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本文利用EM400T透射电子显微镜和EDAX9100能谱仪研究微量元素在晶界的偏聚。通过本文采用的电子束直径小到40A的微探针,低背底样品台,沿晶界拉长束斑,分段积分等措施,明显地提高了分析灵敏度。用这种方法测量了含磷820ppm的Si-Mn高强度钢和含镁94ppm的GH169高温合金中P和Mg的晶界偏析,测出含P820ppm钢的晶界区含P量为0.46%,经计算后相当晶界含P量为2.3%,而用俄歇谱仪测出晶界含P量为1.2~3.9%。同样测出含P160ppm钢的晶界含P量为1.5%。对含Mg94ppm的GH169高温合金,测出晶界含Mg量为1.8%,而含MC型炭化物的晶界含Mg量更高,达4%。
In this paper, EM400T transmission electron microscopy and EDAX9100 spectrometer to study the segregation of trace elements in the grain boundary. The sensitivity of this method is obviously improved by using micro-probe with electron beam diameter as small as 40A, low back sample stage, beam spot spreading along the grain boundaries and segmental integral. The grain boundary segregation of P and Mg in Si-Mn high-strength steel containing 820 ppm phosphorus and 94 ppm high-temperature magnesium alloy containing 94 ppm of phosphorus was measured by this method. The P content in the grain boundary region containing P820 ppm steel was measured to be 0.46% Calculated after the equivalent grain boundary P content of 2.3%, and measured by Auger spectroscopy P content of grain boundaries of 1.2 to 3.9%. Also measured with P160ppm steel containing P content of 1.5%. For the GH949 superalloy containing Mg94ppm, the content of Mg in the grain boundaries was found to be 1.8%, while the content of Mg in the grain boundaries containing MC-type carbides was higher, reaching 4%.