CN103643294B - A kind of size uniformity, polyhedron morphology the preparation method of silicon carbide microcrystalline - Google Patents
A kind of size uniformity, polyhedron morphology the preparation method of silicon carbide microcrystalline Download PDFInfo
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- CN103643294B CN103643294B CN201310611182.1A CN201310611182A CN103643294B CN 103643294 B CN103643294 B CN 103643294B CN 201310611182 A CN201310611182 A CN 201310611182A CN 103643294 B CN103643294 B CN 103643294B
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Abstract
The preparation method that the present invention relates to the silicon carbide microcrystalline of a kind of size uniformity, polyhedron morphology, comprises the following steps: be positioned in crucible by SiC raw material, and microcrystalline deposition catcher is fixed on inside crucible cover, after screwing up crucible, is placed in crystal growing furnace；Crystal growth system is evacuated to < 5 × 10-3Pa, then pour 1～20000Pa atmosphere gas；Promoting the temperature of crystal growth system, the temperature making raw material district is 1800～2200 DEG C, and the temperature of crucible cover place microcrystalline deposition catcher is 1750～2100 DEG C, proceeds by microcrystalline growth；After microcrystalline growth 0.5～2 hour, close crystal growing furnace power supply.The present invention is not related to other predecessor any and catalyst, and raw material district and deposition growing distinguish from, obtain SiC crystallite dimension adjustable in 10～50 micrometer ranges, and be separated from each other, present polyhedron pattern, and the microcrystalline growth cycle is short, method is simple, large-scale industrial production easy to spread, applicable, has very strong practical value.
Description
Technical field
The preparation method that the present invention relates to a kind of silicon carbide microcrystalline, the preparation method particularly relating to the silicon carbide microcrystalline of a kind of size uniformity, polyhedron morphology, belong to carborundum crystals preparation field.
Background technology
At present, carborundum (SiC) crystallite is substantially by sieving what the different size SiC particulate of synthesis obtained, and its dimensional homogeneity is poor, microcrystal grain is reunited seriously, pattern is different.SiC crystallite micro Process cutlery, high-effect abrasive material, ceramic matrix strengthening material etc. in have broad application prospects, and polyhedron pattern, size uniformity, discrete SiC crystallite can efficiently be applied to above-mentioned field undoubtedly.Therefore, a kind of method developing SiC crystallite synthesizing size uniformity, polyhedron pattern, it is highly significant, has broad application prospects.
Acheson method [Acheson, G. (1893) United States Patent (USP) 492, 767 " Productionofartificialcrystallinecarbonaceousmaterial "] it is growth single-crystal silicon carbide granule, and the maturation method that widespread commercial uses, thin silica dioxide granule is mixed by the method with coke, insert in the electric furnace that graphite is electrode, it is heated to the high temperature between 1600 to 2500 DEG C to prepare, but the method synthesis SiC single crystal particle size difference big (1 micron～several millimeters), particle agglomeration phenomenon is serious, in crystal grain, impurity content is high, need Material disintegrator to carry out raw material to crush, then screen, for different aspect, such as SiC abrasive material etc..For discrete, size uniformity, have the SiC crystallite (described SiC crystallite refers to the SiC single crystal for being smaller in size than 50 microns) of multi-plane shape, the method is difficult to obtain.
Summary of the invention
The preparation method that the technical problem to be solved is to provide the silicon carbide microcrystalline of a kind of size uniformity, polyhedron morphology.
The preparation method that the technical scheme is that the silicon carbide microcrystalline of a kind of size uniformity, polyhedron morphology, comprises the following steps:
(1) being positioned in crucible by SiC raw material, microcrystalline deposition catcher is fixed on inside crucible cover, after screwing up crucible, is placed in crystal growing furnace, enclosed crystal growth furnace, forms crystal growth system；
(2) crystal growth system is evacuated to < 5 × 10-3PaPa, then pour 1～20000Pa atmosphere gas；
(3) promoting the temperature of crystal growth system, the temperature making raw material district is 1800～2200 DEG C, and the temperature of crucible cover place microcrystalline deposition catcher is 1750～2100 DEG C, proceeds by microcrystalline growth；
(4) the microcrystalline growth time is generally 30 minutes to 2 hours, after growth terminates, closes crystal growing furnace power supply, obtains the silicon carbide microcrystalline of described size uniformity, polyhedron morphology at microcrystalline deposition catcher place.
Applied Physics gas phase transmission (PVT) method of the present invention synthesizes SiC crystallite, basic process is: SiC raw material is placed on the high-temperature region of reaction system, sediment trap is placed at low-temperature space place, the SiC raw material of such high-temperature region decomposes and transmits to low-temperature space, by strictly set the thermograde of growth system, system atmosphere constitute and the factor such as Gaseous partial pressures, catcher, realize the homogeneous nucleation to carborundum gaseous material and the orientation of growth is modulated, can the homogeneous polygon SiC crystallite of growth size, can be used for multinomial field.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in described step (1), SiC raw material is that silicon carbide abrasive, silicon carbide powder, the mixed powder of Si and C or SiC block are brilliant.
Further, in described step (1), crucible is graphite crucible, ramet crucible, niobium carbide crucible or tungsten crucible.In order to increase the increment of crystallite, can be designed crucible size used by microcrystalline growth adjusting.
Crystal growth system is evacuated to < 5 × 10 in (2) by described step-3The order of PaPa is moisture and oxygen, the nitrogen of removing absorption in growth system.
Further, in described step (2), atmosphere gas is one or both mixing in hydrogen, argon.
Further, in described step (3), the temperature of microcrystalline deposition catcher is lower than the temperature in raw material district, and when control microcrystalline growth is in low degree of supersaturation.
By designing warm field in microcrystalline growth system, atmosphere, air pressure, realize being uniformly distributed of SiC crystallite, size regulation and control (1～50 micron) and polyhedron pattern.
SiC microcrystalline growth is based primarily upon the evaporation capacity controlling SiC raw material, and the degree of supersaturation in SiC microcrystalline growth environment, a large amount of gaseous substances are uniform free nucleation in crucible cover place catcher, owing to growing environment supersaturation is relatively low, therefore the high energy crystal plane in crystal growth easily remains, and presents polyhedron SiC crystallite form.This kind of surface texture, is conducive to high accuracy, high efficiency mill, cuts the purposes of field aspect, and in micro Process cutlery, abrasive material, parent strengthening material, application is advantageously.
The present invention (includes Ar, hydrogen) in various atmosphere, and under the growth air pressure of broadening (1-20000Pa), in the temperature range of broadening, (1750-2100 DEG C) can realize SiC microcrystalline growth, and namely microcrystalline growth window is very wide；The present invention is by the accurate control of radial direction temperature field in growth system, realize the uniform spontaneous nucleation of SiC crystallite, the homogeneity of size and the controllability present invention by controlling axial temperature field in growth system, carborundum gaseous material is made to have low degree of supersaturation on the collector, therefore the high energy crystal plane in microbody growth can remain, and presents polyhedron SiC crystallite form.
The invention has the beneficial effects as follows: the present invention is successfully realized size uniformity, controlled, there is the growth of polygon pattern silicon carbide microcrystalline, use silicon carbide abrasive, silicon carbide powder, mixed powder or the SiC block crystalline substance of Si and C are raw material, it is not related to other predecessor any and catalyst, and raw material district and deposition growing distinguish from (affecting with avoiding impurity and other miscellaneous product), obtain SiC crystallite dimension adjustable in 10～50 micrometer ranges, and be separated from each other, present polyhedron pattern, and the microcrystalline growth cycle is short, method is simple, easy to spread, it is suitable for large-scale industrial production, there is very strong practical value.
By selecting Si source gas (such as silane), C source gas (such as ethane), it is likely in conjunction with technical scheme and prepares similar SiC crystallite.The present invention is not fully defined in conjunction SiC crystallite, it is also possible to be used for synthesizing the micro crystal materials such as AlN, GaN, ZnO.
Detailed description of the invention
Hereinafter principles of the invention and feature being described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1
Crystal growing furnace put into by crucible that is SiC block is brilliant and that secure microcrystalline deposition catcher.Crystal growth system is evacuated to 10-3After Pa, after pouring 15000Pa hydrogen, promote system temperature and make raw material have high evaporating temperature (1950～2000 DEG C), catcher place has relatively low temperature (1950 DEG C), carries out SiC microcrystalline growth, after growth in 30 minutes terminates, closing crystal growing furnace power supply, product cools to room temperature with the furnace.Take out attachment SiC microcrystalline product on the collector, carry out morphology observation.The SiC crystallite dimension grown is homogeneous (40～50 microns), it does not have agglomeration, SiC crystallite presents polyhedron pattern.
Embodiment 2
Silicon carbide abrasive and the crucible securing microcrystalline deposition catcher are put into crystal growing furnace.Crystal growth system is evacuated to 3 × 10-3Pa, after pouring 8000Pa hydrogen and argon gaseous mixture again, promoting system temperature makes raw material have high evaporating temperature (1850-1900 DEG C), catcher place has relatively low temperature (1800 DEG C), carry out SiC microcrystalline growth, after 1 hours growth terminates, closing crystal growing furnace power supply, product cools to room temperature with the furnace.Take out attachment SiC microcrystalline product on the collector, carry out morphology observation.The SiC crystallite dimension grown is homogeneous (30～40 microns), it does not have agglomeration, SiC crystallite presents polyhedron pattern.
Embodiment 3
By the mixed powder of Si, C with secure the crucible of microcrystalline deposition catcher and put into crystal growing furnace.Crystal growth system is evacuated to 10-3Pa, is re-filled with 10Pa argon, promotes system temperature and makes raw material have high evaporating temperature (1800-1850 DEG C), catcher place has relatively low temperature (1750 DEG C), carries out SiC microcrystalline growth, after 2 hours growth terminate, closing crystal growing furnace power supply, product cools to room temperature with the furnace.Take out attachment SiC microcrystalline product on the collector, carry out morphology observation.The SiC crystallite dimension grown is homogeneous (10～20 microns), is substantially free of agglomeration, and SiC crystallite presents polyhedron pattern.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (3)
1. the preparation method of the silicon carbide microcrystalline of a size uniformity, polyhedron morphology, it is characterised in that comprise the following steps:
(1) being positioned in crucible by SiC raw material, microcrystalline deposition catcher is fixed on inside crucible cover, after screwing up crucible, is placed in crystal growing furnace, enclosed crystal growth furnace, forms crystal growth system；
(2) crystal growth system is evacuated to < 5 × 10-3Pa, then pour 1～20000Pa atmosphere gas, atmosphere gas is one or both mixing in hydrogen, argon；
(3) temperature of crystal growth system is promoted, the temperature making raw material district is 1800～2200 DEG C, the temperature of crucible cover place microcrystalline deposition catcher is 1750～2100 DEG C, the temperature of microcrystalline deposition catcher is lower than the temperature in raw material district, and control microcrystalline growth when being in low degree of supersaturation, proceed by microcrystalline growth；
(4) after microcrystalline growth 0.5～2 hour, close crystal growing furnace power supply, obtain the silicon carbide microcrystalline of described size uniformity, polyhedron morphology at microcrystalline deposition catcher place.
2. the preparation method of the silicon carbide microcrystalline of size uniformity, polyhedron morphology according to claim 1, it is characterised in that in described step (1), SiC raw material is that silicon carbide powder, the mixed powder of Si and C or SiC block are brilliant.
3. the preparation method of the silicon carbide microcrystalline of size uniformity, polyhedron morphology according to claim 1, it is characterised in that in described step (1), crucible is graphite crucible, ramet crucible, niobium carbide crucible or tungsten crucible.
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| CN1038438A (en) * | 1986-08-22 | 1990-01-03 | 斯坦科尔公司 | Their method of six sides' silicon carbide platelets and preform and preparation and use |
| CN101812723A (en) * | 2010-04-20 | 2010-08-25 | 中国科学院上海硅酸盐研究所 | Method and device for growing silicon carbide signal crystals based on physical vapor transport technology |
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| JP2005239496A (en) * | 2004-02-27 | 2005-09-08 | Nippon Steel Corp | Silicon carbide raw material for growing silicon carbide single crystal, silicon carbide single crystal, and method for producing the same |
| KR20110095434A (en) * | 2010-02-19 | 2011-08-25 | 네오세미테크 주식회사 | Synthesis method of silicon carbide powder for single crystal growth |
| JP5696630B2 (en) * | 2011-09-21 | 2015-04-08 | 住友電気工業株式会社 | Silicon carbide substrate and method for manufacturing the same |
| KR101976594B1 (en) * | 2011-12-26 | 2019-05-09 | 엘지이노텍 주식회사 | Silicon carbide powder, method for manufacturing the same and method for fabricating single crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1038438A (en) * | 1986-08-22 | 1990-01-03 | 斯坦科尔公司 | Their method of six sides' silicon carbide platelets and preform and preparation and use |
| CN101812723A (en) * | 2010-04-20 | 2010-08-25 | 中国科学院上海硅酸盐研究所 | Method and device for growing silicon carbide signal crystals based on physical vapor transport technology |
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| Synthesis of High Purity SiC Powder for High-resistivity SiC Single Crystals Growth;Li Wang，等;《J. Mater. Sci. Technol.》;20070130;第23卷(第1期);118-122 * |
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