称取一定量的工业钼粉,放入行星式球磨机中,在氩气保护下球磨24 h,每球磨1 h停机8~10 min,同时改变球磨机转动方向,球料比为10:1;球磨转速为350 r/min,所得钼粉标记为Mo-350r,未球磨的钼粉用Mo表示。采用单向液压压制粉末,压力为300 MPa,不添加成型剂。将压坯置于箱式炉中于氢气氛围下进行烧结,温度区间为1200~1600 ℃,升温速率从室温至1000 ℃为10 ℃/min,1000 ℃至1500 ℃为5 ℃/min升温,1500 ℃至1600 ℃为2 ℃/min,保温时间为2 h,降温与升温速率相同,降温至700 ℃后随炉自然冷却。使用XRD对粉末进行物相分析,步长8°/min,范围10~90°。用阿基米德排水法测试烧结坯的密度(钼的理论密度为10.2 g/cm3),计算其相对密度;采用维氏硬度计测试硬度,取3个点的平均值;使用扫描电镜观察微观形貌;利用线截距法来测量平均晶粒尺寸;采用电感耦合等离子发射光谱仪(ICAP7400 Radial)测试Fe含量。
A certain amount of industrial molybdenum powder was weighed, put into a planetary ball mill, and ball milled for 24 h under argon protection, with 8~10 min stopping for each 1 h of ball milling, while changing the rotation direction of the ball mill, with a ball-to-material ratio of 10:1; the ball milling speed was 350 r/min, and the resulting molybdenum powder was marked as Mo-350r, and the unball-milled molybdenum powder was expressed as Mo. The powder is pressed by unidirectional hydraulic pressure of 300 MPa without adding forming agent. The pressed billet was sintered in a chamber furnace under hydrogen atmosphere at a temperature range of 1200-1600 ℃, with a heating rate of 10 ℃/min from room temperature to 1000 ℃, 5 ℃/min from 1000 ℃ to 1500 ℃, and 2 ℃/min from 1500 ℃ to 1600 ℃, with a holding time of 2 h. The cooling temperature was the same as the heating rate, and then cooled naturally with the furnace after cooling down to 700 ℃. The temperature was reduced to 700 ℃ and then cooled naturally. The powder was analyzed by XRD with a step size of 8°/min and a range of 10~90°. The density of the sintered billet (theoretical density of molybdenum is 10.2 g/cm3) was tested by Archimedes drainage method to calculate its relative density; the hardness was tested by Vickers hardness tester and the average value of three points was taken; the microscopic morphology was observed by scanning electron microscopy; the line intercept method was used to measure the average grain size; and the Fe content was tested by inductively coupled plasma emission spectrometer (ICAP7400 Radial).