CN116789453B - Graphite crucible and preparation method and application thereof - Google Patents
Graphite crucible and preparation method and application thereof Download PDFInfo
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- CN116789453B CN116789453B CN202310419234.9A CN202310419234A CN116789453B CN 116789453 B CN116789453 B CN 116789453B CN 202310419234 A CN202310419234 A CN 202310419234A CN 116789453 B CN116789453 B CN 116789453B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 63
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 16
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 15
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 15
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000002006 petroleum coke Substances 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011593 sulfur Substances 0.000 claims abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 10
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 64
- 239000000843 powder Substances 0.000 claims description 26
- 239000010426 asphalt Substances 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 18
- 238000005470 impregnation Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 9
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- 239000000571 coke Substances 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000005087 graphitization Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000006253 pitch coke Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000011300 coal pitch Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/521—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained by impregnation of carbon products with a carbonisable material
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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- C04B2235/52—Constituents or additives characterised by their shapes
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Abstract
The invention discloses a graphite crucible, and a preparation method and application thereof. The preparation method of the invention comprises the following steps: preparing a mixture, crushing and grinding the mixture, pressing, sintering for the first time, dipping, sintering for the second time and graphitizing. According to the invention, the novel composite material is prepared by creatively combining two traditional materials of carbon nitride, graphene and carbon nano tube, pitch coke and petroleum coke and sulfur, and the graphite crucible prepared based on the novel composite material has excellent flexural strength and compressive strength, and the heat conduction performance and the heat stability are greatly improved.
Description
Technical Field
The invention belongs to the field of special graphite, and particularly relates to a graphite crucible, and a preparation method and application thereof.
Background
In recent years, graphite crucibles are mainly suitable for smelting copper, alloy materials, silver and other metal products, more than 80% of domestic high-end graphite crucibles are imported, petroleum coke and asphalt binder are generally combined as main materials in the preparation method, and the graphite crucible prepared by the preparation method has a large improvement space in the aspects of compression strength, breaking strength and other performances.
In recent years, carbon nitride is widely applied to the field of photocatalysis due to good photocatalysis performance, but the application in the field of graphite crucibles is not reported yet; carbon nitride imparts its extremely strong hardness and modulus of elasticity due to its special structure.
The breaking strength of the graphene is 200 times higher than that of the best steel, the graphene has good elasticity, and the stretching amplitude can reach 20% of the self size, besides, the graphene also has good heat conductivity and thermal stability, and the graphene is low in cost and high in cost performance, and is called as a new material king.
The carbon nano tube has good mechanical property, the tensile strength reaches 50-200 GPa, which is 100 times of steel, and is at least an order of magnitude higher than that of the conventional graphite fiber; the elastic modulus of the alloy can reach 1TPa, which is equivalent to that of diamond and is about 5 times of that of steel; the carbon nano tube is a material with the highest specific strength which can be prepared at present, if other materials are taken as a matrix and the carbon nano tube is used for preparing a composite material, the composite material can show good strength, elasticity, fatigue resistance and isotropy, and the performance of the composite material is greatly improved.
Chinese patent CN110590390a discloses a carbon fiber graphite crucible for metallurgical casting furnaces and a method for preparing the same, and the graphite crucible prepared from petroleum coke, carbon fiber, pitch coke, medium-temperature coal pitch of carbon black and modified coal pitch has improved compression and fracture resistance, but has no mention of thermal stability and thermal conductivity.
Therefore, the novel graphite crucible with excellent flexural strength and compressive strength, good heat conductivity and thermal stability is prepared by utilizing the excellent performance of the novel material, and has wide development prospect in the field of special graphite.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a graphite crucible, and a preparation method and application thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a graphite crucible comprises the following steps:
(1) Preparation of the mixture: firstly, placing asphalt coke, petroleum coke, carbon nitride, graphene, carbon nanotubes and sulfur in a constant-temperature mixing pot for first mixing; adding stearic acid into the constant temperature mixing pot after the first mixing is completed, and then carrying out second mixing; adding modified asphalt into the constant-temperature mixing pot after the second mixing is completed, and then carrying out third mixing; cooling treatment is carried out after the third mixing is completed, and then the mixture after the cooling treatment is placed in a material box to be naturally cooled to room temperature, so as to obtain a material a;
(2) Crushing and grinding the mixture: crushing the material a obtained in the step (1) in a crusher, grinding the crushed product after crushing, uniformly mixing the powder obtained after grinding in a mixing pot to obtain a material b, and filling the material b into a material bag for standby;
(3) And (3) pressing: placing the material b obtained in the step (2) into a press die for press molding to obtain a material c;
(4) And (3) primary sintering: carrying out primary sintering treatment on the material c obtained in the step (3) to obtain a material d;
(5) Dipping treatment: placing the material d obtained in the step (4) into an impregnation tank, then starting the equipment, and sucking asphalt liquid into the impregnation tank in vacuum; then pressurizing and impregnating the material d to obtain an impregnated product, and naturally cooling and airing the impregnated product to obtain a material e;
(6) And (3) sintering for the second time: carrying out secondary sintering treatment on the material e obtained in the step (5) to obtain a material f;
(7) Graphitizing: and (3) placing the material obtained in the step (6) into a graphitizing furnace for graphitizing treatment to obtain the graphite crucible.
Preferably, in the step (1), the mass ratio of each raw material is 100 percent: 20-40% of asphalt coke, 10-20% of petroleum coke, 5-10% of carbon nitride, 5-10% of graphene, 5-10% of carbon nano tube, 2-5% of sulfur, 1-2% of stearic acid and the balance of modified asphalt; the first mixing temperature is 90-100 ℃, and the first mixing time is 20-40 min; the second mixing temperature is 160-180 ℃, and the second mixing time is 30-50 min; the third mixing temperature is 160-200 ℃, and the third mixing time is 120-150 min; the temperature of the cooling treatment is controlled between 90 and 110 ℃.
Preferably, in the step (2), the particle size of the powder is controlled to be less than or equal to 80 mu m, and the powder is mixed in a mixing pot for 2-4 hours.
Preferably, in the step (3), the pressing pressure is controlled to be 20-25 MPa, and the density of the material c is controlled to be 1.4-1.6 g/cm 3 。
Preferably, in the step (4), the sintering temperature of the first sintering is 900-1000 ℃ and the roasting time is 50-55d.
Preferably, in the step (5), the pressure of the pressurized impregnation is controlled to be 2-3.5 MPa, and the impregnation time is 3-5h.
Preferably, in the step (6), the sintering temperature of the second sintering is 900-1000 ℃. The roasting time is 35-45d.
Preferably, in the step (7), the graphitization temperature is controlled to be 2600-2800 ℃.
At the same time, the invention also claims the graphite crucible prepared by any one of the above methods.
Meanwhile, the invention also claims the application of the graphite crucible in special graphite materials.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, three novel materials of carbon nitride, graphene and carbon nano tube are creatively added into the preparation of the graphite crucible as raw materials, and compared with the traditional graphite crucible, the graphite crucible product prepared according to the specific proportion has better physical, mechanical and chemical properties;
(2) The graphite crucible prepared by the preparation method inherits good fracture resistance, compression resistance and thermal stability of carbon nitride, graphene and carbon nano tubes, and prolongs the service life of the product; meanwhile, good heat conductivity of graphene and carbon nanotubes is inherited, so that the smelting time of a product can be shortened when the product is used, the smelting efficiency is improved, and energy sources are saved;
(3) The addition of sulfur in the preparation of the method improves the carbon residue rate of the product, helps the wetting and coating of the binder on the carbon material, and helps the carbon formation.
Drawings
FIG. 1 is a flow chart of the production process of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Although the steps of the present invention are arranged by reference numerals, the order of the steps is not limited, and the relative order of the steps may be adjusted unless the order of the steps is explicitly stated or the execution of a step requires other steps as a basis. It is to be understood that the term "and/or" as used herein relates to and encompasses any and all possible combinations of one or more of the associated listed items.
The modified asphalt is a conventional material and is purchased from the wu-ban group limited company.
Example 1
A preparation method of a graphite crucible comprises the following steps:
(1) Preparation of the mixture: firstly, putting 25kg of asphalt coke, 20kg of petroleum coke, 10kg of carbon nitride, 5kg of graphene, 5kg of carbon nano tube and 5kg of sulfur into a constant temperature mixing pot at 95 ℃ for mixing for 30 minutes, then adding 2kg of stearic acid, adjusting the temperature to 170 ℃ and then continuing mixing for 40 minutes, then adding 28kg of modified asphalt, adjusting the temperature to 180 ℃ and then mixing again for 135 minutes, cooling to 100 ℃ after mixing is completed, and then putting the obtained mixture into a material box for cooling to room temperature;
(2) Crushing and grinding the mixture: crushing the materials obtained in the step (1) into powder in a crusher, then putting the crushed powder in an ultrafine mill for milling treatment, and putting the obtained powder with the granularity of 75 mu m into a V-shaped mixing pot for mixing for 3 hours and then filling into a material bag for later use;
(3) And (3) pressing: placing the powder in the material bag in the step (2) into a special press die of 1200 tons, and pressing and forming the powder under the pressure of 25MPa, wherein the density of the formed material is controlled to be 1.5g/cm 3 ；
(4) And (3) primary sintering: placing the product pressed and formed in the step (3) into a roasting kiln at 950 ℃ to be sintered for 53d;
(5) Dipping treatment: placing the roasted product in the step (4) into an impregnation tank, starting equipment, pumping 500kg of asphalt liquid into the tank in vacuum, pressurizing to 3MPa, impregnating for 4 hours, naturally cooling after the impregnation is finished, and airing the product;
(6) And (3) sintering for the second time: putting the product immersed in the step (5) into a roasting kiln at 950 ℃ again for sintering for 40d;
(7) Graphitizing: and (3) placing the sintered product in the step (6) into a graphitizing furnace for graphitizing treatment, wherein the graphitizing temperature is 2700 ℃, and the graphite crucible is obtained.
Example 2
A preparation method of a graphite crucible comprises the following steps:
(1) Preparation of the mixture: firstly, placing 35kg of asphalt coke, 20kg of petroleum coke, 5kg of carbon nitride, 10kg of graphene, 10kg of carbon nano tube and 5kg of sulfur into a constant temperature mixing pot at 95 ℃ for mixing for 30 minutes, then adding 2kg of stearic acid, adjusting the temperature to 170 ℃ and then continuing mixing for 40 minutes, then adding 13kg of modified asphalt, adjusting the temperature to 180 ℃ and then mixing again for 135 minutes, cooling to 100 ℃ after mixing is completed, and then placing the obtained mixture into a material box for cooling to room temperature;
(2) Crushing and grinding the mixture: crushing the materials obtained in the step (1) into powder in a crusher, then putting the crushed powder in an ultrafine mill for milling treatment, and putting the obtained powder with the granularity of 75 mu m into a V-shaped mixing pot for mixing for 3 hours and then filling into a material bag for later use;
(3) And (3) pressing: placing the powder in the material bag in the step (2) into a special press die of 1200 tons, and pressing and forming the powder under the pressure of 25MPa, wherein the density of the formed material is controlled to be 1.5g/cm 3 ；
(4) And (3) primary sintering: placing the product pressed and formed in the step (3) into a roasting kiln at 950 ℃ to be sintered for 53d;
(5) Dipping treatment: placing the roasted product in the step (4) into an impregnation tank, starting equipment, pumping asphalt liquid into the tank in vacuum, pressurizing to 3MPa, impregnating for 4 hours, naturally cooling after the impregnation is finished, and airing the product;
(6) And (3) sintering for the second time: putting the product immersed in the step (5) into a roasting kiln at 950 ℃ again for sintering for 40d;
(7) Graphitizing: and (3) placing the sintered product in the step (6) into a graphitizing furnace for graphitizing treatment, wherein the graphitizing temperature is 2700 ℃, and the graphite crucible is obtained.
Example 3
A preparation method of a graphite crucible comprises the following steps:
(1) Preparation of the mixture: firstly, placing 35kg of asphalt coke, 20kg of petroleum coke, 10kg of carbon nitride, 5kg of graphene, 10kg of carbon nano tube and 5kg of sulfur into a constant temperature mixing pot at 95 ℃ for mixing for 30 minutes, then adding 2kg of stearic acid, adjusting the temperature to 170 ℃ and then continuing mixing for 40 minutes, then adding 13kg of modified asphalt, adjusting the temperature to 180 ℃ and then mixing again for 135 minutes, cooling to 100 ℃ after mixing is completed, and then placing the obtained mixture into a material box for cooling to room temperature;
(2) Crushing and grinding the mixture: crushing the materials obtained in the step (1) into powder in a crusher, then putting the crushed powder in an ultrafine mill for milling treatment, and putting the obtained powder with the granularity of 75 mu m into a V-shaped mixing pot for mixing for 3 hours and then filling into a material bag for later use;
(3) And (3) pressing: placing the powder in the material bag in the step (2) into a special press die of 1200 tons, and pressing and forming the powder under the pressure of 25MPa, wherein the density of the formed material is controlled to be 1.5g/cm 3 ；
(4) And (3) primary sintering: placing the product pressed and formed in the step (3) into a roasting kiln at 950 ℃ to be sintered for 53d;
(5) Dipping treatment: placing the roasted product in the step (4) into an impregnation tank, starting equipment, pumping asphalt liquid into the tank in vacuum, pressurizing to 3MPa, impregnating for 4 hours, naturally cooling after the impregnation is finished, and airing the product;
(6) And (3) sintering for the second time: putting the product immersed in the step (5) into a roasting kiln at 950 ℃ again for sintering for 40d;
(7) Graphitizing: and (3) placing the sintered product in the step (6) into a graphitizing furnace for graphitizing treatment, wherein the graphitizing temperature is 2700 ℃, and the graphite crucible is obtained.
Comparative example 1
A preparation method of a graphite crucible comprises the following steps:
(1) Preparation of the mixture: firstly, 40kg of asphalt coke and 30kg of petroleum coke are placed in a constant temperature mixing pot at 95 ℃ for mixing for 30 minutes, then 2kg of stearic acid is added, the temperature is regulated to 170 ℃ and then mixing is continued for 40 minutes, then 28kg of modified asphalt is added, the temperature is regulated to 180 ℃ and then mixing is carried out again for 135 minutes, after mixing is completed, the temperature is reduced to 100 ℃, and then the obtained mixture is placed in a material box and cooled to room temperature;
(2) Crushing and grinding the mixture: crushing the materials obtained in the step (1) into powder in a crusher, then putting the crushed powder in an ultrafine mill for milling treatment, and putting the obtained powder with the granularity of 75 mu m into a V-shaped mixing pot for mixing for 3 hours and then filling into a material bag for later use;
(3) And (3) pressing: placing the powder in the material bag in the step (2) into a special press die of 1200 tons, and pressing and forming the powder under the pressure of 25MPa, wherein the density of the formed material is controlled to be 1.5g/cm 3 ；
(4) And (3) primary sintering: placing the product pressed and formed in the step (3) into a roasting kiln at 950 ℃ to be sintered for 53d;
(5) Dipping treatment: placing the roasted product in the step (4) into an impregnation tank, starting equipment, pumping asphalt liquid into the tank in vacuum, pressurizing to 3MPa, impregnating for 4 hours, naturally cooling after the impregnation is finished, and airing the product;
(6) And (3) sintering for the second time: putting the product immersed in the step (5) into a roasting kiln at 950 ℃ again for sintering for 40d;
(7) Graphitizing: and (3) placing the sintered product in the step (6) into a graphitizing furnace for graphitizing treatment, wherein the graphitizing temperature is 2700 ℃, and the graphite crucible is obtained.
The graphite crucibles prepared in examples 1 to 3 of the present application were subjected to performance testing as follows:
carbon residue rate: JB/T6774-2017
Flexural strength: GB/T3074.1-2021
Compressive strength: GB/T1431-2019
Shore hardness: GB/T39535-2020
Bulk density: GB/T24528-2009
Resistivity: GB/T24525-2009
Modulus of elasticity: GB/T3074.2-2008
Coefficient of thermal expansion: GB/T3074.4-2016
Thermal conductivity: GB/T8722-2019
Particle size: GB/T21354-2008.
The results are shown in the following table:
TABLE 1 Performance test results of graphite crucible
As can be seen from Table 1, examples 1-3 and comparative example 1 show that the flexural strength, compressive strength, shore hardness, bulk density, thermal conductivity and carbon residue ratio of examples 1-3 are all higher than those of comparative example 1, and the resistivity, thermal expansion coefficient and average particle size are lower than those of comparative example 1, which means that the physical and mechanical properties of the graphite crucible prepared by using carbon nitride, graphene, carbon nanotube and sulfur as raw materials are stronger than those of the graphite crucible prepared from ordinary materials, and the thermal conductivity and thermal stability are improved, and the carbon residue ratio is improved.
The foregoing is a further detailed description of the present invention in connection with specific embodiments, and it is not intended to limit the practice of the invention to such specific embodiments, but it will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and the invention is to be considered as falling within the scope of the invention.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The preparation method of the graphite crucible is characterized by comprising the following steps:
(1) Preparation of the mixture: firstly, placing asphalt coke, petroleum coke, carbon nitride, graphene, carbon nanotubes and sulfur in a constant-temperature mixing pot for first mixing; adding stearic acid into the constant temperature mixing pot after the first mixing is completed, and then carrying out second mixing; adding modified asphalt into the constant-temperature mixing pot after the second mixing is completed, and then carrying out third mixing; cooling treatment is carried out after the third mixing is completed, and then the mixture after the cooling treatment is placed in a material box to be naturally cooled to room temperature, so as to obtain a material a;
(2) Crushing and grinding the mixture: crushing the material a obtained in the step (1) in a crusher, grinding the crushed product after crushing, uniformly mixing the powder obtained after grinding in a V-shaped mixing pot to obtain a material b, and filling the material b into a material bag for later use;
(3) And (3) pressing: placing the material b obtained in the step (2) into a press die for press molding to obtain a material c;
(4) And (3) primary sintering: carrying out primary sintering treatment on the material c obtained in the step (3) to obtain a material d;
(5) Dipping treatment: placing the material d obtained in the step (4) into an impregnation tank, then starting the equipment, and sucking asphalt liquid into the impregnation tank in vacuum; then pressurizing and impregnating the material d to obtain an impregnated product, and naturally cooling and airing the impregnated product to obtain a material e;
(6) And (3) sintering for the second time: carrying out secondary sintering treatment on the material e obtained in the step (5) to obtain a material f;
(7) Graphitizing: placing the material obtained in the step (6) into a graphitizing furnace for graphitizing treatment to obtain the graphite crucible;
in the step (1), the mass ratio of the raw materials is 100 percent: 20-40% of asphalt coke, 10-20% of petroleum coke, 5-10% of carbon nitride, 5-10% of graphene, 5-10% of carbon nano tube, 2-5% of sulfur, 1-2% of stearic acid and the balance of modified asphalt; the first mixing temperature is 90-100 ℃, and the first mixing time is 20-40 min; the second mixing temperature is 160-180 ℃, and the second mixing time is 30-50 min; the third mixing temperature is 160-200 ℃, and the third mixing time is 120-150 min; the temperature of the cooling treatment is controlled between 90 and 110 ℃.
2. The method according to claim 1, wherein in the step (2), the powder is controlled to have a particle size of 80 μm or less, and the powder is mixed in the V-type mixing pot for 2 to 4 hours.
3. The method of producing a graphite crucible as claimed in claim 1, wherein in the step (3), the pressing pressure is controlled to 20 to 25MPa, and the density of the material c is controlled to 1.4 to 1.6g/cm 3 。
4. The method of producing a graphite crucible as defined in claim 1, wherein in the step (4), the sintering temperature for the first sintering is 900 to 1000 ℃ and the firing time is 50 to 55d.
5. The method of producing a graphite crucible as defined in claim 1, wherein in the step (5), the pressure of the pressurized impregnation is controlled to be 2 to 3.5MPa and the impregnation time is controlled to be 3 to 5 hours.
6. The method for producing a graphite crucible as defined in claim 1, wherein in the step (6), the sintering temperature of the second sintering is 900 to 1000 ℃; the roasting time is 35-45d.
7. The method of producing a graphite crucible as defined in claim 1, wherein in the step (7), the graphitization temperature is controlled to be 2600 to 2800 ℃.
8. A graphite crucible prepared by the method of any one of claims 1 to 7.
9. Use of the graphite crucible of claim 8 in the field of specialty graphite.
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