一种​碳化硅​纳米​管​的​制备​方法

源语言标题
(CN105217634B) 一种​碳化硅​纳米​管​的​制备​方法
公开号/公开日
CN105217634 A 2016-01-06 [CN105217634]CN105217634 B 2017-08-01 [CN105217634B] / 2016-01-062017-08-01
申请号/申请日
2015CN-0511864 / 2015-08-19
发明人
MA JIANFENG;LIU QING;YAO CHAO;
申请人
CHANGZHOU UNIVERSITY;
主分类号
IPC分类号
B82Y-030/00B82Y-040/00C01B-032/97
摘要
(CN105217634B) 本​发明​公开​种​碳化硅​纳米​管​的​制备​方法,包括​以下​步骤:在​水浴​下向​埃洛​石​的​悬浊液​中​滴​加​八​烷基​三甲​基​溴​化​铵​溶液,滴​加​完毕​后再​滴​加​丙酮,滴​加​完毕​后于​相同​条件下​继续​搅拌,最后​离心​分离,洗涤​烘干​并​研磨;将​粉末​置于​管​式​炉​中通​N​保护​下​碳化,将​碳化​后的​固体物​放入​瓶中,加入​盐酸​溶液,搅拌,固​液​分离,洗涤,烘干;将​得到​的​颗粒​置于​管​式​炉​中,在​氩气​保护​下,程序​升温​煅烧​后​冷却​至​室温,将​煅烧​的​产物​浸泡​于​氢氟酸​与​盐酸​的​混合​酸​中,清洗掉​未​反应​二氧化硅,用去​离子水​洗涤​烘干,得到​碳化硅​纳米​管。该​方法​以​埃洛​石​中的​硅​为​原材料,充分​利用​埃洛​石​的​管状​结构,原料​来源​廉价,过程​可控,易于​实现​工业化生产。
地址
代理人
代理机构
;
优先权号
2015CN-0511864 2015-08-19
主权利要求
(CN105217634B) 1. One method for producing a silicon carbide nano-tubes, characterized in that in turn comprises the following steps: At (1) 60-65 Ć under a water bath containing added dropwise to a suspension containing 10g halioysite 8-16mmol eight-methyl ammonium bromide solution, eight-methyl ammonium bromide solution has a concentration of 1-4 mol/L, stirring was continued during the addition, the addition was complete re-dropped after acetone 7-9 ml, after the addition was complete stirring was continued under the same conditions 2-3h, centrifuged, washed with deionized water the resulting solid 4-5 times, 100-105 Ć under drying, the solids were milled 50-80 mesh powder, in which the cationic surfactant through electrostatic interaction during as single molecules are fixed to the halioysite surface; The powder was (2) placed in a tube furnace with N2 protection, at 500-800 Ć carbonized at 4-6h, for a further pass N2 cooled to room temperature, the organics are high temperature carbonization, carbonaceous layer formed on the surface of the halloysite; The solids of the (3) carbonized after 2-4g placed in a bottle, add 10-15 ml concentration of 20-40% of hydrochloric acid solution, stirred for 20-30h, dissolved in the alumina structure halioysite, solid-liquid separation, washed with deionized water, 60-70 Ć thermostatic drying 5-6h, to obtain binding particles coated with carbon to silicon carbon layer of silicon oxide; Binding particles in the carbon to silicon will (4) be placed in a tube furnace, under an argon atmosphere, at a temperature raising rate of 10-15 Ć/min was heated to 600 Ć, thermostat 60-120min, further increasing the temperature, rate of 10-15 Ć/min, temperature was raised to 1400-1500 Ć, thermostat 240-360min, the temperature is decreased to 300-400 Ć, vented to atmosphere, calcined 60-120min, cooled to room temperature, immersed in hydrofluoric acid and hydrochloric acid of the calcined product in a mixed acid, hydrofluoric acid and hydrochloric acid in a molar ratio of 0.5-10: 1, mixed acid treatment time of 4-24h, washing away unreacted silica, with deionized water until pH=7 after, 80-105 Ć drying, to obtain silicon carbide nanotube.
法律状态
(CN105217634B) LEGAL DETAILS FOR CN105217634  Actual or expected expiration date=2035-08-19    Legal state=ALIVE    Status=GRANTED     Event publication date=2015-08-19  Event code=CN/APP  Event indicator=Pos  Event type=Examination events  Application details  Application country=CN CN201510511864  Application date=2015-08-19  Standardized application number=2015CN-0511864     Event publication date=2016-01-06  Event code=CN/A  Event type=Examination events  Published application  Publication country=CN  Publication number=CN105217634  Publication stage Code=A  Publication date=2016-01-06  Standardized publication number=CN105217634     Event publication date=2016-01-06  Event code=CN/C06  Event indicator=Pos  Event type=Examination events  Publication    Event publication date=2016-02-03  Event code=CN/C10  Event type=Examination events  Request of examination as to substance    Event publication date=2017-08-01  Event code=CN/B  Event indicator=Pos  Event type=Event indicating In Force  Granted patent for invention  Publication country=CN  Publication number=CN105217634  Publication stage Code=B  Publication date=2017-08-01  Standardized publication number=CN105217634B     Event publication date=2017-08-01  Event code=CN/GR01  Event indicator=Pos  Event type=Event indicating In Force  PATENT GRANT
专利类型码
AB
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