CN114106756A - Seed crystal bonding glue and seed crystal bonding method - Google Patents
Seed crystal bonding glue and seed crystal bonding method Download PDFInfo
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- CN114106756A CN114106756A CN202111421772.9A CN202111421772A CN114106756A CN 114106756 A CN114106756 A CN 114106756A CN 202111421772 A CN202111421772 A CN 202111421772A CN 114106756 A CN114106756 A CN 114106756A
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- 239000013078 crystal Substances 0.000 title claims abstract description 141
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000003292 glue Substances 0.000 title claims description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000853 adhesive Substances 0.000 claims abstract description 71
- 230000001070 adhesive effect Effects 0.000 claims abstract description 71
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 56
- 239000010439 graphite Substances 0.000 claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 238000003763 carbonization Methods 0.000 claims abstract description 18
- 238000005087 graphitization Methods 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 28
- 238000001723 curing Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 14
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 239000011265 semifinished product Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 38
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 37
- 238000010438 heat treatment Methods 0.000 abstract description 23
- 238000000197 pyrolysis Methods 0.000 abstract description 4
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 3
- 230000008646 thermal stress Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 24
- 238000003756 stirring Methods 0.000 description 21
- 238000004528 spin coating Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 3
- 238000004807 desolvation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000005007 epoxy-phenolic resin Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 229910002601 GaN Inorganic materials 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J201/00—Adhesives based on unspecified macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
-
- 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
- C30B33/06—Joining of crystals
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of seed crystal bonding, and provides a seed crystal bonding adhesive and a seed crystal bonding method. When the seed crystal adhesive is used for seed crystal adhesion, the graphene and the adhesive can form a three-dimensional conduction network structure through hot-pressing curing and carbonization-graphitization, the three-dimensional conduction network structure can transmit thermal stress generated by a bearing wafer (such as a silicon carbide wafer) in a heating process, the expansion of microcracks of graphite paper can be prevented, and the adhesion strength of the graphite paper is improved. Meanwhile, the three-dimensional conduction network structure avoids the too fast pyrolysis of the adhesive in the crystal growth process, and solves the problems of crystal thermal decomposition cavities and hexagonal cavities. In addition, the three-dimensional conductive network imparts good thermal conductivity to the graphite paper. In addition, the graphene has a large specific surface area, and can fill gaps formed after carbonization of the adhesive, so that the density of the graphite paper is improved, and the thermal conductivity of the graphite paper is improved.
Description
Technical Field
The invention relates to the technical field of seed crystal bonding, in particular to seed crystal bonding glue and a seed crystal bonding method.
Background
Semiconductor chip structures are divided into substrate, epitaxial and device structures. The substrate usually plays a supporting role, the epitaxy is a specific film required by the device, and the device structure is a topological structure with a certain circuit pattern processed by utilizing the procedures of photoetching, etching and the like. The third generation semiconductor material is mainly divided into silicon carbide (SiC) and gallium nitride (GaN), and compared with the first and second generation semiconductors, the third generation semiconductor material has higher forbidden bandwidth, high breakdown voltage, electric conductivity and thermal conductivity, and is expected to replace the first two generations of semiconductor materials in the fields of high temperature, high pressure, high power and high frequency. Because of the lack of large-size single crystals, the third-generation semiconductor materials are mainly silicon carbide-based silicon carbide epitaxial devices and silicon carbide-based gallium nitride epitaxial devices. Meanwhile, the thermal conductivity of the silicon carbide is about 3 times that of the gallium nitride, so that the silicon carbide epitaxial device has stronger heat conduction capability, the service life of the epitaxial device is longer, the reliability is higher, and a heat dissipation system required by the system is smaller. Silicon carbide is therefore more widely used.
Through many years of research, the technology of growing SiC crystals by using a physical vapor transport method (also called a PVT method) is mature. The SiC crystal is grown typically using a graphite crucible with the SiC feedstock placed in the lower portion of the growth chamber and the seed crystal held in a graphite disk at the top of the growth chamber. By controlling the temperature and pressure conditions of the growth chamber, the SiC raw material is sublimated from the lower part of the crucible and rises to the seed crystal for accumulation growth, and finally the SiC single crystal is obtained.
The seed crystal in the growth system needs to be fixed on a graphite circular plate at the upper part of a graphite crucible, and the fixing method mainly comprises the following steps: mechanical fixation or seed bonding. Due to the machining precision of the graphite circular plate, the mechanical fixation is difficult to avoid the existence of air holes between the back surface of the seed crystal and the graphite circular plate. The traditional seed crystal bonding mainly comprises the following processes: the adhesive is uniformly coated on the back of the seed crystal and the graphite circular plate, so that the seed crystal and the graphite circular plate are tightly adhered, the fixation and the protection of the seed crystal are facilitated, the cracking of the seed crystal can be avoided, and the uniform growth of the SiC crystal can be realized. However, the adhesion between the seed crystal and the graphite circular plate is not tight, and the used adhesive contains certain moisture, in the adhesion heating process, if the adhesive is pyrolyzed too fast, the local boiling phenomenon can occur, and the bubbles caused by boiling can make the local adhesive difficult to effectively connect the seed crystal and the graphite, namely, a local cavity can exist on the interface of the seed crystal and the seed crystal table, the heat conduction difference of the cavity generates a temperature difference, and the temperature difference can make the back of the seed crystal generate decomposition sublimation, thereby causing the generation of a pyrolysis cavity and a hexagonal cavity. In order to overcome the problems of using the adhesive only, scientific researchers introduce a layer of graphite paper between the graphite circular plate and the seed crystal. However, the graphite paper has low carbon residue rate and low bonding strength, and is easy to cause ablation due to seed crystal falling or local infirm bonding in the growth process.
Disclosure of Invention
In view of the above, the present invention provides a seed crystal adhesive and a seed crystal bonding method, and the seed crystal adhesive provided by the present invention can improve the bonding strength of graphite paper in the crystal growth process.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides seed crystal adhesive which comprises an adhesive and graphene.
Preferably, the viscosity of the seed crystal bonding glue is 500-1000 mPa & s/25 ℃.
Preferably, the adhesive comprises one or more of B glue, 502 glue, epoxy resin and phenolic resin.
Preferably, the mass percentage of the adhesive in the seed crystal adhesive glue is 15-30%.
Preferably, the mass percentage of the graphene in the seed crystal adhesive is 30-40%.
Preferably, the solvent of the seed bonding glue comprises a volatile solvent.
Preferably, the volatile solvent comprises diacetone alcohol and/or acetone.
The invention also provides a seed crystal bonding method, which comprises the following steps:
coating glue on two sides of the graphite paper, the part of the graphite circular plate needing to be bonded and the part of the seed crystal needing to be bonded;
sequentially placing the glue-coated graphite paper and the glue-coated seed crystals on the surface of the graphite circular plate coated with the glue, and sequentially performing desolventizing, hot-pressing curing, carbonization and graphitization on the obtained semi-finished product;
the glue is the seed crystal bonding glue in the technical scheme.
Preferably, the carbonization temperature is 600-800 ℃ and the carbonization time is 0.5-1.0 h.
Preferably, the graphitization temperature is 1800-2000 ℃, and the time is 1-2 h.
The invention provides seed crystal adhesive which comprises an adhesive and graphene. When the seed crystal adhesive is used for seed crystal adhesion, graphene and the adhesive can form a three-dimensional conduction network structure through hot-pressing curing, carbonization and graphitization, the three-dimensional conduction network structure can transmit thermal stress generated in a heating process of a bearing wafer (such as a silicon carbide wafer), can prevent microcracks of graphite paper from expanding, and improves the adhesive strength of the graphite paper. Meanwhile, the three-dimensional conduction network structure avoids the too fast pyrolysis of the adhesive in the crystal growth process, and solves the problems of crystal thermal decomposition cavities and hexagonal cavities. In addition, the three-dimensional conductive network imparts good thermal conductivity to the graphite paper. In addition, the graphene has a large specific surface area, and can fill gaps formed after carbonization of the adhesive, so that the density of the graphite paper is improved, and the thermal conductivity of the graphite paper is improved.
The invention also provides a seed crystal bonding method, which comprises the following steps: coating glue on two sides of the graphite paper, the part of the graphite circular plate needing to be bonded and the part of the seed crystal needing to be bonded; sequentially placing the glue-coated graphite paper and the glue-coated seed crystals on the surface of the graphite circular plate coated with the glue, and sequentially performing desolventizing, hot-pressing curing, carbonization and graphitization on the obtained semi-finished product; the glue is the seed crystal bonding glue in the technical scheme. Because the seed crystal adhesive comprises the adhesive and the graphene, the graphene and the adhesive can form a three-dimensional conduction network structure through hot-pressing curing, carbonization and graphitization, the three-dimensional conduction network structure can transmit thermal stress generated by a bearing wafer (such as a silicon carbide wafer) in a heating process, and can prevent microcracks of the graphite paper from expanding, so that the bonding strength of the graphite paper is improved. Meanwhile, the three-dimensional conduction network structure avoids the too fast pyrolysis of the adhesive in the crystal growth process, and solves the problems of crystal thermal decomposition cavities and hexagonal cavities. In addition, the three-dimensional conductive network imparts good thermal conductivity to the graphite paper. In addition, the graphene has a large specific surface area, and can fill gaps formed after carbonization of the adhesive, so that the density of the graphite paper is improved, and the thermal conductivity of the graphite paper is improved.
Drawings
FIG. 1 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 1 glue for 100 hours;
FIG. 2 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 13 glue for 100 hours;
FIG. 3 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing 100h of a seed crystal bonded by using No. 14 glue;
FIG. 4 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 15 glue for 100 hours;
FIG. 5 is a photograph of a bonding surface of a silicon carbide crystal grown for 100 hours with a seed crystal bonded with No. 16 glue.
Detailed Description
The invention provides seed crystal adhesive which comprises an adhesive and graphene.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
In the present invention, the adhesive preferably includes one or more of B glue, 502 glue, epoxy resin and phenolic resin, and further preferably includes B glue, 502 glue, epoxy resin or phenolic resin. In the invention, the mass percentage of the adhesive in the seed crystal adhesive is preferably 15-30%. In the invention, the glue B is glue B in glue AB.
In the present invention, the solvent of the seed crystal bonding paste preferably includes a volatile solvent; in the seed crystal adhesive, the mass percentage of the volatile solvent is preferably 35-45%. In the present invention, the volatile solvent preferably includes diacetone alcohol and/or acetone, and more preferably a mixed solvent of diacetone alcohol and acetone. In the invention, when the volatile solvent is preferably a mixed solvent of diacetone alcohol and acetone, the mass percentage of diacetone alcohol in the seed crystal adhesive is preferably 15-30%; the content of the acetone is preferably 10-20% by mass.
In the invention, the viscosity of the seed crystal bonding glue is preferably 500-1000 mPa & s/25 ℃.
In the present invention, when the volatile solvent is preferably a mixed solvent of diacetone alcohol and acetone, the method for preparing the seed crystal adhesive preferably comprises the steps of:
mixing diacetone alcohol with acetone and graphene in sequence, then stirring and primarily mixing, adding an adhesive, and stirring and finally mixing to obtain the seed crystal adhesive. In the present invention, the rotation speed of the stirring primary mixing is preferably 80rpm to 100rpm, and the time of the stirring primary mixing is not particularly limited as long as diacetone alcohol, acetone and graphene can be uniformly mixed; the rotation speed of the stirring and final mixing is preferably 100 rpm-120 rpm, and the time is preferably 2-4 h.
Mixing diacetone alcohol, acetone and an adhesive in sequence, and stirring and primarily mixing; adding graphene, stirring and mixing to obtain the seed crystal adhesive; the rotation speed of the stirring primary mixing is preferably 100 rpm-120 rpm, and the time of the stirring primary mixing is not particularly limited as long as diacetone alcohol, acetone and the adhesive can be uniformly mixed; the rotation speed of the stirring and final mixing is preferably 100-120 rpm, and the time is preferably 2-4 h.
Carrying out first stirring and mixing on diacetone alcohol and graphene to obtain a first mixture; carrying out second stirring and mixing on the acetone and the adhesive to obtain a second mixture; and mixing the first mixture and the second mixture, and carrying out third stirring and mixing to obtain the seed crystal bonding glue. In the present invention, the rotation speed of the first stirring and mixing is preferably 80rpm to 100rpm, and the time of the first stirring and mixing is not particularly limited as long as diacetone alcohol and graphene can be uniformly mixed; the rotation speed of the second stirring and mixing is preferably 100-120 rpm, and the time of the second stirring and mixing is not particularly limited as long as the acetone and the adhesive can be uniformly mixed; the rotation speed of the third stirring and mixing is preferably 100-120 rpm, and the time of the third stirring and mixing is not particularly limited as long as the first mixture and the second mixture can be uniformly mixed.
The invention also provides a seed crystal bonding method, which comprises the following steps:
coating glue on two sides of the graphite paper, the part of the graphite circular plate needing to be bonded and the part of the seed crystal needing to be bonded;
sequentially placing the glue-coated graphite paper and the glue-coated seed crystals on the surface of the graphite circular plate coated with the glue, and sequentially performing desolventizing, hot-pressing curing, carbonization and graphitization on the obtained semi-finished product;
the seed crystal adhesive is the seed crystal adhesive in the technical scheme.
The invention coats the seed crystal bonding glue on the two surfaces of the graphite paper, the part of the graphite circular plate needing bonding and the part of the seed crystal needing bonding.
In the invention, the thickness of the graphite paper is preferably 0.25-0.5 mm.
In the present invention, the seed preferably comprises a silicon carbide seed.
In the present invention, the coating method is preferably spin coating.
In the invention, the spin coating parameters are preferably selected according to the viscosity of the seed crystal bonding glue, and particularly preferably:
when the viscosity of the seed crystal adhesive is 500-600 mPas/25 ℃, the parameters of the spin coating are preferably four-step spin coating at 500rpm multiplied by 10s, 1000rpm multiplied by 10s, 3000rpm multiplied by 20s and 500rpm multiplied by 10 s.
When the viscosity of the seed crystal adhesive is 600-800 mPa & s/25 ℃, the parameters of the spin coating are preferably four-step spin coating at 500rpm × 10s, 1000rpm × 10s, 4000rpm × 20s and 500rpm × 10 s.
When the viscosity of the seed crystal adhesive is 800-900 mPas/25 ℃, the parameters of the spin coating are preferably four-step spin coating at 500rpm multiplied by 10s, 1000rpm multiplied by 10s, 5000rpm multiplied by 20s and 500rpm multiplied by 10 s.
After the glue is coated, the glue-coated graphite paper and the glue-coated seed crystal are sequentially placed on the surface of the graphite circular plate coated with the glue, and the obtained semi-finished product is sequentially subjected to desolventizing, hot-press curing and carbonization-graphitization.
In the present invention, the desolvation preferably comprises two-stage desolvation or three-stage desolvation; the two-section desolventizing comprises sequentially carrying out one-section desolventizing and two-section desolventizing; the temperature of the first-stage desolventizing agent is preferably 60-80 ℃, the time is preferably 2-3 h, and the time for heating from room temperature to the temperature of the first-stage desolventizing agent is preferably 0.5-2 h; the temperature of the second-stage desolventizing agent is preferably 100-120 ℃, the time is preferably 1-2 hours, and the time from the temperature of the first-stage desolventizing agent to the temperature of the second-stage desolventizing agent is preferably 0.5-2 hours.
In the invention, the three-stage desolventizing process comprises the steps of sequentially carrying out first-stage desolventizing, second-stage desolventizing and third-stage desolventizing; the temperature of the first-stage desolventizing is preferably 60 ℃, the time is preferably 0.5-2 h, and the time for heating from room temperature to the temperature of the first-stage desolventizing is preferably 0.5-2 h; the temperature of the second-stage desolventizing agent is preferably 80 ℃, the time is preferably 0.5-1.0 h, and the time from the temperature of the first-stage desolventizing agent to the temperature of the second-stage desolventizing agent is preferably 0.5-2 h; the temperature of the third-stage desolventizing is preferably 100 ℃, and the time is preferably 0.5-1 h; the time from the temperature of the second-stage desolventizing to the temperature of the third-stage desolventizing is preferably 0.5-2 h.
In the present invention, the hot press curing is preferably gradient hot press curing; the gradient hot-pressing curing procedure is preferably selected according to the type of the adhesive in the seed crystal adhesive, and specifically comprises the following steps:
in the present invention, when the adhesive is preferably B glue, the procedure of gradient thermocompression curing preferably comprises: 2 hours at 150 ℃, 1 hour at 200 ℃, 1 hour at 400 ℃ and 3 hours at 500 ℃; the time for raising the temperature from room temperature to 150 ℃, the time for raising the temperature from 150 ℃ to 200 ℃, the time for raising the temperature from 200 ℃ to 400 ℃ and the time for raising the temperature from 400 ℃ to 500 ℃ are independently preferably 0.5-2 h. In the invention, the pressure of the gradient hot-pressing curing is preferably 200-400 kg in the whole process.
In the present invention, when the adhesive is preferably 502 glue, the procedure of gradient thermocompression curing preferably comprises: multiplying by 3 hours at 100 ℃ and multiplying by 3 hours at 200 ℃; the time for raising the temperature from room temperature to 100 ℃ and the time for raising the temperature from 100 ℃ to 200 ℃ are independently preferably 0.5-2 h. In the invention, the pressure of the gradient hot-pressing curing is preferably 400-600 kg in the whole process.
In the present invention, when the adhesive is preferably an epoxy resin, the procedure of the gradient thermocompression curing preferably includes: 2 hours at 120 ℃, 1 hour at 180 ℃, 1 hour at 300 ℃ and 3 hours at 500 ℃; the time for raising the temperature from room temperature to 120 ℃, the time for raising the temperature from 120 ℃ to 180 ℃, the time for raising the temperature from 180 ℃ to 300 ℃ and the time for raising the temperature from 300 ℃ to 500 ℃ are independently preferably 0.5-2 h. In the invention, the pressure of the gradient hot-pressing curing is preferably 800-1000 kg in the whole process.
In the present invention, when the binder is preferably a phenolic resin, the procedure of the gradient hot press curing preferably comprises: 2 hours at 120 ℃, 1 hour at 180 ℃, 1 hour at 250 ℃ and 3 hours at 400 ℃; the time for raising the temperature from room temperature to 120 ℃, the time for raising the temperature from 120 ℃ to 180 ℃, the time for raising the temperature from 180 ℃ to 250 ℃ and the time for raising the temperature from 250 ℃ to 400 ℃ are independently preferably 0.5-2 h. In the invention, the pressure of the gradient hot-pressing curing is preferably 800-1000 kg in the whole process.
In the invention, the carbonization temperature is preferably 600-800 ℃, and more preferably 700 ℃; the time is preferably 0.5-1.0 h; the time for raising the temperature from room temperature to the carbonization temperature is preferably 0.5-2 h.
In the invention, the graphitization temperature is preferably 1800-2000 ℃, and more preferably 1900 ℃; the time is preferably 1-2 h; the time for raising the temperature from the carbonization temperature to the graphitization temperature is preferably 0.5-2 h.
In the present invention, the carbonization and graphitization processes are preferably performed in a furnace; the carbonization and graphitization with the furnace means that: covering the graphite round plate bonded with the seed crystal on a crucible for crystal growth; in the process of crystal growth, the seed crystal adhesive provided by the invention is carbonized and graphitized. The parameters of the crystal growth are not specifically limited, and can be set according to actual conditions. In the present invention, the carbonization and graphitization process is performed along with the furnace, which can save resources.
The seed crystal bonding paste and the seed crystal bonding method according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Examples
The formulation of the seed bond paste is shown in table 1.
TABLE 1 seed Crystal adhesive formulation
The preparation method of the seed crystal adhesive comprises the following steps:
firstly adding diacetone alcohol, then adding acetone, then adding graphene, stirring and mixing at 80-100 rpm, finally adding an adhesive, and stirring and mixing at 100-120 rpm for 3 h.
The seed crystal bonding method using the seed crystal bonding glue comprises the following steps:
spin-coating silicon carbide seed crystal bonding glue on two surfaces of graphite paper (with the thickness of 0.25mm), the part of a graphite circular plate needing bonding and the part of the silicon carbide seed crystal needing bonding;
sequentially placing the glue-coated graphite paper and the glue-coated silicon carbide seed crystal on the glue-coated surface of the graphite circular plate, and sequentially removing a solvent and carrying out hot-pressing curing on the obtained semi-finished product; adding a silicon carbide material into the crucible, and covering the graphite round cover bonded with the seed crystal in the crucible for crystal growth; and the growth temperature of the crystal is 2100-2300 ℃, the crystal grows for 100 hours, and the morphology of the obtained silicon carbide crystal is observed.
For the formulas 1# -3#, B gum in table 1, the recipe is 1), the spin coating process is 500rpm × 10s, 1000rpm × 10s, 5000rpm × 20s, 500rpm × 10 s; the drying process is 60 multiplied by 2 h; multiplying by 2 hours at 80 ℃; multiplying by 4 hours at 100 ℃;
for the formula 4# -6#, 502 type glue in table 1, the recipe is 2); the spin coating process is 500rpm multiplied by 10s, 1000rpm multiplied by 10s, 4000rpm multiplied by 20s, 500rpm multiplied by 10 s; the drying process is 60 multiplied by 2 h; multiplying by 2 hours at 80 ℃; multiplying by 4 hours at 100 ℃;
for the formulation 7# -12# in table 1, the recipe for the resin glue is 3); the spin coating process is 500rpm × 10s, 1000rpm × 10s, 3000rpm × 20s, 500rpm × 10 s; the drying process is 60 multiplied by 2 h; multiplying by 2 hours at 80 ℃; 100 ℃ for 4 h.
The solvent removal process comprises the following steps: x 2h at 60 ℃; multiplying by 2 hours at 80 ℃; 100 ℃ for 4h, and the time for heating from room temperature to 60 ℃, the time for heating from 60 ℃ to 80 ℃ and the time for heating from 80 ℃ to 100 ℃ are all 1 h.
The procedure of hot-pressing solidification comprises the following steps:
b, glue B: 2 hours at 150 ℃, 1 hour at 200 ℃, 1 hour at 400 ℃ and 3 hours at 500 ℃; the time for heating from room temperature to 150 ℃, the time for heating from 150 ℃ to 200 ℃, the time for heating from 200 ℃ to 400 ℃ and the time for heating from 400 ℃ to 500 ℃ are all 1 h; the pressure is 300kg in the whole process;
glue 502: multiplying by 3 hours at 100 ℃ and multiplying by 3 hours at 200 ℃; the time for heating from room temperature to 100 ℃ and the time for heating from 100 ℃ to 200 ℃ are both 0.5-2 h; the pressure is 500kg in the whole process;
epoxy resin: 2 hours at 120 ℃, 1 hour at 180 ℃, 1 hour at 300 ℃ and 3 hours at 500 ℃; the time for heating from room temperature to 120 ℃, the time for heating from 120 ℃ to 180 ℃, the time for heating from 180 ℃ to 300 ℃ and the time for heating from 300 ℃ to 500 ℃ are all 1 h; the pressure is 900kg in the whole process;
phenolic resin: 2 hours at 120 ℃, 1 hour at 180 ℃, 1 hour at 250 ℃ and 3 hours at 400 ℃; the time for heating from room temperature to 120 ℃, the time for heating from 120 ℃ to 180 ℃, the time for heating from 180 ℃ to 250 ℃ and the time for heating from 250 ℃ to 400 ℃ are all 1 h; the pressure was 800kg throughout.
FIG. 1 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 1 glue for 100 hours; as can be seen from fig. 1: cavities and hexagonal voids are not present in the silicon carbide crystal.
The photo of the bonding surface of the silicon carbide crystal obtained by growing 100h of the glue of example 2# to the glue of 12# is similar to that of FIG. 1.
FIG. 2 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 13 glue for 100 hours; as can be seen from fig. 2: the silicon carbide crystal has back corrosion and hexagonal cavity defects.
FIG. 3 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing 100h of a seed crystal bonded by using No. 14 glue; as can be seen from fig. 3: back corrosion and hexagonal cavity defects of the silicon carbide crystal appear, and are shown in picture 2;
FIG. 4 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 15 glue for 100 hours; as can be seen from fig. 4: the silicon carbide crystal has edge burning defects.
FIG. 5 is a photograph of a bonding surface of a silicon carbide crystal obtained by growing a seed crystal bonded by using No. 16 glue for 100 hours; as can be seen from fig. 5: the silicon carbide crystal has edge burning defects.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The seed crystal adhesive is characterized by comprising an adhesive and graphene.
2. The seed crystal adhesive according to claim 1, wherein the seed crystal adhesive has a viscosity of 500 to 1000 mPa-s/25 ℃.
3. The seed adhesive of claim 1, wherein the adhesive comprises one or more of a B glue, a 502 glue, an epoxy resin, and a phenolic resin.
4. A seed crystal adhesive according to claim 1 or 3, wherein the mass percentage of the adhesive in the seed crystal adhesive is 15-30%.
5. The seed crystal adhesive according to claim 1, wherein the mass percentage of graphene in the seed crystal adhesive is 30-40%.
6. The seed bonding paste as claimed in claim 1, wherein the solvent of the seed bonding paste comprises a volatile solvent.
7. The seed crystal adhesive according to claim 6, wherein the volatile solvent comprises diacetone alcohol and/or acetone.
8. A seed crystal bonding method is characterized by comprising the following steps:
coating glue on two sides of the graphite paper, the part of the graphite circular plate needing to be bonded and the part of the seed crystal needing to be bonded;
sequentially placing the glue-coated graphite paper and the glue-coated seed crystals on the surface of the graphite circular plate coated with the glue, and sequentially performing desolventizing, hot-pressing curing, carbonization and graphitization on the obtained semi-finished product;
the glue is the seed crystal bonding glue as defined in any one of claims 1 to 7.
9. A seed crystal bonding method according to claim 8, wherein the temperature of the carbonization is 600 to 800 ℃ and the time is 0.5 to 1.0 h.
10. A seed crystal bonding method according to claim 8, wherein the graphitization temperature is 1800-2000 ℃ and the time is 1-2 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115815619A (en) * | 2022-12-15 | 2023-03-21 | 天工爱和特钢有限公司 | Binder for binder injection additive manufacturing nickel-based alloy and preparation method and application thereof |
| CN116856066A (en) * | 2023-09-01 | 2023-10-10 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074338A (en) * | 2018-10-22 | 2020-04-28 | Skc株式会社 | Seed crystal with protective film, method of manufacturing the same, method of attaching the same, and method of manufacturing ingot using the same |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074338A (en) * | 2018-10-22 | 2020-04-28 | Skc株式会社 | Seed crystal with protective film, method of manufacturing the same, method of attaching the same, and method of manufacturing ingot using the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115815619A (en) * | 2022-12-15 | 2023-03-21 | 天工爱和特钢有限公司 | Binder for binder injection additive manufacturing nickel-based alloy and preparation method and application thereof |
| CN116856066A (en) * | 2023-09-01 | 2023-10-10 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
| CN116856066B (en) * | 2023-09-01 | 2023-11-14 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
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