用Czochralski方法生长KMgF_3晶体的研究

先把KF和MgF2以1∶1摩尔比混合后在Ar气体环境中650℃的恒温下烧结成KMgF3化合物。然后仍在Ar气体环境中用Czochralski方法生长了KMgF3∶Cr2+、KMgF3∶Eu2+、KMgF3∶Sm2+等无色、透明的优质单晶体。并分析了能够成功地生长优质氟化物晶体的各个关键环节。

Czochralski法生长Lu_2SiO_5:Ce晶体的发光特性(英文)

本文使用铱坩埚感应加热Czochralski法成功地生长出了无色透明且尺寸达5 0mm× 6 0mm的Lu2 SiO5:Ce晶体。XRD结构分析表明 ,该晶体为单斜结构。在室温下分别以X射线和紫外光为激发源测量了该晶体的发射光谱 ,获得的发射波长分别为 4 0 3nm和 4 2 0nm ,光衰减时间为 4 1ns,光产额达 32 0 0 0p/MeV。发射光谱的双峰结构以及晶体的发光特性证明其发光源于Ce3 + 离子的 5d1→5F5/ 2 和 5d1→5F7/ 2 跃迁。

轴向磁场作用下Czochralski浅液池内热对流特性研究

为了有效抑制熔体热对流并提高晶体的生长质量,采用三维数值模拟方法研究了轴向磁场对双向温差作用下Czochralski浅液池内Marangoni-热毛细对流的影响。在一个给定的底部热流密度条件下,探讨了轴向磁场对稳态流动和非稳态流动的影响,确定了不同磁场强度下流动由三维稳态流动向三维非稳态流动转变的临界Macri。结果表明:随着磁场强度的增大,临界Macri不断增大。轴向磁场对液池内稳态和非稳态Marangoni-热毛细对流均具有较好的抑制效果。对于稳态流动,磁场的引入会使自由表面温度波动幅值受到削弱,波数减少;对于非稳态流动,监测点P处的温度振荡随着磁场强度的增加不断逐渐减弱直至消失,流动由三维非稳态过渡为三维稳态,相应地,温度波动结构也会发生转变。

Impact of Heat Shield Structure in the Growth Process of Czochralski Silicon Derived from Numerical Simulation

Further development of the photovoltaic industry is restricted by the productivity of mono-crystalline silicon technology due to its requirements of low cost and high efficient photocells. The heat shield is not only the important part of the thermal field in Czochralski（Cz） mono-crystalline silicon furnace, but also one of the most important factors influencing the silicon crystal growth. Large-diameter Cz-Si crystal growth process is taken as the study object, Based on FEM numerical simulation, different heat shield structures are analyzed to investigate the heater power, the melt-crystal interface shape, the argon flow field, and the oxygen concentration at the melt-crystal interface in the process of large Cz-Si crystal growth. The impact of these factors on the growth efficiency and crystal quality are analyzed. The results show that the oxygen concentration on the melt-crystal interface and the power consumption of the heater stay high due to the lack of a heat shield in the crystal growth system. Argon circumfluence is generated on the external side of the right angle heat shield. By the right-angle heat shield, the speed of gas flow is lowered on the melt free surface, and the temperature gradient of the free surface is increased around the melt-crystal interface. It is not conducive for the stable growth of crystal. The shape of the melt-crystal interface and the argon circulation above the melt free surface are improved by the inclined heat shield. Compared with the others, the system pulling rate is increased and the lowest oxygen concentration is achieved at the melt-crystal interface with the composite heat shield. By the adoption of the optimized composite heat shield in experiment, the real melt-crystal interface shapes and its deformation laws obtained by Quick Pull Separation Method at different pulling rates agree with the simulation results. The results show that the method of simulation is feasible. The proposed research provides the theoretical foundation for the thermal field design of the large diameter Cz-Si monocrystalline growth.

Optimal Control of Oxygen Concentration in a Magnetic Czochralski Crystal Growth by Response Surface Methodology

Concepts and techniques of response surface methodology have been widely applied in many branches of engineering, especially in the chemical and manufacturing areas. This paper presents an application of the methodology in a magnetic crystal Czochralski growth system for single crystal silicon to optimize the oxygen concentration at the crystal growth interface in a cusp magnetic field. The simulation demonstrates that the response surface methodology is a feasible algorithm for the optimization of the Czochralski crystal growth process.

Determination of Ge content in high concentration Ge-doped Czochralski Si single crystals by FTIR

SiGe single crystals with different Ge concentrations were measured by Fourier transform infrared （FTIR） spectroscopy at room temperature （RT） and 10 K. A new peak appears at the wave number of 710 cm^-1 and the spectroscopy becomes clearer with an increase in Ge content. The absorption strength and wave sharp of the 710 cm^-1 peak are independent of temperature. The relation of the absorption coefficient amax, the band width of half maximum （BWHM） Wit2 of the 710 cm^-1 peak, and the Ge concentration is determined with the Ge content obtained by SEM-EDX. The conversion factor is k = 1.211 at 10 K. Therefore, the Ge content in high concentration Ge doped CZ-Si single crystals can be determined by FTIR.

Simulation of Heat Transfer and Oxygen Transport in a Czochralski Silicon System with and Without a Cusp Magnetic Field

Simulations of heat transfer and oxygen transport during a Czochralski growth of silicon with and without a cusp magnetic field were carried out. A finite volume method with a low-Reynolds number K-e model proposed by Jones-Launder was employed. The numerical results were compared with the experimental data in the literature. It is found that the calculated results are in good agreement with the experimental data.

Effects of Germanium on Movement of Dislocations in p-Type Czochralski Silicon

By indentation at room temperature followed by annealing at high temperatures, the pinning effect of germanium on dislocations in germanium-doped Czochralski silicon was investigated. Experimental results show that the dislocations in germanium-doped Czochralski silicon move shorter and slower than those in Czochralski silicon undoping with germanium when the concentration of germanium is over 1×1018 cm-3. The retarding velocity of dislocations is contributed to the dislocations pinning effect of the strain field introduced by the high concentration germanium, and the Ge4B cluster and the oxygen precipitation those are preferred to form at higher concentration germanium.

KCl Single Crystals Growth with Mn, Ag and In Impurities by Czochralski Method and Study of Impurities Influence on Their Properties

In this research KCl, KCl:Mn, KCl:Ag and KCl:In single crystals have been grown by Czochralski method. X-ray diffraction confirms KCl single crystal formation. In this work also influence of mentioned impurities on the optical property of KCl single crystal has been studied by chemical etching. Then the hardness of these crystals have been measured by Vickers micro hardness. The result indicate the positive effect of the impurity on optical and mechanical properties.

Microstructure of flow pattern defects in boron-doped Czochralski-grown silicon

The morphology and microstructure of flow pattern defects （FPDs） in lightly boron-doped Czochralski-grown silicon （Cz-Si） crystals were investigated using optical microscopy and atomic force microscopy. The experimental results showed that the morphology of FPDs was parabola-like with several steps. Single-type and dual-type voids were found on the tip of FPDs and two heaves exist on the left and right sides of the void. All the results have proved that FPDs were void-type defects. These results are very useful to investigate FPDs in Cz-Si wafers further and explain the annihilation of FPDs during high-temperature annealing.

物性参数对硅单晶Czochralski生长过程的影响

为了了解硅单晶C zochra lsk i(C z)法生长时物性参数对熔体流动和氧传输过程的影响,利用有限元法对炉内的传递过程进行了全局数值模拟,假定熔体和气相中的流动都为准稳态轴对称层流,熔体为不可压缩流体,C z炉外壁温度维持恒定。结果表明:熔体的导热系数及发射率对熔体流动、加热器功率、结晶界面形状、晶体内轴向温度梯度和氧浓度有重要影响,而熔体的密度、黏度系数及熔解热对硅单晶C z法生长过程影响较小。

γ-LiAlO_2 Single Crystal Grown by Czochralski Technique and Modified by Vapor Transport Equilibration (VTE) Technique

Large-sized （～2 inch, 50.8 mm） γ-LiAlO2 single crystal has been grown by conventional Czochralski （Cz） method, but the crystal has a milky, dendriform center. The samples taken from transparent and milky parts were ground and examined by X-ray diffraction. All diffraction peaks could be indexed in γ-LiAlO2. The crystal quality was characterized by X-ray rocking curve. The full-width at half-maximum （FWHM） values are 116.9 and 132.0 arcsec for transparent and milky parts, respectively. The vapor transport equilibrium （VTE） technique was introduced to modify the crystal quality. After 1000℃/48 h, 1100℃/48 h, 1200℃/48 h VTE processes, the FWHM values dropped to 44.2 and 55.2 arcsec for transparent and milky part, respectively. The optical transmission of transparent part was greatly enhanced from 85% to 90%, and transmission of milky part from 75% to 80% in the range of 190~1900 nm at room temperature. When the VTE temperature was raised to 1300℃, the sample cracked and FWHM values of transparent and milky parts were increased to 55.2 and 80.9 arcsec, respectively. By combining Cz technique with VTE technique, large-sized and high quality γ-LiAlO2 crystal can be obtained.

Electrical Activity of Frank Partial Dislocations and the influence of Metallic Impurities in Czochralski-Grown Silicon

Electrical activity of Frank partial dislocations bounding stacking faults and the influence of Fe impurities in Czochralski-grown silicon are investigated by means of the electron-beam-induced-current(EBIC)technique.Frank partials free from metallic impurities exhibit EBIC contrast at low temperature but not at room temperature,indicating that they are only accompanied with shallow energy levels in the band gap.The energy level related to a Frank partial is determined to be about Ec-0.08eV in n-type Si.Frank partials decorated by Fe impurities become EBIC active at room temperature.

Structure and Optical Properties of ZnO Thin Films Prepared by the Czochralski Method

The zinc oxide seed film was coated on conductive glass (FTO) substrate by the Czochralski method,Zinc acetate and hexamethylenetetramine were used as raw materials to prepare growth solution,and then ZnO film was prepared by a low-temperature solution method.The effects of annealing temperature on the morphology,structure,stress and optical properties of ZnO films were studied.The thin films were characterized by X-ray diffraction (XRD),scanning electron microscopy (SEM),UV-visible absorption spectra (UV-vis),photoluminescence (PL) and X-ray photoelectron spectroscopy (XPS).The results show that the films are ZnO nanorods.With the increase of annealing temperature,the diameter of the rod increases,and the nanorods tend to be oriented.The band gap of the sample obtained from the light absorption spectra first increases and then decreases with the increase of annealing temperature.When the annealing temperature is 350 ℃,the crystallinity of zinc oxide film is the highest,the band gap is close to the theoretical value of pure ZnO.

Defects in Fast-Neutron Irradiated Nitrogen-Doped Czochralski Silicon after Annealing at High Temperature

Fast-neutron irradiated nitrogen-doped Czochralski silicon(NCZ-Si)was annealed at 1100℃for different time,then FTIR and optical microscope were used to study the behavior of oxygen.It is found that[Oi]increase at the early stage then decrease along with the increasing of anneal time.High density induced-defects can be found in the cleavage plane.By comparing NCZ-Si with Czochralski silicon(CZ-Si),[Oi]in NCZ-Si decrease more after anneal 24 h.

Denuded Zone Formation in Germanium Codoped Heavily Phosphorus-Doped Czochralski Silicon

The formation of a denuded zone(DZ)by conventional furnace annealing(CFA)and rapid thermal annealing(RTA)based denudation processing is investigated and the gettering of copper(Cu)atoms in germanium co-doped heavily phosphorus-doped Czochralski(GHPCZ)silicon wafers is evaluated.It is suggested that both a good quality defect-free DZ with a suitable width in the sub-surface area and a high density bulk micro-defect(BMD)region could be formed in heavily phosphorus-doped Czochralski(HPCZ)silicon and GHPCZ silicon wafers.This is ascribed to the formation of phosphorus-vacancy(P-V)related complexes and germanium-vacancy(GeV)related complexes.Compared with HPCZ silicon,the DZ width is wider in the GHPCZ silicon sample with CFA-based denudation processing but narrower in the one with two-step RTA pretreatments.These phenomena are ascribed to the enhancing effect of germanium on oxygen out-diffusion movement and oxygen precipitate nucleation,respectively.Furthermore,fairly clean DZs near the surface remain in both the HPCZ and GHPCZ silicon wafers after Cu in-diffusion,except for the HPCZ silicon wafer which underwent denudation processing with a CFA pretreatment,suggesting that germanium doping could improve the gettering of Cu contamination.

Radiative Heat Transfer and Thermocapillary Effects on the Structure of the Flow during Czochralski Growth of Oxide Crystals

A numerical study was carried out to describe the flow field structure of an oxide melt under 1) the effect of internal radiation through the melt (and the crystal), and 2) the impact of surface tension-driven forces during Czochralski growth process. Throughout the present Finite Volume Method calculations, the melt is a Boussinnesq fluid of Prandtl number 4.69 and the flow is assumed to be in a steady, axisymmetric state. Particular attention is paid to an undulating structure of buoyancy-driven flow that appears in optically thick oxide melts and persists over against forced convection flow caused by the externally imposed rotation of the crystal. In a such wavy pattern of the flow, particularly for a relatively higher Rayleigh number , a small secondary vortex appears nearby the crucible bottom. The structure of the vortex which has been observed experimentally is studied in some details. The present model analysis discloses that, though both of the mechanisms 1) and 2) end up in smearing out the undulating structure of the flow, the effect of thermocapillary forces on the flow pattern is distinguishably different. It is shown that for a given dynamic Bond number, the behavior of the melt is largely modified. The transition corresponds to a jump discontinuity in the magnitude of the flow stream function.

Analysis of μ-Czochralski Technique Using Two-Dimensional Crystallization Simulator

μ-Czochralski technique has been analyzed using two-dimensional crystallization simulator. It is observed that the temperature is relatively uniform in the entire Si region after the laser irradiation because the heat conductivity of the Si region is much higher than that of the underneath SiO2. Grain growth advances from the grain filter to the channel region and continues until it collides with what advances from random nucleation in the channel region. When the initial temperature is high, the random nucleation rarely occurs even under the supercooling condition, and the grain size becomes large. Moreover, it is qualitatively reproduced that the grain size increases as the irradiated energy of the laser irradiation increases.

Pr_3Co单晶的Czochralski pulling法制备研究

笔者对用Czochralskipulling法制备Pr_3Co单晶的生长条件进行了研究，首次用此法成功地制备了Pr_3Co单晶，为研究其物理特性提供了必要条件。

Microstructure of flow pattern defects in boron-doped Czochralski-grown silicon

The morphology and microstructure of flow pattern defects (FPDs) in lightly boron-doped Czochralski-grown silicon (Cz-Si) crystals were investigated using optical microscopy and atomic force microscopy. The experimental results showed that the morphology of FPDs was parabola-like with several steps. Single-type and dual-type voids were found on the tip of FPDs and two heaves exist on the left and right sides of the void. All the results have proved that FPDs were void-type defects. These results are very useful to investigate FPDs in Cz-Si wafers further and explain the annihilation of FPDs during high-temperature annealing.