氧离子束辅助激光淀积生长ZnO/Si的XPS探究

为了探究ZnO/Si内部化学成分及有关信息,用氧离子束辅助(O+-assisted)脉冲激光淀积(PLD)法在不同实验条件下生长成ZnO/Si(111)样品.利用X射线光电子能谱(XPS)对长成的ZnO/Si异质结构进行了异位测试.通过对O1s峰及其肩状结构进行拟合、分析,得到了原子数密度比n(O)∶n(Zn),进而探究了原子数密度比与生长质量的关系.结果表明,用氧离子束辅助PLD法,可在较低的衬底温度190℃和适当O+束流条件下,生长出正化学比接近于1,且c轴单一取向最佳的ZnO/Si薄膜.用氧离子束辅助PLD淀积法生长ZnO薄膜,可以改善缺氧状况,能提供一个富氧环境.     

氧离子束辅助激光淀积生长ZnO/Si薄膜深度剖析

对于在Si(111)上用氧离子束辅助(O -assisted)脉冲激光淀积(PLD)生长的ZnO薄膜,用X射线光电子能谱(XPS)深度剖析方法对长成的样品进行了异位测试,分析了导致各峰峰位能移的因素;通过异位与原位XPS谱图的比较,指出O -assisted PLD法生成的ZnO薄膜中存在孔隙;指出生长出的ZnO薄膜中含si成分的厚度不超过18 nm;同时探讨了在长成的ZnO/Si上继续生长GaN薄膜的可行性.     

PLD生长的ZnO薄膜的微结构及其发光特性研究

在不同的衬底温度下，通过脉冲激光淀积（PLD）方法在Si衬底上生长出c轴高度取向的ZnO薄膜。ZnO薄膜的结构分别通过X射线衍射（XRD）和广延X射线吸收精细结构（EXAFS）来表征，而表面成份和化学态则通过X射线光电子能谱来研究。利用光致发光（PL）来研究样品的发光特性。XRD结果和EXAFS结果都表明了500℃时生长的ZnO薄膜的结晶性比300℃时生长的要好。EXAFS结果和XPS结果显示，300℃时生长的ZnO薄膜处于富氧状态，而500℃时生长的则处于缺氧状态。结合XRD谱、EXAFS谱、XPS谱和PL谱的结果可以看到：随着ZnO薄膜的结晶性变好，它的紫外发光增强；另一方面，随着ZnO薄膜中O的含量减少，绿光发射变强。我们的结果表明绿光发射与ZnO中氧空位（V0）有关。     

Zr/Nb薄膜材料的制备及界面结构研究

通过直流磁控溅射法在单晶Si(100)基底上制备了Zr/Nb/Si薄膜材料。X射线衍射(XRD)研究表明Zr薄膜以多晶形式存在,而Nb薄膜则形成了(110)晶面择优生长。薄膜中Zr和Nb晶粒大小分别为14,6 nm。扫描电镜研究表明形成的薄膜表面平整光滑,没有微裂纹存在。扫描俄歇电子能谱及X射线光电子能谱的研究表明,Zr/Nb/Si薄膜样品具有清晰的界面结构。在薄膜表面形成了致密的氧化层物种,而在膜层内部少量氧则以吸附态形式存在。     

新型工艺制备ZnO薄膜的结构与形貌研究

采用了一种新型工艺制备ZnO薄膜。新工艺采用二步法,首先在N型Si(100)衬底上用离子束沉积溅射一层金属Zn膜,然后通过热氧化金属Zn膜制备ZnO薄膜。通过X射线衍射、原子力显微镜对不同制备工艺下的ZnO薄膜进行结构与形貌的分析比较。研究表明,Zn膜的离子束溅射沉积时间、热氧化时间和辅助枪的离子束对热氧化后的ZnO薄膜再轰击处理对ZnO薄膜的结构与形貌都会产生影响。     

低温水热法生长ZnO纳米棒阵列的电子结构及光学特性(英文)

使用低温水热法在Si衬底上生长ZnO纳米棒阵列.通过X射线衍射和扫描电子显微镜对ZnO纳米棒的结晶性和形貌进行观测.结果表明,六棱柱形ZnO纳米棒沿c轴方向的阵列性良好,且均匀致密的生长在衬底上.室温光致发光谱表明应用低温水热法可以得到光学性质良好的ZnO纳米棒阵列.使用同步辐射对ZnO纳米棒阵列的氧K带边进行X射线吸收近带边谱测量,研究了不同半径ZnO纳米棒阵列的局部电子结构及其半径对电子结构的影响.另外,对ZnO纳米棒及ZnO薄膜的局部电子结构进行了对比研究.     

ZnO多角晶须的制备及表征

采用脉冲激光沉积技术先在Si(111)衬底上制备Zn薄膜,然后在石英炉中热蒸发金属锌粉的方法制备了ZnO晶须。分别用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)和光致发光(PL)谱对样品的结构、成分、形貌和光学特性进行了表征。结果表明,采用此方法得到的ZnO多角晶须为六方纤锌矿结构,其根部直径大约在100～500nm之间,尖部直径大约为40nm左右,长约几个微米。Zn薄膜能够有效地促使晶核的形成与长大从而促进了ZnO晶须的形成。最后,简单讨论了ZnO纳米晶须的生长机制。     

RF溅射稀土（La，Nd）掺杂ZnO薄膜的结构

通过射频磁控溅射技术在Si(111)衬底上制备了未掺杂和镧、钕掺杂ZnO薄膜.XRD分析表明,ZnO薄膜具有c轴择优生长,镧、钕掺杂ZnO薄膜为自由生长的纳米多晶薄膜.用AFM观测薄膜的表面形貌,镧、钕掺杂ZnO薄膜表面形貌粗糙.     

3C-SiC/Si(111)的掠入射X射线衍射研究

在衬底温度为1000℃条件下, 利用固源分子束外延(SSMBE)技术在Si衬底上生长3C-SiC单晶薄膜. RHEED结果显示在Si(111)上所生长的SiC薄膜为3C-SiC, 并与衬底的取向基本一致. 采用同步辐射掠入射X射线衍射(GID)技术并结合常规X射线衍射(XRD)研究了SiC薄膜内的应变和晶体质量. 常规衍射的联动扫描曲线得到薄膜处于双轴张应变状态. 3C-SiC薄膜和Si衬底的晶格失配和热膨胀系数失配是导致双轴张应变的原因. 根据不同角度的掠入射衍射Phi扫描的摇摆曲线结果, 发现薄膜晶体质量在远离SiC/Si界面区变好. 这是由于SiC薄膜中的缺陷随着远离界面逐渐减少的原因. GID和XRD的摇摆曲线结果表明薄膜中镶嵌块的倾斜大于扭转, 表明SiC薄膜在面内的晶格排列要比垂直方向更加有序.     

6H-SiC单晶表面ZnO薄膜的制备及其结构表征

利用脉冲激光淀积(PLD)技术在6H-SiC单晶衬底上制备了ZnO薄膜. 利用X射线衍射(XRD), 反射式高能电子衍射(RHEED)和同步辐射掠入射X射线衍射(SRGID)φ扫描等实验技术研究了ZnO薄膜的结构. 结果表明:在单晶6H-SiC衬底上制备的ZnO薄膜已经达到单晶水平, 不同入射角的SRGID结果, 显示了ZnO薄膜内部不同深度处a方向的晶格弛豫是不一致的, 从接近衬底界面处到薄膜的中间部分再到薄膜的表面处, a方向的晶格常数分别为0.3264、0.3272和0.3223nm. 通过计算得到ZnO薄膜的泊松比为0.504, ZnO薄膜与单晶6H-SiC衬底在平行于衬底表面a轴方向的实际晶格失配度为5.84%.     

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.