CN115351629A - BN plate recycling method - Google Patents
BN plate recycling method Download PDFInfo
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- CN115351629A CN115351629A CN202211003211.1A CN202211003211A CN115351629A CN 115351629 A CN115351629 A CN 115351629A CN 202211003211 A CN202211003211 A CN 202211003211A CN 115351629 A CN115351629 A CN 115351629A
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004064 recycling Methods 0.000 title claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 128
- 239000002002 slurry Substances 0.000 claims abstract description 111
- 238000005245 sintering Methods 0.000 claims abstract description 80
- 238000000227 grinding Methods 0.000 claims abstract description 52
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 238000000576 coating method Methods 0.000 claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims description 68
- 239000010439 graphite Substances 0.000 claims description 68
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 16
- 239000006229 carbon black Substances 0.000 claims description 9
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 27
- 239000002344 surface layer Substances 0.000 abstract description 9
- 230000005012 migration Effects 0.000 abstract description 6
- 238000013508 migration Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 24
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- 239000002270 dispersing agent Substances 0.000 description 13
- 238000003475 lamination Methods 0.000 description 13
- 239000010410 layer Substances 0.000 description 13
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 13
- 239000002904 solvent Substances 0.000 description 13
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
- B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5062—Borides, Nitrides or Silicides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a recycling method of a BN plate, belonging to the technical field of ceramics, comprising the following steps: coating the used BN plate with a carbon-containing slurry; sintering the BN plate coated with the slurry; and thinning the BN plate after sintering, wherein the thinning thickness is 30-50 um. According to the invention, the used BN plate is coated with the carbon-containing slurry, sintering is carried out, and after sintering, the used BN plate is ground, so that impurities can be effectively removed, and after treatment, the grinding thickness is greatly reduced (0.4-0.8 mm is needed without treatment), so that the BN plate can be continuously used; the YAG has certain fluidity at high temperature, and the phenomenon of migration from a place with high concentration to a place with low concentration exists, the invention utilizes the reaction of carbon and the YAG on the surface layer to promote the migration of the internal YAG to the surface layer, and only 30-50 um is needed to be ground to remove impurities, thereby greatly prolonging the service life of the BN plate.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a recycling method of a BN plate.
Background
The BN plate is generally used in a sintering process of an aluminum nitride substrate and plays a role of firing. Yttrium Aluminum Garnet (YAG) can be generated in the aluminum nitride sintering process, impurities such as a small amount of YAG and aluminum oxide permeate the BN plate in the sintering process, and meanwhile, the small amount of aluminum nitride is also adsorbed on the surface of the BN plate by the YAG, so that the subsequent performances such as sintering appearance, heat conduction and strength of the aluminum nitride substrate are influenced, the service life of the BN plate is greatly reduced, and the production cost is increased.
In the prior art, the BN plate is usually directly ground by grinding treatment so as to remove YAG impurities on the surface, but the grinding needs to be carried out for 0.4-0.8 mm, so that the use of the BN plate is extremely influenced and the resource waste is caused. Therefore, how to treat the used BN plate to remove the YAG on the surface so that it can be used continuously becomes a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for recycling BN plates, which can effectively remove impurities, and greatly reduce the grinding thickness (0.4-0.8 mm is needed without processing) after processing, thereby enabling the BN plates to be continuously used.
In order to achieve the purpose, the invention adopts the technical scheme that:
a recycling method of BN plate comprises the following steps:
coating the used BN plate with a carbon-containing slurry;
sintering the BN plate coated with the slurry;
and thinning the BN plate after sintering, wherein the thinning thickness is 30-50 um.
The inventors of the present invention have found, through extensive studies, that the used BN plate has impurities on the surface thereof, which affects the appearance and performance thereof, and that the continued use thereof affects the sintered appearance, heat conductivity, strength and other properties of the aluminum nitride substrate, and therefore, the BN plate needs to be subjected to a recovery treatment.
The method comprises the steps of coating the used BN plate with the carbon-containing slurry, sintering, grinding after sintering to effectively remove impurities, and greatly reducing the grinding thickness (grinding for 0.4-0.8 mm without treatment) after the treatment so as to enable the BN plate to be continuously used.
The inventors have further studied the mechanism and found that YAG has a certain fluidity at high temperature (sintering), and migrates from a place having a high concentration to a place having a low concentration, and that internal YAG migrates to the surface layer is promoted by the reaction of carbon with the YAG at the surface layer, and that impurities can be removed only by grinding 30 to 50um, thereby greatly improving the service life of the BN plate.
As a preferred embodiment of the present invention, the carbon-containing slurry includes at least one of graphite slurry, carbon black slurry, activated carbon slurry, carbon nanotube slurry, and graphene slurry.
The inventors have found that, when the inorganic carbon source slurry described above is used, the slurry can effectively react with YAG to remove YAG, and the YAG can be removed by grinding, but since the organic carbon source contains H and O, H and O need to be removed before sintering, which greatly increases the number of processing steps and increases the cost, it is necessary to select an inorganic carbon source such as graphite, carbon black, activated carbon, carbon nanotubes, and graphene in the present invention.
As a preferred embodiment of the present invention, the carbonaceous slurry includes at least one of graphite slurry, carbon black slurry, and activated carbon slurry.
As a preferred embodiment of the present invention, the carbonaceous slurry is a graphite slurry.
In a preferred embodiment of the present invention, the graphite slurry has a mass concentration of 10 to 50%; the mass concentration of the carbon black slurry is 10-50%; the mass concentration of the active carbon slurry is 10-50%; the mass concentration of the carbon nano tube slurry is 10-50%; the mass concentration of the graphene slurry is 10-50%.
In the present invention, the mass concentrations of the graphite slurry, the carbon black slurry, the activated carbon slurry, the carbon nanotube slurry, and the graphene slurry are not particularly limited in the present invention, and the effects of promoting migration of YAG inside to the surface layer can be achieved.
That is, one skilled in the art can select the graphite slurry from the group consisting of graphite slurry and graphite powderSpecific coating amount is selected according to mass concentration of carbon black slurry, activated carbon slurry, carbon nanotube slurry and graphene slurry, so that the effect of promoting internal YAG to migrate to a surface layer is achieved, and when the mass concentration of the slurry is low, the coating amount can be increased (more than 10 mg/cm) 2 ) When the concentration of the slurry is high, the coating amount can be reduced appropriately (more than 10 mg/cm) 2 )。
As a preferred embodiment of the present invention, the coating amount of the carbon-containing slurry is 10mg/cm or more 2 . The inventor researches the coating amount of the carbon-containing slurry and finds that the coating amount of the carbon-containing slurry is more than or equal to 10mg/cm 2 When the coating amount is less than 10mg/cm, migration of YAG to the surface layer can be well promoted, so that the YAG can be removed 2 In the process, YAG impurities in the BN plate are not completely removed, and the impurities cannot be removed by grinding the BN plate to 30-50 mu m, so that the coating amount of the carbon-containing slurry is strictly controlled in the invention.
As a preferred embodiment of the present invention, the BN plate is sintered under a nitrogen atmosphere. Under a nitrogen atmosphere, the carbon reacts with YAG to form YN (sintered product) which can then be removed by grinding, and the reaction equation is as follows:
C+N 2 +Y 2 O 3 ·Al 2 O 3 →YN+AlN+CO。
as a preferred embodiment of the present invention, the BN plate sintering is performed in a graphite furnace. The sintering furnace is generally only two types, namely a metal furnace and a graphite furnace, wherein H needs to be introduced when the metal furnace is used 2 Protecting the heating element and the frame, and H 2 Reacts with C and therefore needs to be sintered in a graphite furnace.
As a preferred embodiment of the invention, the sintering temperature is 1400-1900 ℃, preferably 1400-1700 ℃, and the sintering time is 4-8 h. The invention further inspects the influence of the sintering temperature and time on the YAG migration effect, and finds that if the sintering temperature is lower than 1400 ℃ and/or the sintering time is lower than 4h, impurities in the BN plate can not be well migrated, impurities still exist in grinding 50um, and if the sintering temperature is higher than 1900 ℃ and/or the sintering time is higher than 8h, the energy consumption is overlarge, so that the treatment cost is increased.
As a preferred embodiment of the present invention, the thinning treatment is grinding wheel grinding.
As a preferred embodiment of the present invention, the method further comprises laminating the BN plates coated with the slurry before sintering. In the present invention, the slurry-coated BN plate may be sintered in a stacked manner or may be sintered alone.
As a preferred embodiment of the invention, the reduction thickness is 30-50 um.
The invention has the beneficial effects that: (1) According to the invention, the used BN plate is coated with the carbon-containing slurry, sintered and ground after sintering, so that impurities can be effectively removed, and after treatment, the grinding thickness is greatly reduced (0.4-0.8 mm of grinding is needed without treatment), so that the BN plate can be continuously used; (2) Under high temperature (sintering), YAG has certain fluidity and migrates from a place with high concentration to a place with low concentration, the invention utilizes the reaction of carbon and the YAG on the surface layer to promote the migration of the internal YAG to the surface layer, and only 30-50 um is needed to be ground to remove impurities, thereby greatly prolonging the service life of the BN plate.
Drawings
FIG. 1 is a diagram of a used BN plate;
FIG. 2 is a diagram of a BN plate treated after high-temperature sintering in example 1;
FIG. 3 is a view of a BN plate subjected to the grinding treatment of example 1;
FIG. 4 is a view showing a laminate of BN plates according to example 2;
FIG. 5 is a view of a BN plate subjected to grinding treatment of comparative example 1;
FIG. 6 is a drawing of a BN plate subjected to grinding treatment of comparative example 3;
fig. 7 is a view of the BN plate of comparative example 4 after grinding of 50um.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents or instruments used in the present invention are not indicated by manufacturers, and are all conventional products commercially available.
The used BN plates are all the same batch of BN plates used for sintering the aluminum nitride substrate, and as shown in figure 1, the surfaces of the used BN plates have a large amount of impurities.
Example 1
A recycling method of BN plates comprises the following steps:
coating used BN plate (as shown in figure 1) with graphite slurry, wherein the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
placing the BN plate coated with the slurry into a graphite furnace, sintering at 1600 ℃ for 6 hours in a nitrogen atmosphere, wherein the sintered BN plate is shown in figure 2, and thus, a large amount of impurities migrate to the surface after sintering;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 30um, and the grinded BN plate is shown in figure 3, so that the surface is free of impurities after grinding for 30um and can be normally used.
Example 2
A recycling method of BN plate comprises the following steps:
the used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
performing lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, and the laminated BN plate is placed into a graphite furnace as shown in figure 4 and sintered in a nitrogen atmosphere, wherein the sintering temperature is 1600 ℃, and the sintering time is 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 3
A recycling method of BN plates comprises the following steps:
used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 15mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 4
A recycling method of BN plate comprises the following steps:
the used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 20mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 5
A recycling method of BN plate comprises the following steps:
used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 15mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, stacking the BN plate by 50 layers, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1400 ℃ for 8 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50 mu m.
Example 6
A recycling method of BN plate comprises the following steps:
used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 15mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, stacking the BN plate by 50 layers, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1700 ℃ for 4 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 7
A recycling method of BN plate comprises the following steps:
the used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 20mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 10% of graphite powder, 88% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 8
A recycling method of BN plate comprises the following steps:
coating used BN plate (as shown in figure 1) with graphite slurry, wherein the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 50% graphitePowder, 48 percent of absolute ethyl alcohol (solvent) and 2 percent of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Example 9
A recycling method of BN plates comprises the following steps:
coating used BN plate (as shown in figure 1) with graphite slurry, wherein the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of activated carbon, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50 mu m.
Example 10
A recycling method of BN plates comprises the following steps:
coating used BN plate (as shown in figure 1) with graphite slurry, wherein the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% carbon black, 58% absolute ethyl alcohol (solvent), 2% polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Comparative example 1
A recycling method of BN plates comprises the following steps:
coating used BN plate (as shown in figure 1) with graphiteThe coating amount of the graphite slurry is 8mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, wherein the BN plate is 50 layers/laminated, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1600 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um, the thinned BN plate is as shown in figure 5, and a large amount of impurities still exist on the surface after 50um is thinned due to too low coating amount of graphite slurry.
Comparative example 2
A recycling method of BN plate comprises the following steps:
the used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
performing lamination treatment on the BN plate coated with the slurry, namely 50 layers/lamination, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at 1300 ℃ for 6 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um.
Comparative example 3
A recycling method of BN plate comprises the following steps:
the used BN plate (as shown in figure 1) is coated with graphite slurry, and the coating amount of the graphite slurry is 10mg/cm 2 The graphite slurry comprises the following components in percentage by mass: 40% of graphite powder, 58% of absolute ethyl alcohol (solvent) and 2% of polyvinyl butyral (dispersant);
carrying out lamination treatment on the BN plate coated with the slurry, stacking the BN plate by 50 layers, putting the BN plate into a graphite furnace, and sintering the BN plate in a nitrogen atmosphere at the sintering temperature of 1700 ℃ for 2 hours;
and grinding and thinning the BN plate by using a grinding wheel after sintering, wherein the thinning thickness is 50um, and the thinned BN plate is shown in figure 6, and because the sintering time is too short, a large amount of impurities still exist on the surface after 50um is thinned.
Comparative example 4
Comparative example 4 is a used BN plate (see fig. 1), but without any treatment, after grinding 50um, a large amount of impurities still remained on the surface as shown in fig. 7.
Test example
In the recycling methods described in examples 1 to 10 and comparative examples 1 to 4, the coating slurry, the coating amount, the number of stacked layers, the sintering temperature, and the sintering time are shown in table 1, and the experimental results are shown in table 2, in which YN is a sintered product, which is a product of the reaction of carbon and YAG.
TABLE 1
TABLE 2 test results
As can be seen from table 1, the method for recovering a BN plate according to the present invention can effectively remove impurities, and after treatment, it can be reused.
Comparing examples 1 to 10 with comparative example 4, it can be seen that the untreated BN plate has many impurities on the surface after grinding 50um, and after the treatment of the present invention, the impurities are removed after grinding 50um, the surface is smooth, and the BN plate can be reused.
As can be seen from the comparison of example 2 with comparative example 1, if the coating amount is less than 10mg/m 2 Since the coating amount is too low to allow impurities to completely migrate to the surface and thus to be removed, the coating amount needs to be strictly controlled in the present invention.
As can be seen from the comparison of example 2 and comparative example 2, when the sintering temperature is too low, the YAG flowability is poor, and impurities cannot be completely migrated to the surface to be removed, so that the sintering temperature needs to be strictly controlled in the present invention.
As is clear from the comparison of example 2 and comparative example 3, if the sintering time is too short, the impurities cannot be completely migrated to the surface and removed, and thus, it is necessary to control the sintering time so that the impurities are migrated to the surface.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A recycling method of BN plate is characterized by comprising the following steps:
coating the used BN plate with a carbon-containing slurry;
sintering the BN plate coated with the slurry;
and thinning the BN plate after sintering, wherein the thinning thickness is 30-50 um.
2. The method for recycling a BN sheet according to claim 1, wherein the carbonaceous slurry comprises at least one of a graphite slurry, a carbon black slurry, an activated carbon slurry, a carbon nanotube slurry, and a graphene slurry; preferably comprises at least one of graphite slurry, carbon black slurry and activated carbon slurry, and more preferably graphite slurry.
3. The method for recycling a BN plate according to claim 2, wherein the amount of the carbon-containing slurry applied is not less than 10mg/cm 2 。
4. The method of recycling a BN plate as claimed in claim 1, wherein the BN plate is sintered under a nitrogen atmosphere.
5. The method of recycling a BN plate as claimed in claim 4, wherein the BN plate sintering is performed in a graphite furnace.
6. The method for recycling a BN plate according to claim 1, wherein the sintering temperature is 1400 to 1900 ℃.
7. The method for recycling a BN plate according to claim 6, wherein the sintering temperature is 1400 to 1700 ℃.
8. The method of claim 1, wherein the sintering time is 4 to 8 hours.
9. The method of recycling a BN plate as claimed in claim 1, wherein said thinning process is grinding with a grinding wheel.
10. The method for recycling a BN plate according to claim 1, further comprising laminating the BN plate coated with the slurry before sintering.
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