以钨酸钠和硝酸铜为原料,通过水热合成反应及550℃/1.5 h焙烧得到氧化钨铜复合粉体,氢气还原后获得W-20%Cu复合粉体,采用X射线衍射(XRD)、扫描电镜(SEM)和高分辨透射电镜(HTEM),对该复合粉体的组织与结构进行表征。结果表明:采用水热合成法制备氧化钨铜的前驱体时混合溶液应调整为碱性,最好将pH值控制在9,水热反应产物主要是由CuWO4·2H2O与Cu2WO4(OH)2组成的复合络合物;550℃温度下焙烧时水热合成产物完全分解为由WO3、CuO和CuWO4-x组成的复合氧化物,粒度在2~5μm之间,分布均匀;复合氧化物在700~900℃下氢气还原成为典型的铜包钨结构的钨铜复合粉体,呈规则球形,晶粒度在70 nm左右,钨铜分布均匀,两相一体,保留了溶液中分子级的混合状态。
The W-Cu oxide precursor composite powders were fabricated by hydrothermal synthesis method and 550 ℃/1.5 h calcination using sodium tungstate and copper nitrate as raw materials, and the W-20%Cu composite powders were obtained through hydrogen reduction. The microstructures of the prepared powders were characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM) and high-resolution transmission electron microscopy(HTEM). The results show that the mixed solution should be adjusted for alkaline; pH value should be controlled at 9 when the W-Cu oxide precursor is prepared by hydrothermal synthesis method. The hydrolyzates are mainly consist of CuWO4·2H2O and Cu2WO4(OH)2, and can be completely decomposed into the oxide composite powders composed of WO3, CuO and CuWO4-x when calcinating at 550 ℃. The oxide composite powders particles distribute uniformly, and the particle size is about 2~5 μm. Moreover, W-Cu composite powders can be reduced at 700~900 ℃. The morphology of the W-Cu powders shows the typical structure of tungsten covered by copper, the partcle size of the composite powders is around 70 nm. W-Cu composite powder particle presents sphericity, W and Cu elements distribute uniformly, express two phases integration and retain the molecular level of mixed state in the solution.