六面顶压机合成腔中心温度轨迹控制方法研究

金刚石合成过程中,稳定的最终压力和温度区域、初始升温升压的时间及方式都是合成工艺研究的重点,各边界温度条件对合成腔内温度都有重要影响.利用有限元方法建立了六面顶压机合成金刚石环境的热电耦合数值模型,对合成腔中心温度控制方法进行了研究.研究表明,合成腔中心升温时间效应对升温特征的描述是有效的,基于升温时间效应曲线和温度静态关系可以对腔体中心温度进行预测和控制.控制的关键是升温时间效应曲线的选取、变载点的确定和后继功率的施加方式.     

人造金刚石高压腔结构及温度场分布的改善

传统的直接加热式合成腔组装结构,存在两个问题:一是原材料本身通电发热,原料发生反应时电阻就会变化,加热功率也随之变化,造成温度波动,不利于金刚石生长;二是高压腔内各部位温度高低与压力高低不一致.间接加热式金刚石合成腔,原料本身不通电发热,由外部发热体发热,热量由外向内传导,间接使原料加热.压力与温度梯度方向一致,互相匹配,解决了高压腔各部位压力和温度高低互不匹配的难题;而且,在原料发生反应时,电阻不变,温度不会波动.实现了压力和温度的均匀、稳定,从而生产出高品级产品.单次合成金刚石500克拉以上,高品级率达到60;.     

PECVD腔室热流场数值仿真研究

等离子辅助化学气相沉积(PECVD)腔室的气流分布、温度分布是影响薄膜沉积工艺均匀性以及沉积速率的重要原因之一.本文对PECVD腔室气流建立连续流体和传热模型,研究了腔室内流场和温度分布特性;讨论了四种不同稳流室结构的PECVD腔室,在加热盘恒温400℃、质量流量5000 sccm、抽气口压力133 Pa的工艺条件下12英寸晶圆片附近上方流速、压力、温度分布情况;选择了其中一种稳流室结构作了多种质量流量( 20 ～ 5000 sccm)入口条件下的流场分析.仿真研究发现:在抽气口位置偏置的情况下,四种不同稳流室结构的腔室内热流场并未出现明显偏置,这表明抽气口偏置对工艺均匀性没有明显影响.加热盘附近上方2 mm处温度场大面均匀、稳定,且随入口质量流量变化波动很小,表现出良好的稳定性;气压分布呈现中心高边缘低的抛物线特征,流速呈现中心低边缘高的线性特征,且晶圆片附近以及喷淋头( Showerhead)入口压力和流速均随着入口质量流量的增加而升高.研究结果对PECVD腔室结构设计及工艺控制具有重要意义.     

绝缘片在粉末工艺合成人造金刚石中的试验研究

本文介绍了一种用氧化铝陶瓷基片制作的绝缘片,应用在粉末工艺合成人造金刚石中.通过在六面顶压机上进行人造金刚石高温、超高压合成的对比实验,结果表明:绝缘片能有效地改善合成腔体内部的温度分布差异,为金刚石的成核生长提供良好的环境.具有绝缘片的粉末合成块在粉末合成工艺中较没有绝缘片粉末合成块合成工艺更稳定.同时由于合成腔体的温场均匀,合成的金刚石颜色、透明度、单产都有很大提高.为进一步提高金刚石的品位进行了实验摸索.     

人造金刚石加热系统分析及其精密交流调功器设计

建立了加热系统的数学模型,深入分析各类交流加热的特性及差别,指出恒功率加热方式温控效果最佳且与直流加热无明显区别.建立恒功率交流加热系统SABER仿真模型并深入分析系统构成特性,设计一个基于适当功率滤波和输出偏置的模拟PID控制器.仿真和实验结果表明,所设计交流调功器具有成本低、实时性强、适应性好、控制性能佳、温控精度高等特点,能较好地满足金刚石合成工艺的要求.     

高岭石质密封传压介质金刚石合成扩大试验研究

以高岭石替代叶蜡石为主要原料制作密封传压介质并进行了金刚石合成扩大试验.分别以试块密度、腔体直径和热处理工艺为因素进行了条件试验.根据平均单产量、粗粒级含量、高强度颗粒含量、锤耗以及合成稳定性对实验结果进行表征.结果表明:φ40 mm腔体与φ42mm腔体使用效果较好,而φ44mm腔体合成稳定性相对较差.通过三段升温,最高温度320℃的低温长时热处理工艺,φ44mm腔体密封传压介质稳定性明显增加.采用以上最优条件,φ44mm腔体高岭石质密封传压介质的使用效果为:平均单产120 ct,≥130 N晶粒所占比例为40;,≥50/60晶粒比例为80;,锤耗小于1.2 kg/1×104 ct,合成稳定性较好.通过以上结果得出结论:高岭石质密封传压介质合成金刚石的效果与叶蜡石质密封传压介质相当,试验中采用的高岭石适合制作金刚石合成用密封传压介质.     

DRF-B80型蓝宝石晶体生长炉的研制

本文主要介绍采用冷心放肩微量提拉法技术生长高质量大尺寸蓝宝石晶体的新型设备,由于晶体生长是在高温、高真空、籽晶升降与旋转平稳、晶体测重精准、功率稳定的状态下进行生长.所以我们配备了具有高冷却性能的腔体部件;大抽速,低反油率的高真空系统;无抖动、无爬行籽晶轴(俗称:籽晶热交换器)升降及旋转系统;高精度、高分辨率测重系统;稳定可靠的电控系统及电源加热系统.实验结果表明:设备简化的设计模式,不仅提高了工人的操作速度,操作更加简单,节约了劳动时间,提高了设备的利用率.优良的测重系统在早期晶种生长的好坏,有这很大的关系;解决晶体是否粘埚也起着很大的作用.电控系统对加热电源的稳定控制是能否生长高质量大尺寸晶体关键之一.     

升温程序对6H-SiC晶体生长初期籽晶石墨化的影响

本文利用有限元方法模拟不同升温程序对籽晶石墨化的影响,计算表明籽晶表面石墨化层厚度是由“倒温度差”区间的温度、持续时间和“倒温度差”绝对值综合决定.在升温程序初期可以采用较小功率阶梯加热,迅速升温节约时间;中期可以采用从现有功率线性加热至额定功率,这样使得籽晶原料“倒温度差”区间内温度值变小且减缓反应;同时还使“倒温度差”绝对值减小,抑制籽晶和原料间的输运.同时籽晶石墨化实验通过元素线扫描测量出石墨层厚度,也证实了理论计算的结果.     

SiC晶体PVT生长系统的流体力学模型及其有限元分析

本文根据SiC晶体PVT生长炉的实际提出了生长系统温度场计算的流体力学模型,采用有限元法分析了生长腔内的热传导、辐射和对流对生长腔内和生长晶体中温度空间分布的影响.通过对生长腔内及生长晶体中温度瞬态和稳态分布的分析,得出在加热的初始阶段腔内气体对流对坩埚内的温度分布有较大影响,在系统热平衡后辐射对腔内温度分布起决定作用的结论.     

影响金刚石合成的粉末触媒形态因素

采用相同成分体系的片状、球状Ni-Mn-Cu粉末触媒体为原料,在六面顶压机上进行人造金刚石高温、超高压合成的对比实验.结果表明:具有片状等不规则形状的NiMnCu粉末触媒合成工艺较球状同类粉末触媒合成工艺更稳定、易于掌握.针对上述结果,结合金刚石成核、生长过程中合成腔体内温度变化对上述实验结果进行了讨论.     

Relationship of Morphological Types of Dynamic Forms of Crystals

Crystallography Reports - The relationship of morphological spectra (sets of data on the morphological types of real polyhedral crystals and their probabilities under current physicochemical...     

A review of measurement of thermophysical properties of silicon melt

Measurements of thermophysical properties of Si melt and supplementary study of X-ray scattering/diffraction by the authors' group were reviewed. The values obtained differed variously from those of literature. Density was 2–3% larger, surface tension 20–30% smaller, viscosity up to 40% larger, electrical conductivity 8% smaller, spectral emissivity more or less in good agreement with literature values, and thermal diffusivity a few percent larger. An anomalous density jump was found near the melting point. Surface tension and viscosity also showed anomaly. A strange time-dependent change of density was observed over 3 h after melting. X-ray analyses suggested a slight change in local atom ordering, but showed no sign of cluster formation. An addition of 0.1 at% gallium caused the density jump to disappear, while that of boron caused no change. An EXAFS study of the former melt indicated a strong interaction between Ga and Si atoms as if molecules of GaSi₃ existed. The implications of the measured properties are a possibility of soft-turbulence in an Si melt in a relatively large crucible, a more complicated manner of intake of oxygen depleted molten Si from the free surface region to underneath the growing crystal, and a relaxation of the melt after melting arising from trapped gas species.     

Generation of crystal structures of heteromolecular compounds by the method of discrete modeling of packings

Within the method of discrete modeling of packings, an algorithm of generation of possible crystal structures of heteromolecular compounds containing two or three molecules in the primitive unit cell, one of which has an arbitrary shape and the other (two others) has a shape close to spherical, is proposed. On the basis of this algorithm, a software package for personal computers is developed. This package has been approved for a number of compounds, investigated previously by X-ray diffraction analysis. The results of generation of structures of five compounds—four organic salts (with one or two spherical anions) and one solvate—are represented.     

Development of Pauling's concepts of geometric characteristics of atoms

The evolution of the geometric characteristics introduced by Pauling and their dependence on the specific features of the structure and chemical bonds have been considered. The values of the covalent and van der Waals radii are given as well as their relationships and mutual transitions.     

Investigation of the Mechanism of Influence of Stress Corrosion on the Development of Macroplastic Instabilities of Aluminum–Magnesium Alloy

Crystallography Reports - Macroscopic jumps of plastic deformation (few percent in amplitude) on creep curves of aluminum–magnesium alloy, caused by a local effect of concentrated solution of...     

Comparative analysis of two methods of calculation of the orientation of domain walls in ferroelastics

Two types of domain-wall equations are analyzed: the equations derived by the Sapriel method and the equations obtained by interface matching of the thermal-expansion tensor. It is shown that, for W-type domain walls, these methods yield the same equations. For W′-type domain walls, the equations obtained by different methods coincide for proper ferroelastics and differ for improper ferroelastics.     

Dependence of the parameters of equations of viscous flow on chemical composition of silicate melts

The temperature dependence of viscosity of silicate melts is discussed in the framework of the Avramov–Milchev (AM) equation. The composition is described by means of two parameters: the molar fraction, x, and the “lubricant fraction”, l. The molar fraction is the sum of the molar parts x_i of all oxides dissolved in SiO₂, the molar fraction of the latter being 1 ? x. It is shown that, with sufficient precision, two of the parameters of the AM equation can be presented as unique functions of the molar fraction. On the other hand, x is not sufficient to determine properly the reference temperature T_r , at which viscosity is η_r = 10¹³ [dPa.s]. Therefore, additional parameter, “lubricant fraction” l, is introduced. For each of the components, l_i is a product of molar part x_i and a specific dimensionless coefficient 0 ≤ k_i ≤ 1 accounting for the specific contribution of this component to the increased mobility of the system. It is demonstrated that, for l > 0, the reference temperature is related to the “lubricant fraction” l through the reference temperature T_r,SiO2 of pure SiO₂.     

A SAXS study of kinetics of aggregation of silica sols

SAXS in situ experiments on the evolution of TMOS solutions during hydrolysis and polycondensation lead to power laws with scaling exponents ≈ 2. It is suggested that this could be the result of the polydispersity of the samples and that only an apparent fractal dimension can be obtained in this way. Kinetic studies tend to indicate that agglomeration in the sol is the result of a diffusion-controlled process.     

Study of the possibility of interactive control of the surface profile of X-ray optical elements

We investigate the possibility of controlling the curvature parameters of parabolic mirrors that are modular elements of two types consisting of a base and thin inserts placed at the opposite side of the work surface. In the first type of modular elements, bending is controlled by the difference in the coefficients of the thermal expansion of the base and inserts. In the second type of elements, the profile is changed by the piezoelectric straining of the inserts under an electric field. A correlation is established between the parameters of modular elements and their surface curvature profile.