CN113148991A - Preparation process of graphene heat-conducting film - Google Patents
Preparation process of graphene heat-conducting film Download PDFInfo
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- CN113148991A CN113148991A CN202110608962.5A CN202110608962A CN113148991A CN 113148991 A CN113148991 A CN 113148991A CN 202110608962 A CN202110608962 A CN 202110608962A CN 113148991 A CN113148991 A CN 113148991A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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Abstract
The invention discloses a preparation process of a graphene heat-conducting membrane, which comprises the following steps of a, preparing 5-50% concentration graphene slurry, and regulating the solid content of the graphene slurry to 5-50% and the viscosity to 10000-1000000 mpa.s; b. directly extruding and molding the graphene slurry into a sheet material by adopting an extrusion molding technology; c. and sintering, namely drying the sheet material at a low temperature, then performing carbonization and graphitization treatment, and finally rolling to form the graphene heat-conducting film. The preparation process of the graphene heat-conducting film provided by the invention has simple steps, can effectively reduce the cost, can effectively improve the qualification rate of products compared with the existing complex process, can save electricity and reduce energy consumption, and in addition, the equipment related to the preparation process is reduced in scale, the occupied area is reduced, and the difficulty in building plant sites is reduced.
Description
Technical Field
The invention relates to the technical field of high-molecular heat-conducting films, in particular to a preparation process of a graphene heat-conducting film.
Background
Along with the increasing intellectualization and integration degree of electronic equipment, the electronic response speed is faster and faster, so that the heat productivity of the electronic equipment is increased rapidly, and therefore a heat dissipation component with high heat conductivity and high heat flux is required for heat dissipation. At present, electronic equipment radiates heat by taking a new-generation graphene heat-conducting film as a heat-radiating part, and the graphene heat-conducting film has higher heat conductivity than natural graphite paper and has higher thickness and higher heat flux than an artificial graphite film, so that the graphene heat-conducting film becomes a favorite in the field of high-heat-conductivity market products.
The existing preparation method of the graphene heat-conducting film is to coat and dry graphene slurry into a graphite film, and then to form a graphite film sheet with high heat-conducting performance through carbonization, graphitization and flat pressing. Due to the fact that the specific surface area of graphene is high, if the concentration of graphene in the graphene slurry is too high, the viscosity of the slurry is too high and the slurry does not have fluidity, and effective coating cannot be performed, so that the mainstream preparation method of the graphene heat conduction film has the following defects:
(1) the slurry solids content was too low: at present, the solid content of graphene slurry is lower than 5%, and the slurry contains a large amount of water and needs to be dried, so that the coating and drying efficiency is low, namely the production cost of a coating working section is high
(2) The process is too many: the graphene film coated and dried at present can be prepared into the graphene film with high heat conductivity only by three procedures of pretreatment in a high-temperature oven, carbonization and graphitization
In view of the above disadvantages, it is urgently needed to invent a novel graphene thermal conductive film preparation method to solve the defects of the prior art.
Disclosure of Invention
The invention aims to provide a preparation process of a graphene heat-conducting film, which is simple in process forming and high in yield.
In order to achieve the above object, the present invention provides a preparation process of a graphene thermal conductive film, comprising the following steps,
a. preparing 5-50% concentration graphene slurry, and regulating the solid content of the graphene slurry to 5-50%, and regulating the viscosity to 10000-1000000 mpa.s;
b. directly extruding and molding the graphene slurry into a sheet material by adopting an extrusion molding technology;
c. and sintering, namely drying the sheet material at a low temperature, then performing carbonization and graphitization treatment, and finally rolling to form the graphene heat-conducting film.
As a further improvement of the present invention, in the step b, a silicone rubber extruder is used for extrusion molding.
As a further improvement of the invention, the extrusion width of the sheet material is 100-3000mm, and the thickness is 0.1-100 mm.
As a further improvement of the invention, in the step c, the low-temperature drying temperature is controlled to be 50-100 ℃, and the drying time is 0.5-5 hours.
As a further improvement of the invention, in the step c, the temperature of the carbonization treatment is controlled at 800-1200 ℃, and the carbonization time is 10-50 hours.
As a further improvement of the invention, in the step c, the temperature of the graphitization treatment is controlled to 2700-.
As a further improvement of the invention, in the step c, a multifunctional sintering furnace is adopted to carry out drying, carbonization and graphitization processes on the sheet material.
The invention has the beneficial effects that:
the preparation process of the graphene heat-conducting film provided by the invention has simple steps, can effectively reduce the cost, can effectively improve the qualification rate of products compared with the existing complex process, can save electricity and reduce energy consumption, and in addition, the equipment related to the preparation process is reduced in scale, the occupied area is reduced, and the difficulty in building plant sites is reduced.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The embodiment provides a preparation process of a graphene heat-conducting film, which comprises the following steps,
a. preparing 5-50% concentration graphene slurry, and regulating the solid content of the graphene slurry to 5-50%, and regulating the viscosity to 10000-1000000 mpa.s;
b. directly extruding and molding the graphene slurry into a sheet material by adopting an extrusion molding technology;
c. and sintering, namely drying the sheet material at a low temperature, then performing carbonization and graphitization treatment, and finally rolling to form the graphene heat-conducting film.
In the step b, a silicon rubber extruder is adopted for extrusion molding, the extrusion width of the sheet material is 100-3000mm, and the thickness of the sheet material is 0.1-100 mm.
In the step c, the low-temperature drying temperature is controlled to be 50-100 ℃, the drying time is 0.5-5 hours, the carbonization temperature is controlled to be 800-.
The invention is further illustrated by the following specific examples.
Example 1
a. Preparing 5% graphene slurry, and adjusting the solid content of the graphene slurry to 5% and the viscosity to 50000 mpa.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 100mm and the thickness of 0.1 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 50 ℃, the drying time at 5 hours, the temperature of carbonization at 800 ℃, the carbonization time at 10 hours, the graphitization temperature at 2700 ℃, the graphitization time at 50 hours, and finally rolling to form the graphene heat-conducting film.
Example 2
a. Preparing graphene slurry with the concentration of 50%, and preparing the solid content of the graphene slurry to 50% and the viscosity to 1000000 map.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 3000mm and the thickness of 100 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 100 ℃, the drying time at 0.5 hour, the temperature of carbonization at 1200 ℃, the carbonization time at 50 hours, the graphitization temperature at 3200 ℃, the graphitization time at 10 hours, and finally rolling to form the graphene heat-conducting film.
Example 3
a. Preparing graphene slurry with the concentration of 24%, and preparing the solid content of the graphene slurry to 24% and the viscosity to 300000 map.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 800mm and the thickness of 20 mm;
c. the method comprises the steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 70 ℃ for 3 hours, controlling the temperature of carbonization at 1100 ℃ for 30 hours, controlling the temperature of graphitization at 2900 ℃ for 22 hours, and finally rolling to form the graphene heat-conducting film.
Example 4
a. Preparing 33% graphene slurry, and adjusting the solid content of the graphene slurry to 33% and the viscosity to 450000 mpa.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 1200mm and the thickness of 70 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 80 ℃, the drying time at 3.5 hours, the temperature of carbonization at 960 ℃, the carbonization time at 27 hours, the graphitization temperature at 3050 ℃, the graphitization time at 31 hours, and finally rolling to form the graphene heat-conducting film.
Example 5
a. Preparing 19% graphene slurry, and adjusting the solid content of the graphene slurry to 19% and the viscosity to 230000 mpa.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 2100mm and the thickness of 80 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by adopting a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 95 ℃ for 2 hours, controlling the temperature of carbonization at 1070 ℃ for 36 hours, controlling the temperature of graphitization at 3100 ℃ for 42 hours, and finally rolling to form the graphene heat-conducting film.
Example 6
a. Preparing graphene slurry with the concentration of 37%, and adjusting the solid content of the graphene slurry to 37% and the viscosity to 510000 map.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 1900mm and the thickness of 70 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 55 ℃, the drying time at 4 hours, the temperature of carbonization at 1220 ℃, the carbonization time at 39 hours, the graphitization temperature at 2950 ℃, the graphitization time at 40 hours, and finally rolling to form the graphene heat-conducting film.
Example 7
a. Preparing 41% graphene slurry, and adjusting the solid content of the graphene slurry to 41% and the viscosity to 670000 mpa.s;
b. carrying out extrusion molding by using a silicone rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 2500mm and the thickness of 60 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the low-temperature drying temperature to be 67 ℃ and the drying time to be 5 hours, controlling the carbonization temperature to be 1130 ℃ and the carbonization time to be 32 hours, controlling the graphitization temperature to be 3040 ℃ and the graphitization time to be 50 hours, and finally rolling to form the graphene heat-conducting film.
Example 8
a. Preparing graphene slurry with the concentration of 35%, and preparing the solid content of the graphene slurry to 35% and the viscosity to 430000 map.s;
b. carrying out extrusion molding by using a silicon rubber extruder, and directly extruding and molding the graphene slurry into a sheet material with the width of 2600mm and the thickness of 10 mm;
c. the method comprises the following steps of carrying out drying, carbonization and graphitization on a sheet material by using a multifunctional sintering furnace, controlling the temperature of low-temperature drying at 75 ℃, the drying time at 4 hours, the carbonization temperature at 980 ℃, the carbonization time at 36 hours, the graphitization temperature at 2890 ℃, the graphitization time at 38 hours, and finally rolling to form the graphene heat-conducting film.
The graphene thermal conductive films prepared in the above embodiments are inspected for yield, and in addition, the products prepared in the prior art in the background art are inspected for yield, and the inspection results
Shown in table 1.
| Group of | Product percent of pass |
| Example 1 | 81％ |
| Example 2 | 88％ |
| Example 3 | 95％ |
| Example 4 | 85％ |
| Example 5 | 87％ |
| Example 6 | 83％ |
| Example 7 | 81％ |
| Example 8 | 85％ |
| Existing products | 70％ |
TABLE 1
The data in table 1 show that the yield of the graphene heat-conducting film prepared by the improved preparation process is obviously improved by at least 10%, and the yield is improved by more than 20% under the best condition.
In addition, the invention is provided with:
(1) the extrusion molding process reduces the cost: the method adopts the extrusion technology of high-viscosity materials (equipment and process similar to silicone rubber molding) to extrude and mold the slurry with high solid content, compared with the coating method in the prior art, the method can process the slurry with higher solid content and higher viscosity (the highest content can reach 50 percent), is favorable for reducing the moisture content of the slurry, further reduces the drying cost, and can solve the problem of the requirement of the original coating machine on a factory building with high length;
(2) sintering in a one-step method: compared with three traditional procedures of oven treatment, carbonization and graphitization, the one-step process in the invention can greatly reduce the complex process of the multiple procedures (due to poor toughness of the graphene film, the product is easy to damage in the turnover process caused by complex process at present, so that the yield can not be further improved all the time), improve the qualification rate of the product, frequently switch the temperature rise and fall among the original multiple procedures, consume time and consume power, the one-step sintering in the invention only needs one temperature rise and fall, the cost is greatly reduced, the original multiple procedures need multiple types of equipment, the occupied area of the equipment is large, the power consumption is large, the one-step sintering only needs one type of equipment, and the strict requirements of the original process on the area of a factory building and the power supply are greatly reduced.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (7)
1. A preparation process of a graphene heat-conducting film is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
a. preparing 5-50% concentration graphene slurry, and regulating the solid content of the graphene slurry to 5-50%, and regulating the viscosity to 10000-1000000 mpa.s;
b. directly extruding and molding the graphene slurry into a sheet material by adopting an extrusion molding technology;
c. and sintering, namely drying the sheet material at a low temperature, then performing carbonization and graphitization treatment, and finally rolling to form the graphene heat-conducting film.
2. The process for producing a heat conductive film according to claim 1, wherein: and in the step b, a silicon rubber extruder is adopted for extrusion molding.
3. The process for producing a heat conductive film according to claim 2, wherein: the extrusion width of the sheet material is 100-3000mm, and the thickness is 0.1-100 mm.
4. The process for producing a heat conductive film according to claim 1, wherein: in the step c, the low-temperature drying temperature is controlled to be 50-100 ℃, and the drying time is 0.5-5 hours.
5. The process for producing a heat conductive film according to claim 4, wherein: in the step c, the temperature of the carbonization treatment is controlled at 800-1200 ℃, and the carbonization time is 10-50 hours.
6. The process for producing a heat conductive film according to claim 4, wherein: in the step c, the temperature of the graphitization treatment is controlled to 2700-.
7. The process for producing a heat conductive film according to claim 1, wherein: and in the step c, a multifunctional sintering furnace is adopted to carry out drying, carbonization and graphitization process treatment on the sheet material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116693291A (en) * | 2023-05-24 | 2023-09-05 | 杭州嘉悦智能设备有限公司 | Improved production process and sintering equipment for graphene heat conducting film |
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