CN110304625A - Graphene induces the preparation method of the high thermal conductivity graphite film of orientation of polyimide crystallization - Google Patents
Graphene induces the preparation method of the high thermal conductivity graphite film of orientation of polyimide crystallization Download PDFInfo
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Abstract
The present invention provides the preparation methods of a kind of graphene induced orientation and the high thermal conductivity graphite film of crystallization.The preparation method is using graphene and composite polyimide material as graphite film precursor, and in high temperature cabonization and graphitizing process, graphene promotes the graphitization of polyimides as orientation and crystallization inducer, prepares the graphite film of high thermal conductivity.The flake nano graphene oxide introduced in graphite film in the present invention has intrinsic crystalline graphite carbon structure, it is in stretching and graphitizing process, it can be used as the template of graphitized carbon, induce polyimide molecule orientation and graphitized carbon crystallization process, the generation for reducing unformed shape defect in graphitizing process, to improve graphite film thermal conductivity and mechanical property.Using the height of high thermal conductivity graphite film graphite crystallization degree made from the method provided by the present invention, flexility is good, and thermal conductivity is high, can satisfy the requirement of the high heat dissipation of present microelectronics industry.
Description
Technical field
The present invention relates to thermally conductive film fields, and in particular to a kind of high thermal conductivity of graphene induction orientation of polyimide crystallization
The preparation method of graphite film.
Background technique
With modern microelectronic industry and the fast development of the high-frequency high-speed communication technology, electronic equipment and integrated circuit towards
Miniaturization, densification direction develop, miniature high density interconnection (HDI) integrated circuit is at following one of the development trend.
In HDI, conducting wire and electronic component density are significantly increased, and the heat locally generated accumulates rapidly, increases, to electronic component
Service life has negative effect, while influencing the stability and reliability of component.In addition, in high-frequency high-speed communication system
In, what the calorific value of component will be big compared to LF communication is more, this more requires to lead in electronic equipment and integrated circuit with height
The radiating subassembly of hot property can in time, rapidly transfer heat to heat dissipation equipment or outside, to ensure making for electronic equipment
With service life and stability.
Heat is conducted usually using sheet metal or graphite film in electronic component at present, heat dissipation metal tablet quality is larger,
It is flexible poor, it is not able to satisfy the frivolous demand for development of electronic equipment.Graphite film as a heat transfer medium, have the advantages that it is light,
It is widely used in the portable electronic devices such as mobile phone, computer.There are mainly two types of the preparation methods of graphite film: first is that by artificial stone
Mo Jing pressing film forming, this method is easy to operate, but the graphite film prepared is all undesirable on heating conduction and mechanical property, especially
It is that flexible and intensity cannot be met the requirements；Second is that directly preparing graphite film, this method preparation using the graphitization of macromolecule membrane
Graphite film generally there is good flexible and thermal conductivity, but energy consumption is very big during high temperature graphitization, and is easy to produce
Largely incomplete graphited unformed shape defect, seriously affects the thermally conductive and electric conductivity of graphite film.Therefore, how to reduce
Graphitization temperature, while graphitization crystalline structure is improved, reducing indefiniteness defect is the weight solved required for high thermal conductivity graphite film
Want project.
Summary of the invention
The purpose of the present invention is to solve the defects of present technology, and it is brilliant to provide a kind of graphene induction orientation of polyimide
The preparation method of the high thermal conductivity graphite film of change.On the one hand this method can reduce graphitization technique temperature, reduce energy consumption；Another party
The crystallinity of graphite film can be improved in face, reduces unformed shape defect, promotes the thermal conductivity and mechanical property of graphite film.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of the high thermal conductivity graphite film of graphene induction orientation of polyimide crystallization, the preparation method with
Graphene and composite polyimide material are graphite film precursor, and in high temperature cabonization and graphitizing process, graphene is as orientation
And crystallization inducer promotes the graphitization of polyimides, prepares the graphite film of high thermal conductivity.
Further, the specific steps are as follows:
Step 1: sequentially adding organic solvent, graphene oxide, modified additive in a kettle, stirred at 5-30 DEG C anti-
Answer 2-12h.Carboxylic acid dianhydride, diamine compound are sequentially added in above-mentioned reaction system, it is anti-at 5-30 DEG C under the protection of nitrogen
2-16h is answered, graphene hydridization polyamic acid solution is obtained.Carboxylic acid dianhydride and the molar ratio of diamine compound 1 in reaction system:
0.95-1.0, the quality of graphene oxide are the 0.1-5wt% of carboxylic acid dianhydride and diamine compound gross mass, the matter of modified additive
Amount accounts for the 2-5wt% of graphene oxide quality, and the total solid content of graphene hydridization polyamic acid solution is controlled in 9-28wt%.
Step 2: catalyst is added in the graphene hydridization polyamic acid solution that step 1 obtains, is cast after mixing
Film dries in 40-60 DEG C, then at 70-160 DEG C of reaction 5-90min, obtains graphene Hybrid Polyimide Film；It is described to urge
The quality of agent is the 0.1-2wt% of carboxylic acid dianhydride and diamine compound gross mass；
Step 3: gained graphene Hybrid Polyimide Film in step 2 being subjected to biaxial stress drawing process, stretches work
Skill are as follows: 80-200 DEG C of temperature, tensile strength 10-60Mpa, stretching time 5-65min.
Step 4: the graphene Hybrid Polyimide Film that step 3 obtains being sent in carbide furnace by double roller, double roller
Between keep tensile strength 10-100Mpa, be first carbonized at 800-1500 DEG C 2-6h in carbide furnace, then is warming up to 2000-
3000 DEG C of graphitization 1-6h take out calendering and obtain the high thermal conductivity graphite film of graphene induced orientation and crystallization.
Further, polar solvent is by N-Methyl pyrrolidone (NMP), n,N-Dimethylformamide (DMF), N, N- diformazan
One or more of yl acetamide (DMAc), dimethyl sulfoxide (DMSO) form in any proportion.
Further, graphene oxide is sheet-like morphology, and the number of plies of graphene oxide is 1-00 layers, planar dimension 10-
1000nm。
Further, modified additive is by organosilicone compounds, including one in KH550, KH560, KH570, KH590
Kind or several form in any proportion.
Further, carboxylic acid dianhydride is by pyromellitic acid anhydride, 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydrides, Isosorbide-5-Nitrae, 5,8- naphthalenes
One or more of tetracarboxylic acid dianhydride, 2,3,6,7- naphthalenetetracarbacidic acidic dianhydride, 3,4,9,10- tetracarboxylic acid dianhydride are in any proportion
Composition.
Further, diamine compound by p-phenylenediamine, 1,3- diaminobenzene, 4,4- benzidine, 1,2- diaminobenzene,
One or more of 4,4 '-diamino-diphenyl propane, 4,4 '-diamino-diphenyl ethers, 4,4 '-diamino-diphenyl ketone are pressed
Arbitrary proportion composition.
Further, catalyst is that one or more of acetic anhydride, pyridine, quinoline form in any proportion.
The beneficial effects of the present invention are: the present invention provides a kind of graphene induced orientation and the high thermal conductivity graphite of crystallization
The preparation method of film.On the one hand this method can reduce graphite film graphitization technique temperature, reduce energy consumption；On the other hand it can mention
The crystallinity of high graphite film reduces unformed shape defect, promotes the thermal conductivity and mechanical property of graphite film.It is provided using the present invention
High thermal conductivity graphite film graphite crystallization degree made from method is high, and flexility is good, thermal conductivity and electric conductivity are high, tensile strength is big,
It can satisfy the requirement of the high heat dissipation of present microelectronics industry.
Specific embodiment
The present invention provides a kind of graphene induction orientation of polyimide and crystallization high thermal conductivity graphite film preparation method,
This method is using graphene and composite polyimide material as graphite film precursor, in high temperature cabonization and graphitizing process, graphene
The graphitization for promoting polyimides as orientation and crystallization inducer, prepares the graphite film of high thermal conductivity.Wherein flake nano aoxidizes
Graphene has intrinsic crystalline graphite carbon structure, is stretching in carbonisation, can be used as the mould of graphitized carbon
Plate, induction polyimide molecule orientation and graphitized carbon crystallization process, reduce the generation of unformed shape defect in graphitizing process,
To improve graphite film thermal conductivity and mechanical property.
In order to better understand the present invention, below with reference to specific embodiment, the present invention will be further described in detail,
But the scope of protection of the invention is not limited to range represented by embodiment, the process conditions such as temperature, time in preparation method
Selection can adaptation to local conditions and to result have no substantial effect reality.
Embodiment 1
88L DMF, 7.5g graphene oxide, 0.15g KH550, the mechanical stirring at 5 DEG C are sequentially added in a kettle
React 2h.20mol1,4,5,8- naphthalenetetracarbacidic acidic dianhydrides, 20mol p-phenylenediamine, in nitrogen are sequentially added in above-mentioned reaction system
Protection under react 2h at 5 DEG C, obtain graphene hydridization polyamic acid solution.In above-mentioned graphene hydridization polyamic acid solution
Middle addition 7.5g pyridine, agitating solution 1h utilize casting machine, at room temperature by above-mentioned graphene hydridization polyamic acid solution later
Casting film dries after film in 40 DEG C, then at 70 DEG C of reaction 5min, obtains graphene Hybrid Polyimide Film, Zhi Houli
Graphene Hybrid Polyimide Film is removed from curtain coating carrier band with peel-off device.Above-mentioned gained graphene hybrid polyimide
After film removing, further progress biaxial stress drawing process, drawing process are as follows: 80 DEG C of temperature, tensile strength 10Mpa, draw
Stretch time 5min.Above-mentioned graphene Hybrid Polyimide Film is sent in carbide furnace by double roller, keeps drawing between double roller
Intensity 10Mpa is stretched, be first carbonized at 800 DEG C 2h in carbide furnace, then is warming up to 2000 DEG C of graphitization 1h, takes out calendering and obtains
The high thermal conductivity graphite film of graphene induced orientation and crystallization, thermal coefficient 1982W/mk.
Embodiment 2
60L DMF, 100g graphene oxide, 3g KH550 are sequentially added in a kettle, and mechanical stirring is anti-at 20 DEG C
Answer 6h.20mol1,4,5,8- naphthalenetetracarbacidic acidic dianhydrides, 20mol p-phenylenediamine, in nitrogen are sequentially added in above-mentioned reaction system
6h is reacted at 25 DEG C under protection, obtains graphene hydridization polyamic acid solution.In above-mentioned graphene hydridization polyamic acid solution
Middle addition 120g pyridine, agitating solution 1h utilize casting machine, at room temperature by above-mentioned graphene hydridization polyamic acid solution later
Casting film dries after film in 50 DEG C, then at 90 DEG C of reaction 50min, obtains graphene Hybrid Polyimide Film, Zhi Houli
Graphene Hybrid Polyimide Film is removed from curtain coating carrier band with peel-off device.Above-mentioned gained graphene hybrid polyimide
After film removing, further progress biaxial stress drawing process, drawing process are as follows: 120 DEG C of temperature, tensile strength 40Mpa, draw
Stretch time 25min.Above-mentioned graphene Hybrid Polyimide Film is sent in carbide furnace by double roller, one is kept between double roller
Fixed lateral tensile stress, tensile strength 50Mpa, be first carbonized at 1200 DEG C 3h in carbide furnace, then is warming up to 2400 DEG C of stones
Inkization 2h takes out calendering and obtains the high thermal conductivity graphite film of graphene induced orientation and crystallization, thermal coefficient 2032W/mk.
Embodiment 3
30L DMF, 376g graphene oxide, 18.8g KH550, the mechanical stirring at 30 DEG C are sequentially added in a kettle
React 12h.20mol1,4,5,8- naphthalenetetracarbacidic acidic dianhydrides, 20mol p-phenylenediamine, in nitrogen are sequentially added in above-mentioned reaction system
16h is reacted at 30 DEG C under the protection of gas, obtains graphene hydridization polyamic acid solution.In above-mentioned graphene hydridization polyamic acid
In solution be added 150.4g pyridine, agitating solution 5h, later utilize casting machine, by above-mentioned graphene hydridization polyamic acid solution in
Casting film at room temperature dries after film in 60 DEG C, then at 160 DEG C of reaction 90min, it is thin to obtain graphene hybrid polyimide
Film is later removed graphene Hybrid Polyimide Film using peel-off device from curtain coating carrier band.Above-mentioned gained graphene is miscellaneous
After changing Kapton removing, further progress biaxial stress drawing process, drawing process are as follows: 200 DEG C of temperature, tensile strength
For 60Mpa, stretching time 65min.Above-mentioned graphene Hybrid Polyimide Film is sent in carbide furnace by double roller, double roller
Between keep certain lateral tensile stress, tensile strength 100Mpa, be first carbonized at 1500 DEG C 6h in carbide furnace, then heats up
To 3000 DEG C of graphitization 6h, takes out calendering and obtain the high thermal conductivity graphite film of graphene induced orientation and crystallization, thermal coefficient is
2108W/m·k。
Comparative example
60L DMF is sequentially added in a kettle, sequentially adds 20mol1,4,5,8- naphthalenetetracarbacidic acidic dianhydride, 20mol to benzene
Diamines reacts 6h at 25 DEG C under the protection of nitrogen, obtains polyamic acid solution.It is added in above-mentioned polyamic acid solution
120g pyridine, agitating solution 1h utilize casting machine later, by above-mentioned polyamic acid solution casting film at room temperature, after film
It is dried in 50 DEG C, then at 90 DEG C of reaction 50min, obtains Kapton, utilize peel-off device by Kapton later
It is removed from curtain coating carrier band.After above-mentioned gained Kapton removing, further progress biaxial stress drawing process stretches work
Skill are as follows: 120 DEG C of temperature, tensile strength 40Mpa, stretching time 25min.Above-mentioned graphene Hybrid Polyimide Film is passed through
Double roller is sent in carbide furnace, and certain lateral tensile stress is kept between double roller, and tensile strength 50Mpa is first in carbide furnace
Be carbonized 3h at 1200 DEG C, then is warming up to 3000 DEG C of graphitization 2h, takes out calendering and obtains graphite film, thermal coefficient 1708W/
m·k。
On the one hand can be seen that method of the invention by embodiment and comparative example can reduce graphite film graphitization technique
Temperature reduces energy consumption；On the other hand the crystallinity of graphite film can be improved, reduce unformed shape defect, promote leading for graphite film
Hot and mechanical property.Using the height of high thermal conductivity graphite film graphite crystallization degree made from the method provided by the present invention, flexility is good,
Thermal conductivity and electric conductivity height, tensile strength are big, can satisfy the requirement of the high heat dissipation of present microelectronics industry.
Claims (8)
1. a kind of preparation method of the high thermal conductivity graphite film of graphene induction orientation of polyimide crystallization, which is characterized in that described
Preparation method is using graphene and composite polyimide material as graphite film precursor, in high temperature cabonization and graphitizing process, graphite
Alkene promotes the graphitization of polyimides as orientation and crystallization inducer, prepares the graphite film of high thermal conductivity.
2. preparation method according to claim 1, which is characterized in that specific step is as follows:
Step 1: sequentially adding organic solvent, graphene oxide, modified additive in a kettle, be stirred to react 2- at 5-30 DEG C
12h.Carboxylic acid dianhydride, diamine compound are sequentially added in above-mentioned reaction system, react 2- at 5-30 DEG C under the protection of nitrogen
16h obtains graphene hydridization polyamic acid solution.The molar ratio 1:0.95- of carboxylic acid dianhydride and diamine compound in reaction system
1.0, the quality of graphene oxide is the 0.1-5wt% of carboxylic acid dianhydride and diamine compound gross mass, and the quality of modified additive accounts for
The total solid content of the 2-5wt% of graphene oxide quality, graphene hydridization polyamic acid solution are controlled in 9-28wt%.
Step 2: catalyst is added in the graphene hydridization polyamic acid solution that step 1 obtains, after mixing casting film,
It is dried in 40-60 DEG C, then at 70-160 DEG C of reaction 5-90min, obtains graphene Hybrid Polyimide Film；The catalyst
Quality is the 0.1-2wt% of carboxylic acid dianhydride and diamine compound gross mass；
Step 3: gained graphene Hybrid Polyimide Film in step 2 is subjected to biaxial stress stretching, drawing process are as follows: temperature
80-200 DEG C, tensile strength 10-60Mpa, stretching time 5-65min.
Step 4: the graphene Hybrid Polyimide Film that step 3 obtains being sent in carbide furnace by double roller, between double roller
Tensile strength 10-100Mpa is kept, be first carbonized at 800-1500 DEG C 2-6h in carbide furnace, then is warming up to 2000-3000 DEG C
It is graphitized 1-6h, calendering is taken out and obtains the high thermal conductivity graphite film of graphene induced orientation and crystallization.
3. preparation method according to claim 2, which is characterized in that polar solvent by N-Methyl pyrrolidone (NMP),
One or more of n,N-Dimethylformamide (DMF), n,N-dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO) are pressed
Arbitrary proportion composition.
4. preparation method according to claim 2, which is characterized in that graphene oxide is sheet-like morphology, graphene oxide
The number of plies be 1-00 layers, planar dimension 10-1000nm.
5. preparation method according to claim 2, which is characterized in that modified additive is organosilicone compounds, by
One or more of KH550, KH560, KH570, KH590 are formed in any proportion.
6. preparation method according to claim 2, which is characterized in that carboxylic acid dianhydride is by pyromellitic acid anhydride, 3, and 3 ', 4,
4 '-bibenzene tetracarboxylic dianhydrides, 1,4,5,8 naphthalenetetracarboxylic acid dianhydride, 2,3,6,7- naphthalenetetracarbacidic acidic dianhydride, 3,4,9,10- tetracarboxylic acid
One or more of dianhydride forms in any proportion.
7. preparation method according to claim 2, which is characterized in that diamine compound is by p-phenylenediamine, 1,3- diamino
Benzene, 4,4- benzidine, 1,2- diaminobenzene, 4,4 '-diamino-diphenyl propane, 4,4 '-diamino-diphenyl ethers, 4,4 '-
One or more of diamino-diphenyl ketone forms in any proportion.
8. preparation method according to claim 2, which is characterized in that catalyst is by one of acetic anhydride, pyridine, quinoline
Or it several forms in any proportion.
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| CN111547716A (en) * | 2020-06-19 | 2020-08-18 | 天津单从新材料科技有限公司 | Preparation method of independent self-supporting artificial nano graphite 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 |
| CN113184842A (en) * | 2021-06-03 | 2021-07-30 | 中山大学 | High-graphitization graphite thick film and preparation method thereof |
| CN113353927A (en) * | 2021-07-14 | 2021-09-07 | 长沙新材料产业研究院有限公司 | Heat-conducting composite graphite film and preparation method thereof |
| CN113372590A (en) * | 2021-05-12 | 2021-09-10 | 浙江中科玖源新材料有限公司 | Polyimide graphene composite film and graphite film |
| CN114605153A (en) * | 2022-04-14 | 2022-06-10 | 中汇睿能凤阳新材料科技有限公司 | Preparation method of high-thermal-conductivity graphite film |
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Application publication date: 20191008 |