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用XRF对磁光新晶体生长前后分别进行了定量分析,并比较了不同的制样方法和分析方法。测试结果显示:熔片法比压片法准确度高,定量分析比半定量分析准确度高;通过定量分析对新晶体材料的标定,发现新晶体是非常接近化学计量比的单晶晶体生长过程;而当晶体生长失败后,能通过定量和半定量分析得到验证,说明采用定量方法更能够准确的对磁光晶体生长过程进行表征,而半定量分析则可以快速简便的筛选出晶体生长中失败的晶体材料。最后对定量分析结果的不确定度进行了分析和评定,计算出晶体材料中各元素Tb,Ga,Al的合成绝对标准不确定为0.2%~0.3%,扩展不确定为0.4%~0.6%,置信概率95%。
The XRF was used to quantitatively analyze the new magneto-optical crystals before and after their growth, and different preparation methods and analytical methods were compared. The results of the test show that the melting method is more accurate than the compression method and the quantitative analysis is more accurate than the semi-quantitative analysis. Through the quantitative analysis of the new crystal material, the new crystal is found to be very close to the stoichiometric single crystal growth process ; And when the crystal growth fails, can be verified by quantitative and semi-quantitative analysis shows that the use of quantitative methods can more accurately characterize the growth of magneto-optical crystals, and semi-quantitative analysis can quickly and easily filter out the growth of the crystal failed Crystalline material. Finally, the uncertainty of quantitative analysis is analyzed and evaluated. The absolute standard of synthesis of Tb, Ga and Al in crystalline materials is 0.2% -0.3%, 0.4% -0.6% Confidence 95% probability.