CN113150665A - Medium-high temperature graphene heating slurry and preparation method thereof - Google Patents
Medium-high temperature graphene heating slurry and preparation method thereof Download PDFInfo
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- CN113150665A CN113150665A CN202110042739.9A CN202110042739A CN113150665A CN 113150665 A CN113150665 A CN 113150665A CN 202110042739 A CN202110042739 A CN 202110042739A CN 113150665 A CN113150665 A CN 113150665A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
Abstract
The invention discloses medium-high temperature graphene heating slurry which comprises the following components in parts by weight: 2 to 7 parts of graphene; 2 to 7 parts of carbon nanotubes; 0.5 to 2 parts of dimethylformamide; 0.1 to 1.5 parts of n-butanol; 1 to 6 parts of a thermoplastic polyurethane elastomer rubber; 2 to 5 parts of natural mica; 80 to 95 parts of N-methylpyrrolidone; the invention also discloses a preparation method and a film forming method of the heating slurry; according to the invention, the graphene and the carbon nano tube are effectively combined to form the heating slurry, and the slurry has good heat conduction effect and stable heat resistance after film forming.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to medium-high temperature graphene heating slurry, a preparation method and a film forming method.
Background
Along with the improvement of living standard of people, the demand for heating and thermal equipment is continuously improved, and the main heating components of the equipment in the current market are mostly quartz heating pipes, heating wires, PTC heating components, halogen tubes and the like, and the products often have the problems of short service life, high energy consumption and the like.
In the new graphene heating plate material, the heating base material is mostly high polymer base material, the heating temperature is low, and the overall heating speed is slow. When the temperature of the heating plate is slightly high, the whole heating element is easy to deform and bend, and the obtained medium-high heat material is pyrolyzed, so that the thermal stability is poor, and the service life is short in the using process.
Disclosure of Invention
The invention aims to provide medium-high temperature graphene heating slurry, which effectively combines graphene and carbon nanotubes to form heating slurry, and the slurry has good heat conduction effect and stable heat resistance after film formation.
In order to solve the technical problem, the technical scheme of the invention is as follows: the medium-high temperature graphene heating slurry comprises the following components in parts by weight:
preferably, the composition also comprises the following components in parts by weight:
and 0.5 to 3.5 parts of sodium carboxymethyl cellulose.
Preferably comprises the following components in parts by weight:
most preferably comprises the following components in parts by weight:
the invention also aims to provide a preparation method of the medium-high temperature graphene heating slurry, wherein the carbon nano tubes, the high molecular components and the natural mica enter into the graphene layers along with dissolution in the process of forming graphene by graphite layering, and the graphene, the carbon nano tubes and other components are uniformly dispersed.
In order to solve the technical problem, the technical scheme of the invention is as follows: a preparation method of medium-high temperature graphene heating slurry comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, thermoplastic polyurethane elastomer rubber, natural mica, N-methylpyrrolidone and sodium carboxymethylcellulose in parts by weight, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
adding the graphite powder in parts by weight into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and allowing the carbon nano tubes to enter the graphite interlayer gaps along with liquid in the system along with the gradual increase of the graphite interlayer gaps until the graphite is stripped into graphene in a liquid system;
and step three, removing part of the N-methyl pyrrolidone to obtain the graphene carbon nanotube heating slurry with proper viscosity.
Preferably, steps one through three are performed under vacuum. The method is carried out under vacuum, on one hand, the influence of air in the environment on materials such as graphene, carbon nanotubes and the like is reduced, and the excellent heat conduction effect of the obtained slurry after film forming is ensured.
Preferably, the viscosity of the graphene carbon nanotube heating slurry after the third step is 60 to 70Pa ×.s. The slurry obtained by optimizing the components and the using amount is suitable for coating, good in film forming performance, uniform and compact in film layer obtained after coating on the surface of a substrate, and suitable for production.
The third purpose of the invention is to provide a film forming process of the medium-high temperature graphene heating slurry, the film is formed by controlling the drying condition and the temperature and slowly drying, the formed film is compact, the intermediate polymer and other compositions are effectively coated by the graphene, the carbon nano tubes and the like, the target film has good heat conduction effect and is stable in heat resistance.
In order to solve the technical problem, the technical scheme of the invention is as follows: the film forming method of the medium-high temperature graphene heating slurry comprises the following steps:
step one, coating medium-high temperature graphene heating slurry on the surface of a base material;
and step two, drying in vacuum to form the film after film forming.
Preferably, the vacuum drying conditions in the second step are as follows:
the temperature is 120 ℃ to 150 ℃;
for a period of 3 to 5 hours.
According to the invention, the film layer obtained by coating is dried at low temperature for a long time in a vacuum environment, so that the N-methyl pyrrolidone in the film layer is slowly and thoroughly volatilized, a compact and non-porous film layer is obtained, the graphene is formed to coat and protect other active substances distributed in the film layer, the graphene effectively shields oxygen in the atmosphere and in a high-temperature environment, the substances in the film layer are prevented from reacting or decomposing with the oxygen, and the thermal stability of the film layer is effectively improved.
Preferably, the resulting film has a thermal conductivity of 2600W/(m × K) to 4200W/(m × K). The film layer obtained by the invention has good heat conduction effect and is suitable for being applied to electric heating radiators or other fields needing quick heat dissipation, such as mobile phones, computers and the like.
By adopting the technical scheme, the invention has the beneficial effects that:
the invention obtains a medium-high temperature graphene heat dissipation slurry, which is compounded with thermoplastic polyurethane elastomer rubber and natural mica to obtain a heating slurry with proper viscosity and suitable coating through the composite use of graphene and carbon nano tubes;
the heating slurry prepared by the invention is a uniformly mixed slurry prepared by preparing graphene in situ and embedding the rest components into graphene layers along with graphite layering under the action of ultrasonic waves; the mixture obtained in the dynamic process prevents the secondary aggregation of graphene or carbon nanotubes, and the carbon nanotubes and other components effectively separate and mix the graphite; carbon nanotubes uniformly dispersed in an organic liquid system are gradually inserted between graphene layers along with organic liquid in the graphite stripping process, and dimethylformamide, n-butanol and epoxy resin enter between the graphene layers; the n-butyl alcohol plays an emulsification role to disperse the graphene and the carbon nanotubes and stably disperse the graphene and the carbon nanotubes distributed between the graphene layers, and effectively prevents the graphene and the carbon nanotubes from re-agglomerating due to the attraction of Van der Waals force respectively; thereby obtaining the heating slurry with uniformly dispersed graphene and carbon nano tubes;
the natural mica is added, so that the resistivity and the mechanical property of the film layer are effectively improved, and the reliability of the film layer obtained by the method is improved;
after the film is formed, TPU uniformly dispersed between graphene and carbon nanotubes in the slurry is used as a binder to promote film forming and curing of the film layer, so that the mechanical strength of the cured heat-conducting film is effectively improved, and meanwhile, the heat conductivity of the film layer formed by the carbon nanotubes and the graphene in a directional insertion arrangement mode is 2600W/m K to 4200W/m K, and the heat-conducting effect is good.
Thereby achieving the above object of the present invention.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Example 1
The embodiment discloses medium-high temperature graphene heating slurry, the specific composition of which is shown in table 1 in detail, and the specific preparation method comprises the following steps:
the method comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, TPU, natural mica and N-methylpyrrolidone according to the weight parts recorded in table 1, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound in the first step are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is between 5 and 15 minutes.
Step two, adding graphite powder in parts by weight recorded in table 1 into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and gradually increasing the interlayer gap of the graphite, wherein the carbon nano tube enters the interlayer gap of the graphite along with liquid in the system until the graphite is stripped into graphene in a liquid system;
the process conditions of the ultrasound in the step two are as follows:
1200W to 2000W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is 15 to 25 minutes.
And step three, removing part of the solvent to obtain the graphene carbon nanotube heating slurry with the viscosity of 60-70 Pa s.
The prepared medium-high temperature graphene heating slurry is subjected to film forming according to the following steps:
step one, coating medium-high temperature graphene heating slurry on the surface of a base material;
the base material of the embodiment is copper foil, and the thickness of the copper foil is 50 microns; the coating thickness of the heating slurry is 50-100 micrometers;
step two, vacuum drying after film forming, wherein the specific process conditions are as follows:
the temperature is 120 ℃ to 150 ℃;
for a period of 3 to 5 hours;
and (4) film forming.
Example 2
The main differences between this example and example 1 are detailed in table 1.
Example 3
The main differences between this example and example 1 are detailed in table 1.
Example 4
The main differences between this example and example 1 are detailed in table 1.
Example 5
The main differences between this example and example 1 are detailed in table 1.
Example 6
The main differences between this example and example 1 are detailed in table 1.
Example 7
The main differences between this example and example 1 are detailed in table 1.
Example 8
The main differences between this example and example 1 are detailed in table 1.
Comparative example 1
The main differences between this example and example 1 are detailed in table 1.
Comparative example 2
The main differences between this example and example 1 are detailed in table 1.
Comparative example 3
The main differences between this example and example 1 are detailed in table 1.
Comparative example 4
The main differences between this example and example 1 are detailed in table 1.
Table 1 examples 1 to 9 and comparative examples 1 to 4 heat generating paste raw material components and parts by weight
| Item | Graphene | CNT | DMF | N-butanol | TPU | Natural mica | NMP | CMC |
| Example 1 | 2 | 2 | 0.5 | 0.1 | 1 | 2 | 80 | 0.5 |
| Example 2 | 2.5 | 2.5 | 1.2 | 0.6 | 2 | 3 | 85 | 1.8 |
| Example 3 | 2.8 | 2.8 | 1.2 | 0.7 | 2.5 | 2 | 90 | 2.3 |
| Example 4 | 3.2 | 3.2 | 1.3 | 0.8 | 3 | 3 | 85 | 2.6 |
| Example 5 | 4.5 | 4.5 | 1.5 | 1.2 | 4 | 4 | 90 | 3.2 |
| Example 6 | 5 | 5 | 1.6 | 0.6 | 2 | 2 | 82 | 0.8 |
| Example 7 | 6 | 6 | 1.8 | 1.3 | 5 | 3 | 88 | 1.0 |
| Example 8 | 7 | 7 | 2 | 1.5 | 6 | 5 | 95 | 3.5 |
| Comparative example 1 | 3.2 | 3.2 | 1.3 | 0.8 | 3 | / | 85 | 2.6 |
| Comparative example 2 | 3.2 | 3.2 | 1.3 | 0.8 | / | / | 85 | 2.6 |
| Comparative example 3 | 3.2 | 3.2 | 1.3 | 0.8 | / | 3 | 85 | 2.6 |
| Comparative example 4 | 3.2 | 3.2 | / | / | 3 | 3 | 85 | 2.6 |
The copper foil-coated heat conductive films obtained in examples 1 to 8 and comparative examples 1 to 4 were subjected to performance tests, and specific test items and data are shown in table 2.
TABLE 2 tabulation of indexes of performance of the thermally conductive films obtained in examples 1 to 8 and comparative examples 1 to 4
The tensile strength refers to the resistance of the maximum uniform plastic deformation which can be borne by the material, and is used for judging the mechanical property of the material. The universal electronic testing machine model selected in the paper is as follows: an Instron model 5565 electronic universal tester, manufactured by Instron corporation, usa, was used to test the tensile strength of the prepared graphene-based flexible thermally conductive film during the test. And refer to the related test procedure of national standard JB/T9141.2-1999 on tensile strength of film samples.
Thermal stability temperature the thermal properties of the coatings were analyzed using TG and a thermal conductivity analyzer.
According to the data in tables 1 and 2, the thermal stability temperature of the prepared heating slurry is obviously improved after the film is formed, the thermal conductivity of the heating slurry is also obviously improved, the volume resistance is large, and the heating slurry is suitable for being applied to electric heating equipment; compared with comparative examples 1 to 4, the addition of TPU and natural mica is matched with graphene to separate and form the carbon nano tube and other substances effectively inserted between layers, so that on one hand, the medium-high temperature graphene heat dissipation slurry obtained by the invention is improved, and the slurry is compounded with thermoplastic polyurethane elastomer rubber and natural mica to obtain a heating slurry with proper viscosity and suitable coating through the composite use of graphene and carbon nano tube;
the natural mica is added, so that the resistivity and the mechanical property of the film layer are effectively improved, and the reliability of the film layer obtained by the method is improved;
after the film is formed, TPU uniformly dispersed between graphene and carbon nanotubes in the slurry is used as a binder to promote film forming and curing of the film layer, so that the mechanical strength of the cured heat-conducting film is effectively improved, and meanwhile, the heat conductivity of the film layer formed by the carbon nanotubes and the graphene in a directional insertion arrangement mode is 2600W/m K to 4200W/m K, and the heat-conducting effect is good.
Claims (10)
1. The medium-high temperature graphene heating slurry is characterized in that:
comprises the following components in parts by weight:
2. the medium-high temperature graphene exothermic slurry according to claim 1, wherein:
the composition also comprises the following components in parts by weight:
and 0.5 to 3.5 parts of sodium carboxymethyl cellulose.
3. The medium-high temperature graphene exothermic slurry according to claim 2, wherein:
comprises the following components in parts by weight:
4. the medium-high temperature graphene exothermic slurry according to claim 2, wherein: comprises the following components in parts by weight:
5. a preparation method of the medium-high temperature graphene exothermic slurry according to any one of claims 2 to 4, wherein the preparation method comprises the following steps:
the method comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, thermoplastic polyurethane elastomer rubber, natural mica, N-methylpyrrolidone and sodium carboxymethylcellulose in parts by weight, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
adding the graphite powder in parts by weight into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and allowing the carbon nano tubes to enter the graphite interlayer gaps along with liquid in the system along with the gradual increase of the graphite interlayer gaps until the graphite is stripped into graphene in a liquid system;
and step three, removing part of the N-methyl pyrrolidone to obtain the graphene carbon nanotube heating slurry with proper viscosity.
6. The method of claim 5, wherein: the first step to the third step are carried out under vacuum condition.
7. The method of claim 5, wherein: and the viscosity of the graphene carbon nanotube heating slurry obtained in the third step is 60-70 Pa s.
8. The method for forming a film of the medium-high temperature graphene thermal paste according to any one of claims 1 to 4, comprising:
the method comprises the following steps:
step one, coating medium-high temperature graphene heating slurry on the surface of a base material;
and step two, drying in vacuum to form the film after film forming.
9. The film forming method according to claim 8, wherein:
the vacuum drying conditions in the second step are as follows:
the temperature is 120 ℃ to 150 ℃;
for a period of 3 to 5 hours.
10. The film forming method according to claim 8, wherein:
the thermal conductivity of the obtained film is 2600W/(mK) to 4200W/(mK).
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| CN202110042739.9A CN113150665A (en) | 2021-01-13 | 2021-01-13 | Medium-high temperature graphene heating slurry and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479633A (en) * | 2022-01-18 | 2022-05-13 | 东莞市鹏威能源科技有限公司 | Heating coating, graphene far infrared heating film and application thereof |
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| CN103732847A (en) * | 2011-08-05 | 2014-04-16 | 贝克休斯公司 | Compositions, methods of coating wellbore tools with such compositions, and wellbore tools coated with such compositions |
| CN105463854A (en) * | 2015-11-16 | 2016-04-06 | 江苏东邦科技有限公司 | Electromagnetic shielding cloth and preparation method thereof |
| CN108517123A (en) * | 2018-04-17 | 2018-09-11 | 青岛泰歌新材料科技有限公司 | A kind of modified composite material and preparation method using carbon nanotube and graphene |
| WO2018217682A1 (en) * | 2017-05-23 | 2018-11-29 | Alpha Assembly Solutions Inc. | Graphene enhanced and engineered materials for membrane touch switch and other flexible electronic structures |
-
2021
- 2021-01-13 CN CN202110042739.9A patent/CN113150665A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103732847A (en) * | 2011-08-05 | 2014-04-16 | 贝克休斯公司 | Compositions, methods of coating wellbore tools with such compositions, and wellbore tools coated with such compositions |
| CN105463854A (en) * | 2015-11-16 | 2016-04-06 | 江苏东邦科技有限公司 | Electromagnetic shielding cloth and preparation method thereof |
| WO2018217682A1 (en) * | 2017-05-23 | 2018-11-29 | Alpha Assembly Solutions Inc. | Graphene enhanced and engineered materials for membrane touch switch and other flexible electronic structures |
| CN108517123A (en) * | 2018-04-17 | 2018-09-11 | 青岛泰歌新材料科技有限公司 | A kind of modified composite material and preparation method using carbon nanotube and graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479633A (en) * | 2022-01-18 | 2022-05-13 | 东莞市鹏威能源科技有限公司 | Heating coating, graphene far infrared heating film and application thereof |
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Application publication date: 20210723 |