Abstract:The nanoscale precipitated phases play the role of precipitation strengthening in steel. They are also used as the inhibitor of grain growth to obtain microstructure with specific orientation. Therefore, the systemically analysis of precipitated phases is very important. At present, the statistical analysis of precipitated phases with size less than 50 nm was hardly realized by scanning electron microscope(SEM) and transmission electron microscope(TEM). In the study, the Feature software package in SEM for statistic of inclusions was applied to the energy spectrum control software of TEM, realizing the direct statistical analysis of nanoscale precipitated phases in steel by TEM. Meanwhile, the main factors influencing on the statistical analysis of precipitated phases by TEM, such as sample preparation method, acquisition parameter, classification method and large-area statistic method, were systemically studied. The results showed that the optimal experimental conditions were as follow: the new complex method was adopted for sample preparation; the single-point acquisition time of energy spectrum was 5 s; the image resolution was 2 048; the continuous map collecting statistics mode was adopted; the terminal condition was that when the statistical quantity of precipitated phases exceeded 100. The detailed implementation method for classification rules of precipitated phases was obtained. Combining the experimental statistic results of non-oriented electrical steels W800 and WH470, the type of precipitated phases was core-shell composite precipitation of CuS2 and MnS+CuS2. The minimum size of precipitated phases in statistical analysis by experimental method was 10 nm.
[1] Wang J Y,Ren Q,Luo Y,et al.Effect of non-metallic precipitates and grain size on core loss of non-oriented electrical silicon steels[J].Journal of Magnetism and Magnetic Materials,2018,451:454-462. [2] 朱爱玲,彭晟,张恒华,等.EH40 钢性能即析出相的研究[J].上海金属,2009,31(2):28-31. ZHU Ailing,PENG Sheng,ZHANG Henghua,et al.Property and precipitation behavior of EH40 steel[J].Shanghai Metals,2009,31(2):28-31. [3] 王波.高效率铁芯用低硅无取向电工钢的发展[J].金属功能材料,2004,11(2):24-29. WANG Bo.Development of low silicon non-oriented electrical steel for high-efficiency cores[J].Metallic Functional Materials,2004,11(2):24-29. [4] 崔桂彬,鞠新华,严春莲,等.钢中析出相场发射扫描电镜的自动统计分析技术研究[J].冶金分析,2019,39(2):17-22. CUI Guibin,JU Xinhua,YAN Chunlian,et al.Study on automatic statistical analysis technology of precipitated phased in steel by field emission scanning electron microscope[J].Metallurgical Analysis,2019,39(2):17-22. [5] 张淑兰,徐海峰,杜敏,等.扫描电镜夹杂物的影响因素探讨[J].冶金分析,2017,37(12):7-14. ZHANG Shulan,XU Haifeng,DU Min,et al.Discussion on the factors affecting the measurement of inclusions by scanning electron microscopy[J].Metallurgical Analysis,2017,37(12):7-14. [6] 马超,罗海文.扫描电镜和电解萃取法用于超洁净钢中夹杂物的表征[J].冶金分析,2017,37(8):1-8. MA Chao,LUO Haiwen.Characterization of inclusions in ultra-clean steel by scanning electron microscopy and electrolytic extraction[J].Metallurgical Analysis,2017,37(8):1-8. [7] 严春莲,尹立新,任群,等.钢中夹杂物扫描电镜自动统计分析结果的影响因素探讨[J].冶金分析,2018,38(8):1-10. YAN Chunlian,YIN Lixin,REN Qun,et al.Discussion on influencing factors in automatic statistical analysis of inclusions in steel by scanning electron microscopy[J].Metallurgical Analysis,2018,38(8):1-10. [8] 王顺兴,李延祥,高百宁.GCr15钢中碳化物尺寸统计分布规律的研究[J].理化检验(物理分册),1990,26(5):13-15. WANG Shunxing,LI Yanxiang,GAO Baining.The study on statistical distribution regularity of carbide size in GCr15 bearing steel[J].Physical Testing and Chemical Analysis(Part A:Physical Testing),1990,26(5):13-15. [9] 马红旭,李友国.硅钢中析出物的尺寸分布以及体积分数的测定[J].材料科学与工程,2002,20(3):328-330. MA Hongxu,LI Youguo.Measurement of size distribution and volume fraction of precipitates in silicon steel[J].Materials Science & Engineering,2002,20(3):328-330.