CN105923641B - 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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- CN105923641B CN105923641B CN201610269066.XA CN201610269066A CN105923641B CN 105923641 B CN105923641 B CN 105923641B CN 201610269066 A CN201610269066 A CN 201610269066A CN 105923641 B CN105923641 B CN 105923641B
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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 a kind of preparation method of fire-resistant oxidation resistant heat conduction aluminium oxide/grapheme foam composite, tool
Say it is a kind of preparation method of aluminum oxide coating layer grapheme foam body.
Background technology
Science and technology achieves the development of high speed since 21st century, and efficient conduction of heat and radiating become heat management
The critical problem of Material Field.For example during heat generating device arrangement works, because of resistance, thermal resistance, the electricity of device itself
The effects such as son vortex, build up amount of heat, and particularly at the position that component density is high, heat-dissipating space is narrow, hot-fluid is close
Degree can be especially big, so as to cause integral member temperature extremely uneven.Most of microelectronic chip surface temperature must be maintained at
Its high performance operation is just can ensure that (such as 100 DEG C of silicon device ﹤) under relatively low level, many electronic units are needed at 40～60 DEG C
At a temperature of could normal work, this proposes higher and higher requirement to Heat Conduction Material, and device heat production can discharge in time, device
Part radiating whether uniform high-efficiency be electronic device can fast and stable work deciding factor, greatly have impact on electronic equipment
Performance and quality.In order to by these heat derives, need that development quality is lighter, thermal conductivity is higher in a hurry in time, performance more
Excellent heat conduction new material.
Grapheme foam is a kind of loose porous spongy material obtained through dissolving, reduction, crosslinking by Graphene.
Grapheme foam is less due to the graphitization parietal layer with regular bulk, the obstruction of phonon conduction, and boundary defect is less, heat conduction effect
Rate is very high, thus preparing carbon-based highly heat-conductive material using grapheme foam becomes the emphasis of people's research, also occurs in that similar
The mandate of patent or disclosure.State Intellectual Property Office of the People's Republic of China's grant number be CN104211057A,
The patents of invention such as CN104291324A and CN102585776A are disclosed and prepare grapheme foam and profit using graphene oxide
The technology of heat conduction back bone network in phase-changing energy storage material is prepared with grapheme foam.
Above-described patent of invention disclose only traditional grapheme foam preparation method and processing technique, only obtain
Suitable for the Graphene heat conducting foam material under room temperature hypoxia condition.For grapheme foam Heat Conduction Material, high temperature, aerobic bar
Part is the working environment basis of materials serve heat conduction function, thus in grapheme foam material Graphene in higher temperature, higher
It is easy to oxidation in the working environment of oxygen content, causes graphite lattice structure to produce defect, the conduction of phonon is had a strong impact on, so as to shadow
Ring the heat conductivility of Graphene foamed materialss.After processing through Graphene reduction networking Joining Technology, Graphene directly with
External environment is contacted, thus the antioxygenic property under high temperature aerobic environment all very poor (Samad Y A, Li Y, Schiffer
A,et al.Graphene 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 grapheme foam of the announcements such as the patent application CN104291324A of China does not possess the property of fire-resistant oxidation resistant
Energy.Therefore, existing published patent of invention obtains its ruggedness of Heat Conduction Material far from meeting mainframe computer, highly integrated
The requirement to Heat Conduction Material oxidation resistance such as electronic device, develops a kind of simultaneously with resistance on the basis of material with carbon element is advantageous
The Heat Conduction Material of high-temperature oxidation resistant is particularly important.
The content of the invention
A kind of defect of the grapheme foam antioxygenic property that the present invention is prepared for existing graphene oxide, there is provided resistance to height
Temperature has grapheme foam of antioxygenic property and preparation method thereof simultaneously.It is under air ambient Jing after 800 DEG C of ablations 5 hours
Thermal weight loss is higher than 9W/mK less than 60%, thermal conductivity.As shown in figure 1, aluminium oxide/grapheme foam composite has micro-nano
The foaming structure of meter level hole, the agent structure skeleton for being constituted foam is mutually linked with Graphene, and aluminium oxide is with nano-scale coating
Form even application in Graphene three-dimensional foam structure skeleton surface.
The present invention is employed 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 added in deionized water and is stirred dispersion, configure graphene oxide water solution；
2) graphene oxide water solution is inserted in hydrothermal reaction kettle, then hydrothermal reaction kettle is moved in Muffle furnace and is heated up
To 170～200 DEG C and 10～14 hours are incubated, are cooled to after room temperature the Graphene hydrogel for obtaining reaction, be refrigerated to -30
～-50 DEG C of dryings, the pure graphene aerogel and anhydrous Aluminum chloride powder for subsequently obtaining lyophilizing is added in solvent and is surpassed
Sound disperses, and obtains concentration of aluminum chloride for 4～20mg/ml, the mixing suspension containing graphene aerogel；
3) obtained mixing suspension is added in hydrothermal reaction kettle, then hydrothermal reaction kettle is inserted into intensification in Muffle furnace
To 180～300 DEG C and it is incubated 10～22 hours；
4) it is cooled to after room temperature, the molten of obtained Graphene/aluminium hydroxide mixed sols will be reacted in hydrothermal reaction kettle
Agent is replaced into deionized water, and mixed sols is refrigerated to into -30～-50 DEG C of dryings, by the Graphene/hydrogen-oxygen obtained after lyophilization
Change aluminum mixing aeroge is placed in tube furnace under nitrogen protection atmosphere to be calcined 10～20 hours with 950～1300 DEG C；Obtain oxygen
Change aluminum/grapheme foam composite.
The step 1) preferably graphene oxide water solution concentration is 2～3mg/ml.
The step 1) preferably with 300～600r/min stirring at normal temperature 2～3 hours.
The step 2) preferably Graphene hydrogel is refrigerated to -30～-50 DEG C and to carry out freezing with the air pressure of≤20Pa dry
It is dry.
The step 2) preferably graphene oxide and aluminum chloride mass ratio be 1:12～1:3.
The step 2) to carry out ultrasonic disperse in preferred solvent be little with the power room temperature ultrasound 0.5～2 of 200～300W
When.
The step 2) preferred solvent be ethanol, methanol, ethylene glycol, Nitrobenzol or ether.
The step 4) preferably mixed sols is refrigerated to -30～-50 DEG C and carries out lyophilization with the air pressure of≤20Pa.
The aluminium oxide that the method for the present invention is obtained/grapheme foam composite has the foam knot of micro/nano level hole
Structure, composite foam network structure size is more than graphene aerogel, and the body junction llex cornuta for being constituted foam is mutually linked with Graphene
Frame, as shown in Fig. 2 graphene sheet layer is interconnected to form tridimensional network, aluminium oxide is uniform in the form of nano-scale coating
It is coated on 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 scale
Graphite oxidation, obtain graphite oxide, then by graphite oxide Jing ultrasound lift-off processing for a period of time after, obtain graphite oxide
Alkene.
(2) displacement (step 4) of Graphene/aluminium hydroxide mixed sols solvent：Colloidal sol is placed in bag filter with go from
Sub- water is dialysed 24～48 hours, and the solvent for making colloidal sol is replaced by deionized water, and this is very beneficial for the freezing of colloidal sol, be easy to into
Row lyophilizing processes to obtain aluminium oxide/grapheme foam composite.
The aluminium oxide for finally preparing/grapheme foam composite has the foaming structure of micro/nano level hole, such as
Shown in Fig. 3, composite foam network structure size is significantly greater than graphene aerogel, illustrate aluminium oxide even application in Graphene
Three-dimensional network surface), the agent structure skeleton for being constituted foam is mutually linked with Graphene, provide heat for the foamed composite
Pathway, performance heat conduction function simultaneously provide certain flexibility for composite；Aluminium oxide is uniform in the form of nano-scale coating
Graphene three-dimensional foam structure skeleton surface is coated on, for aluminium oxide/grapheme foam composite high temperature resistant and antioxygen are provided
The functional characteristic of change.
It is combined and lyophilizing molding by the aluminium oxide and Graphene of above step, realizes the Graphene with heat conductivility
Foam is compound with the aluminium oxide with fire-resistant oxidation resistant performance, in lyophilization so that composite ultimately forms airsetting
Glue, obtains heat conduction of 800 DEG C of the Jing ablations 5 hours thermal weight loss less than 60%, thermal conductivity higher than 9W/mK under air ambient and aoxidizes
Aluminum/Graphene 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 simply controllable.This
Microstructure ordering, densification and painting stratification in invention can be completed efficiently, and what is can obtained is carbon-based compound with high antioxidant
Material foams, its oxidation resistance is far superior to traditional thermal conductivity graphene foam and other carbon-based heat-conductive composite materials.
Description of the drawings：
Fig. 1 is the microcosmic macroscopic view schematic diagram of Graphene of the present invention/Alumina Foam composite, including complex form and micro-
See structure；
Fig. 2 is the scanning electron microscopic picture of three-dimensional graphene foam；
Fig. 3 is the scanning electron microscopic picture of final obtained Graphene/Alumina Foam composite.
Specific embodiment
6 embodiments of the present invention are given below, are that the present invention is further illustrated, rather than limit the model of the present invention
Enclose.
Embodiment 1
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 400r/min
3 hours, it is configured to the graphene oxide water solution that concentration is 2mg/ml.40ml graphene oxide water solutions are inserted into hydro-thermal reaction
In kettle, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 170 DEG C and be incubated 10 hours, being cooled to after room temperature will reaction
The Graphene hydrogel for obtaining is refrigerated to -40 DEG C and carries out lyophilization with the air pressure of 20Pa, the pure stone for subsequently obtaining lyophilizing
The anhydrous Aluminum chloride powder of black alkene aeroge and 0.7g is added in ethanol carries out ultrasonic disperse, with the power room temperature ultrasound of 300W
2 hours.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then by hydrothermal reaction kettle
Insert in Muffle furnace and be warming up to 200 DEG C and be incubated 14 hours.After being cooled to room temperature, obtained stone will be reacted in hydrothermal reaction kettle
Black alkene/aluminium hydroxide mixed sols is placed in bag filter is dialysed 24 hours with deionized water, is replaced by the solvent in colloidal sol
Deionized water, the mixed sols that dialysis is obtained is refrigerated to -40 DEG C and carries out lyophilization with the air pressure of 20Pa, by lyophilization
The Graphene for obtaining afterwards/aluminium hydroxide mixing aeroge is placed in tube furnace under nitrogen protection atmosphere little with 1300 DEG C of calcinings 10
When.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 10%, aluminium oxide
90%, 800 DEG C of the Jing thermal weight loss rates 46.1%, thermal conductivity 10.34W/mK of ablation 5 hours under test air ambient.
Embodiment 2
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 500r/min
2 hours, it is configured to the graphene oxide water solution that concentration is 3mg/ml.50ml graphene oxide water solutions are inserted into hydro-thermal reaction
In kettle, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 190 DEG C and be incubated 12 hours, being cooled to after room temperature will reaction
The Graphene hydrogel for obtaining is refrigerated to -30 DEG C and carries out lyophilization with the air pressure of 10Pa, the pure stone for subsequently obtaining lyophilizing
The anhydrous Aluminum chloride powder of black alkene aeroge and 0.3g is added in ethylene glycol carries out ultrasonic disperse, super with the power room temperature of 200W
Sound 1 hour.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then by hydro-thermal reaction
Kettle is inserted in Muffle furnace and is warming up to 180 DEG C and is incubated 16 hours.After being cooled to room temperature, will react obtained in hydrothermal reaction kettle
Graphene/aluminium hydroxide mixed sols is placed in bag filter is dialysed 36 hours with deionized water, is replaced the solvent in colloidal sol
For deionized water, the mixed sols that dialysis is obtained is refrigerated to -30 DEG C and carries out lyophilization with the air pressure of 20Pa, freezing is dry
Graphene/aluminium hydroxide mixing the aeroge obtained after dry is placed in tube furnace under nitrogen protection atmosphere with 1100 DEG C of calcinings 14
Hour.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 30%, oxidation
Aluminum 70%, 800 DEG C of the Jing thermal weight loss rates 55.0%, thermal conductivity 11.96W/mK of ablation 5 hours under test air ambient.
Embodiment 3
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 300r/min
2.5 hours, it is configured to the graphene oxide water solution that concentration is 2.5mg/ml.45ml graphene oxide water solutions are inserted into hydro-thermal
In reactor, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 200 DEG C and be incubated 14 hours, being cooled to after room temperature will
The Graphene hydrogel that reaction is obtained is refrigerated to -50 DEG C and carries out lyophilization with the air pressure of 15Pa, subsequently obtains lyophilizing
The anhydrous Aluminum chloride powder of pure graphene aerogel and 0.5g is added in methanol carries out ultrasonic disperse, with the power room temperature of 250W
Ultrasound 1.5 hours.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then by hydro-thermal
Reactor is inserted in Muffle furnace and is warming up to 300 DEG C and is incubated 10 hours.After being cooled to room temperature, by reaction system in hydrothermal reaction kettle
Graphene/aluminium hydroxide the mixed sols for obtaining is placed in bag filter is dialysed 48 hours with deionized water, makes the solvent quilt in colloidal sol
Deionized water is replaced with, the mixed sols that dialysis is obtained is refrigerated to -50 DEG C and carries out lyophilization with the air pressure of 15Pa, will be cold
Graphene/aluminium hydroxide mixing the aeroge obtained after lyophilizing is dry is placed in tube furnace and is forged with 1200 DEG C under nitrogen protection atmosphere
Burn 15 hours.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 20%,
Aluminium oxide 80%, 800 DEG C of the Jing thermal weight loss rates 42.4%, thermal conductivity 9.53W/mK of ablation 5 hours under test air ambient.
Embodiment 4
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 600r/min
2.5 hours, it is configured to the graphene oxide water solution that concentration is 3mg/ml.40ml graphene oxide water solutions are inserted into hydro-thermal anti-
In answering kettle, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 180 DEG C and be incubated 12 hours, being cooled to after room temperature will be anti-
The Graphene hydrogel that should be obtained is refrigerated to -40 DEG C and carries out lyophilization with the air pressure of 10Pa, subsequently by lyophilizing obtain it is pure
The anhydrous Aluminum chloride powder of graphene aerogel and 0.7g is added in Nitrobenzol carries out ultrasonic disperse, with the power room temperature of 300W
Ultrasound 0.5 hour.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then by hydro-thermal
Reactor is inserted in Muffle furnace and is warming up to 190 DEG C and is incubated 18 hours.After being cooled to room temperature, by reaction system in hydrothermal reaction kettle
Graphene/aluminium hydroxide the mixed sols for obtaining is placed in bag filter is dialysed 30 hours with deionized water, makes the solvent quilt in colloidal sol
Deionized water is replaced with, the mixed sols that dialysis is obtained is refrigerated to -40 DEG C and carries out lyophilization with the air pressure of 13Pa, will be cold
Graphene/aluminium hydroxide mixing the aeroge obtained after lyophilizing is dry is placed in tube furnace and is forged with 1200 DEG C under nitrogen protection atmosphere
Burn 20 hours.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 25%,
Aluminium oxide 75%, 800 DEG C of the Jing thermal weight loss rates 36.9%, thermal conductivity 9.07W/mK of ablation 5 hours under test air ambient.
Embodiment 5
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 500r/min
2 hours, it is configured to the graphene oxide water solution that concentration is 2.8mg/ml.48ml graphene oxide water solutions are inserted into hydro-thermal anti-
In answering kettle, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 180 DEG C and be incubated 14 hours, being cooled to after room temperature will be anti-
The Graphene hydrogel that should be obtained is refrigerated to -30 DEG C and carries out lyophilization with the air pressure of 20Pa, subsequently by lyophilizing obtain it is pure
The anhydrous Aluminum chloride powder of graphene aerogel and 0.4g is added in ethanol carries out ultrasonic disperse, super with the power room temperature of 250W
Sound 0.5 hour.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then hydro-thermal is anti-
Answer kettle to insert in Muffle furnace to be warming up to 210 DEG C and be incubated 22 hours.After being cooled to room temperature, it is obtained reacting in hydrothermal reaction kettle
Graphene/aluminium hydroxide mixed sols be placed in bag filter with deionized water dialyse 40 hours, replaced the solvent in colloidal sol
Deionized water is changed to, the mixed sols that dialysis is obtained is refrigerated to -30 DEG C and carries out lyophilization with the air pressure of 10Pa, will be freezed
Graphene/aluminium hydroxide mixing the aeroge obtained after drying is placed in tube furnace under nitrogen protection atmosphere with 950 DEG C of calcinings
15 hours.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 30%, oxygen
Change aluminum 70%, 800 DEG C of the Jing thermal weight loss rates 48.2%, thermal conductivity 10.77W/mK of ablation 5 hours under test air ambient.
Embodiment 6
Graphene oxide powder is added in deionized water and is stirred dispersion, with the rotating speed stirring at normal temperature of 450r/min
2.5 hours, it is configured to the graphene oxide water solution that concentration is 2.3mg/ml.43ml graphene oxide water solutions are inserted into hydro-thermal
In reactor, then hydrothermal reaction kettle is moved to and be warming up in Muffle furnace 170 DEG C and be incubated 13 hours, being cooled to after room temperature will
The Graphene hydrogel that obtains of reaction is refrigerated to -50 DEG C and carries out lyophilization with the air pressure of 5Pa, subsequently by lyophilizing obtain it is pure
The anhydrous Aluminum chloride powder of graphene aerogel and 0.4g is added in ether carries out ultrasonic disperse, super with the power room temperature of 300W
Sound 1.5 hours.Pure graphene aerogel and liquor alumini chloridi mixing suspension are added in hydrothermal reaction kettle, then hydro-thermal is anti-
Answer kettle to insert in Muffle furnace to be warming up to 180 DEG C and be incubated 19 hours.After being cooled to room temperature, it is obtained reacting in hydrothermal reaction kettle
Graphene/aluminium hydroxide mixed sols be placed in bag filter with deionized water dialyse 34 hours, replaced the solvent in colloidal sol
Deionized water is changed to, the mixed sols that dialysis is obtained is refrigerated to -40 DEG C and carries out lyophilization with the air pressure of 10Pa, will be freezed
Graphene/aluminium hydroxide mixing the aeroge obtained after drying is placed in tube furnace under nitrogen protection atmosphere with 1200 DEG C of calcinings
20 hours.The aluminium oxide for finally preparing/grapheme foam nanocomposite constituents mass percent is：Graphene 22%, oxygen
Change aluminum 78%, 800 DEG C of the Jing thermal weight loss rates 41.7%, thermal conductivity 9.20W/mK of ablation 5 hours under test air ambient.
Claims (9)
1. a kind of preparation method of fire-resistant oxidation resistant heat conduction aluminium oxide/grapheme foam composite, is characterized in that step such as
Under：
1) graphene oxide powder is added in deionized water and is stirred dispersion, configure graphene oxide water solution；
2) graphene oxide water solution is inserted in hydrothermal reaction kettle, then hydrothermal reaction kettle is moved in Muffle furnace and is warming up to
170～200 DEG C and 10～14 hours are incubated, be cooled to after room temperature for the Graphene hydrogel that reaction is obtained to be refrigerated to -30～-
50 DEG C of dryings, the pure graphene aerogel and anhydrous Aluminum chloride powder for subsequently obtaining lyophilizing is added in solvent carries out ultrasound point
Dissipate, obtain concentration of aluminum chloride for 4～20mg/mL, the mixing suspension containing graphene aerogel；
3) obtained mixing suspension is added in hydrothermal reaction kettle, then hydrothermal reaction kettle is inserted in Muffle furnace is warming up to
180～300 DEG C and it is incubated 10～22 hours；
4) it is cooled to after room temperature, the solvent that obtained Graphene/aluminium hydroxide mixed sols is reacted in hydrothermal reaction kettle is put
Deionized water is changed to, mixed sols is refrigerated to into -30～-50 DEG C of dryings, by the Graphene/aluminium hydroxide obtained after lyophilization
Mixing aeroge 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 the step 1) graphene oxide water solution concentration be 2～3mg/
mL。
3. the method for claim 1, is characterized in that the step 1) it is little with 300～600r/min stirring at normal temperature 2～3
When.
4. the method for claim 1, is characterized in that the step 2) Graphene hydrogel is refrigerated to -30～-50 DEG C simultaneously
Lyophilization is carried out with the air pressure of≤20Pa.
5. the method for claim 1, is characterized in that the step 2) contained graphite oxide in graphene oxide water solution
Alkene is 1 with aluminum chloride mass ratio:12～1:3.
6. the method for claim 1, is characterized in that the step 2) to carry out ultrasonic disperse in solvent be with 200～300W
Power room temperature ultrasound 0.5～2 hour.
7. the method for claim 1, is characterized in that the step 2) solvent be ethanol, methanol, ethylene glycol, Nitrobenzol or
Ether.
8. the method for claim 1, is characterized in that the step 4) mixed sols be refrigerated to -30～-50 DEG C and with≤
The air pressure of 20Pa carries out lyophilization.
9. aluminium oxide/grapheme foam composite that the method for claim 1 is obtained, is characterized in that with micro/nano level hole
Foaming structure, composite foam network structure size be more than graphene aerogel, the master for being constituted foam is mutually linked with Graphene
Body structural framework, aluminium oxide in the form of nano-scale coating even application in Graphene three-dimensional foam structure skeleton surface.
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| CN110295298B (en) * | 2019-01-17 | 2020-08-11 | 杭州电缆股份有限公司 | Preparation method of graphene-aluminum composite material |
| CN111974320B (en) * | 2020-08-25 | 2022-04-29 | 航天特种材料及工艺技术研究所 | High-temperature-resistant elastic graphene aerogel and preparation method thereof |
| CN112340724B (en) * | 2020-11-09 | 2021-12-14 | 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 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887508A (en) * | 2012-09-28 | 2013-01-23 | 上海理工大学 | Method for preparing high-strength graphite oxide aerogel |
| CN102906016A (en) * | 2010-04-22 | 2013-01-30 | 巴斯夫欧洲公司 | Method for producing two-dimensional sandwich nano-materials on the basis of graphene |
| CN102941042A (en) * | 2012-10-25 | 2013-02-27 | 北京理工大学 | Graphene/metal oxide hybrid aerogel, preparation method and applications thereof |
| CN103482619A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Graphene-copper oxide three-dimensional foam composite material |
| CN104828807A (en) * | 2015-04-10 | 2015-08-12 | 中国科学院重庆绿色智能技术研究院 | Preparation method of three-dimensional graphene oxide aerogel with high specific surface area |
-
2016
- 2016-04-26 CN CN201610269066.XA patent/CN105923641B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102906016A (en) * | 2010-04-22 | 2013-01-30 | 巴斯夫欧洲公司 | Method for producing two-dimensional sandwich nano-materials on the basis of graphene |
| CN102887508A (en) * | 2012-09-28 | 2013-01-23 | 上海理工大学 | Method for preparing high-strength graphite oxide aerogel |
| CN102941042A (en) * | 2012-10-25 | 2013-02-27 | 北京理工大学 | Graphene/metal oxide hybrid aerogel, preparation method and applications thereof |
| CN103482619A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Graphene-copper oxide three-dimensional foam composite material |
| CN104828807A (en) * | 2015-04-10 | 2015-08-12 | 中国科学院重庆绿色智能技术研究院 | Preparation method of three-dimensional graphene oxide aerogel with high specific surface area |
Non-Patent Citations (1)
| Title |
|---|
| Graphene coated with alumina and its utilization as a thermal conductivity enhancer for alumina sphere/thermoplastic polyurethane composite;Ki Tae Kim, et al.;《Materials Chemistry and Physics》;20150107;第153卷;291-300 * |
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