CZT晶体加工表面/亚表面损伤研究
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摘要
碲锌镉(Cd_(1-x)Zn_xTe,简称CZT)晶体是20世纪80年代一种由CdTe发展起来的性能优异的Ⅱ—Ⅵ族三元化合物半导体材料。它主要有两个用途:一是作为外延生长红外探测器材料HgCdTe衬底材料;另一个是最有潜力的室温x/γ射线探测器材料。目前对CZT晶体的加工工艺为:内圆切割—研磨—机械抛光—化学机械抛光,这些加工工艺对晶片造成的损伤会增大表面漏电流,同时缺陷的存在会成为外延生长HgCdTe的缺陷源,对其制作的探测器性能有严重影响。因此,通过对CZT晶体加工表面/亚表面损伤进行检测和分析,以求实现CZT晶体的高效、低损伤超精密加工。
本文在分析研究硬脆材料已有的损伤检测方法的基础上,通过大量的试验研究,解决了损伤检测中抛光液和腐蚀液配制的难题,最终确定了适合CZT晶体加工表面/亚表面损伤检测方法。利用纳米压痕试验检测CZT晶体不同晶面以及同一晶面不同晶向的纳米硬度和弹性模量,对力学特性的各向异性进行分析;利用Olympus光学显微镜、扫描电子显微镜(SEM)、Newview5022表面形貌轮廓仪等设备,对CZT加工表面质量进行检测;采用截面显微法检测较大的亚表面损伤,角度抛光法检测较小的亚表面损伤,并试验确定了合适的抛光液和腐蚀液;在此基础上对不同加工工艺条件下的表面/亚表面损伤进行检测、分析。
试验结果表明:CZT晶体在不同晶面上以及同一晶面的不同晶向都表现出明显的各向异性;加工工艺从内圆切割—研磨/磨削—抛光,表面质量有明显改善(粗糙度降低,损伤深度不断减小),材料去除从脆性断裂过渡到塑性去除:采用固结磨料磨削工艺代替研磨和机械抛光,从而解决了磨粒嵌入问题,为后续的化学机械抛光做好准备,最终获得低损伤表面。
Cadmium Zinc Telluride (Cd_(1-x)Zn_xTe, CZT) which is developed from CdTe in the eighty age of the twentieth century is one of the excellent ternary semiconducting compunds of II-IV type. It has two primary applications: the one is the substrate for HgCdTe; the other is the most promising detector material. Currently, the processing technology of CdZnTe crystals usually is internal cutting-lapping-mechanical polishing/CMP. The damages which are induced by these processes will seriously influence the performance of the detector, e.g., increasing the surface leakage current and being the defect resource for the epitaxial growth of HgCdTe. Therefore, the surface/subsurface damages are detected and analyzed to achieve the low damage, high effieciency and ultra-precision machining for CZT crystal.
Based on the existed methods for detecting the damage of hard-brittle crystal material, a set of methods suitable for CZT crystal are proposed to meet the different requirements by doing abundant experiments, and the problems of choosing slurry and corrosive liquid are resloved. The micro-hardness and elastic modulus of different crystal planes or different directions on the same plane are measured by nanoindentation, and then anisotropic mechanical property is analyed; the surface quality is measured by equipments, e.g. OLYMPUS optical microscope, SEM and 3D surface profiler; cross section method is used when subsurface damage depth (SSD) is larger and angle polishing method is used when SSD is lower, and then the damages induced by different machining processes are assessed.
We obtain the following results through detection and analysis: the CZT crystal shows the obvious anisotropic characteristic on different planes and directions; great improvement has been made on the surface quality with lower Ra and SSD from internal cutting to lapping/grinding and polishing, the patten of material removal is transformed from brittle fracture to plastic deformation; grinding is adopted to replace lapping and mechanical polishing, resolving the problem of embedded abrasive grain, then it can make good preparation for CMP and finally obtain CZT crystal surface with low damage.
本文在分析研究硬脆材料已有的损伤检测方法的基础上,通过大量的试验研究,解决了损伤检测中抛光液和腐蚀液配制的难题,最终确定了适合CZT晶体加工表面/亚表面损伤检测方法。利用纳米压痕试验检测CZT晶体不同晶面以及同一晶面不同晶向的纳米硬度和弹性模量,对力学特性的各向异性进行分析;利用Olympus光学显微镜、扫描电子显微镜(SEM)、Newview5022表面形貌轮廓仪等设备,对CZT加工表面质量进行检测;采用截面显微法检测较大的亚表面损伤,角度抛光法检测较小的亚表面损伤,并试验确定了合适的抛光液和腐蚀液;在此基础上对不同加工工艺条件下的表面/亚表面损伤进行检测、分析。
试验结果表明:CZT晶体在不同晶面上以及同一晶面的不同晶向都表现出明显的各向异性;加工工艺从内圆切割—研磨/磨削—抛光,表面质量有明显改善(粗糙度降低,损伤深度不断减小),材料去除从脆性断裂过渡到塑性去除:采用固结磨料磨削工艺代替研磨和机械抛光,从而解决了磨粒嵌入问题,为后续的化学机械抛光做好准备,最终获得低损伤表面。
Cadmium Zinc Telluride (Cd_(1-x)Zn_xTe, CZT) which is developed from CdTe in the eighty age of the twentieth century is one of the excellent ternary semiconducting compunds of II-IV type. It has two primary applications: the one is the substrate for HgCdTe; the other is the most promising detector material. Currently, the processing technology of CdZnTe crystals usually is internal cutting-lapping-mechanical polishing/CMP. The damages which are induced by these processes will seriously influence the performance of the detector, e.g., increasing the surface leakage current and being the defect resource for the epitaxial growth of HgCdTe. Therefore, the surface/subsurface damages are detected and analyzed to achieve the low damage, high effieciency and ultra-precision machining for CZT crystal.
Based on the existed methods for detecting the damage of hard-brittle crystal material, a set of methods suitable for CZT crystal are proposed to meet the different requirements by doing abundant experiments, and the problems of choosing slurry and corrosive liquid are resloved. The micro-hardness and elastic modulus of different crystal planes or different directions on the same plane are measured by nanoindentation, and then anisotropic mechanical property is analyed; the surface quality is measured by equipments, e.g. OLYMPUS optical microscope, SEM and 3D surface profiler; cross section method is used when subsurface damage depth (SSD) is larger and angle polishing method is used when SSD is lower, and then the damages induced by different machining processes are assessed.
We obtain the following results through detection and analysis: the CZT crystal shows the obvious anisotropic characteristic on different planes and directions; great improvement has been made on the surface quality with lower Ra and SSD from internal cutting to lapping/grinding and polishing, the patten of material removal is transformed from brittle fracture to plastic deformation; grinding is adopted to replace lapping and mechanical polishing, resolving the problem of embedded abrasive grain, then it can make good preparation for CMP and finally obtain CZT crystal surface with low damage.
引文
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[2]李奇峰.碲锌镉单晶体生长及碲锌镉室温核辐射探测器制备[D].四川大学博士学位论文,2002.
[3]Hofmann D M,Stadler W,Christmann P,et al.Defects in CdTe and Cd_(1-x)Zn_xTe[J].Nuc.Instr.in Physics Research A,1996,380:117-120.
[4]S.SEN,D.R.RHIGER,C.R.CURTIS,et al.Infrared Absorption Behavior in CdZnTe Substrates[J].Journal of ELECTRONIC MATERIALS,2001,30(6):611.
[5]刘克岳,王金义,张学仁,等.HgCdTe外延用的CdZnTe衬底研制,半导体技术,2000,25(2):38.
[6]查刚强.CdZnTe晶体的加工与表面质量控制[D].西北工业大学.硕士学位论文,2004.
[7]高德友.碲锌镉单晶体的生长及性能测定[D].四川大学.硕士学位论文,2003.
[8]李含冬.碲锌镉单晶体的生长和缺陷[D].四川大学.硕士学位论文,2004.
[9]王林军,桑文斌,史伟民.p型高阻CdZnTe晶体表面接触的电学性能研究[J].功能材料与器件学报,1999,5:2.
[10]Shiv Kumar,A.K.Kapoor,A.Nagpal,et al.Effect of substrate dislocations on the Hg in-diffusion in CdZnTe substrates used for HgCdTe epilayer growth[J].Journal of Crystal Growth,2006,297:311-316.
[11]Koyama A,Hichiwa A,Hirano R.Recent progress in CdZnTe crystals[J].J.Electron.Mater.,1999,28:683-689.
[12]Schieber M,Schlesinger T E,James R B,et al.Study of impurity segregation,crystallinity and detector performance of melt-grown cadmium zinc telluride crystals[J].Journal of Crystal Growth,2002,237:2 082-2 090.
[13]黄晖,许京军,张存洲,等.CdZnTe晶片Te夹杂的观察[J].光电子·激光,2001,12:1141-1143.
[14]李国强,华慧,介万奇.CdZnTe晶片的红外透过率研究[J].半导体光电,2003,24(4):276-278.
[15]李奇峰,金应荣,朱兴华,等.碲锌镉单晶生长的研究[J].广西师范大学学报,2000,2:7.
[16]Burger A,Groza M,Cui Y,et al.Characterization of large single-crystal gamma-ray detectors of cadmium zinc telluride[J].Journal of Electron Mater,2003,32:756-760.
[17]Chu M,Terterian S,Ting D,et al.Effects of excess tellurium on the properties of CdZnTe radiation detectors[J].Journal of Electron Mater,2003,32:778-782.
[18]T.E.Schlesinger,J.E.Toney,H.Yoon,etc al.Cadmium zinc telluride and its use as a nuclear radiation detector material[J].Materials Science and Engineering.2001,32:118-125.
[19]徐慧超,张金洲,沈浩元.用于X荧光分析的半导体探测器[J].常熟理工学院学报,2006,20(2):92.
[20]黄晖,潘顺臣,姬荣斌,等.射线探测用碲锌镉晶体及其器件研究[J].发光学报,2005,26(6):807.
[21]Chen H.Low-temperature photoluminescence of detector grade Cd_(1-x) Zn_xTe crystal treated by different chemical etchants[J].J.Appl.Phys.,1996,80(6):3509-3512.
[22]Y.Eisen,Current state-of-the-art industrial and applications using room-temperature CdTe and CdZnTe solid state detectors[J].Nucl.Instr.and Meth.,A380(1996):431-439.
[23]李伟堂.HgI_2室温半导体探测器的研制[D].四川大学硕士学位论文,1993.
[24]丁洪林,张秀凤.化合物半导体探测器及其应用[M],北京原子能出版社,1994.
[25]唐世红.碲锌镉晶体的缺陷及其退火研究[D].四川大学.硕士学位论文,2006.
[26]Csaba Szeles,Scott E.Cameron,Jean-Olivier Ndap,et al.Advances in the High-pressure Crystal Growth Technology of Semi-insulating CdZnTe for Radiation Detector Applications[J].SPIE Conference on Hard X-Ray,San Diego,2003.
[27]B.Pelliciaria,F.Dierrea,D.Brelliera,et al.A new growth method for CdTe:a breakthrough towards large areas[J].Journal of Crystal Growth,2005,275:99-105.
[28]Singh,R,et al.Molecular Beam Epitaxy Growth of High-Quality HgCdTe LWIR Layers on Polished and Repolished CdZnTe Substrates,Journal of Electronic Materials 〈http://www.findarticles.com/p/articles/mi_qa3776〉,2005,34(6):885-890.
[29]汪晓芹,介万奇,杨戈.CdZnTe晶体表面化学抛光研究[J].人工晶体学报,2005,34(5):790-791.
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