ray microfluorescence (SXRF), developed in a scanning electron microscope and applied for the analysis of very thin coatings is compared with electron probe X-ray microanalysis (EPMA). Both experimental results and Monte-Carlo calculations are used in this respect. The signal to background ratio as a function of the primary electron beam energy and angle of incidence, and for different film thicknesses is obtained for both techniques and a comparative study of sensitivity is made. Back-foil SXRF used in optimized experimental conditions, is found to be more sensitive than EPMA, especially in the case of very thin overlayers. The resolving power of back-foil SXRF is also calculated for the anode used by Monte-Carlo simulations.     

Three-dimensional structured on-chip stacked zone plates for nanoscale X-ray imaging with high efficiency

Fresnel zone plates are the key optical elements for nanoscale focusing of X-ray beams with high spatial resolution. Conventional zone plates manufactured by planar nanotechnology processes are limited by the achievable aspect ratios of their zone structures. Additionally, ultra-high resolution X-ray optics with high efficiency requires three-dimensional （3-D） shaped tilted zones. The combination of high spatial resolution and high diffraction efficiency is a fundamental problem in X-ray optics. Based on electrodynamical simulations, we find that the optimized zone plate profile for volume diffraction is given by zone structures with radially increasing tilt angles and decreasing zone heights. On-chip stacking permits the realization of such advanced 3-D profiles without significant loss of the maximum theoretical efficiency. We developed triple layer on-chip stacked zone plates with an overlay accuracy of sub-2 nm which fulfills the nanofabrication requirements. Efficiency measurements of on-chip stacked zone plates show significantly increased values compared to conventional zone plates.     

Analysis of powder X-ray diffraction resolution using collimating and focusing polycapillary optics

Focusing X-ray optics can be used to increase the intensity onto small samples, greatly reducing data collection time. Typically, the beam convergence is restricted to avoid loss of resolution, since the focused beams broaden the resulting powder diffraction rings. However, with smooth Gaussian peaks, the resolution defined by the uncertainty in peak location can be much less than the peak width. Polycapillary X-ray optics were used to collimate and focus X-rays onto standard inorganic powder diffraction samples. Comparisons were made of system resolution and diffracted beam intensity with and without focusing and collimating optics using a standard small spot rotating anode system in point source geometry. The area detector and optics also allowed for the use of a low power 60 W source, without increasing either the collection time or the peak center error compared to the rotating anode no optic case. Resolution and intensity were in good agreement with those obtained from a simple geometrical model developed for the optics, which allows for system design and optimization for the desired sample characteristics. Foils and powders were used to model thin film samples while allowing both reflection and transmission measurements to more effectively verify theoretical modeling of beam parameters.     

Neutron and X-ray reflectivity analysis of ceramic-metal materials

Neutron and X-ray reflectivity measurements of a thin film of cermet (ceramic-metal) made by co-sputtering Pt and Al₂O₃ on the surface of a flat piece of float glass are presented. From the analysis of the specular and off-specular measurements, the morphology of the Pt clusters which are embedded in the Al₂O₃ matrix is determined by adjusting a model to the observed data. It is found that the structure of such films presents a certain degree of order in the direction normal to the surface of the films but no correlation (or with a very short correlation length not measurable by this technique) in the plane of the film.