CN106637418A - Heat treatment method for SiC gemstone - Google Patents
Heat treatment method for SiC gemstone Download PDFInfo
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- CN106637418A CN106637418A CN201611126162.5A CN201611126162A CN106637418A CN 106637418 A CN106637418 A CN 106637418A CN 201611126162 A CN201611126162 A CN 201611126162A CN 106637418 A CN106637418 A CN 106637418A
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- graphite crucible
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention belongs to the technical field of treatment of SiC gemstones, and particularly relates to a heat treatment method for the SiC gemstone. The heat treatment method for the SiC gemstone comprises the following steps of (1) putting a treated SiC gemstone particle into a small porous graphite crucible; (2) putting the small porous graphite crucible into a large graphite crucible to enable the center of the small porous graphite crucible and the center of the large graphite crucible to be on the same axis; (3) filling the large graphite crucible and the periphery of the outer part of the small porous graphite crucible with SiC powder; (4) putting a graphite crucible comprising the small porous graphite crucible and the large graphite crucible into an induction heating furnace, putting an insulation quilt at the periphery of the outer part of the large graphite crucible, and gradually heating to 1000-1500 DEG C; and (5) introducing an inert gas into the induction heating furnace, keeping the pressure in the induction heating furnace to 0.5 atm to 1 atm, and completing the heat treatment of the SiC gemstone. By means of the method, the sublimation of the surface of the SiC gemstone in the process of heat treatment is effectively prevented, and the homogeneity of the quality of the SiC gemstone is improved.
Description
Technical field
The invention belongs to SiC gemstone treatment technical fields, and in particular to a kind of heat treatment method of SiC jewels.
Background technology
Refractive index reflects the ability of crystal refracted light, jewel made by high-index material day light can glisten
With presentation gloss.Hardness embodies the ability of the opposing scribing of jewel, and stability ensure that jewel wear for a long time and
Use.SiC has high refractive index (2.5-2.7), very high hardness (Mohs' hardness 8.5-9.25), and SiC is extremely stable,
More than 1000 DEG C of high temperature is resistant in air, therefore SiC single crystal is especially suitable for making jewel.Prepared by big straight SiC crystal
Common method is physical vapor transport.Sic powder is put into into the crucible bottom of closed graphite composition, is covered on crucible solid
A fixed seed crystal, the diameter of seed crystal will determine the diameter of crystal.Powder is up to sublimation temperature point in the presence of induction coil,
Si, Si that distillation is produced2C and SiC2Molecule is transferred to seed crystal face in the presence of axial-temperature gradient from raw material surface,
The purpose for reaching growth SiC single crystal is slowly crystallized in seed crystal face.The single-crystal silicon carbide of growth, is processed into using line cutting technology
Square thick jewel, recycles the techniques such as polishing and facet to be processed into jewel.
In SiC single crystal growth course, affected by factors such as raw material, thermal field and growth techniques, can be introduced in SiC single crystal
Certain defect, such as micro-pipe, dislocation, wrappage.In addition, in SiC single crystal cutting and process engineering, can be in SiC jewels
Surface causes certain surface damage.The introducing of defect and surface damage can change the color and refractive index for affecting jewel, reduce precious
The quality of stone, it is therefore desirable to which the impact of defect and surface damage is reduced by post processing.Method more traditional at present is direct
SiC jewels after processing are put into into graphite crucible bottom, because SiC jewels can distil in high-temperature heat treatment process, are produced
Raw Si, Si2C and SiC2Deng gaseous component, the main heat-treated temperature of rate of sublimation and surrounding environment gaseous component concentration
Affect, temperature is raised or surrounding gaseous component concentration reduces all promoting SiC jewels to distil, and distillation can cause surface of SiC recessed
Convex injustice, affects jewel outward appearance, because heat treatment adopts inert gas shielding, without Si, Si in atmosphere2C and SiC2Etc. gas phase
Component, therefore SiC jewels are easier to distil；Further, since in heat treatment process, because ambient temperature is higher than center temperature
Degree, causes the SiC gemstone treatment effects of center and surrounding inconsistent.Therefore how to design at a kind of high heat of SiC gem qualities
Reason method becomes the technical problem of this area urgent need to resolve.
The content of the invention
The present invention is directed to the deficiencies in the prior art, it is proposed that a kind of heat treatment method of SiC jewels, and the method is by adopting
The crucible group of size graphite crucible composition, can adopt higher heat treatment temperature, lift the treatment effect to imperfections in precious stones,
SiC gemstone surfaces distillation in heat treatment process is prevented, the homogeneity of SiC gem qualities is improved.
To solve above-mentioned technical problem, the present invention proposes a kind of heat treatment method of SiC jewels, reality of the invention
Example is applied, is comprised the following steps：（1）SiC jewel particles after processing are put in the little graphite crucible of porous, for by the SiC
Jewel is isolated with SiC powders；（2）The little graphite crucible of the porous is put in big graphite crucible, the little graphite earthenware of the porous is made
The center of crucible is centrally located on same axis with big graphite crucible；（3）In the big graphite crucible, the little graphite crucible of porous
Outer surrounding fills the SiC powders, for heat treatment process in, the SiC powders distil, the gaseous component transmission of generation
The little graphite crucible of the porous is entered inside it, improves the gaseous component concentration around SiC jewels, suppresses SiC gemstone surface liters
China；（4）The graphite crucible group that the little graphite crucible of the porous is constituted with big graphite crucible is put in induction heater, described
Big graphite crucible outside surrounding places insulation quilt, is progressively warming up to 1000 DEG C -1500 DEG C；（5）Lead to into the induction heater
Enter inert gas, and the induction heater internal pressure power is maintained at 0.5atm-1atm, completes the heat treatment of SiC jewels.
Inventor's discovery, the method according to embodiments of the present invention, by using the little graphite crucible of porous and big graphite earthenware
The crucible group of crucible composition carries out the SiC jewels after heat treatment process, can adopt higher heat treatment temperature, is lifted in jewel
The treatment effect of defect, prevents SiC gemstone surfaces distillation in heat treatment process, improves the homogeneity of SiC gem qualities.
Embodiments in accordance with the present invention, the little graphite crucible of the porous is cylinder, and cylindrical tip has closing described many
The upper lid of the little graphite crucible in hole, the porosity of the little graphite crucible of the porous is more than 20%, distils for the SiC powders,
The gaseous component of generation is entered inside it through the little graphite crucible of the porous, improves the gaseous component concentration around SiC jewels,
Suppress the distillation of SiC gemstone surfaces.
Embodiments in accordance with the present invention, the gaseous component is Si, Si2C or SiC2。
Embodiments in accordance with the present invention, the big graphite crucible is cylinder, and the little graphite crucible of porous described in volume ratio is big,
The little graphite crucible of the porous is placed in into center in the big graphite crucible, the graphite crucible group, the big graphite is constituted
The porosity of crucible is less than 10%.
Embodiments in accordance with the present invention, the particle diameter of the SiC powders is less than 1mm.
Embodiments in accordance with the present invention, the inert gas is argon gas and helium.
The present invention at least has the advantages that：Heat treatment method of the present invention is by using the little graphite earthenware of porous
The crucible group of crucible and big graphite crucible composition carries out the SiC jewels after heat treatment process, can adopt higher heat treatment temperature,
The treatment effect to imperfections in precious stones is lifted, SiC gemstone surfaces distillation in heat treatment process is prevented, SiC gem qualities are improved
Homogeneity.
Description of the drawings
Fig. 1 is the apparatus structure schematic diagram of SiC jewels heat treatment method of the present invention.
Wherein, insulation quilt 1, induction coil 2, big graphite crucible 3, the little graphite crucible 4 of porous, SiC jewels 5, SiC powders 6,
Upper lid 7.
Specific embodiment
In order that those skilled in the art more fully understand technical scheme, with reference to specific embodiment to this
Invention is described in further detail, and the embodiments described below is exemplary, is only used for explaining the present invention, and can not allow reason
Solve as limitation of the present invention.
The present invention proposes a kind of heat treatment method of SiC jewels, embodiments in accordance with the present invention, and Fig. 1 is SiC of the present invention
The apparatus structure schematic diagram of jewel heat treatment method, with reference to shown in Fig. 1, comprises the following steps：The first step：By the SiC after processing
The particle of jewel 5 is put in the little graphite crucible 4 of porous, some embodiments of the invention, the little graphite earthenware of porous of the present invention
The concrete shape of crucible is unrestricted, can be for square, soccer star or cylinder, and the present invention is preferably cylindrical, and the cylinder top
End has a upper lid 7 of the little graphite crucible of the closing porous, and the porosity of the little graphite crucible of the porous is more than 20%, for will
SiC jewels are isolated with SiC powders 6, after the completion of convenient heat treatment, SiC powders are separated with SiC jewels；Simultaneously when described
When SiC powders distil, Si, Si of generation2C or SiC2Gaseous component is entered in it through the little graphite crucible of the porous
Portion, improves the gaseous component concentration around SiC jewels, suppresses the distillation of SiC gemstone surfaces.
Embodiments in accordance with the present invention, with reference to shown in Fig. 1, second step：The little graphite crucible of the porous is put into into big graphite
In crucible 3, the center and big graphite crucible for making the little graphite crucible of the porous is centrally located on same axis, be specifically by
The little graphite crucible of the porous is placed in center in the big graphite crucible, some embodiments of the invention, institute of the present invention
The concrete shape for stating big graphite crucible is unrestricted, can be for square, and soccer star or cylinder, the present invention is preferably cylindrical, with
The little graphite crucible of the porous is similar, and the little graphite crucible of porous described in volume ratio is big, it is preferred that the hole of the big graphite crucible
Gap rate is less than 10%, can be by further reducing big graphite in the big graphite crucible outer surface coating or deposited metal carbide
The porosity of crucible is to less than 1%.
Embodiments in accordance with the present invention, with reference to shown in Fig. 1, the 3rd step：In the big graphite crucible, the little graphite earthenware of porous
The SiC powders are filled up and down outside crucible, and the little graphite crucible of the porous is surrounded wherein, for heat treatment process
In, the SiC powders distil, Si, Si of generation2C or SiC2Gaseous component is entered through the little graphite crucible of the porous
Inside it, the gaseous component concentration around SiC jewels is improved, suppress the distillation of SiC gemstone surfaces；Some enforcements of the invention
Example, the particle diameter of SiC powders of the present invention is less than 1mm.
Embodiments in accordance with the present invention, with reference to shown in Fig. 1, the 4th step：By the little graphite crucible of the porous and big graphite earthenware
The graphite crucible group of crucible composition is put in induction heater, and the induction heater takes the mode that induction coil 2 is heated to carry out
Heat up heating, is progressively warming up to 1000 DEG C -1500 DEG C, places insulation quilt 1 up and down outside the big graphite crucible, its
In, a through hole is provided with the insulation quilt center of the top, for detecting the temperature inside crucible.
Embodiments in accordance with the present invention, the 5th step：Inert gas is passed through into the induction heater, and the sensing adds
Hot furnace pressure is maintained at 0.5atm-1atm, completes the heat treatment of SiC jewels, wherein, the concrete species of the inert gas is not
It is restricted, can is one or more in argon gas, helium or neon, some embodiments of the invention, the present invention is excellent
Elect argon gas and helium as.
Inventor's discovery, the method according to embodiments of the present invention, by using the little graphite crucible of porous and big graphite earthenware
The crucible group of crucible composition carries out the SiC jewels after heat treatment process, can adopt higher heat treatment temperature, is lifted in jewel
The treatment effect of defect, prevents SiC gemstone surfaces distillation in heat treatment process, improves the homogeneity of SiC gem qualities.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification, simultaneously for one of ordinary skill in the art, according to the think of of the application
Think, will change in specific embodiments and applications.
Claims (6)
1. a kind of heat treatment method of SiC jewels, it is characterised in that comprise the following steps：
（1）SiC jewel particles after processing are put in the little graphite crucible of porous, for by the SiC jewels and SiC powders every
From；
（2）The little graphite crucible of the porous is put in big graphite crucible, center and the great Shi of the little graphite crucible of the porous is made
Black crucible is centrally located on same axis；
（3）In the big graphite crucible, the little graphite crucible of the porous outer surrounding filling SiC powders, for heat treatment process
In, the SiC powders distil, and the gaseous component of generation is entered inside it through the little graphite crucible of the porous, improves SiC
Gaseous component concentration around jewel, suppresses the distillation of SiC gemstone surfaces；
（4）The graphite crucible group that the little graphite crucible of the porous is constituted with big graphite crucible is put in induction heater, in institute
State big graphite crucible outside surrounding and place insulation quilt, be progressively warming up to 1000 DEG C -1500 DEG C；
（5）Inert gas is passed through into the induction heater, and the induction heater internal pressure power is maintained at 0.5atm-
1atm, completes the heat treatment of SiC jewels.
2. heat treatment method according to claim 1, it is characterised in that the little graphite crucible of the porous is cylinder, circle
Capital end has a upper lid of the little graphite crucible of the closing porous, and the porosity of the little graphite crucible of the porous is more than 20%, is used for
The SiC powders distil, and the gaseous component of generation is entered inside it through the little graphite crucible of the porous, improves SiC precious
Gaseous component concentration around stone, suppresses the distillation of SiC gemstone surfaces.
3. the heat treatment method according to any one of claim 1-2, it is characterised in that the gaseous component is Si, Si2C
Or SiC2。
4. heat treatment method according to claim 1, it is characterised in that the big graphite crucible is cylinder, volume ratio
The little graphite crucible of the porous is big, and the little graphite crucible of the porous is placed in into center in the big graphite crucible, and composition is described
Graphite crucible group, the porosity of the big graphite crucible is less than 10%.
5. the heat treatment method according to any one of claim 1-2, it is characterised in that the particle diameter of the SiC powders is little
In 1mm.
6. heat treatment method according to claim 1, it is characterised in that the inert gas is argon gas and helium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611126162.5A CN106637418B (en) | 2016-12-09 | 2016-12-09 | A kind of heat treatment method of SiC jewel |
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| CN201611126162.5A CN106637418B (en) | 2016-12-09 | 2016-12-09 | A kind of heat treatment method of SiC jewel |
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| CN106637418A true CN106637418A (en) | 2017-05-10 |
| CN106637418B CN106637418B (en) | 2019-04-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113174638A (en) * | 2021-04-27 | 2021-07-27 | 云南鑫耀半导体材料有限公司 | High-temperature secondary annealing method of silicon carbide crystals |
| CN116499241A (en) * | 2023-06-29 | 2023-07-28 | 石家庄中正碳素有限公司 | Graphite crucible roasting furnace and roasting production method |
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| CN1884639A (en) * | 2006-05-29 | 2006-12-27 | 中国科学院物理研究所 | Heat treatment method after silicon carbide monocrystal growth |
| JP2010064919A (en) * | 2008-09-10 | 2010-03-25 | Showa Denko Kk | Method for annealing silicon carbide single crystal material, silicon carbide single crystal wafer, and silicon carbide semiconductor |
| US20110086213A1 (en) * | 2009-10-09 | 2011-04-14 | Sicrystal Ag | Method of producing a silicon carbide bulk single crystal with thermal treatment, and low-impedance monocrystalline silicon carbide substrate |
| CN103114336A (en) * | 2013-03-12 | 2013-05-22 | 中国科学院上海硅酸盐研究所 | Method for annealing silicon carbide wafer |
| JP5561676B2 (en) * | 2010-07-21 | 2014-07-30 | 学校法人関西学院 | SiC semiconductor wafer heat treatment equipment |
| CN104357913A (en) * | 2014-12-07 | 2015-02-18 | 中国电子科技集团公司第四十六研究所 | High-temperature annealing treatment method for silicon carbide crystal |
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| CN1884639A (en) * | 2006-05-29 | 2006-12-27 | 中国科学院物理研究所 | Heat treatment method after silicon carbide monocrystal growth |
| JP2010064919A (en) * | 2008-09-10 | 2010-03-25 | Showa Denko Kk | Method for annealing silicon carbide single crystal material, silicon carbide single crystal wafer, and silicon carbide semiconductor |
| US20110086213A1 (en) * | 2009-10-09 | 2011-04-14 | Sicrystal Ag | Method of producing a silicon carbide bulk single crystal with thermal treatment, and low-impedance monocrystalline silicon carbide substrate |
| JP5561676B2 (en) * | 2010-07-21 | 2014-07-30 | 学校法人関西学院 | SiC semiconductor wafer heat treatment equipment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113174638A (en) * | 2021-04-27 | 2021-07-27 | 云南鑫耀半导体材料有限公司 | High-temperature secondary annealing method of silicon carbide crystals |
| CN113174638B (en) * | 2021-04-27 | 2022-06-03 | 云南鑫耀半导体材料有限公司 | High-temperature secondary annealing method of silicon carbide crystals |
| CN116499241A (en) * | 2023-06-29 | 2023-07-28 | 石家庄中正碳素有限公司 | Graphite crucible roasting furnace and roasting production method |
| CN116499241B (en) * | 2023-06-29 | 2023-08-29 | 石家庄中正碳素有限公司 | Roasting production method of graphite crucible |
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