CN104828825B - A kind of method of low cost low temperature synthesizing silicon carbide powder - Google Patents
A kind of method of low cost low temperature synthesizing silicon carbide powder Download PDFInfo
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Abstract
A kind of method of low cost low temperature synthesizing silicon carbide powder of the present invention.High-purity carbon fiber and high-purity silicon powder are used as raw material, in crucible is increased, 500 1000 DEG C of temperature, vacuum are less than 10‑3Under the conditions of Pa, the mixed gas of argon gas or argon gas and hydrogen is filled with into growth room, pressure is 800 900mbar, is warming up to 1,000 1300 DEG C and is synthesized.The present invention uses single sintering method, overcomes secondary synthesis complex procedures, time-consuming, is artificially introduced the shortcomings of impurity.The present invention can disposably synthesize the controllable big grit silicon carbide silica flour material of 5 10kg granularities.Cost is low, and technique is simple.
Description
Technical field
The present invention relates to a kind of method of the low cost low temperature synthesizing silicon carbide powder for silicon carbide monocrystal growth, belong to nothing
Machine field of non-metallic materials.
Background technology
Single-crystal silicon carbide because its have energy gap is big, breakdown electric field is high, thermal conductivity is big, electronics saturation drift velocity is high,
The characteristic that dielectric constant is small, capability of resistance to radiation is strong, good chemical stability etc. is unique, and with first generation semi-conducting material and the
Two generation semi-conducting materials, which are compared, obvious superiority, it is considered to be manufacture opto-electronic device, Deep trench termination, electric power
The preferable semi-conducting material of electronic device, in white-light illuminating, optical storage, screen display, space flight and aviation, hyperthermia radiation environment, stone
Exploration activity, automation, radar and communications, automotive circuit diagram etc. are widely used.In single crystalline substrate, homoepitaxy semiconductor
Film and device technology etc. are quickly grown, and are one of optimal third generation semi-conducting materials.
Sic powder quality plays a very important role in sublimation growth single-crystal silicon carbide, directly affects the knot of monocrystalline
Crystalloid amount and growth thickness.With single-crystal silicon carbide substrate power device and the extensive extensive use of power electronic devices, to big
The demand of diameter single crystal is more and more urgent, and 6 inches even 8 inches are expanded to by 4 inches be widely used at present.But with lining
The increase of bottom diameter, growth crucible size it is bigger, it is necessary to source material carborundum powder increase therewith, 6 inches of crystal growths are per heat
Charge is needed to be up to 2-3kg, current synthetic method cost is high, can not meet the needs of industrialization production, therefore pass through
Synthesis material technology is improved, reduces cost, source material granularity is controllable, it has also become growth large single crystal problem urgently to be resolved hurrily at present.
Chinese patent document CN102701208A discloses the high temperature process heat method of high-purity silicon carbide powder, this method
After high-purity silicon powder and high-purity carbon dust are well mixed, hypertonic solutions are then carried out, i.e., using high purity inert gas in difference
Cleaning is vacuumized under pressure and different temperatures, high―temperature nuclei is then carried out at 1800-2100 DEG C, the final nitrogen content that obtains exists
Below 15ppm high-purity silicon carbide powder.CN103708463A discloses the preparation method of feather weight high-pure SiC power, the party
Method carries out crucible plated film pretreatment first, and silicon carbide film is plated after first plating carbon film, is put into after being then well mixed silica flour and carbon dust
Intermediate-frequency heating furnace, high―temperature nuclei obtains feather weight high-purity silicon carbide powder between 1500-1900 DEG C.CN101302011A is disclosed
It is used for the artificial synthesis of the high-pure SiC power of semiconductor single-crystal growth, mainly using secondary synthesis method, by silica flour
After being mixed with carbon dust, first 1500 DEG C of synthesis of low temperature, are increased the temperature to after then the powder of single sintering is well mixed for the first time
1800-2000 DEG C of progress secondary synthesis, this method can effectively remove the impurity element in removing silicon powder and carbon dust.
The raw material used in existing method described above is pure silicon powder and carbon dust, and especially high-purity carbon dust belongs to external embargo
Goods and materials, it is important national defense applications raw material, expensive, this is also the important original for causing single-crystal silicon carbide substrate price high
Cause.In addition, above-mentioned three kinds of methods use high―temperature nuclei, synthesis temperature reaches as high as 2100 DEG C more than 1500 DEG C, so as to
Equipment outfit to synthesis material requires very high, and such as high temperature is realized, leak rate is small, vacuum is high, cooling capacity is strong, so as to which equipment is thrown
Enter big, cost height.
The content of the invention
Present invention deficiency existing for prior art synthesizing silicon carbide powder, there is provided one kind can be realized inexpensive, low
Warm, low equipment investment, high yield, granularity be big and the preparation method of the sic powder of uniform, controllable.
A kind of method that low cost low temperature prepares sic powder, comprises the following steps：
(1) dispensing：
High-purity carbon fiber and high-purity silicon powder are used as raw material, in molar ratio 1：1 ratio is well mixed.
The purity of high-purity carbon fiber and high-purity silicon powder raw material is all higher than 99%, 7-10 μm of carbon fiber diameter, length 1-
100mm, silicon particle size are less than 500 μm；
(2) synthesize：
The silica flour and carbon fiber are put into and increased in crucible, is placed in Medium Frequency Induction Heating Furnace, heating furnace growth room takes out
Vacuum, oxygen, nitrogen and vapor in growth room are removed, while temperature is increased to 500-1000 DEG C；Then vacuumize, make
Vacuum is less than 10-3Pa；It is filled with the mixed gas of argon gas or argon gas and hydrogen into growth room, pressure 800-900mbar,
It is warming up to 1000-1300 DEG C to be synthesized, generated time is 5-10 hours, is then down to room temperature, you can obtaining epigranular can
The sic powder of control.
According to currently preferred, the mixed of argon gas and hydrogen is filled with step (2) into Medium Frequency Induction Heating Furnace growth room
When closing gas, the volume ratio of argon gas and hydrogen is 5~9：1.Hydrogen is passed through while argon gas is filled with to be advantageous to suppress synthesis material
When nitrogen incorporation.
According to currently preferred, argon gas, the purity of hydrogen are all higher than 99.9% described in step (2).
According to currently preferred, during high―temperature nuclei described in step (2), circulating water is passed through in heating furnace chamber,
With controlling reaction temperature.
According to currently preferred, the crucible material in step (2) is common graphite or high purity graphite.By prior art.
According to currently preferred, increase crucible described in step (2), be highly 400-800mm, can disposably synthesize
5-10kg powders.The crucible can be repeated several times use.
In the present invention, the heating furnace used is Medium Frequency Induction Heating Furnace.
The method of the present invention can the regulatable SiC powders of 50-1000 μm of prepared sizes, especially more than 450 μm particle diameters
Big granularity SiC powders compensate for the SiC powder particles deficiency less than normal of prior art synthesis.Particularly preferred 500-1000 μm of particle diameter
Big granularity SiC powders.
Sic powder produced by the present invention is applicable to the preparation of silicon carbide monocrystal growth and silicon carbide ceramics.
The excellent results of the present invention：
1st, this method can realize the batch production of sic powder without using high-purity carbon dust with high temperature process heat method,
The production cost of silicon carbide products can effectively be reduced.
2nd, this method synthesis temperature is low, less than 1300 DEG C, takes full advantage of the mechanism of raw material self-propagating reaction heat release, saves
The step of high temperature more than 1500 DEG C makes crystal grain grow up, energy-conservation, equipment and relevant configuration input are greatly reduced, processing step letter
It is single.
3rd, the present invention uses single sintering method, overcomes secondary synthesis complex procedures, time-consuming, it is scarce to be artificially introduced impurity etc.
Point.The controllable sic powder of granularity can be disposably synthesized, this method cost is low, can disposably synthesize 5-10kg powders, can criticize
Amount production.
4th, big grit silicon carbide silica flour material, when being grown for SiC single crystal, same crucible size be can obtain under low temperature of the present invention
Under, bulky grain SiC powders are advantageous to increase charge, material utilization rate are improved, so as to greatly improve SiC single crystal yield.
Brief description of the drawings
Fig. 1 is the XRD of synthesizing silicon carbide powder in embodiment 1.Abscissa is 2 θ (°), and ordinate is intensity (a.u.).
Fig. 2 is the SEM figures of synthesizing silicon carbide powder in embodiment 1.Wherein, (B) figure is the partial enlarged drawing of (A) figure.
Fig. 3 is to increase graphite crucible schematic diagram.Wherein, 1, crucible, 2, silica flour and carbon fiber mixed material.
Embodiment
With reference to embodiment, the present invention will be further described, but not limited to this.
It is market purchase that embodiment is raw materials used, and the purity of high-purity carbon fiber and high-purity silicon powder is all higher than 99%, argon gas,
The purity of hydrogen is all higher than 99.9%.
Embodiment 1
A kind of method that low cost low temperature prepares carborundum powder, is comprised the following steps that：
(1) dispensing：Raw material uses high-purity carbon fiber and high-purity silicon powder, and in molar ratio 1：1 ratio is well mixed.Carbon fiber
7 μm of diameter, length 1mm.Silicon particle size is 50 μm.
(2) synthesize：The silica flour and carbon fiber are put into height increasing in crucible for 400mm, are subsequently placed in intermediate frequency sense
Answer in heating furnace, the growth room of heating furnace is vacuumized, remove oxygen, nitrogen and vapor etc. in growth room, while by temperature
Degree is increased to 800 DEG C；Then vacuumize, vacuum is less than 10-3Pa.High-purity argon gas or argon gas and hydrogen are filled with into growth room
Volume ratio is 5：1 mixed gas, argon gas, the purity of hydrogen are all higher than 99.9%, pressure 800mbar, and rise temperature is extremely
1800 DEG C, generated time is 5 hours, is then down to room temperature, you can obtain even-grained sic powder.
Material phase analysis is carried out to synthetic product using powder diffraction method (XRD), obtains XRD as shown in Figure 1, it can be seen that
Synthetic reaction is complete, and SEM figures show even particle size distribution, and granularity is 50-100 μm, suitable for silicon carbide monocrystal growth.
The purity of synthetic product sic powder is more than 99%.
Crucible used of increasing is common graphite crucible, and size is 130mm × 130mm × 400mm, can disposably synthesize 5kg
Sic powder.
Embodiment 2
As described in Example 1, institute's difference is, 10 μm of carbon fiber diameter used, length 100mm.Silicon particle size is
400μm.By two kinds of raw materials in molar ratio 1：1 is put into height increasing in crucible for 800mm, is placed in Medium Frequency Induction Heating Furnace,
The growth room of heating furnace is vacuumized, oxygen, nitrogen and vapor in removing growth room etc., while temperature is increased to 1300
℃；Then vacuumize, vacuum is less than 10-3Pa.The mixed gas of high-purity argon gas or argon gas and hydrogen is filled with into growth room,
Argon gas, the purity of hydrogen are all higher than 99.9%, and the volume ratio of argon gas and hydrogen is 9：1.Pressure is 900mbar, and rise temperature is extremely
2000 DEG C, generated time is 20 hours.For the crucible used for high purity graphite crucible, size is 130mm × 130mm × 800mm, can
Disposable synthesis 10kg sic powders；Carborundum granularity is at 900-1000 μm；Purity is more than 99%.
Embodiment 3
As described in Example 1, institute's difference is, 9 μm of carbon fiber diameter, length 50mm.Silicon particle size is 200 μm.
By two kinds of raw materials in molar ratio 1：1 is put into height increasing in crucible for 640mm, is placed in Medium Frequency Induction Heating Furnace, to heating
The growth room of stove vacuumizes, and removes oxygen, nitrogen and vapor etc. in growth room, while temperature is increased into 1100 DEG C；So
After vacuumize, make vacuum be less than 10-3Pa.The mixed gas of high-purity argon gas or argon gas and hydrogen, argon gas are filled with into growth room
Volume ratio with hydrogen is 8：1.Pressure is 850mbar, and for rise temperature to 1900 DEG C, generated time is 10 hours.The earthenware of use
Crucible is high purity graphite crucible, and size is 130mm × 130mm × 640mm, can disposably synthesize 8kg sic powders.Be carbonized silicon grain
Degree is at 500-600 μm；Purity is more than 99%.
Claims (2)
1. a kind of preparation method of carborundum powder for silicon carbide monocrystal growth, step are as follows：
(1) dispensing：Raw material uses high-purity carbon fiber and high-purity silicon powder, and in molar ratio 1：1 ratio is well mixed；Carbon fiber used
10 μm of diameter, length 100mm；Silicon particle size is 400 μm；
(2) synthesize：The silica flour and carbon fiber are put into height increasing in crucible for 800mm, Medium frequency induction is subsequently placed in and adds
In hot stove, the growth room of heating furnace is vacuumized, removes oxygen, nitrogen and vapor etc. in growth room, while by temperature liter
Up to 1300 DEG C；Then vacuumize, vacuum is less than 10-3Pa；High-purity argon gas or argon gas and hydrogen are filled with into growth room
Product is than being 9：1 mixed gas, argon gas, the purity of hydrogen are all higher than 99.9%, pressure 900mbar, rise temperature to 2000
DEG C, generated time is 20 hours, is then down to room temperature, obtains even-grained sic powder；
For the crucible used for high purity graphite crucible, size is 130mm × 130mm × 800mm, can disposably synthesize 10kg carborundum
Powder；Carborundum granularity is at 900-1000 μm；Purity is more than 99%.
2. a kind of preparation method of carborundum powder for silicon carbide monocrystal growth, step are as follows：
(1) dispensing：Raw material uses high-purity carbon fiber and high-purity silicon powder, and in molar ratio 1：1 ratio is well mixed；Carbon fiber diameter
9 μm, length 50mm, silicon particle size is 200 μm；
(2) synthesize：The silica flour and carbon fiber are put into height increasing in crucible for 640mm, Medium frequency induction is subsequently placed in and adds
In hot stove, the growth room of heating furnace is vacuumized, removes oxygen, nitrogen and vapor etc. in growth room, while by temperature liter
Up to 1100 DEG C；Then vacuumize, vacuum is less than 10-3Pa, high-purity argon gas or argon gas and hydrogen are filled with into growth room
Product is than being 8：1 mixed gas, argon gas, the purity of hydrogen are all higher than 99.9%, pressure 850mbar, rise temperature to 1900
DEG C, generated time is 10 hours, is then down to room temperature, obtains even-grained sic powder；
For the crucible used for high purity graphite crucible, size is 130mm × 130mm × 640mm, can disposably synthesize 8kg carborundum
Powder；Carborundum granularity is at 500-600 μm；Purity is more than 99%.
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| WO2017090718A1 (en) * | 2015-11-25 | 2017-06-01 | 日本碍子株式会社 | Method for substituting inert gas and method for manufacturing ceramic structure using method for substituting inert gas |
| CN106044774B (en) * | 2016-05-31 | 2018-02-27 | 上海纳晶科技有限公司 | A kind of preparation method of low temperature low cost high-purity silicon carbide ultrafine dust |
| CN108946735B (en) * | 2017-05-19 | 2022-11-11 | 新疆天科合达蓝光半导体有限公司 | Synthesis method of large-particle-size silicon carbide powder for silicon carbide crystal growth |
| CN107324338A (en) * | 2017-07-24 | 2017-11-07 | 南京施密特光学仪器有限公司 | A kind of speculum silicon carbide powder and preparation method thereof |
| CN108130592B (en) * | 2017-11-14 | 2019-11-12 | 山东天岳先进材料科技有限公司 | A kind of preparation method of high-purity semi-insulating silicon carbide monocrystalline |
| CN107974712A (en) * | 2017-11-14 | 2018-05-01 | 山东天岳先进材料科技有限公司 | A kind of preparation method of Semi-insulating silicon carbide mono-crystal |
| CN110203933B (en) * | 2019-04-28 | 2022-11-22 | 河北同光半导体股份有限公司 | Method for reducing nitrogen impurity content in silicon carbide powder |
| CN109989103A (en) * | 2019-05-23 | 2019-07-09 | 广州南砂晶圆半导体技术有限公司 | A kind of method of circulating-heating synthesis bulky grain SiC powder |
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