X射线衍射层析术图像重构的若干影响因素研究

三维X射线衍射层析术(3DXRD)是一种快速的、无损的结构表征技术,用于研究毫米尺度的多晶样品中晶粒(亚晶粒)的空间分布。基于上海光源成像线站BL13W1建立了三维X射线衍射层析术实验方法,并对图像重构中的若干影响因素进行了研究。通过椒盐噪声消除、对比度增强,有效提高了寻峰精度;利用德拜-谢勒环粗校与优值方程循环迭代细校相结合的方法,实现了衍射数据的精确校准,进一步采用并行运算,校准效率提高了4.5倍。实验结果表明,该方法可同时实现近场和远场衍射信息探测,从而获取样品中晶粒的尺寸、质心位置、晶体学取向等信息,并能够给出晶粒形变程度的定量信息。     

连续过渡型多晶物相深度分布的X射线衍射测试方法

提出了以X射线衍射测量连续过渡型多晶物相深度分布的方案.该方案在入射角大于全反射角的常规条件下,实现了严格的真实尺度下的物相定量深度分布测量.以计算谱对方法及程序的正确性进行了验证,并用实际样品对方法的可行性进行了验证. 关键词：     

Fe-Ti多层调制膜固态反应扩散的动态原位法X射线衍射研究

本文用动态原位法X射线衍射研究了Fe-Ti多层调制膜的固态反应扩散,比较准确地测量了组份调制衍射峰强度的变化,并同时观测了峰位的移动,计算出不同温度下Fe-Ti多层调制膜的扩散系数,并给出其随时间变化的曲线。根据扩散系数随时间变化率,计算出与粘滞弛豫相关的激活能Q_y=8.3±0.2kcal/mol。 关键词：     

Zn1-xCdx S合金薄膜的结构和光学性质

采用低压金属有机化学气相沉积(LP-MOCVD)技术,在普通石英衬底上制备出不同Cd组分(0．02,0．44,0．59,0．83,0．91)的Zn1-xCdxS合金薄膜材料。X射线测量表明样品为单一取向的纤锌矿结构,并且随着x的增加衍射峰位基本成线性地从ZnS衍射峰向CdS衍射峰移动。此外,在PL谱中还可以看出随着样品中Cd含量的增加,发光峰从3．66eV红移到2．43eV。根据发光峰位与Zn1-xCdxS中x的变化关系,推导出它们之间的关系近似为Eg(Zn1-xCdxS)=3．61-1．56x 0．38x^2。还探讨了不同Cd组分薄膜材料的X射线衍射峰半峰全宽以及发光峰半峰全宽的变化。     

XRD在薄膜结构分析中常见问题的研究

研究了X射线衍射(XRD)在薄膜结构分析中常见问题的解决方法,提出了取向生长薄膜的面内晶胞参数的测试及计算方法。实验表明,X射线束的扫描方向对反映的晶体结构信息产生影响。理论推导表明,在计算中选择合适强度和合适峰位的衍射峰,才能得到准确的晶胞参数。     

聚乙烯薄膜中X射线穿透深度计算方法的验证

通过银镜反应在聚乙烯薄膜一面镀银膜,用不同入射角进行掠入射X射线衍射测量,利用对应银的衍射峰出现的条件验证了X射线穿透深度计算公式在进行高分子薄膜表征中的可行性.     

Be薄膜应力的X射线掠入射侧倾法分析

由于铍薄膜极易被X射线穿透, 传统的几何模式下很难获得有效的X射线衍射应力分析结果. 本文采用掠入射侧倾法分析SiO₂基底上Be薄膜残余应力, 相比其他衍射几何方法, 提高了衍射的信噪比, 获得的薄膜应力拟合曲线线形较好. 对Be薄膜的不同晶面分析, 残余应力结果相同, 表明其力学性质各向同性; 利用不同掠入射角下X射线的穿透深度不同, 获得应力在深度方向上的分布; 由薄膜面内不同方向的残余应力相同, 确定薄膜处于等双轴应力状态. 关键词： Be薄膜 X射线衍射 应力     

拉曼面扫描无损鉴定矿物包裹体：以彩虹方柱石中的磁铁矿包裹体为例

如何利用拉曼光谱对矿物中的微小包裹体进行无损鉴定，是矿物学与宝石学研究中经常遇到的问题。彩虹方柱石是一种含有特殊包裹体的方柱石，其包裹体在反射光下呈现虹彩效应。本文利用超景深显微镜、电子探针、显微激光拉曼光谱、X射线粉晶衍射分析，特别是创新性运用拉曼光谱面扫描填图技术对彩虹方柱石中微小的磁铁矿包裹体进行了无损鉴定研究。显微特征显示，彩虹方柱石的包裹体可能和固溶体出溶有关，微小包裹体平行排列，形成了类似反射型衍射光栅的结构，导致其在反射光下出现彩虹色。根据电子探针测试结果，彩虹方柱石端元组分为Ma_68.2-69.7Me_30.3-31.8，属针柱石亚族。根据拉曼光谱测试结果，部分包裹体出现了位于661 cm-1处的弱拉曼峰。由于图谱信噪比普遍偏低且该峰并不会在所有测试位置出现，所以容易被忽略。为进一步探究该峰的来源，对包裹体部位进行拉曼面扫描，并选择630～680 cm-1范围的拉曼峰进行了相关性分析，确认了包裹体位置普遍存在位于661 cm-1处的弱拉曼峰。该拉曼峰可归属为磁铁矿的A_1g振动峰，从而确认了产生虹彩效应的针状包裹体中包含有更微小的磁铁矿包裹体。XRD测试结果表明，包裹体较多的样品存在位于2.51 Å处的磁铁矿（311）晶面衍射峰，进一步验证了拉曼光谱面扫描的结果。根据上述实验，拉曼面扫描技术或许可以成为鉴定矿物宝石中微小包裹体的有效辅助性手段。该研究创新性提出，如果矿物包裹体的拉曼信号很弱，可以将拉曼面扫描结果与包裹体的分布特征结合分析来判断该信号的有效性。同时为无损鉴定矿物中的包裹体提供了一种新的研究思路与方法。     

Fe-Ti多层调制膜固态反应扩散的动态原位法X射线衍射研究

本文用动态原位法x 射线衍射研究了Fe-Ti 多层调制膜的固态反应扩散, 比较准确地测量了组份调制衍射峰强度的变化,并同时观测了峰位的移动, 计算出不同温度下Fe-Ti 多层调制膜的扩散系数, 并给出其随时间变化的曲线. 根据扩散系数随时间变化率, 计算出与粘滞弛豫相关的激活能 Q=8.3 士0 .2 kcal/ mol. 关键词：     

金属单层膜的小角X射线衍射强度的研究

本文对金属单层膜进行研究,在多种样品中没有发现X射线衍射峰.我们在基底上预先淀积一层重金属膜,然后再淀积所需样品,发现样品有较好的衍射峰产生.我们对此进行了探讨并提出了一个可能的理论定量解释.     

The determination of dislocation density depth profiles in surface layers from broadening of X-ray diffraction profiles

A method is proposed for the determination of dislocation density depth profiles in the thin surface layers comparable to the penetration depth of X-rays, with no need to remove the surface layers by chemical or electrolytic polishing. The dislocation density depth profile is modelled mathematically and the parameters determining the profile can be evaluated from the Fourier transform of the X-ray diffracted profiles with various wavelengths of radiation.     

高质量纳米ZnO薄膜的光致发光特性研究

报道了利用低压-金属有机物化学气相沉积技术生长纳米ZnS薄膜，然后，将ZnS薄膜在氧气中于800℃温度下进行热氧化制备高质量纳米ZnO薄膜.x射线衍射结果表明，纳米ZnO薄膜具有六角纤锌矿多晶结构.室温下观察到一束强的紫外(3.26 eV) 光致发光和很弱的深能级发射.根据激子峰的半高宽度与温度的关系确定了激子-纵向光学声子（LO）的耦合强度（ГLO）.由于量子限域效应使ГLO减少较多. 关键词： 光致发光 热氧化 激子 纳米ZnO薄膜     

不同沉积参量下ZrO2薄膜的微结构和激光损伤阈值

ZrO2采用X射线衍射(XRD)技术分析了不同充氧条件和沉积温度对ZrO2溥膜组成结构的影响,并对不同工艺下制备的薄膜的表面粗糙度和激光损伤阈值进行了测量。结果发现随着氧压的升高,ZrO2溥膜将由单斜相多晶态逐渐转变为非晶态结构,而随着基片温度的增加,溥膜将由非晶态逐渐转变为单斜相多晶态。同时发现随着氧压升高晶粒尺寸减小,而随着沉积温度增加,晶粒尺寸增大。氧压增加时工艺对表面粗糙度有一定程度的改善,而沉积温度升高,工艺对表面粗糙度的改善不明显。晶粒尺寸大小变化与表面粗糙度变化存在对应关系。激光损伤测量表明,氧压条件和沉积温度对ZrO2薄膜的抗激光损伤能力有着较大影响。     

Formation of high quality gallium nitride thin films on Ga-diffused Si(1 1 1) substrate

High quality gallium nitride thin films have been successfully grown on the Ga-diffused Si(1 1 1) substrates through ammoniating Ga₂O₃ thin films deposited by r.f. magnetron sputtering. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), atomic force microscope (AFM) and photoluminescence (PL) were used to characterize the synthesized samples. The analyses reveal that the formed films are high quality polycrystalline hexagonal gallium nitride. The as-formed GaN films show a flat surface topography with RMS roughness varied from 29 to 48 Å. The strong near-band-edge-emission peak around 368 nm was observed at room temperature. This is a novel method to fabricate GaN thin films based on the direct reaction between Ga₂O₃ and NH₃ on the Ga-diffused Si(1 1 1) substrates.     

退火时间对MgB_2超导薄膜的影响

在多晶A l2O3衬底上,以B2H6作为硼源,化学气相沉积先驱B薄膜,采用Mg扩散方法,在不同退火时间条件下制备了MgB2超导薄膜。通过电阻-温度曲线测量、X射线衍射分析和扫描电子显微镜形貌观测方法,研究了退火时间对MgB2薄膜的超导特性、晶体结构、表面形貌的影响。     

Characterization and comparison of X-ray focusing optics for ultrafast X-ray diffraction experiments

We have characterized and compared the performance of different types of multi-layer optics for the focusing of femtosecond X-ray pulses. Using X-ray pulses at 8 keV, from a laser-driven plasma source we have measured the spatial distribution of the diffracted X-rays directly after and in the focal plane of the various X-ray optical devices. For a Montel optic with 7.3× magnification we obtained the largest number of focused X-ray photons per unit angle. The performance of this optic in the X-ray diffraction experiment on a thin germanium film is demonstrated.     

退火对溶胶-凝胶法制备的ZnO薄膜结构和光致发光的影响

采用溶胶-凝胶法在n-Si(100)衬底上制备ZnO薄膜并从三个方面对其研究。X射线衍射结果表明,在含氧气氛中退火的ZnO薄膜为多晶六角纤锌矿结构,有明显的c轴择优结晶取向;退火时间的长短和温度的高低对结晶取向性和粒径均有较大影响,通过进一步的研究发现最佳处理温度在500℃左右。用扫描电子显微镜观察样品的表面和侧面形貌,晶体的生长比较均匀,粒径平均在70~160nm范围内,与XRD测量结果相一致。室温下ZnO胶体的光致发光谱表明,随着胶体老化时间的延长,胶体的紫外峰位发生了蓝移。室温下ZnO薄膜的光致发光谱表明,紫外部分的发光峰位在365,390nm,发光强度较强;在可见光区的发光强度相对较弱,但是还没有被氧完全抑制掉。     

CHARACTERIZATION OF POLYCRYSTALLINE GRADIENT THIN FILM BY X-RAY DIFFRACTION METHOD

A direct method is proposed to quantitatively characterize the structural depth profiles emerged in the polycrystalline thin films based on the information obtained by X-ray diffraction (XRD) with various incident angles and treated by a numerical procedure known as the constrained linear inversion. It should be noted that the proposed method was neither sensitive to the random noise appearing in experiment nor to the error originated from the measured thickness of the specimen. To testify the validity of the method, XRD measurements were carried out on a specially designed Pd/Ag bilayer sample, which was annealed at 490℃ for 20 min, and the depth profiles were accordingly calculated through resolving the obtained XRD patterns. The elemental concentration depth profile of the Pd/Ag bilayer sample was in turn calculated from the resolved patterns, which was in good agreement with those obtained by Auger electron analysis on the annealed sample.     

Fabrication and testing of a newly designed slit system for depth‐resolved X‐ray diffraction measurements

A new system of slits called `spiderweb slits' have been developed for depth‐resolved powder or polycrystalline X‐ray diffraction measurements. The slits act on diffracted X‐rays to select a particular gauge volume of sample, while absorbing diffracted X‐rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range of diffraction angles, and work for X‐ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray‐tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X‐ray Powder Diffraction beamline at the National Synchrotron Light Source II.     

Spatial structure of a focused X‐ray beam diffracted from crystals

The spatial structure of a beam focused by a planar refractive lens and Bragg diffracted from perfect silicon crystals was experimentally studied at the focal plane using a knife‐edge scan and a high‐resolution CCD camera. The use of refractive lenses allowed for a detailed comparison with theory. It was shown that diffraction leads to broadening of the focused beam owing to the extinction effect and, for a sufficiently thin crystal, to the appearance of a second peak owing to reflection from the back surface. It was found that the spatial structure of the diffracted beam depends on whether the crystal diffracts strongly (dynamically) or weakly (kinematically). The results help to understand the physical origin of the diffracted intensity recorded in a typical microbeam diffraction experiment.