CN107791614A - The preparation of graphene composite film and its processing technology - Google Patents
The preparation of graphene composite film and its processing technology Download PDFInfo
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- CN107791614A CN107791614A CN201710952944.2A CN201710952944A CN107791614A CN 107791614 A CN107791614 A CN 107791614A CN 201710952944 A CN201710952944 A CN 201710952944A CN 107791614 A CN107791614 A CN 107791614A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 title claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 35
- 239000010439 graphite Substances 0.000 claims abstract description 35
- 239000000839 emulsion Substances 0.000 claims abstract description 19
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000007800 oxidant agent Substances 0.000 claims abstract description 7
- 229920000620 organic polymer Polymers 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012528 membrane Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004575 stone Substances 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229920002717 polyvinylpyridine Polymers 0.000 claims description 3
- 150000003222 pyridines Chemical class 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000701 coagulant Substances 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation of graphene composite film and its processing technology, the strong oxidizer of the graphite of 10 parts by weight and the mass fraction 85%-98% of 5 parts by weight is taken to mix 5min-8min, standing 20min-30min obtains graphite emulsion I after adding the parts by weight stirring of organic polymer coargulator polyacrylamide 1-3 afterwards, the beneficial effects of the invention are as follows：A kind of preparation of graphene composite film of the invention and its processing technology pass through the redox and extraction to graphene, greatly increase the purity of graphene, the effective impurity as Na and Al eliminated in graphene, and the middle film layer of the graphene composite film produced is provided with circular hole, can be when film body be bent, wider space is provided for film body, substantially increase the pliability of graphene composite film, when manufacturing graphene film, the method for introducing centrifugation film forming, make the graphene film formed more uniform, thin and thick difference is smaller, greatly facilitate the processing of follow-up film body.
Description
Technical field
The present invention relates to the preparation of composite membrane and its processing technology, the preparation of specially a kind of graphene composite film and its add
Work technique.
Background technology
Graphene（It is a kind of cellular flat film formed by carbon atom with sp2 hybrid forms, is a kind of only one
The quasi- two-dimensional material of atomic layer level thickness, monoatomic layer graphite is done so being called.Univ Manchester UK physicist An De
Lie Gaimu and Constantine's Nuo Woxiao loves, graphene is isolated from graphite with micromechanics stripping method success, therefore altogether
With acquisition Nobel Prize in physics in 2010.The method of the common power production of graphene is mechanical stripping method, oxidation-reduction method,
Film production method is chemical vapour deposition technique（CVD）.Because its very good intensity, flexible, conductive, heat conduction, optics are special
Property, it is obtained for significant progress in fields such as physics, materialogy, electronic information, computer, Aero-Space.
The existing pliability on graphene composite film still has much room for improvement, and the purity of graphene is handled in the preparation
It is proper also further to increase, and during graphene film forming, if film body is uniform, advantageously reduce adding for follow-up graphene film
Work, simplify the following process of graphene film.
The content of the invention
It is an object of the invention to provide a kind of preparation of graphene composite film and its processing technology and preparation method thereof, with
Solve the problems, such as to propose in above-mentioned background technology.
The purpose of the present invention is achieved by following technical proposals：The preparation and its processing of a kind of graphene composite film
Technique, comprise the technical steps that：
1）The removal of impurities of graphene：The strong oxidizer of the graphite of 10 parts by weight and the mass fraction 85% -98% of 5 parts by weight is taken to mix
Stir 5min-8min, it is rear add after the parts by weight stirring of organic polymer coargulator polyacrylamide 1-3 stand 20min-
30min obtains graphite emulsion I, and graphite emulsion I then is obtained into aquadag by the filter screen that aperture is 0.1mm -0.3mm
Turbid II, then stirred in inflation by ozone into graphite emulsion II, be continued for 10min -20min and obtain graphite
Emulsion III, finally graphite emulsion IIII will be obtained by the filter screen that aperture is 0.1mm -0.3mm again；
2）The separation of graphene：By step 1）The ethanol solution of obtained graphite emulsion IIII and mass fraction 75% -88% and
Clear water is mixed, and stirs 4min -7min, stands 20min -30min afterwards, and band polyacrylamide is dissolved in ethanol solution, and graphite is quiet
It is placed in lower floor's clear water, isolates the muddy water with graphite, be placed in 65 °C -70 °C of hothouse, by moisture in muddy water
Mass fraction drying is to 50% -60%；
3）Graphene film I preparation：Take step 2）The muddy water with graphite obtained is placed in the container equipped with filter membrane, in vacuum
Spend under the conditions of 0.03~-0.1MPa, to be filtered by vacuum, and make container carry out turning for 200~400rpm of rotating speed when filtering
It is dynamic, continue 1h -2h, make graphene film uniformly be distributed under the influence of centrifugal force on the filter membrane of container, taking-up filter membrane simultaneously will
Graphene film separates with filter membrane；
4）Graphene film II processing：By step 3）Obtain graphene film I to be placed in perforating press, be punched out, processing forms stone
Aperture on black alkene film II, graphene film II is 0.1mm-0.25mm, and every cubic decimeter of average mark be furnished with 80-100 this
The circular hole of sample；
5）Graphene film I's and graphene film II is compound：Between graphene film II is placed in into two graphene film I, and pass through liquid
Glue sticking connects to form graphene composite film；
The strong oxidizer is one or both of the concentrated sulfuric acid and permanganic acid.
The thickness of the graphene film II is 0.6mm -0.8mm.
The thickness of the graphene film I is 0.3mm -0.5mm.
The organic polymer coargulator polyacrylamide can be replaced by polyvinyl pyridine salt or polyethyleneimine.
The step 5）In liquid glue be specially the elastic gums of G -988.
The beneficial effects of the invention are as follows：A kind of preparation of graphene composite film of the invention and its processing technology pass through to graphite
The redox and extraction of alkene, the purity of graphene is greatly increased, effectively eliminate picture Na and Al in graphene
Such impurity, and the middle film layer of the graphene composite film produced is provided with circular hole, can be provided when film body bends for film body
Wider space, the pliability of graphene composite film is substantially increased, when manufacturing graphene film, introduce the side of centrifugation film forming
Method, make the graphene film of formation more uniform, thin and thick difference is smaller, greatly facilitates the processing of follow-up film body.
Embodiment
With reference to embodiment further instruction, but following detailed description should not be done and be managed
Solve the limitation to invent body.Those of ordinary skill in the art can apparently make various on the basis of the present invention
Change and change, it should within the scope of invention.
A kind of preparation of graphene composite film and its processing technology, are comprised the technical steps that：
1）The removal of impurities of graphene：The strong oxidizer of the graphite of 10 parts by weight and the mass fraction 85% -98% of 5 parts by weight is taken to mix
Stir 5min-8min, it is rear add after the parts by weight stirring of organic polymer coargulator polyacrylamide 1-3 stand 20min-
30min obtains graphite emulsion I, and graphite emulsion I then is obtained into aquadag by the filter screen that aperture is 0.1mm -0.3mm
Turbid II, then stirred in inflation by ozone into graphite emulsion II, be continued for 10min -20min and obtain graphite
Emulsion III, finally graphite emulsion IIII will be obtained by the filter screen that aperture is 0.1mm -0.3mm again；
2）The separation of graphene：By step 1）The ethanol solution of obtained graphite emulsion IIII and mass fraction 75% -88% and
Clear water is mixed, and stirs 4min -7min, stands 20min -30min afterwards, and band polyacrylamide is dissolved in ethanol solution, and graphite is quiet
It is placed in lower floor's clear water, isolates the muddy water with graphite, be placed in 65 °C -70 °C of hothouse, by moisture in muddy water
Mass fraction drying, by the reduction and extraction to graphene inside impurity, greatly increases graphene to 50% -60%
Purity, effectively eliminate the impurity as Na and Al in graphene；
3）Graphene film I preparation：Take step 2）The muddy water with graphite obtained is placed in the container equipped with filter membrane, in vacuum
Spend under the conditions of 0.03~-0.1MPa, to be filtered by vacuum, and make container carry out turning for 200~400rpm of rotating speed when filtering
It is dynamic, continue 1h -2h, make graphene film uniformly be distributed under the influence of centrifugal force on the filter membrane of container, taking-up filter membrane simultaneously will
Graphene film separates with filter membrane, introduce centrifugation film forming method, make the graphene film of formation more uniform, thin and thick difference compared with
It is small, greatly facilitate the processing of follow-up film body；
4）Graphene film II processing：By step 3）Obtain graphene film I to be placed in perforating press, be punched out, processing forms stone
Aperture on black alkene film II, graphene film II is 0.1mm-0.25mm, and every cubic decimeter of average mark be furnished with 80-100 this
The circular hole of sample, it can provide wider space when film body bends for film body, substantially increase the pliability of graphene composite film；
5）Graphene film I's and graphene film II is compound：Between graphene film II is placed in into two graphene film I, and pass through liquid
Glue sticking connects to form graphene composite film；
The strong oxidizer is one or both of the concentrated sulfuric acid and permanganic acid.
The thickness of the graphene film II is 0.6mm -0.8mm.
The thickness of the graphene film I is 0.3mm -0.5mm.
The organic polymer coargulator polyacrylamide can be replaced by polyvinyl pyridine salt or polyethyleneimine.
The step 5）In liquid glue be specially the elastic gums of G -988, such a colloid bond to be formed graphene film I and
The material that graphene film II is combined into, it is not easy to fall off because of bending.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology that the particular combination of above-mentioned technical characteristic forms
Scheme, while should also cover in the case where not departing from the inventive concept, carried out by above-mentioned technical characteristic or its equivalent feature
The other technical schemes for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (6)
1. preparation and its processing technology of a kind of graphene composite film, it is characterised in that：Comprise the technical steps that：
1）The removal of impurities of graphene：The strong oxidizer of the graphite of 10 parts by weight and the mass fraction 85% -98% of 5 parts by weight is taken to mix
Stir 5min-8min, it is rear add after the parts by weight stirring of organic polymer coargulator polyacrylamide 1-3 stand 20min-
30min obtains graphite emulsion I, and graphite emulsion I then is obtained into aquadag by the filter screen that aperture is 0.1mm -0.3mm
Turbid II, then stirred in inflation by ozone into graphite emulsion II, be continued for 10min -20min and obtain graphite
Emulsion III, finally graphite emulsion IIII will be obtained by the filter screen that aperture is 0.1mm -0.3mm again；
2）The separation of graphene：By step 1）The ethanol solution of obtained graphite emulsion IIII and mass fraction 75% -88% and
Clear water is mixed, and stirs 4min -7min, stands 20min -30min afterwards, and band polyacrylamide is dissolved in ethanol solution, and graphite is quiet
It is placed in lower floor's clear water, isolates the muddy water with graphite, be placed in 65 °C -70 °C of hothouse, by moisture in muddy water
Mass fraction drying is to 50% -60%；
3）Graphene film I preparation：Take step 2）The muddy water with graphite obtained is placed in the container equipped with filter membrane, in vacuum
Spend under the conditions of 0.03~-0.1MPa, to be filtered by vacuum, and make container carry out turning for 200~400rpm of rotating speed when filtering
It is dynamic, continue 1h -2h, make graphene film uniformly be distributed under the influence of centrifugal force on the filter membrane of container, taking-up filter membrane simultaneously will
Graphene film separates with filter membrane；
4）Graphene film II processing：By step 3）Obtain graphene film I to be placed in perforating press, be punched out, processing forms stone
Aperture on black alkene film II, graphene film II is 0.1mm-0.25mm, and every cubic decimeter of average mark be furnished with 80-100 this
The circular hole of sample；
5）Graphene film I's and graphene film II is compound：Between graphene film II is placed in into two graphene film I, and pass through liquid
Glue sticking connects to form graphene composite film.
2. preparation and its processing technology of a kind of graphene composite film according to claim 1, it is characterised in that：It is described strong
Oxidant is one or both of the concentrated sulfuric acid and permanganic acid.
3. preparation and its processing technology of a kind of graphene composite film according to claim 1, it is characterised in that：The stone
Black alkene film II thickness is 0.6mm -0.8mm.
4. preparation and its processing technology of a kind of graphene composite film according to claim 1, it is characterised in that：The stone
Black alkene film I thickness is 0.3mm -0.5mm.
5. preparation and its processing technology of a kind of graphene composite film according to claim 1, it is characterised in that：It is described to have
Machine high polymer coagulant polyacrylamide can be replaced by polyvinyl pyridine salt or polyethyleneimine.
6. preparation and its processing technology of a kind of graphene composite film according to claim 1, it is characterised in that：Step 5）
In liquid glue be specially the elastic gums of G -988.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710952944.2A CN107791614A (en) | 2017-10-13 | 2017-10-13 | The preparation of graphene composite film and its processing technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710952944.2A CN107791614A (en) | 2017-10-13 | 2017-10-13 | The preparation of graphene composite film and its processing technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107791614A true CN107791614A (en) | 2018-03-13 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710952944.2A Pending CN107791614A (en) | 2017-10-13 | 2017-10-13 | The preparation of graphene composite film and its processing technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111263568A (en) * | 2020-01-22 | 2020-06-09 | Oppo广东移动通信有限公司 | Heat dissipation material, preparation method thereof and electronic equipment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864059A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院兰州化学物理研究所 | Graphene high-efficiency preparation method based on extraction purification technology |
| CN104556018A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of high quality graphene conductive film |
| CN105575679A (en) * | 2015-12-18 | 2016-05-11 | 福州多维炭环保技术有限公司 | Method for preparing graphene membrane electrode |
| CN106139923A (en) * | 2015-04-16 | 2016-11-23 | 中国科学院上海高等研究院 | A kind of graphene oxide framework material composite membrane and its preparation method and application |
| CN106276872A (en) * | 2016-08-03 | 2017-01-04 | 合肥工业大学 | The preparation method of self-supporting transparent conductive graphene membrane |
-
2017
- 2017-10-13 CN CN201710952944.2A patent/CN107791614A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864059A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院兰州化学物理研究所 | Graphene high-efficiency preparation method based on extraction purification technology |
| CN104556018A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of high quality graphene conductive film |
| CN106139923A (en) * | 2015-04-16 | 2016-11-23 | 中国科学院上海高等研究院 | A kind of graphene oxide framework material composite membrane and its preparation method and application |
| CN105575679A (en) * | 2015-12-18 | 2016-05-11 | 福州多维炭环保技术有限公司 | Method for preparing graphene membrane electrode |
| CN106276872A (en) * | 2016-08-03 | 2017-01-04 | 合肥工业大学 | The preparation method of self-supporting transparent conductive graphene membrane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111263568A (en) * | 2020-01-22 | 2020-06-09 | Oppo广东移动通信有限公司 | Heat dissipation material, preparation method thereof and electronic equipment |
| CN111263568B (en) * | 2020-01-22 | 2022-03-11 | Oppo广东移动通信有限公司 | Heat dissipation material, preparation method thereof and electronic equipment |
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Application publication date: 20180313 |