CN107867685A - A kind of preparation method of the native graphite heat dissipation film of high heat conductance - Google Patents
A kind of preparation method of the native graphite heat dissipation film of high heat conductance Download PDFInfo
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- CN107867685A CN107867685A CN201710969349.XA CN201710969349A CN107867685A CN 107867685 A CN107867685 A CN 107867685A CN 201710969349 A CN201710969349 A CN 201710969349A CN 107867685 A CN107867685 A CN 107867685A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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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 large scale, the preparation method of the native graphite heat dissipation film of high heat conductance, 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, the expanded graphite of suboxides degree is prepared by the mode of oxidizing strictly controlled for obtained expanded graphite, after suboxides expanded graphite is cleaned, slurry and the film in substrate are prepared into by way of adding solvent and applying active force, obtained wet film demoulding after drying winding, and carry out graphitization processing, calendering, obtain the natural stone ink film of high heat conductance.3 20 μm of thickness, the mm of width 50 200 can simply be made very much using this method, length is more than 2m inexpensive natural stone ink film, and the thermal conductivity in its face can reach 1250 W m‑1 K‑1, electrical conductivity can reach 4200 S cm‑1。
Description
Technical field
It is more particularly to a kind of inexpensive, high heat conductance natural the present invention relates to a kind of preparation method of natural stone ink film
Graphite radiating membrane preparation method.
Background technology
With the continuous development of integrated circuit, the volume of various electronic components constantly reduces, but because function is continuously increased,
Caused heat is more and more in unit area, therefore the development of integrated circuit proposes higher requirement to heat sink material.
The radiating modes such as currently used heat-conducting silicone grease, heat conduction elargol, metal and water cooling are because thermal conductivity is low, density is big
And the problems such as assembling space limitation, it is increasingly difficult to meet the growth requirement of integrated circuit.In recent years, the graphite film of heat transmission
It is flexible with considerable thermal conductivity and electrical conductivity, and density is relatively low（< 2 g cm-3）, in terms of circuit and battery radiating
With preferable application prospect.
The method of the graphite radiating film of high heat conductance is prepared at present predominantly using polyimides, polyamide, polyetherimide
One or more polymer films such as amine, polyoxadiazoles, polybenzimidazoles, polyimidazole, pressed again by carbonization, graphitizable high temperature processing
Prolong into the electrographite film of high heat conduction（CN103011141A, CN103144387A, CN102803137A）, this electrographite film
Typically there is thermal conductivity in higher face（> 1000 W m-1 K-1）, but because polymer film presoma cost is very high, lead
Cause the price of this kind of electrographite film also higher, limit its application in downstream.And the product of current artificial stone ink film
General thickness is further made thinner sample and is faced with larger challenge at 17-25 μm.
And roll the natural stone ink film of preparation after being expanded using native graphite as raw material then due to being lacked with relatively more
Fall into, thermal conductivity will not be especially high（< 500 W m-1 K-1, Wu H, Drzal L T, Carbon, 2012,50,1135.
Wang L W, Metcalf S J, Critoph R E, et al. Carbon, 2011, 49, 4812）, and mechanical property
Can be also poor compared with electrographite film.Also obtained using graphene oxide or graphene to prepare the research of native graphite heat dissipation film
Good progress, Publication No. CN104936892 patent disclose a kind of method that plating prepares graphene film, can be in electricity
The regulation and control of pole surface grow graphene film；Publication No. CN105523547A patent is disclosed using large stretch of graphene oxide
The preparation method of solution film forming, the heat dissipation film of preparation have very high thermal conductivity.But current graphene and graphite oxide
The price of alkene is still high so that the cost for preparing heat dissipation film for raw material using graphene or graphene oxide may not be certain to compare
Artificial stone ink film it is low.
The content of the invention
The invention aims to solve electrographite film, graphene film cost be too high, natural stone ink film thermal conductivity compared with
Manufacture method low and that the natural stone ink film that a kind of cost is relatively low and thermal conductivity is higher is provided.
A kind of preparation method of high heat conduction native graphite heat dissipation film proposed by the present invention, using crystalline flake graphite as raw material,
The expanded graphite of highly expanded rate is made in method by liquid phase expansion, by the expanded graphite of the highly expanded rate of gained in oxidation processes
Afterwards by washing, be deployed into graphite slurry and film, obtain wet film, graphitization processing is carried out after wet film drying, and roll it is smooth,
The native graphite heat dissipation film of high heat conductance is obtained, is comprised the following steps that：
（1）Crystalline flake graphite is selected, after crystalline flake graphite and the concentrated sulfuric acid-hydrogen peroxide mixed solution blending, 5-60 min is stirred, carries out
Liquid phase expands, and obtains the expanded graphite of high abdominal distension rate, it is 10-60 to control expansion temperatureoC, Bulking Time are 0.5-48 h；
（2）By step（1）The expanded graphite of obtained highly expanded rate is put into the concentrated sulfuric acid, after being subsequently added into potassium permanganate blending,
Oxidation processes are carried out, oxidizing temperature is 20-60oC, oxidization time are to wash the expanded graphite of gained after 0.5-2 h has been aoxidized
Only；
（3）To step（2）Organic solvent is added in obtained expanded graphite, the slurry of expanded graphite is prepared by applying external force
Material, then slurry is concentrated to give, the solid content concentrated in disposed slurry is 2.0-3.5 wt%；
（4）By step（3）Obtained slurry film in substrate, wet film obtain graphite film after drying, passed through after graphite film is stripped
Graphitization processing is crossed, is then placed in mould release membrance and rolls, that is, obtains the native graphite heat dissipation film of high heat conductance.
In the present invention, step（1）Described in crystalline flake graphite be 30-200 mesh.
In the present invention, step（1）Described in the concentrated sulfuric acid-hydrogen peroxide mixed solution in the volume ratio of the concentrated sulfuric acid and hydrogen peroxide
For 15:1-5:1, temperature control is in 0-60 when the concentrated sulfuric acid and hydrogen peroxide mixoC。
In the present invention, step（2）During middle oxidation processes, 1 g expanded graphites need to use the 100-200 mL concentrated sulfuric acids and
0.5-3 g potassium permanganate.
In the present invention, step（2）Described in clean be to be cleaned the expanded graphite after oxidation using deionized water, after washing
Slurry is filtered using the screen cloth of 200-1000 mesh, pH value is 5-7 in the clear liquid filtered out.
In the present invention, step（3）Described in organic solvent be methanol, ethanol, ethylene glycol, propyl alcohol, isopropanol, glycerine or
The mixed solvent of any one Organic Alcohol such as butanol or a variety of Organic Alcohols, control organic solvent and step（2）In obtained expansion
The mass ratio of graphite is 1:1–5:1.
In the present invention, step（3）Described in apply external force prepare slurry mode can be water bath sonicator, Probe Ultrasonic Searching or
Any in high speed shear, processing time is 2-48 h.
In the present invention, step（3）Described in thickening temperature be 80-120oC, concentration time are 0.5-6h.
In the present invention, the substrate of film is off-type force 3-200 gin-1PET mould release membrances, the wet-film thickness of film is
0.05-3 mm, 25-90o0.5-48h is dried under C and obtains dry graphite film.
In the present invention, step（4）Described in graphitization processing when programming rate be 5-10oC min-1, graphited processing
Temperature is 2500-3000oC, the time of graphitization processing is 1-12 h.
In the present invention, step（4）Described in calendering process be roll-in, i.e., the complete graphite film of graphitization processing is placed on two
Piece off-type force is 3-200 gin-1PET mould release membrances between, the roll spacing of roll-in is 100-200 μm, and pressure be 1-11 MPa, is pressed
The native graphite heat dissipation film of high heat conductance is can obtain after having prolonged by demoulding processing.
The beneficial effects of the present invention are：Using a kind of easy graphite slurry preparation method, it is prepared for and Delanium
The ultra-thin high heat conduction natural stone ink film that film properties are suitable, cost but substantially reduces, the application for graphite radiating film downstream provide
More possibilities.Described native graphite film thickness is 3-20 μm, and width be 50-200 mm, and length is more than 2m, hot in face
Conductance may be up to 1250 W m-1 K-1, electrical conductivity can reach 4200 S cm-1。
Embodiment
The present invention is further described below by example.
Embodiment 1
The concentrated sulfuric acid and hydrogen peroxide by volume 9:10oMixed under C, weigh 150 mesh crystalline flake graphite 11g and be put into mixed liquor and stir
Mix 15 min, 25o48 h are expanded under C, the 1.1 L concentrated sulfuric acids and 11 g potassium permanganate are then added, 35o1 h is aoxidized under C, is washed
It is net be filtered dry after, 3.5 L isopropanols are added, 100 after the h of water bath sonicator 10o1 h is concentrated under C, it is 2.8 wt% to obtain solid content
Slurry.It is 5 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 2 mm, 90oC dries 0.5 h, and dry film takes off
It is put into after mould winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 1 h.
It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 5 MPa.
Obtained native graphite radiating film thickness is 7 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1202 W
m-1 K-1, use four probe method to measure electrical conductivity as 4076 S cm-1。
Embodiment 2
The concentrated sulfuric acid and hydrogen peroxide by volume 10:10oMixed under C, weigh 32 mesh crystalline flake graphite 5g and be put into mixed liquor and stir
3 min, 35o6 h are expanded under C, the 1 L concentrated sulfuric acids and 6 g potassium permanganate are then added, 50o1 h is aoxidized under C, cleans and is filtered dry
Afterwards, 1.5 L methanol are added, 80 after the h of Probe Ultrasonic Searching 2o2 h are concentrated under C, obtain the slurry that solid content is 2.5 wt%.Will slurry
It is 14 g in that material, which is coated in off-type force,-1Mould release membrance on, wet-film thickness is 2.5 mm, 50oC dries 12 h, is put after dry film demoulding winding
Enter in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 1 h.The graphite of burning-out
It is 3 g in that film, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 7 MPa.
Obtained native graphite radiating film thickness is 5 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1026 W
m-1 K-1, use four probe method to measure electrical conductivity as 3757S cm-1。
Embodiment 3
The concentrated sulfuric acid and hydrogen peroxide by volume 15:10oMixed under C, weigh 50 mesh crystalline flake graphite 1g and be put into mixed liquor and stir
1 min, 35o24 h are expanded under C, the 200mL concentrated sulfuric acids and 0.5 g potassium permanganate are then added, 35o1 h is aoxidized under C, is cleaned
After being filtered dry, 100mL butanol is added, 100 after the h of Probe Ultrasonic Searching 1o0.5 h is concentrated under C, obtains the slurry that solid content is 3.0 wt%
Material.It is 7 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 3 mm, 25oC dries 36 h, dry film demoulding winding
After be put into graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 1 h.Burn down
It is 3 g in that graphite film, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 5 MPa.
Obtained native graphite radiating film thickness is 10 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1127
W m-1 K-1, use four probe method to measure electrical conductivity as 3982 S cm-1。
Embodiment 4
The concentrated sulfuric acid and hydrogen peroxide by volume 10:10oMixed under C, weigh the g of 80 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 1 min, 25o24 h are expanded under C, the 150mL concentrated sulfuric acids and 0.7 g potassium permanganate are then added, 35o2 h are aoxidized under C, are washed
It is net be filtered dry after, 100mL isopropanols are added, 100 after the h of water bath sonicator 3o2 h are concentrated under C, it is 3.2 wt%'s to obtain solid content
Slurry.It is 14 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 1 mm, 90oC dries 0.5 h, and dry film takes off
It is put into after mould winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 1 h.
It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 11 MPa.
Obtained native graphite radiating film thickness is 3 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1149 W
m-1 K-1, use four probe method to measure electrical conductivity as 4002 S cm-1。
Embodiment 5
The concentrated sulfuric acid and hydrogen peroxide by volume 7:10oMixed under C, weigh the g of 100 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 30 min, 35o48 h are expanded under C, the 100 mL concentrated sulfuric acids and 1 g potassium permanganate are then added, 35o1.5 h are aoxidized under C,
Clean after being filtered dry, 100 mL ethanol of addition, 120 after the h of water bath sonicator 5o1.5 h are concentrated under C, obtain solid content as 2.8
Wt% slurry.It is 5 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 2 mm, 90oC dries 1 h, dry film
It is put into after demoulding winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time 1
h.It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 1 MPa.
Obtained native graphite radiating film thickness is 6 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1209 W
m-1 K-1, use four probe method to measure electrical conductivity as 4124 S cm-1。
Embodiment 6
The concentrated sulfuric acid and hydrogen peroxide by volume 14:10oMixed under C, weigh the g of 200 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 10 min, 25o12 h are expanded under C, the 120 mL concentrated sulfuric acids and 1.5 g potassium permanganate are then added, 35o1.5 are aoxidized under C
H, clean after being filtered dry, 100 mL isopropanols of addition, 90 after the h of Probe Ultrasonic Searching 1o2 h are concentrated under C, obtain solid content as 2.6
Wt% slurry.It is 14 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 2 mm, 90oC dries 1 h, dry film
It is put into after demoulding winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time 1
h.It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 6 MPa.
Obtained native graphite radiating film thickness is 5 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1174 W
m-1 K-1, use four probe method to measure electrical conductivity as 4074S cm-1。
Embodiment 7
The concentrated sulfuric acid and hydrogen peroxide by volume 8:10oMixed under C, weigh the g of 250 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 5 min, 25o48 h are expanded under C, the 100 mL concentrated sulfuric acids and 0.7 g potassium permanganate are then added, 35o2 h are aoxidized under C,
Clean after being filtered dry, 100 mL isopropanols of addition, 100 after the h of water bath sonicator 3o3 h are concentrated under C, obtain solid content as 3.5
Wt% slurry.It is 14 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 1 mm, 90oC dries 0.5 h, does
It is put into after film demoulding winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time 1
h.It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 8 MPa.
Obtained native graphite radiating film thickness is 4 μm, uses laser heat conduction method to measure the thermal conductivity in face as 974W m-1
K-1, use four probe method to measure electrical conductivity as 3744 S cm-1。
Embodiment 8
The concentrated sulfuric acid and hydrogen peroxide by volume 8:10oMixed under C, weigh the g of 150 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 15 min, 35o24 h are expanded under C, the 150 mL concentrated sulfuric acids and 1.2 g potassium permanganate are then added, 35o1 h is aoxidized under C,
Clean after being filtered dry, 100 mL ethanol of addition, 100 after the h of water bath sonicator 12o1.5 h are concentrated under C, obtain solid content as 3.0
Wt% slurry.It is 3 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 2 mm, 90oC dries 1 h, dry film
It is put into after demoulding winding in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time 2
h.It is 3 g in that the graphite film of burning-out, which is placed on two panels off-type force,-1Mould release membrance in, flattened under 6 MPa.
Obtained native graphite radiating film thickness is 5 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1250 W
m-1 K-1, use four probe method to measure electrical conductivity as 4240 S cm-1。
Embodiment 9
The concentrated sulfuric acid and hydrogen peroxide by volume 12:10oMixed under C, weigh the g of 150 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 1 min, 25o24 h are expanded under C, the 200 mL concentrated sulfuric acids and 3 g potassium permanganate are then added, 35o2 h are aoxidized under C, are washed
It is net be filtered dry after, 100mL isopropanols are added, 120 after the h of water bath sonicator 0.5o2 h are concentrated under C, it is 3 wt%'s to obtain solid content
Slurry.It is 3 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 3 mm, 90oC dries 3 h, and the dry film demoulding is received
It is put into after volume in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 1 h.Burn down
Graphite film to be placed on two panels off-type force be 3 g in-1Mould release membrance in, flattened under 1 MPa.
Obtained native graphite radiating film thickness is 6 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1132 W
m-1 K-1, use four probe method to measure electrical conductivity as 4014 S cm-1。
Embodiment 10
The concentrated sulfuric acid and hydrogen peroxide by volume 8:10oMixed under C, weigh the g of 150 mesh crystalline flake graphite 1 and be put into mixed liquor and stir
Mix 10 min, 25o48 h are expanded under C, the 200 mL concentrated sulfuric acids and 2 g potassium permanganate are then added, 35o2 h are aoxidized under C, are washed
It is net be filtered dry after, 100 mL ethanol are added, 120 after the h of water bath sonicator 24o2 h are concentrated under C, it is 3.5 wt%'s to obtain solid content
Slurry.It is 7 g in that slurry is coated in into off-type force-1Mould release membrance on, wet-film thickness is 1 mm, 90oC dries 2 h, and the dry film demoulding is received
It is put into after volume in graphitizing furnace, programming rate 10oC min-1, graphitization temperature 2800oC, processing time are 2 h.Burn down
Graphite film to be placed on two panels off-type force be 3 g in-1Mould release membrance in, flattened under 6 MPa.
Obtained native graphite radiating film thickness is 5 μm, uses laser heat conduction method to measure the thermal conductivity in face as 1247 W
m-1 K-1, use four probe method to measure electrical conductivity as 4239 S cm-1。
Claims (11)
- A kind of 1. preparation method of high heat conduction native graphite heat dissipation film, it is characterised in that：Using crystalline flake graphite as raw material, pass through The expanded graphite of highly expanded rate is made in the method for liquid phase expansion, and the expanded graphite of the highly expanded rate of gained is passed through after the oxidising treat-ment Washing is crossed, is deployed into graphite slurry and film, wet film is obtained, graphitization processing is carried out after wet film drying, and rolls smooth, is obtained The native graphite heat dissipation film of high heat conductance, is comprised the following steps that：（1）Crystalline flake graphite is selected, after crystalline flake graphite and the concentrated sulfuric acid-hydrogen peroxide mixed solution blending, 5-60 min is stirred, carries out Liquid phase expands, and obtains the expanded graphite of high abdominal distension rate, it is 10-60 to control expansion temperatureoC, Bulking Time are 0.5-48 h；（2）By step（1）The expanded graphite of obtained highly expanded rate is put into the concentrated sulfuric acid, after being subsequently added into potassium permanganate blending, Oxidation processes are carried out, oxidizing temperature is 20-60oC, oxidization time are to wash the expanded graphite of gained after 0.5-2 h has been aoxidized Only；（3）To step（2）Organic solvent is added in obtained expanded graphite, the slurry of expanded graphite is prepared by applying external force Material, then slurry is concentrated to give, the solid content concentrated in disposed slurry is 2.0-3.5 wt%；（4）By step（3）Obtained slurry film in substrate, wet film obtain graphite film after drying, passed through after graphite film is stripped Graphitization processing is crossed, is then placed in mould release membrance and rolls, that is, obtains the native graphite heat dissipation film of high heat conductance.
- 2. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（1） Described in crystalline flake graphite be 30-200 mesh.
- 3. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（1） Described in the concentrated sulfuric acid-hydrogen peroxide mixed solution in the volume ratio of the concentrated sulfuric acid and hydrogen peroxide be 15:1-5:1, the concentrated sulfuric acid and dioxygen Temperature control is in 0-60 when water mixesoC。
- 4. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（2） During middle oxidation processes, 1 g expanded graphites need to use the 100-200 mL concentrated sulfuric acids and 0.5-3 g potassium permanganate.
- 5. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（2） Described in clean be to be cleaned the expanded graphite after oxidation using deionized water, filtered after washing using the screen cloth of 200-1000 mesh Slurry, pH value is 5-7 in the clear liquid filtered out.
- 6. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（3） Described in organic solvent be any one Organic Alcohol or more such as methanol, ethanol, ethylene glycol, propyl alcohol, isopropanol, glycerine or butanol The mixed solvent of kind Organic Alcohol, controls organic solvent and step（2）In the obtained mass ratio of expanded graphite be 1:1–5:1.
- 7. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（3） Described in apply external force to prepare the mode of slurry can be any in water bath sonicator, Probe Ultrasonic Searching or high speed shear, during processing Between be 2-48 h.
- 8. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（3） Described in thickening temperature be 80-120oC, concentration time are 0.5-6h.
- 9. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：The base of film Bottom is off-type force 3-200 gin-1PET mould release membrances, the wet-film thickness of film is 0.05-3 mm, 25-90o0.5-48h is dried under C Obtain dry graphite film.
- 10. the preparation method of high heat conductance native graphite heat dissipation film according to claim 1, it is characterised in that：Step（4） Described in graphitization processing when programming rate be 5-10oC min-1, graphited treatment temperature is 2500-3000oC, graphitization The time of processing is 1-12 h.
- 11. the simple method for preparing of native graphite heat dissipation film according to claim 1, it is characterised in that：Step（4）Middle institute The calendering process stated is roll-in, i.e., it is 3-200 gin the complete graphite film of graphitization processing to be placed on into two panels off-type force-1PET from Between type film, the roll spacing of roll-in is 100-200 μm, and pressure is 1-11 MPa, and height is can obtain by demoulding processing after having rolled The native graphite heat dissipation film of thermal conductivity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111232962A (en) * | 2020-01-17 | 2020-06-05 | 深圳垒石热管理技术有限公司 | Method for preparing ultra-thick graphene heat dissipation film |
| CN114715888A (en) * | 2022-03-29 | 2022-07-08 | 临海伟星新型建材有限公司 | High-thermal-conductivity graphite composite film and preparation method thereof |
| WO2022233028A1 (en) * | 2021-05-07 | 2022-11-10 | 中国科学院深圳先进技术研究院 | Expanded graphite thermal interface material and preparation method therefor |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651961A (en) * | 2012-05-29 | 2012-08-29 | 邱璟 | Heat-conduction heat-dissipation interface material and manufacturing method thereof |
| CN105111484A (en) * | 2015-08-28 | 2015-12-02 | 上海利物盛企业集团有限公司 | Method for efficiently and continuously preparing heat-conducting graphite film on large area |
| CN105253878A (en) * | 2015-11-18 | 2016-01-20 | 复旦大学 | Method for directly preparing expanded graphite or graphene under normal temperature and normal pressure |
| CN105293476A (en) * | 2015-11-16 | 2016-02-03 | 复旦大学 | Preparation method of large-size graphene oxide or graphene |
| US9452934B2 (en) * | 2013-09-12 | 2016-09-27 | The Hong Kong University Of Science And Technology | Synthesis of ultra-large graphene oxide sheets |
| CN106564893A (en) * | 2016-11-10 | 2017-04-19 | 电子科技大学 | Hundred micron-order graphene oxide and preparation method thereof |
| CN106629673A (en) * | 2016-09-13 | 2017-05-10 | 钢铁研究总院 | Preparation method for graphene oxide |
-
2017
- 2017-10-18 CN CN201710969349.XA patent/CN107867685A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651961A (en) * | 2012-05-29 | 2012-08-29 | 邱璟 | Heat-conduction heat-dissipation interface material and manufacturing method thereof |
| US9452934B2 (en) * | 2013-09-12 | 2016-09-27 | The Hong Kong University Of Science And Technology | Synthesis of ultra-large graphene oxide sheets |
| CN105111484A (en) * | 2015-08-28 | 2015-12-02 | 上海利物盛企业集团有限公司 | Method for efficiently and continuously preparing heat-conducting graphite film on large area |
| CN105293476A (en) * | 2015-11-16 | 2016-02-03 | 复旦大学 | Preparation method of large-size graphene oxide or graphene |
| CN105253878A (en) * | 2015-11-18 | 2016-01-20 | 复旦大学 | Method for directly preparing expanded graphite or graphene under normal temperature and normal pressure |
| CN106629673A (en) * | 2016-09-13 | 2017-05-10 | 钢铁研究总院 | Preparation method for graphene oxide |
| CN106564893A (en) * | 2016-11-10 | 2017-04-19 | 电子科技大学 | Hundred micron-order graphene oxide and preparation method thereof |
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| CN111232962A (en) * | 2020-01-17 | 2020-06-05 | 深圳垒石热管理技术有限公司 | Method for preparing ultra-thick graphene heat dissipation film |
| WO2022233028A1 (en) * | 2021-05-07 | 2022-11-10 | 中国科学院深圳先进技术研究院 | Expanded graphite thermal interface material and preparation method therefor |
| CN114715888A (en) * | 2022-03-29 | 2022-07-08 | 临海伟星新型建材有限公司 | High-thermal-conductivity graphite composite film and preparation method thereof |
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