微氮直拉硅单晶中氧化诱生层错透射电镜研究

利用透射电镜研究了热氧化过程中含氮（NCZ）和不含氮（CZ）直拉硅单晶的氧化诱生缺陷.研究表明，NCZ中的氧化诱生层错的尺寸随着湿氧氧化时间的延长而减小，并有冲出型位错产生.而在CZ中，生成了大量的多面体氧沉淀，并且随着热氧化时间的延长，层错的尺寸逐渐增大. 关键词： 直拉硅 透射电镜 氧化诱生层错     

直拉硅中氮在高温退火过程中对氧沉淀的影响

研究了掺氮直拉硅单晶（NCZ）中氮在高温退火过程中对氧沉淀的影响.通过不同温度高温退 火后，测量氧沉淀的生成量和观察硅片体内微缺陷（BMD）密度与高温形核时间的变化关系 ，同时用透射电子显微镜(TEM)观察氧沉淀及相关缺陷的微观结构.实验结果表明高温退火后 氮对硅中氧沉淀形核有明显的促进作用，在相同退火条件下NCZ硅中BMD密度要远远高于相应 的普通直拉硅.这是由于氮在高温下与氧反应形成氮氧复合体（N-V-O）促进了氧沉淀的形核 ，而且TEM的结果表明氧沉淀的形态都是平板状，周围存在应力场. 关键词： 直拉硅 掺氮 氧沉淀     

直拉硅单晶中的氧沉淀

目前世界上硅单晶材料中,90%是用直拉(CZ)方法生长的.在这种方法中,固相的石英坩埚与熔融的硅经历下列反应: Si+SiO2→2SiO(I)虽然在一般晶体生长温度(～1420℃)下,SiO是挥发的,但是仍然会有相当多的氧保留在熔硅里,并通过固液界面进入晶体.通常的CZ硅中含有～1018/cm3的氧(较FZ硅高1-2数量级).作为硅中的杂质,如果说碳的作用是在晶体生长阶段有助于微缺陷的形成,那么氧的行为更多地表现在晶体生长以后的热处理中.氧在集成电路的制造工艺的热循环中,会因过饱和而发生沉淀.由于氧沉淀和由它引起的其它缺陷,对器件产生很大影响(有利的和…     

低起始温度的线性升温热处理对直拉硅中氧沉淀的影响

研究了直拉硅片从不同的温度线性升温(Ramping)到750℃,然后在750℃退火64 h过程中的氧沉淀行为. 结果表明,Ramping对硅片中氧沉淀的形成有明显的促进作用,且起始温度越低促进作用越强. 这是因为在Ramping处理中,低温(450—650℃)热处理阶段氧的扩散速率显著增强,促进了氧沉淀核心的形成,且较低的Ramping升温速率有利于氧沉淀核心的稳定和继续长大. 进一步的实验结果还表明,低起始温度的Ramping处理可应用于硅片的内吸杂工艺,能促进氧沉淀的生成提高硅片的内吸杂能力,减少热预 关键词： 直拉硅 氧沉淀 退火     

低温退火对重掺砷直拉硅片的氧沉淀形核的作用

通过对比研究重掺砷直拉硅片和轻掺n型直拉硅片经过低温(450—800℃)和高温(1000℃)两步退火的氧沉淀行为,阐明了低温退火对重掺掺砷直拉硅片的氧沉淀形核的作用.研究指出：重掺砷硅片在450℃和650℃退火时的氧沉淀形核比在800℃退火时更显著,这与轻掺硅片的情况截然相反;此外,与轻掺硅片相比,重掺砷硅片在450℃和650℃退火时氧沉淀的形核得到增强,而在800℃退火时氧沉淀的形核受到抑制.分析认为,重掺砷硅片在450℃和650℃退火时会形成砷-空位-氧(As-V-O)复合体,它们促进了 关键词： 重掺砷直拉硅片 氧沉淀形核 低温退火     

低起始温度的线性升温热处理对直拉硅中氧沉淀的影响

研究了直拉硅片从不同的温度线性升温(Ramping)到750℃，然后在750℃退火64 h过程中的氧沉淀行为. 结果表明，Ramping对硅片中氧沉淀的形成有明显的促进作用，且起始温度越低促进作用越强. 这是因为在Ramping处理中，低温(450—650℃)热处理阶段氧的扩散速率显著增强，促进了氧沉淀核心的形成，且较低的Ramping升温速率有利于氧沉淀核心的稳定和继续长大. 进一步的实验结果还表明，低起始温度的Ramping处理可应用于硅片的内吸杂工艺，能促进氧沉淀的生成提高硅片的内吸杂能力，减少热预     

直拉硅单晶原生漩涡缺陷的研究

本文用化学腐蚀方法, 从含有漩涡缺陷的原生CZ硅单晶中分离出尺寸在1000--6000埃间的氧沉淀, 制成萃取复型样品,用T E M 对氧沉淀作微区电子衍射分析. 同时, 观察硅薄膜中漩涡缺陷的TEM 象, 确定了二者的对应关系. 结果表明, 构成漩涡缺陷的氧沉淀主要是呈方形片的热液石英(keatite, siliea k) 及少量呈六角片的。方英石(a-cristobalite ), 沉淀片周边沿<1 1 0> 方向, 惯习面前者的为{ 100} , 后者的为{ 1 1 1}. 样品的红外吸收光谱表明, 方片状热液石英沉淀可能与1 2 2 4 (1/cm ), 吸收峰相对应. 关键词：     

中子辐照直拉硅中的本征吸除效应

对经中子辐照的直拉硅中的本征吸除效应进行了研究.结果表明:经中子辐照后,直拉硅片经一步短时退火就可以在硅片表面形成完整的清洁区.清洁区宽度受辐照剂量和退火温度所控制,清洁区一旦形成,就不随退火时间变化.大量的缺陷在中子辐照时产生,并同硅中氧相互作用,加速了硅片体内氧的沉淀,是快速形成本征吸除效果的主要因素,从而把热历史的影响降到次要地位 关键词： 本征吸除 中子辐照 直拉硅     

直拉硅单晶原生漩涡缺陷的研究

本文用化学腐蚀方法,从含有漩涡缺陷的原生CZ硅单晶中分离出尺寸在1000—6000?间的氧沉淀,制成萃取复型样品,用TEM对氧沉淀作微区电子衍射分析。同时,观察硅薄膜中漩涡缺陷的TEM象,确定了二者的对应关系。结果表明,构成漩涡缺陷的氧沉淀主要是呈方形片的热液石英(keatite,silicak)及少量呈六角片的α方英石(α-cristobalite),沉淀片周边沿<110>方向,惯习面前者的为{100},后者的为{111}。样品的红外吸收光谱表明,方片状热液石英沉淀可能与1224cm^-1吸收峰相对应。 关键词：     

减压充氮直拉硅单晶技术

硅单晶的生产方法有两种:一是悬浮区熔法(FZ),二是直拉切氏法(CZ).前者硅单晶纯度较高但单晶直径受到一定限制,后者已成为生长大直径硅单晶的主要方法.为保证产品质量,在采用直拉法时,必须使用保护气体在一定压力下生长晶体.氩为惰性气体中较为廉价的一种,因此采用氖保护气拉制硅单晶已成为国际上通行的技术和生产方法.更为廉价的氧、氮一直被视为会起化学反应而未被采用.浙江大学高纯硅及硅烷国家重点实验室研究了氮硅的化学反应,打破了国际公认的氮不能作直拉硅单晶保护气的观点,在国内外首创以纯氮作保护气,制备直拉硅单晶的整套技术.…     

Rapid-thermal-anneal-based internal gettering for?germanium-doped Czochralski silicon

The internal gettering (IG) effects involved with a rapid thermal anneal (RTA) in germanium-doped Czochralski silicon (GCz-Si) wafer have been investigated. It was found that germanium doping could enhance the oxygen precipitation in bulk while shrinking the denuded zone width near the surface through pre-RTA at high temperature plus low–high temperature conventional furnace anneals. Rapid cooling rate after RTA was clarified to be beneficial for oxygen precipitation for GCz-Si wafer. It was suggested that the germanium doping could increase the vacancy concentration in Cz-Si during RTA by forming the germanium–vacancy complexes. In contrast to that in Cz-Si wafer, the smaller-sized higher-density oxygen precipitates were presented in the nucleation anneals, then followed RTA pretreatment while more oxygen precipitates survived during ramping processes after nucleation anneals in the GCz-Si wafer. Enhanced heterogeneous nucleation and reduced critical radius of precipitates associated with the germanium–vacancy complexes have been proposed for the oxygen precipitation enhancement.     

Composition of oxygen precipitates in Czochralski silicon wafers investigated by STEM with EDX/EELS and FTIR spectroscopy

In this work, we investigated the stoichiometry of oxygen precipitates in Czochralski silicon wafers. The thickness dependence of the Cliff–Lorimer sensitivity factor for the silicon/oxygen system was determined and applied for the investigation of the stoichiometry of oxygen precipitates by EDX. The results show that both plate‐like oxygen precipitates and a transitional form between plate‐like and octahedral precipi‐ tates consist of SiO₂. This was confirmed by EELS low loss spectra where the typical spectrum for amorphous SiO₂ was observed. Moreover, the absorption band of plate‐like precipitates at 1227 cm^–1 was found in the low temperature FTIR spectrum. It was demonstrated that this band can only be simulated by the dielectric constants of amorphous SiO₂. (© 2015 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Combined multiparametric X-ray diffraction diagnostics of microdefects in silicon crystals after irradiation by high-energy electrons

The quantitative diagnostics of complex defect structures in silicon crystals grown by the Czochralski method and irradiated with different doses of high-energy electrons (18 MeV) is performed by methods of high-resolution X-ray diffraction. The analysis is based on analytical formulas of the statistical dynamical theory of X-ray diffraction in nonideal crystals with randomly distributed defects of several types. Using the combined treatment of reciprocal space maps and rocking curves, the concentration and average radii of dislocation loops, as well as the concentration and radii of oxygen precipitates in the silicon samples, are determined.     

Accelerated oxygen precipitation in fast neutron irradiated Czochralski silicon

Annealing effect of the oxygen precipitation and the induced defects have been investigated on the fast neutron irradiated Czochralski silicon （CZ-Si） by infrared absorption spectrum and the optical microscopy. It is found that the fast neutron irradiation greatly accelerates the oxygen precipitation that leads to a sharp decrease of the interstitial oxygen with the annealing time. At room temperature （RT）, the 1107cm^-1 infrared absorption band of interstitial oxygen becomes weak and broadens to low energy side. At low temperature, the infrared absorption peaks appear at 1078cm^-1, 1096cm^-1, and 1182cm^-1, related to different shapes of the oxygen precipitates. The bulk microdefects, including stacking faults, dislocations and dislocation loops, were observed by the optical microscopy. New or large stacking faults grow up when the silicon self-interstitial atoms are created and aggregate with oxygen precipitation.     

Detection and mapping of oxygen in silicon wafers by scanning infrared absorption

Scanning Infrared Absorption (S.I.R.A.) setup was carried out for investigating and mapping of microdefects distribution in Czochralski silicon wafers. Using CO₂ laser, this non destructive, non contact test method allows transmitted beam local attenuation from oxygen precipitates to be determined. Transmitted intensity I_t maps from peak height of the 1080 cm⁻¹ absorption band were obtained. An inhomogeneous initial oxygen distribution is found in as-grown samples. The samples were then submitted to preannealing at 750°C for 16 hours, followed by annealing at 900°C for 24 hours. The obtained I_t fluctuations mapping depicts a ring-shaped distribution of oxygen precipitates.     

Flux-enhanced monochromator by ultrasound excitation of annealed Czochralski-grown silicon crystals

The neutron flux from monochromator crystals can be increased by ultrasound excitation or by strain fields. Rocking curves of both a perfect float-zone silicon crystal and an annealed Czochralski silicon crystal with oxygen precipitates were measured at various levels of ultrasound excitation on a cold-neutron backscattering spectrometer. We find that the effects of the dynamic strain field from the ultrasound and the static strain field from the defects are not additive. Rocking curves were also taken at different ultrasound frequencies near resonance of the crystal/ultrasound-transducer system with a time resolution of 1 min. Pronounced effects of crystal heating are observed, which render the conditions for maximum neutron reflectivity delicate. Received: 19 October 2001 / Accepted: 7 March 2002 / Published online: 29 January 2003 RID="*" ID="*"Corresponding author. E-mail: andreas.magerl@krist.uni-erlangen.de     

Small angle neutron scattering from oxygen precipitates in silicon

The formation of silicon oxide precipitates from Czochralski grown silicon depends on the time and temperature of the heat treatment as well as on the initial content of interstitially dissolved oxygen. Samples containing between 5×10¹⁷ O_i/cm³ and 13×10¹⁷ O_i/cm³ have been heated at 750° C for 96 h. SiO₂ precipitates of various shape and size have been obtained and investigated by means of small angle neutron scattering (SANS) in the Q-range 0.05 Å^–1<Q<0.2 Å^–1. The obtained SANS patterns reveal a typical anisotropy of their intensity distribution, which splits into a central peak at Q<0.1 Å^–1 due to the shape of the individual particles and a number of weak intensities for large Q-values, originating from a correlation between defects, possibly between the precipitates. While these correlation peaks in the SANS patterns are seen best for rather low values of about (5–7)×10¹⁷ O_i/cm³ oxygen content, the central peak anisotropy is most pronounced for higher values of ca 10×10¹⁷ O_i/cm³. The integrated intensity of the central peak increases with increasing initial oxygen content. For comparison, untreated samples of the same initial oxygen content do not reveal any anisotropic SAN scattering or a broadened central peak beam.     

铜沉淀对直拉硅单晶中洁净区形成的影响

研究普通热处理和快速热处理工艺下直拉单晶硅中过渡族金属铜杂质对洁净区生成的影响. 通过腐蚀和光学显微镜研究发现,常规高-低-高三步洁净区生成热处理样品中, 第一步高温热处理前对样品铜沾污,样品中没有洁净区生成,高密度的铜沉淀布满了样品整个截面. 而第二步、第三步热处理过程中引入铜杂质不影响洁净区的生成. 研究表明,高温热处理过程中生成的铜沉淀不能溶解是导致洁净区不能形成的最主要原因. 另外,由于不同温度下热处理,导致引入铜杂质的平衡浓度不同,会在一定程度上影响洁净区的厚度. 对于快速热处理样品,可以得到相似的结果. 关键词： 直拉单晶硅 铜沉淀 洁净区