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Process for the production of Pb.sub.x Mo.sub.y S.sub.z Chevrel- phase compounds

机译:制备Pb.sub.Mo.sub.z Chevrel相化合物的方法

摘要

A process for the production of at least a one kilogram block of Chevrel-phase Pb.sub.x Mo.sub.y S.sub.z, wherein x=0.9 to 1.2, y=6.0 to 6. 4, and z=7 to 8, includes mixing thoroughly stoichiometric quantities of starting materials in powdered form. The starting materials are selected from elemental Pb, Mo and S, sulfides of elemental Pb and Mo, and mixtures thereof. The starting mixture is introduced into a metallic container and evacuated to a pressure to 10.sup.4 Pa or less. The evacuated container is subjected to hot isostatic pressing at a constant pressure selected from a pressure ranging from 100 to 300 MPa, at a heating rate ranging from 10° to 100° C./hr., at a final pressing temperature ranging from 800° to 1200° C., and for a pressing period ranging from 10 to 100 hours, whereby the starting materials react to form the block of Chevrel-phase Pb.sub.x Mo.sub.y S. sub.z. The block is cooled at a cooling rate ranging from 50° to 500° C./hr. while maintaining the constant pressure. The process may include the further steps of filling the metallic container after evacuation with an inert gas; re-evacuating the metallic container to remove the inert gas; and heating the metallic container after re- evacuation at a temperature ranging up to but less than 300°, prior to subjecting the metallic container to hot isostatic pressing.
机译:一种生产至少一公斤的雪佛尔相Pb x Mo y S z的方法​​,其中x = 0.9至1.2,y = 6.0至6。4,z =图7至8的实施方式包括将化学计量的量的原料以粉末形式充分混合。起始原料选自元素Pb,Mo和S,元素Pb和Mo的硫化物及其混合物。将起始混合物引入金属容器中并抽空至10.Pa.4 Pa或更低的压力。在从100至300MPa的压力中选择的恒定压力下,以10℃至100℃/ hr的加热速率,在800℃的最终压制温度下对抽空的容器进行热等静压。到1200℃,并持续10至100小时的压制时间,由此起始材料反应形成Chevrel相Pb x Mo y S.z.的嵌段。该块以50℃至500℃/小时的冷却速率冷却。同时保持恒定的压力。该方法可以包括在抽空后用惰性气体填充金属容器的其他步骤;以及重新排空金属容器以去除惰性气体;在对金属容器进行热等静压之前,请先将其抽真空后再加热至不超过300°C的温度。

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