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公开(公告)号：US5441694A
公开(公告)日：1995-08-15
申请号：US258035
申请日：1994-06-10
IPC分类号： C01B21/068 , B22F1/00
CPC分类号： C01B21/0682 , C01P2004/62
摘要： In a method for preparing a high .alpha.-type silicon nitride powder by adding to and mixing with metallic silicon powder a copper catalyst and nitriding the mixture in a non-oxidizing gas atmosphere containing nitrogen or ammonia at 1,000.degree. to 1,500.degree. C., the amount of copper catalyst is limited to from 0.05 % to less than 0.5 % by weight of copper based on the weight of the metallic silicon. There is obtained silicon nitride powder of high purity at low cost and high efficiency since the copper catalyst can be efficiently removed from the silicon nitride powder through conventional acid treatment.
摘要翻译： 在通过在金属硅粉末中加入和混合铜催化剂并在1000℃至1500℃下在含有氮或氨的非氧化性气体气氛中氮化该混合物的方法中制备高α型氮化硅粉末的方法， 基于金属硅的重量，铜催化剂的量限制在0.05至小于0.5重量％的铜。 由于可以通过常规的酸处理从氮化硅粉末中有效地除去铜催化剂，所以以低成本和高效率获得了高纯度的氮化硅粉末。
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公开(公告)号：US5210250A
公开(公告)日：1993-05-11
申请号：US935797
申请日：1992-08-27
申请人： Isao Watanuki , Hiroshi Tsumura , Nobuhiko Kodana , Kazushi Satoh , Masanori Fukuhira , Hidehiko Aonuma
发明人： Isao Watanuki , Hiroshi Tsumura , Nobuhiko Kodana , Kazushi Satoh , Masanori Fukuhira , Hidehiko Aonuma
摘要： A simple but very effective and reliable method is proposed for the decolorizing purification of a halogenated silane compound, e.g., methyl trichlorosilane, colored by containing a very small amount of heavy metal impurities such as iron. The method comprises: contacting the halogenated silane compound with a small amount of a cationic surface active agent which is solid and insoluble in the silane such as a quaternary ammonium salt, e.g., trimethyl octadecyl ammonium chloride, for 2 to 240 minutes; and then separating the silane compound from the cationic surface active agent.
摘要翻译： 提出了一种简单但非常有效和可靠的方法，用于通过含有非常少量的重金属杂质如铁来着色的卤代硅烷化合物，例如甲基三氯硅烷的脱色纯化。 该方法包括：将卤代硅烷化合物与少量固体并不溶于硅烷如阳离子表面活性剂如季铵盐如三甲基十八烷基氯化铵接触2至240分钟; 然后将硅烷化合物与阳离子表面活性剂分离。
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公开(公告)号：US5573689A
公开(公告)日：1996-11-12
申请号：US594156
申请日：1996-01-31
IPC分类号： B01J8/18 , B01J8/24 , C01B21/06 , C01B21/064 , C01B21/068 , C01B21/072 , C04B35/584 , F27B15/00 , F27B5/14
CPC分类号： C04B35/584 , B01J8/1836 , B01J8/1872 , C01B21/06 , C01B21/0641 , C01B21/0682 , C01B21/0722
摘要： In a fluidized bed reactor for preparing a metal nitride by feeding metal powder and a non-oxidizing gas containing N.sub.2 or NH.sub.3 into a reaction tube (1) to form a fluidized bed (2) therein and heating the fluidized bed for nitriding the metal powder, an envelope (11) encloses the reaction tube (1) for preventing the surrounding air from entering the reaction tube. A heater (9) is disposed outside the envelope (11) for heating the fluidized bed (2) to 1,200.degree. C. or higher. The envelope prevents penetration of the surrounding air into the reaction tube and also prevents deterioration of the heater and surrounding components by scattering of metal fines. The reactor ensures safe operation to prepare metal nitride powder of high purity on an industrial scale.
摘要翻译： 在用于通过将金属粉末和含有N 2或NH 3的非氧化气体进料到反应管（1）中以在其中形成流化床（2）而制备金属氮化物的流化床反应器中，并加热流化床以使金属粉末渗氮 ，封套（11）包围用于防止周围空气进入反应管的反应管（1）。 将加热器（9）设置在用于将流化床（2）加热到1200℃以上的外壳（11）的外侧。 外壳防止周围空气渗透到反应管中，并且还防止加热器和周围部件由于金属细粉的散射而变质。 反应器确保安全操作，以工业规模制备高纯度的金属氮化物粉末。
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4.发明授权Preparation of silicon nitride powder by partially nitriding in a fluidized bed and then completing nitridation in a moving bed 失效通过在流化床中部分硝化制备氮化硅粉末，然后在移动床中完成氮化
公开(公告)号：US5232677A
公开(公告)日：1993-08-03
申请号：US647142
申请日：1991-01-29
IPC分类号： C01B21/068
CPC分类号： C01B21/0682
摘要： Silicon nitride powder is produced in two steps, by supplying metallic silicon powder to a fluidized bed composed of silicon nitride and nitrogen or ammonia gas where primary nitriding reaction is effected until the silicon powder is nitrided to an amount of at least 50% and transferring the nitrided product from the fluidized bed into a moving bed where secondary nitriding reaction is effected for nitriding the unreacted silicon with nitrogen or ammonia gas. This method is adapted for manufacture on a commercial scale because the silicon nitride powder thus obtained is consistent and has a very high degree of nitriding and a minimal variation in quality.
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公开(公告)号：US5817285A
公开(公告)日：1998-10-06
申请号：US759378
申请日：1996-12-04
IPC分类号： C01B21/068
CPC分类号： C01B21/0682
摘要： Silicon nitride powder is continuously prepared by feeding metallic silicon powder into a fluidized bed comprising silicon nitride powder and nitrogen or ammonia gas and discharging a nitrided product from the fluidized bed. The metallic silicon powder is pretreated at a temperature of 1,000.degree.-1,400.degree. C. under a vacuum of 0.001-100 Torr before it is subject to nitriding reaction.
摘要翻译： 通过将金属硅粉末进料到包含氮化硅粉末和氮气或氨气的流化床中并从流化床排出氮化产物来连续制备氮化硅粉末。 金属硅粉末在氮化反应之前，在1000-100乇的真空下，在1000°-1,400℃的温度下进行预处理。
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公开(公告)号：US5456896A
公开(公告)日：1995-10-10
申请号：US273829
申请日：1994-07-12
IPC分类号： C01B21/068
CPC分类号： C01B21/0682
摘要： Silicon nitride powder is prepared by nitriding metallic silicon powder in a nitriding gas atmosphere at a temperature of 1,000.degree. C.-1,500.degree. C. Midway the nitriding step, the nitrided product is heat treated in an inert non-oxidizing gas atmosphere or vacuum at a temperature higher than the nitriding temperature, but lower than 1,600.degree. C. The product is nitrided again, obtaining high .alpha.-content silicon nitride powder.
摘要翻译： 氮化硅粉末通过在氮化气体气氛中在1000℃-1,500℃的温度下氮化金属硅粉末制备。在氮化步骤的中途，氮化产物在惰性非氧化性气体气氛或真空中进行热处理 温度高于氮化温度，但低于1600℃。产物再次氮化，获得高含量的氮化硅粉末。
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公开(公告)号：US5073358A
公开(公告)日：1991-12-17
申请号：US557572
申请日：1990-07-24
IPC分类号： C01B21/068
CPC分类号： C01B21/0682
摘要： Silicon nitride powder is prepared by continuously supplying metallic silicon powder to a first fluidized bed which is composed of silicon nitride powder and a non-oxidizing reaction gas containing nitrogen or ammonia gas and maintained at 1,000.degree. to 1,400.degree. C. where primary nitriding reaction takes place, and continuously withdrawing the nitride product from the first fluidized bed and supplying it to a second fluidized bed of similar composition where secondary nitriding reaction takes place for nitriding the unreacted metallic silicon powder.
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