利用粉末冶金法制得了板型规整的纯钼烧结坯,在Gleeble-1500型热模拟实验机上对纯钼板坯进行热压缩变形实验,变形温度为1100°C~1300 °C、变形速率为0.01~10 s-1、真应变为0.3~0.6。将线切割得到的截面试样使用金相镶样机进行镶嵌,先用粗砂纸打磨至表面平整、无明显切割痕迹,然后使用不同粒度金相砂纸打磨、机械抛光至表面光洁无明显划痕。使用Murakami腐蚀剂(铁氰化钾:氢氧化钠:水为1:1:10)腐蚀60 s左右,腐蚀之后用酒精擦洗吹干,利用电子背散射衍射(EBSD)技术分析变形后纯钼微观组织、再结晶晶粒、大小角度晶界和取向角等变化。将样品在电压为20 V,温度为20 °C,电解液为H2SO4: CH3OH为12: 88的混合溶液电解抛光。
A pure molybdenum sintered compact with a regular plate shape was prepared by powder metallurgy. The pure molybdenum slab was subjected to a thermal compression deformation experiment on the Gleeble-1500 thermal simulation test machine. The deformation temperature was 1100°C~1300°C, and the deformation rate was 0.01~ 10 s-1, the true strain is 0.3 to 0.6. The cross-section samples obtained by wire cutting are inlaid with a metallographic inlay machine, first polished with coarse sandpaper to a smooth surface without obvious cutting marks, and then polished with metallographic sandpaper of different grain sizes and mechanically polished to a smooth surface without obvious scratches. Use Murakami etchant (potassium ferricyanide: sodium hydroxide: water 1:1:10) to corrode for about 60 s. After corrosion, use alcohol to scrub and blow dry, and use electron backscatter diffraction (EBSD) technology to analyze the microstructure of pure molybdenum after deformation , Recrystallized grains, size and angle of grain boundaries and orientation angle changes. The sample was electropolished at a voltage of 20 V, a temperature of 20 °C, and a 12:88 mixed solution of H2SO4: CH3OH as the electrolyte.