CN112723345B - Composite graphene slurry with self-assembly property and preparation method thereof - Google Patents
Composite graphene slurry with self-assembly property and preparation method thereof Download PDFInfo
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- CN112723345B CN112723345B CN202011634488.5A CN202011634488A CN112723345B CN 112723345 B CN112723345 B CN 112723345B CN 202011634488 A CN202011634488 A CN 202011634488A CN 112723345 B CN112723345 B CN 112723345B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
Abstract
The invention discloses a composite graphene slurry with self-assembly property and a preparation method thereof, wherein the formula comprises the following steps: the weight ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20:1; a preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; step two, selecting a formula; thirdly, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction; in the first step, the graphene oxide reactant is prepared and cleaned by the Hummer's method, and the solid content of the graphene oxide reactant is 3% -10%, so that the graphene film material with any thickness is formed by stacking and combining, the production difficulty and cost of a coating link are reduced, and meanwhile, the selected binder is a common industrial raw material, is low in cost and good in affinity with the graphene oxide, and provides convenience for large-scale production.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to composite graphene slurry with self-assembly properties and a preparation method thereof.
Background
Graphene has been paid attention to because of its ultra-high thermal conductivity (-5300W/m·k) since 2004, and a graphene-based redox reaction graphene thermal conductive film preparation method and product have been developed in recent years for heat dissipation of electronic products.
The thickness of the conventional heat conducting material of the electronic product, namely the artificial graphite, is limited by a PI film which is a raw material, but cannot exceed 100 mu m at present, and along with the updating of the electronic product, particularly a chip, the use power is gradually improved, the requirement on heat dissipation is also higher and higher, and a thicker heat dissipation material is required to increase the thickness to improve the heat flux on the premise of keeping the current heat conductivity, so that better soaking effect is achieved.
The graphene oxide film obtained by coating the graphene oxide slurry produced by the Hummer's method is difficult to break through more than 100 μm of a single layer due to the limitation of the properties of the graphene oxide film, so that the graphene oxide slurry needs to be modified to adapt to the production of a graphene oxide thick film material.
Disclosure of Invention
The invention aims to provide composite graphene slurry with self-assembly property and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a composite graphene slurry with self-assembly properties, the formulation comprising: the weight ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20:1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; step two, selecting a formula; thirdly, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, graphene oxide reactant which is prepared by a Hummer's method and cleaned is 3% -10% in solid content, viscosity is 100000-1000000cp, and the graphene oxide reactant is added into a planetary disperser and stirred for 1-4 hours to obtain graphene oxide slurry;
wherein in the second step, the solute of the self-assembly aid solution comprises one or more of the following compounds: epoxy resins, polyetherimides, hydroxypropyl methylcellulose ethers, and polyethylenimines; different combinations of solutes and solvents;
in the third step, after the concentration is calculated, pouring a proper amount of self-assembly auxiliary agent solution described in the second step into a beaker, carefully placing the self-assembly auxiliary agent solute binder solute described in the second step, stirring for 0.5-3h by using a magnetic stirrer, stirring for 0.5-1h by using a high-speed dispersing machine after the solute is completely dissolved in the solvent, then placing the completely dispersed binder solution into a defoaming machine for defoaming for 1-2h, and obtaining the self-assembly auxiliary agent for standby after the defoaming is completed;
in the fourth step, adding the self-assembly auxiliary agent obtained in the third step into the graphene slurry obtained in the first step, according to the different formulas of the self-assembly auxiliary agent, the ratio of the graphene oxide slurry to the self-assembly auxiliary agent is between 10-20:1, adding the graphene oxide slurry added with the self-assembly auxiliary agent into a planetary disperser, stirring for 2-4 hours, dispersing by a high-speed shearing disperser, and finally defoaming for 1-2 hours by a defoaming machine to obtain the graphene oxide composite slurry;
in the fifth step, the graphene oxide composite slurry obtained in the fourth step is dried by adopting a manual coating or a coating mode of a coating machine to obtain a graphene oxide film;
in the sixth step, the graphene oxide film material obtained in the fifth step is subjected to heat treatment, and is heated to 2800 ℃ in a staged manner, and then the graphene oxide film material is obtained after heat treatment.
According to the above technical solution, in the second step, the solvent of the self-assembly auxiliary solution may be selected from one of the following: deionized water, ammonia, ethanol, and DMF.
According to the technical scheme, in the second step, the mass concentration of the self-assembly auxiliary agent is 5-20%.
According to the technical scheme, in the fourth step, the rotating speed of the high-speed shearing dispersing machine is 4000-8000rpm.
According to the technical scheme, in the fifth step, the thickness of the graphene oxide film is 10-100 μm.
Compared with the prior art, the invention has the following beneficial effects:
1. the self-assembly auxiliary agent is added in the graphene oxide slurry stage, so that the process of adding the graphene film for lamination after coating is avoided, other special conditions, environments such as high temperature and high pressure and the like are not required, and the production efficiency is improved
2. Only a few graphene films with concentrated standard thickness are required to be produced, and the graphene films with any thickness are stacked and combined by the method, so that the production difficulty and cost of a coating link are reduced.
3. By using the graphene oxide composite slurry, the self-assembly auxiliary agent can guide the graphene oxide sheets to be regularly distributed between layers in the layer, so that the performance of a final finished product is improved, meanwhile, chemical bonds are formed between the self-assembly auxiliary agent and graphene oxide molecules, C-C bonds are reserved after the self-assembly auxiliary agent and the graphene oxide molecules undergo high-temperature thermal reduction, the graphene oxide sheets are effectively connected, a phonon heat transfer process can be performed, and compared with other modes of combining graphene films, the loss of heat conductivity between the layers is avoided to the greatest extent.
4. The binder selected in the method is a common industrial raw material, has low cost and good affinity with graphene oxide, and provides convenience for large-scale production.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a flow chart of the method of the present invention;
fig. 2 is a graph of a graphene film produced in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-2, the present invention provides a technical solution:
example 1:
a composite graphene slurry with self-assembly properties, the formulation comprising: the weight ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20:1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; step two, selecting a formula; thirdly, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 3%, the viscosity is 150000cp, and the graphene oxide reactant is added into a planetary disperser and stirred for 2 hours to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly auxiliary solution is epoxy resin; the solvent of the self-assembly auxiliary agent solution is ethanol, and the mass concentration of the self-assembly auxiliary agent is 5-20%;
in the third step, 5g of epoxy resin is taken and dissolved in 95g of ethanol, a magnetic stirrer is used for stirring for 0.5h at 500rpm, after solute is completely dissolved in solvent, a high-speed dispersing machine is used for dispersing for 0.5h at 2500rpm, then the completely dispersed binder solution is put into a defoaming machine for defoaming for 0.5h, and a self-assembly auxiliary agent with the mass concentration of 5% is obtained for standby after defoaming is completed;
in the fourth step, adding 100g of the self-assembly auxiliary agent obtained in the third step into 1000g of graphene slurry, adding the graphene oxide slurry added with the self-assembly auxiliary agent into a planetary disperser, stirring for 2 hours, dispersing by a high-speed shearing disperser with the rotating speed of 6000rpm, and finally defoaming for 1 hour by a defoaming machine to obtain graphene oxide composite slurry;
in the fifth step, the graphene oxide composite slurry obtained in the fourth step is manually coated by using a bar coater, and dried for 2 hours at the temperature of 80 ℃ to obtain two graphene oxide films with 350mm, 250mm and 20 mu m;
in the sixth step, the graphene oxide films obtained in the fifth step are stacked together, placed in a carbonization furnace to be heated to 1000 ℃, and then placed in a graphitization furnace to be heated to 2800 ℃ to obtain graphene films with thickness of 350mm 250mm 40 μm.
Example 2:
a composite graphene slurry with self-assembly properties, the formulation comprising: the weight ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20:1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; step two, selecting a formula; thirdly, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 6%, the viscosity is 600000cp, and the graphene oxide reactant is added into a planetary disperser and stirred for 4 hours to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly auxiliary agent solution is hydroxypropyl methyl cellulose ether; the solvent of the self-assembly auxiliary agent solution is deionized water, and the mass concentration of the self-assembly auxiliary agent is 5-20%;
in the third step, 20g of hydroxypropyl methyl cellulose ether is taken and dissolved in 180g of deionized water, a magnetic stirrer is used for stirring for 2 hours at 600rpm, after solute is completely dissolved in solvent, a high-speed dispersing machine is used for dispersing for 1 hour at 2000rpm, then a completely dispersed binder solution is placed into a defoaming machine for defoaming, and a self-assembly auxiliary agent with the mass concentration of 10% is obtained for standby after the defoaming is completed;
in the fourth step, 200g of self-assembly auxiliary agent obtained in the third step is added into 4000g of graphene slurry, the graphene oxide slurry added with the self-assembly auxiliary agent is put into a planetary disperser, stirred for 4 hours, then dispersed by a high-speed shearing disperser with the rotating speed of 8000rpm, and finally defoamed for 2 hours by a defoaming machine, so as to obtain graphene oxide composite slurry;
in the fifth step, the graphene oxide composite slurry obtained in the fourth step is coated by using a doctor blade coater, and dried for 2 hours at the temperature of 80 ℃ to prepare four graphene oxide films with the thickness of 450mm and 100 mu m;
in the sixth step, the graphene oxide films obtained in the fifth step are stacked together, placed in a carbonization furnace to be heated to 1000 ℃, and then placed in a graphitization furnace to be heated to 2800 ℃ to obtain the graphene film material with 450mm 400 μm.
The graphene film materials obtained in the above examples were respectively tested, and the obtained data are shown in the following table:
| example 1 | Example 2 | |
| Density of | 2.1g/cm 3 | 2.1g/cm 3 |
| Coefficient of thermal conductivity | 1500W/m·K | 1500W/m·K |
Based on the above, the invention has the advantages that the graphene film material is produced in a stacking way, so that the graphene film material with the required thickness is produced, the production difficulty and cost of a coating link are reduced, meanwhile, the self-assembly auxiliary agent is added, the process of attaching the graphene film after coating is avoided, other special conditions, environments such as high temperature and high pressure and the like are not needed, the production efficiency is improved, meanwhile, the binder selected in the production process is a common industrial raw material, the cost is low, the affinity with graphene oxide is good, and the convenience is provided for large-scale production.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the graphene film material comprises the following steps of firstly, preparing at one time; step two, selecting a formula; thirdly, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction; the method is characterized in that:
in the first step, graphene oxide reactant which is prepared by a Hummer's method and cleaned is 3% -10% in solid content, viscosity is 100000-1000000cp, and the graphene oxide reactant is added into a planetary disperser and stirred for 1-4 hours to obtain graphene oxide slurry;
in the second step, the self-assembly auxiliary solution comprises a solute and a solvent, wherein the solute is one or more of the following compounds: epoxy resins, polyetherimides, hydroxypropyl methylcellulose ethers, and polyethylenimines; the solvent is one of the following compounds: deionized water, ammonia, ethanol and DMF; depending on the self-assembling aid solution, different combinations of solutes and solvents;
in the third step, after the concentration is calculated, pouring a proper amount of self-assembly auxiliary solvent described in the second step into a beaker, carefully placing the self-assembly auxiliary solute described in the second step, stirring for 0.5-3h by using a magnetic stirrer, stirring for 0.5-1h by using a high-speed dispersing machine after the solute is completely dissolved in the solvent, then placing the completely dispersed self-assembly auxiliary into a defoaming machine for defoaming for 1-2h, and obtaining the self-assembly auxiliary after defoaming is finished for later use;
in the fourth step, adding the self-assembly auxiliary agent obtained in the third step into the graphene oxide slurry obtained in the first step, according to the different formulas of the self-assembly auxiliary agent, the ratio of the graphene oxide slurry to the self-assembly auxiliary agent is between 10-20:1, adding the graphene oxide slurry added with the self-assembly auxiliary agent into a planetary disperser, stirring for 2-4h, dispersing by a high-speed shearing disperser, and finally defoaming for 1-2h by a defoaming machine to obtain the composite graphene slurry with self-assembly properties;
in the fifth step, the composite graphene slurry obtained in the fourth step is dried by adopting a manual coating or a coating mode of a coating machine to obtain a graphene oxide film;
in the sixth step, stacking the graphene oxide films obtained in the fifth step, performing heat treatment, heating to 2800 ℃ in stages, and performing heat treatment to obtain the graphene film material.
2. The preparation method of the graphene film material according to claim 1, which is characterized by comprising the following steps: in the second step, the mass concentration of the self-assembly auxiliary agent is 5-20%.
3. The preparation method of the graphene film material according to claim 1, which is characterized by comprising the following steps: in the fourth step, the rotating speed of the high-speed shearing dispersing machine is 4000-8000rpm.
4. The preparation method of the graphene film material according to claim 1, which is characterized by comprising the following steps: in the fifth step, the thickness of the graphene oxide film is 10-100 μm.
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