CN110965039A - Alloy material with graphene heat dissipation film for electronic equipment and preparation method thereof - Google Patents
Alloy material with graphene heat dissipation film for electronic equipment and preparation method thereof Download PDFInfo
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- CN110965039A CN110965039A CN201911253765.5A CN201911253765A CN110965039A CN 110965039 A CN110965039 A CN 110965039A CN 201911253765 A CN201911253765 A CN 201911253765A CN 110965039 A CN110965039 A CN 110965039A
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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Abstract
The invention discloses an alloy material with a graphene heat dissipation film for electronic equipment and a preparation method thereof, wherein the alloy material takes an alloy as a substrate and is coated with a single layer or 2-1000 layers of graphene heat dissipation films; during preparation: cleaning an alloy substrate, cleaning with an acidic liquid to remove chemical impurities, and cleaning and blow-drying; and (3) placing the treated alloy in a chemical vapor deposition reaction chamber and sealing the reaction chamber, reducing the pressure of the reaction chamber to be below 10Pa, introducing hydrogen and protective gas, starting heating and raising the temperature, preserving the temperature when the temperature reaches 1000-1200 ℃, introducing carbon-containing gas and protective gas, continuing preserving the temperature, cracking the carbon-containing gas, depositing graphene on the surface of the alloy, and then cooling to finish the preparation of the alloy material. According to the invention, the alloy is used as a substrate, and the graphene heat dissipation film is deposited on the surface of the alloy by a chemical vapor deposition method, so that the heat conductivity of the alloy can be improved, the heat dissipation and heat transfer characteristics of the alloy can be enhanced, and the heat dissipation material suitable for mass use in the field of electronic equipment can be prepared.
Description
Technical Field
The invention relates to a process technology of a composite material containing alloy, stainless steel and graphene for electronic equipment, in particular to an alloy material with a graphene heat dissipation film for electronic equipment and a preparation method thereof.
Background
With the coming of the intelligent era, the demand of people on the mobile phone is higher and higher, the hardware configuration of the mobile phone is also improved, the CPU is gradually increased to four cores and eight cores from a single core to a double core, and the size and the resolution of a screen are also continuously improved. The problem that mobile phones generate heat more and more seriously is brought along with the improvement of mobile phone hardware and performance, the performance and reliability of electronic products are directly influenced by heat generated in the operation of equipment, and the problems that the mobile phones are scalded, blocked, halted or even exploded and the like are caused if the heat is not timely dissipated. The problem of heat dissipation has been a pain point and difficulty of high concern in the consumer electronics industry.
The heat conduction material is mainly used for solving the problems of heat conduction and heat balance of the electronic equipment. The heat conducting material is mainly applied between system thermal interfaces, and the rough and uneven combined surface is filled, and the thermal interface material with the heat conductivity coefficient far higher than that of air is used for replacing air without heat transfer, so that the thermal resistance passing through the thermal interface is reduced, the heat dissipation efficiency of the semiconductor component is improved, and the heat conducting material is also called as a thermal interface material in the industry.
The heat dissipation technologies used in the current mobile phones mainly include graphite heat dissipation, metal back plate, frame heat dissipation, heat conducting gel heat dissipation, heat pipe heat dissipation, temperature equalization plate, and the like. The graphene has many excellent properties such as high strength, high thermal conductivity and hydrophobicity, and can be coated on the surface of the alloy by utilizing the high thermal conductivity of the graphene film, so that the thermal conductivity of the alloy material is obviously improved.
For example, a graphene film for a mobile phone screen is disclosed in a Chinese patent invention publication with publication number CN 208452480U, publication number of which is 2019, 2 and 1, but a preparation method of graphene is not disclosed; for example, chinese patent application publication No. CN 110182793 a, published as 2019, 8, 30 and 2019, discloses a method for preparing a high thermal conductivity graphene heat sink, in which an aqueous graphene oxide solution is coated on a carbonized polyimide film, and then graphitized to obtain the graphene heat sink, which has a complex process flow and increases thermal resistance after a binder is added.
Therefore, the graphene films for electronic devices disclosed in the prior art are not perfect in the manufacturing process.
Disclosure of Invention
The invention provides an alloy material with a graphene heat dissipation film for electronic equipment and a preparation method thereof.
The technical scheme of the invention is as follows:
the alloy material with the graphene heat dissipation film for the electronic equipment is characterized in that: the substrate of the alloy material is an alloy, and the surface of the substrate is coated with a graphene film; the alloy is a copper alloy, an iron alloy or an aluminum alloy; the graphene film is a single layer or 2-1000 layers. The alloy material is applied to heat transfer, heat dissipation or heat exchange parts of electronic equipment.
The shape of the substrate is designed into a tubular shape, a plate shape, a block shape or a powder shape according to application requirements.
The preparation method of the alloy material with the graphene heat dissipation film for the electronic equipment comprises the following specific steps:
cleaning the alloy serving as a base material by using cleaning liquid, chemically removing impurities from the cleaned alloy by using dilute hydrochloric acid, cleaning and drying;
placing the treated alloy in a chemical vapor deposition reaction chamber, sealing the reaction chamber, using a vacuum pump to enable the pressure of the deposition reaction chamber to be below 10Pa, introducing hydrogen and protective gas to start heating and heating, keeping the temperature for 1 min-120 min after the temperature reaches 1000-1200 ℃, introducing carbon-containing gas and protective gas, continuing to keep the temperature for 1 min-120 min, cracking the carbon-containing gas and depositing the carbon-containing gas to form graphene on the surface of the alloy, then cooling, wherein the cooling rate is 50-300 ℃/min, and completing the chemical vapor deposition of the graphene on the alloy, namely preparing the alloy material with the graphene heat dissipation film for the electronic equipment.
The concentration of the dilute hydrochloric acid is 0.1-2 mol/L, and the chemical impurity removal time is 1-30 min. Preferably, when the concentration of the dilute hydrochloric acid is 0.01-1.5 mol/L, the chemical impurity removal time is 5-30 min.
The cleaning liquid is one or a mixture of more of acetone, alcohol, isopropanol and water in any proportion. Further, the cleaning process for the alloy includes washing and ultrasonic vibration.
The gas used for blow-drying is inert gas which is nitrogen or argon or a mixed gas of nitrogen and argon.
The ratio of the hydrogen to the protective gas is 1: 0-1: 30, and the flow of the introduced hydrogen and the protective gas is as follows: 100 sccm to 1000 sccm.
The ratio of the carbon-containing gas to the protective gas is 1: 0-1: 50, and the flow rates of the carbon-containing gas and the protective gas are as follows: 0.5sccm to 50 sccm; the carbon-containing gas is one or a mixture of more of alkane, alkene, alkyne and arene with carbon atoms within the range of 1-10 in any proportion.
The protective gas is argon or nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
1. the graphene is coated on the surface of the alloy material, no additional adhesive is needed, no additional thermal resistance is added, and the heat transfer effect is better.
2. The graphene is directly deposited on the surface of the alloy in situ, the thickness of the deposited graphene film is in an atomic level, and compared with a coating of graphene, the graphene coating is thin in thickness, light in weight, low in price and capable of achieving full coverage on the surface.
3. The used alloy is industrial grade alloy, the shape can be various complex structures, the price is low, and the industrial large-scale popularization is easy.
4. The gas ratio can be controlled, the deposition temperature and the cooling rate can be controlled to adjust the number of deposited graphene layers, and the regulation and control of the surface performance can be realized.
Drawings
FIG. 1 is a graph showing surface Raman spectrum data of a composite material prepared according to the present invention.
Detailed Description
The present invention will be further described with reference to specific examples to better understand the contents of the present invention, but the present invention is not limited to the following examples.
Example 1
The method for preparing the graphene-coated alloy composite material by taking the BFE10-1-1 copper alloy sheet as a base material comprises the following specific steps:
(1) placing the copper alloy sheet in acetone, ultrasonically vibrating for 5 min to clean the surface of the copper alloy sheet and drying the copper alloy sheet by using nitrogen, and then placing the copper alloy sheet in deionized water, ultrasonically vibrating for 5 min to clean the surface of the copper alloy sheet and drying the copper alloy sheet by using nitrogen;
(2) chemical impurity removal is carried out for 10 min by using 2 mol/L dilute hydrochloric acid, and then deionized water is used for cleaning for 10 min and drying;
(3) placing the treated copper alloy in a chemical vapor deposition reaction chamber, sealing the reaction chamber, using a vacuum pump to enable the pressure of the deposition reaction chamber to be below 10Pa, introducing hydrogen and argon in a ratio of 1:30, enabling the gas flow to be 100 sccm, starting heating and raising the temperature, enabling the temperature raising rate to be 16.7 ℃/min, keeping the temperature for 1 min after the alloy material reaches 1000 ℃, introducing methane and argon in a ratio of 1:50, enabling the flow to be 0.5sccm, keeping the temperature for 1 min again, enabling the methane to be cracked on the surface of the alloy and deposited into graphene, and then cooling to complete the chemical vapor deposition of the graphene on the alloy.
According to the collective material and the prepared graphene-coated alloy composite material, as shown in Raman spectrum data in figure 1, the successful deposition of graphene can be obviously seen.
Example 2
This example used the same preparation procedure as in example 1, wherein the incubation temperature in step (3) was 1100 ℃.
Example 3
This example used the same preparation procedure as in example 1, wherein the holding temperature in step (3) was 1150 ℃.
Example 4
This example used the same preparation procedure as in example 1, wherein the incubation temperature in step (3) was 1200 ℃.
Example 5
This example used the same production procedure as in example 1, wherein the carbon-containing gas used in step (3) was an alkane having 10 carbon atoms.
Example 6
This example used the same production procedure as in example 1, wherein the carbon-containing gas used in step (3) used was an olefin of 10 carbon atoms.
Example 7
This example employed the same production procedure as in example 1, wherein the carbon-containing gas employed in step (3) was an alkyne of 10 carbon atoms.
Example 8
This example used the same preparation procedure as in example 1, wherein the ratio of carbon-containing gas/shielding gas used in step (3) was 1: 0.
Example 9
This example used the same preparation procedure as in example 1, wherein the ratio of hydrogen to shielding gas in step (3) was 1: 0.
Example 10
This example used the same production procedure as in example 1, wherein the flow rates of the carbon-containing gas and the shielding gas in step (3) were 50 sccm.
Example 11
This example used the same preparation procedure as in example 1, wherein the flow rates of hydrogen and the shielding gas in step (3) were 1000 sccm.
Example 12
This example used the same preparation procedure as in example 1, wherein the alloy used in step (1) was one of BFE30-1-1, B10, B19, BMN3-12, BMN40-1-5, H96, H90, H80, H70, H65, H62, HAL77-2, HAL77-2A, 304, 316, 5052-H112, 5083-H112, 6061-T651, 7050-T7451, 7075-T651.
Example 16
This example employed the same production procedure as in example 1, wherein the alloys used in step (1) were industrial-grade copper alloy, iron alloy and aluminum alloy materials.
Claims (11)
1. The alloy material with the graphene heat dissipation film for the electronic equipment is characterized in that: the substrate of the alloy material is an alloy, and the surface of the substrate is coated with a graphene film; the alloy is a copper alloy, an iron alloy or an aluminum alloy; the graphene film is a single layer or 2-1000 layers.
2. The alloy material with a graphene heat dissipation film for electronic devices according to claim 1, wherein: the alloy material is applied to heat transfer, heat dissipation or heat exchange parts of electronic equipment.
3. The alloy material with a graphene heat dissipation film for electronic devices according to claim 2, wherein: the shape of the substrate is designed into a tubular shape, a plate shape, a block shape or a powder shape according to application requirements.
4. A method for producing the alloy material according to claim 1, 2 or 3, characterized in that: firstly, cleaning an alloy serving as a substrate, then chemically removing impurities by using dilute hydrochloric acid, cleaning and drying; then, placing the processed alloy in a chemical vapor deposition reaction chamber, sealing the reaction chamber, reducing the pressure of the chemical vapor deposition reaction chamber to below 10Pa by using a vacuum pump, introducing hydrogen and protective gas, starting heating and raising the temperature, keeping the temperature for 1 min to 120min when the temperature reaches 1000 ℃ to 1200 ℃, introducing carbon-containing gas and protective gas, keeping the temperature for 1 min to 120min until the carbon-containing gas is cracked and graphene is deposited on the surface of the alloy, and then reducing the temperature at a cooling rate of 50 ℃/min to 300 ℃/min, thus completing the preparation of the alloy material with the graphene heat dissipation film for the electronic equipment.
5. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 1, wherein: the alloy is any one of BFE30-1-1, B10, B19, BMN3-12, BMN40-1-5, H96, H90, H80, H70, H65, H62, HAL77-2, HAL77-2A, 304, 316, 5052-H112, 5083-H112, 6061-T651, 7050-T7451 and 7075-T651.
6. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 4, wherein: the concentration of the dilute hydrochloric acid is 0.1-2 mol/L, and the chemical impurity removal time is 1-30 min.
7. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 6, wherein: when the concentration of the dilute hydrochloric acid is 0.01-1.5 mol/L, the chemical impurity removal time is 5-30 min.
8. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 4, wherein: when in cleaning, one or more of acetone, alcohol, isopropanol and water are mixed in any proportion, and the cleaning process comprises rinsing and ultrasonic vibration.
9. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 4, wherein: the gas used for blow-drying is inert gas which is nitrogen or argon or a mixed gas of nitrogen and argon.
10. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 4, wherein: the ratio of the hydrogen to the protective gas is 1: 0-1: 30, and the flow of the introduced hydrogen and the protective gas is as follows: 100 sccm-1000 sccm; the protective gas is argon or nitrogen.
11. The method for preparing the alloy material with the graphene heat dissipation film for the electronic device according to claim 4, wherein: the ratio of the carbon-containing gas to the protective gas is 1: 0-1: 50, and the flow rates of the carbon-containing gas and the protective gas are as follows: 0.5sccm to 50 sccm; the carbon-containing gas is one or a mixture of more of alkane, alkene, alkyne and arene with carbon atoms within the range of 1-10 in any proportion; the protective gas is argon or nitrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114214042A (en) * | 2021-12-15 | 2022-03-22 | 中国科学院金属研究所 | Application of graphene film as high-temperature-resistant thermal interface material or heat dissipation film material |
| CN114437673A (en) * | 2022-01-19 | 2022-05-06 | 东莞市鸿亿导热材料有限公司 | Production process of insulating high-thermal-conductivity graphene heat dissipation film |
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Cited By (3)
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| CN114214042A (en) * | 2021-12-15 | 2022-03-22 | 中国科学院金属研究所 | Application of graphene film as high-temperature-resistant thermal interface material or heat dissipation film material |
| CN114437673A (en) * | 2022-01-19 | 2022-05-06 | 东莞市鸿亿导热材料有限公司 | Production process of insulating high-thermal-conductivity graphene heat dissipation film |
| CN114437673B (en) * | 2022-01-19 | 2023-09-08 | 东莞市鸿亿导热材料有限公司 | Production process of insulating high-thermal-conductivity graphene heat dissipation film |
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