首先采用溶液燃烧法和纯氢还原法制备W纳米粉末,以钼酸铵(NH4)6Mo7O24·4H2O为前驱体。粉末在单轴力下进行压制。烧结实验在高纯氢气气氛中进行,采用了两种不同的加热方案:(i)恒定加热速率烧结,即在不保温的情况下,以5 ℃/min的速度将坯体加热至预设温度(1100-1600℃),然后以10 ℃/min的速度冷却至室温。这些实验用于研究烧结动力学,并寻找合适的第一步烧结条件以优化两步烧结;(ii)两步烧结,将生坯加热至T1,然后冷却至T2并长时间保温。样品的断口在FEI Quanta650场发射扫描电镜下进行观测。使用配备电子背散射衍射(EBSD、AZtec系统、牛津仪器)的场发射枪扫描电子显微镜(FE-SEM、JIB 4600F)对微观结构进行表征。
First, the solution combustion method and the pure hydrogen reduction method are used to prepare W nano-powder, with ammonium molybdate (NH4)6Mo7O24·4H2O as the precursor. The powder is compressed under uniaxial force. The sintering experiment was carried out in a high-purity hydrogen atmosphere, and two different heating schemes were used: (i) Constant heating rate sintering, that is, the green body is heated to the preset temperature at a rate of 5 ℃/min without holding the temperature. (1100-1600°C), then cool to room temperature at a rate of 10°C/min. These experiments are used to study the sintering kinetics and to find suitable first-step sintering conditions to optimize the two-step sintering; (ii) Two-step sintering, heating the green body to T1, then cooling to T2 and holding it for a long time. The fracture of the sample was observed under the FEI Quanta650 field emission scanning electron microscope. A field emission gun scanning electron microscope (FE-SEM, JIB 4600F) equipped with electron backscatter diffraction (EBSD, AZtec system, Oxford Instruments) was used to characterize the microstructure.