重掺杂P型SiC的熔融KOH刻蚀行为研究

本文采用熔融KOH刻蚀方法详细研究了液相法生长的重掺杂P型6H-SiC晶体中的位错情况,探究了时间、温度变化对液相法生长的重掺杂P型6H-SiC晶片表面刻蚀的影响。当提高腐蚀时间或腐蚀温度时,晶片表面的腐蚀坑尺寸均表现出不同程度的增加,过高的温度及长时间刻蚀均导致过腐蚀现象的发生。根据不同腐蚀条件下腐蚀坑的形貌与分布,确定出刻蚀重掺杂P型6H-SiC晶片的最佳工艺参数。利用晶片在不同温度下的腐蚀速率变化关系及阿伦尼乌斯公式计算出晶体的反应活化能为10.59 kcal/mol。最后,对穿透型螺位错(TSD)和穿透型刃位错(TED)的形貌、尺寸和内部结构进行了详细的表征和分析,结果表明P型6H-SiC晶体中腐蚀坑的倾角与腐蚀时间无关。     

热交换法生长c面取向大尺寸蓝宝石晶体的研究

本文使用热交换法直接生长c面取向,尺寸为φ170 mm× 160 mm,重12 kg的蓝宝石晶体.晶体无色透明,内部无散射颗粒.沿c面(0001)方向的晶棒锥光图可观察到同心圆簇的干涉条纹,仅中心较小区域因内应力存在,干涉条纹发生扭曲.将抛光的晶片进行化学腐蚀后,通过金相显微镜检测位错腐蚀坑形貌图,结果显示,腐蚀坑呈三角形,平均位错密度较低,为1.98 × 103 Pits/cm2,X射线衍射半峰宽较小,晶体结构完整.     

Nd,Y:SrF2激光晶体的位错缺陷表征及分布研究

氟化物激光晶体Nd, Y∶SrF₂(NYSF)具有热导率高、发射光谱宽、发射截面适中等特点，在高功率激光技术领域具有重要应用。激光晶体中的位错是反映其晶格完整性的一类重要的微观晶体缺陷，对晶体材料的力学、光学性能具有重要影响。本文采用坩埚下降法制备了NYSF激光晶体，分析了腐蚀实验条件对位错蚀坑形貌的影响，获得了化学腐蚀法研究NYSF晶体位错缺陷的最佳腐蚀工艺，即浓度为4 mol/L的盐酸溶液作为腐蚀液，腐蚀温度为60℃、腐蚀时间为9～12 min;表征了位错腐蚀坑形态的演变过程，探讨了晶格原子排列对位错蚀坑形态的影响；利用化学腐蚀方法表征了位错缺陷在晶体中的分布规律，即轴向分布为从放肩到尾部先减少后增加，径向分布为从中心到边缘逐步增加；分析了晶体生长条件对位错缺陷形成的影响，提出了位错密度随坩埚下降速率的提高而升高的可能原因。     

温梯法Al2O3晶体位错形貌分析

用温度梯度法(Temperature Gradient Technique,简称温梯法或TGT法),定向籽晶[0001]方向,生长出φ110mm×80mm Al2O3单晶,晶体完整、透明.采用硼酸钠玻璃液作为Al2O3晶体的化学抛光和化学腐蚀剂,观察了晶体不同部位处(0001)、(112-0)晶片的化学腐蚀形貌相,(0001)切片的位错腐蚀坑呈三角形,位错密度为2×103～3×103/cm2;(112-0)切片位错腐蚀坑呈菱形,位错密度为7×103～8×103/cm2;而且等径生长部位的完整性比放肩处高.利用同步辐射X射线白光衍射实验分析了(0001)晶片的(2-021),(11-01)和(112-0)衍射面内的位错组态.确定了两组位错线的Burgers矢量,温梯法生长的Al2O3晶体中的位错主要是刃型位错.     

直拉单晶硅片“黑心”现象性质分析

对一种黑心片样品进行了分析.在确认黑心区为低少子寿命区的基础上,发现其电阻率明显偏高;发现黑心区经Secco刻蚀后,表面密布重叠圆形蚀坑,但与普通位错蚀坑有明显特征性区别;从其密度、形状与出现条件来看,它与电子半导体业中普遍报告的氧化堆垛层错(OSF)也不一致;进一步发现黑心区经Sirtle刻蚀后,表面呈现典型的大小明显不同的两种漩涡缺陷蚀坑,其密度明显低于上述Secco蚀坑.根据所得结果推测:黑心区主要密布一种性质上与普通位错相近,而所造成晶格畸变特征与范围不同于普通位错的晶格缺陷,它不属于已知的OSF微缺陷,而可能是一种由结晶生长过程中过饱和氧沉淀诱发形成的位错环;此外,黑心区还含有少量漩涡缺陷.     

EDTA和KCl双掺杂下KDP溶液的稳定性研究

研究了EDTA与KCl不同掺杂浓度和不同过饱和比下KDP溶液的成核过程,测定了不同条件下KDP过饱和溶液的诱导期;根据经典成核理论计算了成核热、动力学参数,并分析了溶液稳定性随掺杂浓度的变化情况。利用化学腐蚀法对KDP晶体(100)面进行了腐蚀,得到了清晰的位错蚀坑,并使用光学显微镜观察了(100)面位错蚀坑的分布特点。结果表明,当过饱和度为4%、掺杂浓度为0.01 mol%EDTA和1 mol%KCl时,不仅KDP过饱和溶液的稳定性比较高,而且位错蚀坑的分布比较均匀、密度小,适合高质量的KDP晶体生长。     

pH值对KDP晶体位错结构的影响

在一定的过饱和度下,分别用点状和片状籽晶在不同pH值溶液中生长出了KDP晶体.利用化学腐蚀法对KDP晶体的不同晶面进行了腐蚀,得到了清晰的位错蚀坑.应用光学显微镜对位错蚀坑的分布特点和密度做了观察分析,发现很多位错蚀坑成线状排布.pH值对KDP晶体位错密度有较大影响,低pH值条件下生长出的晶体位错密度较大.测试了KDP晶体样本的透过率,结果表明位错密度对KDP晶体的透过率没有明显的影响.     

掺质YAG晶体中的缺陷

本文报道了用化学腐蚀法对掺质浓度不同和掺质种类不同的YAG晶体样品进行的腐蚀,详细地观察了样品表面的腐蚀坑形貌,尤其是位错腐蚀坑的形貌和分布,测量了原生态和相应的退火样品上位错腐蚀坑的平均密度.在观测中发现,有些掺钕晶体样品上,位错腐蚀坑在中心区与边缘区的密集程度不同,有明显的分界.对此现象进行了探讨,认为出现在样品边缘区内的密集位错,除了来自于籽晶中以及来自于晶体从籽晶开始生长的起始处外,也由于熔体中出现在晶体周界处的自然对流与强迫对流边界层内的液流不稳,引起了生长界面边缘局部不稳而产生,环境气流起了相当的作用.     

SiC籽晶表面状态对晶体质量的影响

为了研究表面状态对晶体质量的影响,本文分别采用腐蚀后抛光与未抛光的晶片作为籽晶,利用金相显微镜对所得晶体进行了显微观察,结果表明:经过腐蚀后抛光的籽晶生长出的晶体质量高于未抛光籽晶所得晶体;生长前端的位错尺寸以及数量小于未抛光籽晶,说明抛光去除了部分表面浅的缺陷腐蚀坑,同时减小深腐蚀坑的尺寸,使得籽晶生长表面的缺陷密度和尺寸大大降低,有助于减少后期生长的晶体中的缺陷密度,提高结晶质量.     

8英寸导电型4H-SiC单晶衬底制备与表征

使用物理气相传输法(PVT)通过扩径技术制备出直径为209 mm的4H-SiC单晶,并通过多线切割、研磨和抛光等一系列加工工艺制备出标准8英寸SiC单晶衬底。使用拉曼光谱仪、高分辨X射线衍射仪、光学显微镜、电阻仪、偏光应力仪、面型检测仪、位错检测仪等设备,对8英寸衬底的晶型、结晶质量、微管、电阻率、应力、面型、位错等进行了详细表征。拉曼光谱表明8英寸SiC衬底100%比例面积为单一4H晶型;衬底(004)面的5点X射线摇摆曲线半峰全宽分布在10.44″~11.52″;平均微管密度为0.04 cm^-2;平均电阻率为0.020 3 Ω·cm。使用偏光应力仪对8英寸SiC衬底内部应力进行检测表明整片应力分布均匀,且未发现应力集中的区域;翘曲度(Warp)为17.318 μm,弯曲度(Bow)为-3.773 μm。全自动位错密度检测仪对高温熔融KOH刻蚀后的8英寸衬底进行全片扫描,平均总位错密度为3 293 cm^-2,其中螺型位错(TSD)密度为81 cm^-2,刃型位错(TED)密度为3 074 cm^-2,基平面位错(BPD)密度为138 cm^-2。结果表明8英寸导电型4H-SiC衬底质量优良,同比行业标准达到行业先进水平。     

Propagation behavior of threading dislocations during physical vapor transport growth of silicon carbide (SiC) single crystals

The dislocation formation and propagation processes in physical vapor transport (PVT) grown 4H silicon carbide (4H–SiC) single crystals have been investigated using defect selective etching and transmission electron microscopy (TEM). It was found that while the growth initiation process generally increased the density of threading dislocations in the grown crystal, for certain areas of the crystal, threading dislocations were terminated at the growth initiation. Foreign polytype inclusions also introduced a high density of dislocations at the polytype boundary. In the polytype-transformed areas of the crystal, almost no medium size hexagonal etch pits due to threading screw dislocations were observed, indicating that the foreign polytype inclusions had ceased the propagation of threading screw dislocations. Based on these results, we argued the formation and propagation of the threading dislocations in PVT grown SiC crystals, and proposed the dislocation conversion process as a plausible cause of the density reduction of threading dislocations during the PVT growth of SiC single crystals.     

化学腐蚀法研究Nd:YAG晶体位错

采用化学腐蚀法研究Nd∶YAG晶体位错.研究发现,腐蚀剂、腐蚀温度以及腐蚀时间对位错的显示都有影响.浓磷酸腐蚀剂在220 ℃下腐蚀20 min时,显示的位错最为清晰.蚀坑形状为菱形,经过计算,位错密度大约为10~3 cm~(-2).同一种腐蚀剂在不同的腐蚀时间所形成的位错蚀坑大小和形貌是不同的.同时发现在样品的边缘有位错塞积群.     

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.     

温梯法白宝石晶体的缺陷研究

采用导向温梯法(TGT)生长出[0001]方向直径为76mm的白宝石晶体.利用扫描电子显微镜(SEM)观察晶体(0001)面的腐蚀坑形态,并对晶体内部的包裹物进行了能谱(EDS)分析.白宝石晶体中的生长缺陷主要为位错和包裹体等.Al2O3晶体(0001)面的位错腐蚀坑呈六角形,并且有台阶状结构.分析了(0001)面内的位错类型.确定了TGT法生长的白宝石内部的包裹物的主要成分为碳.     

Etching Figures in Neodymium Gallate and Yttrium Aluminate Crystals

The dislocations existing in single crystals of neodymium gallate and yttrium aluminate grown by the Czochralski technique have been studied by means of etch pits. The data concerning their solubility in cases of different directions of a face orientation, various treatment temperatures and several enchant types are reported. The investigation of etch pits in the twinned YAlO₃ and NdGaO₃ crystals showed that twins are formed during a growth process. In the [110]‐pulled NdGaO₃ crystals the discrepancy between the twin and matrix parts of a crystal is accommodated by the dislocation congestion and the dislocation low‐angle boundaries whereas in [010]‐pulled YAlO₃ crystals the microcracks perform this function.     

Investigations of impurity striations in potassium bichromate crystals

Impurity striations in potassium bichromate crystals (KBC, lopezite) formed during crystal growth from aqueous solution were revealed by chemical etching and analyzed. Striations were revealed as etch grooves, as rows of dislocation etch pits and as rows of flat‐bottomed etch pits. Various types and groups of striations have been visualized. Some striations were due to lateral segregation of impurities caused by convection flow of the mother solution, other were formed during growth stoppages whereas induced striations were generated by changes in hydrodynamical conditions. Growth rates changes resulted in zonal distribution of impurities, formation of planar lattice strain, rows of clusters of point defects and rows of dislocations. Generation of striations with different intensities in various sectors is a proof of the selective capture of impurities. Ratios of growth rates of various faces of KBC crystals growing in forced and free convection regimes were determined by induced striations. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Defect characterization and composition distributions of mercury indium telluride single crystals

A mercury indium telluride (MIT) ingot was grown by the vertical Bridgman method. The defects in MIT crystals were characterized by the chemical etching method. A defect etchant for MIT crystals was developed. The etch pits of dislocations, microcracks and boundary was observed by scanning electron microscopy. It was elucidated that the etch pits density of dislocations of MIT wafers was about 4×10⁵ cm⁻². Te and In reduced at the grain boundaries, but were homogeneously distributed within the grains in the as-grown MIT crystals. The distribution of In in MIT crystals along the growth direction and radial direction was analyzed by electronic probe microscopy. It was found that In concentration was higher in the initial part and lower in the final part of the MIT ingot, which indicated that the segregation coefficient of In in MIT crystals was 1.15. The radial In concentration increased from the center to edge of the wafers and homogeneous in the middle part.