CN112723345A - 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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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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 composite graphene slurry with self-assembly property and a preparation method thereof, wherein the formula comprises the following components: the graphene oxide slurry and the self-assembly auxiliary agent are mixed, and 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; selecting a formula; step three, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction; according to the method, graphene oxide reactants which are prepared and cleaned by a Hummer's method are taken, the solid content of the graphene oxide reactants is 3% -10%, the graphene film materials with any required thickness are formed by stacking, the production difficulty and cost of a coating link are reduced, and meanwhile, the selected binder is a common industrial raw material, so that the cost is low, the affinity with graphene oxide is good, and convenience is brought to large-scale production.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to composite graphene slurry with a self-assembly property and a preparation method thereof.
Background
Since the acquisition of graphene in 2004, graphene has attracted attention due to its ultra-high thermal conductivity (-5300W/m · K), and in recent years, a method and a product for preparing a graphene thermal conductive film based on a redox reaction of graphene have been developed for heat dissipation of electronic products.
The thickness of the current commonly used heat conducting material of electronic products, namely artificial graphite, is limited by a raw material PI film, the thickness of the current commonly used heat conducting material of electronic products cannot exceed 100 mu m at present, the using power is gradually improved along with the updating of electronic products, particularly chips, the requirement on heat dissipation is higher and higher, the thickness of the heat conducting material is increased to improve the heat flux on the premise of keeping the current heat conductivity coefficient, and a better heat equalizing 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 present invention is directed to a composite graphene slurry with self-assembly property and a preparation method thereof, so as to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: a composite graphene slurry with self-assembly properties, the formula comprising: the graphene oxide slurry and the self-assembly auxiliary agent are mixed according to a weight ratio of 10-20: 1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; selecting a formula; step three, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, taking the graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 3% -10%, the viscosity is 100000-1000000cp, and adding the graphene oxide reactant into a planetary dispersion machine to stir for 1-4h to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly auxiliary agent solution comprises one or more of the following compounds: epoxy resins, polyetherimides, hydroxypropyl methyl cellulose ethers, and polyethyleneimines; depending on the different combinations of solute and solvent;
after the concentration is calculated in the third step, pouring a proper amount of the self-assembly aid solution described in the second step into a beaker, carefully placing the solute of the self-assembly aid solute described in the second step into the beaker, stirring the mixture for 0.5 to 3 hours by using a magnetic stirrer, after the solute is completely dissolved in the solvent, stirring the mixture for 0.5 to 1 hour by using a high-speed dispersion machine, then placing the completely dispersed binder solution into a defoaming machine for defoaming for 1 to 2 hours, and obtaining the self-assembly aid for later use after defoaming is completed;
adding the self-assembly auxiliary agent obtained in the step three into the graphene slurry obtained in the step one, wherein the ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20: 1 according to different formulas of the self-assembly auxiliary agent, adding the graphene oxide slurry added with the self-assembly auxiliary agent into a planetary dispersing machine, stirring for 2-4h, dispersing by a high-speed shearing dispersing machine, and finally defoaming for 1-2h 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 dried by adopting a manual coating or coating mode of a coating machine to prepare a graphene oxide film;
in the sixth step, the graphene oxide film obtained in the fifth step is subjected to heat treatment, the temperature is raised in stages and finally the graphene oxide film is heated to 2800 ℃, and then the graphene oxide film is subjected to heat treatment.
According to the above technical solution, in the second step, the solvent of the self-assembly auxiliary solution may be one of the following solvents: 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 above technical scheme, in the fourth step, the rotating speed of the high-speed shearing disperser is 4000-8000 rpm.
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 additionally adding a graphene film for lamination after coating is avoided, other special conditions and environments such as high temperature and high pressure are not required, and the production efficiency is improved
2. Only a few concentrated graphene films with standard thickness need to be produced, and the graphene films with any thickness are stacked and combined by the method, so that the production difficulty and the 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 arranged in layers and between layers, 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 can be reserved after high-temperature thermal reduction, the graphene sheets are effectively connected, a phonon heat transfer process can be carried out, and compared with other modes of combining graphene films, the loss of heat conductivity between layers is avoided to the greatest extent.
4. The binder selected in the method is common industrial raw materials, has low cost and good affinity with graphene oxide, and provides convenience for large-scale production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a method of the present invention;
fig. 2 is a diagram of the graphene film produced in example 1 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. 1-2, the present invention provides a technical solution:
example 1:
a composite graphene slurry with self-assembly properties, the formula comprising: the graphene oxide slurry and the self-assembly auxiliary agent are mixed according to a weight ratio of 10-20: 1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; selecting a formula; step three, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, taking a graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 3%, and the viscosity of the graphene oxide reactant is 150000cp, and adding the graphene oxide reactant into a planetary dispersion machine to stir for 2 hours to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly auxiliary agent 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, a high-speed dispersion machine is used for dispersing for 0.5h at 2500rpm after solute is completely dissolved in the solvent, then the completely dispersed binder solution is placed into a defoaming machine for defoaming for 0.5h, and the self-assembly auxiliary agent with the mass concentration of 5% is obtained for standby application after defoaming;
in the fourth step, 100g of the self-assembly auxiliary obtained in the third step is added into 1000g of graphene slurry, the graphene oxide slurry added with the self-assembly auxiliary is put into a planetary dispersion machine, stirred for 2 hours, then dispersed by a high-speed shearing dispersion machine, the rotating speed of the high-speed shearing dispersion machine is 6000rpm, and finally defoamed 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 taken, a wire bar coater is used for manually coating the graphene oxide composite slurry, and the graphene oxide composite slurry is dried for 2 hours at the temperature of 80 ℃ to obtain two graphene oxide films with the thickness of 350mm x 250mm x 20 microns;
and in the sixth step, the graphene oxide films obtained in the fifth step are stacked together, placed in a carbonization furnace and heated to 1000 ℃, and then placed in a graphitization furnace and heated to 2800 ℃ to obtain the graphene film material with the thickness of 350mm x 250mm x 40 mu m.
Example 2:
a composite graphene slurry with self-assembly properties, the formula comprising: the graphene oxide slurry and the self-assembly auxiliary agent are mixed according to a weight ratio of 10-20: 1.
A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; selecting a formula; step three, secondary preparation; step four, preparing for three times; step five, coating and stacking; step six, thermal reduction;
in the first step, taking a graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 6%, and the viscosity of the graphene oxide reactant is 600000cp, adding the graphene oxide reactant into a planetary dispersion machine, and stirring for 4 hours to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly aid 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 dissolved in 180g of deionized water, a magnetic stirrer is used for stirring for 2 hours at 600rpm, after the solute is completely dissolved in the solvent, a high-speed dispersion machine is used for dispersing for 1 hour at 2000rpm, then the completely dispersed binder solution is placed into a defoaming machine for defoaming, and after defoaming is completed, a self-assembly auxiliary agent with the mass concentration of 10% is obtained for standby application;
in the fourth step, 200g of the 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 dispersion machine, stirred for 4 hours, dispersed by a high-speed shearing dispersion machine, the rotating speed of the high-speed shearing dispersion machine is 8000rpm, and finally defoamed for 2 hours 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 taken, a scraper coater is used for coating the graphene oxide composite slurry, and the graphene oxide composite slurry is dried for 2 hours at the temperature of 80 ℃ to obtain four graphene oxide films with the thickness of 450mm by 100 microns;
in the sixth step, the graphene oxide films obtained in the fifth step are stacked together, placed in a carbonization furnace and heated to 1000 ℃, and then placed in a graphitization furnace and heated to 2800 ℃ to obtain the graphene film material with the thickness of 450mm to 400 mu m.
The graphene films obtained in the above embodiments are respectively detected, and the obtained data are as follows:
| example 1 | Example 2 | |
| Density of | 2.1g/cm3 | 2.1g/cm3 |
| Coefficient of thermal conductivity | 1500W/m·K | 1500W/m·K |
Based on the above, the method has the advantages that the graphene film is produced in a stacking mode, the graphene film with the required thickness is favorably produced, the production difficulty and the cost in the coating link are reduced, meanwhile, the self-assembly auxiliary agent is added, the process that the graphene film is additionally added after coating is avoided, other special conditions and environments such as high temperature and high pressure 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 the graphene oxide is good, and convenience is brought to large-scale production.
It is noted that, herein, relational terms such as first and second, and the like may be 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. Also, 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: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A composite graphene slurry with self-assembly properties, the formula comprising: graphene oxide thick liquids and self-assembly auxiliary agent, its characterized in that: the weight ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20: 1.
2. A preparation method of composite graphene slurry with self-assembly property comprises the following steps of firstly, preparing at one time; selecting a formula; step three, 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, taking the graphene oxide reactant which is prepared and cleaned by a Hummer's method, wherein the solid content of the graphene oxide reactant is 3% -10%, the viscosity is 100000-1000000cp, and adding the graphene oxide reactant into a planetary dispersion machine to stir for 1-4h to obtain graphene oxide slurry;
in the second step, the solute of the self-assembly auxiliary agent solution comprises one or more of the following compounds: epoxy resins, polyetherimides, hydroxypropyl methyl cellulose ethers, and polyethyleneimines; depending on the different combinations of solute and solvent;
after the concentration is calculated in the third step, pouring a proper amount of the self-assembly aid solution described in the second step into a beaker, carefully placing the solute of the self-assembly aid solute described in the second step into the beaker, stirring the mixture for 0.5 to 3 hours by using a magnetic stirrer, after the solute is completely dissolved in the solvent, stirring the mixture for 0.5 to 1 hour by using a high-speed dispersion machine, then placing the completely dispersed binder solution into a defoaming machine for defoaming for 1 to 2 hours, and obtaining the self-assembly aid for later use after defoaming is completed;
adding the self-assembly auxiliary agent obtained in the step three into the graphene slurry obtained in the step one, wherein the ratio of the graphene oxide slurry to the self-assembly auxiliary agent is 10-20: 1 according to different formulas of the self-assembly auxiliary agent, adding the graphene oxide slurry added with the self-assembly auxiliary agent into a planetary dispersing machine, stirring for 2-4h, dispersing by a high-speed shearing dispersing machine, and finally defoaming for 1-2h 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 dried by adopting a manual coating or coating mode of a coating machine to prepare a graphene oxide film;
in the sixth step, the graphene oxide film obtained in the fifth step is subjected to heat treatment, the temperature is raised in stages and finally the graphene oxide film is heated to 2800 ℃, and then the graphene oxide film is subjected to heat treatment.
3. The method for preparing the composite graphene paste with the self-assembly property according to claim 2, wherein: in the second step, the solvent of the self-assembly auxiliary agent solution can be selected from one of the following: deionized water, ammonia, ethanol and DMF.
4. The method for preparing the composite graphene paste with the self-assembly property according to claim 2, wherein: in the second step, the mass concentration of the self-assembly auxiliary agent is 5-20%.
5. The method for preparing the composite graphene paste with the self-assembly property according to claim 2, wherein: in the fourth step, the rotating speed of the high-speed shearing dispersion machine is 4000-8000 rpm.
6. The method for preparing the composite graphene paste with the self-assembly property according to claim 2, wherein: in the fifth step, the thickness of the graphene oxide film is 10-100 μm.
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