CN112322258B - Graphene heat-conducting silica gel sheet and preparation method thereof - Google Patents
Graphene heat-conducting silica gel sheet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene heat-conducting silica gel sheet and a preparation method thereof. The graphene heat-conducting silica gel sheet prepared by the invention has high viscosity, high heat conductivity and good tearing resistance, and can meet various heat dissipation requirements.
Description
Technical Field
The invention relates to the technical field of graphene heat conduction materials, in particular to a graphene heat conduction silica gel sheet and a preparation method thereof.
Background
With the development of the electronic information industry and the miniaturization and multi-functionalization of electronic devices, more powerful functions are integrated into smaller electronic components. Therefore, heat dissipation of electronic devices is important in high frequency operation. The two solid surfaces between the electronic device and the heat dissipation device have certain roughness, namely the surfaces are uneven, the actual contact area is only about 10% of the macroscopic contact area, the rest is all gaps, the thermal conductivity of air is about 0.025W/(mK), the thermal resistance is greatly increased, and the heat dissipation efficiency of the electronic device is reduced. Therefore, a layer of high-thermal-conductivity, flexible and easily-deformable thermal interface material is required to be attached to the contact surface, and the thermal interface material is used for filling gaps at the contact surface, so that thermal resistance and heat transfer are reduced as efficiently as possible. The heat-conducting silica gel has certain flexibility, compressibility and natural viscosity, can perfectly fill a gap between an electronic device and a heat dissipation device, and can play a role in shock absorption. However, the existing heat conducting silica gel is generally low in heat conduction, slow in transverse heat transfer and poor in heat soaking effect, and cannot conduct local heat energy to other places quickly.
Graphene, as a novel carbon material, has an ultrahigh thermal conductivity of 5300W/(mK), and is often added with a small amount of thermally conductive silica gel to form a thermally conductive network, so that the graphene is an ideal thermal interface thermally conductive material. However, since the graphene is thick in sheet thickness, small in sheet diameter and easy to agglomerate, the graphene is difficult to uniformly disperse in the heat-conducting silica gel; and because graphite alkene layer self does not have viscidity and tear the performance, lead to graphite alkene layer comparatively fragile, application scope is comparatively little.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the graphene heat-conducting silica gel sheet and the preparation method thereof are provided, and the defect that the application range of a graphene sheet layer is small in the prior art is overcome.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving graphene oxide in distilled water to prepare 0.1-1.5 wt% of graphene oxide aqueous solution;
step two: coating a graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, rolling the film into a roll by using a bundle of carbon fiber bundle as a rolling rod after the film loses 40-50 wt% of water and falls off from the heating plate to obtain a graphene oxide roll, and drying the graphene oxide roll in an oven;
step three: firstly carbonizing the graphene oxide roll, and then graphitizing to obtain the graphene oxide roll with the density of 0.1-0.2 g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; mixing the A/B double-component silica gel in vacuum for 1-2 hours to obtain a heat-conducting silica gel solution;
or weighing the heat-conducting filler, uniformly mixing, adding A/B double-component silica gel, performing vacuum mixing and defoaming, stirring for 2-4 hours, and uniformly stirring to obtain a heat-conducting silica gel solution;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
In order to solve the technical problem, the invention adopts another technical scheme as follows:
a graphene heat-conducting silica gel sheet comprises a graphene roll, heat-conducting silica gel and carbon fiber bundles;
the graphene roll is wound outside the carbon fiber bundle;
the heat-conducting silica gel is attached to the surface of the tiled graphene roll.
The invention has the beneficial effects that: according to the invention, graphene oxide is used as a raw material, a film is firstly prepared, then a coil is prepared, reduction and die cutting are carried out to form sheets, and meanwhile, the heat-conducting silica gel is uniformly dispersed in gaps of graphene sheets by using a dipping process, so that the graphene heat-conducting silica gel sheet with good heat-conducting property, large viscosity and good tearing resistance is prepared. The thermal conductivity of the heat-conducting silica gel prepared by the invention is 50-90 w/(m.k), the hardness is 55-61A, the tear strength is 22-27kN/m, and the heat-radiating requirement can be met. In the sixth step, the graphene roll is immersed in the silica gel, so that the problem of uneven mixing and dispersion of the silica gel and the graphene in the prior art can be solved, and the heat-conducting silica gel is uniformly dispersed in gaps of the graphene sheets; the graphene heat-conducting silicon film prepared by the method has higher strength and is not easy to tear; the preparation method is simple and easy to operate.
Drawings
Fig. 1 is a schematic structural diagram of a graphene heat-conducting silica gel sheet according to the present invention.
Description of reference numerals:
1. a graphene roll; 2. heat conducting silica gel; 3. carbon fiber bundles.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving graphene oxide in distilled water to prepare 0.1-1.5 wt% of graphene oxide aqueous solution;
step two: coating a graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, rolling the film into a roll by using a bundle of carbon fiber bundle as a rolling rod after the film loses 40-50 wt% of water and falls off from the heating plate to obtain a graphene oxide roll, and drying the graphene oxide roll in an oven;
step three: firstly carbonizing the graphene oxide roll, and then graphitizing to obtain the graphene oxide roll with the density of 0.1-0.2 g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; mixing the A/B double-component silica gel in vacuum for 1-2 hours to obtain a heat-conducting silica gel solution;
or weighing the heat-conducting filler, uniformly mixing, adding A/B double-component silica gel, performing vacuum mixing and defoaming, stirring for 2-4 hours, and uniformly stirring to obtain a heat-conducting silica gel solution;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The working principle of the invention is as follows:
the graphene oxide is used as a raw material, a film is firstly prepared, then a coil is prepared, reduction and die cutting are carried out to form the sheet, and meanwhile, the heat-conducting silica gel is uniformly dispersed in gaps of the graphene sheet by using a dipping process to form the graphene heat-conducting silica gel sheet.
From the above description, the beneficial effects of the present invention are: according to the invention, graphene oxide is used as a raw material, a film is firstly prepared, then a coil is prepared, reduction and die cutting are carried out to form sheets, and meanwhile, the heat-conducting silica gel is uniformly dispersed in gaps of graphene sheets by using a dipping process, so that the graphene heat-conducting silica gel sheet with good heat-conducting property, large viscosity and good tearing resistance is prepared. The thermal conductivity of the heat-conducting silica gel prepared by the invention is 50-90 w/(m.k), the hardness is 55-61A, the tear strength is 22-27kN/m, and the heat-radiating requirement can be met. In the sixth step, the graphene roll is immersed in the silica gel, so that the problem of uneven mixing and dispersion of the silica gel and the graphene in the prior art can be solved, and the heat-conducting silica gel is uniformly dispersed in gaps of the graphene sheets; the graphene heat-conducting silicon film prepared by the method has higher strength and is not easy to tear; the preparation method is simple and easy to operate.
Further, the mass ratio of the glue A to the glue B in the step five is 1: 1 to 2.
Further, in the third step, the graphene oxide is carbonized in a tubular furnace for graphene coils.
Further, the temperature rise rate of the tubular furnace in the third step is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h;
and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h;
and a third stage: heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 1 h.
Further, the graphitization in the third step is performed in a graphitization furnace.
Further, the temperature rise of the graphitization in the third step is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min;
and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min;
and a third stage: keeping the temperature at 1300 deg.C for 30 min;
a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min;
the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min;
the sixth stage: heating to 2500 deg.C at 20 deg.C/min;
a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min;
an eighth stage: the incubation was carried out at 2800 ℃ for 1 h.
According to the description, in the third step, the carbonization and the graphitization adopt staged temperature rise, so that the structure between graphene layers can be effectively protected, and the violent reaction in the temperature rise process is prevented, a large amount of gas is generated, and the structure of the graphene film is prevented from being damaged.
Furthermore, the heat-conducting silica gel is a composite prepared by mixing A/B double-component silica gel or A/B double-component silica gel with one or more heat-conducting fillers.
Further, the heat-conducting filler in the fifth step comprises one or more of alumina, aluminum nitride, boron nitride, graphite, silicon carbide, silicon nitride, diamond and metal particles, and the particle size of the heat-conducting filler is 500 nm-100 μm;
the volume ratio of the heat-conducting filler to the cured heat-conducting silica gel is 10-30%.
Further, the volume ratio of the graphene roll to the graphene heat-conducting silica gel sheet is 70% -90%;
the volume ratio of the heat-conducting silica gel to the graphene heat-conducting silica gel sheet is 10% -30%.
A graphene heat-conducting silica gel sheet comprises a graphene roll, heat-conducting silica gel and carbon fiber bundles;
the graphene roll is wound outside the carbon fiber bundle;
the heat-conducting silica gel is attached to the surface of the tiled graphene roll.
The invention is suitable for heat dissipation of electronic products.
Example one
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; the final density was 0.2g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 585g of 5-micrometer alumina is weighed, added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene heat-conducting silica gel sheet prepared in the embodiment was determined to be 75.3w/(m · k), the hardness shore 00 test result was 60, and the tear strength was 23 kN/m.
Example two
Referring to fig. 1, on the basis of the first embodiment, a graphene heat-conducting silica gel sheet is manufactured, and includes a graphene roll 1, heat-conducting silica gel 2 and carbon fiber bundles 3; the graphene roll 1 is wound outside the carbon fiber bundle 3; and the heat-conducting silica gel 2 is attached to the surface of the tiled graphene roll 1.
EXAMPLE III
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; the final density was 0.21g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 480g of aluminum nitride with the particle size of 1 mu m is weighed, added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirred for 3-4 h and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1.5;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene thermal conductive silica gel sheet prepared in the example was determined to be 80.2w/(m · k), the hardness shore 00 test result was 59, and the tear strength was 22 kN/m.
Example four
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; the final density was 0.19g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 405g of aluminum nitride with the particle size of 3 microns is weighed, added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1.2;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene heat-conducting silica gel sheet prepared in the embodiment was determined to be 82.1w/(m · k), the hardness shore 00 test result was 60, and the tear strength was 24 kN/m.
EXAMPLE five
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; the final density was 0.19g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; weighing 337.5g of boron nitride with the particle size of 5 mu m, adding 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirring for 3-4 h, and uniformly stirring to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene heat-conducting silica gel sheet prepared in the embodiment is 71.8w/(m · k), the hardness shore 00 test result is 58, and the tear strength is 22 kN/m.
EXAMPLE six
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; finally obtaining the density of 0.20g/cm after reduction3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 292.5g of alumina with the particle size of 5 microns and 240g of aluminum nitride with the particle size of 1 micron are weighed and mixed uniformly, and added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, and the mixture is stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 2;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene thermal conductive silica gel sheet prepared in this example was 77.9w/(m · k), the hardness shore 00 test result was 61, and the tear strength was 25 kN/m.
EXAMPLE seven
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: at a temperature of 1300 deg.CKeeping the temperature for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; finally obtaining the density of 0.21g/cm after reduction3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 292.5g of alumina with the particle size of 5 microns and 240g of aluminum nitride with the particle size of 1 micron are weighed and mixed uniformly, and added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, and the mixture is stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 2;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene heat-conducting silica gel sheet prepared in the embodiment was measured to be 78.0w/(m · k), the hardness shore 00 test result was 61, and the tear strength was 25 kN/m.
Example eight
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 4.5g of graphene oxide with a solid content of 44.45% in 195.5g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; finally obtaining the density of 0.15g/cm after reduction3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 585g of alumina with the particle size of 5 microns is weighed, added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene thermal conductive silica gel sheet prepared in this example was determined to be 59.0w/(m · k), the hardness shore 00 test result was 59, and the tear strength was 20 kN/m.
Example nine
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 4.5g of graphene oxide with a solid content of 44.45% in 195.5g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: heating to 2500 deg.C at 20 deg.C/min; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; finally obtaining the density of 0.15g/cm after reduction3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, 585g of alumina with the particle size of 5 microns is weighed, added into 350g of A/B double-component silica gel for vacuum mixing and defoaming treatment, stirred for 3-4 hours and uniformly stirred to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene thermal conductive silica gel sheet prepared in this example was determined to be 59.0w/(m · k), the hardness shore 00 test result was 59, and the tear strength was 20 kN/m.
Example ten
A preparation method of a graphene heat-conducting silica gel sheet comprises the following steps:
the method comprises the following steps: dissolving 5.18g of graphene oxide with the solid content of 38.6% in 194.82g of distilled water, and stirring for 2 hours in combination with ultrasonic waves to prepare a 1 wt% graphene oxide aqueous solution;
step two: coating the graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, wherein the temperature of the heating plate is 80 ℃, so that the film loses water; after the film loses 40 wt% of water and falls off from the heating plate, rolling the film into a roll by using a bundle of carbon fiber bundles as a rolling rod to obtain a graphene oxide roll, wherein the interlayer gap of the graphene oxide roll is less than 1mm, and drying the graphene oxide roll in an oven at the drying temperature of 80 ℃ for 2-4 h;
step three: carbonizing the graphene oxide roll in a tubular furnace for graphene rolls, wherein the heating rate of the tubular furnace is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h; and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h; and a third stage: heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1 h;
then graphitizing in a graphitizing furnace, wherein the temperature rise of the graphitizing furnace is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min; and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min; and a third stage: keeping the temperature at 1300 deg.C for 30 min; a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min; the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min; the sixth stage: at a rate of 20 ℃/minHeating to 2500 deg.c; a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min; an eighth stage: keeping the temperature at 2800 ℃ for 1 h; finally obtaining the density of 0.20g/cm after reduction3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; specifically, carrying out vacuum mixing and defoaming treatment on the A/B double-component silica gel, stirring for 1-2 hours, and uniformly stirring to obtain a heat-conducting silica gel solution; wherein the mass ratio of the glue A to the glue B is 1: 1;
step six: and (4) dipping the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the dipping is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film.
The thermal conductivity of the graphene heat-conducting silica gel sheet prepared in the example was determined to be 62.5w/(m · k), the hardness shore 00 test result was 55, and the tear strength was 27 kN/m.
In summary, according to the graphene heat-conducting silicone sheet and the preparation method thereof provided by the invention, the heat-conducting silicone is uniformly distributed in the graphene roll, so that the graphene heat-conducting silicone sheet with good heat-conducting property, large viscosity and good tearing resistance is prepared, and various heat dissipation requirements can be met.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (9)
1. The preparation method of the graphene heat-conducting silica gel sheet is characterized by comprising the following steps:
the method comprises the following steps: dissolving graphene oxide in distilled water to prepare 0.1-1.5 wt% of graphene oxide aqueous solution;
step two: coating a graphene oxide aqueous solution on a heating plate to form a 1-2 mm film, rolling the film into a roll by using a bundle of carbon fiber bundle as a rolling rod after the film loses 40-50 wt% of water and falls off from the heating plate to obtain a graphene oxide roll, and drying the graphene oxide roll in an oven;
step three: firstly carbonizing the graphene oxide roll, and then graphitizing to obtain the graphene oxide roll with the density of 0.1-0.2 g/cm3The graphene roll film of (1);
step four: cutting the graphene roll film into graphene sheets with the thickness not less than 0.3 mm;
step five: preparing a heat-conducting silica gel solution; mixing the A/B double-component silica gel in vacuum for 1-2 hours to obtain a heat-conducting silica gel solution;
or weighing the heat-conducting filler, uniformly mixing, adding A/B double-component silica gel, performing vacuum mixing and defoaming, stirring for 2-4 hours, and uniformly stirring to obtain a heat-conducting silica gel solution;
step six: soaking the graphene sheet in the heat-conducting silica gel solution obtained in the fifth step for 2-4 hours, taking out after the soaking is finished, removing redundant heat-conducting silica gel on the surface of the graphene sheet, and curing in an oven at the temperature of 130 ℃ for 6-8 hours to obtain the graphene heat-conducting silica gel film;
the temperature rise of the graphitization in the step three is divided into eight stages:
the first stage is as follows: heating the carbonized graphene oxide to 1000 ℃ at the speed of 50 ℃/min;
and a second stage: heating to 1300 deg.C at a rate of 10 deg.C/min;
and a third stage: keeping the temperature at 1300 deg.C for 30 min;
a fourth stage: heating to 1500 ℃ at the speed of 10 ℃/min;
the fifth stage: heating to 2000 deg.C at a rate of 25 deg.C/min;
the sixth stage: heating to 2500 deg.C at 20 deg.C/min;
a seventh stage: heating to 2800 ℃ at the speed of 5 ℃/min;
an eighth stage: the incubation was carried out at 2800 ℃ for 1 h.
2. The preparation method of the graphene heat-conducting silica gel sheet according to claim 1, wherein the mass ratio of the glue A to the glue B in the step five is 1: 1 to 2.
3. The method for preparing the graphene heat-conducting silica gel sheet according to claim 1, wherein in the third step, the graphene oxide is carbonized in a tube furnace for graphene coils.
4. The preparation method of the graphene heat-conducting silica gel sheet according to claim 3, wherein the temperature rise rate of the tubular furnace in the three steps is divided into three stages:
the first stage is as follows: insulating the graphene oxide at 105 ℃ for 1 h;
and a second stage: heating to 220 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 1 h;
and a third stage: heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 1 h.
5. The method for preparing the graphene heat-conducting silica gel sheet according to claim 1, wherein the graphitization in the third step is performed in a graphitization furnace.
6. The method for preparing a graphene heat-conducting silica gel sheet according to claim 1, wherein the heat-conducting silica gel is a composite prepared by mixing A/B two-component silica gel or A/B two-component silica gel with one or more heat-conducting fillers.
7. The preparation method of the graphene heat-conducting silica gel sheet according to claim 1, wherein the heat-conducting filler in the fifth step comprises one or more of alumina, aluminum nitride, boron nitride, graphite, silicon carbide, silicon nitride, diamond and metal particles, and the particle size of the heat-conducting filler is 500 nm-100 μm;
the volume ratio of the heat-conducting filler to the cured heat-conducting silica gel is 10-30%.
8. The preparation method of the graphene heat-conducting silica gel sheet according to claim 1, wherein the volume ratio of the volume of the graphene roll to the volume of the graphene heat-conducting silica gel sheet is 70% -90%;
the volume ratio of the heat-conducting silica gel to the graphene heat-conducting silica gel sheet is 10% -30%.
9. A graphene heat-conducting silica gel sheet is prepared by the preparation method of the graphene heat-conducting silica gel sheet according to any one of claims 1 to 8, and is characterized by comprising a graphene roll, heat-conducting silica gel and carbon fiber bundles;
the graphene roll is wound outside the carbon fiber bundle;
the heat-conducting silica gel is attached to the surface of the tiled graphene roll.
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