2μm波段激光晶体Tm:YAP的生长缺陷

采用提拉法沿a、b、c轴方向生长了Tm:YAP晶体,研究了该晶体的几种常见缺陷.通过化学腐蚀,利用光学显微镜观察了Tm:YAP晶体主要晶面的位错腐蚀坑形貌,发现在沿b轴生长晶体的(010)面上存在位错蚀坑密度不同的区域,对其成因进行了分析.借助偏光显微镜研究了晶体中的孪晶及消光现象,分析了成因并提出了消除措施.用He-Ne激光对晶体内的散射颗粒分布进行了研究,在扫描电镜(SEM)下观察到形状不规则的散射颗粒夹杂.上述研究结果对获得优质Tm:YAP晶体具有重要意义.     

燃烧火焰法沉积金刚石的晶体形貌

本文研究了在大气中用燃烧火焰法沉积出的金刚石的结晶形态。结果发现，所沉积出的金刚石除了同体和十四面体单晶外，还有尖晶石型、伪五角型、二十面体型及球型等多重孪晶颗粒（ＭＴＰＳ），并与实验模型进行了对比观察。所有ＭＴＰＳ大多是以｛１１１｝面为孪晶面。在｛１１１｝面上还有大量层错和显微孪晶。本文还对产生上述晶体形貌的原因进行了理论分析。     

近化学计量比铌酸锂晶体中机械孪晶的消除

在用掺钾的助熔剂提拉法生长近化学计量比LiNbO3晶体时,长出的晶体尾部很容易出现孪晶裂纹现象,这种孪晶被认为是机械孪晶.这种孪晶的起因是由于晶体生长的收尾和从熔体中提起晶体阶段,在晶体底部产生直径的缩进,在缩进产生的台阶处出现应力集中,从而造成孪晶的成核.通过采用适当的收尾过程,以避免直径台阶的出现,可以很好地消除这种孪晶及其引起的裂纹.     

Na5[B2P3O13]晶体双晶结构的研究

采用泡生法和b向籽晶生长出尺寸为22mm×24mm×20mm的透明Na5[B2P3O13]晶体.晶体定向中发现(100)和(001)晶面的一级衍射出现双峰;正交偏光显微镜下观察晶体的(010)切片,看到清晰的明暗条纹;当一束激光正入射(010)切片时,产生衍射现象;用同步辐射白光X射线形貌术拍摄了(100)、(010)和(001)切片的Laue像,观察到了晶体的孪晶结构,再借助(010)切片的化学腐蚀研究,推出该晶体为规则的聚片双晶,其结合面为(001).     

Ce:YAP晶体生长和光谱性质

本文报道了用中频感应加热提拉法生长Ce:YAP晶体,晶体尺寸为35mm×80mm.在部分晶体中观察到了开裂、解理、孪晶、云层、核心和生长层等宏观缺陷,分析了缺陷与晶体生长温度梯度等因素的关系,对晶体样品进行了吸收光谱和荧光光谱分析.     

掺杂YCa4O(BO3)3晶体的生长与性质研究

采用提拉方法,首次使用铂坩埚在大气气氛下生长出大尺寸,高质量的非线性光学晶体YCa4O(BO3)3(YCOB).典型晶体尺寸为直径15～20mm,长度30～40mm.对晶体进行掺杂改性研究,已分别生长出掺杂浓度为5;的Nd:YCOB,Er:YCOB和掺杂浓度为20;的Yb:YCOB晶体.对沿不同方向生长的晶体的习性和缺陷进行了研究.晶体的生长是以典型的二维成核层状生长进行的.当沿方向生长时,晶体易出现(010)面孪晶及方向的解理面;而沿〈010〉方向生长时,可避免孪晶和解理面的出现.我们认为〈010〉方向为最佳生长方向.通过测量晶体的室温透过谱发现掺杂的YCOB晶体在深紫外(220nm)有较高的透过率(80;).初步的自倍频实验可观察到Nd:YCOB晶体能够在811nm的LD泵浦下产生较强的绿光,并且阈值较低.这表明掺稀土的YCOB晶体可能是一种有应用前景的自倍频激光材料.     

β-Zn3BPO7晶体的生长研究

采用泡生法生长β-Zn3BPO7(简称ZBP)晶体.用不同方向的籽晶进行晶体生长,分别得到了大尺寸的ZBP单晶.采取了适当措施有效地抑制了ZBP相变的发生,对生长得到的单晶进行X射线衍射分析,确定其为β-Zn3BPO7晶体.对得到的大尺寸单晶进行了形貌研究,并研究了ZBP晶体的生长习性.     

Yb：YAl3（BO3）4晶体形貌与生长速度的关系

观察测量了不同生长速度（相应于不同降温速度）自发成核生成的Yb:YAl3(BO3)4晶体形貌。粒试较大（＞2mm)的晶体不管降温速率快慢形态都很简单,只发育六方柱（1120）和菱面体（1011）,粒度较小（＜2mm)的晶体形态随降温速率增快而变复杂,发育一些罕见的高指数晶面,说明在生长速率较快的条件下,在晶体生长早期,一些高能面发育,在晶体生长后期已尖灭了,晶体生长的大部分时间是在低能面（1120）和（1011）上进行的,对比了不同生长条件下晶面的粗糙度,随着降温速度的增快,六方柱面（1120）和菱面体面（1011）由光滑变粗糙,顶面（0001）永远是粗糙的,从晶体结构上定性地探讨了3种晶面的杰克逊因子a及生长机理。     

Te溶剂-Bridgman法Cd0.9Mn0.1Te晶体生长习性研究

采用Te溶剂-Bridgman法生长了尺寸为φ30 mm× 60 mm的Cd0.9Mn0.1Te:In晶锭,通过淬火得到了生长界面形貌.测试了晶片在近红外波段的透过率和电阻;采用化学腐蚀的方法观察了晶片中位错,Te夹杂和孪晶界;采用光学显微镜和红外成像显微镜观察了生长界面处附近的形貌.测试结果表明,晶锭中部结晶质量较好的晶片红外透过率达到60％,电阻率达到2.828×1011Ω · cm.位错密度在106 cm-2数量级,Te夹杂密度为1.9×104 cm-2,同时孪晶密度明显低于Bridgman法生长的晶锭.生长界面宏观形貌平整,呈现微凹界面.但由于淬火过程的快速生长,界面微观形貌发生变化,呈现不规则界面,并在界面附近形成富Te相的包裹.     

RbTiOAsO4晶体中的生长缺陷和生长机制

采用溶盐法生长了大尺寸ＲｂｉＯＡｓＯ４晶体。利用同步辐射形貌术和化学腐蚀法，研究了ＲｂＴｉＯＡｓＯ４晶体中的生长缺陷。发现该晶体中的生长缺陷主要生长位错和生长扇界。大部分位钷沿「１００」方向，Ｂｕｒｇｅｒｓ适量为「００１」。在扫描电镜下，对原生ＲｂＴｉＯＡｓＯ４晶体的表面形态进行了观察，根据其表面二次电子像的特征，对不同晶面的生长控制机制进行了讨论。     

Growth twins in self-frequency doubling laser crystal YbxY1−xAl3(BO3)4

Using chemical etching.method, the growth twins in self-frequency doubling laser crystal Yb_xY_1−xAl₃(BO₃₄ have been observed. The etching pits on both sides of growth twin boundaries in the (10 1) slice are of the triangles with different orientations. The structure of growth twins is investigated by transmission synchrotron topography. In the transmission synchrotron topograph, the growth twins are visible not by ‘domain contrast’ but by ‘boundary contrast’, i.e. the twins appear in the topograph in form of X-ray kinematical diffraction contrast due to the lattice strain stemming from the impurity incorporation in the boundaries. The growth twins in Yb_xY_1−xAl₃(BO₃)₄ crystal are of inversion types, since no domain contrast was observed.     

6H-SiC单晶中的微管和小角度晶界

利用透射偏光显微术、同步辐射X射线形貌术、高分辨X射线衍射方法对6H-SiC(0001)晶片中的微管和小角度晶界等缺陷进行了研究.实验发现,在透射偏光显微镜下,微管通常呈现为蝴蝶形,这是由于微管周围存在着应力场,且应力分布不均匀,当线偏振光在通过微管周围区域时传播速度不同造成的.从X射线背反射同步辐射形貌像得到晶片中微管的Burgers矢量大小在2c到10c之间.从晶片00012衍射的双晶衍射摇摆曲线可以看出,晶片的中间大部分区域质量很好,双晶衍射峰为单峰且半峰宽很窄,一般为35"左右.在外围区域双晶衍射峰的半峰宽变宽,有些区域还会出现衍射峰的分裂,这说明外围区域有嵌镶块结构存在.     

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.     

The reduction of the misfit dislocation in non-doped AlAs/GaAs DBRs

The non-doped AlAs/GaAs distributed Bragg reflectors (DBRs) with density of misfit dislocation (MD) close to zero had been obtained. The reduction of MD density was achieved by increasing temperature distribution homogeneity on the growing crystal in consequence of higher rotation rate of the wafer. Two structures of DBR were crystallized using molecular beam epitaxy (MBE) under the same optimal growth condition. The growth runs differ only in the rotation rate of the wafers. X-ray topograph showed no residual MDs in case of faster rotation. The DBR structure with residual MD density is still highly strained. No additional relaxation process has occurred, what was confirmed by an angular position of DBR zeroth-order peak on high-resolution X-ray diffractometry (HRXRD) rocking curve.     

Synchrotron White Beam X-Ray Topography Characterization of Defect Structures in 2,10-Undecanedione/Urea Inclusion Compounds

Abstract

The defect structure of a crystal of the urea inclusion compound (UIC) of 2,10-undecanedione was investigated using Synchrotron White Beam X-ray Topography. X-ray transmission topographs recorded from different regions show that the crystal is divided into several twin domains. Each region in the crystal is revealed on the topographs by orientation contrast arising from the mutual misorientation of adjacent regions. Using a combination of pinhole Laue pattern analysis and topographic orientation contrast analysis, the twin operation was determined to be consistent with an approximately 60° rotation about the orthorhombic c-axis. Possible twin boundary structures are also presented. Other defects such as dislocations and inclusions are also characterized.     

Single‐crystal sapphire microstructure for high‐resolution synchrotron X‐ray monochromators

We report on the growth and characterization of sapphire single crystals for X‐ray optics applications. Structural defects were studied by means of laboratory double‐crystal X‐ray diffractometry and white‐beam synchrotron‐radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique. Therein the dislocation density was 10²–10³ cm⁻² and a small area with approximately 2*2 mm² did not show dislocation contrast in many reflections. This crystal has suitable quality for application as a backscattering monochromator. A clear correlation between growth rate and dislocation density is observed, though growth rate is not the only parameter impacting the quality.     

同步辐射单色光形貌术观察6H-SiC单晶中的微管缺陷

采用同步辐射单色光形貌术观察了6H-SiC单晶中的微管缺陷,发现晶片中Burgers矢量为1c的螺位错具有较高的密度.此外,还观察到对应较大Burgers矢量的微管.基于微管附近的应变场,并根据衍射几何,模拟计算了一系列具有不同Burgers矢量的微管在形貌像中的直径,计算结果与实验观察符合较好.     

Characterization of KDP crystal grown from solution with low pH value

Solubility curves of KDP (KH₂PO₄) in solutions with different pH values were measured. It was found that the solubility of KDP crystal increased with the reduction pH value of solution. Transparent KDP crystal was grown from solution with 1.5 pH by point seed. Chemical etching experiments revealed that pyramid sector of the crystal displayed more growth defects. Growth defects, such as growth striation and inclusion, were analyzed by white‐beam synchrotron radiation X‐ray topography. The reasons for the formation of these growth defects were discussed. Transmittance spectra test of both prismatic sector and pyramidal sector was performed. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Sodium acetate tri-hydrate whiskers

A new kind of whisker, which has not been previously reported in the literature, was grown on membranes which were in contact with a saturated aqueous solution of sodium acetate, using several techniques. Cellulose acetate membranes were used in all the cases and growth was successful at 25 ± 2°C and 45–55% relative humidity. A dense colony of whiskers, sometimes stuck together in bundles, usually up to 5 cm in length and ranging in width from 0.3–100 μm, developed within 72 h of growth. The whiskers were identified as sodium acetate tri-hydrate by means of Debye-Scherrer X-ray powder method. Laue transmission photographs indicated the existence of twin crystals within the individual single crystal whiskers as proved by electron diffraction in TEM. Some whiskers included internal and external channels, and there were several secondary effects, such as thickening in the middle of a whisker, formation of arrow-heads or spirals at the tips and various modes of branching. The whisker morphology and the various growth phenomena may be explained as a whisker growth process from their bases, when we consider a continuous crystallization from material which is supplied through and over the membrane.     

4 inch低位错密度InP单晶的VGF生长及性质研究

采用高压垂直温度梯度凝固法(VGF)生长了非掺、掺硫和掺铁的4 inch直径(100)InP单晶,获得的单晶的平均位错密度均小于5000 cm-2.对4 inch InP晶片上进行多点X-射线双晶衍射测试, 其(004)X-射线双晶衍射峰的半峰宽约为30弧秒且分布均匀.与液封直拉法(LEC)相比, VGF-InP单晶生长过程的温度梯度很低,导致其孪晶出现的几率显著增加.然而大量晶体生长结果表明VGF-InP晶锭上出现孪晶后,通常晶体的生长方向仍为(100)方向,这确保从生长的4 inchVGF-InP(100)晶锭上仍能获得相当数量的2~4 inch(100)晶片.由于铁在InP中的分凝系数很小,掺Fe-InP单晶VGF生长过程中容易出现组份过冷,导致多晶生长.通过控制生长温度梯度及掺铁量,可获得较高的掺铁InP单晶成晶率.对VGF-InP单晶的电学性质、位错密度及位错的分布特点、晶体完整性等进行了研究.