CN106167693B - Preparation method of graphene-based film product - Google Patents
Preparation method of graphene-based film product Download PDFInfo
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- CN106167693B CN106167693B CN201610451638.6A CN201610451638A CN106167693B CN 106167693 B CN106167693 B CN 106167693B CN 201610451638 A CN201610451638 A CN 201610451638A CN 106167693 B CN106167693 B CN 106167693B
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Abstract
The invention discloses a preparation method of a graphene-based film product, which comprises the following steps: (1) preparing slurry; (2) coating under a magnetic field. The invention provides a preparation method of a graphene-based film product, which can be used for preparing a graphene heat-conducting film with high heat conduction efficiency. The graphene-based film product is prepared by preparing slurry by selecting specific graphene, a heat conduction auxiliary agent, an adhesion auxiliary agent, a binder and a solvent, and coating and drying the slurry under the action of a magnetic field. Compared with the graphene heat-conducting film prepared by the traditional method, the film product disclosed by the invention is good in heat-conducting property, and the cooling amplitude is about 4.9 ℃. After the film is coated and dried under the action of a magnetic field, the film product disclosed by the invention has the advantages that the film layer density is improved, and the density is increased by about 30-50%. The heat-conducting film has good binding force, is not easy to fall off and has excellent water resistance. The preparation method disclosed by the invention is simple in process steps, easy to operate and implement, mild in preparation conditions and easy to control.
Description
Technical Field
The invention relates to a preparation method of a graphene-based film product, and particularly belongs to the technical field of graphene.
Background
Graphene is the thinnest, hardest nanomaterial known to the world, and it is almost completely transparent, absorbing only 2.3% of light; the heat conductivity coefficient is as high as 5300W/m.K, higher than that of carbon nano tube and diamond, and its electron mobility is over 15000cm at normal temp2V.s, higher than carbon nanotube or silicon crystal, and a resistivity of only about 10-6Omega cm, lower than copper or silver, is the material with the smallest resistivity in the world. Because of its extremely low resistivity and high electron transfer rate, it is expected to be used for the development of a new generation of thinner and higher-conduction electronic devices or transistors. Since graphene is essentially a transparent and good conductor, it is also suitable for manufacturing transparent touch screens, optical panels, and even solar cells.
Graphene is often used to prepare thermally conductive films due to its thermal conductivity. The heat-conducting film prepared by the traditional preparation process of the graphene heat-conducting film is not excellent enough in heat-conducting property and limited in cooling amplitude. Therefore, it is especially necessary to research a preparation method of a graphene heat-conducting film which can obtain excellent heat-conducting performance and improve the cooling range.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a graphene-based film product, which can be used for preparing a graphene heat-conducting film with high heat conduction efficiency.
In order to achieve the above object, the present invention adopts the following technical solutions:
a method for preparing a graphene-based film product, comprising the steps of: (1) preparing slurry; (2) coating under a magnetic field.
The preparation method of the graphene-based film product specifically comprises the following steps:
(1) preparation of slurry: adding graphene, a heat conduction auxiliary agent and a bonding auxiliary agent into a ball milling tank in which ball milling beads are added in advance, then dropwise adding a bonding agent, then adding a solvent, carrying out ball milling, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use;
(2) coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and drying in the presence of the magnetic field to obtain the coating material.
In the preparation method of the graphene-based film product, in the step (2), the magnetic field is arranged at a position 0-3 cm away from the substrate, and the strength of the magnetic field is 10 mT-1000 mT.
In the preparation method of the graphene-based film product, in the step (1), the graphene is water-soluble graphene or oil-soluble modified graphene, the heat conduction auxiliary agent is nano ceramic particles, nano zinc oxide, carbon black, carbon nano tubes or boron nitride, the bonding auxiliary agent is cellulose, a cellulose derivative, polyvinyl alcohol or fumed silica, the binder is epoxy resin, polyurethane resin or styrene-butadiene resin, and the solvent is water, ethanol, polyol, acetone, butanone or N-methylpyrrolidone. And a surfactant can be added into the system to promote the system fusion.
The preparation method of the graphene-based film product comprises the step (1), wherein graphene, a heat conduction auxiliary agent and a bonding auxiliary agent are 30-60: 200-500: 40-120 in mass ratio.
According to the preparation method of the graphene-based film product, in the step (1), the mass ratio of the binder to the bonding auxiliary agent is 1-10: 3-80.
In the preparation method of the graphene-based film product, in the step (1), the mass of the graphene is greater than the volume of the solvent by A g: B mL according to the mass-volume ratio, wherein A is greater than or equal to 0 and less than or equal to 10, and B is greater than 0 and less than or equal to 800.
In the preparation method of the graphene-based film product, in the step (1), the ball milling time is 1-36 hours, the weight of ball milling beads is 0.5-5 kg, and the mass ratio of the ball milling beads with different particle diameters is as follows: the ratio of the 1mm particle size ball milling beads to the 5mm particle size ball milling beads to the 10mm particle size ball milling beads is 1-20: 1-10: 1-8. The mass ratio of the ball milling beads with different particle diameters can be adjusted according to the size of the ball mill, and when a small ball mill is adopted, the mass ratio of the ball milling beads with different particle diameters is preferably as follows: the ratio of 2mm particle diameter ball milling beads to 8mm particle diameter ball milling beads is 1-15: 1-6.
In the preparation method of the graphene-based film product, in the step (1), the stirring speed is 100-3000 rpm, and the time is 0.1-12 h.
In the preparation method of the graphene-based film product, in the step (2), the base material is a copper foil, an aluminum foil or a PET film, the thickness of a coating wet film of the coating wire bar is 10-250 micrometers, and the drying is performed at 45-150 ℃.
In order to ensure the scientificity and reasonability of the method, the inventor carries out a series of tests.
The graphene heat-conducting film prepared by the preparation method of the graphene-based film product is subjected to heat-conducting performance test. The graphene heat-conducting film prepared by the method and the heat-conducting film prepared by the traditional method are used for conducting heat-conducting performance test through a device in ZL 2016202621805. The test result shows that the temperature of the heat-conducting film prepared by the method is reduced by about 4.9 ℃, while the temperature of the heat-conducting film prepared by the traditional method is reduced by less than 3.5 ℃. The graphene thermal conductive film is coated under the action of a magnetic field, so that the performance of the graphene thermal conductive film is improved.
The preparation method provided by the invention dries the heat-conducting film in the presence of a magnetic field, so that the performance of the heat-conducting film can be effectively improved. The heat-conducting performance test shows that the heat-conducting film is not directly dried in the presence of a magnetic field, and the cooling amplitude of the heat-conducting film is about 3.5 ℃, which is lower than that of the heat-conducting film prepared by the method.
The magnetic field setting according to the present invention is preferably as shown in fig. 1. The magnetic field is arranged below the base material, and the base material can continuously move due to the arrangement of the guide roller, so that the slurry can be continuously coated on the base material under the magnetic field. The optimal magnetic field is arranged at a position 0-3 cm away from the base material, the magnetic field intensity is 10 mT-1000 mT, and the maximum cooling amplitude can be achieved. When the magnetic field is set by the preparation method, the magnetic force lines are not too dense, and the graphene film is preferably in a stripe shape. A rubber magnetic plate is preferably used as the magnetic field. When the rubber magnetic plate is coated when arranged as a magnetic field, obvious zebra stripes appear on the heat-conducting film in a wet state, and the temperature is reduced by about 4.9 ℃. May be related to the special manufacturing process of the rubber magnetic plate, because the grain is almost the same as the zebra stripe shape of the rubber magnetic plate in the magnetizing mode NSNSNSNS. When the ferrite is arranged as a magnetic field, no obvious magnetic stripe appears due to the over-dense magnetic lines, and the temperature reduction range is about 3.5 ℃.
Compared with the traditional heat-conducting film, the density of the film layer of the graphene heat-conducting film prepared by the method is increased by 30-50%. The binding force of the product is tested by a test method in the standard ISO2409-1992, and the result shows that the graphene heat-conducting film is good in binding force and not easy to fall off. The water resistance test is carried out by directly dripping water on the film layer of the sample to be tested and wiping with a non-woven fabric. The water resistance experiment result shows that the product prepared by the invention has no obvious fading and good water resistance, and the water resistance is gradually improved along with the increase of the dosage of the binder.
According to the invention, nano ceramic particles, nano zinc oxide, carbon black, carbon nano tubes or boron nitride are selected as heat conduction additives, a series of graphene heat conduction films are prepared by adding different heat conduction additives, and the heat conduction performance of the graphene heat conduction films is tested. The results are shown in Table 1. As can be seen from Table 1, the heat-conducting film prepared by using the heat-conducting additive of the invention has large cooling range and good heat-conducting property.
TABLE 1
| Heat-conducting auxiliary | Magnitude of temperature decrease (. degree. C.) |
| Without adding heat-conducting auxiliary agent | 3.6 |
| Nano metal particles | 3.6 |
| Metal powder | 3.7 |
| Nano ceramic powder | 4.7 |
| Nano zinc oxide | 4.5 |
| Carbon nanotube | 4.9 |
| Carbon black | 4.7 |
| Boron nitride | 4.4 |
The invention has the advantages that: the invention provides a preparation method of a graphene-based film product, which can be used for preparing a graphene heat-conducting film with high heat conduction efficiency. The graphene heat-conducting film is prepared by preparing slurry by selecting specific graphene, a heat-conducting auxiliary agent, a bonding agent and a solvent, and coating and drying the slurry under the action of a magnetic field. Compared with the graphene heat-conducting film prepared by the traditional method, the graphene heat-conducting film disclosed by the invention is good in heat-conducting property, and the cooling amplitude is about 4.9 ℃. After the graphene heat-conducting film is coated and dried under the action of a magnetic field, the density of the graphene heat-conducting film layer is improved, and is increased by about 30-50%. The heat-conducting film has good binding force, is not easy to fall off and has excellent water resistance. The preparation method disclosed by the invention is simple in process steps, easy to operate and implement, mild in preparation conditions and easy to control.
Drawings
FIG. 1 is a schematic diagram of the magnetic field arrangement of the present invention;
the meaning of the reference symbols in the figures: 1-base material, 2-guide roller and 3-magnetic plate.
Detailed Description
The invention is further described with reference to specific examples.
The reagents used in the present invention are all commercially available products.
Example 1
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding water-soluble graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 30: 200: 40 into a ball milling tank in which ball milling beads with the weight of 0.5kg are added in advance, then dropwise adding a bonding agent, subsequently adding a solvent, carrying out ball milling for 1h, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring rotation speed is 100rpm, and the stirring time is 12 h. Wherein, the ball milling beads with different particle diameters have the mass ratio: 1: 5: 10mm diameter ball milling bead 1: 1; the heat conduction auxiliary agent is nano ceramic particles; the bonding auxiliary agent is cellulose; the binder is polyurethane resin; the solvent is water; according to the mass ratio, the adhesive agent is 1: 3; according to the mass-volume ratio, the mass of the graphene is 0.1g to 10mL relative to the volume of the solvent.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 3cm away from the substrate, the strength of the magnetic field is 1000mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 150 ℃, so that the coating is obtained. Wherein the base material is copper foil, and the coating wet film thickness of the coating wire rod is 10 microns.
Example 2
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding water-soluble graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 60: 500: 120 into a ball milling tank in which ball milling beads with the weight of 5kg are added in advance, then dropwise adding a bonding agent, subsequently adding a solvent, carrying out ball milling for 36h, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring speed is 3000rpm, and the stirring time is 0.1 h. Wherein, the ball milling beads with different particle diameters have the mass ratio: ball milling beads with particle size of 1 mm: 5 mm: 10 mm: 20: 10: 8; the heat-conducting auxiliary agent is nano zinc oxide; the bonding auxiliary agent is polyvinyl alcohol; the binder is styrene-butadiene resin; the solvent is ethanol; according to the mass ratio, the adhesive agent is 10: 80; according to the mass-volume ratio, the mass of the graphene is 10g to 800mL, and the volume of the solvent is 10g to 800 mL.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 0cm away from the substrate, the strength of the magnetic field is 10mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 45 ℃, so that the coating is obtained. Wherein the substrate is an aluminum foil, and the wet coating film thickness of the coating wire rod is 250 micrometers.
Example 3
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding water-soluble graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 50: 300: 100 into a ball milling tank in which ball milling beads with the weight of 4kg are added in advance, then dropwise adding a bonding agent, subsequently adding a solvent, carrying out ball milling for 18 hours, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring speed is 2000rpm, and the stirring time is 6 hours. Wherein, the ball milling beads with different particle diameters have the mass ratio: ball milling beads with particle size of 1 mm: 5 mm: 10 mm: 5: 4; the heat-conducting auxiliary agent is carbon black; the bonding auxiliary agent is fumed silica; the binder is styrene-butadiene resin; the solvent is a polyol; according to the mass ratio, the adhesive agent is 5: 40; according to the mass-volume ratio, the mass of the graphene is 5g to 300mL relative to the volume of the solvent.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 20mm away from the substrate, the strength of the magnetic field is 500mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 100 ℃, so that the coating is obtained. Wherein the base material is a PET film, and the thickness of the coating wet film of the coating wire rod is 200 microns.
Example 4
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding oil-soluble modified graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 55: 400: 60 into a ball milling tank in which ball milling beads with the weight of 3kg are added in advance, then dropwise adding a bonding agent, subsequently adding a solvent, carrying out ball milling for 12 hours, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring rotation speed is 1500rpm, and the stirring time is 3 hours. Wherein, the ball milling beads with different particle diameters have the mass ratio: ball milling beads with particle size of 1 mm: 5 mm: 10 mm: 15: 2: 7; the heat conduction auxiliary agent is a carbon nano tube; the bonding auxiliary agent is fumed silica; the binder is polyurethane resin; the solvent is acetone; according to the mass ratio, the adhesive agent is mixed with the adhesive auxiliary agent by 9: 20; according to the mass-volume ratio, the mass of the graphene is larger than the volume of the solvent, and the volume of the graphene is 2g to 600 mL.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 10mm away from the substrate, the strength of the magnetic field is 800mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 120 ℃, so that the coating is obtained. Wherein the base material is copper foil, and the coating wet film thickness of the coating wire rod is 50 microns.
Example 5
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding oil-soluble modified graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 35: 450: 110 into a ball milling tank in which ball milling beads with the weight of 0.8kg are added in advance, then dropwise adding a binder, subsequently adding a solvent, carrying out ball milling for 24 hours, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring rotation speed is 2500rpm, and the stirring time is 9 hours. Wherein, the ball milling beads with different particle diameters have the mass ratio: ball milling beads with the particle size of 1 mm: 5 mm: 10mm ═ 6: 9: 2; the heat conduction auxiliary agent is boron nitride; the bonding auxiliary agent is a cellulose derivative; the binder is epoxy resin; the solvent is butanone; according to the mass ratio, the adhesive agent is mixed with the adhesive auxiliary agent at a ratio of 4: 70; according to the mass-volume ratio, the mass of the graphene is 8g to 150 mL.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 6mm away from the substrate, the strength of the magnetic field is 100mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 80 ℃, so that the coating is obtained. Wherein the substrate is an aluminum foil, and the wet coating film thickness of the coating wire rod is 100 micrometers.
Example 6
A method for preparing a graphene-based film product, comprising the steps of:
(1) preparation of slurry: adding oil-soluble modified graphene, a heat conduction auxiliary agent and a bonding auxiliary agent in a mass ratio of 55: 200: 45 into a ball milling tank in which ball milling beads with the weight of 3.5kg are added in advance, then dropwise adding a binder, subsequently adding a solvent, carrying out ball milling for 6 hours, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use, wherein the stirring rotation speed is 500rpm, and the stirring time is 0.5 hour. Wherein, the ball milling beads with different particle diameters have the mass ratio: ball milling beads with particle size of 1 mm: 5 mm: 10mm ═ 11: 3: 5; the heat conduction auxiliary agent is a carbon nano tube; the bonding auxiliary agent is polyvinyl alcohol; the binder is epoxy resin; the solvent is N-methyl pyrrolidone; according to the mass ratio, the adhesive agent is mixed with the adhesive auxiliary agent by 2: 16; according to the mass-volume ratio, the mass of the graphene is larger than the volume of the solvent, and the volume of the graphene is 1g to 120 mL.
(2) Coating under a magnetic field: and (2) placing the substrate treated by the ethanol on a magnetic field, wherein the magnetic field is arranged at a position 1.5cm away from the substrate, the strength of the magnetic field is 400mT, coating the slurry prepared in the step (1) on the substrate through a coating wire rod, and then drying in the presence of the magnetic field, wherein the drying temperature is 100 ℃, so that the coating is obtained. Wherein the base material is a PET film, and the thickness of the coating wet film of the coating wire rod is 30 micrometers.
Claims (5)
1. A preparation method of a graphene-based film product is characterized by comprising the following steps: the method comprises the following steps: (1) preparing slurry; adding graphene, a heat conduction auxiliary agent and a bonding auxiliary agent into a ball milling tank in which ball milling beads are added in advance, then dropwise adding a bonding agent, then adding a solvent, carrying out ball milling, taking out slurry after the ball milling is finished, and removing bubbles through stirring for later use; (2) coating under a magnetic field: placing the substrate treated by the ethanol on a magnetic field, coating the slurry prepared in the step (1) on the substrate by a coating wire rod, and then drying in the presence of the magnetic field to obtain the coating,
the graphene is water-soluble graphene or oil-soluble modified graphene; the heat conduction auxiliary agent is nano ceramic particles, nano zinc oxide, carbon black, carbon nano tubes or boron nitride; the adhesive auxiliary agent is cellulose, cellulose derivative or fumed silica, the adhesive is polyurethane resin or styrene-butadiene resin, the solvent is ethanol, polyalcohol, acetone, butanone or N-methyl pyrrolidone,
in the step (1), the ball milling time is 1-36 h, the weight of ball milling beads is 0.5-5 kg, and the mass ratio of the ball milling beads with different particle diameters is as follows: the coating line bar comprises 1mm particle size ball milling beads, 5mm particle size ball milling beads, 10mm particle size ball milling beads, 1-20: 1-10: 1-8, wherein in the step (2), a magnetic field is arranged at a position 0-3 cm away from a base material, the strength of the magnetic field is 10 mT-1000 mT, in the step (2), the base material is a copper foil, an aluminum foil or a PET film, the thickness of a coating wet film of the coating line bar is 10-250 micrometers, and the drying is drying at 45-150 ℃.
2. The method of preparing a graphene-based film product according to claim 1, characterized in that: in the step (1), graphene, a heat conduction auxiliary agent and a bonding auxiliary agent are 30-60: 200-500: 40-120 by mass ratio.
3. The method of preparing a graphene-based film product according to claim 1, characterized in that: in the step (1), the mass ratio of the binder to the bonding auxiliary agent is 1-10: 3-80.
4. The method of preparing a graphene-based film product according to claim 1, characterized in that: in the step (1), the mass of the graphene and the volume of the solvent are Ag: B mL according to the mass-volume ratio, wherein A is more than 0 and less than or equal to 10, and B is more than 0 and less than or equal to 800.
5. The method of preparing a graphene-based film product according to claim 2, characterized in that: in the step (1), the stirring speed is 100-3000 rpm, and the time is 0.1-12 h.
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| CN108328938B (en) * | 2017-01-20 | 2020-10-30 | 株洲晨昕中高频设备有限公司 | Heat-conducting graphite sheet and production method thereof |
| JP6831017B2 (en) * | 2017-09-22 | 2021-02-17 | 住友化学株式会社 | Composition, film and method for producing the film |
| CN107916041A (en) * | 2017-12-14 | 2018-04-17 | 深圳市国创珈伟石墨烯科技有限公司 | Graphene heat dissipation copper foil coating, preparation method and application |
| CN109679525A (en) * | 2018-12-29 | 2019-04-26 | 厦门十一维科技有限公司 | The preparation facilities of conductive tape and preparation method thereof based on graphene |
| CN109536142B (en) * | 2019-01-15 | 2020-07-31 | 苏州世华新材料科技股份有限公司 | Preparation method of graphene film heat conduction material |
| CN111037971B (en) * | 2019-11-25 | 2020-08-21 | 江苏鸿凌达科技有限公司 | Graphene heat-conducting thick film manufacturing process |
| CN112277435B (en) * | 2020-10-10 | 2021-07-13 | 山东华冠智能卡有限公司 | Production equipment and production method of graphene RFID tag antenna |
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| CN103224638A (en) * | 2013-05-03 | 2013-07-31 | 中国科学院上海硅酸盐研究所 | Filler-textured polymer matrix composite material with high thermal conductivity and preparation method thereof |
| CN103694706A (en) * | 2013-12-26 | 2014-04-02 | 昆山攀特电陶科技有限公司 | High-thermal-conductivity magnetic composite material and preparation method thereof |
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| CN103224638A (en) * | 2013-05-03 | 2013-07-31 | 中国科学院上海硅酸盐研究所 | Filler-textured polymer matrix composite material with high thermal conductivity and preparation method thereof |
| CN103694706A (en) * | 2013-12-26 | 2014-04-02 | 昆山攀特电陶科技有限公司 | High-thermal-conductivity magnetic composite material and preparation method thereof |
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