CN113666363A - Preparation method of graphene oxide material with high thermal radiation coefficient and high electromagnetic shielding - Google Patents
Preparation method of graphene oxide material with high thermal radiation coefficient and high electromagnetic shielding Download PDFInfo
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- CN113666363A CN113666363A CN202110897805.0A CN202110897805A CN113666363A CN 113666363 A CN113666363 A CN 113666363A CN 202110897805 A CN202110897805 A CN 202110897805A CN 113666363 A CN113666363 A CN 113666363A
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Abstract
A preparation method of a graphene oxide material with high thermal radiation coefficient and high electromagnetic shielding belongs to the technical field of materials. The invention aims to solve the problem that the existing composite material has poor heat dissipation effect and electromagnetic shielding effect, and the method comprises the following steps: uniformly stirring the graphene oxide slurry; carrying out vacuum freeze drying treatment; hydrazine hydrate reduction treatment; performing high-temperature graphitization treatment; carrying out vacuum cold pressing treatment; the machining center carries out machining; polishing by using a mechanical flat grinder; preheating a heating table; uniformly spraying a thermal radiation coating on the surface of the graphene plate by using a spray gun; the thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: 5-6, proportioning; and curing the sprayed graphene plate. The thickness of the material is only 0.5-2mm, the electromagnetic shielding performance is 50-70 dB on the whole, and the thermal radiation coefficient of the graphene plate sprayed with the thermal radiation coating is 0.34-0.41 higher than that of the graphene plate which is not sprayed.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a graphene oxide material with high thermal radiation coefficient and high electromagnetic shielding.
Background
In order to timely transmit heat to a heat dissipation device and the external surrounding environment, the surface of a heating electronic element must be provided with the heat dissipation device, and the electronic element emits a large amount of heat instantly to carry out cooling protection, so that a heat dissipation material with rapid heat absorption and dissipation efficiency is needed. The miniaturization development of electronic equipment increases the difficulty of heat dissipation management in a small space, and meanwhile, the higher the integration level is, the larger the electromagnetic generation is, the more and more the electromagnetic interference to the outside is, and the demands on thinning, miniaturization and electromagnetic shielding of the heat dissipation sheet are generated. However, to date, the development of such a multifunctional material remains a significant challenge.
Disclosure of Invention
The invention aims to solve the problem that the existing composite material is poor in heat dissipation effect and electromagnetic shielding effect, and provides a preparation method of a graphene oxide material with high thermal radiation coefficient and high electromagnetic shielding.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a graphene oxide material with high thermal emissivity and high electromagnetic shielding comprises the following specific steps:
the method comprises the following steps: uniformly stirring the graphene oxide slurry;
step two: carrying out vacuum freeze drying treatment on the uniformly stirred graphene oxide slurry;
step three: carrying out hydrazine hydrate reduction treatment on the material subjected to vacuum freeze drying treatment;
step four: carrying out high-temperature graphitization treatment on the material subjected to hydrazine hydrate reduction treatment;
step five: carrying out vacuum cold pressing treatment on the sample subjected to the high-temperature graphitization treatment;
step six: carrying out machining on the cold-pressed graphene sample by 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 thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: 5-6 (in any range);
step ten: and curing the sprayed graphene plate.
Further, in the first step, the solid content of the graphene oxide slurry is 1-15 mg/ml, and the stirring time is 1-5 h (within the range).
Further, in the second step, the vacuum freeze-drying treatment specifically comprises: the temperature is gradually increased from-45 ℃ to 45 ℃, and the heating rate is 1-2 ℃/h (within the range).
Further, in the third step, the hydrazine hydrate reduction treatment specifically comprises: treating for 2-48 h (in the range) at the temperature of 80-90 ℃.
Further, in the fourth step, the high-temperature graphitization treatment specifically comprises: the temperature is raised from 2500 ℃ to 3000 ℃, and the temperature raising rate is 5-10 ℃/min (the temperature raising rate is adjusted freely in the range).
Further, in the fifth step, the pressure of the vacuum cold pressing treatment is 100t-120t (within the range), the treatment time is 10min, and the vacuum degree is 0.05-0.2 Pa.
Further, in the sixth step, the thickness of the machining is controlled to be 0.5-2mm, 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 Ra 1.6; and seventhly, controlling the rough degree of the grinding to be Ra 12.5.
Further, in the eighth step, the temperature of the preheating is 70 ℃ to 80 ℃ (any temperature range can be used).
Further, in step nine, the thickness of the heat radiation coating layer is controlled to be 4 μm to 6 μm (any within this range).
Further, in step ten, the curing procedure specifically includes: curing at room temperature for 60min and at 300 ℃ for 60 min.
Compared with the prior art, the invention has the beneficial effects that: the invention aims to solve the requirements of thinning and miniaturization, and has simple process and easy realization. The thickness of the material is only 0.5 mm-2 mm, the electromagnetic shielding performance is 50-70 dB on the whole, and the thermal radiation coefficient of the graphene plate sprayed with the thermal radiation coating is 0.34-0.41 higher than that of the graphene plate which is not sprayed.
Drawings
FIG. 1 is an electromagnetic shielding diagram of example 1;
fig. 2 is a graph of the thermal radiation coefficient of the graphene board without thermal radiation coating sprayed thereon in example 1;
fig. 3 is a graph of the thermal radiation coefficient of the graphene plate sprayed with the thermal radiation coating in example 1;
FIG. 4 is an electromagnetic shield diagram of example 2;
fig. 5 is a graph of thermal radiation coefficient of a graphene plate sprayed with a thermal radiation coating in example 2;
FIG. 6 is an electromagnetic shield diagram of embodiment 3;
fig. 7 is a graph of the thermal radiation coefficient of the graphene plate sprayed with the thermal radiation coating 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:
a preparation method of a graphene oxide material with high thermal emissivity and high electromagnetic shielding comprises the following steps:
(1) uniformly stirring 100ml of graphene oxide slurry with the solid content of 1mg/ml for 1 h;
(2) carrying out vacuum freeze drying treatment on the uniformly stirred graphene oxide slurry, gradually heating up to 45 ℃ at the temperature of minus 45 ℃, wherein the heating-up rate is 1 ℃/h;
(3) carrying out hydrazine hydrate reduction treatment on the material subjected to vacuum freeze drying treatment, and treating for 2h at 80 ℃;
(4) carrying out high-temperature graphitization treatment on the material subjected to hydrazine hydrate reduction treatment, heating to 2500 ℃ to 3000 ℃, and heating at a rate of 5 ℃/min;
(5) and carrying out vacuum cold pressing treatment on the sample subjected to high-temperature graphitization treatment, wherein the pressure is 100t, the treatment time is 10min, and the vacuum degree is about 0.1 Pa.
(6) Machining a machining center on the cold-pressed graphene sample, wherein the thickness is controlled to be 0.5mm, 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 Ra 1.6;
(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 4 micrometers; the thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: and 5, proportioning.
(10) And curing the sprayed graphene plate at room temperature for 60min, and then curing at 300 ℃ for 60 min.
The electromagnetic shielding performance of the material obtained in the present example was tested by using a waveguide method, and the result is shown in fig. 1, where the specific value is about 50 dB; 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 emissivity coated graphene sheet was measured to be 0.34 higher than that of the uncoated graphene sheet (as shown in fig. 2), as shown in fig. 3.
Example 2:
a preparation method of a graphene oxide material with high thermal emissivity and high electromagnetic shielding comprises the following steps:
(1) uniformly stirring 100ml of graphene oxide slurry with the solid content of 9mg/ml for 3 hours;
(2) carrying out vacuum freeze drying treatment on the uniformly stirred graphene oxide slurry, gradually heating up to 45 ℃ at the temperature of minus 45 ℃, wherein the heating-up rate is 1.5 ℃/h;
(3) carrying out hydrazine hydrate reduction treatment on the material subjected to vacuum freeze drying treatment, and treating for 24h at 85 ℃;
(4) carrying out high-temperature graphitization treatment on the material subjected to hydrazine hydrate reduction treatment, heating to 2500 ℃ to 3000 ℃, and heating at a speed of 7 ℃/min;
(5) and carrying out vacuum cold pressing treatment on the sample subjected to high-temperature graphitization treatment, wherein the pressure is 110t, the treatment time is 10min, and the vacuum degree is about 0.1 Pa.
(6) Machining a machining center on the cold-pressed graphene sample, wherein the thickness is controlled to be 1.5mm, 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 Ra 1.6;
(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 75 ℃ 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 5 mu m; the thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: and 5.5, proportioning.
(10) Curing the sprayed graphene plate at room temperature for 60min, and then curing at 300 ℃ for 60 min;
the electromagnetic shielding performance of the material obtained in this example was tested by the waveguide method, and the result is shown in fig. 4, where the specific value is about 55 dB. 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 0.4 higher than that of the uncoated graphene sheet, as shown in fig. 5.
Example 3:
a preparation method of a graphene oxide material with high thermal emissivity and high electromagnetic shielding comprises the following steps:
(1) uniformly stirring 100ml of graphene oxide slurry with the solid content of 15mg/ml for 5 hours;
(2) carrying out vacuum freeze drying treatment on the uniformly stirred graphene oxide slurry, gradually heating up to 45 ℃ at the temperature of minus 45 ℃, wherein the heating-up rate is 2 ℃/h;
(3) carrying out hydrazine hydrate reduction treatment on the material subjected to vacuum freeze drying treatment, and treating for 48h at 90 ℃;
(4) carrying out high-temperature graphitization treatment on the material subjected to hydrazine hydrate reduction treatment, heating to 2500 ℃ to 3000 ℃, and heating at a speed of 10 ℃/min;
(5) and carrying out vacuum cold pressing treatment on the sample subjected to high-temperature graphitization treatment, wherein the pressure is 120t, the treatment time is 10min, and the vacuum degree is about 0.1 Pa.
(6) Machining a cold-pressed graphene sample in a machining center, wherein the thickness is controlled to be 2mm, 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 Ra 1.6;
(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 80 ℃ 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 6 microns; the thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: and 6, proportioning.
(10) Curing the sprayed graphene plate at room temperature for 60min, and then curing at 300 ℃ for 60 min;
the electromagnetic shielding performance of the material obtained in this example was tested by the waveguide method, and the result is shown in fig. 6, where the specific value is about 65 dB. 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 0.41 higher than that of the uncoated graphene sheet, as shown in fig. 7.
Claims (10)
1. A preparation method of a graphene oxide material with high thermal emissivity and high electromagnetic shielding is characterized by comprising the following steps: the method comprises the following specific steps:
the method comprises the following steps: uniformly stirring the graphene oxide slurry;
step two: carrying out vacuum freeze drying treatment on the uniformly stirred graphene oxide slurry;
step three: carrying out hydrazine hydrate reduction treatment on the material subjected to vacuum freeze drying treatment;
step four: carrying out high-temperature graphitization treatment on the material subjected to hydrazine hydrate reduction treatment;
step five: carrying out vacuum cold pressing treatment on the sample subjected to the high-temperature graphitization treatment;
step six: carrying out machining on the cold-pressed graphene sample by 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; the thermal radiation coating comprises zirconium dioxide, ferric oxide, chromium oxide and graphene powder, and is prepared according to the following steps of 2: 1: 2: 5-6, proportioning;
step ten: and curing the sprayed graphene plate.
2. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the first step, the solid content of the graphene oxide slurry is 1-15 mg/ml, and the stirring time is 1-5 hours.
3. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the second step, the vacuum freeze drying treatment specifically comprises the following steps: the temperature is gradually increased from minus 45 ℃ to 45 ℃, and the heating rate is 1-2 ℃/h.
4. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the third step, the hydrazine hydrate reduction treatment specifically comprises the following steps: treating for 2-48 h at 80-90 ℃.
5. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the fourth step, the high-temperature graphitization treatment specifically comprises the following steps: the temperature is raised from 2500 ℃ to 3000 ℃, and the temperature raising rate is 5-10 ℃/min.
6. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the fifth step, the pressure of the vacuum cold pressing treatment is 100t-120t, the treatment time is 10min, and the vacuum degree is 0.05-0.2 Pa.
7. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: step six, controlling the thickness of the machining to be 0.5-2mm, the length to be 75mm +/-0.2 mm, the width to be 25 +/-0.25 mm and the surface thickness to be Ra1.6; and seventhly, controlling the rough degree and the super degree of the grinding to be Ra12.5.
8. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the eighth step, the preheating temperature is 70-80 ℃.
9. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the ninth step, the thickness of the heat radiation coating is controlled to be 4-6 μm.
10. The method for preparing the graphene oxide material with high thermal emissivity and high electromagnetic shielding according to claim 1, wherein the graphene oxide material comprises: in the tenth step, the curing procedure specifically comprises: curing at room temperature for 60min and at 300 ℃ for 60 min.
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