CN116920642B - Mixing method for solid phase synthesis of silicon carbide and synthesis method - Google Patents
Mixing method for solid phase synthesis of silicon carbide and synthesis method Download PDFInfo
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- CN116920642B CN116920642B CN202311183495.1A CN202311183495A CN116920642B CN 116920642 B CN116920642 B CN 116920642B CN 202311183495 A CN202311183495 A CN 202311183495A CN 116920642 B CN116920642 B CN 116920642B
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 172
- 238000002156 mixing Methods 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000010532 solid phase synthesis reaction Methods 0.000 title claims abstract description 40
- 238000001308 synthesis method Methods 0.000 title description 2
- 238000005520 cutting process Methods 0.000 claims abstract description 167
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 144
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 123
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 118
- 239000000463 material Substances 0.000 claims abstract description 112
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 39
- 238000003786 synthesis reaction Methods 0.000 claims description 38
- 229910002804 graphite Inorganic materials 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 20
- 230000003247 decreasing effect Effects 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- 239000003082 abrasive agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract description 40
- 238000001212 derivatisation Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 19
- 239000002245 particle Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 8
- 235000013312 flour Nutrition 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 239000000428 dust Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910021487 silica fume Inorganic materials 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
Classifications
-
- 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
- C01B32/984—Preparation from elemental silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/60—Mixing solids with solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
Abstract
The invention belongs to the technical field of silicon carbide crystal growth derivatization, and particularly relates to a mixing method and a synthesizing method for solid phase synthesis of silicon carbide. The mixing method comprises the following steps: dividing carbon powder and silicon powder into preset parts respectively, alternately paving each part of carbon powder and each part of silicon powder into a mixing container, mixing the carbon powder and the silicon powder to obtain a mixture of the carbon powder, the silicon powder and abrasive, separating the abrasive from the mixture, and obtaining a raw material for solid phase synthesis of silicon carbide after the carbon powder and the silicon powder are uniformly mixed; the mixing treatment process comprises the following steps: sequentially carrying out first mixing and second mixing, and controlling the motor to carry out forward rotation and reverse rotation alternate circulation operation; the abrasive is a hard material cutting block, and the hard material cutting block comprises a volume of 0.9cm 3 ~1.1cm 3 And a volume of 0.45cm 3 ~0.65cm 3 Is a second hard material cutting block. The method can fully mix the carbon powder and the silicon powder and improve the discharge rate of solid phase synthesis.
Description
Technical Field
The invention relates to the technical field of derivatization of silicon carbide crystal growth, in particular to a mixing method and a synthesizing method for solid phase synthesis of silicon carbide.
Background
Silicon carbide is taken as one of wide forbidden band semiconductor materials with excellent physical properties, has particularly great application potential in the aspects of high temperature, high frequency, high power, radiation resistance and the like, is an ideal substrate material for preparing high-temperature, high-frequency, high-power and radiation resistance devices, and is a brand-new corner in the fields of hybrid electric vehicles, high-voltage transmission, LED illumination, aerospace and the like, the acquisition of high-quality SiC crystals is the basis for realizing the excellent properties of the SiC-based devices, and the preparation method of the silicon carbide single crystal is a physical gas phase transport method at present, specifically, silicon carbide polycrystal is taken as a raw material, and the silicon carbide single crystal is obtained through sublimation, transport, surface reaction and crystallization. During sublimation of the silicon carbide polycrystal, the purity, particle size and carbon-silicon ratio of the silicon carbide polycrystal influence the stability of mass transfer, and the stability of mass transfer directly influences the morphology, crystal form and defect distribution of the silicon carbide monocrystal.
At present, in the process of preparing silicon carbide polycrystal, carbon powder and silicon powder are put into a ball mill tank body according to a certain carbon-silicon ratio, carbon powder and silicon powder are mixed through the ball mill, after the mixing is finished, the mixed raw materials are put into a high-temperature preparation furnace for solid-phase synthesis, however, as the relative density difference between the carbon powder and the silicon powder is large, the carbon powder and the silicon powder are difficult to uniformly mix in the ball mill, a mixing dead angle exists, further a product block obtained by solid-phase synthesis is caused, the problems that partial areas are unreacted, the carbonization of the partial areas is too serious and the crystallinity of the raw materials is difficult to be ensured exist, and therefore, the requirement of silicon carbide single crystal preparation on the raw materials cannot be met, and the raw material discharge rate is low.
Disclosure of Invention
The invention aims to solve the problems that in the mixing process of solid phase synthesis silicon carbide in the prior art, due to uneven mixing of carbon powder and silicon powder, the obtained silicon carbide block body has unreacted partial areas, serious carbonization of the partial areas, difficulty in guaranteeing crystallinity and low discharge rate.
To achieve the above object, in a first aspect, the present invention provides a mixing method for solid phase synthesis of silicon carbide, the method comprising:
dividing carbon powder and silicon powder into preset parts respectively, alternately paving each part of carbon powder and each part of silicon powder into a mixing container, wherein the alternately paving is that the carbon powder and the silicon powder are alternately paved, so that the carbon powder and the silicon powder are mixed to obtain a mixture of the carbon powder, the silicon powder and the grinding material for mixing treatment, and separating the grinding material from the mixture to obtain a raw material for solid phase synthesis of silicon carbide after the carbon powder and the silicon powder are uniformly mixed;
the conditions of the mixing treatment include: sequentially carrying out first mixing and second mixing, wherein the value range of the rotating speed of the first mixing is 90 r/min-119 r/min, the value range of the rotating speed of the second mixing is 120 r/min-150 r/min, and controlling a motor used for mixing treatment to carry out forward rotation and reverse rotation alternate circulation operation;
the abrasive is a hard material cutting block, the hard material cutting block comprises a first hard material cutting block and a second hard material cutting block, and the volume of each first hard material cutting block is 0.9cm 3 ~1.1cm 3 Each of said firstThe volume of the two hard material cutting blocks is 0.45cm 3 ~0.65cm 3 。
In some preferred embodiments, the first hard material cutting block is 0.1% -2% by volume and the second hard material cutting block is 0.1% -1% by volume based on the volume of the mixture.
In some preferred embodiments, the hard material cutting block further comprises third hard material cutting blocks, each of which has a volume ranging from 0.2cm 3 -0.4cm 3 。
More preferably, the volume of the first hard material cutting block is 0.1% -2%, the volume of the second hard material cutting block is 0.1% -1%, and the volume of the third hard material cutting block is 0.1% -0.5% based on the volume of the mixture.
In some preferred embodiments, the hard material cutting block is a silicon carbide cutting block.
In some preferred embodiments, the abrasive is added to the carbon powder and the silica fume, respectively, and then the carbon powder containing abrasive and the silica fume containing abrasive are alternately laid into the mixing container.
More preferably, the conditions for alternate laying include: alternately paving each part of carbon powder containing the abrasive and each part of silicon powder containing the abrasive according to a preset sequence;
the preset sequence comprises the following steps: the number of the first hard material cutting blocks in each part of the abrasive-containing carbon powder is gradually decreased in proportion, the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion, the number of the first hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually decreased in proportion, and the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion;
wherein the number of the first hard material cutting blocks and the number of the second hard material cutting blocks are determined based on the total number of the abrasives in each of the abrasive-containing carbon powder or the abrasive-containing silicon powder.
In some preferred embodiments, the conditions of the mixing process further comprise: the interval between the forward rotation and the reverse rotation is 5min-10min, and the time of each forward rotation and each reverse rotation is 20min-40min.
According to the mixing method in the first aspect, carbon powder and silicon powder are uniformly mixed to obtain a raw material for solid phase synthesis of silicon carbide, the molar ratio of the carbon powder to the silicon powder of the raw material for solid phase synthesis of silicon carbide is 1:1.01-1.1, the raw material for solid phase synthesis of silicon carbide is filled into a graphite crucible, the graphite crucible is placed into a synthesis furnace for solid phase synthesis of silicon carbide, the synthesis furnace is vacuumized, inert gas is introduced into a chamber of the synthesis furnace until the temperature of the synthesis furnace reaches 1300-1600 ℃, the temperature is kept for 3-5 h, the temperature is kept to be 600-800 mbar when the pressure in the chamber is reached, the temperature of the synthesis furnace reaches 1800-2300 ℃, the gas in the chamber is pumped out until the pressure in the chamber is 5-20 pa, the pressure is kept for 5-20 h, the inert gas is introduced into the chamber of the synthesis furnace, and the silicon carbide is obtained after cooling.
In some preferred embodiments, when the temperature of the synthesis furnace reaches 1000-1500 ℃, the graphite crucible is made to move downwards in the vertical direction, the downward moving speed is 3-8 mm/h, and when the temperature of the synthesis furnace reaches 1800-2300 ℃, the graphite crucible is made to move upwards in the vertical direction, and the upward moving speed is 3-8 mm/h.
According to the invention, the carbon powder and the silicon powder are divided into preset parts, each part of carbon powder and each part of silicon powder are alternately paved into the mixing container, then the carbon powder and the silicon powder are mixed, forward and reverse transfer circulation operation is carried out in the mixing process, the mixture is firstly mixed at a small rotating speed of 90-119 r/min, then mixed at a large rotating speed of 120-150 r/min, and the use volume is 0.9cm 3 ~1.1cm 3 And a volume of 0.45cm 3 ~0.65cm 3 Is cut of a second hard materialThe block is used as an abrasive for mixing treatment, and the carbon powder and the silicon powder can be mixed more uniformly in the mixing process, so that the carbon powder and the silicon powder are ensured to react fully and uniformly in the solid phase synthesis process of the silicon carbide polycrystalline block, the crystallinity of the polycrystalline block is controlled, and the discharge rate is improved.
Specifically, carbon powder and silicon powder are alternately paved in a mixing container, so that the influence of the relative density difference of the carbon powder and the silicon powder on the full mixing of the carbon powder and the silicon powder can be reduced, the mixing of the carbon powder and the silicon powder is more uniform, and the volume of the mixing container is 0.9cm 3 ~1.1cm 3 And a volume of 0.45cm 3 ~0.65cm 3 The second hard material cutting block is used as a mixed abrasive, so that the auxiliary mixing effect of the abrasive can be exerted to the greatest extent under the condition that the cutting block is not crashed by collision, and the abrasive is easily separated from the mixture after the mixture is finished, so that the raw material for solid phase synthesis of silicon carbide, in which carbon powder and silicon powder are uniformly mixed, is obtained. The solution of the invention is more advantageous for promoting the mixing of carbon powder and silicon powder than using only a first hard material cutting block or only a second hard material cutting block, and than using cutting blocks of other dimensions. In the mixing treatment process, forward and reverse transfer circulation operation is carried out, so that the raw materials can be prevented from being deposited at the bottom of a mixing container, the raw materials are mixed more uniformly, the mixture is firstly mixed at a small rotating speed of 90-119 r/min, heat accumulation caused by high-speed operation can be avoided, and then the mixture is mixed at a large rotating speed of 120-150 r/min, so that the raw materials can be mixed more uniformly.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventor of the invention researches and discovers that when carbon powder and silicon powder are mixed in the process of solid phase synthesis of silicon carbide, the carbon powder and the silicon powder are difficult to uniformly mix, so that a product block obtained by solid phase synthesis is caused, partial areas are unreacted, the partial areas are seriously carbonized, the crystallinity is difficult to ensure, and the discharge rate is low.
In this regard, in a first aspect, the present invention provides a compounding method for solid phase synthesis of silicon carbide, the method comprising:
dividing carbon powder and silicon powder into preset parts respectively, alternately paving each part of carbon powder and each part of silicon powder into a mixing container, wherein the alternately paving is that the carbon powder and the silicon powder are alternately paved, so that the carbon powder and the silicon powder are mixed to obtain a mixture of the carbon powder, the silicon powder and the grinding material for mixing treatment, and separating the grinding material from the mixture to obtain a raw material for solid phase synthesis of silicon carbide after the carbon powder and the silicon powder are uniformly mixed;
the conditions of the mixing treatment include: sequentially carrying out first mixing and second mixing, wherein the value range of the rotating speed of the first mixing is 90 r/min-119 r/min, the value range of the rotating speed of the second mixing is 120 r/min-150 r/min, and controlling a motor used for mixing treatment to carry out forward rotation and reverse rotation alternate circulation operation;
the abrasive is a hard material cutting block, the hard material cutting block comprises a first hard material cutting block and a second hard material cutting block, and the volume of each first hard material cutting block is 0.9cm 3 ~1.1cm 3 The volume of each second hard material cutting block is in the range of 0.45cm 3 ~0.65cm 3 。
The mixing treatment is carried out, the forward and reverse transfer circulation operation is carried out, the first mixing and the second mixing are carried out in sequence, the rotating speed of a motor for the second mixing is 120 r/min-150 r/min, the stirring and mixing effect can be improved, the deposition of raw materials at the bottom of a mixing container is avoided, finally, the influence of large relative density difference between carbon powder and silicon powder can be overcome in the mixing treatment process, the carbon powder and the silicon powder are more uniformly mixed, the full uniform reaction of the carbon powder and the silicon powder is ensured in the solid phase synthesis process of the silicon carbide polycrystalline block, the crystallinity of the polycrystalline block is controlled, and the discharge rate is improved. According to the research of the inventor, if the rotating speed of the second mixed motor is less than 120r/min, the mixing effect of carbon powder and silicon powder is affected, and if the rotating speed is more than 150r/min, heat accumulation is easily caused.
Wherein, the volume is 0.9cm 3 ~1.1cm 3 And a volume of 0.45cm 3 ~0.65cm 3 The mixed abrasive composed of the second hard material cutting blocks can play the role of auxiliary mixing of the abrasive to the greatest extent under the condition that the cutting blocks are not crashed by collision, and the abrasive is easily separated from the mixture after the mixture is finished, so that the raw material for solid phase synthesis of silicon carbide, in which carbon powder and silicon powder are uniformly mixed, is obtained. The solution of the invention is more advantageous for promoting the mixing of carbon powder and silicon powder than using only a first hard material cutting block or only a second hard material cutting block, and than using cutting blocks of other dimensions.
The volume of the first hard material cutting block in the invention may be, for example, 0.9cm 3 、0.95cm 3 、1.0cm 3 、1.05cm 3 、1.1cm 3 The volume of the second hard material cutting block may be, in particular, 0.45cm, for example 3 、0.50cm 3 、0.55cm 3 、0.60cm 3 、0.65cm 3 。
The hard material cutting block may be selected from silicon carbide cutting blocks, graphite cutting blocks, and the like. In some preferred embodiments, the hard material cutting block is a silicon carbide cutting block, and in the preferred embodiment, the silicon carbide cutting block is used, so that impurities are prevented from being introduced into the raw material for synthesizing the silicon carbide through the solid phase synthesis due to the use of the cutting block, and the purity and the discharge rate of the product block obtained through the solid phase synthesis are influenced.
In some preferred embodiments, the first hard material cutting block is 0.1% -2% by volume and the second hard material cutting block is 0.1% -1% by volume based on the volume of the mixture. Under this preferred scheme, more do benefit to make carbon dust and silica flour misce bene, control the volume ratio of first hard material cutting piece be not less than 0.1%, more do benefit to the stirring, control the volume ratio of first hard material cutting piece be not more than 2%, more do benefit to the improvement carbon dust silica flour ratio, improve compounding efficiency, control the volume ratio of second hard material cutting piece be not less than 0.1%, more do benefit to the stirring, control the volume ratio of second hard material cutting piece be not more than 1%, more do benefit to the improvement carbon dust silica flour ratio, improve compounding efficiency. The first hard material cutting block may, for example, comprise 0.1%, 0.4%, 0.7%, 1%, 1.3%, 1.7% and 2% by volume, and the second hard material cutting block may, for example, comprise 0.1%, 0.3%, 0.5%, 0.7%, 0.9% and 1% by volume.
In some preferred embodiments, the hard material cutting block further comprises third hard material cutting blocks, each of which has a volume ranging from 0.2cm 3 -0.4cm 3 . Under the preferred scheme, the carbon powder and the silicon powder are more favorably mixed uniformly, and the volume of the third hard material cutting block is not less than 0.2cm 3 The method is more beneficial to preventing the cutting blocks from being crashed and broken, separating the cutting blocks after the mixing is completed, avoiding the use of screening to separate the cutting blocks, avoiding the introduction of impurities into the raw materials for synthesizing the silicon carbide in a solid phase, and avoiding layering of carbon powder and silicon powder due to larger relative density difference in the screening process.
In some preferred embodiments, the first hard material cutting block is 0.1% -2% by volume, the second hard material cutting block is 0.1% -1% by volume, and the third hard material cutting block is 0.1% -0.5% by volume, based on the volume of the mixture. Under this preferred scheme, more do benefit to make carbon dust and silica flour misce bene, control the volume ratio of first hard material cutting piece be not less than 0.1%, more do benefit to the stirring, control the volume ratio of first hard material cutting piece be not more than 2%, more do benefit to the improvement carbon dust silica flour ratio, improve the compounding efficiency, control the volume ratio of second hard material cutting piece be not less than 0.1%, more do benefit to the stirring, control the volume ratio of second hard material cutting piece be not more than 1%, more do benefit to the improvement carbon dust silica flour ratio, improve the compounding efficiency, control the volume ratio of third hard material cutting piece be not less than 0.1%, more do benefit to the stirring, control the volume ratio of third hard material cutting piece be not more than 0.5%, more do benefit to the improvement silica flour ratio, improve the compounding efficiency. The first hard material cutting block may, for example, have a volume percentage of 0.1%, 0.4%, 0.7%, 1%, 1.3%, 1.7% and 2%, the second hard material cutting block may, for example, have a volume percentage of 0.1%, 0.3%, 0.5%, 0.7%, 0.9% and 1%, and the third hard material cutting block may, for example, have a volume percentage of 0.1%, 0.2%, 0.3%, 0.4%, 0.5%.
One reliable guess for the reason that the use of multi-sized cutting blocks helps to maximize the abrasive assisted mixing while ensuring that the cutting blocks are not broken by impact is to reduce the gap between the cutting blocks, allowing for more thorough mixing.
The method for adding the abrasive is not particularly limited, the abrasive can be placed into the mixing container after each layer of carbon powder and each layer of silicon powder are alternately paved into the mixing container, in some preferred embodiments, the abrasive is respectively added into each part of carbon powder and each part of silicon powder, and then each part of carbon powder containing the abrasive and each part of silicon powder containing the abrasive are alternately paved into the mixing container.
More preferably, the conditions for alternate laying include: alternately paving each part of carbon powder containing the abrasive and each part of silicon powder containing the abrasive according to a preset sequence; the preset sequence comprises the following steps: the number of the first hard material cutting blocks in each part of the abrasive-containing carbon powder is gradually decreased in proportion, the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion, the number of the first hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually decreased in proportion, and the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion; wherein the number of the first hard material cutting blocks and the number of the second hard material cutting blocks are determined based on the total number of the abrasives in each of the abrasive-containing carbon powder or the abrasive-containing silicon powder. According to the preferable scheme, according to the sequence that the number of the first hard material cutting blocks is gradually decreased part by part and the number of the second hard material cutting blocks is gradually increased part by part, each part of carbon powder containing abrasive and each part of silicon powder containing abrasive are paved, the first hard material cutting blocks with larger proportion are paved in the carbon powder and the silicon powder of the lower layer, the second hard material cutting blocks with larger proportion are paved in the carbon powder and the silicon powder of the upper layer, the abrasive effect is better exerted, and the carbon powder and the silicon powder are promoted to be uniformly mixed.
In some preferred embodiments, the conditions of the mixing process further comprise: the interval between the forward rotation and the reverse rotation is 5min-10min, and the time of each forward rotation and each reverse rotation is 20min-40min. Under the preferred scheme, the interval between the forward rotation and the reverse rotation is 5-10min, so that heat accumulation caused by high-speed operation of the ball milling device is avoided, the time of each forward rotation and each reverse rotation is 20-40 min, the effect of promoting material mixing by forward and reverse rotation alternate circulation operation is better exerted, and carbon powder and silicon powder are uniformly mixed.
In some preferred embodiments, the second mixing is performed in the last cycle of the forward rotation and reverse rotation alternating operation, that is, in the last cycle of the forward rotation and reverse rotation alternating operation, the rotating speed of the motor is increased to 120r/min to 150 r/min.
In a second aspect, the present invention provides a method for synthesizing silicon carbide, the method comprising, in order: according to the mixing method of the first aspect, carbon powder and silicon powder are uniformly mixed to obtain a raw material for solid phase synthesis of silicon carbide, the molar ratio of the carbon powder to the silicon powder of the raw material for solid phase synthesis of silicon carbide is 1:1.01-1.1, the raw material for solid phase synthesis of silicon carbide is put into a graphite crucible, the graphite crucible is put into a synthesis furnace for solid phase synthesis of silicon carbide, the synthesis furnace is vacuumized, the temperature of the synthesis furnace is raised to 1300-1600 ℃, the temperature is kept for 3-5 h, inert gas is introduced into a chamber of the synthesis furnace, the pressure is kept when the pressure in the chamber is 600 mbar-800 mbar, the temperature of the synthesis furnace is raised to 1800-2300 ℃, the gas in the chamber is pumped out, the pressure is kept for 5-20 h, the inert gas is introduced into the chamber of the synthesis furnace, and the silicon carbide is obtained after cooling. In the heating process of solid phase synthesis silicon carbide, silicon powder is completely melted at about 1500 ℃, carbon powder reacts with silicon when the temperature reaches more than 2000 ℃, because a temperature gradient exists longitudinally in a graphite crucible, before the reaction temperature reaches more than 2000 ℃, the silicon powder volatilizes to cause the reduction of the silicon content at the bottom of the raw material, so that a carbon-rich layer is formed at the bottom, a silicon-rich layer is formed at the top, the balanced silicon carbide of the silicon-carbon ratio cannot be obtained at the bottom and the top, and if the unbalanced raw material of the carbon-silicon ratio is used for growing silicon carbide single crystals, the defects of wrappage, hexagonal cavities, dislocation, polytype symbiosis and the like are easily caused.
According to the preferred scheme, according to the mixing method of the first aspect, the influence of a large relative density gap between carbon powder and silicon powder is overcome, the carbon powder and the silicon powder are mixed more uniformly, the mole ratio of the carbon powder to the silicon powder is 1:1.01-1.1, the formation of a bottom carbon-rich layer and a top silicon-rich layer can be restrained on the basis of fully mixing the carbon powder and the silicon powder, a product block with balanced carbon-silicon ratio is obtained, the temperature of a synthesis furnace reaches 1300-1600 ℃ under the vacuum condition, the temperature is kept for 3-5 h, the temperature of the synthesis furnace reaches 1800-2300 ℃ when the pressure in a chamber is 600 mbar-800 mbar, the pressure is kept for 5-20 h when the pressure in the chamber is 5 pa-20 pa, the raw materials can be further fully and uniformly reacted on the basis of uniformly mixing the raw materials with the mole ratio of 1:1.01-1.1, the carbon-rich layer and the silicon-rich layer are avoided, the crystallinity of silicon carbide is ensured, and the discharging rate is improved.
In some preferred embodiments, when the temperature of the synthesis furnace reaches 1000-1500 ℃, the graphite crucible is moved downwards in the vertical direction at a speed of 3-8 mm/h, and when the temperature of the synthesis furnace reaches 1800-2300 ℃, the graphite crucible is moved upwards in the vertical direction at a speed of 3-8 mm/h. According to the preferable scheme, on the basis of uniformly mixing raw materials with the molar ratio of carbon powder to silicon powder of 1:1.01-1.1, the graphite crucible is enabled to move downwards at the temperature of 1000-1500 ℃, so that the stripping of adsorbed gas is facilitated, nitrogen is discharged, nitrogen element impurities in silicon carbide are reduced, the graphite crucible is enabled to move upwards at the temperature of 1800-2300 ℃, the longitudinal temperature gradient is facilitated to be increased, and the gas transmission is facilitated.
The invention will be further described in detail with reference to specific examples.
Example 1
A method for solid phase synthesis of silicon carbide comprising the steps of:
according to the capacity of a ball milling tank and the mole ratio of carbon powder to silicon powder of 1:1, calculating the respective mass of the required carbon powder and silicon powder, and respectively dividing the silicon powder and the carbon powder into 5 parts;
step two, alternately paving each part of carbon powder and each part of silicon powder in a ball milling tank, and adding a first silicon carbide cutting block and a second silicon carbide cutting block into the ball milling tank, wherein the volume of each first silicon carbide cutting block is 0.9cm 3 ~1.1cm 3 Each second silicon carbide cutting block had a volume of 0.45cm 3 ~0.65cm 3 The volume ratio of the first silicon carbide cutting block is 0.08 percent and the volume ratio of the second silicon carbide cutting block is 0.08 percent based on the total volume of the carbon powder, the silicon powder and the silicon carbide cutting block;
step three: according to the procedure that the interval between each forward rotation and each reverse rotation of a motor in a ball milling tank is 5min, each forward rotation is 15min, each reverse rotation is 15min, alternating circulation operation of the forward rotation and the reverse rotation of the motor is carried out, so that carbon powder and silicon powder are mixed, wherein the alternating circulation operation is carried out for 8 times, in the first 7 circulation, the rotating speed of the motor is 90r/min, and in the 8 th circulation, the rotating speed of the motor is 120r/min, the mixture of carbon powder, silicon powder and silicon carbide cutting blocks is obtained after the mixing treatment, the silicon carbide cutting blocks are selected from the mixture, and the raw material for solid phase synthesis of silicon carbide, in which the carbon powder and the silicon powder are uniformly mixed, is obtained;
step four: and (3) loading the raw material for solid-phase synthesis of silicon carbide obtained in the step (III) into a graphite crucible, putting the graphite crucible into a synthesis furnace for solid-phase synthesis of silicon carbide, vacuumizing the synthesis furnace, heating to 1700 ℃, preserving heat for 6 hours, introducing inert gas into a chamber of the synthesis furnace, maintaining the pressure until the pressure in the chamber reaches 700mbar, continuously heating to 2400 ℃, extracting gas in the chamber, maintaining the pressure until the pressure in the chamber is 10pa, preserving heat for 25 hours, introducing inert gas into the chamber of the synthesis furnace after the heat preservation is finished, and cooling to obtain a silicon carbide product block.
The thickness of the lower carbonized layer of the product block of example 1 was 13%, and the 8-40 mesh particles were 57.1% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block. The thickness ratio of the carbonized layer is the average value obtained after measuring the thicknesses of 5 positions of the lower carbonized layer.
Example 2
Reference example 1 was made, except that the first silicon carbide cutting block was placed into the ball milling pot with a volume ratio of 1.5% and a volume ratio of 0.8% based on the total volume of carbon powder, silicon powder, and silicon carbide cutting block.
The thickness of the lower carbonized layer of the product block of example 2 was 11.8%, and the 8-40 mesh particles were 64.2% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 3
With reference to example 1, the difference was that a first silicon carbide cutting block, a second silicon carbide cutting block, and a third silicon carbide cutting block, each having a volume of 0.2cm, were added to the ball milling pot 3 -0.4cm 3 The first silicon carbide cutting block had a volume of 0.08%, the second silicon carbide cutting block had a volume of 0.08%, and the third silicon carbide cutting block had a volume of 0.08% based on the volume of the mixture of carbon powder, silicon powder, and silicon carbide cutting blocks.
The thickness of the lower carbonized layer of the product block of example 3 was 12.5%, and the 8-40 mesh particles were 67.8% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 4
Reference is made to example 3, except that the first silicon carbide cutting block has a volume ratio of 1.5%, the second silicon carbide cutting block has a volume ratio of 0.5%, and the third silicon carbide cutting block has a volume ratio of 0.4%.
The thickness of the lower carbonized layer of the product block of example 4 was 11.3%, and the 8-40 mesh particles were 73.5% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 5
With reference to example 3, the difference is that each third silicon carbide cutting block has a volume of 0.15cm 3 -0.18cm 3 The silicon carbide cutting blocks are separated from the mixture by sieving.
The thickness of the lower carbonized layer of the product block of example 5 was 14.6%, and the 8-40 mesh particles were 62.3% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 6
With reference to example 1, the difference is that after the silicon powder and the carbon powder are divided into 5 parts, a first silicon carbide cutting block and a second silicon carbide cutting block are added to each part of the carbon powder and each part of the silicon powder respectively, so as to obtain each part of the carbon powder containing the silicon carbide cutting block and each part of the silicon powder containing the silicon carbide cutting block, the number of the first silicon carbide cutting block is gradually decreased, the number of the second silicon carbide cutting block is gradually increased, the number of the first silicon carbide cutting block is gradually decreased, the number of the second silicon carbide cutting block is gradually decreased, the number of the first silicon carbide cutting block is gradually increased, the number of the second silicon carbide cutting block is gradually decreased, the number of the silicon carbide cutting blocks is alternately paved in a ball mill tank, and after the silicon carbide cutting blocks are alternately paved.
The thickness of the lower carbonized layer of the product block of example 6 was 11.6%, and the 8-40 mesh particles were 65.3% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 7
With reference to example 6, the difference is that the number of the first silicon carbide cutting blocks is decreased in parts by parts according to the number of the first silicon carbide cutting blocks in each part of the carbon powder containing the silicon carbide cutting blocks, the number of the second silicon carbide cutting blocks is increased in parts by parts, the number of the first silicon carbide cutting blocks is decreased in parts by parts, the number of the second silicon carbide cutting blocks is increased in parts by parts, and the carbon powder containing the silicon carbide cutting blocks and the silicon powder containing the silicon carbide cutting blocks are alternately paved in a ball milling tank, and then the third step is performed.
The thickness of the lower carbonized layer of the product block of example 7 was 11.2%, and the 8-40 mesh particles were 75.1% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 8
Reference example 1 was made, except that the motor in the milling pot was run for 30min each time of forward rotation for 30min each time. The thickness of the lower carbonized layer of the product block of example 8 was 10.9%, and the 8-40 mesh particles were 73.4% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 9
Reference example 1 was performed, with the difference that the molar ratio of carbon powder to silicon powder was 1:1.05. The thickness of the lower carbonized layer of the product block of example 9 was 8.2%, and the 8-40 mesh particles were 64.9% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 10
The procedure of example 9 was carried out in accordance with the difference that the temperature was raised to 1400℃in the synthesis furnace and maintained for 4 hours, and the inert gas was introduced into the chamber of the synthesis furnace until the pressure in the chamber became 600mbar, the temperature was continuously raised to 1900℃in the synthesis furnace, and the gas in the chamber was withdrawn and maintained for 10 hours until the pressure in the chamber became 10 pa. The thickness of the lower carbonized layer of the product block of example 10 was 7.7%, and the 8-40 mesh particles were 68.1% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Example 11
With reference to example 10, the difference was that when the temperature of the synthesis furnace reached 1400 ℃, the graphite crucible was moved downward at a rate of 3mm/h in the vertical direction while maintaining the temperature, and the temperature was continuously raised to 1900 ℃ in the synthesis furnace, and the graphite crucible was moved upward at a rate of 3mm/h in the vertical direction while maintaining the temperature. The thickness of the lower carbonized layer of the product block of example 11 was 7.5%, and the 8-40 mesh particles were 69.4% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Comparative example 1
Reference example 1 was made, except that the carbon powder and the silicon powder were not equally divided, and were separately laid into a ball mill pot.
The thickness of the lower carbonized layer of the product block of comparative example 1 was 19.2%, and the 8-40 mesh particles were 32.1% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Comparative example 2
Reference example 1 was made, except that only the first silicon carbide cutting block was added to the milling pot.
The thickness of the lower carbonized layer of the product block of comparative example 2 was 15.8%, and the 8-40 mesh particles were 44.9% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Comparative example 3
Reference example 1 was made, except that only a second silicon carbide cutting block was added to the milling pot.
The thickness of the lower carbonized layer of the product block of comparative example 3 was 16.5%, and the 8-40 mesh particles were 38.9% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Comparative example 4
With reference to example 1, the difference is that the volume of the first silicon carbide cutting block is 1.2cm 3 ~1.4cm 3 。
The thickness of the lower carbonized layer of the product block of comparative example 4 was 15.9%, and the 8-40 mesh particles were 52.4% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
Comparative example 5
Reference example 1 was made, except that only forward rotation was performed, with an interval of 5min between each forward rotation, 16 forward rotations were performed, the first 14 times, the rotational speed of the motor was 90r/min, 15 th to 16 th times, and the rotational speed of the motor was 120r/min.
The thickness of the lower carbonized layer of the product block of comparative example 5 was 18.4%, and the 8-40 mesh particles were 27.8% in the silicon carbide powder obtained by crushing the silicon carbide product block with the silicon carbide crystal block in the growth crystal direction of the silicon carbide product block.
As can be seen from comparative examples 1 and 1, the carbon powder and the silicon powder are alternately laid after being divided into the predetermined parts, so that the carbon powder and the silicon powder can be mixed more uniformly, the crystallinity of the solid phase synthesized silicon carbide is higher, the silicon carbide powder obtained by crushing the silicon carbide product block along the growth crystallization direction of the silicon carbide product block has larger occupation ratio of large particles of 8-40 meshes, and the discharge rate of the solid phase synthesized silicon carbide can be improved. Comparative examples 1 and comparative examples 2 to 4 showed that the volume was 0.9cm 3 ~1.1cm 3 And a volume of 0.45cm 3 ~0.65cm 3 The second hard material cutting blocks are used as abrasive materials together, so that the carbon powder and the silicon powder can be mixed more uniformly, and the crystallinity of the solid phase synthesized silicon carbide is higher. In comparative examples 1 and 5, the carbon powder and the silicon powder can be mixed more uniformly by adopting the forward and reverse transfer circulation operation, and the crystallinity of the solid phase synthesized silicon carbide is higher.
As can be seen from comparative examples 1 and 2, the volume ratio of the first hard material cutting block to the second hard material cutting block is not less than 0.1% based on the volume of the mixture, which is more favorable for uniform mixing of carbon powder and silicon powder and improves the crystallinity of silicon carbide. Comparative example 1 and examples 3-5, adding a third cutting block having a smaller volume than the second cutting block of hard material, more advantageous to the uniform mixing of carbon powder and silicon powder, and improving the crystallinity of silicon carbide, further making the volume of the third cutting block of hard material 0.2cm 3 -0.4cm 3 The method is more beneficial to improving the crystallinity and the discharge rate, and further ensures that the volume ratio of the first hard material cutting block, the second hard material cutting block and the third hard material cutting block is not lower than 0.1%, is more beneficial to uniformly mixing carbon powder and silicon powder, and improves the crystallinity of silicon carbide. As can be seen from comparative examples 1, 6 and 7, the abrasive is added to each of the carbon powder and the silicon powder, and then each of the carbon powder containing abrasive and each of the silicon powder containing abrasive are alternately laid into a mixing container, which is more favorable for uniform mixing of the carbon powder and the silicon powder, and further adopts a specific methodThe number of the first hard material cutting blocks is gradually decreased from part to part, the number of the second hard material cutting blocks is gradually increased from part to part, the uniform mixing of carbon powder and silicon powder is facilitated, and the crystallinity and the discharge rate of silicon carbide are improved. Comparative examples 1 and 8 show that the time for each forward rotation and each reverse rotation is 20min-40min, which is more favorable for uniform mixing of carbon powder and silicon powder and improves the crystallinity and the discharge rate of silicon carbide. As can be seen from comparative example 1 and examples 9-11, the molar ratio of carbon powder to silicon powder is 1:1.01-1.1, which is more favorable for reducing the thickness of the bottom carbon-rich layer, improving the crystallinity and the discharge rate of silicon carbide, heating to the temperature of 1300-1600 ℃ of the synthesis furnace, preserving heat, introducing inert gas into the chamber of the synthesis furnace, maintaining the pressure when the pressure in the chamber is 600-800 mbar, heating to the temperature of 1800-2300 ℃ of the synthesis furnace, preserving heat, and being more favorable for improving the crystallinity and the discharge rate of the silicon carbide.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (7)
1. A mixing method for solid phase synthesis of silicon carbide, characterized in that the method comprises the following steps:
dividing carbon powder and silicon powder into preset parts respectively, alternately paving each part of carbon powder and each part of silicon powder into a mixing container, wherein the alternately paving is that the carbon powder and the silicon powder are alternately paved, so that the carbon powder and the silicon powder are mixed to obtain a mixture of the carbon powder, the silicon powder and the grinding material for mixing treatment, and separating the grinding material from the mixture to obtain a raw material for solid phase synthesis of silicon carbide after the carbon powder and the silicon powder are uniformly mixed;
the conditions of the mixing treatment include: sequentially carrying out first mixing and second mixing, wherein the value range of the rotating speed of the first mixing is 90 r/min-119 r/min, the value range of the rotating speed of the second mixing is 120 r/min-150 r/min, and controlling a motor used for mixing treatment to carry out forward rotation and reverse rotation alternate circulation operation;
the abrasive is a hard material cutting block, the hard material cutting block comprises a first hard material cutting block and a second hard material cutting block, and the volume of each first hard material cutting block is 0.9cm 3 ~1.1cm 3 The volume of each second hard material cutting block is in the range of 0.45cm 3 ~0.65cm 3 ；
Based on the volume of the mixture, the volume of the first hard material cutting block accounts for 0.1% -2%, and the volume of the second hard material cutting block accounts for 0.1% -1%;
adding the abrasive into each part of carbon powder and each part of silicon powder respectively, and then alternately paving each part of carbon powder containing the abrasive and each part of silicon powder containing the abrasive into the mixing container;
the conditions for the alternate laying include: alternately paving each part of carbon powder containing the abrasive and each part of silicon powder containing the abrasive according to a preset sequence;
the preset sequence comprises the following steps: the number of the first hard material cutting blocks in each part of the abrasive-containing carbon powder is gradually decreased in proportion, the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion, the number of the first hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually decreased in proportion, and the number of the second hard material cutting blocks in each part of the abrasive-containing silicon powder is gradually increased in proportion;
wherein the number of the first hard material cutting blocks and the number of the second hard material cutting blocks are determined based on the total number of the abrasives in each of the abrasive-containing carbon powder or the abrasive-containing silicon powder.
2. A method of blending in accordance with claim 1 wherein said hard material cutting blocks further comprise third hard material cutting blocks, each of said third hard material cutting blocks having a volume ranging from 0.2cm 3 -0.4cm 3 。
3. The mixing method according to claim 2, wherein the volume of the first hard material cutting block is 0.1% -2%, the volume of the second hard material cutting block is 0.1% -1%, and the volume of the third hard material cutting block is 0.1% -0.5% based on the volume of the mixture.
4. A method of blending according to claim 1 or 2, wherein the cutting block of hard material is a cutting block of silicon carbide.
5. The compounding method of claim 1, wherein the conditions of the compounding process further comprise: the interval between the forward rotation and the reverse rotation is 5min-10min, and the time of each forward rotation and each reverse rotation is 20min-40min.
6. The method for synthesizing the silicon carbide is characterized by sequentially comprising the steps of uniformly mixing carbon powder and silicon powder to obtain a raw material for solid phase synthesis of the silicon carbide, wherein the carbon powder and the silicon powder are uniformly mixed according to the mixing method of any one of claims 1-5, the molar ratio of the carbon powder to the silicon powder of the raw material for solid phase synthesis of the silicon carbide is 1:1.01-1.1, the raw material for solid phase synthesis of the silicon carbide is filled into a graphite crucible, the graphite crucible is placed into a synthesis furnace for solid phase synthesis of the silicon carbide, the synthesis furnace is vacuumized, inert gas is introduced into a chamber of the synthesis furnace until the temperature of the synthesis furnace reaches 1300-1600 ℃, the pressure in the chamber is 600-800 mbar, the pressure is maintained when the temperature of the synthesis furnace reaches 1800-2300 ℃, the gas in the chamber is pumped out, the pressure is maintained for 5-20 h, the inert gas is introduced into the chamber of the synthesis furnace, and the silicon carbide is obtained after cooling.
7. The method according to claim 6, wherein the graphite crucible is moved downward in the vertical direction at a rate of 3mm/h to 8mm/h when the temperature of the synthesis furnace reaches 1000 ℃ to 1500 ℃, and the graphite crucible is moved upward in the vertical direction at a rate of 3mm/h to 8mm/h when the temperature of the synthesis furnace reaches 1800 ℃ to 2300 ℃.
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