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CN113880595B - Graphite film with high heat conductivity in vertical direction and preparation method thereof - Google Patents

Graphite film with high heat conductivity in vertical direction and preparation method thereof Download PDF

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CN113880595B
CN113880595B CN202111358301.8A CN202111358301A CN113880595B CN 113880595 B CN113880595 B CN 113880595B CN 202111358301 A CN202111358301 A CN 202111358301A CN 113880595 B CN113880595 B CN 113880595B
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graphite film
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CN113880595A (en
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吴伯丽
李金明
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Jiangxi Hongmei New Energy Technology Co ltd
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/74Ceramic products containing macroscopic reinforcing agents containing shaped metallic materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/52Shaped 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
    • C04B35/522Graphite
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62218Forming 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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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/9607Thermal properties, e.g. thermal expansion coefficient

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  • Ceramic Engineering (AREA)
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Abstract

The invention discloses a graphite film with high heat conductivity in the vertical direction and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Providing a release film, coating a sizing material on the surface of the release film to form a glue layer, wherein the sizing material comprises an adhesive and metal particles, (2) performing magnetic orientation to ensure that the magnetic pole direction of the metal particles is arranged along the thickness direction of the glue layer, and then drying and volatilizing a solvent in the adhesive to prepare a first product; (3) Providing a PI film, heating, carbonizing, graphitizing, performing first calendering treatment to obtain a semi-finished product, (4) taking the two first products prepared in the step (2), placing the semi-finished product between glue layers of the two first products, performing second calendering treatment, and applying pressure to the two first products to enable the first products on two sides of the semi-finished product to move towards the direction of the semi-finished product, so that metal particles in the two first products are embedded into the semi-finished product, and thus obtaining the graphite film. The graphite film has high thermal conductivity in the vertical direction, and does not affect the thermal conductivity in the horizontal direction.

Description

Graphite film with high heat conductivity in vertical direction and preparation method thereof
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a graphite film with high heat conduction in the vertical direction and a preparation method thereof.
Background
At present, in the conventional method for manufacturing a graphite heat sink, a PI (Polyimide) film (Polyimide film) is first fed into a carbonization furnace, and the PI film is heated and carbonized at a heating temperature of 1100 ℃ to 1300 ℃ to form a PI carbonized piece after the PI film is carbonized; then, cooling the PI carbonized sheet to room temperature, then sending the PI carbonized sheet into a graphitization furnace, heating and graphitizing the PI carbonized sheet at the heating temperature of 2800-3000 ℃ to graphitize the PI carbonized sheet to form a PI graphite radiating sheet; and then cooling the PI graphite radiating fin to room temperature, and rolling the PI graphite radiating fin to the thickness by using a rolling device, so that the PI graphite radiating fin is rolled to form a graphite radiating fin finished product with the thickness of 15-200 mu m, wherein the finished product is also called an artificial graphite film.
The artificial graphite fin manufactured by the method for manufacturing the graphite fin has thermal conductivity in the horizontal direction (namely, the X-axis direction and the Y-axis direction) as high as 1600W/(m.k), but the thermal conductivity in the thickness direction (namely, the Z-axis direction) is lower than 5W/(m.k), and is seriously lower.
With the development of communication and new energy industries, especially the increasing prevalence of 5G technologies, autopilot and electric vehicles, as the power of electronic products is continuously increased, the thinner the products are, the lighter, thinner, shorter, smaller and more complex electronic instruments and devices are developed. Under high-frequency working frequency, the heat generated by the electronic element is rapidly accumulated and increased, and the technical problem that the heat cannot be timely dissipated is increasingly shown. In this case, it is imperative to improve the thermal conductivity of the artificial graphite fin in the thickness direction (i.e., Z-axis direction).
Therefore, it is necessary to provide a graphite film with high thermal conductivity in the vertical direction to solve the above-mentioned deficiencies of the prior art.
Disclosure of Invention
To overcome the disadvantages of the prior art, it is an object of the present invention to provide a graphite film that can improve the thermal conductivity in the vertical direction (i.e., Z-axis direction) without reducing or affecting the thermal conductivity in the horizontal direction (i.e., X-axis and Y-axis directions).
In order to achieve the purpose, the invention discloses a preparation method of a graphite film with high heat conductivity in the vertical direction, which comprises the following steps:
(1) Providing a release film, then coating a sizing material on the surface of the release film to form a glue layer, wherein the sizing material comprises an adhesive and metal particles,
(2) Magnetic orientation is carried out, so that the magnetic pole direction of the metal particles is arranged along the thickness direction of the adhesive layer, and then the solvent in the adhesive is dried and volatilized, so that a first product is prepared;
(3) Providing a PI film, heating, carbonizing, graphitizing, performing first rolling treatment to obtain a semi-finished product,
(4) And (3) taking the two first products prepared in the step (2), placing the semi-finished product between the glue layers of the two first products, carrying out secondary calendering treatment, and applying pressure to the two first products to enable the first products on two sides of the semi-finished product to move towards the direction of the semi-finished product, so that the metal particles in the two first products are embedded into the semi-finished product, and thus the graphite film is prepared.
Compared with the prior art, the preparation method of the graphite film with high heat conductivity in the vertical direction has the advantages that the metal particles are added into the adhesive layer, the magnetic pole direction of the metal particles is arranged along the thickness direction of the adhesive layer through magnetic orientation, the adhesive layer and the graphite film are matched and rolled, the metal particles in the adhesive layer are enabled to be embedded into the graphite film, the upper side and the lower side of the graphite film are embedded by the metal particles, even the upper metal particles and the lower metal particles are abutted, so that heat can be rapidly conducted out through the vertical direction (namely the Z-axis direction), the graphite film has good heat transfer performance in the vertical direction (namely the Z-axis direction), meanwhile, the heat conductivity in the horizontal direction (namely the X-axis direction and the Y-axis direction) cannot be reduced, the preparation method is simple, and the cost is low. In addition, the adhesive layer can prevent the graphite film from falling off powder and can provide adhesion with an attached object.
Correspondingly, the invention also provides a graphite film with high heat conductivity in the vertical direction, and the graphite film is prepared by the preparation method.
Drawings
Fig. 1 is a schematic structural diagram of a graphite film with high thermal conductivity in the vertical direction according to the present invention.
FIG. 2 is a schematic diagram showing the state of magnetic alignment in the method for producing a graphite film according to the present invention.
Fig. 3 is a schematic view showing the state of the second rolling treatment in the method for producing a graphite film of the present invention.
Description of the symbols:
the production method comprises the following steps of a graphite film 10, a magnetic device 20, an adhesive layer 30, a rolling device 40, a release film 50, a first product 60, metal particles 70 and a semi-finished product 80.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the present invention in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.
Referring to fig. 1, the graphite film with high thermal conductivity in the vertical direction provided by the present invention includes a graphite film 10, adhesive layers 30 located at two sides of the graphite film 10, and a release film 50 located at the outer sides of the adhesive layers 30, wherein metal particles 70 are embedded between the graphite film 10 and the adhesive layers 30. Specifically, a part of the metal particles 70 (may be referred to as upper metal particles 70) in the glue layer 30 positioned on the upper side of the graphite film 10 is positioned in the glue layer 30, and another part of the metal particles 70 is positioned in the graphite film 10; also, a part of the metal particles 70 (which may be referred to as lower metal particles 70) in the paste layer 30 located on the lower side of the graphite film 10 is located in the paste layer 30, and another part of the metal particles 70 is located in the graphite film 10. It will be appreciated that the upper metal particles 70 and the lower metal particles 70 are embedded in the graphite film 10, and a part of the upper metal particles 70 and a part of the lower metal particles 70 are also in abutment, so that heat can be rapidly conducted away in the vertical direction (i.e., the Z-axis direction).
For the graphite film with high heat conductivity in the vertical direction, the invention provides a preparation method thereof, which comprises the following steps:
(1) Providing a release film 50, then coating a sizing material on the surface of the release film 50 to form a glue layer 30, wherein the sizing material comprises an adhesive and metal particles 70,
(2) Magnetically orienting so that the magnetic pole direction of the metal particles 70 is set along the thickness direction of the glue layer 30, and then drying to volatilize the solvent in the adhesive to obtain a first product 60;
(3) Providing a PI film, heating, carbonizing, graphitizing, performing first rolling treatment to obtain a semi-finished product 80,
(4) And (3) taking the two first products 60 prepared in the step (2), placing the semi-finished product 80 between the glue layers 30 of the two first products 60, performing second rolling treatment, and pressing the two first products 60 to enable the first products 60 on the two sides of the semi-finished product 80 to move towards the semi-finished product 80, so that the metal particles 70 in the two first products 60 are embedded into the semi-finished product 80, and the semi-finished product 80 becomes thinner after the second rolling to form the graphite film 10, so that the graphite film with high heat conductivity in the vertical direction is prepared.
Specifically, as for steps (1) - (2), referring to fig. 2, a glue layer 30 is formed by coating a glue material on the surface of a release film 50, the glue material contains a binder and metal particles 70, then the metal particles 70 are magnetically oriented by a magnetic device 20, so that the magnetic pole direction of the metal particles 70 is arranged along the thickness direction of the glue layer 30, and then the first product 60 is prepared by heating, drying and volatilizing the solvent in the binder.
Preferably, the release film 50 is a PET film, but is not limited thereto. The thickness of the release film 50 is 50-100 μm, for example, the thickness of the release film 50 is 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm.
Preferably, the adhesive is selected from pressure sensitive adhesive resins with a solid content of 10-50%, such as acrylic pressure sensitive adhesive resins, but not limited thereto.
It will be appreciated that the metal particles 70 are magnetically attractable metal particles 70, that is to say that magnetic orientation of the metal particles 70 can be achieved by the magnetic means 20. Preferably, the metal particles 70 are selected from at least one of iron powder, cobalt powder, nickel powder, and iron-, cobalt-, and nickel-plated copper powder. Note that the term "copper powder plated with iron, cobalt, or nickel" means that an iron layer, a cobalt layer, or a nickel layer is plated on the surface of the copper powder. For example, the metal particles 70 are selected from any one of iron powder particles, cobalt powder particles, and nickel powder particles; for example, the metal particles 70 may be selected from any of iron-plated copper powder, cobalt-plated copper powder, and nickel-plated copper powder. The shape of the metal particles 70 may be at least one selected from the group consisting of diamond, stripe, flake, and needle, but not limited thereto. Preferably, the particle size of the metal particles 70 is 5 to 100 μm, such as 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, of the metal particles 70. Preferably, the metal particles 70 are present in the size in a proportion of 3 to 10%.
The semifinished product 80 is obtained by carbonization, graphitization and a first calendering in step (3), which are well known to those skilled in the art and will not be described in detail here. Preferably, the thickness of the semi-finished product 80 is 5-150 μm, for example, the thickness of the semi-finished product 80 is 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 80 μm, 100 μm, 120 μm, 140 μm, 150 μm. Wherein the thickness of the semi-finished product 80 can be controlled according to the pressure of the calendering process.
As for the step (4), referring to fig. 3, two first products 60 are respectively located at two sides of the semi-finished product 80, and one side of the adhesive layer 30 is close to the semi-finished product 80, the two first products 60 and the semi-finished product 80 are subjected to a second rolling process by the rolling device 40, so that the first products 60 on the upper side and the lower side of the semi-finished product 80 both move towards the direction of the semi-finished product 80 and are attached to the semi-finished product 80, and then rolling is performed, so that the metal particles 70 in the first product 60 on the upper side are downward embedded into the semi-finished product 80, and the metal particles 70 in the first product 60 on the lower side are upward embedded into the semi-finished product 80, so that the semi-finished product 80 is embedded with a plurality of metal particles 70 in the thickness direction, and even the upper and lower metal particles 70 are abutted, and the semi-finished product 80 forms the graphite film 10 (it is required to point that the semi-finished product 80 becomes thinner after the second rolling to form the graphite film 10), so that heat can be quickly conducted through the graphite film 10 in the vertical direction (i.e., the Z-axis direction), so that the graphite film 10 has good heat dissipation performance in the vertical direction (i.e., the Z-axis direction, and at the same time, the X-axis direction, the horizontal direction, and the heat conductivity in the Y-axis direction is not reduced, and the preparation cost is low.
The graphite film with high thermal conductivity in the vertical direction of the present invention will be illustrated by several specific examples, but the scope of the present invention is not limited thereto.
Example 1
(1) Providing a PET release film, and then coating a sizing material on the surface of the release film to form a glue layer, wherein the sizing material comprises acrylic pressure-sensitive adhesive resin with the solid content of 20% and nickel powder accounting for 5% of the sizing material content, and the particle size of the nickel powder is 10-15 microns;
(2) Magnetic orientation, namely arranging the magnetic pole direction of the nickel powder along the thickness direction of the adhesive layer by means of a magnetic orientation device, and then heating, drying and volatilizing a solvent in the adhesive to obtain a first product;
(3) Feeding the PI film with the thickness of 50 micrometers into a carbonization furnace, heating to 1000 ℃ for heating carbonization, cooling to obtain a carbonized film, feeding the carbonized film into a graphitization furnace, heating to 2500 ℃ for graphitization, cooling to obtain a graphitized film, and performing primary calendering treatment on the graphitized film to obtain a semi-finished product.
(4) And (3) taking the two first products prepared in the step (2), placing the semi-finished product between the glue layers of the two first products, performing secondary calendering treatment by using a calendering device to enable the first products on the two sides of the semi-finished product to move towards the direction of the semi-finished product and be attached to the semi-finished product, and then calendering to enable the nickel powder particles in the first product on the upper side to be downwards embedded into the semi-finished product and the nickel powder particles in the first product on the lower side to be upwards embedded into the semi-finished product, so that a plurality of metal particles are embedded into the semi-finished product in the thickness direction of the semi-finished product, and the situation that the upper metal particles and the lower metal particles are abutted occurs, thereby preparing the graphite film with high heat conductivity in the vertical direction.
Example 2
Example 2 is the same as example 1 except that: in example 2, the metal particles are selected from iron powder, and the rest is the same as example 1, and will not be described in detail.
Example 3
Example 3 is the same as example 1 except that: in example 3, the metal particles were selected from nickel-plated copper powder, and the rest was the same as in example 1, and will not be described in detail.
Comparative example 1
Comparative example 1 as a control, comparative example 1 was the same as example 1 except that no metal particles were added and no magnetic alignment was performed, and detailed description thereof is omitted.
And (4) performance testing:
the graphite films obtained in examples 1 to 3 of the present invention and comparative example 1 were subjected to a thermal conductivity test, and the results are shown in table 1.
TABLE 1 thermal conductivity test results
Figure BDA0003356955860000071
As can be seen from the data in table 1, the graphite film prepared by the method of the present invention can effectively improve the thermal conductivity in the vertical direction (i.e., Z-axis direction) without decreasing the thermal conductivity in the horizontal direction (i.e., X-axis and Y-axis directions) as compared to comparative example 1. It is also found that the use of nickel-plated copper powder as the metal particles is more effective in improving the thermal conductivity in the vertical direction (i.e., Z-axis direction) than iron powder or nickel powder.
The above disclosure is only for the preferred embodiment of the present invention, and it should be understood that the present invention is not limited thereto, and the invention is not limited to the above disclosure.

Claims (6)

1. A preparation method of a graphite film with high heat conductivity in the vertical direction is characterized by comprising the following steps:
(1) Providing a release film, then coating a sizing material on the surface of the release film to form a glue layer, wherein the sizing material comprises an adhesive and metal particles,
(2) Magnetic orientation is carried out, so that the magnetic pole direction of the metal particles is arranged along the thickness direction of the adhesive layer, and then the solvent in the adhesive is dried and volatilized, so that a first product is prepared;
(3) Providing a PI film, heating, carbonizing, graphitizing, performing first rolling treatment to obtain a semi-finished product,
(4) Taking the two first products prepared in the step (2), placing the semi-finished product between the glue layers of the two first products, carrying out secondary rolling treatment, applying pressure to the two first products to enable the first products on the upper side and the lower side of the semi-finished product to move towards the semi-finished product, enabling metal particles in the first products on the upper side to be downwards embedded into the semi-finished product, enabling metal particles in the first products on the lower side to be upwards embedded into the semi-finished product, enabling the semi-finished product to be embedded into a plurality of metal particles in the thickness direction, enabling the upper metal particles to be abutted against the lower metal particles, and preparing a graphite film,
the metal particles are selected from at least one of iron powder, cobalt powder, nickel powder, iron-plated copper powder, cobalt-plated copper powder and nickel-plated copper powder, and the shape of the metal particles is selected from at least one of diamond, strip, sheet and needle.
2. The method of preparing a highly thermally conductive, vertically oriented graphite film according to claim 1 wherein said binder is selected from the group consisting of pressure sensitive adhesive resins having a solids content of 10-50%.
3. The method of preparing a vertically highly thermally conductive graphite film according to claim 1, wherein the metal particles have a particle size of 5 to 100 μm.
4. The method of preparing a highly thermally conductive vertically graphitic film according to claim 1, wherein said semifinished product has a thickness of 5 to 150 μm.
5. The method of preparing a highly thermally conductive, vertically oriented graphite film according to claim 1 wherein the metal particles are present in the size in a proportion of 3 to 10%.
6. A graphite film having a high thermal conductivity in the vertical direction, which is produced by the production method according to any one of claims 1 to 5.
CN202111358301.8A 2021-11-16 2021-11-16 Graphite film with high heat conductivity in vertical direction and preparation method thereof Active CN113880595B (en)

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JP2000281995A (en) * 1999-03-30 2000-10-10 Polymatech Co Ltd Thermally conductive adhesive film and semiconductor device
JP2006306068A (en) * 2005-03-29 2006-11-09 Kaneka Corp Heat conductive sheet
CN106398570A (en) * 2014-01-26 2017-02-15 斯迪克新型材料(江苏)有限公司 High-compactness graphite soaking adhesive tape
CN105235307B (en) * 2015-09-01 2016-04-27 山东安诺克新材料有限公司 A kind of heat conducting film graphite composite material
CN112406213A (en) * 2020-11-18 2021-02-26 信骅(上海)器材有限公司 Continuous production method of highly oriented and high-thickness radiating fin and radiating fin
CN112770592A (en) * 2020-11-18 2021-05-07 信骅(上海)器材有限公司 Method for improving heat transfer performance of radiating fin in vertical direction and radiating fin
CN113587061B (en) * 2021-07-12 2023-09-08 泰兴挚富显示技术有限公司 High-heat-conductivity composite graphite radiating fin and preparation method thereof

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