CN113307626A - Preparation method of graphene heat dissipation material with high infrared emissivity - Google Patents

Preparation method of graphene heat dissipation material with high infrared emissivity Download PDF

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CN113307626A
CN113307626A CN202110647291.3A CN202110647291A CN113307626A CN 113307626 A CN113307626 A CN 113307626A CN 202110647291 A CN202110647291 A CN 202110647291A CN 113307626 A CN113307626 A CN 113307626A
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graphene
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dissipation material
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徐帆
付华庆
候嘉兴
赵旭
彭庆宇
赫晓东
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Shenzhen Xichuang Technology Co ltd
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Abstract

A preparation method of a graphene heat dissipation material with high infrared emissivity belongs to the technical field of materials. The invention aims to solve the problem of low thermal emissivity of a graphene plate, and the method comprises the following steps: carrying out vacuum freezing treatment on the graphene slurry; pre-pressing the graphene block after freeze drying; carrying out vacuum degreasing treatment on the graphene pre-pressed block; carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block; carrying out high-temperature graphitization treatment on the graphene plate after vacuum hot pressing sintering; machining the graphene plate in a machining center; polishing the surface of the graphene plate by using a mechanical flat grinder; preheating a graphene plate by using a heating table; uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun; and curing the sprayed graphene plate. The preparation method of the graphene heat dissipation material with high infrared emissivity is firm in coating and bonding, high in heat radiation coefficient, simple in process and easy to realize.

Description

Preparation method of graphene heat dissipation material with high infrared emissivity
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a graphene heat dissipation material with high infrared emissivity.
Background
Graphene, as a carbon material, has a unique set of properties: ultrahigh electric conductivity, super-large heat conductivity, extremely large specific surface area, strong wave-absorbing capacity and the like. The graphene plate is formed by stacking layers of graphene, the problem of high heat conduction of macroscopic materials is solved due to the graphene plate, the graphene plate has great significance for heat dissipation development of electronic devices, and the graphene plate has a very deep application prospect from aerospace to smart phones. However, the biggest problem in applying the graphene board to the field of electronic devices is that due to the characteristics of the graphene board, the thermal emissivity of the surface of the graphene board is very low, and therefore, heat cannot be better spread out. Therefore, finding an effective method to improve the thermal emissivity of the graphene plate has great significance for the application of the graphene plate in the fields of electronic devices and the like.
Disclosure of Invention
The invention aims to solve the problem of low thermal emissivity of a graphene plate and provides a preparation method of a graphene heat dissipation material with high infrared emissivity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a graphene heat dissipation material with high infrared emissivity comprises the following specific steps:
the method comprises the following steps: carrying out vacuum freezing treatment on the graphene slurry;
step two: pre-pressing the graphene block after freeze drying;
step three: carrying out vacuum degreasing treatment on the graphene pre-pressed block;
step four: carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block;
step five: carrying out high-temperature graphitization treatment on the graphene plate after vacuum hot pressing sintering;
step six: machining the graphene plate in a machining center;
step seven: polishing the surface of the graphene plate by using a mechanical flat grinder;
step eight: preheating a graphene plate by using a heating table;
step nine: uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun; the heat radiation coating layer includes: zirconium dioxide, ferric oxide, chromium oxide, silicon dioxide and graphene powder according to the ratio of 2-3: 1: 1-2: 1: 1-2.
Step ten: and curing the sprayed graphene plate.
Further, in the step one, the vacuum freezing treatment is to gradually increase the temperature from-45 ℃ to 45 ℃, and the temperature increase rate is 1-2 ℃/h.
Further, in the second step, the pre-pressure treatment is to gradually increase the pressure from 0t to 10t at a pressure increasing rate of 1t-1.5t/h (the pressure increasing rate can be adjusted freely within the range).
Further, in the third step, the temperature of the vacuum degreasing is gradually increased from 600 ℃ to 1100 ℃, and the temperature increasing rate is 10-15 ℃/min (the temperature increasing rate is randomly adjusted in the range).
Further, in the fourth step, the sintering temperature is gradually increased from 2000 ℃ to 2600 ℃, and the temperature increasing rate is 7-10 ℃/min (the temperature increasing rate is adjusted freely in the range).
Further, in the fifth step, the high temperature is gradually increased from 2500 ℃ to 2900 ℃, and the temperature increasing rate is 5-10 ℃/min (the temperature increasing rate is randomly adjusted in the range).
Further, in the sixth step, the thickness of the processed graphene plate is controlled to be 2-3mm, the length is controlled to be 75mm +/-0.2 mm, the width is controlled to be 25 +/-0.25 mm, and the surface roughness is controlled to be Ra1.6.
Further, in the seventh step, the rough oversize Ra 12.5 after polishing; in step eight, the preheating temperature is 60 ℃ to 70 ℃ (which can be used in the temperature range).
Further, in the ninth step, the thickness of the coating is 3 μm to 5 μm.
Further, in the tenth step, the curing is specifically room temperature curing for 30min, and then curing at 250 ℃ for 30 min.
Compared with the prior art, the invention has the beneficial effects that: the heat conductivity and the heat dissipation efficiency of the surface are improved; the preparation method of the graphene heat dissipation material with high infrared emissivity is firm in coating and bonding, high in heat radiation coefficient, simple in process and easy to realize. According to practical application, the emissivity can be accurately controlled in different areas, and the coating is simple and convenient, firm in coating and combination and high in emissivity.
Drawings
FIG. 1 is a thermal infrared image spectrum of a thermal radiation coating without spraying;
FIG. 2 is a thermal infrared image spectrum of the thermal radiation coating sprayed in example 1;
FIG. 3 is a thermal infrared image spectrum of the thermal radiation coating sprayed in example 2;
fig. 4 is a thermal infrared image of the thermal radiation coating sprayed in example 3.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
1) carrying out vacuum freezing treatment on the graphene slurry at the temperature of-45 ℃, and gradually heating at the heating rate of 1.5 ℃/h;
2) pre-pressing the frozen and dried graphene block body for 0t to 10t, gradually increasing the pressure, wherein the pressure increasing rate is 1.5 t/h;
3) carrying out vacuum degreasing treatment on the graphene pre-pressed block, heating the temperature to 1100 ℃ at a heating rate of 13 ℃/min;
4) carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block at 2000 ℃ to 2600 ℃, wherein the heating rate is 8 ℃/min;
5) carrying out high-temperature graphitization treatment on the graphene plate subjected to vacuum hot pressing sintering at 2500 ℃ to 2900 ℃, wherein the heating rate is 7 ℃/min;
6) machining a graphene plate in a machining center, wherein the thickness is controlled to be 2-3mm, the length is controlled to be 75mm +/-0.2 mm, the width is controlled to be 25 +/-0.25 mm, and the surface thickness and the surface super-roughness are controlled to be Ra1.6;
7) polishing the surface of the graphene plate by using a mechanical flat grinder, wherein the roughness is Ra 12.5;
8) preheating a graphene plate to 70 ℃ by using a heating table;
9) uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun, wherein the thickness is controlled to be 3-5 μm; the radiation coating comprises: the zirconium dioxide, the ferric oxide, the chromium oxide, the silicon dioxide and the graphene powder are mixed according to the ratio of 3:1:1:1: 1.
10) And curing the sprayed graphene plate at room temperature for 30min, and then curing at 250 ℃ for 30 min.
11) Testing the thermal emissivity: and measuring the thermal emissivity of the graphene plate sprayed with the thermal radiation coating by using an infrared thermal imager under the condition that the temperature of the sample is 400 ℃. The thermal emissivity of the thermal radiation coated graphene sheet was measured to be 0.37 higher than that of the uncoated graphene sheet, as shown in fig. 2.
Example 2:
(1) carrying out vacuum freezing treatment on the graphene slurry at the temperature of-45 ℃, and gradually heating at the heating rate of 1-2 ℃/h;
(2) pre-pressing the frozen and dried graphene block body for 0t to 10t, gradually increasing the pressure, wherein the pressure increasing rate is 1.5 t/h;
(3) carrying out vacuum degreasing treatment on the graphene pre-pressed block, heating the temperature to 1100 ℃ at a heating rate of 10 ℃/min;
(4) carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block at 2000 ℃ to 2600 ℃, wherein the heating rate is 7 ℃/min;
(5) carrying out high-temperature graphitization treatment on the graphene plate subjected to vacuum hot pressing sintering at 2500 ℃ to 2900 ℃, wherein the heating rate is 5 ℃/min;
(6) machining a graphene plate in a machining center, wherein the thickness is controlled to be 2-3mm, the length is controlled to be 75mm +/-0.2 mm, the width is controlled to be 25 +/-0.25 mm, and the surface thickness and the surface super-roughness are controlled to be Ra1.6;
(7) polishing the surface of the graphene plate by using a mechanical flat grinder, wherein the roughness is Ra 12.5;
(8) preheating a graphene plate to 70 ℃ by using a heating table;
(9) uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun, wherein the thickness is controlled to be 3-5 μm; the radiation coating comprises: zirconium dioxide, ferric oxide, chromium oxide, silicon dioxide and graphene powder are mixed according to the ratio of 2:1:1.5:1: 1.5.
(10) And curing the sprayed graphene plate at room temperature for 30min, and then curing at 250 ℃ for 30 min.
(11) Testing the thermal emissivity: and measuring the thermal emissivity of the graphene plate sprayed with the thermal radiation coating by using an infrared thermal imager under the condition that the temperature of the sample is 400 ℃. The thermal emissivity of the graphene sheet coated with the thermal radiation coating was measured to be 0.40 higher than that of the uncoated graphene sheet, as shown in fig. 3.
Example 3:
(1) carrying out vacuum freezing treatment on the graphene slurry at the temperature of-45 ℃, and gradually heating at the heating rate of 1-2 ℃/h;
(2) pre-pressing the frozen and dried graphene block body for 0t to 10t, gradually increasing the pressure, wherein the pressure increasing rate is 1 t/h;
(3) carrying out vacuum degreasing treatment on the graphene pre-pressed block, heating the temperature to 1100 ℃ at a heating rate of 15 ℃/min;
(4) carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block at 2000 ℃ to 2600 ℃, wherein the heating rate is 10 ℃/min;
(5) carrying out high-temperature graphitization treatment on the graphene plate subjected to vacuum hot pressing sintering at 2500 ℃ to 2900 ℃, wherein the heating rate is 10 ℃/min;
(6) machining a graphene plate in a machining center, wherein the thickness is controlled to be 2-3mm, the length is controlled to be 75mm +/-0.2 mm, the width is controlled to be 25 +/-0.25 mm, and the surface thickness and the surface super-roughness are controlled to be Ra1.6;
(7) polishing the surface of the graphene plate by using a mechanical flat grinder, wherein the roughness is Ra 12.5;
(8) preheating a graphene plate to 65 ℃ by using a heating table;
(9) uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun, wherein the thickness is controlled to be 3-5 μm; the radiation coating comprises: the zirconium dioxide, the ferric oxide, the chromium oxide, the silicon dioxide and the graphene powder are mixed according to the ratio of 2:1:2:1: 2.
(10) And curing the sprayed graphene plate at room temperature for 30min, and then curing at 250 ℃ for 30 min.
(11) Testing the thermal emissivity: and measuring the thermal emissivity of the graphene plate sprayed with the thermal radiation coating by using an infrared thermal imager under the condition that the temperature of the sample is 400 ℃. The thermal emissivity of the graphene sheet coated with the thermal radiation coating was measured to be 0.43 higher than that of the uncoated graphene sheet, as shown in fig. 4.

Claims (10)

1. A preparation method of a graphene heat dissipation material with high infrared emissivity is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: carrying out vacuum freezing treatment on the graphene slurry;
step two: pre-pressing the graphene block after freeze drying;
step three: carrying out vacuum degreasing treatment on the graphene pre-pressed block;
step four: carrying out vacuum hot-pressing sintering treatment on the degreased graphene pre-pressed block;
step five: carrying out high-temperature graphitization treatment on the graphene plate after vacuum hot pressing sintering;
step six: machining the graphene plate in a machining center;
step seven: polishing the surface of the graphene plate by using a mechanical flat grinder;
step eight: preheating a graphene plate by using a heating table;
step nine: uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun; the heat radiation coating layer includes: zirconium dioxide, ferric oxide, chromium oxide, silicon dioxide and graphene powder according to the ratio of 2-3: 1: 1-2: 1: 1-2, proportioning;
step ten: and curing the sprayed graphene plate.
2. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the first step, the vacuum freezing treatment is to gradually increase the temperature from-45 ℃ to 45 ℃, and the temperature increase rate is 1-2 ℃/h.
3. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the second step, the pre-pressing treatment is to gradually increase the pressure from 0t to 10t, and the pressure increasing rate is 1t-1.5 t/h.
4. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the third step, the temperature of the vacuum degreasing is gradually increased from 600 ℃ to 1100 ℃, and the temperature increasing rate is 10-15 ℃/min.
5. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the fourth step, the sintering temperature is gradually increased from 2000 ℃ to 2600 ℃, and the temperature increasing rate is 7-10 ℃/min.
6. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the fifth step, the temperature is gradually increased from 2500 ℃ to 2900 ℃, and the temperature increasing rate is 5-10 ℃/min.
7. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the sixth step, the thickness of the processed graphene plate is controlled to be 2-3mm, the length is controlled to be 75mm +/-0.2 mm, the width is controlled to be 25 +/-0.25 mm, and the surface roughness is controlled to be Ra1.6.
8. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: step seven, the rough excess Ra 12.5 after polishing; in the eighth step, the preheating temperature is 60-70 ℃.
9. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the ninth step, the thickness of the coating is 3 μm to 5 μm.
10. The preparation method of the graphene heat dissipation material with high infrared emissivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the step ten, the curing is specifically room temperature curing for 30min, and then curing at 250 ℃ for 30 min.
CN202110647291.3A 2021-06-10 2021-06-10 Preparation method of graphene heat dissipation material with high infrared emissivity Pending CN113307626A (en)

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CN108172554A (en) * 2018-03-27 2018-06-15 梧州三和新材料科技有限公司 A kind of high heat conduction and high-heating radiation piece and preparation method thereof
CN109880408A (en) * 2019-01-19 2019-06-14 深圳市国创珈伟石墨烯科技有限公司 A kind of inorganic modified high temperature resistant high emissivity graphene coating and preparation method thereof
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