CN115196623A - Preparation method of low-resilience graphene foam - Google Patents
Preparation method of low-resilience graphene foam Download PDFInfo
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- CN115196623A CN115196623A CN202210523136.5A CN202210523136A CN115196623A CN 115196623 A CN115196623 A CN 115196623A CN 202210523136 A CN202210523136 A CN 202210523136A CN 115196623 A CN115196623 A CN 115196623A
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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
- C01B32/19—Preparation by exfoliation
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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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The invention discloses a preparation method of low-resilience graphene foam, which comprises the following steps: s1: preparing graphene oxide composite slurry: mixing, stirring and dispersing 1-10 parts by mass of graphene oxide and 0-10 parts by mass of graphene in 70-98 parts by mass of deionized water, dispersing by various processes such as ultrasonic treatment, homogeneous stripping and the like to obtain high-monolayer graphene oxide/graphene slurry, adding 1-10 parts by mass of hollow material, and stirring until uniform mixing is achieved to obtain the graphene oxide composite slurry. According to the invention, the addition of the hollow material improves the porosity of the original material graphene oxide membrane. Meanwhile, the high-expansion graphene foam is obtained through clamp constraint and a high-temperature heat treatment process, and the foam has high expansion and high thermal conductivity due to the adoption of the high-temperature heat treatment.
Description
Technical Field
The invention relates to the technical field of graphene foam, in particular to a preparation method of low-resilience graphene foam.
Background
With the development of electronic devices, more and more integrated chips are used for smart devices used by the public, industrial-grade manufacturing devices, and high-power devices such as radars for national defense security. The manufacturing processes of the chips are more and more precise, the number of transistors contained in a unit is increased, so that the heat generation amount per unit area is increased, and some devices integrate more chips in a limited space, so that the chips inevitably generate a large amount of heat in the operation process, and therefore higher requirements are put on heat dissipation.
In the heat conduction of electronic devices, heat dissipation is mainly achieved by heat conduction and heat convection, in which heat convection is achieved by means of a fan or the like, and heat conduction is mainly achieved by a highly heat conductive material. However, in electronic devices, heat conduction between different structural components is sometimes required due to structural component design influences. In this case, the conventional method adopts heat-conducting silicone grease or heat-conducting silicone gel as an interface material to perform a heat-conducting function. However, the heat-conducting silicone grease or the heat-conducting silicone rubber has the defects of low heat-conducting coefficient, poor temperature resistance, easy failure for a long time and the like, and is easy to cause thermal failure.
The graphene heat dissipation film is a novel interface heat conduction material, and the excellent heat conduction performance enables the graphene to be an ideal heat dissipation material for a super-large-scale nanometer integrated circuit, so that the requirement of replacing heat conduction silicone grease or heat conduction silicone gel for the attachment of a thermal interface material is completely met.
Disclosure of Invention
The invention aims to: in order to solve the problems, the preparation method of the low-resilience graphene foam is provided.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of low-resilience graphene foam comprises the following steps:
s1: preparing graphene oxide composite slurry: mixing, stirring and dispersing 1-10 parts by mass of graphene oxide and 0-10 parts by mass of graphene in 70-98 parts by mass of deionized water, dispersing by various processes such as ultrasonic treatment, homogeneous stripping and the like to obtain high-single-layer graphene oxide/graphene slurry, adding 1-10 parts by mass of a hollow material, and stirring until the mixture is uniformly mixed to prepare graphene oxide composite slurry;
s2: preparing a pre-foamed graphene oxide film: coating, drying and film-forming the prepared graphene oxide composite slurry by adopting a coating mode to prepare a pre-foamed graphene oxide film with the thickness of 10-1000 mu m;
s3: preparing a primarily foamed graphene oxide film: pretreating the prepared pre-foamed graphene oxide film at 60-300 ℃, accurately controlling the temperature rise rate and the heat preservation time, and controlling the release quantity and the release rate of decomposed gas to obtain a primarily foamed graphene oxide film;
s4: preparing high-rate expanded graphene foam: treating the preliminarily foamed graphene oxide film prepared in the previous step by using a special constraint fixture, then placing the treated film into a high-temperature graphite furnace, heating to 1700-3000 ℃ in a gradient manner, and keeping vacuum or inert gas protection in the whole process to obtain high-magnification expanded graphene foam;
s5: preparing graphene foam with a specific foaming rate; pressing the prepared high-magnification expanded graphene foam to the density of 0.1-1g/cm by adopting a calender 3 And obtaining the graphene foam meeting the specific foaming multiplying power.
Preferably, the thickness of the low resilience graphene foam prepared in the step S5 is 10-1000 microns.
Preferably, the graphene oxide in S1 is chemical graphene oxide or electrochemical graphene oxide.
Preferably, the graphene in S1 is mechanically exfoliated graphene, electrochemically exfoliated graphene or reduced graphene oxide.
Preferably, the hollow material in S1 is a hollow glass microsphere, a porous carbon microsphere or yangbuck powder, and the yangbuck powder is an expandable plastic microsphere.
Preferably, the coating mode in S2 is knife coating, flat coating, roll coating or transfer coating.
Preferably, the rolling method in S5 is rolling, flat pressing or static pressing.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the method, the porosity of the original material graphene oxide membrane is improved by adding the hollow material. Meanwhile, the high-expansion graphene foam is obtained through the clamp constraint and high-temperature heat treatment process, and the high-expansion graphene foam has high expansion and high heat conductivity due to the adoption of high-temperature heat treatment.
2. Compared with the traditional graphene oxide film with the thickness of 10-50 microns, the graphene oxide film coated with the graphene oxide film has a wider application range, and the overflow speed of thermal decomposition gas can be controlled by adopting a heat treatment process with a certain temperature rise speed at 60-300 ℃, so that the film can not be crushed in the expansion process. And graphitizing at high temperature to obtain graphene foam with flat surface, high expansion rate and high heat conductivity, and pressing the graphene oxide film with high expansion rate into a compact high heat conductivity graphene heat dissipation film with the density of 0.1-1g/cm & lt 3 & gt and the heat conductivity coefficient of more than 50 w/m.k through a calendar.
Drawings
FIG. 1 shows a schematic representation of the steps of a preparation method provided according to an embodiment of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
a preparation method of low-resilience graphene foam comprises the following steps:
s1: preparing graphene oxide composite slurry: mixing, stirring and dispersing 1-10 parts by mass of graphene oxide and 0-10 parts by mass of graphene in 70-98 parts by mass of deionized water, dispersing by multiple processes such as ultrasonic treatment and homogeneous stripping to obtain high single-layer graphene oxide/graphene slurry, adding 1-10 parts by mass of a hollow material, stirring until the mixture is uniformly mixed, and preparing graphene oxide composite slurry;
s2: preparing a pre-foamed graphene oxide film: coating, drying and film-forming the prepared graphene oxide composite slurry by adopting a coating mode to prepare a pre-foamed graphene oxide film with the thickness of 10-1000 mu m;
s3: preparing a primarily foamed graphene oxide film: pretreating the prepared pre-foamed graphene oxide film at 60-300 ℃, accurately controlling the temperature rise rate and the heat preservation time, and controlling the release quantity and the release rate of decomposed gas to obtain a primarily foamed graphene oxide film;
s4: preparing high-rate expanded graphene foam: treating the preliminarily foamed graphene oxide film prepared in the last step by using a special constraint fixture, then placing the treated film into a high-temperature graphite furnace, heating to 1700-3000 ℃ in a gradient manner, and keeping vacuum or inert gas protection in the whole process to obtain high-magnification expanded graphene foam;
s5: preparing graphene foam with a specific foaming multiplying power; pressing the prepared high-magnification expanded graphene foam to the density of 0.1-1g/cm by adopting a calender 3 And obtaining the graphene foam meeting the specific foaming multiplying power.
The thickness of the low-resilience graphene foam prepared in the S5 is 10-1000 microns.
The graphene oxide in the S1 is chemical graphene oxide or electrochemical graphene oxide.
In S1, the graphene is mechanically stripped graphene, electrochemically stripped graphene or reduced graphene oxide
The hollow material in S1 is hollow glass microsphere, porous carbon microsphere or Yangbuck powder, and the Yangbuck powder is expandable plastic microsphere.
The coating mode in S2 is knife coating, flat coating, roll coating or transfer coating.
And the rolling method in the S5 is rolling, flat pressing or static pressing.
The previous description of the embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A preparation method of low-resilience graphene foam is characterized by comprising the following steps:
s1: preparing graphene oxide composite slurry: mixing, stirring and dispersing 1-10 parts by mass of graphene oxide and 0-10 parts by mass of graphene in 70-98 parts by mass of deionized water, dispersing by multiple processes such as ultrasonic treatment and homogeneous stripping to obtain high single-layer graphene oxide/graphene slurry, adding 1-10 parts by mass of a hollow material, stirring until the mixture is uniformly mixed, and preparing graphene oxide composite slurry;
s2: preparing a pre-foamed graphene oxide film: coating, drying and film-forming the prepared graphene oxide composite slurry by adopting a coating mode to prepare a pre-foamed graphene oxide film with the thickness of 10-1000 mu m;
s3: preparing a primarily foamed graphene oxide film: pretreating the prepared pre-foamed graphene oxide film at 60-300 ℃, accurately controlling the heating rate and the heat preservation time, and controlling the release quantity and the release rate of decomposition gas to obtain a pre-foamed graphene oxide film;
s4: preparing high-rate expanded graphene foam: treating the preliminarily foamed graphene oxide film prepared in the previous step by using a special constraint fixture, then placing the treated film into a high-temperature graphite furnace, heating to 1700-3000 ℃ in a gradient manner, and keeping vacuum or inert gas protection in the whole process to obtain high-magnification expanded graphene foam;
s5: preparing graphene foam with a specific foaming multiplying power; pressing the prepared high-magnification expanded graphene foam to the density of 0.1-1g/cm by adopting a calender 3 And obtaining the graphene foam meeting the specific foaming multiplying power.
2. The method for preparing the low resilience graphene foam according to claim 1, wherein the thickness of the low resilience graphene foam prepared in the step S5 is 10-1000 microns.
3. The preparation method of the low resilience graphene foam according to claim 1, wherein the graphene oxide in S1 is chemical graphene oxide or electrochemical graphene oxide.
4. The preparation method of the low resilience graphene foam according to claim 1, wherein the graphene in the S1 is mechanically exfoliated graphene, electrochemically exfoliated graphene or reduced graphene oxide.
5. The preparation method of the low resilience graphene foam according to claim 1, wherein the hollow material in S1 is hollow glass microspheres, porous carbon microspheres or yangbuck powder, and the yangbuck powder is expandable plastic microspheres.
6. The preparation method of the low resilience graphene foam according to claim 1, wherein the coating mode in the S2 is knife coating, flat coating, roller coating or transfer coating.
7. The preparation method of the low resilience graphene foam according to claim 1, wherein the S5 medium rolling method is rolling, flat pressing or static pressing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210523136.5A CN115196623A (en) | 2022-05-13 | 2022-05-13 | Preparation method of low-resilience graphene foam |
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| CN202210523136.5A CN115196623A (en) | 2022-05-13 | 2022-05-13 | Preparation method of low-resilience graphene foam |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601476A (en) * | 2017-09-11 | 2018-01-19 | 长沙小新新能源科技有限公司 | A kind of preparation method of High-performance graphene perforated membrane |
| CN111286309A (en) * | 2020-03-24 | 2020-06-16 | 昆山印可达新材料科技有限公司 | High-performance graphene heat dissipation film, and preparation method and application thereof |
| CN112374492A (en) * | 2020-10-27 | 2021-02-19 | 武汉汉烯科技有限公司 | High-electric-conductivity high-thermal-conductivity coiled material graphene film and preparation method thereof |
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- 2022-05-13 CN CN202210523136.5A patent/CN115196623A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601476A (en) * | 2017-09-11 | 2018-01-19 | 长沙小新新能源科技有限公司 | A kind of preparation method of High-performance graphene perforated membrane |
| CN111286309A (en) * | 2020-03-24 | 2020-06-16 | 昆山印可达新材料科技有限公司 | High-performance graphene heat dissipation film, and preparation method and application thereof |
| CN112374492A (en) * | 2020-10-27 | 2021-02-19 | 武汉汉烯科技有限公司 | High-electric-conductivity high-thermal-conductivity coiled material graphene film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 房永广等: "《赤泥资源化利用理论及技术》", 中国建材工业出版社, pages: 59 * |
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