LCD溅射靶材用大尺寸钼板工艺、组织、织构与性能研究

RESEARCH ON TECHNOLOGY,MICROSTRUCTURE,TEXTURE AND PROPERTIES OF LARGE-SIZED MOLYBDENUM PLATE TO PRODUCE LCD SPUTTERING TARGET

进行了烧结、轧制工艺对比试验,研究了粉末粒度、形貌和烧结工艺对大型钼烧结板坯组织和性能的影响;轧制方式对LCD溅射靶材用大尺寸钼板微观组织、织构以及性能的影响,探讨了影响LCD溅射靶材用大尺寸钼板组织、织构及性能的主要因素。结果表明:制备大型烧结钼板坯可选用颗粒大小较为均匀、分布疏松、粗细搭配合理的中等粒度钼粉;相比普通钼板坯而言,通过延长保温时间,1 900℃高温氢气中频烧结,可制备轧制大尺寸钼靶材用大型钼板坯;LCD溅射靶材用大尺寸钼板轧制总加工率需大于70%;采用1火次多道次单向轧制工艺,正常轧制的LCD溅射靶材用长条形钼板再结晶退火后可得到均匀细小的等轴晶粒组织;由于纵向开坯轧制阶段的不均匀变形(非正常轧制),导致包覆横轧得到的LCD溅射靶材用宽幅矩形钼板再结晶退火后组织不均匀,细晶粒和粗大晶粒并存;单向正常轧制的LCD溅射靶材用长条形钼板再结晶退火后近表层无明显优先织构取向。纵向开坯轧制,然后用包覆换向横轧得到的LCD溅射靶材用宽幅钼板再结晶退火后近表层存在较强的{0,0,1}<1,-1,0>、{0,0,1}<6,-1,0>和{0,1,1}<1,0,0>织构。

The comparing experiments of sintering and rolling about large - sized molybdenum plate to produce LCD sputtering target have been carried out . The influences of molybdenum powder particle size, morphology and sintering process parameters on the microstructure and properties of large sintering slab were studied initially. Then the influences of rolling methods on the microstructure, texture and properties of large - sized molybdenum plate to produce LCD sputtering target have been investigated emphatically. The main factors affecting the microstructure, tex- ture and properties of large - sized molybdenum plate to produce LCD sputtering target have been analyzed . The results show that the medium - size molybdenum powder is aslo suitable for production of large sintering slab, but the powder particle size should be relatively uniform, its distribution is loose , and also its large particle and small particle are collocated reasonably. Compared with common molybdenum sintering slab , the large sintering slab can be obtained using medium -frequency induction sintering method in hydrogen atmosphere at 1 900 ~C. The general rolling deformation rate of large - sized molybdenum plate to produce LCD sputtering target should be greater than 70%. Adopting one heat multi -pass rolling process （only longitudinal rolling） , the recrystallized mierostructure of elongated molybdenum plate to produce LCD sputtering target is fine equiaxed grains normally. But, Adopting case transverse rolling after longitudinal cogging process, the recrystallized microstructure of wide rectangular molybdenum plate to produce LCD sputtering target is not uniform. In the other words, fine grains and coarse grains coexist. The possible reason is that inhomogeneous deformation is produced because of abnormal rolling in longitu-dinal cogging stage. There is no obvious priority texture near the surface of large elongated molybdenum plate after recrystallization annealing. But, the main texture components near the surface of wide rectangular molybdenum plate are{0,0,1} 〈1,-1,0〉,{0,0,1} 〈6,-1,0〉 and {0,1,1} 〈1,0,0〉 textures.