CN109502589A - A method of preparing high-purity silicon carbide powder - Google Patents
A method of preparing high-purity silicon carbide powder Download PDFInfo
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- CN109502589A CN109502589A CN201811338323.6A CN201811338323A CN109502589A CN 109502589 A CN109502589 A CN 109502589A CN 201811338323 A CN201811338323 A CN 201811338323A CN 109502589 A CN109502589 A CN 109502589A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
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Abstract
The invention proposes a kind of methods for preparing high-purity silicon carbide powder, which is characterized in that (1) selects high-purity silicon powder and high-purity carbon dust；(2) primary purification and secondary purification are carried out to high-purity carbon dust, graphite crucible and insulation construction, wherein primary purification is purified using vacuum outgas, and secondary purification uses the high temperature purification under inert gas；(3) high-purity silicon powder in high-purity carbon dust and step (1) that step (2) secondary purification obtains is placed in the graphite crucible that step (2) secondary purification obtains, reaction obtains high-purity silicon carbide powder.The present invention reduces the nitrogen content and metals content impurity of high-purity carbon dust by carrying out pretreatment to carbon dust and graphite crucible and insulation construction, compared to hydrometallurgical process is carried out after synthesizing silicon carbide again, it is more environmentally friendly, and process is simpler, while ensure that and will not introduce impurity from graphite crucible and insulation construction when synthesizing silicon carbide powder.
Description
Technical field
The present invention relates to crystalline material preparation technical field more particularly to a kind of high-purity silicon carbide powder and its preparation sides
Method.
Background technique
As one of most important third generation semiconductor material, single-crystal silicon carbide is because of its broad-band gap, reactance voltage breakdown capability
By force, the advantages that thermal conductivity is high, saturated electrons migration rate is high, and be widely used in civilian lighting, screen is shown, aviation
The fields such as space flight, hyperthermia radiation environment, oil exploration, radar communication and automotive circuit diagram.Single-crystal silicon carbide usually passes through distillation
Method is prepared by sic powder, therefore the purity of sic powder used in sublimed method, granularity and crystal form are to carbon
SiClx monocrystalline quality significantly affects.
Most common SiC powder synthetic method is self-propagating high-temperature synthesis in production at present, is incuded in intermediate frequency electromagnetic
High-purity carbon dust and silicon powder are heated to 2000 DEG C or more in furnace, in argon gas or helium atmosphere (or the gaseous mixture of argon gas and helium
Atmosphere) under synthesizing silicon carbide powder.But with the increase of silicon carbide substrates diameter, sic powder needed for crystal ingot grows single furnace
Amount increases therewith, and the graphite crucible diameter of used production sic powder increases, in reaction process in sidewall of crucible and crucible
The temperature difference of the heart increases, and to ensure going on smoothly for self-propagating high-temperature reaction, it is excessively high crucible wall temperature often occur, leads to sidewall of crucible
Neighbouring synthesis material carbonization so as to cause the decline of yield and the raising of production cost, and makes to dissociate in gained sic powder
Carbon content increases.
For how to improve the purity of synthesizing silicon carbide powder, technical staff increasingly payes attention to, and has also carried out correlative study.
CN103508454B discloses the method for synthesizing silicon carbide raw material three times, and first synthesizing silicon carbide powder at high temperature leads to after crushing
Oxygen high-temperature calcination at 800~1200 DEG C, then calcined sic powder high-temperature vacuum is deaerated, most afterwards through hydrometallurgy
Control to obtain high-purity silicon carbide powder.CN101659412A discloses the method purified to existing sic raw material, through washing, alkali
It washes, pickling removal impurity, then through 1600~1800 DEG C of high-temperature calcinations, 3~5 minutes removal free carbons, finally obtains purity and reach
99.99% high-purity silicon carbide raw material.CN102674357A discloses a kind of high-purity silicon carbide for silicon carbide monocrystal growth
The synthetic method of raw material, pretreatment process: high-purity Si powder and high-purity C powder being put into crucible, are subsequently placed in heating furnace, to adding
Growth room's pumping high vacuum of hot stove is to 1 × 10-3Pa hereinafter, raise the temperature to 600~1300 DEG C simultaneously.CN102701208A is public
A kind of high temperature process heat method of high-purity silicon carbide powder is opened, hypertonic solutions process: high-purity Si and C powder are put into earthenware
It in crucible, is subsequently placed in heating furnace, to growth room's pumping high vacuum of heating furnace to 9 × 10-4Pa hereinafter, raise the temperature to simultaneously
600~1300 DEG C, holding 2 hours or more (Fruit storage, including carbon dust, silicon powder and crucible).CN105417541A is disclosed
A kind of preparation method of high-purity silicon carbide powder, the raw material mixed is placed in high purity graphite crucible, graphite crucible is set
In Medium Frequency Induction Heating Furnace；High-purity H is injected into furnace chamber when not beginning to warm up2To 800mbar, pressure is then kept
800mbar, and keep H2It is persistently filled with 1 hour；Equipment is vacuumized, so that vacuum degree reaches 5 × 10-6Mbar, then slowly
Slightly below 1000 DEG C are warming up to, certain time is stopped, so that vacuum degree reaches 5 × 10 again-6mbar.CN101302011A is disclosed
A kind of artificial synthesis of the high-pure SiC power for semiconductor single-crystal growth, taken Si powder and C powder are uniformly mixed
After be put into crucible, crucible is placed in Medium Frequency Induction Heating Furnace, growth room is vacuumized, raises the temperature to 1000 DEG C.
CN103708463A discloses a kind of preparation method of feather weight high-pure SiC power, and graphite crucible is plated carbon film by (1)；(2) will
The graphite crucible of plated carbon film plates silicon carbide.
The method of the purifying silicon carbide powder disclosed in above-mentioned existing patent document is right again after synthesizing silicon carbide raw material
Sic powder is purified, and leads to oxygen calcining removal free carbon in 800 DEG C or more high temperature, then remove gold by hydrometallurgical processes
Belong to impurity.Although above-mentioned prior art improves the purity of powder, but process is tedious, and hydrometallurgical processes pollution is big, increases
Production cost, while sic powder is easy to harden after hydrometallurgical processes re-dry, be unfavorable for crystal growth, such as uses powder
Broken technique crushes the sic powder of agglomeration, and is easily introduced new impurity.
It discloses in above-mentioned existing patent document and is first located in advance before high-purity carbon dust and high-purity silicon powder carry out synthetic reaction
Reason, preprocess method is by carbon dust and silicon powder while to carry out purification processes, and part side reaction may be caused in purification process,
So that purifying is not thorough enough, the purity of sic powder finally will affect.
Summary of the invention
The present invention problem not high for the sic powder purity of prior art synthesis, provides a kind of high-purity silicon carbide
Powder preparation method, the preparation method comprises the following steps: (1) selecting high-purity silicon powder and high-purity carbon dust；(2) to high-purity carbon
Powder, graphite crucible and insulation construction carry out primary purification and secondary purification, wherein and primary purification is purified using vacuum outgas, and two
Secondary purification is using the high temperature purification under inert gas；(3) in the high-purity carbon dust and step (1) for obtaining step (2) secondary purification
High-purity silicon powder be placed in the graphite crucible that step (2) secondary purification obtains, reaction obtain high-purity silicon carbide powder.The preparation side
The process of method is simple and environmentally-friendly, low energy consumption, and the purity is high of gained sic powder.
On the one hand, the present invention provides a kind of method for preparing high-purity silicon carbide powder, the preparation method includes following
Step: (1) high-purity silicon powder and high-purity carbon dust are selected；(2) to high-purity carbon dust, graphite crucible and insulation construction carry out primary purification and
Secondary purification, wherein primary purification is purified using vacuum outgas, and secondary purification uses the high temperature purification under inert gas；(3) will
The high-purity silicon powder in high-purity carbon dust and step (1) that step (2) secondary purification obtains is placed in the stone that step (2) secondary purification obtains
In black crucible, reaction obtains high-purity silicon carbide powder.
The present invention only carries out purification processes to high-purity carbon dust, graphite crucible and insulation construction, the reason is as follows that: silicon powder first
The temperature for melting distillation is far below carbon dust, and silicon powder can liquefy and even gasify at a temperature of same treatment, causes damages；Secondly as
Graphite crucible and insulation construction are graphite material, if purified with graphite crucible to silicon powder, silicon powder can be with graphite crucible
It is reacted, causes to corrode.And if purified using low temperature to silicon powder, the nitrogen adsorbed on silicon powder first is due to temperature
Low, desorption degree is low, when preparing sic powder using these silicon powder high temperature, wherein the nitrogen adsorbed can still take off at high temperature
It is attached；Secondly low temperature desorption can not make the distillation volatilization of part metals impurity, and purification purpose is not achieved.
Why the present invention purifies high-purity carbon dust, graphite crucible and insulation construction twice, and concrete reason is as follows:
Vacuum outgas purification main purpose is the nitrogen and part metals impurity for removing crucible absorption, makes to be adsorbed on carbon by high-temperature vacuum
Nitrogen desorption in powder, crucible, while so that part metals impurity is volatilized by elevated temperature in vacuo.Using the height under inert gas
The main purpose of temperature purification is the nitrogen in removal heat preservation, and due to keeping the temperature material properties itself, temperature outside is than crucible
Temperature is low, it is therefore necessary to which heat preservation heats up when by improving crucible heating temperature, to carry out nitrogen desorption.Meanwhile being passed through helium
Or/and the purpose of argon gas is the nitrogen preferably displaced in carbon dust, crucible and heat preservation, further decreases nitrogen content.
Further, high-purity silicon powder described in step (1) and the molar ratio of high-purity carbon dust are 0.9-1.2.
Further, after step (3), further include the steps that low temperature is carried out to high-purity silicon carbide powder leads to oxygen calcining.
Further, in step (2), the concrete operations of the vacuum outgas purification are as follows: high-purity carbon dust is placed in
In graphite crucible, under vacuum conditions by graphite crucible and insulation construction, heating degassing purification.
Further, it is warming up to 1000-1500 DEG C, degassing purification 5-20h.Preferably, it is warming up to 1200-1400 DEG C,
Degassing purification 8-15h.It is furthermore preferred that 1300 DEG C are warming up to, degassing purification 10h.
Further, in step (2), the concrete operations of the high temperature purification under the inert gas are as follows: to graphite crucible
With inert gas is passed through in insulation construction, be to slowly warm up to 1800-2300 DEG C and purified, obtain low nitrogen content and low metal is miscellaneous
High-purity carbon dust, graphite crucible and the insulation construction of matter content.
Further, described to be to slowly warm up to the time that 1800-2300 DEG C is purified as 5-50h.Preferably, described
Being to slowly warm up to the time that 1900-2200 DEG C is purified is 10-40h.It is furthermore preferred that described be to slowly warm up to 2100 DEG C of progress
The time of purification is 30h.
Further, the inert gas is selected from argon gas and/or helium.
Further, the concrete operations of the step (3) are as follows: high-purity carbon dust that step (2) secondary purification is obtained and
High-purity silicon powder in step (1) mixes, and is placed in the graphite crucible that step (2) secondary purification obtains, later, graphite crucible is existed
Heated under vacuum carries out synthetic reaction；After synthetic reaction, it is passed through inert gas, slowly heating progress conversion reaction obtains
High-purity silicon carbide powder.
Further, the temperature of the synthetic reaction is 1000-1500 DEG C, and the time of synthetic reaction is 5-15h.It is preferred that
, the temperature of the synthetic reaction is 1200-1400 DEG C, and the time of synthetic reaction is 8-12h.It is furthermore preferred that the synthesis is anti-
The temperature answered is 1300 DEG C, and the time of synthetic reaction is 10h.
Further, the temperature of the conversion reaction is 1800-2300 DEG C, and the time of conversion reaction is 5-50h.It is preferred that
, the temperature of the conversion reaction is 1900-2200 DEG C, and the time of conversion reaction is 15-30h.It is furthermore preferred that the conversion is anti-
The temperature answered is 2100 DEG C, and the time of conversion reaction is 25h；
Further, the inert gas is selected from argon gas and/or helium.
Further, the low temperature leads to oxygen calcining to lead to air roasting 3h or more at 500-1000 DEG C.Preferably, described
Low temperature leads to oxygen calcining to lead to air roasting 10h at 800 DEG C.
On the other hand, the present invention also provides a kind of high-purity silicon carbide powders, prepare high-purity silicon carbide powder by above-mentioned
Method be prepared.
The invention has the following beneficial effects:
1. the present invention before synthesizing silicon carbide, is contained by the nitrogen content that pretreatment reduces high-purity carbon dust with metal impurities
Amount, it is more environmentally friendly compared to carrying out hydrometallurgical process after synthesizing silicon carbide again, and process is simpler.
2. the present invention purifies graphite crucible and insulation construction while purification to high-purity carbon dust, without mentioning in batches
Pure, to achieve the purpose that energy-saving, while while ensure that synthesizing silicon carbide powder, will not be from graphite crucible and insulation construction
Middle introducing impurity, improves the purity of synthesizing silicon carbide powder.
3. the present invention, which leads to oxygen calcining using low temperature, removes extra free carbon, more energy saving, single-crystal silicon carbide can be reduced
Carbon inclusion enclave quantity and microtubule content in growth.
Specific embodiment
General idea of the invention is illustrated in order to clearer, is described in detail below with reference to following specific embodiments,
But it does not limit the scope of the invention.
Embodiment 1
The method for preparing high-purity silicon carbide powder, the preparation method comprising the following specific steps
(1) molar ratio of offer high-purity silicon powder and high-purity carbon dust, high-purity silicon powder and high-purity carbon dust is 0.9；
(2) high-purity carbon dust is placed in graphite crucible, then graphite crucible and insulation construction is placed in heating furnace, it is right
Heating stove evacuation makes vacuum degree reach 1x10-4Mbar is warming up to 1000 DEG C and is de-gassed purification, continues 8h；
(3) at step (2) described temperature, inert gas is injected in Xiang Suoshu heating furnace, is to slowly warm up to 1800 DEG C again
It is secondary to be purified, the purification time be 20h, obtain low nitrogen content and low metal impurity content carbon dust and graphite crucible and heat preservation knot
Structure；
(4) step (3) high-purity carbon dust is uniformly mixed with step (1) described high-purity silicon powder, it is described is placed in step (3)
In graphite crucible after purification, graphite crucible and step (3) described insulation construction are placed in heating furnace, stove evacuation will be heated
Vacuum degree is set to reach 1x10-4Mbar is warming up to 1000 DEG C of progress synthetic reactions, reacts and continues 10h；
(5) inert gas is injected at step (4) described temperature to 800mbar, is to slowly warm up to 1800 DEG C and is converted
30h is reacted, sic powder is obtained；
(6) step (5) described sic powder is led to air roasting 3h or more at 600 DEG C, removes extra free carbon,
High-purity silicon carbide powder after being purified.
Embodiment 2
The method for preparing high-purity silicon carbide powder, the preparation method comprising the following specific steps
(1) molar ratio of offer high-purity silicon powder and high-purity carbon dust, high-purity silicon powder and high-purity carbon dust is 1.2；
(2) high-purity carbon dust is placed in graphite crucible, then graphite crucible and insulation construction is placed in heating furnace, it is right
Heating stove evacuation makes vacuum degree reach 1x10-4Mbar is warming up to 1500 DEG C and is de-gassed purification, continues 6h；
(3) at step (2) described temperature, inert gas is injected in Xiang Suoshu heating furnace, is to slowly warm up to 2300 DEG C again
It is secondary to be purified, the purification time be 15h, obtain low nitrogen content and low metal impurity content carbon dust and graphite crucible and heat preservation knot
Structure；
(4) step (3) high-purity carbon dust is uniformly mixed with step (1) described high-purity silicon powder, it is described is placed in step (3)
In graphite crucible after purification, graphite crucible and step (3) described insulation construction are placed in heating furnace, stove evacuation will be heated
Vacuum degree is set to reach 1x10-4Mbar is warming up to 1500 DEG C of progress synthetic reactions, reacts and continues 9h；
(5) inert gas is injected at step (4) described temperature to 1000mbar, is to slowly warm up to 2300 DEG C and is converted
20h is reacted, sic powder is obtained；
(6) step (5) described sic powder is led to air roasting 3h or more at 800 DEG C, removes extra free carbon,
High-purity silicon carbide powder after being purified.
Embodiment 3
The method for preparing high-purity silicon carbide powder, the preparation method comprising the following specific steps
(1) molar ratio of offer high-purity silicon powder and high-purity carbon dust, high-purity silicon powder and high-purity carbon dust is 1.1；
(2) high-purity carbon dust is placed in graphite crucible, then graphite crucible and insulation construction is placed in heating furnace, it is right
Heating stove evacuation makes vacuum degree reach 1x10-4Mbar is warming up to 1100 DEG C and is de-gassed purification, continues 10h；
(3) at step (2) described temperature, inert gas is injected in Xiang Suoshu heating furnace, is to slowly warm up to 1900 DEG C again
It is secondary to be purified, the purification time be 15h, obtain low nitrogen content and low metal impurity content carbon dust and graphite crucible and heat preservation knot
Structure；
(4) step (3) high-purity carbon dust is uniformly mixed with step (1) described high-purity silicon powder, it is described is placed in step (3)
In graphite crucible after purification, graphite crucible and step (3) described insulation construction are placed in heating furnace, stove evacuation will be heated
Vacuum degree is set to reach 1x10-4Mbar is warming up to 1100 DEG C of progress synthetic reactions, reacts and continues 12h；
(5) inert gas is injected at step (4) described temperature to 900mbar, is to slowly warm up to 2100 DEG C and is converted
30h is reacted, sic powder is obtained；
(6) step (5) described sic powder is led to air roasting 3h or more at 700 DEG C, removes extra free carbon,
High-purity silicon carbide powder after being purified.
Embodiment 4
The method for preparing high-purity silicon carbide powder, the preparation method comprising the following specific steps
(1) molar ratio of offer high-purity silicon powder and high-purity carbon dust, high-purity silicon powder and high-purity carbon dust is 1.0；
(2) high-purity carbon dust is placed in graphite crucible, then graphite crucible and insulation construction is placed in heating furnace, it is right
Heating stove evacuation makes vacuum degree reach 1x10-4Mbar is warming up to 1300 DEG C and is de-gassed purification, continues 5h；
(3) at step (2) described temperature, inert gas is injected in Xiang Suoshu heating furnace, is to slowly warm up to 2200 DEG C again
It is secondary to be purified, the purification time be 15h, obtain low nitrogen content and low metal impurity content carbon dust and graphite crucible and heat preservation knot
Structure；
(4) step (3) high-purity carbon dust is uniformly mixed with step (1) described high-purity silicon powder, it is described is placed in step (3)
In graphite crucible after purification, graphite crucible and step (3) described insulation construction are placed in heating furnace, stove evacuation will be heated
Vacuum degree is set to reach 1x10-4Mbar is warming up to 1200 DEG C of progress synthetic reactions, reacts and continues 15h；
(5) inert gas is injected at step (4) described temperature to 1000mbar, is to slowly warm up to 2200 DEG C and is converted
10h is reacted, sic powder is obtained；
(6) step (5) described sic powder is led to air roasting 3h or more at 700 DEG C, removes extra free carbon,
High-purity silicon carbide powder after being purified.
Embodiment 5
The method for preparing high-purity silicon carbide powder, the preparation method comprising the following specific steps
(1) molar ratio of offer high-purity silicon powder and high-purity carbon dust, high-purity silicon powder and high-purity carbon dust is 1.0；
(2) high-purity carbon dust is placed in graphite crucible, then graphite crucible and insulation construction is placed in heating furnace, it is right
Heating stove evacuation makes vacuum degree reach 1x10-4Mbar is warming up to 1200 DEG C and is de-gassed purification, continues 8h；
(3) at step (2) described temperature, inert gas is injected in Xiang Suoshu heating furnace, is to slowly warm up to 2200 DEG C again
It is secondary to be purified, the purification time be 20h, obtain low nitrogen content and low metal impurity content carbon dust and graphite crucible and heat preservation knot
Structure；
(4) step (3) high-purity carbon dust is uniformly mixed with step (1) described high-purity silicon powder, it is described is placed in step (3)
In graphite crucible after purification, graphite crucible and step (3) described insulation construction are placed in heating furnace, stove evacuation will be heated
Vacuum degree is set to reach 1x10-4Mbar is warming up to 1500 DEG C of progress synthetic reactions, reacts and continues 10h；
(5) inert gas is injected at step (4) described temperature to 1000mbar, is to slowly warm up to 2300 DEG C and is converted
20h is reacted, sic powder is obtained；
(6) step (5) described sic powder is led to air roasting 3h or more at 600 DEG C, removes extra free carbon,
High-purity silicon carbide powder after being purified.
Comparative example
To become apparent from the purity is high for illustrating silicon carbide obtained by the method for the present invention, to using commonsense method and the method for the present invention system
The impurity content of the silicon carbide obtained is detected, and detection method uses GDMS (glow discharge spectrometry).Test data such as table 1
It is shown.
Table 1 uses the impurity content of silicon carbide made from commonsense method and the method for the present invention
It can be seen that the impurity content for using silicon carbide made from method of the invention as the impurity content data of table 1
It is lower, only 1.78ppm wt, far below the impurity content 21.29ppm wt using silicon carbide made from commonsense method.Using
The content of every kind of impurity of silicon carbide made from method of the invention, also below using the corresponding of silicon carbide made from commonsense method
The content of impurity.
Impurity nitrogen content is qualitatively judged by the color of gained silicon carbide, using silicon carbide made from method of the invention
Color is ivory buff, and uses the color of silicon carbide made from commonsense method for green or burnt hair partially, to illustrate using this
The nitrogen content of silicon carbide made from the method for invention is lower.
All the embodiments in this specification are described in a progressive manner, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.
The above description is only an embodiment of the present invention, is not intended to restrict the invention.For those skilled in the art
For, the invention may be variously modified and varied.All any modifications made within the spirit and principles of the present invention are equal
Replacement, improvement etc., should be included within scope of the presently claimed invention.
Claims (10)
1. a kind of method for preparing high-purity silicon carbide powder, which is characterized in that the preparation method comprises the following steps:
(1) high-purity silicon powder and high-purity carbon dust are selected；
(2) primary purification and secondary purification are carried out to high-purity carbon dust, graphite crucible and insulation construction, wherein primary purification uses
Vacuum outgas purification, secondary purification use the high temperature purification under inert gas；
(3) high-purity silicon powder in high-purity carbon dust and step (1) that step (2) secondary purification obtains is placed in step (2) is secondary to be mentioned
In pure obtained graphite crucible, reaction obtains high-purity silicon carbide powder.
2. the method according to claim 1 for preparing high-purity silicon carbide powder, which is characterized in that after step (3), also wrap
It includes and the step of low temperature leads to oxygen calcining is carried out to high-purity silicon carbide powder.
3. the method according to claim 1 for preparing high-purity silicon carbide powder, which is characterized in that described true in step (2)
The concrete operations of sky degassing purification are as follows:
High-purity carbon dust is placed in graphite crucible, under vacuum conditions by graphite crucible and insulation construction, heating degassing mentions
It is pure.
4. the method according to claim 3 for preparing high-purity silicon carbide powder, which is characterized in that be warming up to 1000-1500
DEG C, degassing purification 5-20h；Preferably, it is warming up to 1200-1400 DEG C, degassing purification 8-15h；It is furthermore preferred that being warming up to 1300
DEG C, degassing purification 10h.
5. the method according to claim 1 to 3 for preparing high-purity silicon carbide powder, which is characterized in that in step (2),
The concrete operations of high temperature purification under the inert gas are as follows:
It is passed through inert gas into graphite crucible and insulation construction, 1800-2300 DEG C is to slowly warm up to and is purified, obtains low nitrogen
High-purity carbon dust, graphite crucible and the insulation construction of content and low metal impurity content.
6. the method according to claim 5 for preparing high-purity silicon carbide powder, which is characterized in that
It is described to be to slowly warm up to the time that 1800-2300 DEG C is purified as 5-50h；Preferably, described to be to slowly warm up to 1900-
2200 DEG C of times purified are 10-40h；It is to slowly warm up to the time that 2100 DEG C are purified it is furthermore preferred that described and is
30h；
The inert gas is selected from argon gas and/or helium.
7. the method according to claim 1 for preparing high-purity silicon carbide powder, which is characterized in that the tool of the step (3)
Gymnastics is made as follows: the high-purity silicon powder in the high-purity carbon dust and step (1) that step (2) secondary purification is obtained mixes, and is placed in step
(2) in the graphite crucible that secondary purification obtains, later, graphite crucible is heated under vacuum conditions and carries out synthetic reaction；Synthesis
After reaction, it is passed through inert gas, slowly heating carries out conversion reaction and obtains high-purity silicon carbide powder.
8. the method according to claim 7 for preparing high-purity silicon carbide powder, which is characterized in that
The temperature of the synthetic reaction is 1000-1500 DEG C, and the time of synthetic reaction is 5-15h；Preferably, the synthetic reaction
Temperature be 1200-1400 DEG C, time of synthetic reaction is 8-12h；It is furthermore preferred that the temperature of the synthetic reaction is 1300
DEG C, the time of synthetic reaction is 10h；
The temperature of the conversion reaction is 1800-2300 DEG C, and the time of conversion reaction is 5-50h；Preferably, the conversion reaction
Temperature be 1900-2200 DEG C, time of conversion reaction is 15-30h；It is furthermore preferred that the temperature of the conversion reaction is 2100
DEG C, the time of conversion reaction is 25h；
The inert gas is selected from argon gas and/or helium.
9. the method according to claim 2 for preparing high-purity silicon carbide powder, which is characterized in that the low temperature leads to oxygen calcining
To lead to air roasting 3h or more at 500-1000 DEG C；Preferably, the low temperature leads to oxygen calcining to lead to air roasting at 800 DEG C
10h。
10. the high-pure SiC power being prepared by any method for preparing high-purity silicon carbide powder of claim 1-9
Material.
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| CN201811338323.6A CN109502589A (en) | 2018-11-12 | 2018-11-12 | A method of preparing high-purity silicon carbide powder |
| PCT/CN2018/123715 WO2020098094A1 (en) | 2018-11-12 | 2018-12-26 | Method for preparing high-purity silicon carbide powder |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110078044A (en) * | 2019-04-10 | 2019-08-02 | 张家港宝诚电子有限公司 | It is a kind of to prepare high-purity carbon dust devices and methods therefor using diesel oil |
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| CN115872405B (en) * | 2022-12-30 | 2023-08-08 | 宁波合盛新材料有限公司 | Method for recycling silicon carbide waste |
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| CN110078044A (en) * | 2019-04-10 | 2019-08-02 | 张家港宝诚电子有限公司 | It is a kind of to prepare high-purity carbon dust devices and methods therefor using diesel oil |
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| 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 |
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| CN113788480B (en) * | 2021-09-29 | 2023-12-19 | 浙江大学杭州国际科创中心 | Preparation method of high-purity silicon carbide and corresponding high-purity silicon carbide |
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| CN117049533A (en) * | 2023-09-26 | 2023-11-14 | 黑龙江工业学院 | Method for purifying graphite by electric field induced graphite acid method and application |
| CN117049533B (en) * | 2023-09-26 | 2024-04-30 | 黑龙江工业学院 | Method for purifying graphite by electric field induced graphite acid method and application |
| CN117342560A (en) * | 2023-12-06 | 2024-01-05 | 通威微电子有限公司 | Method and equipment for synthesizing silicon carbide powder |
| CN117342560B (en) * | 2023-12-06 | 2024-02-27 | 通威微电子有限公司 | Silicon carbide powder synthesis method |
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