硅酸钛钡高温压电晶体及其传感器件研究进展

压电材料作为重要的功能材料,由其制备的结构健康检测器件已被广泛应用于国民经济的诸多领域。随着现代工业技术特别是航空航天、核电能源和智能制造等的发展,各类高温工况环境对压电材料的性能提出了更高的要求,因此研制综合性能优异的高温压电材料并将其应用到具有更高服役温度的传感器件中受到了研究者的广泛关注。硅酸钛钡(Ba_(2)TiSi_(2)O_(8),BTS)晶体具有较高的电阻率、较低的介电损耗和优良的压电性能,是一种具有良好应用前景的高温压电单晶材料。本文主要介绍了BTS晶体的提拉法生长制备工艺、单晶电弹性能表征、材料相变调控以及采用该晶体为核心元件研制的声表面波传感器和高温振动传感器的研究进展,最后对新型高温压电晶体及其传感器件的研发进行了总结和展望。

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。

直拉法单晶硅生长原理、工艺及展望

碳达峰、碳中和理念提出后,太阳能作为一种可再生绿色能源备受关注。单晶硅作为主要的光伏材料,其质量决定着太阳能电池效率的高低,为了降低成本和提高产能,人们对单晶硅提出越来越高的要求。直拉法(CZ法)是单晶硅的主要制备方法,其生产效率高,可实现自动化,直拉单晶硅市场占比超过90%,目前正朝着大尺寸、N型、薄片化、低氧低碳的方向发展。然而随着晶棒尺寸增大,热场变化更加复杂,现有CZ工艺难以满足市场需求。未来降低度电成本仍是晶硅光伏发展的驱动力,应通过技术革新、产业标准化、成本控制等手段推动光伏产业发展。本文介绍了CZ法生长单晶硅的基本原理和生长工艺,分别对缺陷控制、热场优化、氧含量控制等进行了分析,在总结工艺现状和单晶生长特点的基础上对直拉法生长单晶硅的发展方向进行了展望。

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。

8英寸铌酸锂晶体生长研究

铌酸锂单晶薄膜(LNOI)在新一代信息技术中关键通信器件领域的作用日益显著,随着铌酸锂单晶薄膜制备技术和光子集成技术的发展,降低芯片成本、增加芯片集成度是光子集成芯片永恒不变的发展方向,因此迫切需求大尺寸铌酸锂晶体。本文讨论了大尺寸坩埚中熔体自然对流随着液面下降的变化规律,研究了8英寸(1英寸=2.54 cm)铌酸锂Z轴、X轴两个提拉方向的生长特点,获得等径尺寸大于φ210 mm×50 mm的8英寸Z轴、X轴铌酸锂晶体。1 mm厚X轴铌酸锂晶圆的透过率显示波长380~3 300 nm光谱的透过率超过了70%,晶片纹影图像显示晶体中存在折射率脉理缺陷。

大尺寸优质Cr^(3+)∶BeAl_(2)O_(4)晶体生长与性能研究

本文采用感应加热提拉法结合上称重自动控径技术,成功生长出大尺寸、高质量的翠绿宝石(Cr^(3+)∶BeAl_(2)O_(4))晶体。晶坯等径圆柱体尺寸达到ϕ70 mm×140 mm,晶坯质量超过2800 g。通过冷光源照射晶坯,发现晶坯中心区域ϕ10~15 mm存在气泡。采用5 mW绿光激光照射ϕ8 mm×130 mm的翠绿宝石晶体棒,晶体内部无散射颗粒。利用Zygo激光平面干涉仪对晶体棒进行测试,波前畸变为0.3λ@632.8 nm。用电感耦合等离子体原子发射光谱法测定了翠绿宝石晶体的铬离子掺杂浓度,并计算出轴向浓度梯度为0.5×10^(-4)~1.9×10^(-4)cm^(-1)(摩尔分数)。用Perkin Elmer Lambda-950紫外可见近红外分光光度计测试了不同掺杂浓度的翠绿宝石晶体在室温下的吸收光谱,并计算了吸收系数。这些研究结果为翠绿宝石晶体的应用提供了重要的基础数据。

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。

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.

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.

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.

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.

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.

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.

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.

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.