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CN111205513B - Graphene-based heat-conducting composite filler and preparation method and application thereof - Google Patents

Graphene-based heat-conducting composite filler and preparation method and application thereof Download PDF

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CN111205513B
CN111205513B CN202010182875.3A CN202010182875A CN111205513B CN 111205513 B CN111205513 B CN 111205513B CN 202010182875 A CN202010182875 A CN 202010182875A CN 111205513 B CN111205513 B CN 111205513B
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graphene
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silver
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conducting composite
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CN111205513A (en
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许超
王祥
庞旗旗
涂丽园
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Xiamen Badou New Material Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/00Use of inorganic substances as compounding ingredients
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    • C08K3/04Carbon
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    • C08K3/08Metals
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0806Silver
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

According to the invention, high-quality graphene is prepared by a solid-phase microwave reduction method, and is dry-blended with silver acetate powder, so that the high-purity nano-silver loaded graphene-based heat-conducting composite filler is rapidly prepared by the solid-phase microwave reduction method. The nano silver loaded on the surface of the graphene obtained by the preparation method disclosed by the invention is uniform in distribution and good in crystallinity, and the preparation method disclosed by the invention is efficient in process, safe and environment-friendly and the product is pure. The nano-silver loaded graphene-based heat-conducting composite filler can be used in the field of heat-conducting materials, can effectively improve the heat-radiating efficiency of the surface of an electronic device, and has a good industrial application prospect.

Description

Graphene-based heat-conducting composite filler and preparation method and application thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a graphene-based heat-conducting composite filler and a preparation method and application thereof.
Background
Graphene is a compound represented by sp2The hybrid carbon atoms are mutually connected to form a two-dimensional carbon material with a honeycomb lattice structure, the thermal conductivity of graphene is 5300W/(m.K), and the high thermal conductivity of the graphene is derived from the perfect lattice structure and is mainly transmitted through phonons. Researches show that the graphene can effectively improve the thermal conductivity of the polymer matrix and has wide application prospects in the field of heat conduction materials. The graphene has high thermal conductivity, and the specific surface area of the graphene is very high, so that the graphene is fully filled in the material, and the heat dissipation surface area of the material can be increased. However, since the graphene surface has no functional group, the chemical stability is high, the compatibility in the material polymer matrix is poor, and the problems of stacking and agglomeration are easily caused, the advantages of high specific surface area and strong heat conductivity are difficult to exert. The nano silver also has higher thermal conductivity which can reach 397W/(m.K), can be used as a load to be modified on the surface of graphene, and can be used for functionally modifying the graphene, and has the following advantages: as a spacer, the interlayer spacing between graphene sheets can be effectively increased, the graphene sheets are prevented from being folded back,the dispersibility of the material in a polymer matrix is improved; the graphene is loaded between the graphene layers, so that a bridging effect is achieved, a good vertical heat conduction path structure can be formed, and the heat conductivity of the composite material is improved.
The prior patent technology mentions that graphene is used as a heat-conducting filler to improve the heat-conducting property of the composite material, but the problem of dispersion of graphene in a composite material system is not solved. The related patent technology also mentions that the metal surface modified graphene is prepared by adopting a liquid phase chemical reduction method, nano metal is uniformly dispersed on the surface of the graphene, but the product obtained by liquid phase reduction still needs post-treatment, the process time is long, and the adopted hydrazine hydrate reducing agent has high toxicity and is harmful to human bodies.
Therefore, the graphene-based heat-conducting composite filler which is good in dispersibility, pure in components, efficient in process, safe and environment-friendly, and the preparation method and the application thereof are problems to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides the graphene-based heat-conducting composite filler and the preparation method and application thereof, and the graphene-based heat-conducting composite filler has the advantages of good dispersibility, pure components, high process efficiency, safety, environmental friendliness and good industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
the graphene-based heat-conducting composite filler is composed of high-quality graphene and elemental silver, and has no other impurities; the mass ratio of carbon, oxygen and silver elements in the composite filler is 68-92: 1-5: 5-30; the simple substance silver in the composite filler is silver nanoparticles, the particle size is 50-180 nm, and the silver nanoparticles are uniformly attached to the surface of the high-quality graphene and between graphene sheets.
Further, a preparation method of the graphene-based heat-conducting composite filler comprises the following specific steps:
(1) doping graphene into graphite oxide, and mixing to obtain a mixture; the graphene is a microwave sensing material; the mass ratio of the graphite oxide to the graphene is 1: 0.1-0.2;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas containing argon and hydrogen, and controlling the microwave reaction power and time to obtain high-quality graphene; the volume ratio of the argon to the hydrogen is 9: 1;
(3) mixing the high-quality graphene obtained in the step (2) with silver acetate powder to obtain a mixture; the mass ratio of the high-quality graphene to the silver acetate powder is 1: 0.1-0.7;
(4) and (4) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, and controlling the microwave reaction power and time to obtain the nano-silver loaded graphene-based heat-conducting composite filler.
Further, the carbon-oxygen ratio of the graphite oxide in the step (1) is 2-3, and the carbon-oxygen ratio of the graphene is 10-50.
Further, mixing in the step (1) by adopting a V-shaped mixer for 5-20 min.
Further, the microwave reaction power in the step (2) is 1000-1600W, and the microwave reaction time is 1-5 min.
Further, mixing in the step (3) by adopting a V-shaped mixer for 5-20 min.
Further, the microwave reaction power in the step (4) is 400-1000W, and the microwave reaction time is 5-30 min.
Further, the application of the graphene-based heat-conducting composite filler in heat-conducting materials.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the interlayer spacing of graphene sheets is increased by introducing silver nanoparticles into the surface of graphene, the graphene filler is effectively prevented from being folded back in a matrix, the dispersibility of the graphene filler in the matrix of the composite material is increased, and the advantage of high specific surface area is kept; the graphene sheets are bridged up and down to play a good role of a heat conduction bridge; through the synergistic effect of metal particles with different sizes and two-dimensional sheet graphene, an efficient heat conduction path structure is constructed, and the application of the efficient heat conduction path structure in heat conduction materials is realized;
(2) compared with the traditional liquid phase chemical method, the method adopts the solid phase microwave method to prepare the nano silverThe loaded graphene-based heat-conducting composite filler has a pure product and good crystallinity, and has no other impurity phase; thermal degradation of silver acetate under microwave heating condition to generate nano silver, acetic acid and CO2(ii) a Acetic acid and CO2The metal nanoparticles can escape in a gas form, graphene is used as a substrate, metal atoms are migrated to nucleation sites through self-induction to aggregate and grow up to generate metal nanoparticles, the metal nanoparticles are independently distributed and do not aggregate, the particle size distribution is uniform, the crystallinity is good, and the purity is high;
(3) compared with the traditional liquid phase chemical method, the method has the problems of toxic solvent, long reaction time and the like; the preparation method disclosed by the invention has the advantages that the graphene-based heat-conducting composite filler loaded with nano-silver is prepared by adopting a solid-phase microwave method, a solvent and a reducing agent are not required, the process is efficient, the safety and the environmental friendliness are realized, and the industrial application prospect is good.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is an SEM image of a graphene-based thermally conductive composite filler according to example 1 of the present invention;
fig. 2 is an EDS image of the graphene-based thermally conductive composite filler of example 1 of the present invention;
fig. 3 is an attached drawing showing an XRD image of the graphene-based thermally conductive composite filler of example 1 of the present invention;
fig. 4 is an SEM image of the graphene-based thermally conductive composite filler according to example 2 of the present invention;
fig. 5 is an SEM image of the graphene-based thermally conductive composite filler according to example 3 of the present invention;
fig. 6 is an SEM image of the graphene-based thermally conductive composite filler according to example 4 of the present invention;
fig. 7 is an SEM image of the graphene-based thermally conductive composite filler of comparative example 2 according to 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.
Example 1
A preparation method of a graphene-based heat-conducting composite filler comprises the following specific steps:
(1) doping 1g of graphene (carbon-oxygen ratio is 10) into 10g of graphite oxide (carbon-oxygen ratio is 2), and blending by adopting a V-shaped mixer for 10min to obtain a mixture of the two;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas of argon and hydrogen (the volume ratio is 9: 1), controlling the microwave reaction power to be 1600W, and keeping the microwave reaction power for 1min to obtain high-quality graphene;
(3) blending 10g of high-quality graphene obtained in the step (2) and 1.2g of silver acetate by using a V-shaped mixer for 5 min;
(4) and (3) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, controlling the microwave reaction power to be 1000W, and controlling the microwave reaction power to be 5min to obtain the nano-silver loaded graphene-based heat-conducting composite filler, and observing under SEM (scanning electron microscope), wherein the result is shown in figure 1.
As can be seen from fig. 1, the graphene sheet is thin, translucent yarn-shaped, and has wrinkles; the silver nanoparticles are about 50-80 nm in size, independently distributed on the surface of graphene, do not agglomerate, and are uniformly attached to the surface of the graphene and between graphene sheets.
EDS analysis was performed on the graphene-based thermally conductive composite filler, and the results are shown in fig. 2.
As can be seen from FIG. 2, the spectrogram contains three elements of carbon, oxygen and silver through energy spectrum scanning, wherein the mass ratio of the elements of carbon, oxygen and silver is 89.79: 3.16: 7.05, and no other impurity elements exist, which indicates that the graphene-based heat-conducting composite filler is pure in component. XRD analysis was performed on the graphene-based thermally conductive composite filler, and the result is shown in fig. 3.
As can be seen from fig. 3, the diffraction peaks at 38.0 °, 44.2 °, 64.3 ° and 77.2 ° correspond to the (111), (200), (220) and (311) crystal planes of silver, respectively, and the diffraction peak at 26 ° corresponds to the (002) crystal plane of graphene, and no other impurity peak is present in the figure. The components of the graphene-based heat-conducting composite filler prepared by the invention are high-quality graphene and simple substance silver, and no other impurity phase exists.
Example 2
A preparation method of a graphene-based heat-conducting composite filler comprises the following specific steps:
(1) 1.3g of graphene (carbon-oxygen ratio is 20) is doped into 10g of graphite oxide (carbon-oxygen ratio is 2.3), and a V-shaped mixer is adopted for blending for 5min to obtain a mixture of the two;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas of argon and hydrogen (the volume ratio is 9: 1), controlling the microwave reaction power to be 1400W, and keeping the microwave reaction power for 2min to obtain high-quality graphene;
(3) blending 10g of high-quality graphene obtained in the step (2) and 2.8g of silver acetate by using a V-shaped mixer for 10 min;
(4) and (3) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, controlling the microwave reaction power to be 800W, and controlling the time to be 10min to obtain the nano-silver loaded graphene-based heat-conducting composite filler, and observing under SEM (scanning electron microscope), wherein the result is shown in figure 4.
As can be seen from fig. 4, the graphene sheets are thin, translucent yarn-like, and have wrinkles; the silver nanoparticles are about 60-100 nm in size, independently distributed on the surface of graphene, do not agglomerate, and are uniformly attached to the surface of the graphene and between graphene sheets.
EDS analysis is carried out on the graphene-based heat-conducting composite filler, and the result shows that the composite filler contains three elements of carbon, oxygen and silver, wherein the mass ratio of the carbon, the oxygen and the silver is 80.09: 4.64: 15.27, and no other impurity elements exist, so that the graphene-based heat-conducting composite filler sample is pure in component.
Example 3
A preparation method of a graphene-based heat-conducting composite filler comprises the following specific steps:
(1) doping 1.6g of graphene (carbon-oxygen ratio is 30) into 10g of graphite oxide (carbon-oxygen ratio is 2.6), and blending by adopting a V-shaped mixer for 15min to obtain a mixture of the two;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas of argon and hydrogen (the volume ratio is 9: 1), controlling the microwave reaction power to be 1200W, and keeping the time for 3.5min to obtain high-quality graphene;
(3) blending 10g of high-quality graphene obtained in the step (2) and 4.5g of silver acetate by using a V-shaped mixer for 15 min;
(4) and (3) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, controlling the microwave reaction power to be 600W, and controlling the microwave reaction time to be 20min to obtain the nano-silver loaded graphene-based heat-conducting composite filler, and observing under SEM (scanning electron microscope), wherein the result is shown in figure 5.
As can be seen from fig. 5, the graphene sheets are thin, translucent yarn-shaped, and have wrinkles; the silver nanoparticles are about 80-160 nm in size, are independently distributed on the surface of graphene, do not agglomerate, and are uniformly attached to the surface of the graphene and between graphene sheets.
EDS analysis is carried out on the graphene-based heat-conducting composite filler, and the result shows that the composite filler contains three elements of carbon, oxygen and silver, wherein the mass ratio of the carbon, the oxygen and the silver is 76.13: 1.95: 21.92, and no other impurity elements exist, so that the pure components of the graphene-based heat-conducting composite filler sample are shown.
Example 4
A preparation method of a graphene-based heat-conducting composite filler comprises the following specific steps:
(1) 1.9g of graphene (carbon-oxygen ratio 45) is doped into 10g of graphite oxide (carbon-oxygen ratio 2.8), and a V-shaped mixer is adopted for blending, wherein the mixing time is 20 min;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas of argon and hydrogen (the volume ratio is 9: 1), controlling the microwave reaction power to be 1000W, and keeping the microwave reaction power for 5min to obtain high-quality graphene;
(3) blending 10g of high-quality graphene obtained in the step (2) and 6.5g of silver acetate by using a V-shaped mixer for 20 min;
(4) and (3) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, controlling the microwave reaction power to be 400W, and controlling the microwave reaction power to be 30min to obtain the nano-silver loaded graphene-based heat-conducting composite filler, and observing under SEM (scanning electron microscope), wherein the result is shown in figure 6.
As can be seen from fig. 6, the graphene sheets are thin, translucent yarn-shaped, and have wrinkles; the silver nanoparticles are about 80-180 nm in size, are independently distributed on the surface of graphene, do not agglomerate, and are uniformly attached to the surface of the graphene and between graphene sheets.
EDS analysis is carried out on the graphene-based heat-conducting composite filler, and the result shows that the composite filler contains three elements of carbon, oxygen and silver, wherein the mass ratio of the carbon, the oxygen and the silver is 68.64: 2.58: 28.78, and no other impurity elements exist, so that the graphene-based heat-conducting composite filler sample is pure in components.
Comparative example 1
A preparation method of a graphene-based heat-conducting composite filler comprises the following specific steps:
(1) doping 1g of graphene (carbon-oxygen ratio is 10) into 10g of graphite oxide (carbon-oxygen ratio is 2), and blending by adopting a V-shaped mixer for 10min to obtain a mixture of the two;
(2) and (2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas of argon and hydrogen (the volume ratio is 9: 1), controlling the microwave reaction power to be 1600W, and keeping the microwave reaction power for 1min to obtain the high-quality graphene.
Comparative example 2
The difference between the preparation method of the graphene-based heat-conducting composite filler and the embodiment 4 is that 9g of silver acetate (the mass ratio of the high-quality graphene to the silver acetate powder is 1: 0.9) is added in the step (3), and the other preparation steps are consistent.
When the graphene-based heat-conducting composite filler is observed under an SEM (scanning electron microscope), as can be seen from figure 7, the size of the silver nanoparticles is increased to 150-300 nm along with the further increase of the addition amount of the silver acetate powder, and an agglomeration phenomenon occurs.
EDS analysis is carried out on the graphene-based heat-conducting composite filler, and the result shows that the composite filler contains three elements of carbon, oxygen and silver, wherein the mass ratio of the carbon, the oxygen and the silver is 60.31: 3.59: 36.10.
The heat-conducting composite filler described in the embodiments 1-4, the comparative examples 1 and 2 is prepared into a composite material, and the preparation formula comprises the following components in parts by weight: 97 parts of epoxy resin (E-44), 5 parts of heat-conducting composite filler and 48 parts of curing agent (R3609).
The thermal conductivity lambda of the obtained composite material is measured by adopting a laser induced thermal analyzer indirect method: λ ═ α × cpX ρ; the thermal diffusion coefficient alpha is measured by adopting a laser thermal conductivity instrument, and the specific requirements refer to GB/T22588-2008; the density rho is calculated by the ratio of the mass to the volume of the composite material sample; specific heat capacity cpMeasured by a differential scanning calorimeter by a sapphire method, and the specific requirement is that GB/T19466.4-2016 is referred.
The results of the thermal conductivity test of the composite material are shown in table 1.
Table 1 results of thermal conductivity test of composite materials
Figure BDA0002413171690000071
Note: the blank is a pure epoxy (E-44) composite without any thermally conductive filler added.
Compared with the test results of the examples 1-4 and the blank examples, the graphene-based heat-conducting composite filler obtained by the invention can obviously improve the heat-conducting property of the composite material; as shown by comparison of test results of examples 1-4 and comparative example 1, the thermal conductivity of the composite material can be effectively improved by adopting the nano-silver-loaded modified graphene thermal conductive filler; as can be seen from the comparison of the test results of example 4 and comparative example 2, the silver particle size in the heat-conducting composite filler is increased due to the excessive addition of silver acetate, so that the aggregation phenomenon occurs, and the heat-conducting property of the prepared composite material is reduced.
According to the invention, high-quality graphene is prepared by a solid-phase microwave reduction method, and is dry-blended with silver acetate powder, so that the high-purity nano-silver loaded graphene-based heat-conducting composite filler is rapidly prepared by the solid-phase microwave reduction method. The nano silver loaded on the surface of the graphene obtained by the preparation method disclosed by the invention is uniform in distribution and good in crystallinity, and the preparation method disclosed by the invention is efficient in process, safe and environment-friendly and the product is pure. The nano-silver loaded graphene-based heat-conducting composite filler can be used in the field of heat-conducting materials, can effectively improve the heat-radiating efficiency of the surface of an electronic device, and has a good industrial application prospect.
The previous description of the disclosed 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. The graphene-based heat-conducting composite filler is characterized by consisting of high-quality graphene and elemental silver, and no other impurities; the mass ratio of carbon, oxygen and silver elements in the composite filler is 68-92: 1-5: 5-30; in the composite filler, the simple substance silver is silver nanoparticles, the particle size is 50-180 nm, and the simple substance silver is uniformly attached to the surface of the high-quality graphene and between graphene sheets;
the preparation method of the graphene-based heat-conducting composite filler comprises the following steps:
(1) doping graphene into graphite oxide, and mixing to obtain a mixture; the graphene is used as a microwave sensing material; the mass ratio of the graphite oxide to the graphene is 1: 0.1-0.2;
(2) placing the mixture obtained in the step (1) in a microwave reactor, introducing a mixed gas containing argon and hydrogen, and controlling the microwave reaction power and time to obtain high-quality graphene; the volume ratio of the argon to the hydrogen is 9: 1;
(3) mixing the high-quality graphene obtained in the step (2) with silver acetate powder to obtain a mixture; the mass ratio of the high-quality graphene to the silver acetate powder is 1: 0.1-0.7;
(4) and (4) placing the mixture obtained in the step (3) in a microwave reactor, introducing argon, and controlling the microwave reaction power and time to obtain the nano-silver loaded graphene-based heat-conducting composite filler.
2. The graphene-based heat-conducting composite filler according to claim 1, wherein the carbon-to-oxygen ratio of the graphite oxide in the step (1) is 2-3, and the carbon-to-oxygen ratio of the graphene is 10-50.
3. The graphene-based heat-conducting composite filler according to claim 2, wherein the mixing in step (1) is performed by a V-shaped mixer for 5-20 min.
4. The graphene-based heat-conducting composite filler according to claim 3, wherein the microwave reaction power in the step (2) is 1000-1600W, and the microwave reaction time is 1-5 min.
5. The graphene-based heat-conducting composite filler according to claim 4, wherein the mixing in step (3) is performed by a V-shaped mixer for 5-20 min.
6. The graphene-based heat-conducting composite filler according to claim 5, wherein the microwave reaction power in the step (4) is 400-1000W, and the microwave reaction time is 5-30 min.
7. Use of the graphene-based thermally conductive composite filler according to any one of claims 1 to 6 in a thermally conductive material.
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CN104759282A (en) * 2014-12-01 2015-07-08 青岛科技大学 Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst
CN106391002A (en) * 2015-08-03 2017-02-15 北京化工大学 Nanosilver/graphene oxide composite dispersion fluid, and preparation method and application thereof
CN106903324A (en) * 2015-12-22 2017-06-30 湖南利德电子浆料股份有限公司 A kind of preparation method of Graphene-nano silver dispersion

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KR101765586B1 (en) * 2015-08-25 2017-08-07 현대자동차 주식회사 Graphene-containing organic-inorganic hybrid coating film, and method for preparing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104759282A (en) * 2014-12-01 2015-07-08 青岛科技大学 Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst
CN106391002A (en) * 2015-08-03 2017-02-15 北京化工大学 Nanosilver/graphene oxide composite dispersion fluid, and preparation method and application thereof
CN106903324A (en) * 2015-12-22 2017-06-30 湖南利德电子浆料股份有限公司 A kind of preparation method of Graphene-nano silver dispersion

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