基于静力悬浮原理的单晶硅球间微量密度差异精密测量方法研究

单晶硅球间微量密度差异测量是阿伏伽德罗常数量子基准定义的重要研究内容, 也是半导体产业中高纯度单晶硅制备工艺质量控制的主要方法. 为了改善现有非接触相移干涉法测量装置复杂和静力称重法测量不确定度低的特点, 根据单晶硅密度精密测量需要, 实现了一种基于静力悬浮原理的单晶硅球密度相对参比测量方法. 通过改变静压力和温度进行三溴丙烷和二溴乙烷混合液体密度的微量调节, 分别使两个待测单晶硅球在液体中悬浮, 根据悬浮状态时的液体温度和悬浮高度计算出待测单晶硅球密度差值. 通过双循环水浴和PID温度控制系统实现±100 μK的恒温液体测量环境. 通过图像识别和迭代拟合算法实现单晶硅球悬浮高度的测量. 使用PID静压力控制系统实现单晶硅球的稳定悬浮控制, 同时减少Joule-Thomson效应引起的液体温度改变. 利用静力悬浮模型中的温度变化和静压力变化线性关系准确测量出标准液体的压缩系数. 试验结果表明, 这种测量方法可以避免液体液面张力的影响, 测量相对标准不确定度达到2.1×10^-7, 能够实现单晶硅球密度差值的精密测量.

Method of accurately measuring silicon sphere density difference based on hydrostatic suspension principls

The micro density difference between silicon single crystal spheres is not only important for the research on the redefinition of Avogadro constant based on quantum standard, but also a key solution for quality control for the production of silicon single crystal with ultra-high purity in semi-conductor industry. To overcome the complexity of non-contact laser interferometer method and improve the accuracy of hydro-weight method, a method based on the hydrostatic suspension principle is realized. The silicon single spheres to be measured are immersed into mixture liquid including 1,2,3-tribromopropane and 1,2-dibromoethane, and floated freely by adjusting the temperature and pressure of the liquid. The micro density difference between two silicon single crystal spheres is calculated based on a mathematical model by using liquid temperature, pressure, and central floatation height difference in the floatation condition. The stable constant temperature liquid with maximal error ± 100 μ K is realized by two-cycle water bath and PID control system. The floatation height of silicon single crystal sphere is determined by binary image and iterative algorithm. The stable suspension is achieved by the PID pressure control system, and the temperature fluctuation due to Joule-Thomson effect is reduced. By means of linearity between changes of temperature and pressure in hydrostatic suspension model, the compressibility of mixture liquid is measured. The experimental results show that the influence from liquid surface tension is avoided by using the hydrostatic suspension method, and accurate measurement of density difference between silicon single crystal spheres can be achieved with an uncertainty of 2.1× 10^-7 (expand factor k=1).