静压触煤法制备的人造金刚石中的晶体缺陷

本文首次采用透射电子显微术系统地研究了由FeNi触媒制备的金刚石单晶的微观结构,分析了人造金刚石中存在的晶体缺陷,探讨了这些晶体缺陷形成的原因,研究发现金刚石中存在层错,棱柱位错,位错列和位错网络等晶体缺陷,研究结果表明,金刚石中的晶体缺陷与金刚石的高温高压合成过程密不可分,主要起源于金刚石中大量过饱和的空位和观杂质所引起的内应力。     

Nd:LuVO4晶体缺陷的研究

采用提拉法生长的Nd:LuVO4晶体是一种适合二极管泵浦的新型激光晶体,运用化学腐蚀结合光学显微术和同步辐射白光X射线形貌术对Nd:LuVO4晶体缺陷进行观察,结果表明:晶体的主要缺陷为位错和小角晶界.利用高分辨X射线衍射仪进一步验证了这一结果.并初步讨论了缺陷形成的原因.     

DKDP晶体的柱面形貌与缺陷分析

采用原子力显微镜观测全方位生长的DKDP晶体的{100}面形貌,发现有螺旋位错,由此推断DKDP晶体{100}面以螺旋位错机制生长;利用同步辐射X射线白光形貌术观测了DKDP晶体缺陷,探讨了不同生长条件及生长阶段对晶体完整性的影响.     

Cr:KTiOPO4晶体缺陷的研究

首次报道了利用光学显微法和同步辐射白光X射线形貌术对Cr:KTP晶体缺陷的研究结果.光学显微法采用热磷酸作为腐蚀剂,用Opton大型显微镜反射法观察,观测到(100)面和(021)面的位错蚀坑以及(021)面的小角度晶界.用同步辐射白光X射线形貌术作出(001)面、(010)面和(100)面形貌图,从图中可明显观察到生长层、扇形界及位错线.由此得出,Cr:KTP晶体的主要缺陷是位错、生长扇形界、生长层等.     

KTiOAsO4晶体的铁电畴与位错的多种实验方法研究

利用原子力显微镜,同步辐射X射线形貌术和化学腐蚀光学显微等方法深入研究了KTiOAsO4晶体缺陷中的铁电畴和位错.首次用原子力显微镜给出了用两种腐蚀剂腐蚀过的KTA晶体表面的铁电畴和位错蚀坑的照片及定量信息,如发现铁电畴的明区要高于暗区,且两者的粗糙度明显不同.这为研究各种晶体的生长缺陷开辟了一条新的途径.     

高温相偏硼酸钡(α-BaB2O4)晶体的缺陷行为分析

运用同步辐射X射线白光形貌研究了α-BaB2O4晶体内部的完整性,并分析了α-BaB2O4晶体的缺陷行为及缺陷形成原因.在(001)面发现生长扇界和亚晶界,而在(100)面和(120)面分别观察到了位错、位错簇以及针状包裹体.使用双晶衍射实验发现在(001)面有生长条纹,这些生长条纹呈环形,该条纹与熔体中温度波动而导致的生长速率波动有关.运用白光形貌拍摄到高清晰的劳埃斑,表明晶体为三方结构.     

人造含硼金刚石单晶表面形貌与生长机制研究

本文借助Olympus光学显微镜、扫描电子显微镜(SEM)和原子力显微镜(AFM)对高温高压合成的含硼金刚石单晶表面形貌进行了分析.研究发现,含硼金刚石表面存在蚀坑、球形颗粒集团、平行台阶、花瓣状生长丘和三角形螺旋台阶等多种表面形貌.这些形貌与晶体内部的缺陷有关,硼原子的进入使金刚石晶体生长速度增加,位错增多,进而导致不同表面形貌的形成,螺旋位错生长是含硼金刚石的主要生长方式.     

YVO4晶体缺陷分析

运用同步辐射白光X射线形貌术分析了YVO4的结构和缺陷行为,也观测了YVO4晶体(001)、(100)面的缺陷.发现在(001)面出现应力生长区、沿[100]方向的位错线以及晶体中镶嵌结构.运用白光形貌术拍摄到的劳埃斑,证明晶体为四方晶系.确定了小角晶界是引起多晶的主要原因.采用电子探针仪分析了散射颗粒形成是由杂质铁和铝的引入造成.     

非线性光学晶体BaAlBO3F2的生长与缺陷研究

采用B2O3-LiF-NaF助熔剂体系、中部籽晶法生长出BaAlBO3F2(BABF)晶体,对该晶体的弱吸收性能进行了表征.利用同步辐射白光X射线形貌术和化学腐蚀法研究了BABF晶体的缺陷,观察到BABF晶体中的主要缺陷是生长条纹和位错,并根据形貌和结构特点对生长条纹产生的原因进行了分析讨论,提出了一些减少缺陷和提高晶体质量的措施和方法.     

γ-LiAlO2晶体的生长缺陷研究

γ-LiAlO2晶体是一种非常有前途的GaN衬底材料,本文利用化学腐蚀光学显微术和同步辐射X射线形貌术研究了LiAlO2晶体的缺陷.结果表明,提拉法生长的γ-LiAlO2晶体中的缺陷主要为位错、包裹物和亚晶界.并发现在其(100)晶片上的腐蚀形貌两面有较大差异.     

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likely due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.     

Optical microscopic, synchrotron X-ray topographic and reticulographic study of homoepitaxial CVD diamond

Surface topography and crystal-lattice perfection of homoepitaxial layers deposited by microwave plasma CVD on (0 0 1) and near-(0 0 1) facets polished on HPHT synthetic diamond are described. Optical micrographic techniques included birefringence, Nomarski and 2-beam interference. The synchrotron X-ray experiments comprised Laue topography plus a recently developed sensitive misorientation-measuring technique, reticulography. Two special circumstances enhanced information yield from the experiments. First, the substrate crystal was unusually strain-free and had a very low dislocation content. Second, epilayer growth had taken place in two stages, depositing thicknesses of 10 μm and 30–34 μm, respectively. This double deposition complicated the observations, but added features of scientific and practical interest. Epilayer cracking finally present had occurred almost entirely before the second growth stage. With assistance from quantitative data provided by reticulography, the X-ray diffraction properties of the substrate and epilayers are analysed. Lattice misorientations on the untreated lower surface of the substrate were only 1 arcsec except close to growth-sector boundaries and dislocation outcrops. The final epilayer growth surface above areas where cracking in the first epilayer was absent or sparse exhibited near-perfect-crystal diffraction behaviour.     

Defects in natural diamonds: Recent observations by new methods

The observations presented concern both grown-in defects and those which develop after growth. They will deal principally with impurity platelets precipitated on {100} planes and with dislocations. The former defects are a notable feature in the most common variety of natural diamond (Type Ia.) The experimental techniques used are of the direct-imaging, topographic type and include ultraviolet absorption topography, X-ray topography, cathodoluminescence topography (both with visible and near infrared wavelengths) and transmission electron microscopy at 100 kV, 120 kV and 1 MeV. Spectrography and colour photography are informative in cathodoluminescence studies. The cathodolumisnecent images of individual dislocation lines can be photographed, whether the dislocations be grown-in or arise from plastic deformation post growth, provided that they lie in matrices sufficiently free from point defects acting as strong electron-hole recombination centres. In practice this requirement implies a low concentration of nitrogen impurity much of which is distributed in “small clusters” which give rise to the bright blue cathodoluminescent emission characteristic of Type Ia diamonds. The luminescence from individual dislocation lines may be either a violet-coloured emission, or an emission which is dominantly a system (known as “H3”) having a zero-phonon line at 2.46 eV and stretching from green to orange in the visible spectrum. The violet dislocation emission is strongly polarised with E vector parallel to the dislocation line. New observations on platelets have been mainly concerned with those attaining diameters of 1 μm or more which can be observed individually by X-ray topography and cathodoluminescence topography. However, evidence from electron and X-ray diffraction contrast indicates that these “giant platelets” produce the same matrix lattice displacements as the more familiar submicrometre-sized platelets in Type Ia diamond and may be presumed to have essentially the same structure and composition. Near infrared cathodoluminescence has been recorded from individual large platelets and it has been discovered that this emission is highly polarised with the E vector in the platelet plane. Available evidence on the structure and properties of the platelets weighs against a currently mooted hypothesis that they are composed of interstitial carbon, and does not conflict with an older idea, that they are composed of nitrogen impurity.     

直流喷射电弧等离子体制备金刚石单晶的研究

通过利用光发射谱技术,探测了大功率直流喷射电弧等离子体增强化学气相沉积方法中沉积区域的气相激元分布,进而优选了金刚石生长的位置.在沉积过程中,不断使衬底做背向等离子体的运动,实现了大颗粒金刚石的连续生长,颗粒尺寸达到约1 mm3.采用劳厄背反射X射线衍射测试技术和拉曼谱技术,对所制备的样品进行了测试,结果表明:所制备的颗粒为金刚石单晶.对于大尺寸衬底,研究了背向运动速度对沉积晶体的形貌和质量的影响,发现了ATG型不稳定形貌.     

碲锌镉晶体晶格畸变的测定与分析

在高分辨X射线衍射仪上,利用不对称布拉格衍射STD技术与单晶摇摆曲线技术相结合的方法,对碲锌镉单晶材料的晶格畸变进行了分析测定.此方法实现了一次装样,多角度、多次测定晶体的摇摆曲线,从而利用多组实验数据完成多元线性回归方程组的求解,避开了一般应变测定方法中难以确定无应力状态下衍射角的问题.所测定的生长态碲锌镉晶片晶格畸变量为10-3～10-2数量级,该畸变量是碲锌镉晶片存在成份偏析、位错和空位等缺陷以及晶片受到的应力综合作用的结果.     

Study of X-ray diffraction from a surface acoustic wave in the grazing geometry with allowance for the curvature of the unperturbed crystal surface

Fresnel X-ray diffraction from a concave crystal surface in the presence of a surface acoustic wave (SAW) has been considered for grazing angles of incidence in noncoplanar symmetric Laue geometry. It is shown that the main peak and diffraction satellites are focused at different distances from a crystal. The effect of deviation from the Bragg angle, the spectral line width, and the SAW amplitude on the X-ray diffraction pattern has been analyzed. It is established that the contrast of an X-ray diffraction pattern of an SAW in Bragg-Laue grazing geometry is related to the character of irregularities of the crystal surface, and the pattern details depend on the measurement mode. The sensitivity of the method is about a nanometer. The focal image of the SAW serves as a scale landmark for determining the crystal surface characteristics.     

The application of synchrotron X-ray techniques to problems in crystal science and engineering

The basic physical principles synchrotron radiation generation and related experimental techniques are outlined together with an appraisal of their utility in the characterization of some of the structural aspects associated with crystal growth and related processes. The paper provides an overview of some recent studies through a number of case examples:

• •|extended X-ray absorption fine structure (EXAFS) and its application to studies of the local environment around surface oxides and extrinsic dopants in group III–V semiconductors;

• •|X-ray standing waves and their application to studies of ionically adsorbed crystal habit modifiers;

• •|dynamic X-ray powder diffraction and its applications to the in-situ examination of the solution crystallization of n-alkanes and the electrochemical crystallization of PbO₂;

• •|X-ray Laue topography and its application to the characterization of crystal lattice defects;

• •|high resolution X-ray multiple diffraction and its use in probing lattice coherence in compound semiconductor multilayers;

• •|the use of surface X-ray duffraction to examine structural order at the crystal solution interface.

Current trends and likely future developments in these and related techniques are outlined.