Graphene plate preparation method for graphene solid vapor chamber and graphene solid vapor chamber

Abstract

The application relates to a graphene plate preparation method for a graphene solid-state heat-distribution plate, which comprises the following steps: mixing and stirring graphene oxide and deionized water to prepare graphene oxide slurry; coating and drying the graphene oxide slurry in a coating mode to obtain graphene oxide film; performing concave-convex treatment on the surface of the graphene oxide film to obtain expanded graphene heat-distribution film; using a whole-width needle to needle the graphene heat-distribution film; then rubbing a layer of scratches on the surface of the graphene heat-distribution film; using a calender to press the graphene heat-distribution film into a preset thickness through a multi-layer stacking mode, and the graphene plate for the graphene solid-state heat-distribution plate is obtained. Meanwhile, the graphene solid-state heat-distribution plate made of the graphene plate is provided. The graphene plate preparation method for the graphene solid-state heat-distribution plate and the graphene solid-state heat-distribution plate provided in the technical scheme can effectively solve the liquid leakage risk and long-term failure problems existing in the prior art.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of graphene plate, and particularly relates to a graphene plate preparation method for a graphene solid vapor chamber and the graphene solid vapor chamber. BACKGROUND

[0002] The liquid cooling plate is a device for heat dissipation, which is usually applied to high-performance computers, servers and other occasions requiring a large amount of operation and data processing. It reduces the chip temperature by introducing water or other liquids into the heat sink and cooling the silicon chip by using the fluid. Although it has the advantages of good effect, etc., compared with some servers, aerospace, radar and other equipment, the liquid cooling plate has the disadvantages of liquid leakage risk and long-term failure.

[0003] The graphene vapor chamber is a new material combining graphene material and vapor chamber. Since graphene is a nano material with greater strength, the thinnest thickness and almost transparent in the world, and has high mechanical properties, excellent thermal conductivity, electrical conductivity, light transmittance, toughness and extremely small resistivity, the performance of the graphene vapor chamber is greatly improved compared with other types of vapor chambers. However, the graphene vapor chamber still needs to be studied in view of the problems of liquid leakage risk and long-term failure. SUMMARY

[0004] The purpose of the present application is to provide a graphene plate preparation method for a graphene solid vapor chamber, which can effectively solve the problems of liquid leakage risk and long-term failure existing in the prior art.

[0005] To solve the above technical problems, the present application adopts the following technical scheme:

[0006] A graphene plate preparation method for a graphene solid vapor chamber, comprising the following steps:

[0007] S1, preparing an oxidized graphene film: mixing and stirring oxidized graphene and deionized water to disperse, after the viscosity of the mixture is initially stirred to rise to 10000 mPa·s, using a high-pressure homogenizer to stir and disperse, after the dispersion is completed, adjusting the pH value of the mixture to above 7, stirring until the slurry viscosity rises to above 3 mPa·s, to prepare an oxidized graphene slurry; coating and drying the oxidized graphene slurry into a film by coating to obtain an oxidized graphene film;

[0008] S2, performing concave-convex treatment on the surface of the oxidized graphene film: the oxidized graphene film is subjected to roller pressing treatment to obtain an oxidized graphene film with uneven surface, and then the oxidized graphene film is pretreated in an oven to remove part of the oxygen-containing groups, so that the carbon-oxygen ratio of the oxidized graphene film is increased to above 4 to obtain a pretreated oxidized graphene film; then the pretreated oxidized graphene film is placed in a graphite furnace, and is heated to 1700-3000 DEG C at a gradient, and is kept in vacuum or inert gas protection throughout the process to obtain an expanded graphene heat dissipation film;

[0009] S3, needle punching and scratching treatment on the surface of the graphene heat dissipation film: an entire width of needle is used to punch the graphene heat dissipation film, so as to build an escape channel for the air in the graphene heat dissipation film during the calendering process; then a layer of scratches is scratched on the surface of the graphene heat dissipation film, so as to provide an anchoring node between layers for the next stage of multi-layer calendering, and improve the interlayer bonding force of the product.

[0010] S4, compaction treatment: the graphene heat dissipation film is pressed into a graphene plate with a thickness of 0.1-500 mm through multi-layer stacking by using a calender, so as to obtain the graphene plate for graphene solid vapor chamber.

[0011] In step S1, the graphene oxide accounts for 4-15 parts by mass; the deionized water accounts for 84-95.9 parts by mass; and the thickness of the prepared graphene oxide film is 10-1000 μm.

[0012] In step S2, the temperature of the oven pretreatment is 60℃-300℃; and the thickness of the obtained graphene heat dissipation film is 100-500 μm; in step S3, the distance between the needles is 1-10 mm, and the size of the needle holes is 0.01-0.5 mm.

[0013] In addition, the application also provides a graphene solid vapor chamber made of the graphene plate.

[0014] The graphene plate preparation method provided in the above technical solution expands the graphene heat dissipation film through high-temperature treatment after the surface of the prepared graphene oxide film is processed to be concave-convex, and then performs needle punching treatment on the expanded graphene heat dissipation film, so as to build an escape channel for the air in the graphene heat dissipation film during the calendering process; the subsequent scratching treatment can provide an anchoring node between layers for the next stage of multi-layer calendering, and improve the interlayer bonding force of the product. The graphene solid vapor chamber made of the graphene plate is full solid and has no liquid leakage, and has the characteristics of high safety and long-term reliability. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a test site physical diagram of example 2 of the application;

[0016] Figure 2 It is a test result diagram of example 2;

[0017] Figure 3 It is a test result diagram of example 2; Figure 2 It is a part of the enlarged view of the test result. DETAILED DESCRIPTION

[0018] In order to make the objects and advantages of the present application more clear, the present application is specifically described below in conjunction with examples. It should be understood that the following description is only used to describe one or several specific embodiments of the present application, and does not strictly limit the protection scope of the present application.

[0019] Example 1

[0020] The present embodiment is a preparation method of graphene plate for graphene solid vapor chamber, specifically comprising the following steps:

[0021] S1, preparation of graphene oxide film

[0022] 4 parts by mass of graphene oxide is mixed and stirred in 95.9 parts by mass of deionized water by using a planetary mixer to disperse, after the initial stirring viscosity of the mixture rises to 10,000 mPa·s, further stirring and dispersing are performed by using a high-pressure homogenizer, after the dispersion is completed, the pH value of the mixture is adjusted to 8, and the slurry viscosity is stirred to rise to more than 3 mPa·s, thereby obtaining a graphene oxide slurry; the obtained graphene oxide slurry is coated and dried into a film by using a doctor blade coater in a coating manner, thereby preparing a graphene oxide film with a thickness of 10-1000 μm;

[0023] S2, surface roughening treatment of graphene oxide film: the graphene oxide film is subjected to roll pressing treatment by using a roll press to obtain a graphene oxide film with uneven surface, the obtained graphene oxide film is pretreated in a high-temperature oven at 250°C to remove part of oxygen-containing groups, thereby increasing the carbon-oxygen ratio of the graphene oxide film to more than 4, and obtaining a pretreated graphene oxide film; the pretreated graphene oxide film is placed in a high-temperature graphite furnace, and is subjected to gradient heating to 2000°C, and the whole process is kept in vacuum or inert gas protection, thereby obtaining a graphene heat dissipation film with an expanded thickness of 100-500 μm;

[0024] S3, surface needling and scratching treatment of expanded graphene film: the needling treatment is performed by using a whole-width needle to needle the expanded graphene film, the distance between the needles is 1-10 mm, and the needle hole size is 0.01-0.5 mm, the purpose is to build an escape channel for air in the expanded graphene film during calendering; the scratching treatment is performed by using a hard brush to scratch a layer of scratches on the surface of the expanded graphene film, thereby providing anchor nodes between layers for the next stage of multi-layer calendering, and improving the interlayer bonding force of the product;

[0025] S4, compaction treatment: the single-layer graphene film with a thickness of 100-500 μm is pressed into a graphene plate for graphene solid vapor chamber with a thickness of 0.1-500 mm by using a vacuum calender in a multi-layer stacking manner.

[0026] The graphene plate obtained by using the above preparation method can reach a certain thickness, and has high interlayer bonding force between the layers, and the stacking is more compact.

[0027] Embodiment 2

[0028] The embodiment is a graphene plate preparation method for a graphene solid vapor chamber, specifically comprising the following steps:

[0029] S1, graphene oxide film preparation

[0030] The planetary mixer is used to mix and stir 15 parts by mass of graphene oxide into 85 parts by mass of deionized water for dispersion. After the initial stirring viscosity of the mixture rises to 10,000 mPa·s, a high-pressure homogenizer is used for further stirring and dispersion. After the dispersion is completed, the pH value of the mixture is adjusted to 8, and the slurry viscosity is stirred to rise above 3 mPa·s. The obtained graphene oxide slurry is coated and dried into a film by a coating method using a doctor blade coater, and a graphene oxide film with a thickness of 10-1000 μm is prepared.

[0031] S2, surface roughening treatment of graphene oxide film: the graphene oxide film is subjected to roll pressing treatment by a roll press to obtain a graphene oxide film with a rough surface. The obtained graphene oxide film is pretreated in a high-temperature oven at 250°C to remove part of the oxygen-containing groups and increase the carbon-oxygen ratio of the graphene oxide film to above 4, thereby obtaining a pretreated graphene oxide film. The pretreated graphene oxide film is placed in a high-temperature graphite furnace, and a gradient heating to 2000°C is performed, with the whole process being kept in vacuum or inert gas protection, thereby obtaining a graphene heat dissipation film with an expanded thickness of 100-500 μm.

[0032] S3, surface needling and scratching treatment of the expanded graphene film: the needling treatment is performed by using a whole-width needle to needle the expanded graphene film, with a distance between the needles of 1-10 mm and a needle hole size of 0.01-0.5 mm. The purpose is to build an escape channel for air in the expanded graphene film during calendering. The scratching treatment is performed by using a hard brush to scratch a layer of scratches on the surface of the expanded graphene film, thereby providing anchor nodes between the layers for the next stage of multi-layer calendering and improving the interlayer bonding force of the product.

[0033] S4, compaction treatment: a vacuum calender is used to press the single-layer graphene film with a thickness of 100-500 μm into a graphene plate for a graphene solid vapor chamber with a thickness of 0.1-500 mm by multi-layer lamination.

[0034] The graphene plate obtained by the above preparation method can achieve a certain thickness, and has a high interlayer bonding force between the layers, and the lamination is more compact.

[0035] Embodiment 3

[0036] The embodiment is a graphene plate preparation method for a graphene solid vapor chamber, specifically comprising the following steps:

[0037] S1, graphene oxide film preparation

[0038] 9 parts by mass of graphene oxide was mixed and stirred into 91 parts by mass of deionized water using a planetary mixer, and after the initial stirring viscosity of the mixture rose to 10,000 mPa·s, a high-pressure homogenizer was used for further stirring and dispersion. After the dispersion was completed, the pH value of the mixture was adjusted to 8, and the slurry was stirred until the viscosity rose to more than 3 mPa·s, to prepare a graphene oxide slurry. The obtained graphene oxide slurry was coated and dried into a film by a coating method using a doctor blade coater, to produce a graphene oxide film with a thickness of 10-1000 μm.

[0039] S2, surface roughening treatment of graphene oxide film: the graphene oxide film was subjected to roll pressing treatment by a roll press to obtain a graphene oxide film with a rough surface, and the obtained graphene oxide film was pretreated in a high-temperature oven at 250°C to remove part of the oxygen-containing groups and increase the carbon-oxygen ratio of the graphene oxide film to more than 4, to obtain a pretreated graphene oxide film. The pretreated graphene oxide film was placed in a high-temperature graphite furnace, and a gradient heating to 2000°C was performed, with the whole process being kept in vacuum or inert gas protection, to obtain a graphene heat dissipation film with an expanded thickness of 100-500 μm.

[0040] S3, surface needling and scratching treatment of expanded graphene film: the needling treatment was performed by using a whole-width needle to needle the expanded graphene film, with a distance between the needles of 1-10 mm and a needle hole size of 0.01-0.5 mm, to build an escape channel for the air in the expanded graphene film during calendering. The scratching treatment was performed by using a hard brush to scratch a layer of scratches on the surface of the expanded graphene film, to provide anchoring nodes between the layers for the multi-layer calendering in the next stage and to improve the interlayer bonding force of the product.

[0041] S4, compaction treatment: a vacuum calender was used to press the single-layer graphene film with a thickness of 100-500 μm into a graphene plate with a thickness of 0.1-500 mm by multi-layer lamination, to obtain a graphene plate for graphene solid vapor chamber.

[0042] The graphene plate obtained by the above preparation method can achieve a certain thickness, and has a high interlayer bonding force between the layers, and the lamination is more compact.

[0043] Example 4

[0044] The present embodiment is a preparation method of a graphene plate for graphene solid vapor chamber, which specifically comprises the following steps:

[0045] S1, graphene oxide film preparation

[0046] The 9 parts of graphene oxide are mixed into 91 parts of deionized water by using a planetary mixer to mix and stir and disperse, after the viscosity of the mixture is initially stirred to 10,000 mPa·s, a high-pressure homogenizer is used for further stirring and dispersing, after the dispersion is completed, the pH value of the mixture is adjusted to 8, and the slurry viscosity is stirred to above 3 mPa·s, to prepare a graphene oxide slurry; the obtained graphene oxide slurry is coated and dried into a film by using a doctor blade coater in a coating manner, to prepare a graphene oxide film with a thickness of 10-1000 μm;

[0047] S2, surface roughening treatment of graphene oxide film: the graphene oxide film is subjected to roll pressing treatment by a roll press to obtain a graphene oxide film with uneven surface, the obtained graphene oxide film is pretreated in a high-temperature oven at 250°C to remove part of oxygen-containing groups, and the carbon-oxygen ratio of the graphene oxide film is increased to 3, to obtain a pretreated graphene oxide film; the pretreated graphene oxide film is placed in a high-temperature graphite furnace, and is heated to 2000°C by gradient heating, and the whole process is kept in vacuum or inert gas protection, to obtain a graphene heat dissipation film with an expanded thickness of 100-500 μm;

[0048] S3, surface needling and scratching treatment of the expanded graphene film: the needling treatment is performed by using a whole surface of needles to needle the expanded graphene film, the distance between the needles is 1-10 mm, and the needle hole size is 0.01-0.5 mm, the purpose is to build an escape channel for the air in the expanded graphene film during calendering; the scratching treatment is performed by using a hard brush to scratch a layer of scratches on the surface of the expanded graphene film, to provide anchoring nodes between layers for the multi-layer calendering in the next stage, and to improve the interlayer bonding force of the product;

[0049] S4, compaction treatment: the single-layer graphene film with a thickness of 100-500 μm is pressed into a graphene plate with a thickness of 0.1-500 mm by using a vacuum calender, to obtain a graphene plate for graphene solid vapor chamber.

[0050] Example 5

[0051] The graphene solid vapor chamber of the present embodiment uses the graphene plate of Example 3 as the core, and an aluminum plate as the shell, and forms a sandwich structure by using vacuum diffusion welding or friction welding, to obtain a graphene solid vapor chamber.

[0052] The following tests are performed on several commonly used materials in the art, and the tested products are as follows:

[0053] Heating sheet (blank test) ; copper VC, 300 μm thick; stainless steel VC, 300 μm thick; graphene plate (obtained from the graphene plate prepared in Example 3, and selected to have a thickness of 300 μm), 300 μm thick; then tested using a multi-channel temperature meter, with a direct current stabilized power supply output of 4 W, four identical ceramic heating sheets each having a diameter of 24 mm connected in series to the stabilized power supply, and an ambient temperature of 25 °C; the upper end of the test sample was attached to the heating sheet, with 10 mm of the test sample protruding from the heating sheet (as shown in Figure 1

[0054] The test results are shown in Figure 2 and Figure 3 From the graph, it can be seen that the heat conduction coefficient of the vapor chamber is higher, so the core temperature of the graphene heat dissipation is higher than that of the stainless steel VC within 0-519 s, but as time goes on, the vapor chamber gradually fails due to the influence of the internal working medium, and the temperature is higher than that of the graphene plate after 519 s. The graphene plate does not fail during use, and the comprehensive heat dissipation performance is better than that of the vapor chamber.

[0055] The embodiments of the present application are described in detail above in combination with examples, but the present application is not limited to the above-described embodiments. For those of ordinary skill in the art, after learning the content described in the present application, they can make several equivalent transformations and substitutions without departing from the principles of the present application, and these equivalent transformations and substitutions should also be considered to belong to the protection scope of the present application.​

Claims

1. A method for manufacturing a graphene plate for a graphene solid-thermal plate, characterized by, The method comprises the following steps: S1, preparing a graphene oxide film: mixing and stirring graphene oxide and deionized water to disperse, after the viscosity of the mixture is increased to 10000 mPa·s, using a high-pressure homogenizer to stir and disperse, after the dispersion is completed, adjusting the pH value of the mixture to 7 or more, stirring until the viscosity of the slurry is increased to 3 mPa·s or more, to prepare a graphene oxide slurry; coating and drying the graphene oxide slurry into a film to obtain a graphene oxide film; S2, performing concave-convex treatment on the surface of the graphene oxide film: the graphene oxide film is subjected to roller pressing treatment to obtain a graphene oxide film with uneven surface, and then is subjected to pretreatment in an oven to remove part of the oxygen-containing groups, increase the carbon-oxygen ratio of the graphene oxide film to 4 or more, and obtain a pretreated graphene oxide film; then the pretreated graphene oxide film is placed in a graphite furnace, and is heated to 1700-3000℃ in a gradient, and is kept in vacuum or inert gas protection during the whole process, to obtain an expanded graphene heat dissipation film; S3, performing needling and scratching treatment on the surface of the graphene heat dissipation film: using a whole-width needle to needle the graphene heat dissipation film to form air escape channels for the graphene heat dissipation film in the calendering process; then scratching a layer of scratches on the surface of the graphene heat dissipation film to provide anchoring nodes between layers for the next stage of multi-layer calendering; S4, compaction treatment: using a calender to press the graphene heat dissipation film into a graphene plate with a thickness of 0.1-500 mm through multi-layer stacking, to obtain a graphene plate for graphene solid vapor chamber.

2. The method of claim 1, wherein the method further comprises: In step S1, the amount of graphene oxide is 4-15 parts by mass; and the amount of deionized water is 84-95.9 parts by mass.

3. The method of claim 2, wherein the method further comprises: The thickness of the graphene oxide film prepared in step S1 is 10-1000 μm.

4. The method of claim 1, wherein the method further comprises: forming a graphene plate on the graphene film. In step S2, the temperature of the oven pretreatment is 60-300℃; and the thickness of the graphene heat dissipation film is 100-500 μm.

5. The method of claim 1, wherein the method further comprises: In step S3, the distance between the needles is 1-10 mm, and the size of the needle holes is 0.01-0.5 mm. ​ 6. A graphene solid vapor chamber made of the graphene plate prepared by the method of any one of claims 1-5.

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