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    • 10. 发明授权
    • Method for making submicrometer transition metal carbonitrides
    • 亚微米过渡金属碳氮化物的制备方法
    • US5756410A
    • 1998-05-26
    • US807165
    • 1997-02-27
    • Stephen D. DunmeadAlan W. Weimer
    • Stephen D. DunmeadAlan W. Weimer
    • C04B35/56C01B21/082C01G41/00C04B35/58C01B21/00
    • B82Y30/00C01B21/0828C01P2004/61C01P2004/62C01P2004/64
    • A submicrometer transition metal carbonitride is produced having the formula: M.sub.a M'.sub.b M".sub.(1-a-b) (C.sub.1-x) N.sub.x).sub.z wherein M is Ti, Zr or Hf; M' is V, Nb or Ta; M" is Cr, Mo or W; a ranges from 0 to 1; b ranges from 0 to 1 with the proviso that (a +b) is less than or equal to 1; x ranges from about 0.02 to about 0.95 and z ranges from about 0.9 to about 2. The transition metal carbonitride is produced by mixing (a) a transition metal oxide source of a transition metal in the above formula and (b) a carbon source such as carbon black. This mixture is heated at a rate of between about 100K/sec to about 100,000,000K/sec in a nitrogen containing non-oxidizing gas such as nitrogen or nitrogen mixed with argon to an elevated temperature that makes carbothermal reduction of the transition metal oxide source thermodynamically favorable for a residence time sufficient to convert the transition metal oxide source into at least one product selected from the group consisting of (i) a transition metal carbonitride and (ii) a transition metal carbonitride precursor. The product may be exposed to a finishing step involving heating the product to a temperature less than the elevated temperature in a finishing atmosphere such as nitrogen, hydrogen, inert gas or combinations thereof to form submicrometer carbonitrides of higher purity or different stoichiometry.
    • 制备亚微米过渡金属碳氮化物,其具有下式:MaM'bM“(1-a-b)(C1-x)Nx)z,其中M是Ti,Zr或Hf; M'为V,Nb或Ta; M“是Cr,Mo或W; a范围从0到1; b的范围为0至1,条件是(a + b)小于或等于1; x的范围为约0.02至约0.95,z的范围为约0.9至约2.过渡金属碳氮化物通过将(a)过渡金属的过渡金属氧化物源与上述式(b)中的碳源 作为炭黑。 将这种混合物在氮气或氮气混合的含氮非氧化性气体的氮气中以约100K /秒至约100,000,000K /秒的速率加热至高温,从而使过渡金属氧化物源热力学地进行碳热还原 有利于将过渡金属氧化物源转化成选自(i)过渡金属碳氮化物和(ii)过渡金属碳氮化物前体中的至少一种产物的停留时间。 该产品可能暴露于整理步骤,包括在最终气氛例如氮气,氢气,惰性气体或其组合中将产品加热至低于升高温度的温度,以形成更高纯度或不同化学计量的亚微米碳氮化物。