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以普通粉末衍射仪用单边法并峰值定位法(不借助内标)测定高纯硅粉的点阵常数,目的是提高测定的精确度和准确度。考虑了各种误差。对焦点偏移误差进行了分析、确定了准直的要求并以实验方法消除了此误差。用实验方法测定了衍射峰位的垂直发散几何偏差从而解决了此误差的校正问题。对峰值法的Lorentz等物理偏差进行了以实验数据为根据的校核。多次点阵常数测定值的标准误差仅为百万分之三,达到了高精确度。用不同靶的特征谱线对这一结果进行了验证,结果良好。因解决了上述误差的校正问题,准确度也达到相应水平,因而解决了单晶法与多晶法测定硅点阵常数不符的问题。分析及实验数据说明用普通衍射仪并单边峰值定位法测定结晶良好的高对称晶系样品的点阵常数,其精确度和准确度可达百万分之四。
The determination of the lattice constant of high purity silica fume by the unilateral method with the peak position method (without the aid of an internal standard) with ordinary powder diffractometer aims to improve the accuracy and accuracy of the determination. Considered a variety of errors. The focus offset error was analyzed, the collimation requirements were determined and the error was eliminated experimentally. The experimental method was used to determine the vertical divergence geometry of the diffraction peak to solve the problem of correcting the error. The Lorentz and other physical deviations of the peak method were verified based on experimental data. The standard error of the measured values of the lattice constant is only three parts per million, reaching a high degree of accuracy. The results were validated by the characteristic lines of different targets and the results were good. Due to the correction of the above-mentioned error correction problem, the accuracy has also reached a corresponding level, thus solving the single crystal method and polycrystalline silicon lattice constant method does not match the problem. Analysis and experimental data show that the lattice constant of the crystal with good symmetry and high crystallinity can be measured with ordinary diffractometer and unilateral peak localization method with accuracy and accuracy up to four parts per million.