CN107792851A - A kind of simple method for preparing of native graphite heat dissipation film - Google Patents
A kind of simple method for preparing of native graphite heat dissipation film Download PDFInfo
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- CN107792851A CN107792851A CN201710969631.8A CN201710969631A CN107792851A CN 107792851 A CN107792851 A CN 107792851A CN 201710969631 A CN201710969631 A CN 201710969631A CN 107792851 A CN107792851 A CN 107792851A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The present invention relates to a kind of simple method for preparing of large scale native graphite heat dissipation film, raw material is used as using natural crystalline flake graphite, the method expanded by liquid phase, obtain the liquid phase expanded graphite of highly expanded multiplying power, after expanded graphite is cleaned into drying, it is placed on again on mould release membrance, expanded graphite is directly pressed into by natural stone ink film by calendering.20 150 μm of thickness, the mm of width about 200 can simply be made very much using this method, length is more than 500 mm inexpensive natural stone ink film, and the thermal conductivity in its face can reach 600 W m‑1 K‑1, electrical conductivity can reach 3400 S cm‑1。
Description
Technical field
The present invention relates to a kind of preparation method of natural stone ink film, more particularly to a kind of low cost, the natural stone of high heat conduction
Ink film preparation method.
Background technology
It is gradually reduced with the size of integrated circuit, function gradually strengthens, and integrated level is continuously increased, and is distributed in unit area
Heat out also becomes larger, and this just proposes higher requirement to heat sink material.
At present, the conventional heat sink material being mounted on the electronic products such as computer is heat-conducting silicone grease and metal heat-conducting tube, and
The heat dissipation equipments such as radiator, fan are carried on product framework.Because the thermal conductivity of heat sink material is not high, density is big, radiating effect
Rate can than relatively low, and equipment size do it is small after, the assembling space of heat dissipation equipment also can be by more limitation.It would therefore be desirable to
A kind of thermal conductivity is high, density is small and compares the flexible material of easy processing to meet the radiating requirements increasingly increased.Therefore, high heat conduction
Graphite film obtained extensive development and application.The preparation method of existing natural stone ink film is mainly by intercalator to stone
Ink carries out intercalation processing, then thermal expansion graphite is made with modes such as high-temperature heating, microblogging processing, then rolls and native graphite is made
Film [Xiang J L, Drzal L T, Carbon, 2011,49,773. Wu H, Drzal L T, Carbon,
2012, 50, 1135. Wang L W, Metcalf S J, Critoph R E, et al. Carbon, 2011, 49,
4812].Because the active force of expansion process is very big so that the lamella size of crystalline flake graphite receives serious destruction, calendering
Cause its thermal conductivity especially high between graphite flake after into graphite film（Typically< 500 W m-1 K-1）, native graphite radiating
The application of film in a portable device is also restricted.
The content of the invention
Native graphite caused by receiving destruction the invention aims to the scale structure solved due to crystalline flake graphite
Film thermal conductivity is relatively low and provides a kind of manufacturer for the natural stone ink film that preparation technology is fairly simple, cost is low and thermal conductivity is higher
Method.
A kind of simple method for preparing of native graphite heat dissipation film proposed by the present invention, using crystalline flake graphite as raw material, warp
The expanded graphite of highly expanded rate is made in the method for crossing liquid phase expansion, and gained expanded graphite is placed on after washing, drying
The natural stone ink film of high heat conduction is pressed or be rolled into direct plate between two panels PET mould release membrances, comprises the following steps that：
（1）Crystalline flake graphite is selected, after crystalline flake graphite and the concentrated sulfuric acid-hydrogen peroxide mixed solution blending, stirs 5-60 min, then
Liquid phase expansion is carried out, it is 10-60 to control liquid phase expansion temperatureoC, Bulking Time are 0.5-48 h, obtain the liquid of highly expanded multiplying power
Phase expanded graphite；
（2）By step（1）Obtained liquid phase expanded graphite is cleaned, and is dried into fluffy powder；
（3）By step（2）Obtained powder is laid among two layers of PET mould release membrance, is entered roll-in under andante pressure or roll spacing and is flattened,
Native graphite heat dissipation film is obtained after the demoulding.
In the present invention, step（1）Described in crystalline flake graphite be 30-250 mesh.
In the present invention, step（1）Described in the concentrated sulfuric acid-hydrogen peroxide mixed solution in, the volume of the concentrated sulfuric acid and hydrogen peroxide
Than for 15:1-5:1, it is 0-60 to control mixing temperature during mixingoC。
In the present invention, step（2）In net liquid phase expanded graphite is washed with deionized water, liquid phase expanded graphite is upper after having cleaned
Clear liquid pH value reaches 5-7.
In the present invention, step（2）It is middle that to control liquid phase expanded graphite drying temperature be 70-120oC, drying time 5-12
h。
In the present invention, step（3）In, before calendering expanded graphite powder need to be placed on the PET of light two layers off-type force from
Between type film, the off-type force of film is 3-30 g in-1, thickness is 50-100 μm.
In the present invention, step（3）Middle powder is during graphite film is rolled into, if using plate pressure, it is 5- to control pressure
30 MPa；If using roll-in, roll spacing is 100-200 μm, and the pressure of roll-in is 1-100 MPa.
The beneficial effects of the present invention are：By the present invention in that with a kind of gentle liquid phase expanding method, lamella chi is obtained
Very little and raw materials size identical expanded graphite, and directly high heat conduction natural stone ink film is made in calendering, compared with thermal expansion graphite film
Improved with thermal conductivity, cost, which has, compared with artificial stone ink film significantly declines.Natural stone of the present invention
Ink film thicknesses are 20-150 μm, and width is about 200 mm, and length is more than 500 mm, and thermal conductivity may be up to 600 W m in face-1 K-1, electrical conductivity can reach 3400 S cm-1。
Embodiment
The present invention is further described below by example.
Embodiment 1
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 30 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.The 100 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 20 μm, uses laser heat conduction method to measure the thermal conductivity in face as 684 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 3447 S cm-1。
Embodiment 2
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 70 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.The 100 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 20 μm, uses laser heat conduction method to measure the thermal conductivity in face as 598 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 3027 S cm-1。
Embodiment 3
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 100 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.The 100 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 20 μm, uses laser heat conduction method to measure the thermal conductivity in face as 531 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 2798 S cm-1。
Embodiment 4
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 150 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.The 100 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 20 μm, uses laser heat conduction method to measure the thermal conductivity in face as 497 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 2460 S cm-1。
Embodiment 5
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 30 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.The 10 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 45 μm, uses laser heat conduction method to measure the thermal conductivity in face as 472 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 2297 S cm-1。
Embodiment 6
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 30 mesh
In, 15 min are stirred, 35o24 h are expanded under C, have been washed after 80o6 h are dried under C.1 MPa roll-in pressures of obtained dry powder
Natural stone ink film is made.
The graphite film thickness of gained is 100 μm, uses laser heat conduction method to measure the thermal conductivity in face as 217 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 1655 S cm-1。
Embodiment 7
The concentrated sulfuric acid and hydrogen peroxide by volume 10:10oIt is well mixed under C, mixed liquor is put into from the crystalline flake graphite of 30 mesh
In, 30 min are stirred, 35o48 h are expanded under C, have been washed after 80o6 h are dried under C.The 40 MPa roll-ins of obtained dry powder
It is pressed into natural stone ink film.
The graphite film thickness of gained is 25 μm, uses laser heat conduction method to measure the thermal conductivity in face as 535 W m-1 K-1,
Four probe method is used to measure electrical conductivity as 2843 S cm-1。
Claims (7)
1. a kind of simple method for preparing of native graphite heat dissipation film, it is characterized in that：Using crystalline flake graphite as raw material, by liquid phase
The expanded graphite of highly expanded rate is made in the method for expansion, and gained expanded graphite is placed on two panels after washing, drying
The natural stone ink film of high heat conduction is pressed or be rolled into direct plate between PET mould release membrances, comprises the following steps that：
（1）Crystalline flake graphite is selected, after crystalline flake graphite and the concentrated sulfuric acid-hydrogen peroxide mixed solution blending, stirs 5-60 min, then
Liquid phase expansion is carried out, it is 10-60 to control liquid phase expansion temperatureoC, Bulking Time are 0.5-48 h, obtain the liquid of highly expanded multiplying power
Phase expanded graphite；
（2）By step（1）Obtained liquid phase expanded graphite is cleaned, and is dried into fluffy powder；
（3）By step（2）Obtained powder is laid among two layers of PET mould release membrance, enters andante pressure or roll-in flattens, after the demoulding
Obtain native graphite heat dissipation film.
2. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（1）Middle institute
The crystalline flake graphite stated is 30-250 mesh.
3. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（1）Middle institute
In the concentrated sulfuric acid-hydrogen peroxide mixed solution stated, the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 15:1-5:1, the concentrated sulfuric acid mixes with hydrogen peroxide
It is 0-60 that mixing temperature is controlled during conjunctionoC。
4. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（2）Middle use
Deionized water cleans liquid phase expanded graphite, and the supernatant pH value of liquid phase expanded graphite reaches 5-7 after having cleaned.
5. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（2）Middle control
Liquid phase expanded graphite drying temperature processed is 70-120oC, drying time are 5-12 h.
6. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（3）In,
Expanded graphite powder need to be placed between the PET mould release membrances of light two layers off-type force before calendering, and the off-type force of film is 3-30 g
in-1, thickness is 50-100 μm.
7. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（3）Middle powder
Body is during graphite film is rolled into, if using plate pressure, it is 5-30 MPa to control pressure；If use roll-in, roll spacing 100-
200 μm, the pressure of roll-in is 1-100 MPa.
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| CN201710969631.8A CN107792851A (en) | 2017-10-18 | 2017-10-18 | A kind of simple method for preparing of native graphite heat dissipation film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171823A (en) * | 2019-04-11 | 2019-08-27 | 华碳(重庆)新材料产业发展有限公司 | A kind of boron doping natural graphite heat dissipation film and preparation method thereof |
| CN110526242A (en) * | 2019-09-19 | 2019-12-03 | 北京中石伟业科技无锡有限公司 | A kind of two-step method graphite calendering device and calendering process |
| CN115959657A (en) * | 2023-03-16 | 2023-04-14 | 清华大学 | Natural graphite-based heat dissipation film and preparation method thereof |
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| CN110171823A (en) * | 2019-04-11 | 2019-08-27 | 华碳(重庆)新材料产业发展有限公司 | A kind of boron doping natural graphite heat dissipation film and preparation method thereof |
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Application publication date: 20180313 |