CN114195133A - Graphene-containing graphite flake production process and heat dissipation graphite flake - Google Patents
Graphene-containing graphite flake production process and heat dissipation graphite flake Download PDFInfo
- Publication number
- CN114195133A CN114195133A CN202111489132.1A CN202111489132A CN114195133A CN 114195133 A CN114195133 A CN 114195133A CN 202111489132 A CN202111489132 A CN 202111489132A CN 114195133 A CN114195133 A CN 114195133A
- Authority
- CN
- China
- Prior art keywords
- carbonization
- treatment
- graphite
- graphitization
- graphene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 200
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 149
- 239000010439 graphite Substances 0.000 title claims abstract description 149
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 64
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 99
- 238000005087 graphitization Methods 0.000 claims abstract description 77
- 239000000463 material Substances 0.000 claims abstract description 67
- 239000002994 raw material Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 22
- 230000004907 flux Effects 0.000 claims abstract description 13
- 238000003490 calendering Methods 0.000 claims description 26
- 229920001721 polyimide Polymers 0.000 claims description 23
- 239000004642 Polyimide Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000000704 physical effect Effects 0.000 abstract description 6
- 238000011112 process operation Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 46
- 238000004321 preservation Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- -1 graphite alkene Chemical class 0.000 description 15
- 230000009467 reduction Effects 0.000 description 13
- 238000003756 stirring Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 238000005303 weighing Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 229920000747 poly(lactic acid) Polymers 0.000 description 4
- 239000004626 polylactic acid Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000000071 blow moulding Methods 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910021485 fumed silica Inorganic materials 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- MWNQXXOSWHCCOZ-UHFFFAOYSA-M sodium percarbonate Chemical compound [Na+].OOC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-M 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229940095709 flake product Drugs 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 239000008946 yang xin Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
Abstract
The application relates to the technical field of graphite flakes, in particular to a graphene-containing graphite flake production process and a heat dissipation graphite flake. The method comprises the steps of sequentially carrying out preheating treatment, carbonization treatment, graphitization treatment and cooling treatment on a raw material coiled material, directly heating to carry out graphitization treatment after the carbonization treatment is finished, wherein the heating rate of the carbonization treatment is 10-15 ℃/min, and the heating rate of the graphitization treatment is 6-10 ℃/min. The application shortens the time for preparing the graphite flakes to 22-26 h by forming a continuous heating mode in the carbonization process and the graphitization process, simplifies the process operation process, and increases the capacity of enterprises; meanwhile, the graphite flake prepared by the method has the advantages of thin thickness, high heat conductivity coefficient, high toughness, high heat flux, good heat dissipation and long thermal saturation time, thereby improving the physical property of the graphite flake and having high practicability.
Description
Technical Field
The application relates to the technical field of graphite flakes, in particular to a graphene-containing graphite flake production process and a heat dissipation graphite flake.
Background
People search for a raw material more suitable for heat dissipation of electronic products by different methods, wherein the raw material comprises carbonized graphene. Graphene carbide is generally used to manufacture heat dissipation plates due to its advantages of high thermal stability, chemical stability, mechanical stability, light transmittance, and electron mobility.
The preparation of graphite flake usually carries out the carbonization with raw material coiled material (raw material coiled material is the PI membrane) earlier in the present market, after carrying out the graphitization with the midbody that the carbonization made again, just can make the graphite flake, and graphitization and carbonization process are mutually independent, need carry out the carbonization through rising temperature, cool down, rise temperature again and carry out graphitization and cool down again, make the time of graphite flake preparation lengthen, generally need 3 ~6 days to accomplish production and preparation, and technology operation is troublesome, need use the high temperature graphitization stove among the graphitization process, need use the high temperature carbonization stove among the carbonization process, high temperature graphitization stove and high temperature carbonization stove area are big, and rise temperature repeatedly, the operation of cooling increases the energy consumption, need great product area, thereby make the operating cost and the manufacturing cost increase of enterprise.
Disclosure of Invention
In order to solve the above technical problem, the present application provides a graphene-containing graphite sheet production process and a heat dissipation graphite sheet.
In a first aspect, the present application provides a graphene-containing graphite sheet production process, which adopts the following technical scheme: a graphite flake production process containing graphene sequentially carries out preheating treatment, carbonization treatment, graphitization treatment and cooling treatment on a raw material coiled material, after the carbonization treatment is finished, the temperature is directly raised for the graphitization treatment, the temperature rise rate of the carbonization treatment is 10-15 ℃/min, and the temperature rise rate of the graphitization treatment is 6-10 ℃/min.
By adopting the technical scheme, the carbonization process and the graphitization process are integrated, the temperature continuously changes and rises, the graphitization is directly carried out after carbonization, the preparation time of the carbonized graphite flake can be effectively shortened, the preparation process of the graphite flake is shortened to 22-26 h, the process is simple, the capacity is high, the raw material coiled material directly enters graphitization after carbonization, the temperature in the whole process is continuously increased, the temperature is not required to be reduced and then transferred to a graphitization furnace to be raised for graphitization treatment, the operation is simple and quick, and the capacity of enterprises is increased; meanwhile, the graphite flake prepared by the method has the advantages of thin thickness, high heat conductivity coefficient, high toughness, high heat flux, good heat dissipation and long thermal saturation time, thereby improving the physical property of the graphite flake and having high practicability. The carbonization heating rate is 10-15 ℃/min, the graphitization treatment heating rate is 6-10 ℃/min, and by controlling the heating rates of the two treatment processes, on one hand, the polyimide film can be uniformly heated, uniformly carbonized and uniformly graphitized to prepare the graphite sheet with uniform heat conductivity; on the other hand, the structure of the graphene can be kept to be completed in the preparation process of carbonization and graphitization, the possibility of damage of the graphene is reduced, and the heat conducting performance of the prepared graphite sheet is improved.
Preferably, the preheating temperature in the preheating treatment stage is 950-1100 ℃, so as to obtain the preheated raw material coiled material.
Through adopting above-mentioned technical scheme, make the raw materials coiled material can be heated evenly in the in-process of carbonization for the graphite flake product surface that finally makes is smooth level and smooth, in case the raw materials coiled material is heated inhomogeneously, and then the product thickness after the carbonization is uneven, and also probably makes product surface damaged, leads to the product to be unable, and the rejection rate increases.
Preferably, the carbonization treatment stage is used for carbonizing the preheated raw material coiled material, the carbonization temperature is 1500-1700 ℃, and the carbonization time is 5-6 hours, so that the carbonized coiled material is prepared.
Through adopting above-mentioned technical scheme, the carbonization coiled material that the carbonization degree is high that obtains, the temperature can shorten the carbonization time of preheating raw materials coiled material at 1500~1700 ℃ within range, reduces the time cost, and the carbonization time is in 5~6h, and the carbonization degree that can make preheating raw materials coiled material is higher, can reduce effectively simultaneously and preheat the excessive carbonization possibility of raw materials coiled material.
Preferably, the graphitizing treatment stage is used for graphitizing the carbonized coiled material at 2800-3000 ℃ for 5-6 h to obtain the graphite sheet.
Through adopting above-mentioned technical scheme, the graphite flake that the graphitization degree is high that obtains, the temperature is in 2800~3000 ℃ within ranges, can shorten the graphitization time of carbonization coiled material, reduces the time cost, and the carbonization time is in 5~6h, and the graphitization degree that enables the carbonization coiled material is higher, can reduce the excessive graphitization's of carbonization coiled material possibility effectively simultaneously.
Preferably, the cooling rate of the cooling treatment is 2-5 ℃/min, the cooling time is 10-12 h, and the temperature of the cooling treatment is reduced to 20-30 ℃.
Through adopting above-mentioned technical scheme, reduce carbonization graphite alkene because of the temperature reduces the possibility that the shrink appears at the excessive speed, the speed in the stage of cooling is 2~5 ℃/min, can make the temperature evenly reduce, makes the graphite flake get the thickness change less, and the thickness of the graphite flake that makes is even.
Preferably, the raw material coiled material comprises, by weight, 10-20 parts of polyimide and 0.5-1 part of graphene.
Through adopting above-mentioned technical scheme for the graphite flake that arrives has good physical properties, and polyimide's coefficient of thermal expansion is good, has good dielectric property, and polyimide uses with the graphite alkene cooperation, and the graphite flake coefficient of thermal conductivity who makes is high, thickness is thin, toughness is high, intensity is moderate, heat flux is high and good heat dissipation, can be applicable to fields such as mobile device chip, mobile device battery, new forms of energy battery package, photovoltaic module.
Preferably, the using amount ratio of the graphene to the polyimide is (15-20): 1.
by adopting the technical scheme, the graphite flake has the advantages of larger heat flux, better heat conductivity coefficient, better toughness, better heat dissipation and longer heat saturation time. Preferably, the polyimide may also be replaced with other materials, such as polyacrylamide, polyhexamethylene adipamide, or polyetherimide; the substances have good thermal expansion coefficient, and the graphite flake prepared by the substances and the graphene has larger heat flux, better heat conductivity coefficient, better toughness and better heat dissipation.
The graphene can be modified graphene, and the modified graphene is prepared by the following steps:
s1, weighing 1-3 parts of silane coupling agent, 10-15 parts of alcohol solvent, 5-8 parts of water and 15-20 parts of graphene powder according to parts by weight, uniformly stirring, adding 0.1-0.2 part of alkaline catalyst, adjusting the pH value to 8-10, and stirring for reaction to obtain alkaline graphene;
s2, weighing 2-6 parts by weight of polylactic acid, 1-2 parts by weight of titanate coupling agent, 15-20 parts by weight of 1-5% sodium hydroxy carbonate solution and alkaline graphene, uniformly mixing, heating to 60-65 ℃, reacting for 0.5-1 h, keeping the reaction in a stirring state all the time in the reaction process, adding 3-5 parts by weight of fumed silica, stirring for 20-30 min, filtering, and drying to obtain the modified graphene.
This application regards as the silicon dioxide precursor with silane coupling agent, alcoholic solution and aqueous solution, do benefit to silane coupling agent and disperse in the graphite alkene surface, under the effect of alkaline catalyst, make alkaline graphite alkene, alkaline graphite alkene surface adsorption power reduces, it is easy to disperse, then regard as the modifier with polylactic acid and titanic acid ester jointly to modify alkaline graphite alkene, mix silicon dioxide and modified alkaline graphite alkene, make graphite alkene powder parcel silicon dioxide, strengthen the mobility of graphite alkene powder, make can evenly mix with polyimide, silicon dioxide also has the reinforcement effect, the graphite flake that is made through adding modified graphite alkene powder and polyimide is strong, the heat flux is bigger, the coefficient of heat conductivity is better, toughness is better, the thermal diffusivity is longer with the time of thermal saturation.
In a second aspect, the present application provides a heat dissipation graphite sheet prepared by the above graphene film production method, which adopts the following technical scheme:
the utility model provides a heat dissipation graphite flake, the thickness of heat dissipation graphite flake after the extension is pressed is 30~400 um.
This application adopts above-mentioned preparation step, adopts the polyimide film that contains graphite alkene to pass through carbonization, graphitization continuous processing back, and the heat dissipation graphite flake thickness that makes through the calendering is 30~400 mu m, and thickness is thinner than the heat dissipation graphite flake on market, and density is big for heat conductivity and heat-sinking capability of heat dissipation graphite flake improve, and it is longer to make the hot saturation time simultaneously, is favorable to the application of heat dissipation graphite flake. The thickness of heat dissipation graphite flake is thinner, density is just bigger, the thermal conductivity is better, but the heat conduction volume on the thickness direction of heat dissipation graphite flake is less simultaneously, consequently, add polyimide behind the graphite alkene, can have the density of preferred under the 30~400 mu m circumstances, make the heat dissipation graphite flake have good physical properties, on having the heat conduction basis on the heat dissipation graphite flake horizontal direction simultaneously, certain thickness has increased the heat conduction of heat dissipation graphite flake on the thickness direction, the thermal conductivity of heat dissipation graphite flake has been improved, make the heat dissipation graphite flake can extensively apply to new energy battery package, photovoltaic module is isometric great product heat dissipation direction. If the thickness of the heat dissipation graphene film is larger than 400um, the density of the graphene film is reduced, and the heat conduction performance of the graphene film is poor; if the thickness of the heat dissipation graphene film is less than 30um, the graphene has good heat conductivity, but is easy to break, and the application of the heat dissipation graphene is not easy.
Preferably, the surface of the heat dissipation graphite sheet is plated with a metal layer.
Through adopting above-mentioned technical scheme, the intensity and the hardness of multiplicable heat dissipation graphite flake make the heat dissipation graphite flake have the heat conductivility that the heat conductivility of thickness direction has again simultaneously the heat conductivility that has the horizontal direction promptly, have higher coefficient of heat conductivity, improve the heat conductivility of heat dissipation graphite flake.
Preferably, the heat flux of the heat dissipation graphite sheet is 1.5-2 W.m-2。
By adopting the technical scheme, the heat conduction effect of the heat dissipation graphite flake is better, the application range of the heat dissipation graphite flake is enlarged, and the heat dissipation graphite flake with good heat conduction effect can be applied to the fields of new energy, aerospace, energy storage, photoelectricity, heat dissipation, medicines, composite materials, heating materials and the like.
In summary, the present application has the following beneficial effects:
1. according to the method, the carbonization process and the graphitization process form a continuous heating mode, so that the time for preparing the graphite flakes is shortened to 22-26 h, the process operation process is simplified, and the capacity of enterprises is increased; meanwhile, the graphite flake prepared by the method has the advantages of thin thickness, high heat conductivity coefficient, high toughness, high heat flux, good heat dissipation and long thermal saturation time, thereby improving the physical property of the graphite flake and having high practicability.
2. Polyimide and graphite alkene mixed use in this application raw materials coiled material for the graphite flake has good physical properties, and polyimide and graphite alkene cooperation are used, and the graphite flake coefficient of heat conductivity that finally makes is high, thickness is thin, toughness is high, intensity is moderate, heat flux is high and good heat dissipation.
3. This application increases the intensity and the hardness of heat dissipation graphite flake through at heat dissipation graphite flake surface electricity plate metal layer, makes the heat conductivility that the heat dissipation graphite flake has the horizontal direction promptly simultaneously have the ascending heat conductivility of thickness side again to improve the heat conductivility of heat dissipation graphite flake, the coefficient of heat conductivity promotes.
Drawings
FIG. 1 is a graph of time versus temperature for the examples.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples.
The raw materials in the examples and the preparation examples of the application can be purchased from commercial products, and the following are the sources and types of part of the raw materials in the application:
polyimide was purchased from Shanghai plastic hong International trade company, Inc. with a model number of 73G 15;
the graphene is purchased from Yangxin trade company Limited in Guangzhou city, and the specification is in nanometer level; silicon carbide was purchased from Yuying refractory Co., Ltd, consolidated City, and specified 80 mesh.
Tetramethoxysilane is available from North Huco Word chemical Co., Ltd, model number 681-84-5.
Methyltriethoxysilane is available from Jining Sanshi Biotech, Inc. under the model SH-658796.
Preparation of modified graphene
Preparation example 1
The modified graphene is prepared by the following method:
s1, weighing 0.1 kg of methyltriethoxysilane, 1 kg of ethanol solvent, 0.5 kg of water and 1.5 kg of graphene powder, uniformly stirring, adding 0.01 kg of tetramethylguanidine, adjusting the pH value to 8, and stirring for reaction to obtain alkaline graphene;
s2, weighing 0.2 kg of polylactic acid, 0.1 kg of titanate coupling agent and 1.5 kg of 1% sodium hydroxy carbonate solution by mass, uniformly mixing with the alkaline graphene, heating to 60 ℃, reacting for 0.5h, keeping the stirring state in the reaction process, adding 0.3 kg of fumed silica, stirring for 20min, filtering, and drying to obtain the modified graphene.
Preparation example 2
The modified graphene is prepared by the following method:
s1, weighing 0.3 kg of trimethoxy silane, 1.5 kg of methanol solvent, 0.8 kg of water and 2 kg of graphene powder, uniformly stirring, adding 0.02 kg of tetramethyl guanidine, adjusting the pH value to 10, and stirring for reaction to obtain alkaline graphene;
s2, weighing 0.6 kg of polylactic acid, 0.2 kg of titanate coupling agent and 2 kg of 5% sodium hydroxy carbonate solution by mass, uniformly mixing with the alkaline graphene, heating to 65 ℃, reacting for 1h, keeping the stirring state in the reaction process, adding 0.5 kg of fumed silica, stirring for 30min, filtering, and drying to obtain the modified graphene.
Preparation example of raw Material coil
Preparation example 3
The preparation method of the raw material coiled material comprises the following steps:
respectively weighing 20 kg of polyimide, 5 kg of graphene (the dosage ratio of the graphene to the polyimide is 1:4), 1 kg of starch, 0.1 kg of silicon carbide and 0.1 kg of stearate, uniformly mixing, adding the mixture into a screw rod material of an extruder barrel for plasticizing and extruding to form a tube blank, performing blow molding, cooling, drawing and coiling to obtain the IP film.
Preparation example 4
The preparation method of the raw material coiled material comprises the following steps:
respectively weighing 15 kg of polyimide, 10 kg of graphene (the dosage ratio of the graphene to the polyimide is 2:3), 1 kg of kaolin, 5 kg of diphenylsilanediol, 0.1 kg of silicon carbide and 0.1 kg of stearate, uniformly mixing, adding the mixture into a screw rod material of an extruder barrel for plasticizing and extruding to form a tube blank, and carrying out blow molding, cooling, traction and coiling to obtain the IP film.
Preparation example 5
The preparation method of the raw material coiled material comprises the following steps:
respectively weighing 20 kg of polyimide, 5 kg of graphene (the dosage ratio of the graphene to the polyimide is 1:4), 1 kg of kaolin, 5 kg of diphenylsilanediol, 0.1 kg of silicon carbide and 0.1 kg of stearate, uniformly mixing, adding the mixture into a screw rod material of an extruder barrel for plasticizing and extruding to form a tube blank, and carrying out blow molding, cooling, traction and coiling to obtain the IP film.
Preparation example 6
The difference between the preparation example and the preparation example 5 is that: the amount of polyimide used was 20 kg, the amount of graphene used was 15 kg, and the remaining amounts and steps were identical to those of preparation example 5.
Preparation example 7
The difference between the preparation example and the preparation example 5 is that: 20 kg of polyacrylamide was used instead of polyimide, and the amount of graphene used was 15 kg, and the remaining amount and procedure were identical to those of preparation example 5.
Preparation example 8
The difference between the preparation example and the preparation example 5 is that: graphene was changed to the modified graphene from preparation example 1, and the remaining amounts and steps were identical to those of preparation example 5.
Preparation example 9
The difference between the preparation example and the preparation example 5 is that: graphene was changed to the modified graphene from preparation example 2, and the remaining amounts and steps were identical to those of preparation example 5.
Examples
Example 1
A heat-dissipating graphite sheet, prepared by the steps of:
adding a commercially available PI film into a tunnel furnace, sequentially arranging a preheating region, a carbonization region, a graphitization region and a cooling region in the tunnel furnace for the commercially available PI film, wherein the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, preheating the raw material coil in the preheating region of the tunnel furnace for 2h, obtaining a preheated raw material coil after preheating, feeding the preheated raw material coil into the carbonization region, starting heating up from 950 ℃ in the carbonization region at a heating rate of 10 ℃/min for 55min, keeping for 245min in the carbonization region after heating up to 1500 ℃, completing carbonization to obtain a carbonized coil, feeding the carbonized coil into the graphitization region, starting heating up from 1500 ℃ in the graphitization region at a heating rate of 6 ℃/min for 216min, keeping for 84min in the graphitization region after heating up to 2800 ℃, completing carbonization, and preparing a graphite sheet, and (3) the graphite flake enters a heat preservation area, the temperature of the heat preservation area is reduced from 2800 ℃, the temperature reduction rate is 3.9/min, the temperature reduction time is 12h, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 30MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 50 um.
Example 2
A heat-dissipating graphite sheet, prepared by the steps of:
adding the raw material coiled material prepared in preparation example 3 into a tunnel furnace, wherein the raw material coiled material is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a cooling region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coiled material enters the preheating region of the tunnel furnace to be preheated for 2h, after preheating is completed, the preheated raw material coiled material is obtained, the preheated raw material coiled material enters the carbonization region, the temperature of the carbonization region starts to rise from 950 ℃, the temperature rise rate is 10 ℃/min, the temperature rise time is 55min, after the temperature rises to 1500 ℃, the carbonization region is kept for 245min, carbonization is completed, the carbonized coiled material enters the graphitization region, the temperature of the graphitization region starts to rise from 1500 ℃, the temperature rise rate is 6 ℃/min, the temperature rise time is 216min, after the temperature rises to 2800 ℃, the graphitization region is kept for 84min, and graphite flakes are prepared, and (3) the graphite flake enters a heat preservation area, the temperature of the heat preservation area is reduced from 2800 ℃, the temperature reduction rate is 3.9/min, the temperature reduction time is 12h, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 31MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 60 um.
Example 3
A heat-dissipating graphite sheet, prepared by the steps of:
adding the raw material coiled material prepared in the preparation example 3 into a tunnel furnace, wherein the raw material coiled material is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a cooling region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coiled material enters the preheating region of the tunnel furnace to be preheated, the preheating time is 2h, after the preheating is finished, the preheated raw material coiled material is obtained, the preheated raw material coiled material enters the carbonization region, the temperature of the carbonization region starts to rise from 950 ℃, the temperature rise rate is 13 ℃/min, the temperature rise time is 44min, after the temperature rises to 1500 ℃, the carbonization region is kept for 256min, the carbonization is finished, the carbonized coiled material is obtained, the carbonized coiled material enters the graphitization region, the graphitization region starts to rise from 1500 ℃, the temperature rise rate is 8 ℃/min, the temperature rise time is 162min, after the temperature rises to 2800 ℃, the carbonization is kept for 138min, and the graphite flake is prepared, and (3) the graphite flake enters a heat preservation area, the temperature of the heat preservation area is reduced from 2800 ℃, the temperature reduction rate is 2/min, the temperature reduction time is 12h, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 32MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 70 um.
Example 4
A heat-dissipating graphite sheet, prepared by the steps of:
adding the raw material coiled material prepared in the preparation example 3 into a tunnel furnace, wherein the raw material coiled material is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a cooling region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coiled material enters the preheating region of the tunnel furnace to be preheated, the preheating time is 2h, after the preheating is finished, the preheated raw material coiled material is obtained, the preheated raw material coiled material enters the carbonization region, the temperature of the carbonization region starts to rise from 950 ℃, the temperature rise rate is 15 ℃/min, the temperature rise time is 38min, after the temperature rises to 1500 ℃, the temperature is kept in the carbonization region for 262min, the carbonization is finished, the carbonized coiled material is obtained, the carbonized coiled material enters the graphitization region, the graphitization region starts to rise from 1500 ℃, the temperature rise rate is 10 ℃/min, the temperature rise time is 130min, after the temperature rises to 2800 ℃, the carbonization region is kept for 170min, and graphite flakes are prepared, the graphite flake enters a heat preservation area, the temperature of the heat preservation area is reduced from 2900 ℃, the temperature reduction rate is 2/min, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 33MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 80 um.
Example 5
The present embodiment is different from embodiment 3 in that: the starting coils used were from preparation example 4 with the remaining amounts and steps in accordance with example 3.
Example 6
The present embodiment is different from embodiment 3 in that: the starting coil used was from preparation 5, the remaining amounts and steps corresponding to example 3.
Example 7
The present embodiment is different from embodiment 3 in that: the starting coil used was from preparation 6, the remaining amounts and procedures being in accordance with example 3.
Example 8
The present embodiment is different from embodiment 3 in that: the starting coil used was from preparation 7, the remaining amounts and procedures being in accordance with example 3.
Example 9
The present embodiment is different from embodiment 3 in that: the starting coil used was from preparation 8, the remaining amounts and steps corresponding to example 3.
Example 10
The present embodiment is different from embodiment 3 in that: the starting coil used was from preparation 9, the remaining amounts and procedures being in accordance with example 3.
Example 11
A heat-dissipating graphite sheet, prepared by the steps of:
adding a raw material coil into a tunnel furnace, wherein the raw material coil sequentially enters a preheating region, a carbonization region, a graphitization region and a cooling region which are arranged in the tunnel furnace, the temperature of the preheating region is 1100 ℃, the temperature of the carbonization region is 1700 ℃, the temperature of the graphitization region is 3000 ℃, the raw material coil enters the preheating region of the tunnel furnace to be preheated, the preheating time is 2 hours, after the preheating is finished, the preheated raw material coil is obtained, the preheated raw material coil enters the carbonization region, the carbonization region starts to heat up from 950 ℃, the heating rate is 15 ℃/min, the heating time is 40min, after the heating is up to 1500 ℃, the carbonization region is kept for 260min to finish the carbonization to obtain the carbonized coil, the carbonized coil enters the graphitization region, the graphitization region starts to heat up from 1700 ℃, the heating rate is 10 ℃/min, the heating time is 130min, after the heating is up to 2800 ℃, the graphitization region is kept for 170min to finish the carbonization to obtain graphite flakes, and the graphite flakes enter the heat preservation region, the temperature of the heat preservation area is reduced from 2900 ℃, the temperature reduction rate is 2/min, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 30MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 50 um.
Comparative example
Comparative example 1
A graphite flake, prepared by the steps of:
adding a raw material coiled material into a tunnel furnace, wherein the raw material coiled material is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a cooling region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coiled material enters the preheating region of the tunnel furnace to be preheated, the preheating time is 2 hours, after the preheating is finished, the preheated raw material coiled material is obtained, the preheated raw material coiled material enters the carbonization region, the carbonization region starts to heat up from 950 ℃, the heating rate is 8 ℃/min, the heating time is 71min, after the temperature is raised to 1500 ℃, 229min is reserved in the carbonization region to finish carbonization, the carbonized coiled material is obtained, the carbonized coiled material enters the graphitization region, the graphitization region starts to heat up from 1500 ℃, the heating rate is 5 ℃/min, the heating time is 260min, after the temperature is raised to 2800 ℃, the graphitizing region is reserved for 40min to finish carbonization, graphite flakes are prepared, and enter the heat preservation region, the temperature of the heat preservation area is reduced from 2900 ℃, the temperature reduction rate is 2/min, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 30MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 50 um.
Comparative example 2
A graphite flake, prepared by the steps of:
adding a raw material coil into a tunnel furnace, wherein the raw material coil is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a cooling region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coil enters the preheating region of the tunnel furnace to be preheated for 2h, after preheating is completed, the preheated raw material coil enters the carbonization region, the carbonization region starts to heat up from 950 ℃, the heating rate is 17 ℃/min, the heating time is 34min, after the temperature is raised to 1500 ℃, 266min is reserved in the carbonization region to complete carbonization, the carbonized coil enters the graphitization region, the graphitization region starts to heat up from 1500 ℃, the heating rate is 11 ℃/min, the heating time is 118min, after the temperature is raised to 2800 ℃, 172min is reserved in the graphitization region to complete carbonization, graphite flakes are prepared, and the graphite flakes enter a heat preservation region, the temperature of the heat preservation area is reduced from 2900 ℃, the temperature reduction rate is 2/min, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 30MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 50 um.
Comparative example 3
Adding a raw material coiled material into a tunnel furnace, wherein the raw material coiled material is sequentially arranged in a preheating region, a carbonization region, a graphitization region and a temperature reduction region of the tunnel furnace, the temperature of the preheating region is 950 ℃, the temperature of the carbonization region is 1500 ℃, the temperature of the graphitization region is 2800 ℃, the raw material coiled material enters the preheating region of the tunnel furnace to be preheated for 2 hours, after preheating is completed, the preheated raw material coiled material is obtained, the preheated raw material coiled material enters the carbonization region, the temperature of the carbonization region starts to rise from 950 ℃, the temperature rise rate is 13 ℃/min, the temperature rise time is 44min, after the temperature rises to 1500 ℃, 256min is kept in the carbonization region, the temperature of the carbonization region starts to fall from 1500 ℃, the temperature fall rate is 2/min, the temperature fall time is 12 hours, the temperature falls to 20 ℃, carbonization is completed, the carbonized coiled material enters the graphitization region, the temperature of the graphitization region starts to rise from 1500 ℃, the temperature rise rate is 8 ℃/min, and the temperature rise time is 162min, the graphite flake is kept for 138min in the graphitization zone after the temperature rises to 2800 ℃, carbonization is completed, the graphite flake is prepared, the graphite flake enters the heat preservation zone, the temperature of the heat preservation zone starts to be reduced from 2800 ℃, the temperature reduction rate is 2/min, the temperature reduction time is 12h, the temperature is reduced to 20 ℃, and a finished product is taken out.
And then, the finished product passes through a calendering machine, the calendering pressure is 32MPa, and after calendering, the heat dissipation graphite flake is prepared, wherein the thickness of the heat dissipation graphite flake is 70 um.
Table 1 source of example and comparative graphene
The performance test detects the heat flux, the in-plane heat conductivity coefficient, the out-of-plane heat conductivity coefficient, the graphitization degree and the thermal expansion coefficient of the prepared graphite flake.
Detection method/test method
The graphitization degree of the graphite sheet is measured by a Raman spectrometer.
The thermal conductivity of the graphite flake is measured by a thermal conductivity meter.
The coefficient of thermal expansion of the carbonized graphene was measured by a thermomechanical analyzer.
TABLE 1 data of performance testing experiments for examples 1-8 and comparative examples 1-3
It can be seen by combining examples 1 to 3 and comparative examples 1 to 3 and table 2 that the values of the heat flux, the in-plane thermal conductivity and the out-of-plane thermal conductivity of the graphite radiator sheets in examples 1 to 3 are higher than those of the graphite radiator sheets in comparative examples 1 to 3, the thermal expansion coefficient of the graphite radiator sheets in examples 1 to 3 is lower than that of the graphite radiator sheets in comparative examples 1 to 3, and the higher the thermal conductivity, the stronger the thermal conductivity, which indicates that the graphite radiator sheet prepared by the process of the present application has a higher graphitization degree and a good thermal conductivity. The degree of graphitization of the graphite heat dissipating sheets in examples 1 to 3 is smaller than that in comparative examples 1 to 3, and the smaller the value, the higher the degree of graphitization
It can be seen by combining examples 1 to 11 and comparative examples 1 to 3 and table 2 that the values of the heat flux, the in-plane thermal conductivity, and the out-of-plane thermal conductivity of the graphite sheets in examples 1 to 11 are higher than those of the graphite sheets in comparative examples 1 to 3, the thermal expansion coefficient of the graphite sheets in examples 1 to 8 is lower than that of the graphite sheets in comparative examples 1 to 5, and the higher the thermal conductivity, the stronger the thermal conductivity, which indicates that the graphite sheets prepared by the formulation of the present application and the preparation process of the present application have higher graphitization degree and good thermal conductivity. The degree of graphitization of the heat dissipating graphite sheets in examples 1 to 11 is smaller than that in comparative examples 1 to 3, and the smaller the value, the higher the degree of graphitization.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A production process of graphite flakes containing graphene is characterized by comprising the following steps: the method comprises the steps of sequentially carrying out preheating treatment, carbonization treatment, graphitization treatment and cooling treatment on a raw material coiled material, directly heating to carry out graphitization treatment after the carbonization treatment is finished, wherein the heating rate of the carbonization treatment is 10-15 ℃/min, and the heating rate of the graphitization treatment is 6-10 ℃/min.
2. The process for producing graphene-containing graphite sheets according to claim 1, wherein: and the preheating temperature of the preheating treatment is 950-1100 ℃, so that the preheated raw material coiled material is obtained.
3. A process for producing graphene-containing graphite flakes according to claim 2, wherein: and the carbonization treatment is to carbonize the preheated raw material coiled material, wherein the carbonization temperature is 1500-1700 ℃, and the carbonization time is 5-6 hours, so as to prepare the carbonized coiled material.
4. A process for producing graphene-containing graphite flakes according to claim 3, wherein: and the graphitization treatment is to graphitize the carbonized coiled material, wherein the graphitization temperature is 2800-3000 ℃, and the graphitization time is 5-6 h, so as to prepare the graphite sheet.
5. The process for producing graphene-containing graphite sheets according to claim 1, wherein: the cooling rate of the cooling treatment is 2-5 ℃/min, the cooling time is 10-12 h, and the temperature of the cooling treatment is reduced to 20-30 ℃.
6. The process for producing graphene-containing graphite sheets according to claim 1, wherein: the raw material coiled material comprises, by weight, 10-20 parts of polyimide and 0.5-1 part of graphene.
7. The process for producing graphene-containing graphite sheets according to claim 6, wherein: the using amount ratio of the graphene to the polyimide is (15-20): 1.
8. a heat-dissipating graphite sheet produced by the process for producing a graphene-containing graphite sheet according to any one of claims 1 to 7, wherein: the thickness of the heat dissipation graphite sheet after calendering is 30-400 um.
9. A graphite heat dissipating sheet according to claim 8, wherein: the surface of the heat dissipation graphite sheet is electroplated with a metal layer.
10. A graphite heat dissipating sheet according to claim 8, wherein: the heat flux of the heat dissipation graphite flake is 1.5-2W and is characterized by m-2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111489132.1A CN114195133A (en) | 2021-12-07 | 2021-12-07 | Graphene-containing graphite flake production process and heat dissipation graphite flake |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111489132.1A CN114195133A (en) | 2021-12-07 | 2021-12-07 | Graphene-containing graphite flake production process and heat dissipation graphite flake |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114195133A true CN114195133A (en) | 2022-03-18 |
Family
ID=80651131
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111489132.1A Pending CN114195133A (en) | 2021-12-07 | 2021-12-07 | Graphene-containing graphite flake production process and heat dissipation graphite flake |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114195133A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| CN106829930A (en) * | 2017-02-27 | 2017-06-13 | 深圳丹邦科技股份有限公司 | A kind of web-like continuous graphite alkene film and preparation method thereof |
| CN107804843A (en) * | 2017-11-20 | 2018-03-16 | 苏州世华新材料科技有限公司 | A kind of preparation technology of uniformly high heat conduction graphite film coiled material |
| CN108751184A (en) * | 2018-08-21 | 2018-11-06 | 北京中石伟业科技股份有限公司 | A kind of carbonization of graphite guide hotting mask and graphitization continuous process system and method |
| WO2020183910A1 (en) * | 2019-03-12 | 2020-09-17 | 株式会社カネカ | Heating furnace and production method for graphite |
| CN213029050U (en) * | 2020-09-27 | 2021-04-20 | 广州宏庆电子有限公司 | Composite heat dissipation film |
| CN112919452A (en) * | 2021-03-23 | 2021-06-08 | 苏州烯时代材料科技有限公司 | High-heat-flux graphene-polyimide carbonized film and preparation method and application thereof |
-
2021
- 2021-12-07 CN CN202111489132.1A patent/CN114195133A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| CN106829930A (en) * | 2017-02-27 | 2017-06-13 | 深圳丹邦科技股份有限公司 | A kind of web-like continuous graphite alkene film and preparation method thereof |
| CN107804843A (en) * | 2017-11-20 | 2018-03-16 | 苏州世华新材料科技有限公司 | A kind of preparation technology of uniformly high heat conduction graphite film coiled material |
| CN108751184A (en) * | 2018-08-21 | 2018-11-06 | 北京中石伟业科技股份有限公司 | A kind of carbonization of graphite guide hotting mask and graphitization continuous process system and method |
| WO2020183910A1 (en) * | 2019-03-12 | 2020-09-17 | 株式会社カネカ | Heating furnace and production method for graphite |
| CN213029050U (en) * | 2020-09-27 | 2021-04-20 | 广州宏庆电子有限公司 | Composite heat dissipation film |
| CN112919452A (en) * | 2021-03-23 | 2021-06-08 | 苏州烯时代材料科技有限公司 | High-heat-flux graphene-polyimide carbonized film and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| （加）GEORGE WYPYCH编著；程斌等译, 中国轻工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103663444B (en) | A kind of Graphene composite film for heat dissipation and preparation method thereof | |
| CN101973532B (en) | Method for preparing nano aluminum nitride powder | |
| CN103833370B (en) | Near shape preparation method of multiphase ceramic Si3N4-SiC | |
| CN105502359A (en) | Preparation method of low-cost porous graphene | |
| CN104909765B (en) | A kind of low cost, quick preparation high-performance Si3N4The method of Ceramic Balls | |
| CN109868118B (en) | Preparation method of aluminum nitride-aluminum oxide core-shell structure with high thermal conductivity | |
| CN105541328A (en) | Graphene oxide based method for preparing highly oriented pyrolytic graphite film | |
| CN104876638B (en) | A kind of nanometer porous pottery pore creating material and its preparation method and application | |
| CN106431418A (en) | Method for preparing nanometer AlN powder through hydrothermal method and intermediate and product produced through method | |
| CN110304625A (en) | Graphene induces the preparation method of the high thermal conductivity graphite film of orientation of polyimide crystallization | |
| CN105272269A (en) | Preparation method of Si3N4/h-BN nano-composite ceramics | |
| CN102838106A (en) | Method for preparing carbon film by using silicon carbide-enhanced polyimide composite film | |
| CN106083046A (en) | A kind of preparation method of Graphene/polyimides copolymerization heat conducting film | |
| CN111453706A (en) | Synthesis method of hexagonal boron nitride | |
| CN110745827A (en) | Preparation method of two-dimensional flaky SiC material | |
| CN113353947A (en) | Method for preparing high-activity titanium boride ceramic powder by low-temperature microwave carbothermic reduction | |
| CN102674819B (en) | High-toughness aluminum oxide ceramic, and preparation method and application thereof | |
| WO2019232765A1 (en) | Preparation method for ultrathin boron nitride nanosheet | |
| CN103450857A (en) | Composite graphite heat-conducting membrane material with controllable heat conductivity and preparation process thereof | |
| CN114195133A (en) | Graphene-containing graphite flake production process and heat dissipation graphite flake | |
| CN105692589A (en) | Preparation method of glassy carbon material based on modified phenolic resin precursor | |
| Sun et al. | Fast one‐step carbothermal reduction and nitridation method using nano‐sized Al2O3 and carbon black to prepare aluminium oxynitride powder for highly transparent ceramics | |
| CN116536034A (en) | Preparation method of polyimide graphitized film | |
| Wang et al. | Preparation of spherical α‐Al2O3 nanoparticles by microwave hydrothermal synthesis and addition of nano‐Al seeds | |
| CN107955998A (en) | A kind of high soft mullite of lightweight is ultra-fine/nano ceramic fibers and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220318 |
|
| RJ01 | Rejection of invention patent application after publication |