CN110294469A - A kind of three-dimensional graphene composite material and preparation method thereof - Google Patents
A kind of three-dimensional graphene composite material and preparation method thereof Download PDFInfo
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- CN110294469A CN110294469A CN201810241330.8A CN201810241330A CN110294469A CN 110294469 A CN110294469 A CN 110294469A CN 201810241330 A CN201810241330 A CN 201810241330A CN 110294469 A CN110294469 A CN 110294469A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The present invention relates to a kind of three-dimensional graphene composite materials and preparation method thereof, the preparation includes: after mixing graphene oxide, water soluble phenol resin and water, 120~200 DEG C hydro-thermal reaction 3~24 hours, obtain three-dimensional grapheme hydrogel, washing and drying are placed in inert atmosphere, it is heat-treated 0.5~10 hour at 400~1000 DEG C, obtains three-dimensional graphene composite material.
Description
Technical field
The present invention relates to a kind of three-dimensional graphene composite materials and preparation method thereof, belong to graphene composite material preparation skill
Art field.
Background technique
From 2004 graphene (graphene) be found since, due to its excellent machinery, electricity, thermodynamic property,
Extraordinary prospect is considered to have in every field and is had wide range of applications, therefore graphene rapidly becomes green wood in recent years
The hot spot of material and the concern of new energy grade high frontier.Three-dimensional grapheme is to be assembled by two-dimensional graphene and remained two-dimentional stone
The black good physical and chemical performance of alkene, at the same also have high specific surface area, porous network structure and it is reusable the features such as.
Three-dimensional grapheme and its excellent characteristic of composite material and unique microstructure make its absorption, catalysis, sensor, heat dissipation and
Energy storage etc. is excellent in, and is expected to that practical application can be obtained.
Under the action of single graphene film is because of strong pi-pi bond, it may occur that polymerization is reunited, and graphene is so then greatly reduced
Specific surface area, and as lamella contact it is undesirable, cause the internal resistance of original high conductivity graphene larger and conductive
Property substantially reduces.In order to solve described problem, a possible solution be exactly preparation have high conductivity, high surface area,
The graphene three-dimensional structure of macroporosity.Preparing three-dimensional grapheme at present mainly includes chemical vapour deposition technique, redox
Method, hydro-thermal process method.Wherein, chemical vapour deposition technique can prepare large area, the graphene of high quality, but this method graphene and produce
It measures low, it is difficult to large-scale production；Though oxidation-reduction method has large-scale production potentiality, surface oxygen functional group is difficult thoroughly to go
It removes, will lead to serious agglomeration in preparation process, and then substantially reduce graphene specific surface area；Hydro-thermal method easily realizes the three-dimensional stone of preparation
Black alkene, and simple process.However, hydro-thermal process method also will appear the problems such as porosity is small, and conductivity is lower, and thermal conductivity is poor.
To further increase three-dimensional grapheme physical and chemical performance, it is necessary to carry out regulation modification to three-dimensional grapheme, this is also for three
Tieing up graphene next step large-scale application has important promotion meaning.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide one kind to have highly conductive, high thermal conductivity and good adsorption properties
Three-dimensional graphene composite material and preparation method thereof.
On the one hand, the present invention provides a kind of preparation methods of three-dimensional graphene composite material, comprising:
By graphene oxide, water soluble phenol resin and water mix after, 120~200 DEG C hydro-thermal reaction 3~24 hours, obtain
Three-dimensional grapheme hydrogel, washed and drying are placed in inert atmosphere, and it is small that 0.5~10 is heat-treated at 400~1000 DEG C
When, obtain three-dimensional graphene composite material.
The present invention is compound with graphene oxide by water soluble phenol resin, and (temperature is 120~200 DEG C to hydrothermal condition, the time
Be 3~24 hours) under form three-dimensional grapheme hydrogel, be heat-treated (temperature 400 under an inert atmosphere after washed and dry
~1000 DEG C, 0.5~10 hour time), obtain three-dimensional graphene composite material.Wherein, phenolic resin has macromolecular three-dimensional
The characteristics of network structure and high crosslink density, inter-atomic bond energy are high, and intermolecular cohesion is big, have after pyrolysis high fixing carbon and at
The high characteristic of carbon structure intensity.When under hydrothermal conditions, water soluble phenol resin and the crosslinking of graphene oxide hydro-thermal are formed three-dimensional
Reticular structure improves three-dimensional grapheme specific surface area.In follow-up heat treatment process, phenolic resin pyrolysis has high fixing carbon
And the characteristic high at carbon structure intensity, be conducive to the conduction for improving three-dimensional grapheme, thermally conductive, absorption property.
Preferably, the graphene oxide is prepared using modified Hummers method.
Preferably, the mass ratio of the water soluble phenol resin and graphene oxide be 1~30wt%, preferably 10~
20wt%.
Preferably, the drying is vacuum drying, natural drying, freeze-drying or supercritical drying.
Also, temperature is -44~-78 DEG C (preferably -50~-70 DEG C) preferably, the air pressure of the freeze-drying is less than 2Pa,
Time is 24~72 hours；The vacuum drying vacuum degree is less than -0.1MPa, and temperature is 60~90 DEG C, and the time is 12~48
Hour.
Preferably, the inert atmosphere is argon gas or/and nitrogen.
On the other hand, the present invention also provides a kind of three-dimensional grapheme composite woods prepared according to above-mentioned preparation method
Material, the density of the three-dimensional graphene composite material are 0.1~600mg/cm3, 100~800m of specific surface area2/ g, square resistance
For 0.5~8.0 Ω/sq-1。
Beneficial effects of the present invention:
The graphene oxide and water soluble phenol resin after evenly mixing, crosslink, shape both in hydrothermal reaction process
At tridimensional network, improves three-dimensional grapheme specific surface area and improve three-dimensional grapheme specific surface area.Moreover, water soluble phenolic resin
Rouge be heat-treated under inert gas protection can be pyrolyzed to be formed with high fixing carbon and high intensity at carbon structure, and companion in being heat-treated
As graphene defect reduces, be conducive to the conduction for improving three-dimensional grapheme, thermally conductive, absorption property.In addition, using water-soluble phenolic
Urea formaldehyde modified graphene can not only replace a large amount of organic molten water soluble molecules to reduce environmental pollution with water, reduce cost, and
And be conducive to further promote three-dimensional grapheme physics, chemical property；
The present invention simply utilizes hydro-thermal method to combine heat treatment, and preparation cost is low, and preparation method is simple, and preparation process is easily-controllable, system
Standby raw material only need water soluble phenol resin, graphene oxide and water, it is not necessary that other reagents are added, and can prepare and lead
Electricity, thermally conductive, the three-dimensional graphene composite material that absorption property etc. is had excellent performance, the material can be applied to energy storage, and environment is inhaled
It is attached, the fields such as high thermal conductivity.
Detailed description of the invention
Fig. 1 shows three-dimensional graphene composite material photomacrograph prepared by embodiment 1；
Fig. 2 shows three-dimensional graphene composite material stereoscan photographs prepared by embodiment 2.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention mixes water soluble phenol resin and graphene oxide solution, the inert atmosphere after hydro-thermal reaction, dry
Lower heat treatment, obtains the three-dimensional graphene composite material.Specifically, graphite oxide is prepared using modified Hummers method
Alkene is raw material, then with the aqueous solution with water soluble phenol resin, passes through water soluble phenol resin in hydro-thermal reaction and oxidation stone
Black alkene is cross-linked to form tridimensional network, under inert gas shielding phenolic resin be pyrolyzed to obtain with high fixing carbon and it is high-intensitive at
Carbon structure is conducive to improve three-dimensional grapheme thermal conductivity.It is reduced in subsequent heat treatment along with graphene defect, from
And it is prepared with excellent conductive, thermally conductive, absorption property three-dimensional graphene composite material.
The present invention prepares three-dimensional graphene composite material, this method using graphene oxide and water soluble phenol resin are compound
Preparation process is simple and preparation process is easy to control.Illustrate to following exemplary three-dimensional graphene composite material provided by the invention
Preparation method.
The preparation of graphene oxide.Using the graphene oxide solution of modified Hummers method preparation.Gained graphite oxide
The concentration of alkene solution can be 0.1~20mg/ml.It should be noted that selecting graphene oxide to be not limited only to above method system in the present invention
It is standby to obtain.
Graphene oxide solution and water soluble phenol resin aqueous solution are uniformly mixed into (water soluble phenol resin and oxidation stone
The mass ratio of black alkene is 1~30wt%), it is put into hydrothermal reaction kettle, (is obtained within hydro-thermal reaction 3~24 hours at 120~200 DEG C
Three-dimensional grapheme hydrogel), then it is washed and dry, obtain response sample.When water soluble phenol resin and graphene oxide
When mass ratio is more than 30wt%, the density of gained three-dimensional graphene composite material increases, and specific surface area reduces, and square resistance
Increase.The drying means includes but is not limited to directly vacuum drying, natural drying, freeze-drying or supercritical drying.Institute
Cleaning solution used in the washing stated is water, acetone, ethyl alcohol, the one or more kinds of mixtures of ether.
Response sample is heat-treated 0.5~10 hour with 400~1000 DEG C under inert atmosphere conditions, drops to room to temperature
It is taken out after temperature, obtains three-dimensional graphene composite material.The inert atmosphere is the one or two of argon gas or nitrogen.
In the present invention, the density of three-dimensional graphene composite material three-dimensional graphene composite material can be 0.1~600mg/
cm3, specific surface area can be 100~800m2/ g, square resistance can be 0.5~8.0 Ω/sq-1, there is height to adsorb, is conductive,
Thermal conduction characteristic, the material can be applied to energy storage, environment absorption, the fields such as high thermal conductivity.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 8mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Alkene is added water soluble phenol resin (water soluble phenol resin and graphene oxide mass ratio 5wt%), after mixing evenly, ultrasound 8
Hour, it is packed into 45ml hydrothermal reaction kettle, 140 DEG C are reacted 10 hours, and sample is taken out after being cooled to room temperature, and successively pass through deionization
Water, ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, at 500 DEG C at heat
Reason 6 hours, is cooled to room temperature to obtain final three-dimensional graphene composite material, the visible Fig. 1 of photomacrograph, after tested, preparation
Three-dimensional porous graphene density is 16.3mg/cm3, specific surface area 430m2/ g, square resistance are 5.2 Ω/sq-1。
Embodiment 2
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 5mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Water soluble phenol resin (water soluble phenol resin and graphene oxide mass ratio 10wt%), after mixing evenly, ultrasound is added in alkene
8 hours, it is packed into 45ml hydrothermal reaction kettle, 160 DEG C are reacted 8 hours, and sample is taken out after being cooled to room temperature, and successively pass through deionization
Water, ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, at 800 DEG C at heat
Reason 7 hours, is cooled to room temperature to obtain final three-dimensional graphene composite material, the visible Fig. 2 of microscopic appearance, scanning electron microscope
Under observe the material be three-dimensional netted material.After tested, the three-dimensional porous graphene density of preparation is 14.7mg/cm3, compare table
Area 500m2/ g, square resistance are 3.8 Ω/sq-1。
Embodiment 3
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 5mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Water soluble phenol resin (water soluble phenol resin and graphene oxide mass ratio 10wt%), after mixing evenly, ultrasound is added in alkene
8 hours, it is packed into 45ml hydrothermal reaction kettle, 180 DEG C are reacted 16 hours, and sample is taken out after being cooled to room temperature, and successively pass through deionization
Water, ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, at 900 DEG C at heat
Reason 6 hours, is cooled to room temperature to obtain final three-dimensional graphene composite material.After tested, the three-dimensional grapheme density of preparation is
9.8mg/cm3, specific surface area 560m2/ g, square resistance are 2.8 Ω/sq-1.By comparison, it was found that passing through water soluble phenol resin
With the three-dimensional graphene composite material that graphene oxide is compounded to form compared with conventional three-dimensional grapheme material (comparative example 1), tool
There are more excellent electric conductivity and higher specific surface area.
Embodiment 4
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 8mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Alkene is added water soluble phenol resin (water soluble phenol resin and graphene oxide mass ratio 15wt%), after mixing evenly, ultrasound
8 hours, it is packed into 45ml hydrothermal reaction kettle, 120 DEG C are reacted 20 hours, and sample is taken out after being cooled to room temperature, and successively pass through deionization
Water, ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, at 400 DEG C at heat
Reason 10 hours, is cooled to room temperature to obtain final three-dimensional graphene composite material.After tested, the three-dimensional grapheme density of preparation is
15.8mg/cm3, specific surface area 490m2/ g, square resistance are 3.6 Ω/sq-1。
Embodiment 5
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 8mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Alkene is added water soluble phenol resin (water soluble phenol resin and graphene oxide mass ratio 30wt%), after mixing evenly, ultrasound
8 hours, it is packed into 45ml hydrothermal reaction kettle, 140 DEG C are reacted 10 hours, and sample is taken out after being cooled to room temperature, and successively pass through deionization
Water, ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, at 500 DEG C at heat
Reason 6 hours, is cooled to room temperature to obtain final three-dimensional graphene composite material.After tested, the three-dimensional porous graphene density of preparation
For 19.3mg/cm3, specific surface area 470m2/ g, square resistance are 5.1 Ω/sq-1。
Comparative example 1
Graphene oxide preparation: the graphene oxide for using modified Hummers method to prepare concentration as 5mg/ml, under room temperature
It stirs and is ultrasonically treated 10 hours, graphene oxide solution that treated is placed spare.Take the graphite oxide of the above-mentioned preparation of 30ml
Alkene is packed into 45ml hydrothermal reaction kettle, and 180 DEG C are reacted 16 hours, and sample is taken out after being cooled to room temperature, and successively passes through deionized water,
Ethyl alcohol, after deionized water washing, freeze-drying.Sample after drying is heat-treated under the protection of argon gas, is heat-treated 6 at 900 DEG C
Hour, it is cooled to room temperature to obtain final sample.After tested, the three-dimensional grapheme density of preparation is 20.1mg/cm3, specific surface area
260m2/ g, square resistance are 13 Ω/sq-1。
Comparative example 2
The water soluble phenol resin is heat-treated under the protection of argon gas, is heat-treated 6 hours, is cooled to room temperature at 900 DEG C
To final sample.The sample specific surface area 8.5m of preparation2/ g, square resistance are 21.0 Ω/sq-1。
Claims (7)
1. a kind of preparation method of three-dimensional graphene composite material characterized by comprising
By graphene oxide, water soluble phenol resin and water mix after, 120~200 DEG C hydro-thermal reaction 3~24 hours, obtain
Three-dimensional grapheme hydrogel, washing and drying are placed in inert atmosphere, and it is small that 0.5~10 is heat-treated at 400~1000 DEG C
When, obtain three-dimensional graphene composite material.
2. preparation method according to claim 1, which is characterized in that the graphene oxide is using modified Hummers
Method is prepared.
3. the preparation method according to right 1 or 2, which is characterized in that the water soluble phenol resin and graphene oxide
Mass ratio is 1~30 wt%, preferably 10~20wt%.
4. the preparation method according to any one of right 1-3, which is characterized in that the drying is vacuum drying, does naturally
Dry, freeze-drying or supercritical drying.
5. according to preparation method described in right 4, which is characterized in that the air pressure of the freeze-drying is less than 2Pa, and temperature is -44
~-78 DEG C, the time is 24~72 hours；The vacuum drying vacuum degree is less than -0.1MPa, and temperature is 60~90 DEG C, the time
It is 12~48 hours.
6. the preparation method according to any one of right 1-5, which is characterized in that the inert atmosphere is argon gas or/and nitrogen
Gas.
7. a kind of three-dimensional graphene composite material of the preparation of the preparation method according to any one of right 1-6, feature exist
In the density of the three-dimensional graphene composite material is 0.1~600 mg/cm3, 100~800 m of specific surface area2/ g, square electricity
Resistance is 0.5~8.0/sq-1。
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Cited By (3)
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| CN113097604A (en) * | 2021-04-02 | 2021-07-09 | 信骅(上海)器材有限公司 | Special graphene heat dissipation assembly with low thermal resistance, high compressibility and buffering function for electric automobile and preparation method of special graphene heat dissipation assembly |
| CN113911382A (en) * | 2021-11-02 | 2022-01-11 | 中国商用飞机有限责任公司 | Air cavity shelf, method for manufacturing air cavity shelf and electronic equipment shelf |
| CN115818628A (en) * | 2022-09-30 | 2023-03-21 | 中国人民解放军陆军装甲兵学院 | Three-dimensional graphene foam, preparation method and application thereof, and wave-absorbing material |
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Application publication date: 20191001 |