CN106011756A - Metal olefinic carbon heat conduction film and preparation method thereof - Google Patents
Metal olefinic carbon heat conduction film and preparation method thereof Download PDFInfo
- Publication number
- CN106011756A CN106011756A CN201610327285.9A CN201610327285A CN106011756A CN 106011756 A CN106011756 A CN 106011756A CN 201610327285 A CN201610327285 A CN 201610327285A CN 106011756 A CN106011756 A CN 106011756A
- Authority
- CN
- China
- Prior art keywords
- film
- metal
- acid
- 30min
- olefinic carbon
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a metal olefinic carbon heat conduction film and a preparation method thereof. The metal olefinic carbon heat conduction film is formed by compounding at least one layer of graphene film and at least one layer of metal film; and the metal film is deposited on the graphene film, and the thickness ratio of the graphene film to the metal film is 2-9:1. According to the metal olefinic carbon heat conduction film, the metal film is deposited on the graphene film, the metal film and the graphene film are combined without glue, heat resistance is avoided, and the heat conduction coefficients are improved. According to the metal olefinic carbon heat conduction film and the preparation method thereof, the heat conduction coefficients of products can be improved, products of various thicknesses and different heat conduction coefficients can be prepared, and the metal olefinic carbon heat conduction film can be applied to consumer electronics such as mobile products, flat computers and televisions.
Description
Technical field
The invention belongs to Heat Conduction Material field, be specifically related to a kind of metal olefinic carbon heat conducting film and preparation method thereof.
Background technology
Along with microelectronic component develops to miniaturization, high power and high speed, its high heat produced must remove as early as possible so that it is works at a temperature of the operation of safety, is otherwise easily reduced the performance of device, has a strong impact on reliability and the service life of device.
Graphene is a kind of carbon molecule being carried out according to hexagon by carbon atom and arranging and be connected with each other, and its structure is highly stable, and being currently the thinnest is the hardest nano material also, and it is almost fully transparent, only absorbs the light of 2.3%；Heat conductivity is up to 5000W/m K, higher than CNT and diamond, under room temperature, its electron mobility is more than 15000cm2/V s, ratio CNT or silicon wafer height, resistivity about 10-6 Ω cm, lower than copper or silver, because Graphene has the features such as high conductivity, high-termal conductivity, high tenacity, high intensity, extra specific surface area, can be used widely in fields such as electronics, space flight military project, new forms of energy, new materials.
Chinese patent application CN103407268A discloses the preparation method of a kind of composite heat conduction film containing Graphene, comprise the following steps: preparation complexing agent, complexing agent is made up of according to weight ratio following component: copper powder 3～5 parts, butyl acrylate 10～20 parts, guar gum 5～10 parts, magnesium silicate 1～3 parts；By copper powder, butyl acrylate, guar gum and magnesium silicate mix homogeneously at normal temperatures, after mix homogeneously, complexing agent uniform application preparation obtained is on base material；Graphene film is covered above complexing agent, at 50 DEG C, toasts 30min；Again by complexing agent uniform application above graphene film；Composite heat conduction film containing Graphene is cut.The use of glue in the prior art, improves the thermal resistance value of Heat Conduction Material, reduces its thermal conduction effect.
Summary of the invention
In order to overcome problems of the prior art, the present invention provides a kind of metal olefinic carbon heat conducting film, and it does not contains the composition of glue, has given full play to the heat conduction advantage of Graphene, uses again metal material as matrix, has expanded the heat conduction application of Graphene.
The concrete technical scheme of the present invention is:
A kind of metal olefinic carbon heat conducting film, is composited by least one of which graphene film and at least one of which metal film, and metal film deposits on graphene film, and the thickness ratio of graphene film and metal film is for 2-9: 1；The preparation method of metal olefinic carbon heat conducting film comprises the steps: to spray on Copper Foil by watersoluble plumbago alkene dispersion liquid, it is dried 2-3 hour at 80-100 DEG C, the full-automatic tablet machine of dried employing is compacted, pressure is 13-20MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device carry out metal vacuum ion film plating, vacuum-10-6Pa, after plated film at 450-500 DEG C, in inert gas shielding atmosphere, to metal film sprays insulating material；
The preparation method of watersoluble plumbago alkene dispersion liquid comprises the steps: under condition of ice bath, is joined by 1-3g graphite in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20-30min；Further 8-10g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 20-30min；Above-mentioned mixed liquor is transferred in the water-bath of 35-40 DEG C, be slowly added to 20-30g sodium nitrate, stir 20-30min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 70-90 DEG C of temperature transferred to by mixed liquor, stirs 20-30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20-30min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 10-12ml, at a temperature of 40-60 DEG C, react 1h；In above-mentioned solution, drip at least one of 10-12ml acetic acid or hydroiodic acid further, continue reaction 20-60min；
In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 1-2；The concentration of aqueous solution of acetic acid and hydroiodic acid is 5-20wt%；The concentration of aqueous solution of PVP, PVA, PEG is 5-20wt%.
Described metal film is copper film, aluminum film or titanium film.
Described insulant is macromolecular material, and its molecular weight is 1,000,000-140 ten thousand.
Described insulant is polyethylene or polypropylene.
The present invention also provides for the method preparing above-mentioned metal olefinic carbon heat conducting film, comprises the steps:
1) preparation of watersoluble plumbago alkene dispersion liquid: under condition of ice bath, joins in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20-30min by 1-3g graphite；Further 8-10g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 20-30min；Above-mentioned mixed liquor is transferred in the water-bath of 35-40 DEG C, be slowly added to 20-30g sodium nitrate, stir 20-30min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 70-90 DEG C of temperature transferred to by mixed liquor, stirs 20-30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20-30min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 10-12ml, at a temperature of 40-60 DEG C, react 1h；In above-mentioned solution, drip at least one of 10-12ml acetic acid or hydroiodic acid further, continue reaction 20-60min；
2) preparation of metal olefinic carbon heat conducting film: watersoluble plumbago alkene dispersion liquid is sprayed on Copper Foil, being dried 2-3 hour at 80-100 DEG C, the full-automatic tablet machine of dried employing is compacted, and pressure is 13-20MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device carry out metal vacuum ion film plating, vacuum-10-6Pa, after plated film at 450-500 DEG C, in inert gas shielding atmosphere, to metal film sprays insulating material.
Step 1) in mixed acid the volume ratio of concentrated sulphuric acid and concentrated nitric acid be 1: 1-2.
Step 1) in the concentration of aqueous solution of acetic acid and hydroiodic acid be 5-20wt%.
Step 1) in the concentration of aqueous solution of PVP, PVA, PEG be 5-20wt%.
Metal film of the present invention deposits on graphene film, metal film and graphene film combine not by the effect of glue, avoid the generation of thermal resistance, improve heat conductivity, conventional metals Graphene heat conducting film thickness is 0.1-0.2mm, the coefficient of heat conduction is 100-300W/ (m K), and metallic graphite carbon alkene heat conducting film thickness prepared by the present invention is 0.015-0.5mm, and the coefficient of heat conduction is 600-1800W/ (m K).The coefficient of heat conduction of product can be improved by the present invention, multi-thickness, the product of the different coefficient of heat conduction can be prepared, can be applicable to the consumer electronics products such as mobile phone products, panel computer, TV.
Detailed description of the invention
Concrete technology and the parameter of the present invention are as follows:
1) graphene film is formed:
Step is: unreel (speed 1-3m/ is divided) → spraying → dry → calendering (80-100 DEG C) → stripping (15-20Mpa 130-150gf) → rolling (speed 1-3m/ is divided).
2) vacuum ion membrane plating:
Step is: unreel (speed 1-3m/ is divided) → evaporation (vacuum-10-6Pa) → rolling (speed 1-3m/ is divided) → be posted (1-3g/ adhesiveness) → unreel (speed 1-3m/ is divided) → evaporation (vacuum-10-6Pa) → rolling (speed 1-3m/ is divided).
3) thermal spraying:
Step is: unreel (speed 1-3m/ is divided) → thermal spraying (450-500 DEG C) → rolling (speed 1-3m/ is divided) → be posted (1-3g/ adhesiveness) → unreel (speed 1-3m/ is divided) → thermal spraying (450-500 DEG C) → rolling (speed 1-3m/ is divided).
Embodiment 1:
A kind of metal olefinic carbon heat conducting film, is composited by a layer graphene film and one layer of copper film, and copper film deposits on graphene film, and the thickness ratio of graphene film and copper film is 3: 1.The method preparing above-mentioned metal olefinic carbon heat conducting film, comprises the steps:
1) watersoluble plumbago dispersion liquid is formed: under condition of ice bath, joined by 3g graphite in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 30min；Further 10g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 30min；Above-mentioned mixed liquor is transferred in the water-bath of 40 DEG C, be slowly added to 30g sodium nitrate, stir 30min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 90 DEG C of temperature transferred to by mixed liquor, stirs 30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 30min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 12ml, at a temperature of 60 DEG C, react 1h；In above-mentioned solution, drip at least one of 12ml acetic acid or hydroiodic acid further, continue reaction 60min；In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 2；The concentration of aqueous solution of acetic acid and hydroiodic acid is 20wt%；The concentration of aqueous solution of PVP, PVA, PEG is 20wt%.
2) preparation of metal olefinic carbon heat conducting film: watersoluble plumbago alkene dispersion liquid is sprayed on Copper Foil, being dried 3 hours at 100 DEG C, the full-automatic tablet machine of dried employing is compacted, and pressure is 20MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device carry out copper vacuum ion membrane plating, vacuum-10-6Pa, after plated film at 500 DEG C, in inert gas shielding atmosphere, to copper film sprays insulating material.
The copper olefinic carbon heat conducting film thickness of the present embodiment is 0.1-0.2mm, and the coefficient of heat conduction is 800-1200W/ (m K).
Embodiment 2:
A kind of metal olefinic carbon heat conducting film, is composited by a layer graphene film and one layer of titanium film, and titanium film deposits on graphene film, and the thickness ratio of graphene film and titanium film is 6: 1.The method preparing above-mentioned metal olefinic carbon heat conducting film, comprises the steps:
1) watersoluble plumbago dispersion liquid is formed: under condition of ice bath, joined by 1g graphite in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20min；Further 8g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 20min；Above-mentioned mixed liquor is transferred in the water-bath of 35 DEG C, be slowly added to 20g sodium nitrate, stir 20min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 70 DEG C of temperature transferred to by mixed liquor, stirs 20min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 10ml, at a temperature of 40 DEG C, react 1h；In above-mentioned solution, drip at least one of 10ml acetic acid or hydroiodic acid further, continue reaction 20min；In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 1；The concentration of aqueous solution of acetic acid and hydroiodic acid is 5wt%；The concentration of aqueous solution of PVP, PVA, PEG is 5wt%.
2) preparation of metal olefinic carbon heat conducting film: watersoluble plumbago alkene dispersion liquid is sprayed on Copper Foil, being dried 2 hours at 80 DEG C, the full-automatic tablet machine of dried employing is compacted, and pressure is 13MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device carry out titanium vacuum ion membrane plating, vacuum-10-6Pa, after plated film at 450 DEG C, in inert gas shielding atmosphere, to titanium film sprays insulating material.
The titanium olefinic carbon heat conducting film thickness of the present embodiment is 0.015-0.1mm, and the coefficient of heat conduction is 1200-1800W/ (m K).
Embodiment 3:
A kind of metal olefinic carbon heat conducting film, is formed by a layer graphene film and one layer are aluminum film compounded, and aluminum film deposits on graphene film, and the thickness ratio of graphene film and aluminum film is 5: 1.The method preparing above-mentioned metal olefinic carbon heat conducting film, comprises the steps:
1) watersoluble plumbago dispersion liquid is formed: under condition of ice bath, joined by 2g graphite in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20min；Further 9g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 20min；Above-mentioned mixed liquor is transferred in the water-bath of 40 DEG C, be slowly added to 30g sodium nitrate, stir 30min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 80 DEG C of temperature transferred to by mixed liquor, stirs 20min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 10ml, at a temperature of 60 DEG C, react 1h；In above-mentioned solution, drip at least one of 12ml acetic acid or hydroiodic acid further, continue reaction 20min；In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 1；The concentration of aqueous solution of acetic acid and hydroiodic acid is 10wt%；The concentration of aqueous solution of PVP, PVA, PEG is 10wt%.
2) preparation of metal olefinic carbon heat conducting film: watersoluble plumbago alkene dispersion liquid is sprayed on Copper Foil, being dried 2 hours at 90 DEG C, the full-automatic tablet machine of dried employing is compacted, and pressure is 18MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device carry out aluminum vacuum ion membrane plating, vacuum-10-6Pa, after plated film at 480 DEG C, in inert gas shielding atmosphere, to aluminum film sprays insulating material.
The metal olefinic carbon heat conducting film thickness of the present embodiment is 0.05-0.015mm, and the coefficient of heat conduction is 600-800W/ (m K).
Embodiment 4:
A kind of metal olefinic carbon heat conducting film, is composited by a layer graphene film and two-layer copper film, and copper film deposits on graphene film, and the thickness ratio of a layer graphene film and two-layer copper film is 2: 1.The method preparing above-mentioned metal olefinic carbon heat conducting film, comprises the steps:
1) watersoluble plumbago dispersion liquid is formed: under condition of ice bath, joined by 2g graphite in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20min；Further 8g potassium permanganate is joined in above-mentioned mixed liquor, strong agitation 20min；Above-mentioned mixed liquor is transferred in the water-bath of 35 DEG C, be slowly added to 20g sodium nitrate, stir 20min；Under agitation, 100ml deionized water is added continuously in above-mentioned mixed liquor, during then the oil bath of 70 DEG C of temperature transferred to by mixed liquor, stirs 30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 30min；Under agitation, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG, after dissolving, drips the hydrazine hydrate solution of 12ml, at a temperature of 60 DEG C, react 1h；In above-mentioned solution, drip at least one of 12ml acetic acid or hydroiodic acid further, continue reaction 60min；In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 2；The concentration of aqueous solution of acetic acid and hydroiodic acid is 20wt%；The concentration of aqueous solution of PVP, PVA, PEG is 20wt%.
2) preparation of metal olefinic carbon heat conducting film: watersoluble plumbago alkene dispersion liquid is sprayed on Copper Foil, being dried 3 hours at 100 DEG C, the full-automatic tablet machine of dried employing is compacted, and pressure is 20MPa, use full-automatic laminating seperator to peel off after compacting, obtain graphene film；Graphene film use sputtering type evaporated device graphene film two surface is all carried out copper vacuum ion membrane plating, vacuum-10-6Pa, after plated film at 500 DEG C, in inert gas shielding atmosphere, to metal film sprays insulating material.
The metal olefinic carbon heat conducting film thickness of the present embodiment is 0.2-0.5mm, and the coefficient of heat conduction is 600-1000W/ (m K).
Claims (8)
1. a metal olefinic carbon heat conducting film, it is characterised in that: by least one of which graphene film and at least one of which gold
Belonging to film to be composited, metal film deposits on graphene film, and the thickness ratio of graphene film and metal film is
2-9∶1；The preparation method of metal olefinic carbon heat conducting film comprises the steps: to spray to watersoluble plumbago alkene dispersion liquid
On Copper Foil, being dried 2-3 hour at 80-100 DEG C, the full-automatic tablet machine of dried employing is compacted, pressure
Power is 13-20MPa, uses full-automatic laminating seperator to peel off, obtain graphene film after compacting；At Graphene
Sputtering type evaporated device is used to carry out metal vacuum ion film plating, vacuum-10 on film-6Pa, after plated film
At 450-500 DEG C, in inert gas shielding atmosphere, to metal film sprays insulating material；
The preparation method of watersoluble plumbago alkene dispersion liquid comprises the steps: under condition of ice bath, by 1-3g graphite
Join in the concentrated sulphuric acid of 50ml and the mixed acid of concentrated nitric acid, strong agitation 20-30min；Further will
8-10g potassium permanganate joins in above-mentioned mixed liquor, strong agitation 20-30min；Above-mentioned mixed liquor is shifted
In the water-bath of 35-40 DEG C, it is slowly added to 20-30g sodium nitrate, stirs 20-30min；Under agitation,
Being added continuously in above-mentioned mixed liquor by 100ml deionized water, then 70-90 DEG C of temperature transferred to by mixed liquor
In oil bath, stir 20-30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20-30min；Stirring
Under the conditions of mixing, the graphene oxide solution of previous step adds at least one of PVP, PVA, PEG,
Drip the hydrazine hydrate solution of 10-12ml after dissolving, at a temperature of 40-60 DEG C, react 1h；Further above-mentioned
Solution drips at least one of 10-12ml acetic acid or hydroiodic acid, continues reaction 20-60min；
In mixed acid, the volume ratio of concentrated sulphuric acid and concentrated nitric acid is 1: 1-2；The concentration of aqueous solution of acetic acid and hydroiodic acid is
5-20wt%；The concentration of aqueous solution of PVP, PVA, PEG is 5-20wt%.
2. a kind of metal olefinic carbon heat conducting film as claimed in claim 1, it is characterised in that: described metal film is
Copper film, aluminum film or titanium film.
3. a kind of metal olefinic carbon heat conducting film as claimed in claim 1, it is characterised in that: described insulant
For macromolecular material, its molecular weight is 1,000,000-140 ten thousand.
4. a kind of metal olefinic carbon heat conducting film as claimed in claim 1, it is characterised in that: described insulant
For polyethylene or polypropylene.
5. preparation method of metal olefinic carbon heat conducting film as described in claim 1-4 is arbitrary, it is characterised in that bag
Include following steps:
1) preparation of watersoluble plumbago alkene dispersion liquid: under condition of ice bath, joins 50ml's by 1-3g graphite
In the mixed acid of concentrated sulphuric acid and concentrated nitric acid, strong agitation 20-30min；Further 8-10g potassium permanganate is added
Enter in above-mentioned mixed liquor, strong agitation 20-30min；Above-mentioned mixed liquor is transferred to the water-bath of 35-40 DEG C
In, it is slowly added to 20-30g sodium nitrate, stirs 20-30min；Under agitation, by 100ml deionization
Water is added continuously in above-mentioned mixed liquor, during then the oil bath of 70-90 DEG C of temperature transferred to by mixed liquor, and stirring
20-30min；It is added dropwise over 10ml hydrogen peroxide again, continues reaction 20-30min；Under agitation, exist
In the graphene oxide solution of previous step add PVP, PVA, PEG at least one, after dissolving drip
The hydrazine hydrate solution of 10-12ml, reacts 1h at a temperature of 40-60 DEG C；Drip in above-mentioned solution further
At least one of 10-12ml acetic acid or hydroiodic acid, continues reaction 20-60min；
2) preparation of metal olefinic carbon heat conducting film: spray on Copper Foil by watersoluble plumbago alkene dispersion liquid, at 80～100 DEG C
Under be dried 2～3 hours, dried use full-automatic tablet machine to be compacted, pressure is 13-20MPa, compacting
Rear employing automatically fit seperator peel off, obtain graphene film；Graphene film uses sputtering type evaporation
Equipment carries out metal vacuum ion film plating, vacuum-10-6Pa, after plated film at 450-500 DEG C, at indifferent gas
In body protection atmosphere, to metal film sprays insulating material.
6. method as claimed in claim 5, it is characterised in that: step 1) in concentrated sulphuric acid and dense in mixed acid
The volume ratio of nitric acid is 1: 1-2.
7. method as claimed in claim 5, it is characterised in that: step 1) in acetic acid and hydroiodic acid water-soluble
Liquid concentration is 5-20wt%.
8. method as claimed in claim 5, it is characterised in that: step 1) in the water of PVP, PVA, PEG
Solution concentration is 5-20wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610327285.9A CN106011756B (en) | 2016-05-17 | 2016-05-17 | A kind of metal olefinic carbon heat conducting film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610327285.9A CN106011756B (en) | 2016-05-17 | 2016-05-17 | A kind of metal olefinic carbon heat conducting film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106011756A true CN106011756A (en) | 2016-10-12 |
| CN106011756B CN106011756B (en) | 2018-09-18 |
Family
ID=57097562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610327285.9A Active CN106011756B (en) | 2016-05-17 | 2016-05-17 | A kind of metal olefinic carbon heat conducting film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106011756B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106455442A (en) * | 2016-11-02 | 2017-02-22 | 上海博息电子科技有限公司 | Ultra-thin graphene high-conductivity composite |
| CN107876343A (en) * | 2017-12-17 | 2018-04-06 | 张龙远 | A kind of automatic material spray rolling equipment of graphene heat conducting film and material spray calendering technology |
| CN108067375A (en) * | 2017-12-17 | 2018-05-25 | 张龙远 | A kind of automatic material spray equipment of graphene and material spray technique |
| CN109764321A (en) * | 2019-03-08 | 2019-05-17 | 南京理工大学 | A kind of cooling structure of LED illumination lamp and preparation method thereof |
| CN117183539A (en) * | 2023-09-26 | 2023-12-08 | 湖北汇启丰板材有限责任公司 | Novel plate facing processing technology |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101474898A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Conductive carbon film based on graphene as well as preparation method and application |
| CN104070715A (en) * | 2014-06-10 | 2014-10-01 | 广州市尤特新材料有限公司 | Graphene heat conduction and soaking film |
| CN204031708U (en) * | 2014-07-17 | 2014-12-17 | 苏州滕艺科技有限公司 | A kind of heat conduction and heat radiation and electromagnetic wave eliminator |
| CN204466141U (en) * | 2015-04-09 | 2015-07-08 | 新纶科技（常州）有限公司 | A kind of Graphene composite radiating film |
| US20150371848A1 (en) * | 2014-06-20 | 2015-12-24 | The Regents Of The University Of California | Method for the fabrication and transfer of graphene |
-
2016
- 2016-05-17 CN CN201610327285.9A patent/CN106011756B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101474898A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Conductive carbon film based on graphene as well as preparation method and application |
| CN104070715A (en) * | 2014-06-10 | 2014-10-01 | 广州市尤特新材料有限公司 | Graphene heat conduction and soaking film |
| US20150371848A1 (en) * | 2014-06-20 | 2015-12-24 | The Regents Of The University Of California | Method for the fabrication and transfer of graphene |
| CN204031708U (en) * | 2014-07-17 | 2014-12-17 | 苏州滕艺科技有限公司 | A kind of heat conduction and heat radiation and electromagnetic wave eliminator |
| CN204466141U (en) * | 2015-04-09 | 2015-07-08 | 新纶科技（常州）有限公司 | A kind of Graphene composite radiating film |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106455442A (en) * | 2016-11-02 | 2017-02-22 | 上海博息电子科技有限公司 | Ultra-thin graphene high-conductivity composite |
| CN107876343A (en) * | 2017-12-17 | 2018-04-06 | 张龙远 | A kind of automatic material spray rolling equipment of graphene heat conducting film and material spray calendering technology |
| CN108067375A (en) * | 2017-12-17 | 2018-05-25 | 张龙远 | A kind of automatic material spray equipment of graphene and material spray technique |
| CN109764321A (en) * | 2019-03-08 | 2019-05-17 | 南京理工大学 | A kind of cooling structure of LED illumination lamp and preparation method thereof |
| CN117183539A (en) * | 2023-09-26 | 2023-12-08 | 湖北汇启丰板材有限责任公司 | Novel plate facing processing technology |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106011756B (en) | 2018-09-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106011756A (en) | Metal olefinic carbon heat conduction film and preparation method thereof | |
| CN104130719B (en) | A kind of graphene oxide conductive adhesive and preparation and application thereof | |
| Wang et al. | Low‐cost metallic anode materials for high performance rechargeable batteries | |
| KR100841665B1 (en) | Method for forming fine copper particle sintered product type of electric conductor having fine shape, method for forming fine copper wiring and thin copper film using said method | |
| KR101398821B1 (en) | Method of manufacturing metal nano-particle, conductive ink composition having the metal nano-particle and method of forming conductive pattern using the same | |
| TWI342030B (en) | Electrode member for capacitor and method for manufacturing the same, and capacitor including the electrode member | |
| TW201117231A (en) | Ink for printing, metal nanoparticle utilized in ink, wiring, circuit substrate and semiconductor package | |
| CN107394224A (en) | It is a kind of that the method in slim switch-board thermoelectric pond and slim switch-board thermoelectric pond are prepared based on fused salt plasma spray technology lamination | |
| EP2171755A1 (en) | Methods for attachment and devices produced using the methods | |
| CN103131232A (en) | High-performance aqueous graphene paint and preparation method thereof | |
| CN103456926A (en) | Preparation methods of silicon-graphene composite material and lithium ion battery | |
| CN108206285A (en) | A kind of nanometer tin negative pole material of compound coating and its preparation method and application | |
| CN105084858B (en) | A kind of preparation method of graphene film | |
| CN102826540B (en) | A kind of method preparing reduced graphene or graphene film | |
| CN105950904A (en) | Preparing method for silver plating graphene enhanced copper-based electric contact material | |
| CN105523552A (en) | Graphene compound conductive powder and preparation method thereof | |
| CN114951947A (en) | Preparation and packaging method of graphene reinforced tin-based composite solder | |
| CN105800597B (en) | A kind of preparation method of mechanical stripping high conductivity composite graphite alkene | |
| CN105590753A (en) | Preparation method of shell-core carbon coating manganese nanocomposite particles and hell-core carbon coating manganese alloy oxide nanocomposite particles, and application thereof | |
| JP5764452B2 (en) | Method for manufacturing metal structure, metal structure, and metal part | |
| CN109763321B (en) | Conductive graphene/silver composite aramid fiber tow and preparation method thereof | |
| CN114672233A (en) | Photothermal super-hydrophobic coating based on MXene @ Au hybrid and preparation method thereof | |
| CN103579626A (en) | Graphene/tin composite material, preparation method of grapheme/tin composite material, lithium ion battery and preparation method of lithium ion battery | |
| Li et al. | Na-K liquid alloy: A review on wettability enhancement and ionic carrier selection mechanism | |
| CN105401149B (en) | A kind of preparation method of copper diamond composite gold tin welding coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhang Xin Inventor after: Zeng Junxin Inventor before: Zhang Xin |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230831 Address after: 266000 Tonghe Industrial Park, Pingdu City, Qingdao, Shandong Province Patentee after: Qingdao Sanchuan Tianrun Carbon Co.,Ltd. Address before: No. 12 Tongkang Road, Tonghe Industrial Park, Pingdu City, Qingdao, Shandong Province, 266706 Patentee before: QINGDAO HAOTIAN KAWASAKI CARBON MATERIALS TECHNOLOGY Co.,Ltd. |