CN103693646B - Method for spheroidizing and purifying silicon carbide micropowder - Google Patents
Method for spheroidizing and purifying silicon carbide micropowder Download PDFInfo
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Abstract
The invention discloses a method for spheroidizing and purifying silicon carbide micropowder. The method comprises the following steps of: adding pure water accounting for 30-50% of the mass of the silicon carbide micropowder into the silicon carbide micropowder, simultaneously adding a binding agent accounting for 0.5-2% of the mass of the silicon carbide micropowder, dispersing uniformly, and then granulating by using a spray drying method to obtain granulation powder; feeding the granulation powder into a vertical carbon tube furnace in the protective atmosphere of pure argon, and from top to bottom, feeding the granulation powder to a preheating zone to be heated gradually to more than 1700 DEG C, to a high temperature zone to be preserved at the temperature of 1700-2200 DEG C for 30-120min, and then to a cooling zone to be cooled to be below 100 DEG C to obtain spheroidized and purified powder. The spherical silicon carbide micropowder prepared according to the invention is increased in flowability and reduced in natural angle of repose and also significantly improves apparent density and tap density; the content of silicon carbide in the powder can reach more than 99%, and the content of SiO2 is reduced to be below 0.2%.
Description
Technical field
The present invention relates to material preparation technology, refer to a kind of method making silicon carbide micro-powder spheroidization and purifying further.
Background technology
Carborundum (SiC) has the features such as high strength, high rigidity, corrosion-resistant, wear-resistant, anti-oxidant, stable chemical nature because of it, to obtain apply more and more widely as high-temperature structural material, abrasive polishing materials, resistant material etc. in fields such as space flight and aviation, electronic information, machinery, chemical industry, metallurgy.At present, industrial sic raw material, mainly by the a-SiC that carbothermic method is smelted under 2500 DEG C of high temperature, then obtains the silicon carbide powder with different-grain diameter by the method for mechanical crushing.Although the purity of high-grade carborundum block can reach 99.5% after smelting, but can the impurity such as iron be brought into and make particle surface form oxide-film in follow-up fragmentation repeatedly, grinding, purification, classification process, therefore, silicon-carbide particle after processing is thinner, its purity is lower, when particle size reaches 1 microns, common silicon carbide powder purity can only reach 98% or lower.In addition, the silicon carbide powder particle prepared by mechanical crushing is multi-angular irregular shape (see accompanying drawing 2), the poor fluidity of powder, for the packed density of particle and the compact density of product can be affected during sintering silicon carbide products, easily produce cut for during polishing material, affect polishing efficiency and the surface roughness of polished product.Therefore, develop a kind of highly purified spheroidization silicon carbide micro-powder, to preparation high-quality silicon carbide articles or high efficiency precise polished powder is all very important.
In order to reduce the sharp corners of silicon carbide powder, common way powder is put into ball mill carry out shaping.The sharp-pointed corner angle of part can be removed by ball milling, but powder cannot be made to reach spherical or subsphaeroidal, and also can bring impurity into further in reforming process, reduce the purity of silicon carbide powder.
Closely during the last ten years; many research workers adopt sol-gel processing, chemical vapour deposition technique, self-propagating high-temperature synthesis etc. also to prepare some subglobose low temperature Emission in Cubic b-SiC micro mist or nano-powders in laboratory; but because particle is too thin and reunite serious; preparation cost is high, is difficult to realize batch production and large-scale industrial application.
Summary of the invention
The technical problem to be solved in the present invention is,, out-of-shape multi-angular for existing silicon carbide micro-powder and the lower technical barrier of purity, develop and a kind ofly not only can improve the purity of silicon carbide micro-powder but also the technology of irregular silicon carbide micro-powder spheroidizing of particles can be made, obtain that carborundum content reaches more than 99%, particle is spherical or subglobose silicon carbide micro-powder, to meet the preparation of high-quality silicon carbide articles and the high efficiency precise polished application demand to high-purity spheroidization silicon carbide micro-powder.
For achieving the above object, technical scheme of the present invention is:
Make a method for silicon carbide micro-powder spheroidization and purifying, comprise the following steps:
(1) in silicon carbide micro-powder, add the pure water accounting for silicon carbide micro-powder quality 30% ~ 50%, add the binding agent accounting for silicon carbide micro-powder quality 0.5% ~ 2% simultaneously, be uniformly dispersed, then use spray drying process granulation, obtain granulation powder;
(2) described granulation powder is entered vertical carbon shirt-circuiting furnace under the protective atmosphere of pure argon, first with the time of 60 minutes ~ 90 minutes, granulation powder is progressively heated to more than 1700 DEG C in preheating zone from top to bottom; Then enter high-temperature region to keep 30 minutes ~ 120 minutes at the temperature of 1700 DEG C ~ 2200 DEG C, then be cooled to less than 100 DEG C through cooling zone, obtain the powder after spheroidization and purifying;
Described vertical carbon shirt-circuiting furnace comprises preheating zone, high-temperature region and cooling zone from top to bottom successively, and described preheating zone bottom outer wall and high-temperature region outer wall are provided with heater, and the outer wall of described cooling zone is provided with cooler; Top, described preheating zone is provided with exhaust outlet, and the sidewall of preheating zone is provided with charge door; Be provided with air inlet below the sidewall of described cooling zone, bottom cooling zone, be provided with discharging opening.
Step (1) described silicon carbide micro-powder is preferably that average grain diameter is 0.3 micron ~ 3 microns, carborundum content be not less than 98% silicon carbide micro-powder.
Step (1) described binding agent is preferably at least one of hydroxypropyl methylcellulose and polyvinyl alcohol.
Described step (2) is specifically preferably:
A, the charge door of vertical carbon shirt-circuiting furnace and discharging opening closed, vacuumizing in stove from exhaust outlet with vavuum pump, when vacuum is less than 5Pa, is the argon gas of 99.99% from air inlet purity; When furnace pressure reaches pressure-fired (being greater than 20 millimeters of water), reduce or stop argon gas passing into, start to heat up to vertical carbon shirt-circuiting furnace, make the temperature in furnace high-temperature district reach 1700 DEG C ~ 2200 DEG C and keep its temperature stabilization;
B, described granulation powder is added in stove by the charge door on vertical carbon shirt-circuiting furnace top, rely on the deadweight of powder and good mobility, granulation powder flows to preheating zone from charge door, in preheating zone, with 60 minutes ~ 90 minutes, powder is progressively heated to more than 1700 DEG C; Along with the rising of powder temperature, binding agent occurs decompose and discharge from upper air vent;
When c, described pre-heating powder flow through the high-temperature region of vertical carbon shirt-circuiting furnace, keep 30 minutes ~ 120 minutes at 1700 DEG C ~ 2200 DEG C, obtain the product after spheroidization and purifying; Gaseous substance in product together to be overflowed vertical carbon shirt-circuiting furnace from upper air vent with protective gas in stove;
Product after d, spheroidization and purifying continues to move down, enter the cooling zone of vertical carbon shirt-circuiting furnace, the product fast cooling after spheroidization and purifying, when powder temperature is reduced to below 100 DEG C, flow out from the outlet bottom vertical carbon shirt-circuiting furnace, obtain the powder after spheroidization and purifying.
Further preferably, by described for step (2) be that abrasive body carries out ball milling or pulverizes in airslide disintegrating mill by the powder after spheroidization and purifying with the carborundum ball of carborundum powder weight 1.5 times ~ 3 times.
The diameter of described ball milling carborundum ball is 5 millimeters ~ 20 millimeters, and relative density is not less than 98%.
The present invention is preferably not less than the silicon carbide micro-powder of 98% for raw material with purity on existing market, in the vertical carbon shirt-circuiting furnace taking graphite as heater, added by silicon carbide micro-powder from top charge door, relies on micro mist deadweight to move down, and progressively by carbon pipe heat temperature raising.Pass into argon gas in the bottom of carbon shirt-circuiting furnace, make to keep pressure-fired in stove, cause product to be oxidized to prevent stove outer air from entering.When temperature reaches between 1700 DEG C ~ 2200 DEG C, the vapour pressure at silicon carbide micro-powder sharp comer position is higher, produces evaporation and again condenses in the lower plane of vapour pressure or concave surface position, particle is changed to spheroidization, simultaneously the SiO on material powder surface
2also can obtain purifying by following reaction:
2SiO
2+SiC→3SiO+CO
SiO and CO in product is gaseous substance, together will to overflow system with protective gas.In addition, the a small amount of iron tramp remaining in silicon carbide micro-powder surface at processing crushing process also can at high temperature partly volatilize effusion, free silica and free carbon then can react Formed SiClx at this temperature, thus realize while silicon carbide powder spheroidization, reduce the oxygen content in powder and the content of other impurity, make the content of carborundum in product bring up to more than 99% by about 98%.
Below the present invention is made and further illustrating.
Principle of the present invention is: utilize the evaporation of the vapour pressure higher prior at silicon carbide micro-powder sharp comer position under high temperature and the plane forced down at steam or the concave surface position know-why of again condensing, make the irregular silicon carbide micro-powder of pattern achieve particle at 1700 ~ 2200 DEG C to change to spheroidization, simultaneously the SiO on material powder surface
2also can by reaction 2SiO
2+ SiC → 3SiO+CO obtains purifying, because the product S iO of this reaction and CO is gaseous substance, will overflow from reaction system.
Technical contribution of the present invention is, be that the common silicon carbide micro-powder of 0.3 micron ~ 3 microns is for raw material with the average grain diameter of suitability for industrialized production on market, first the mobility of powder is improved by mist projection granulating, then in specific vertical carbon shirt-circuiting furnace, utilize irregular pattern silicon carbide powder under certain high temperature, have the feature of different vapour pressure, within the scope of 1700 DEG C ~ 2200 DEG C, because the vapour pressure at silicon carbide micro-powder sharp comer position is higher, produce evaporation and the plane forced down at steam or concave surface position are condensed again, particle is changed to spheroidization, thus realize the spheroidization of silicon carbide micro-powder.While the spontaneous spheroidization of silicon carbide micro-powder particle, the oxide layer (SiO of particle surface
2) at high temperature also will there is following reaction: 2SiO
2+ SiC → 3SiO+CO; gaseous products SiO and CO generated overflows from system with protective gas; at this temperature; a small amount of iron tramp on silicon carbide micro-powder surface also can at high temperature partly volatilize effusion; free silica and free carbon then can react Formed SiClx at this temperature; thus realize while silicon carbide powder spheroidization, reduce the oxygen content in powder and the content of other impurity, make the content of carborundum in product bring up to more than 99% by about 98%.Owing to adopting shaft (tower) furnace carbon pipe, logistics direction is contrary with direction of heat flow, has maximally utilised heat energy, reduces process energy consumption.Meanwhile, micro mist is flowing in high temperature spheroidization process, also decreases the adhesion agglomeration between particle to greatest extent, reduces the difficulty of spheroidization product postprocessing (ball milling or air-flow crushing).
High-purity spheroidization silicon carbide micro-powder prepared by the present invention has following technical advantage with the silicon carbide micro-powder ratio of existing suitability for industrialized production: (1) mobility of particle increases, and the natural angle of repose of powder is reduced to 35 ° ~ 47 ° by 50 before spheroidization ° ~ 65 °; (2) apparent density of powder and tap density are respectively by 0.55 ~ 0.75g/cm before spheroidization
3with 0.90 ~ 1.21g/cm
3bring up to 0.80 ~ 0.97g/cm
3with 1.25 ~ 1.41g/cm
3; (3) in powder, the content of carborundum brings up to 99.2 ~ 99.5%, SiO by 98.0 ~ 98.5% before spheroidization
2content is reduced to less than 0.2%.
As known from the above, the present invention is a kind of preparation method of high-purity spheroidization silicon carbide micro-powder, and the method, by significantly improving the spheroidization degree of silicon carbide micro-powder, significantly improves mobility and the packed density of powder, simultaneously by significantly reducing the SiO in micro mist
2content improves the purity of spheroidization micro mist, is expected the density significantly improving silicon carbide ceramics formed body, improves its performance; In precise polished, the surface roughness of polished material can be reduced, improve quality of finish.
Accompanying drawing explanation
Fig. 1 is vertical carbon shirt-circuiting furnace structural representation described in the application;
Fig. 2 is the shape appearance figure of raw material before treatment;
Fig. 3 is through the shape appearance figure of the product after method process of the present invention;
Wherein 1-exhaust outlet, 2-charge door, 3-preheating zone, 4-high-temperature region, 5-heater, 6-cooling zone, 7-cooler, 8-air inlet, 9-discharging opening.
Detailed description of the invention
embodiment 1:
A kind of vertical carbon shirt-circuiting furnace, it comprises preheating zone 3, high-temperature region 4 and cooling zone 6 from top to bottom successively, and described preheating zone bottom outer wall and high-temperature region outer wall are provided with heater 5, and the outer wall of described cooling zone is provided with cooler 7; Top, described preheating zone 3 is provided with exhaust outlet 1, and the sidewall of preheating zone 3 is provided with charge door 2; Be provided with air inlet 8 below the sidewall of described cooling zone 6, bottom cooling zone 6, be provided with discharging opening 9.
Make a method for silicon carbide micro-powder spheroidization and purifying, comprise the following steps:
(1) be 0.5 micron by 50kg average grain diameter, purity be 98.1% silicon carbide micro-powder add 25kg pure water, add the polyvinyl alcohol of hydroxypropyl methylcellulose and 0.7% accounting for silicon carbide micro-powder quality 0.8% as binding agent simultaneously, uniform slurry is separated into homogenizer, then use spray drying process granulation, obtain the granulation powder with good fluidity.
(2) charge door 2 of vertical carbon shirt-circuiting furnace and discharging opening 9 are closed, vacuumize in stove from exhaust outlet 1 with vavuum pump, when vacuum is less than 5Pa, the argon gas that purity is 99.99% is filled with in stove, when furnace pressure is pressure-fired, reduce or stop argon gas passing into, start to heat up to vertical carbon shirt-circuiting furnace, make the temperature in furnace high-temperature district 4 reach 1850 DEG C and be incubated.
(3) granulation powder is added the charge door 2 on vertical carbon shirt-circuiting furnace top, make granulation powder enter preheating zone 3 from charge door 2, stop 60 minutes in this district, temperature reaches 1750 DEG C.Along with powder temperature rises gradually, binding agent occurs decompose and overflow from upper air vent 1.
(4) when granulation powder enters the high-temperature region 4 of vertical carbon shirt-circuiting furnace, stop 60 minutes in this district, temperature remains on about 1850 DEG C.Because the vapour pressure at silicon carbide micro-powder sharp comer position is higher, preferential evaporation the plane forced down at steam or concave surface position are condensed again, and particle is changed to spheroidization; The SiO on granulation powder surface simultaneously
2by reacting acquisition purifying as follows: 2SiO
2+ SiC → 3SiO+CO, SiO and CO in product is gaseous substance, together to overflow system from upper air vent 1 with protective gas in stove.
(5) powder after step (4) spheroidization and purifying continues to move down, and enters the cooling zone 5 of vertical carbon shirt-circuiting furnace, powder fast cooling; When powder temperature is reduced to below 100 DEG C, flows out from the outlet 9 bottom vertical carbon shirt-circuiting furnace, obtain spheroidization powder.
(6) further spheroidization powder is placed in polyurethane ball-milling pot, to add 2 times of diameters to carborundum powder weight be the carborundum ball of 5 millimeters ~ 20 millimeters is abrasive body, and ball milling 3 hours, makes powder disperse.
The high-purity spheroidization silicon carbide micro-powder (product pattern is shown in Fig. 3) prepared with said method, its carborundum content reaches 99.23%, SiO
2content only 0.18%, the natural angle of repose of powder is 46 °, apparent density and tap density 0.85g/cm respectively
3and 1.26g/cm
3.
embodiment 2: a kind of method making silicon carbide micro-powder spheroidization and purifying, comprises the following steps:
(1) be 1.5 microns by 50kg average grain diameter, purity be 98.3% silicon carbide micro-powder add 25kg pure water, add the polyvinyl alcohol of hydroxypropyl methylcellulose and 0.6% accounting for silicon carbide micro-powder quality 1.0% as binding agent simultaneously, uniform slurry is separated into homogenizer, then use spray drying process granulation, obtain the granulation powder with good fluidity.
(2) charge door 2 of vertical carbon shirt-circuiting furnace (with embodiment 1) and discharging opening 9 are closed, vacuumize in stove from exhaust outlet 1 with vavuum pump, when vacuum is less than 5Pa, the argon gas that purity is 99.99% is filled with in stove, when furnace pressure is pressure-fired, reduce or stop argon gas passing into, start to heat up to vertical carbon shirt-circuiting furnace, make the temperature in furnace high-temperature district 4 reach 1950 DEG C and be incubated.
(3) granulation powder is added the charge door 2 on vertical carbon shirt-circuiting furnace top, make granulation powder enter preheating zone 3 from charge door 2, stop 75 minutes in this district, temperature reaches 1800 DEG C.Along with powder temperature rises gradually, binding agent occurs decompose and overflow from upper air vent 1.
(4) when granulation powder enters the high-temperature region 4 of vertical carbon shirt-circuiting furnace, stop 75 minutes in this district, temperature remains on about 1950 DEG C.Because the vapour pressure at silicon carbide micro-powder sharp comer position is higher, preferential evaporation the plane forced down at steam or concave surface position are condensed again, and particle is changed to spheroidization; The SiO on granulation powder surface simultaneously
2by reacting acquisition purifying as follows: 2SiO
2+ SiC → 3SiO+CO, SiO and CO in product is gaseous substance, together to overflow system from upper air vent 1 with protective gas in stove.
(5) powder after step (4) spheroidization and purifying continues to move down, and enters the cooling zone 5 of vertical carbon shirt-circuiting furnace, powder fast cooling; When powder temperature is reduced to below 100 DEG C, flows out from the outlet 9 bottom vertical carbon shirt-circuiting furnace, obtain spheroidization powder.
(6) further spheroidization powder is placed in polyurethane ball-milling pot, to add 2 times of diameters to carborundum powder weight be the carborundum ball of 5 millimeters ~ 20 millimeters is abrasive body, and ball milling 3 hours, makes powder disperse.
The high-purity spheroidization silicon carbide micro-powder (product pattern is shown in Fig. 3) prepared with said method, its carborundum content reaches 99.36%, SiO
2content only 0.12%, the natural angle of repose of powder is 42 °, apparent density and tap density 0.91g/cm respectively
3and 1.38g/cm
3.
embodiment 3: a kind of method making silicon carbide micro-powder spheroidization and purifying, comprises the following steps:
(1) be 2.5 microns by 50kg average grain diameter, purity be 98.5% silicon carbide micro-powder add 25kg pure water, add the polyvinyl alcohol of hydroxypropyl methylcellulose and 0.5% accounting for silicon carbide micro-powder quality 1.2% as binding agent simultaneously, uniform slurry is separated into homogenizer, then use spray drying process granulation, obtain the granulation powder with good fluidity.
(2) charge door 2 of vertical carbon shirt-circuiting furnace (with embodiment 1) and discharging opening 9 are closed, vacuumize in stove from exhaust outlet 1 with vavuum pump, when vacuum is less than 5Pa, the argon gas that purity is 99.99% is filled with in stove, when furnace pressure is pressure-fired, reduce or stop argon gas passing into, start to heat up to vertical carbon shirt-circuiting furnace, make the temperature in furnace high-temperature district 4 reach 2050 DEG C and be incubated.
(3) granulation powder is added the charge door 2 on vertical carbon shirt-circuiting furnace top, make granulation powder enter preheating zone 3 from charge door 2, stop 90 minutes in this district, temperature reaches 1900 DEG C.Along with powder temperature rises gradually, binding agent occurs decompose and overflow from upper air vent 1.
(4) when granulation powder enters the high-temperature region 4 of vertical carbon shirt-circuiting furnace, stop 90 minutes in this district, temperature remains on about 2050 DEG C.Because the vapour pressure at silicon carbide micro-powder sharp comer position is higher, preferential evaporation the plane forced down at steam or concave surface position are condensed again, and particle is changed to spheroidization; The SiO on granulation powder surface simultaneously
2by reacting acquisition purifying as follows: 2SiO
2+ SiC → 3SiO+CO, SiO and CO in product is gaseous substance, together to overflow system from upper air vent 1 with protective gas in stove.
(5) powder after step (4) spheroidization and purifying continues to move down, and enters the cooling zone 5 of vertical carbon shirt-circuiting furnace, powder fast cooling; When powder temperature is reduced to below 100 DEG C, flows out from the outlet 9 bottom vertical carbon shirt-circuiting furnace, obtain spheroidization powder.
(6) pulverized by spheroidization powder airslide disintegrating mill further, the particle mean size controlling discharging opening is 2 microns ~ 3 microns, and powder is disperseed.
The high-purity spheroidization silicon carbide micro-powder (product pattern is shown in Fig. 3) prepared with said method, its carborundum content reaches 99.45%, SiO
2content only 0.1%, the natural angle of repose of powder is 37 °, apparent density and tap density 0.95g/cm respectively
3and 1.36g/cm
3.
Claims (5)
1. make a method for silicon carbide micro-powder spheroidization and purifying, comprise the following steps:
(1) in silicon carbide micro-powder, add the pure water accounting for silicon carbide micro-powder quality 30% ~ 50%, add the binding agent accounting for silicon carbide micro-powder quality 0.5% ~ 2% simultaneously, be uniformly dispersed, then use spray drying process granulation, obtain granulation powder;
(2) described granulation powder is entered vertical carbon shirt-circuiting furnace under the protective atmosphere of pure argon, first with 60 minutes ~ 90 minutes, granulation powder is progressively heated to more than 1700 DEG C in preheating zone from top to bottom; Then enter high-temperature region to keep 30 minutes ~ 120 minutes at the temperature of 1700 DEG C ~ 2200 DEG C, then be cooled to less than 100 DEG C through cooling zone, obtain the powder after spheroidization and purifying;
Described vertical carbon shirt-circuiting furnace comprises preheating zone, high-temperature region and cooling zone from top to bottom successively, and described preheating zone bottom outer wall and high-temperature region outer wall are provided with heater, and the outer wall of described cooling zone is provided with cooler; Top, described preheating zone is provided with exhaust outlet, and the sidewall of preheating zone is provided with charge door; Be provided with air inlet below the sidewall of described cooling zone, bottom cooling zone, be provided with discharging opening;
This step is specially:
A, the charge door of vertical carbon shirt-circuiting furnace and discharging opening to be closed, vacuumize in stove from exhaust outlet with vavuum pump, when vacuum is less than 5Pa, be filled with from air inlet the argon gas that purity is 99.99%; When furnace pressure reaches pressure-fired, reduce or stop argon gas passing into, start to heat up to vertical carbon shirt-circuiting furnace, make the temperature in furnace high-temperature district reach 1700 DEG C ~ 2200 DEG C and keep its temperature stabilization;
B, described granulation powder is added in stove by the charge door on vertical carbon shirt-circuiting furnace top, rely on the deadweight of powder and good mobility, granulation powder flows to preheating zone from charge door, in preheating zone, with 60 minutes ~ 90 minutes, powder is progressively heated to more than 1700 DEG C; Along with the rising of powder temperature, binding agent occurs decompose and discharge from upper air vent;
When c, described pre-heating powder flow through the high-temperature region of vertical carbon shirt-circuiting furnace, keep 30 minutes ~ 120 minutes at 1700 DEG C ~ 2200 DEG C, obtain the product after spheroidization and purifying; Gaseous substance in product together to be overflowed vertical carbon shirt-circuiting furnace from upper air vent with protective gas in stove;
Product after d, spheroidization and purifying continues to move down, enter the cooling zone of vertical carbon shirt-circuiting furnace, the product fast cooling after spheroidization and purifying, when powder temperature is reduced to below 100 DEG C, flow out from the outlet bottom vertical carbon shirt-circuiting furnace, obtain the powder after spheroidization and purifying.
2. make the method for silicon carbide micro-powder spheroidization and purifying according to claim 1, it is characterized in that, step (1) described silicon carbide micro-powder is average grain diameter 0.3 micron ~ 3 microns, carborundum content be not less than 98% silicon carbide micro-powder.
3. according to claim 1 or 2, make the method for silicon carbide micro-powder spheroidization and purifying, it is characterized in that, step (1) described binding agent is at least one of hydroxypropyl methylcellulose and polyvinyl alcohol.
4. according to claim 1 or 2, make the method for silicon carbide micro-powder spheroidization and purifying, it is characterized in that, by described for step (2) be that abrasive body carries out ball milling or pulverizes in airslide disintegrating mill by the powder after spheroidization and purifying with the carborundum ball of carborundum powder weight 1.5 times ~ 3 times.
5. make the method for silicon carbide micro-powder spheroidization and purifying according to claim 4, it is characterized in that, the diameter of ball milling carborundum ball is 5 millimeters ~ 20 millimeters, and relative density is not less than 98%.
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CN102491330A (en) * | 2011-11-14 | 2012-06-13 | 朱胜利 | Production process of silicon carbide |
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