不同氧化物掺杂钼合金粉末的形貌变化  

Morphology Changes of Molybdenum Alloy Powders Doped with Different Oxides

作　　者：宋万里 徐流杰[1,2] 尚清毅 黄志民 SONG Wan-li;XU Liu-jie;SHANG qing-yi;HUANG Zhi-min(School of Materials Science and Engineering,Henan University of Science and Technology,Luoyang 471003,China;National Joint Engineering Research Center for Abrasion Control and Molding of Metal Materials,Henan University of Science and Technology,Luoyang 471003,China;Luoyang Quality Metrological Inspection and Testing Center,Luoyang 471003,China;China National R&D Center for Tungsten Technology,Xiamen Tlungsten Co.,Ltd.,Xiamen 361000,China)

机构地区：[1]河南科技大学材料科学与工程学院,河南洛阳471003 [2]河南科技大学金属材料磨损控制与成型技术国家地方联合工程研究中心,河南洛阳471003 [3]洛阳市质量计量检测中心,河南洛阳471003 [4]厦门钨业股份有限公司国家钨材料工程技术中心,福建厦门361000

出　　处：《稀有金属与硬质合金》2021年第1期40-47,共8页Rare Metals and Cemented Carbides

基　　金：国家自然科学基金(U1704152);长江学者和创新团队发展计划资助项目(IRT1234)。

摘　　要：以硝酸铝、硝酸镧、硝酸锆和四钼酸铵为主要原材料,通过水热合成法、低温煅烧和两段还原工艺分别制备出Al_(2)O_(3)、La_(2)O_(3)、ZrO_(2)三种氧化物掺杂钼粉。利用SEM、XRD、EDS等检测手段对各制备阶段下的粉末形貌和相结构进行分析。结果表明:在制备过程中,钼的演变过程为h-MoO_(3)→α-MoO_(3)→MoO_(2)→Mo,氧化物的掺杂对各阶段均有影响。将第二相悬浊液与h-MoO_(3)悬浊液混合后,由于各组悬浊液pH值不同,会造成混合液pH值不同,使六方微米柱结构的h-MoO_(3)出现不同程度的分解;煅烧过程中h-MoO_(3)晶型转变成为具有层状结构的α-MoO_(3),在第二相的作用下混合粉末中α-MoO_(3)表面有明显的片状结构;一段还原后粉末形貌均不规则,混合粉末中MoO_(2)颗粒尺寸较小,有明显的粘连现象;二段还原后Mo颗粒为近球状,第二相均可明显细化Mo颗粒,不同氧化物细化Mo颗粒的效果由强到弱依次为La_(2)O_(3)、ZrO_(2)、Al_(2)O_(3),其中La_(2)O_(3)细化效果最好,La_(2)O_(3)掺杂Mo颗粒平均尺寸可达1μm。With Al(NO_(3))_(3),La(NO_(3))_(3),Zr(NO3)4 and(NH4)2Mo4O13 as raw materials, the Al_(2)O_(3),La_(2)O_(3) and ZrO_(2) doped molybdenum powders were prepared by hydrothermal synthesis, low temperature calcination and two-stage reduction processes.SEM,XRD,EDS and other detection methods were used to analyze the morphology and phase structure of the powders in each preparation stage.The results show that the evolution of molybdenum in the preparation process is h-MoO_(3)→α-MoO_(3)→MoO_(2)→Mo, and the doping of oxides has influence on each stage.The pH value of the mixture is different due to the different pH value of each group after the second phase suspension is mixed with h-MoO_(3) suspension, which results in the decomposition of h-MoO_(3) with the hexagonal micron column structure to different degrees.The crystal form of h-MoO_(3) transforms into α-MoO_(3) with layered structure during calcination, the surface of α-MoO_(3) in the mixed powder has obvious lamellar structure under the action of the second phase.The morphology of the powder is irregular and MoO_(2) particles in the mixed powder have small size and obvious adhesion after the primary reduction.Mo particles are nearly spherical and the second phase can obviously refine Mo particles after the two-stage reduction.The effects of different oxides to refine Mo particles are La_(2)O_(3),ZrO_(2) and Al_(2)O_(3) from strong to weak, among which La_(2)O_(3) has the best refining effect, and the average size of La_(2)O_(3)-doped Mo particles can reach 1 μm.

关 键 词：钼粉 水热合成 低温煅烧 两段还原 氧化物掺杂 粉末形貌 

分 类 号：TG146.412[一般工业技术—材料科学与工程]