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Process for the manufacture of shaped articles from reaction- bonded silicon nitride by nitridation under elevated nitrogen gas pressure

机译:在升高的氮气压力下通过氮化由反应结合的氮化硅制造成型制品的方法

摘要

The invention is a process for the manufacture of shaped articles of reaction-bonded silicon nitride in which pre-shaped articles of silicon powder are heated in a first stage under a nitrogen gas pressure of at least 6 MPa at a heating rate of not more than 50° C. per hour to a reaction temperature below the melting point of silicon, the article is maintained at the reaction temperature for at least 0.5 hours and subsequently, in a second stage, heating the article at a heating rate of at least 500° C. per hour to a temperature above the melting point of silicon and maintaining the article at that temperature for from 1 to 7 hours. The process can nitridate both pre-shaped articles consisting of silicon powder and, optionally, up to 15% by weight Si.sub. 3 N.sub.4 powder and those containing up to 10% by weight of a sintering aid such as Y.sub.2 O.sub.3. In the former case, porous shaped articles having a density of from 87 to 91% TD and, in the latter case, dense shaped articles having a density of more than 98% TD, are obtained. In all cases, in a total nitridation time of less than 15 hours, a conversion of at least 95% of the silicon originally present into silicon nitride is achieved, which, in the finished shaped article, is substantially in the . beta.-modification.
机译:本发明是一种制备反应结合氮化硅的成型制品的方法,其中在第一阶段中,在至少6MPa的氮气压力下,以不高于200℃的加热速率加热硅粉的预成型制品。以每小时50℃的速度加热至低于硅熔点的反应温度,将制品在反应温度下保持至少0.5小时,随后在第二阶段中以至少500℃的加热速率加热制品每小时将其加热到高于硅熔点的温度,并将制品在该温度下保持1至7小时。该方法可以氮化由硅粉和任选地至多15重量%的Si组成的预成型制品。 3 N.sub.4粉末和含有不超过10%重量的烧结助剂(例如Y.sub.2 O.sub.3)的粉末。在前一种情况下,可获得密度为87-91%TD的多孔成形制品,在后一种情况下,可获得密度为TD大于98%的致密成形制品。在所有情况下,在少于15小时的总氮化时间内,至少存在最初存在的95%的硅转化为氮化硅,这在成品成型制品中基本上处于。 beta-修改。

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