CN1721583A - Process for preparing silicon carbide crystal whisker - Google Patents
Process for preparing silicon carbide crystal whisker Download PDFInfo
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- CN1721583A CN1721583A CN 200510042708 CN200510042708A CN1721583A CN 1721583 A CN1721583 A CN 1721583A CN 200510042708 CN200510042708 CN 200510042708 CN 200510042708 A CN200510042708 A CN 200510042708A CN 1721583 A CN1721583 A CN 1721583A
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Abstract
The present invention discloses silicon carbide crystal whisker preparing process and aims at preparing silicon carbide crystal whisker separated from residual carbon powder. The technological scheme is to use carbonized rice hull as both silicon source and carbon source to prepare silicon carbide crystal whisker via carbon fiber induction. The preparation process includes crushing rice hull, carbonizing rice hull at 650-700 deg.c in one first-opening-then-closing process, mixing with catalyst in certain weight ratio, loading the mixed material inside graphite crucible, arranging carbon fiber on the upper part of the mixed material, covering the crucible, setting the crucible inside vertical vacuum furnace with graphite heater, and growing silicon carbide crystal whisker on the carbon fiber white introducing argon for protection. The said process realizes the automatic separation of crystal whisker from residual carbon powder to obtain crystal whisker with high straight crystal rate.
Description
Technical field
The present invention relates to a kind of method for preparing silicon carbide whisker.
Background technology
The preparation of silicon carbide whisker is divided with the original state of raw material gas phase and two kinds of preparation methods of solid phase.Solid phase raw material method is to adopt different reaction raw materials, adds suitable catalyzer, reacts in protective atmosphere, obtains the silicon carbide whisker of different qualities specification.Because of this method is more suitable in batch process, institute thinks at present extensively employing.Prepare silicon carbide whisker with carbonization rice husk and just belong to a kind of of solid phase method.
Document " prepares silicon carbide whisker with rice husk, progress in materials science 1989No2 " introduced the Bai Chungen of Metal Inst., Chinese Academy of Sciences etc. with the carbonization rice husk ash and in super carbon black 1: 2 mixing by weight, use Fe, H respectively
3BO
3, NaCl makees catalyzer, at 1400 ℃～1600 ℃ mixtures of having produced silicon carbide whisker and residual carbon, behind the blowing air burn off carbon, obtains β-SiC whisker.
Document " silicon carbide whisker quality and influence factor; artificial lens journal 1996No4 " has been introduced the Han Min of Beijing Post-graduate Dept., China Mining Univ virtue etc., and to select silicon-dioxide, carbon black, rice husk for use be raw material, add proper catalyst, in hydrogen, argon gas or the two mixed atmosphere, be heated to 1500 ℃～1700 ℃, constant temperature burnt till in 4～6 hours, made the mixture of β-SiC whisker and resistates such as carbon black, through flotation separation, obtain silicon carbide whisker.
It is raw material that document " rice husk synthesizes β-SiC whisker and growth mechanism research, New Chemical Materials 1996No2 " has been introduced the charring rice husk of employings such as the Wang Qi of Beijing Post-graduate Dept., China Mining Univ treasured after impurity is removed in acid treatment, and a certain amount of SiO
2Or rice hull ash is adjusted the SiO in the raw material
2With the ratio of C, evenly add and make composite catalyst by oneself, temperature of reaction is 1600 ℃, and feeds Ar gas do protection gas, constant temperature burnt till material in 4 hours after separating purification, obtained β-SiC whisker.
Document " Chinese patent 92111736.1 " discloses a kind ofly produces the method for graphite coat of silicon carbide and β-SiC fine powder and β-SiC whisker with rice hulls, is to use the coking rice husk, or the burnt rice husk that utilizes rice husk power generating factory to burn, and presses SiO
2The weight ratio of/C is 60: 32～60: 35 batch mixings, with NaCl or Fe, H
3BO
3, NaCl makees catalyzer; adopt shaft furnace or high temperature graphitization kiln; space, top temperature remains on 1400～1450 ℃; bottom reaction material temperature remains on 1600～1700 ℃; feed hydrogen and make protection gas, be incubated 4～6 hours and obtain graphite coat of silicon carbide and β-SiC fine powder and β-SiC whisker.
Above-mentioned document prepares the method for silicon carbide whisker, complex process not only, and resultant is whisker and carbon and the mixture that burns till resistates, need de-carbon and resistates just can obtain silicon carbide whisker later on, this process be difficult to be separated thoroughly, and whisker mixes generation with powder, occurs the bent crystal easily, so just influenced the quality of silicon carbide whisker, the whisker quality can not get guaranteeing.
Summary of the invention
In order to overcome the prepared silicon carbide whisker of prior art is whisker and carbon and the mixture that burns till resistates, need de-carbon and resistates just can obtain the deficiency of silicon carbide whisker later on, improve the quality of whisker, the invention provides a kind of method for preparing silicon carbide whisker, adopt carbon fiber to induce direct generation silicon carbide whisker.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method for preparing silicon carbide whisker is characterized in that following step:
1) with clear water with the rice husk washes clean, oven dry under 80～100 ℃ temperature, the particle that is crushed to 0.1～0.5mm are stand-by;
2) will put into electric furnace through the rice husk particle that step (1) the is handled aluminum oxide saggar of packing into, the stove carbonization is closed in the big flame burning of first blow-on 2～10 minutes again, and carbonization temperature is 650～700 ℃, is incubated 3～5 hours;
3) the carbonization rice husk particle is put into grinding pot, adding distilled water is dried under 80～100 ℃ temperature after being placed on and grinding 10～15 minutes on the speed muller;
4) will make compound by wet method or dry method through the carbonization rice husk particle of grinding and 1～4% catalyzer;
5) with plumbago crucible in 40～70 ℃ of preheatings, the mashed prod brushing uniformly of the separant mixed well and binding agent is put into the vertical vacuum furnace that graphite is made heating member with plumbago crucible on the plumbago crucible inwall, fire at 2000～2100 ℃, when reaching top temperature, be incubated 1 hour;
6) with resulting compound in the step (4), in the plumbago crucible of packing into, account for 3/4 height of crucible, the carbon fiber of arranging on the top of crucible is built crucible cover; Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, and after vacuumizing, logical Ar gas shiled is warming up to 1400～1450 ℃, is incubated 3～5 hours, is cooled to 970 ℃ with 8～10 ℃/minute, and powered-down is cooled to room temperature.
Described compound wants layering to pack in the plumbago crucible of packing into the time, separates with the carbon felt between the bed of material.
Described catalyzer is a halogenide.
Described separant be boron nitride, silicic acid Zirconium, molybdenum silicide any or several; Described binding agent be honey, peach gum, carboxymethyl cellulose any or several.
The invention has the beneficial effects as follows: owing to adopt with carbonization rice husk is unique reaction raw materials, carbonization rice husk not only is the silicon source but also do carbon source, and induce the generation silicon carbide whisker with carbon fiber, based on vapor phase growth mechanism, whisker depends on carbon fibre growth, the whisker of growth is on the carbon fiber of top, and unreacted remains the silicon carbide powder of carbon and generation completely in crucible, whisker has been realized in process of growth and the separating automatically of powder, and, reduced the remaining carbon of whisker, thereby the straight brilliant rate and the purity of whisker have been improved because of not introducing external carbon source, simplify production technique, reduced cost.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings
Accompanying drawing is the made silicon carbide whisker microcosmic of a present invention SEM shape appearance figure
Embodiment
Embodiment 1:
(1) with clear water with silt, the dust washes clean of being stained with on the rice husk, under 80 ℃ temperature with its oven dry.The clean rice husk of oven dry is stand-by with the particle that pulverizer is crushed to 0.1mm.
(2) will put into electric furnace through the rice husk particle that step (1) the is handled aluminum oxide saggar of packing into, and adopt the big flame burning of first blow-on to close the technology of stove carbonization again, the rice husk particle will be carried out carbonizing treatment.Big flame combustion time is 2 minutes, and carbonization temperature is 700 ℃, is incubated 5 hours, why adopts such carbonization technique, and being has a suitable carbon silicon ratio in order to guarantee in the carbonization rice husk particle.
(3) the carbonization rice husk particle is put into grinding pot, adds distilled water and be placed on and grind on the speed muller after 10 minutes, under 80 ℃ temperature with its oven dry.
(4) will press wet method and carbonization rice husk mixing through the carbonization rice husk particle of grinding and 4% catalyst n aF, compound is made in oven dry.
Wet method is at first to be dissolved in catalyzer in the distilled water, pour into and be equipped with in the carbonization rice husk particulate mud tank, add a certain proportion of grinding medium, mud tank is placed on the twin rollers mixes, how many mixing times decides on material, after mixing certain hour slurry is emitted, oven dry is compound.
(5) with plumbago crucible in 40 ℃ of preheatings, to mix well into mashed prod with binding agent honey less than 325 purpose separant boron nitride, brush equably on the plumbago crucible inwall, plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, fire at 2000 ℃, when reaching 2000 ℃ of top temperatures, be incubated 1 hour.This process can be carried out repeatedly, and is even up to the crucible inside coating.
(6) with resulting compound in the step (4), in the plumbago crucible of packing into, account for 3/4 height of crucible, the carbon fiber of arranging on the top of crucible is built crucible cover; Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member.After vacuumizing, logical Ar gas shiled is warming up to 1400 ℃, be incubated 5 hours, is cooled to 970 ℃ with 10 ℃/minute, and powered-down is cooled to room temperature, opens crucible after the blow-on, the taking-up silicon carbide whisker.
Compound wants layering to pack in the plumbago crucible of packing into the time, separates with the carbon felt between the bed of material, to guarantee the ventilation property of material in the reaction process, is beneficial to uploading of gas.
Embodiment 2:
(1) with clear water with silt, the dust washes clean of being stained with on the rice husk, under 100 ℃ temperature with its oven dry.The clean rice husk of oven dry is stand-by with the particle that pulverizer is crushed to 0.5mm.
(2) will put into electric furnace through the rice husk particle that step (1) the is handled aluminum oxide saggar of packing into, and adopt the big flame burning of first blow-on to close the technology of stove carbonization again, the rice husk particle will be carried out carbonizing treatment.Big flame combustion time is 10 minutes, and carbonization temperature is 650 ℃, is incubated 3 hours.
(3) the carbonization rice husk particle is put into grinding pot, adds distilled water and be placed on and grind on the speed muller after 15 minutes, under 100 ℃ temperature with its oven dry.
(4) will press dry method and carbonization rice husk mixing with 2～3% catalyst n aF and 1～2% KF through the carbonization rice husk particle that grinds, make compound.
Dry method is exactly with a certain amount of carbonization rice husk particle and a certain amount of catalyzer, is incorporated with in the grinding pot of a certain proportion of grinding medium, is placed on the twin rollers to mix, and behind the mixing certain hour grinding medium is screened out, and has just obtained compound;
(5) with the plumbago crucible internal layer, brushing one deck separant in advance.During brushing, to mix well less than 325 purpose separant silicic acid Zirconium and binding agent peach gum, with plumbago crucible in 70 ℃ of preheatings, with the mashed prod brushing uniformly of the separant mixed well and binding agent on the plumbago crucible inwall, plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, fire at 2100 ℃, when reaching top temperature, be incubated 1 hour.This process can be carried out repeatedly, and is even up to the crucible inside coating.
(6) with resulting compound in the step (4), in the plumbago crucible of packing into, account for 3/4 height of crucible, the carbon fiber of arranging on the top of crucible is built crucible cover; Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member.After vacuumizing, logical Ar gas shiled is warming up to 1450 ℃, be incubated 3 hours, is cooled to 970 ℃ with 8 ℃/minute, and powered-down is cooled to room temperature, opens crucible after the blow-on, the taking-up silicon carbide whisker.
Compound wants layering to pack in the plumbago crucible of packing into the time, separates with the carbon felt between the bed of material, to guarantee the ventilation property of material in the reaction process, is beneficial to uploading of gas.
Embodiment 3:
(1) with clear water with silt, the dust washes clean of being stained with on the rice husk, under 90 ℃ temperature with its oven dry.The clean rice husk of oven dry is stand-by with the particle that pulverizer is crushed to 0.3mm.
(2) will put into electric furnace through the rice husk particle that step (1) the is handled aluminum oxide saggar of packing into, and adopt the big flame burning of first blow-on to close the technology of stove carbonization again, the rice husk particle will be carried out carbonizing treatment.Big flame combustion time is 6 minutes, and carbonization temperature is 680 ℃, is incubated 4 hours.
(3) the carbonization rice husk particle is put into grinding pot, adds distilled water and be placed on and grind on the speed muller after 13 minutes, under 90 ℃ temperature with its oven dry.
(4) will press wet method and carbonization rice husk mixing through the carbonization rice husk particle of grinding and 3% catalyst n aCl, compound is made in oven dry.
(5) with the plumbago crucible internal layer, brushing one deck separant in advance.During brushing, to mix well less than 325 purpose separant molybdenum silicides and binding agent carboxymethyl cellulose, with plumbago crucible in 50 ℃ of preheatings, with the mashed prod brushing uniformly of the separant mixed well and binding agent on the plumbago crucible inwall, plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, fire at 2000 ℃, when reaching top temperature, be incubated 1 hour.This process can be carried out repeatedly, and is even up to the crucible inside coating.
(6) with resulting compound in the step (4), in the plumbago crucible of packing into, account for 3/4 height of crucible, the carbon fiber of arranging on the top of crucible is built crucible cover; Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member.After vacuumizing, logical Ar gas shiled is warming up to 1400 ℃, be incubated 4 hours, is cooled to 970 ℃ with 10 ℃/minute, and powered-down is cooled to room temperature, opens crucible after the blow-on, the taking-up silicon carbide whisker.
Compound wants layering to pack in the plumbago crucible of packing into the time, separates with the carbon felt between the bed of material, to guarantee the ventilation property of material in the reaction process, is beneficial to uploading of gas.
Made whisker as shown in drawings, as we can see from the figure, the SiC that is generated
wPercent of straight SiC whisker nearly 100%; The whisker regular shape, diameter is tiny, and length-to-diameter ratio is big in 0.5～2 mu m range, length in 10～500 mu m ranges, smooth surface; And in whisker, do not find inclusion and spherocrystal, the pick-up rate of whisker is 100%.
Claims (4)
1, a kind of method for preparing silicon carbide whisker is characterized in that following step:
1) with clear water with the rice husk washes clean, oven dry under 80～100 ℃ temperature, the particle that is crushed to 0.1～0.5mm are stand-by;
2) will put into electric furnace through the rice husk particle that step (1) the is handled aluminum oxide saggar of packing into, the stove carbonization is closed in the big flame burning of first blow-on 2～10 minutes again, and carbonization temperature is 650～700 ℃, is incubated 3～5 hours;
3) the carbonization rice husk particle is put into grinding pot, adding distilled water is dried under 80～100 ℃ temperature after being placed on and grinding 10～15 minutes on the speed muller;
4) will make compound by wet method or dry method through the carbonization rice husk particle of grinding and 1～4% catalyzer;
5) with plumbago crucible in 40～70 ℃ of preheatings, the mashed prod brushing uniformly of the separant mixed well and binding agent is put into the vertical vacuum furnace that graphite is made heating member with plumbago crucible on the plumbago crucible inwall, fire at 2000～2100 ℃, when reaching top temperature, be incubated 1 hour;
6) with resulting compound in the step (4), in the plumbago crucible of packing into, account for 3/4 height of crucible, the carbon fiber of arranging on the top of crucible is built crucible cover; Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, and after vacuumizing, logical Ar gas shiled is warming up to 1400～1450 ℃, is incubated 3～5 hours, is cooled to 970 ℃ with 8～10 ℃/minute, and powered-down is cooled to room temperature.
2, the method for preparing silicon carbide whisker according to claim 1 is characterized in that: described compound wants layering to pack in the plumbago crucible of packing into the time, separates with the carbon felt between the bed of material.
3, the method for preparing silicon carbide whisker according to claim 1 is characterized in that: described catalyzer is a halogenide.
4, the method for preparing silicon carbide whisker according to claim 1 is characterized in that: described separant be boron nitride, silicic acid Zirconium, molybdenum silicide any or several; Described binding agent be honey, peach gum, carboxymethyl cellulose any or several.
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| CN101864619A (en) * | 2010-06-18 | 2010-10-20 | 吉林大学 | Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls |
| CN101333685B (en) * | 2008-07-29 | 2010-12-08 | 浙江理工大学 | Three-chamber continuous whisker-generating vacuum furnace for continuously preparing silicon carbide whisker |
| CN105220220A (en) * | 2015-10-29 | 2016-01-06 | 无锡桥阳机械制造有限公司 | A kind of preparation method of silicon carbide whisker |
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| CN1042830C (en) * | 1992-11-27 | 1999-04-07 | 中南工业大学 | Preparing graphite silicon carbide coating and carbon silicon compound by using rice husk |
| CN1112466C (en) * | 1999-07-21 | 2003-06-25 | 中国科学院山西煤炭化学研究所 | Preparation method of nanometer silicon carbide whiskers |
| CN1239758C (en) * | 2003-07-17 | 2006-02-01 | 上海交通大学 | Massive prepn process of nano beta-Sic crystal whisker |
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| CN101864619A (en) * | 2010-06-18 | 2010-10-20 | 吉林大学 | Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls |
| CN105220220A (en) * | 2015-10-29 | 2016-01-06 | 无锡桥阳机械制造有限公司 | A kind of preparation method of silicon carbide whisker |
| CN106219548A (en) * | 2016-07-15 | 2016-12-14 | 宁波工程学院 | A kind of preparation method of B doping SiC nanowire |
| CN106282927A (en) * | 2016-08-05 | 2017-01-04 | 宁波高新区斯汀环保科技有限公司 | A kind of preparation method of molybdenum carbon modified SiClx/copper composite electron encapsulating material |
| CN107059129B (en) * | 2017-04-05 | 2019-04-19 | 西北工业大学 | The preparation method of co-precipitation and thermal evaporation techniques fabricated in situ cone cell SiC whisker |
| CN107059129A (en) * | 2017-04-05 | 2017-08-18 | 西北工业大学 | Co-precipitation and the preparation method of thermal evaporation techniques fabricated in situ taper SiC whiskers |
| CN107587187A (en) * | 2017-08-04 | 2018-01-16 | 海南大学 | A kind of method that SiC Nanometer Whiskers are prepared using crystalline silicon cutting waste mortar |
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