CN105923641A - Preparation method of high-temperature and oxidation resisting heat conduction alumina/graphene foam composite material - Google Patents
Preparation method of high-temperature and oxidation resisting heat conduction alumina/graphene foam composite material Download PDFInfo
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- CN105923641A CN105923641A CN201610269066.XA CN201610269066A CN105923641A CN 105923641 A CN105923641 A CN 105923641A CN 201610269066 A CN201610269066 A CN 201610269066A CN 105923641 A CN105923641 A CN 105923641A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The invention relates to a preparation method of a high-temperature and oxidation resisting heat conduction alumina/graphene foam composite material. The preparation method comprises the following steps: placing an aqueous solution of graphene oxide in a hydrothermal reaction kettle, heating the aqueous solution to 170-200DEG C, keeping the temperature for 10-14h, cooling the heated aqueous solution to obtain graphene hydrogel, adding pure graphene aerogel obtained after lyophilization and anhydrous aluminum chloride powder to a solvent, and carrying out ultrasonic dispersion; adding the above prepared mixed suspension to the hydrothermal reaction kettle, heating the mixed suspension to 180-300DEG C, and keeping the temperature for 10-22h; displacing the solvent of the above prepared graphene/aluminum hydroxide mixed sol with deionized water, lyophilizing the obtained sol, and calcining the lyophilized graphene/aluminum hydroxide mixed aerogel at 950-1300DEG C for 10-20h to obtain the alumina/graphene foam composite material. The thermal weight loss of the composite material is lower than 60% after the composite material is ablated at 800DEG C for 5h, and the heat conductivity of the composite material is higher than 9W/m.K.
Description
Technical field
The present invention relates to the preparation method of a kind of fire-resistant oxidation resistant heat conduction aluminium oxide/grapheme foam composite, specifically
A kind of preparation method of aluminum oxide coating layer grapheme foam.
Background technology
Since 21st century, science and technology achieves development at a high speed, and efficient conduction of heat and heat radiation become thermal management materials neck
The critical problem in territory.Such as during heat generating device arrangement works, because of the resistance of device itself, thermal resistance, electronics eddy current
Etc. effect, building up amount of heat, the position particularly high in component density, heat-dissipating space is narrow, heat flow density can spy
Not big, thus cause integral member temperature the most uneven.Major part microelectronic chip surface temperature must be maintained at relatively low water
Just can ensure that (such as silicon device 100 DEG C) under Ping that its high performance operation, many electronic units need ability at a temperature of 40～60 DEG C
Can normally work, this proposes the highest requirement to Heat Conduction Material, and can device heat production discharge in time, device heat radiation is
No uniform high-efficiency be electronic device can fast and stable work deciding factor, greatly have impact on performance and the matter of electronic equipment
Amount.In order to be derived by these heats in time, need the heat conduction that development quality is lighter, thermal conductivity is higher, performance is more excellent in a hurry
New material.
Grapheme foam is through dissolving, reduce, cross-linking a kind of loose porous spongy material obtained by Graphene.Graphite
Alkene foam is owing to having the graphitization parietal layer of regular bulk, and the obstruction of phonon conduction is less, and boundary defect is less, and heat transfer efficiency is very
Height, thus utilize grapheme foam to prepare carbon back highly heat-conductive material and become the emphasis of people's research, also occur in that similar patent
Authorize or open.State Intellectual Property Office of the People's Republic of China's grant number be CN104211057A, CN104291324A and
The patents of invention such as CN102585776A disclose and utilize graphene oxide prepare grapheme foam and utilize grapheme foam to prepare
The technology of heat conduction back bone network in phase-changing energy storage material.
Above-described patent of invention disclose only traditional grapheme foam preparation method and processing technique, only obtains applicable
Graphene heat conducting foam material under room temperature hypoxia condition.For grapheme foam Heat Conduction Material, high temperature, aerobic conditions are materials
Material plays the working environment basis of heat conduction function, therefore in grapheme foam material Graphene in higher temperature, high oxygen content
Working environment is prone to oxidation, causes graphite wafer lattice structure to produce defect, have a strong impact on the conduction of phonon, thus affect Graphene
The heat conductivility of foamed materials.After processing through Graphene reduction networking Joining Technology, Graphene directly connects with external environment
Touch, thus the most very poor (Samad Y A, Li Y, Schiffer A, the et al.Graphene of antioxygenic property under high temperature aerobic environment
Foam Developed with a Novel Two‐Step Technique for Low and High Strains and Pressure‐
Sensing Applications[J].Small,2015,11(20):2380-2385.).The public affairs such as the patent application CN104291324A of China
The grapheme foam of cloth does not the most possess the performance of fire-resistant oxidation resistant.Therefore, existing the obtained heat conduction material of published patent of invention
Expect its ruggedness far from meeting the requirement to Heat Conduction Material oxidation resistance such as mainframe computer, highly integrated electronic device, at carbon
Material is developed a kind of Heat Conduction Material with fire-resistant oxidation resistant and is particularly important on the basis of having superiority.
Summary of the invention
The present invention is directed to the defect of grapheme foam antioxygenic property prepared by existing graphene oxide, it is provided that a kind of high temperature resistant while
Grapheme foam with antioxygenic property and preparation method thereof.Its under air ambient after 800 DEG C of ablations 5 hours thermal weight loss
Less than 60%, thermal conductivity is higher than 9W/m K.As it is shown in figure 1, aluminium oxide/grapheme foam composite has micro/nano level
The foaming structure of hole, is linked the agent structure skeleton being constituted foam mutually with Graphene, and aluminium oxide is with the form of nano-scale coating
Even application is in Graphene three-dimensional foam structure skeleton surface.
The present invention is by the following technical solutions:
A kind of preparation method of fire-resistant oxidation resistant heat conduction aluminium oxide/grapheme foam composite, step is as follows:
1) graphene oxide powder is joined deionized water is stirred dispersion, configure graphene oxide water solution；
2) graphene oxide water solution is inserted in hydrothermal reaction kettle, then move to hydrothermal reaction kettle Muffle furnace is warming up to
170～200 DEG C and be incubated 10～14 hours, the Graphene hydrogel after being cooled to room temperature, reaction obtained, it is refrigerated to-30～-50 DEG C
Being dried, pure graphene aerogel lyophilizing obtained subsequently and anhydrous Aluminum chloride powder join and carry out ultrasonic disperse in solvent,
It is 4～20mg/ml to concentration of aluminum chloride, the mixing suspension containing graphene aerogel；
3) prepared mixing suspension is joined in hydrothermal reaction kettle, then hydrothermal reaction kettle is inserted in Muffle furnace be warming up to
180～300 DEG C and be incubated 10～22 hours；
4), after being cooled to room temperature, the solvent displacement of prepared Graphene/aluminium hydroxide mixed sols will in hydrothermal reaction kettle, be reacted
For deionized water, mixed sols is refrigerated to-30～-50 DEG C be dried, the Graphene/aluminium hydroxide gaseous mixture that will obtain after lyophilization
Gel is placed in tube furnace under nitrogen protection atmosphere to be calcined 10～20 hours with 950～1300 DEG C；Obtain aluminium oxide/grapheme foam
Composite.
Described step 1) preferential oxidation graphene aqueous solution concentration is 2～3mg/ml.
Described step 1) preferably with 300～600r/min stirring at normal temperature 2～3 hours.
Described step 2) preferably Graphene hydrogel is refrigerated to-30～-50 DEG C and carry out lyophilization with the air pressure of≤20Pa.
Described step 2) preferential oxidation Graphene and aluminum chloride mass ratio be 1:12～1:3.
Described step 2) preferred solvent carries out ultrasonic disperse it is the power room temperature with 200～300W ultrasonic 0.5～2 hour.
Described step 2) preferred solvent is ethanol, methanol, ethylene glycol, Nitrobenzol or ether.
Described step 4) preferably mixed sols is refrigerated to-30～-50 DEG C and carry out lyophilization with the air pressure of≤20Pa.
The aluminium oxide that the method for the present invention obtains/grapheme foam composite has the foaming structure of micro/nano level hole, compound vacuole
Foam network structure size is more than graphene aerogel, is linked the agent structure skeleton being constituted foam mutually with Graphene, such as Fig. 2 institute
Showing, graphene sheet layer is interconnected to form tridimensional network, aluminium oxide with the form even application of nano-scale coating in Graphene
Three-dimensional foam structure skeleton surface.
It is described as follows:
(1) preparation of graphene oxide: first with strong oxidizer such as concentrated sulphuric acid, concentrated nitric acid, potassium permanganate etc. by natural flake graphite
Oxidation, it is thus achieved that graphite oxide, then by graphite oxide after ultrasonic lift-off processing a period of time, it is thus achieved that graphene oxide.
(2) displacement (step 4) of Graphene/aluminium hydroxide mixed sols solvent: colloidal sol is placed in bag filter with deionized water
Dialysing 24～48 hours, make the solvent of colloidal sol be replaced by deionized water, this is very beneficial for the freezing of colloidal sol, it is simple to freeze
Dry processing is to obtain aluminium oxide/grapheme foam composite.
The aluminium oxide finally prepared/grapheme foam composite has the foaming structure of micro/nano level hole, as it is shown on figure 3,
Composite foam network structure size is significantly greater than graphene aerogel, illustrates that aluminium oxide even application is in Graphene three-dimensional network table
Face), it is linked the agent structure skeleton being constituted foam with Graphene mutually, heat pathway is provided for this foamed composite, sends out
Wave heat conduction function and provide certain flexibility for composite；Aluminium oxide with the form even application of nano-scale coating in Graphene three
Dimension foaming structure skeleton surface, provides high temperature resistant and antioxidative functional characteristic for aluminium oxide/grapheme foam composite.
Compound and the lyophilizing molding by the aluminium oxide of above step and Graphene, it is achieved that have the grapheme foam of heat conductivility with
There is aluminium oxide compound of fire-resistant oxidation resistant performance, make composite ultimately form aeroge in lyophilization, obtain
Through 800 DEG C of ablations heat conduction aluminium oxide/graphite that thermal weight loss was less than 60% in 5 hours, thermal conductivity is higher than 9W/m K under air ambient
Alkene composite foam.
Beneficial effects of the present invention: the matrix material graphene oxide of the present invention is easy to get, and aluminum oxide coating layer is the most controlled.The present invention
Middle microstructure ordering, densification and painting stratification can efficiently complete, the C-base composte material bubble with high antioxidant that can obtain
Foam, its oxidation resistance is far superior to traditional thermal conductivity graphene foam and other carbon back heat-conductive composite materials.
Accompanying drawing illustrates:
Fig. 1 is the microcosmic macroscopic view schematic diagram of Graphene of the present invention/Alumina Foam composite, including complex form and microstructure；
Fig. 2 is the scanning electron microscopic picture of three-dimensional graphene foam；
Fig. 3 is the scanning electron microscopic picture of the final Graphene/Alumina Foam composite prepared.
Detailed description of the invention
6 embodiments of the present invention are given below, are the present invention to be further illustrated rather than limits the scope of the present invention.
Embodiment 1
Graphene oxide powder is joined deionized water is stirred dispersion, with the rotating speed stirring at normal temperature 3 hours of 400r/min,
It is configured to the graphene oxide water solution that concentration is 2mg/ml.40ml graphene oxide water solution is inserted in hydrothermal reaction kettle,
Then move to hydrothermal reaction kettle Muffle furnace is warming up to 170 DEG C and is incubated 10 hours, after being cooled to room temperature, reaction is obtained
Graphene hydrogel is refrigerated to-40 DEG C and carries out lyophilization with the air pressure of 20Pa, pure Graphene airsetting lyophilizing obtained subsequently
The anhydrous Aluminum chloride powder of glue and 0.7g joined and carries out ultrasonic disperse in ethanol, with ultrasonic 2 hours of the power room temperature of 300W.
Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then hydrothermal reaction kettle is inserted Muffle
Stove is warming up to 200 DEG C and is incubated 14 hours.After being cooled to room temperature, prepared Graphene/hydrogen-oxygen in hydrothermal reaction kettle, will be reacted
Change aluminum mixed sols to be placed in bag filter with deionized water dialysis 24 hours, make the solvent in colloidal sol be replaced by deionized water, will
The mixed sols that dialysis obtains is refrigerated to-40 DEG C and carries out lyophilization with the air pressure of 20Pa, the graphite that will obtain after lyophilization
Alkene/aluminium hydroxide gaseous mixture gel is placed in tube furnace under nitrogen protection atmosphere to be calcined 10 hours with 1300 DEG C.Finally it is prepared into
To aluminium oxide/grapheme foam nanocomposite constituents mass percent be: Graphene 10%, aluminium oxide 90%, test air ring
Through 800 DEG C of ablations 5 hours thermal weight loss rates 46.1%, thermal conductivity 10.34W/m K under border.
Embodiment 2
Graphene oxide powder is joined deionized water is stirred dispersion, with the rotating speed stirring at normal temperature 2 hours of 500r/min,
It is configured to the graphene oxide water solution that concentration is 3mg/ml.50ml graphene oxide water solution is inserted in hydrothermal reaction kettle,
Then move to hydrothermal reaction kettle Muffle furnace is warming up to 190 DEG C and is incubated 12 hours, after being cooled to room temperature, reaction is obtained
Graphene hydrogel is refrigerated to-30 DEG C and carries out lyophilization with the air pressure of 10Pa, pure Graphene airsetting lyophilizing obtained subsequently
The anhydrous Aluminum chloride powder of glue and 0.3g joined and carries out ultrasonic disperse in ethylene glycol, with ultrasonic 1 hour of the power room temperature of 200W.
Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then hydrothermal reaction kettle is inserted Muffle
Stove is warming up to 180 DEG C and is incubated 16 hours.After being cooled to room temperature, prepared Graphene/hydrogen-oxygen in hydrothermal reaction kettle, will be reacted
Change aluminum mixed sols to be placed in bag filter with deionized water dialysis 36 hours, make the solvent in colloidal sol be replaced by deionized water, will
The mixed sols that dialysis obtains is refrigerated to-30 DEG C and carries out lyophilization with the air pressure of 20Pa, the graphite that will obtain after lyophilization
Alkene/aluminium hydroxide gaseous mixture gel is placed in tube furnace under nitrogen protection atmosphere to be calcined 14 hours with 1100 DEG C.Finally it is prepared into
To aluminium oxide/grapheme foam nanocomposite constituents mass percent be: Graphene 30%, aluminium oxide 70%, test air ring
Through 800 DEG C of ablations 5 hours thermal weight loss rates 55.0%, thermal conductivity 11.96W/m K under border.
Embodiment 3
Being joined by graphene oxide powder and be stirred dispersion in deionized water, the rotating speed stirring at normal temperature 2.5 with 300r/min is little
Time, it is configured to the graphene oxide water solution that concentration is 2.5mg/ml.45ml graphene oxide water solution is inserted hydro-thermal reaction
In still, then move to hydrothermal reaction kettle Muffle furnace is warming up to 200 DEG C and is incubated 14 hours, will reaction after being cooled to room temperature
The Graphene hydrogel obtained is refrigerated to-50 DEG C and carries out lyophilization, pure graphite lyophilizing obtained subsequently with the air pressure of 15Pa
The anhydrous Aluminum chloride powder of alkene aeroge and 0.5g joins and carries out ultrasonic disperse in methanol, and the power room temperature with 250W is ultrasonic
1.5 hour.Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then by hydrothermal reaction kettle
Insert and Muffle furnace is warming up to 300 DEG C and is incubated 10 hours.After being cooled to room temperature, prepared stone in hydrothermal reaction kettle, will be reacted
Ink alkene/aluminium hydroxide mixed sols be placed in bag filter with deionized water dialyse 48 hours, make the solvent in colloidal sol be replaced by from
Sub-water, mixed sols dialysis obtained is refrigerated to-50 DEG C and carries out lyophilization with the air pressure of 15Pa, obtaining after lyophilization
Graphene/aluminium hydroxide gaseous mixture the gel obtained is placed in tube furnace under nitrogen protection atmosphere to be calcined 15 hours with 1200 DEG C.?
The aluminium oxide prepared eventually/grapheme foam nanocomposite constituents mass percent is: Graphene 20%, aluminium oxide 80%, surveys
Through 800 DEG C of ablations 5 hours thermal weight loss rates 42.4%, thermal conductivity 9.53W/m K under examination air ambient.
Embodiment 4
Being joined by graphene oxide powder and be stirred dispersion in deionized water, the rotating speed stirring at normal temperature 2.5 with 600r/min is little
Time, it is configured to the graphene oxide water solution that concentration is 3mg/ml.40ml graphene oxide water solution is inserted hydrothermal reaction kettle
In, then move to hydrothermal reaction kettle Muffle furnace is warming up to 180 DEG C and is incubated 12 hours, will react after being cooled to room temperature
To Graphene hydrogel be refrigerated to-40 DEG C and carry out lyophilization, pure Graphene lyophilizing obtained subsequently with the air pressure of 10Pa
The anhydrous Aluminum chloride powder of aeroge and 0.7g joins and carries out ultrasonic disperse in Nitrobenzol, and the power room temperature with 300W is ultrasonic
0.5 hour.Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then by hydrothermal reaction kettle
Insert and Muffle furnace is warming up to 190 DEG C and is incubated 18 hours.After being cooled to room temperature, prepared stone in hydrothermal reaction kettle, will be reacted
Ink alkene/aluminium hydroxide mixed sols be placed in bag filter with deionized water dialyse 30 hours, make the solvent in colloidal sol be replaced by from
Sub-water, mixed sols dialysis obtained is refrigerated to-40 DEG C and carries out lyophilization with the air pressure of 13Pa, obtaining after lyophilization
Graphene/aluminium hydroxide gaseous mixture the gel obtained is placed in tube furnace under nitrogen protection atmosphere to be calcined 20 hours with 1200 DEG C.?
The aluminium oxide prepared eventually/grapheme foam nanocomposite constituents mass percent is: Graphene 25%, aluminium oxide 75%, surveys
Through 800 DEG C of ablations 5 hours thermal weight loss rates 36.9%, thermal conductivity 9.07W/m K under examination air ambient.
Embodiment 5
Graphene oxide powder is joined deionized water is stirred dispersion, with the rotating speed stirring at normal temperature 2 hours of 500r/min,
It is configured to the graphene oxide water solution that concentration is 2.8mg/ml.48ml graphene oxide water solution is inserted in hydrothermal reaction kettle,
Then move to hydrothermal reaction kettle Muffle furnace is warming up to 180 DEG C and is incubated 14 hours, after being cooled to room temperature, reaction is obtained
Graphene hydrogel is refrigerated to-30 DEG C and carries out lyophilization with the air pressure of 20Pa, pure Graphene airsetting lyophilizing obtained subsequently
The anhydrous Aluminum chloride powder of glue and 0.4g joined and carries out ultrasonic disperse in ethanol, with ultrasonic 0.5 hour of the power room temperature of 250W.
Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then hydrothermal reaction kettle is inserted Muffle
Stove is warming up to 210 DEG C and is incubated 22 hours.After being cooled to room temperature, prepared Graphene/hydrogen-oxygen in hydrothermal reaction kettle, will be reacted
Change aluminum mixed sols to be placed in bag filter with deionized water dialysis 40 hours, make the solvent in colloidal sol be replaced by deionized water, will
The mixed sols that dialysis obtains is refrigerated to-30 DEG C and carries out lyophilization with the air pressure of 10Pa, the graphite that will obtain after lyophilization
Alkene/aluminium hydroxide gaseous mixture gel is placed in tube furnace under nitrogen protection atmosphere to be calcined 15 hours with 950 DEG C.Finally prepare
Aluminium oxide/grapheme foam nanocomposite constituents mass percent be: Graphene 30%, aluminium oxide 70%, test air ambient
Lower through 800 DEG C of ablations 5 hours thermal weight loss rates 48.2%, thermal conductivity 10.77W/m K.
Embodiment 6
Being joined by graphene oxide powder and be stirred dispersion in deionized water, the rotating speed stirring at normal temperature 2.5 with 450r/min is little
Time, it is configured to the graphene oxide water solution that concentration is 2.3mg/ml.43ml graphene oxide water solution is inserted hydro-thermal reaction
In still, then move to hydrothermal reaction kettle Muffle furnace is warming up to 170 DEG C and is incubated 13 hours, will reaction after being cooled to room temperature
The Graphene hydrogel obtained is refrigerated to-50 DEG C and carries out lyophilization, pure Graphene lyophilizing obtained subsequently with the air pressure of 5Pa
The anhydrous Aluminum chloride powder of aeroge and 0.4g joins and carries out ultrasonic disperse in ether, with the power room temperature ultrasonic 1.5 of 300W
Hour.Pure graphene aerogel is joined in hydrothermal reaction kettle with liquor alumini chloridi mixing suspension, then hydrothermal reaction kettle is put
Enter Muffle furnace is warming up to 180 DEG C and be incubated 19 hours.After being cooled to room temperature, prepared graphite in hydrothermal reaction kettle, will be reacted
Alkene/aluminium hydroxide mixed sols is placed in bag filter dialyses 34 hours with deionized water, makes the solvent in colloidal sol be replaced by deionization
Water, mixed sols dialysis obtained is refrigerated to-40 DEG C and carries out lyophilization with the air pressure of 10Pa, will obtain after lyophilization
Graphene/aluminium hydroxide gaseous mixture gel be placed in tube furnace under nitrogen protection atmosphere with 1200 DEG C calcine 20 hours.Finally
The aluminium oxide prepared/grapheme foam nanocomposite constituents mass percent is: Graphene 22%, aluminium oxide 78%, test
Through 800 DEG C of ablations 5 hours thermal weight loss rates 41.7%, thermal conductivity 9.20W/m K under air ambient.
Claims (9)
1. a preparation method for fire-resistant oxidation resistant heat conduction aluminium oxide/grapheme foam composite, is characterized in that step is as follows:
1) graphene oxide powder is joined deionized water is stirred dispersion, configure graphene oxide water solution；
2) graphene oxide water solution is inserted in hydrothermal reaction kettle, then move to hydrothermal reaction kettle Muffle furnace is warming up to
170～200 DEG C and be incubated 10～14 hours, Graphene hydrogel reaction obtained after being cooled to room temperature is refrigerated to
-30～-50 DEG C be dried, pure graphene aerogel lyophilizing obtained subsequently and anhydrous Aluminum chloride powder join in solvent and carry out
Ultrasonic disperse, obtaining concentration of aluminum chloride is 4～20mg/ml, the mixing suspension containing graphene aerogel；
3) prepared mixing suspension is joined in hydrothermal reaction kettle, then hydrothermal reaction kettle is inserted in Muffle furnace be warming up to
180～300 DEG C and be incubated 10～22 hours；
4), after being cooled to room temperature, the solvent reacting prepared Graphene/aluminium hydroxide mixed sols in hydrothermal reaction kettle is put
Be changed to deionized water, mixed sols is refrigerated to-30～-50 DEG C be dried, the Graphene/aluminium hydroxide that will obtain after lyophilization
Gaseous mixture gel is placed in tube furnace under nitrogen protection atmosphere to be calcined 10～20 hours with 950～1300 DEG C；Obtain aluminium oxide/
Grapheme foam composite.
2. the method for claim 1, is characterized in that described step 1) graphene oxide water solution concentration is 2～3mg/ml.
3. the method for claim 1, is characterized in that described step 1) with 300～600r/min stirring at normal temperature 2～3 hours.
4. the method for claim 1, is characterized in that described step 2) Graphene hydrogel be refrigerated to-30～-50 DEG C and with≤
The air pressure of 20Pa carries out lyophilization.
5. the method for claim 1, is characterized in that described step 2) graphene oxide with aluminum chloride mass ratio is
1:12～1:3.
6. the method for claim 1, is characterized in that described step 2) to carry out ultrasonic disperse in solvent be with 200～300W
Ultrasonic 0.5～2 hour of power room temperature.
7. the method for claim 1, is characterized in that described step 2) solvent is ethanol, methanol, ethylene glycol, Nitrobenzol
Or ether.
8. the method for claim 1, is characterized in that described step 4) mixed sols is refrigerated to-30～-50 DEG C and with≤20Pa
Air pressure carry out lyophilization.
9. aluminium oxide/grapheme foam composite that the method for claim 1 obtains, is characterized in that having micro/nano level hole
Foaming structure, composite foam network structure size is more than graphene aerogel, is linked the main body being constituted foam with Graphene mutually
Structural framework, aluminium oxide with the form even application of nano-scale coating in Graphene three-dimensional foam structure skeleton surface.
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| CN111974320A (en) * | 2020-08-25 | 2020-11-24 | 航天特种材料及工艺技术研究所 | High-temperature-resistant elastic graphene aerogel and preparation method thereof |
| CN112340724A (en) * | 2020-11-09 | 2021-02-09 | 安徽宇航派蒙健康科技股份有限公司 | Preparation method for preparing high-thermal-conductivity three-dimensional graphene composite gel based on hydrothermal method |
| CN114956834A (en) * | 2022-06-14 | 2022-08-30 | 天津城建大学 | Reinforced graphene composite aerogel and preparation method thereof |
| CN115448341A (en) * | 2022-08-26 | 2022-12-09 | 广西大学 | Preparation method of flaky beta-alumina |
| CN115650221A (en) * | 2022-10-28 | 2023-01-31 | 航天特种材料及工艺技术研究所 | Antioxidant elastic graphene aerogel and preparation method thereof |
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