CN109437905B - Preparation method of tear-resistant graphite film - Google Patents
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Abstract
The invention discloses a preparation method of a tear-resistant graphite film, which comprises the steps of coating polyamide acid liquid on the surface of a graphite mixture, baking at a temperature in steps to reach imidization degree, and rolling. The graphite mixture comprises, by weight, 40-50 parts of graphite powder, 20-30 parts of acetylene carbon black, 2-5 parts of silicon carbide and 1-5 parts of graphene. The coating thickness of the polyamic acid was varied from 2 to 12 μm. The imidized polyimide surface can have various colors, such as red, green, black, blue, yellow and the like. The finally obtained tear-resistant graphite film has the bonding of more than 10N/mm and is not layered.
Description
Technical Field
The invention relates to a graphite film, in particular to a preparation method of a tear-resistant graphite film.
Background
Graphite films are used as heat radiating members for semiconductor elements and other heat generating components mounted on various electronic and electrical devices such as computers. However, both natural graphite films and artificial graphite films applied to the existing markets have a problem that the graphite films are easy to shed powder and torn when the bent graphite films need to be cut.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a preparation method of a tear-resistant graphite film.
In order to achieve the purpose, the preparation method of the tear-resistant graphite film comprises the following steps: firstly, diamine is put into a reaction kettle and dissolved by a polar solvent, then modified nano powder and pigment are put into the reaction kettle, and finally dianhydride is added into the reaction kettle in batches and stirred to prepare the needed polyamic acid solution; wherein the modified nano powder comprises 20 to 30 parts by weight of silicon tetrafluoride, 10 to 15 parts by weight of aluminum oxide, 30 to 40 parts by weight of silicon oxide, 1 to 5 parts by weight of titanium oxide and 0.1 to 0.3 part by weight of hafnium oxide; the pigment is iron green, cobalt green, iron red, cadmium red, perylene red, quinacridone, phthalocyanine and benzimidazolone; and step two, preparing a graphite film, namely mixing 40-50 parts of graphite powder, 20-30 parts of acetylene carbon black, 2-5 parts of silicon carbide and 1-5 parts of graphene according to parts by weight, crushing the mixture into powder to obtain a graphite mixture, then putting the graphite mixture into a heating furnace, carbonizing the graphite mixture, graphitizing the graphite mixture, naturally cooling the graphite mixture to 40-50 ℃ after the graphitization operation, then coating a layer of polyamide acid liquid with the thickness of 2-12 mu m on the surface of the graphite mixture, putting the graphite mixture onto a conveying belt provided with an oven to complete imidization of polyamide acid, and then rolling the polyamide acid, wherein the gradient temperature of the oven is 80-400 ℃, and the speed of the conveying belt is 2-15 m/min.
The gradient temperature of the oven is specifically from 80 ℃ to 100 ℃, the temperature is kept for 30-60min, the temperature is raised to 160 ℃, the temperature is kept for 15-30min, the temperature is raised to 200 ℃, the temperature is kept for 15-30min, the temperature is raised to 250 ℃, the temperature is kept for 30-60min, the temperature is raised to 300 ℃, the temperature is kept for 15-30min, the temperature is raised to 400 ℃, and the temperature is kept for 5-15 min.
The polyamic acid liquid is coated on the surface of the graphite mixture on a single side or on the surface of the graphite mixture on two sides. The coating may be in the form of any one of a doctor blade method, an extrusion die method, and a transfer coating method.
The thickness of the graphite mixture is 13-50 μm.
The dianhydride in the polyamic acid solution preparation is one or more of pyromellitic dianhydride (PMDA), 3',4,4' -biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA), 4,4 '-diphenyl ether dianhydride (ODPA), bisphenol A dianhydride (BPADA) and 4,4' - (hexafluoroisopropylidene) diphthalic anhydride (6 FPA); the diamine is one or more of 4, 4-diaminodiphenyl ether (ODA), p-phenylenediamine (PPD), 4-diaminodiphenylmethane (MDA), 2 '-bis (trifluoromethyl) -4,4' -diaminobiphenyl (TFMB) (TFMB), 4-diaminobenzene sulfone (4, 4-DDS) and 1, 4-bis (4-amino-2-trifluoromethylphenoxy) benzene (6 FAPB); the polar solvent is one or more of Dimethylacetamide (DMAC), N-methylpyrrolidone (NMP) and Dimethylformamide (DMF).
According to the preparation method of the tear-resistant graphite film, the polyamic acid liquid is coated on the surface of the graphite mixture, and the mixture is subjected to gradient baking at a temperature to reach an imidization degree and then is rolled. The coating thickness of the polyamic acid was varied from 2 to 12 μm. The imidized polyimide surface can have various colors, such as red, green, black, blue, yellow and the like. The finally obtained tear-resistant graphite film has the adhesive force of more than 10N/mm and is not layered.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1: the preparation method of the tear-resistant graphite film provided by the embodiment comprises the following steps: firstly, diamine is put into a reaction kettle and dissolved by a polar solvent, then modified nano powder and pigment are put into the reaction kettle, and finally dianhydride is added into the reaction kettle in batches and stirred to prepare the needed polyamic acid solution; wherein the modified nano powder comprises 30 parts by weight of silicon tetrafluoride, 15 parts by weight of aluminum oxide, 0 part by weight of silicon oxide, 5 parts by weight of titanium oxide and 0.3 part by weight of hafnium oxide; the pigment is phthalocyanine; and step two, preparing a graphite film, namely mixing 50 parts of graphite powder, 30 parts of acetylene carbon black, 5 parts of silicon carbide and 5 parts of graphene according to parts by weight, crushing the mixture into powder to obtain a graphite mixture, then putting the graphite mixture into a heating furnace, carbonizing the graphite mixture, graphitizing the graphite mixture, naturally cooling the graphite mixture to 40-50 ℃ after the graphitization operation, then coating a layer of polyamide acid liquid with the thickness of 2-12 mu m on the surface of the graphite mixture, then putting the graphite mixture onto a conveying belt provided with an oven to complete imidization of the polyamide acid, and then rolling the polyamide acid liquid, wherein the gradient temperature of the oven is 80-400 ℃, and the speed of the conveying belt is 2-15 m/min.
The gradient temperature of the oven is specifically from 80 ℃ to 100 ℃, the temperature is kept for 30-60min, the temperature is raised to 160 ℃, the temperature is kept for 15-30min, the temperature is raised to 200 ℃, the temperature is kept for 15-30min, the temperature is raised to 250 ℃, the temperature is kept for 30-60min, the temperature is raised to 300 ℃, the temperature is kept for 15-30min, the temperature is raised to 400 ℃, and the temperature is kept for 5-15 min.
The polyamic acid liquid is coated on the surface of the graphite mixture on a single side or on the surface of the graphite mixture on two sides. The coating may be in the form of any one of a doctor blade method, an extrusion die method, and a transfer coating method. The thickness of the graphite mixture is 13-50 μm.
The dianhydride in the polyamic acid solution preparation is one or more of pyromellitic dianhydride (PMDA), 3',4,4' -biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA), 4,4 '-diphenyl ether dianhydride (ODPA), bisphenol A dianhydride (BPADA) and 4,4' - (hexafluoroisopropylidene) diphthalic anhydride (6 FPA); the diamine is one or more of 4, 4-diaminodiphenyl ether (ODA), p-phenylenediamine (PPD), 4-diaminodiphenylmethane (MDA), 2 '-bis (trifluoromethyl) -4,4' -diaminobiphenyl (TFMB) (TFMB), 4-diaminobenzene sulfone (4, 4-DDS) and 1, 4-bis (4-amino-2-trifluoromethylphenoxy) benzene (6 FAPB); the polar solvent is one or more of Dimethylacetamide (DMAC), N-methylpyrrolidone (NMP) and Dimethylformamide (DMF).
Example 2: the preparation method of the tear-resistant graphite film provided by the embodiment comprises the following steps: firstly, diamine is put into a reaction kettle and dissolved by a polar solvent, then modified nano powder and pigment are put into the reaction kettle, and finally dianhydride is added into the reaction kettle in batches and stirred to prepare the needed polyamic acid solution; wherein the modified nano powder comprises 20 parts by weight of silicon tetrafluoride, 10 parts by weight of aluminum oxide, 30 parts by weight of silicon oxide, 1 part by weight of titanium oxide and 0.1 part by weight of hafnium oxide; the pigment is cadmium red; and step two, preparing a graphite film, namely mixing 40 parts of graphite powder, 20 parts of acetylene carbon black, 2 parts of silicon carbide and 1 part of graphene according to parts by weight, crushing the mixture into powder to obtain a graphite mixture, then putting the graphite mixture into a heating furnace, carbonizing the graphite mixture, graphitizing the graphite mixture, naturally cooling the graphite mixture to 40-50 ℃ after the graphitization operation, then coating a layer of polyamide acid liquid with the thickness of 2-12 mu m on the surface of the graphite mixture, then putting the graphite mixture onto a conveying belt provided with an oven to complete imidization of the polyamide acid, and then rolling the polyamide acid liquid, wherein the gradient temperature of the oven is 80-400 ℃, and the speed of the conveying belt is 2-15 m/min.
Example 3: the preparation method of the tear-resistant graphite film provided by the embodiment comprises the following steps: firstly, diamine is put into a reaction kettle and dissolved by a polar solvent, then modified nano powder and pigment are put into the reaction kettle, and finally dianhydride is added into the reaction kettle in batches and stirred to prepare the needed polyamic acid solution; wherein the modified nano powder comprises 25 parts by weight of silicon tetrafluoride, 12 parts by weight of aluminum oxide, 35 parts by weight of silicon oxide, 3 parts by weight of titanium oxide and 0.2 part by weight of hafnium oxide; the pigment is benzimidazolone; and step two, preparing a graphite film, namely mixing 44 parts of graphite powder, 22 parts of acetylene carbon black, 4 parts of silicon carbide and 3 parts of graphene according to parts by weight, crushing the mixture into powder to obtain a graphite mixture, then putting the graphite mixture into a heating furnace, carbonizing the graphite mixture, graphitizing the graphite mixture, naturally cooling the graphite mixture to 40-50 ℃ after the graphitization operation, then coating a layer of polyamide acid liquid with the thickness of 2-12 mu m on the surface of the graphite mixture, then putting the graphite mixture onto a conveying belt provided with an oven to complete imidization of the polyamide acid, and then rolling the polyamide acid liquid, wherein the gradient temperature of the oven is 80-400 ℃, and the speed of the conveying belt is 2-15 m/min.
Claims (4)
1. A preparation method of a tear-resistant graphite film is characterized by comprising the following steps: the method comprises the following steps:
firstly, diamine is put into a reaction kettle and dissolved by a polar solvent, then modified nano powder and pigment are put into the reaction kettle, and finally dianhydride is added into the reaction kettle in batches and stirred to prepare the needed polyamic acid solution; wherein the modified nano powder comprises 20 to 30 parts by weight of silicon tetrafluoride, 10 to 15 parts by weight of aluminum oxide, 30 to 40 parts by weight of silicon oxide, 1 to 5 parts by weight of titanium oxide and 0.1 to 0.3 part by weight of hafnium oxide; the pigment is iron green, cobalt green, iron red, cadmium red, perylene red, quinacridone, phthalocyanine and benzimidazolone;
and step two, preparing a graphite film, namely mixing 40-50 parts of graphite powder, 20-30 parts of acetylene carbon black, 2-5 parts of silicon carbide and 1-5 parts of graphene according to parts by weight, crushing the mixture into powder to obtain a graphite mixture, then putting the graphite mixture into a heating furnace, carbonizing the graphite mixture, graphitizing the graphite mixture, naturally cooling the graphite mixture to 40-50 ℃ after the graphitization operation, then coating a layer of polyamide acid liquid with the thickness of 2-12 mu m on the surface of the graphite mixture, wherein the thickness of the graphite mixture is 13-50 mu m, then putting the graphite mixture onto a conveying belt provided with an oven to complete imidization of polyamide acid, and then rolling the polyamide acid, wherein the gradient temperature of the oven is 80-400 ℃, and the speed of the conveying belt is 2-15 m/min.
2. The method for preparing a tear-resistant graphite film according to claim 1, wherein: the polyamic acid liquid is coated on the surface of the graphite mixture on a single side or on the surface of the graphite mixture on two sides, wherein the coating form is any one of a scraper method, an extrusion die head method and a transfer coating method.
3. The method for preparing a tear-resistant graphite film according to claim 1, wherein: the dianhydride in the polyamic acid solution is one or more of pyromellitic dianhydride, 3',4,4' -biphenyl tetracarboxylic dianhydride, 3',4,4' -benzophenone tetracarboxylic dianhydride, 4,4 '-diphenyl ether dianhydride, bisphenol A dianhydride and 4,4' - (hexafluoroisopropylidene) diphthalic anhydride; the diamine is one or more of 4, 4-diaminodiphenyl ether, p-phenylenediamine, 4-diaminodiphenylmethane, 2 '-bis (trifluoromethyl) -4,4' -diaminobiphenyl, 4-diaminobenzene sulfone and 1, 4-bis (4-amino-2-trifluoromethylphenoxy) benzene; the polar solvent is one or more of dimethylacetamide, N-methylpyrrolidone and dimethylformamide.
4. The method for preparing a tear-resistant graphite film according to claim 1, wherein: the gradient temperature of the oven is specifically as follows:
heating from 80 deg.C to 100 deg.C, maintaining the temperature for 30-60min,
heating to 160 deg.C, maintaining the temperature for 15-30min,
heating to 200 deg.C, maintaining the temperature for 15-30min,
heating to 250 deg.C, maintaining the temperature for 30-60min,
heating to 300 deg.C, maintaining the temperature for 15-30min,
heating to 400 deg.C, and keeping the temperature for 5-15 min.
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