CN108584942A - A kind of preparation method of grapheme foam carbon composite - Google Patents
A kind of preparation method of grapheme foam carbon composite Download PDFInfo
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- CN108584942A CN108584942A CN201810643104.2A CN201810643104A CN108584942A CN 108584942 A CN108584942 A CN 108584942A CN 201810643104 A CN201810643104 A CN 201810643104A CN 108584942 A CN108584942 A CN 108584942A
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The invention discloses a kind of preparation methods of grapheme foam carbon composite.Crossing ultrasonic disperse makes graphene and foam carbon precursor be uniformly mixed, and is then foamed, carbonized and is graphitized again, realizes that graphene is evenly dispersed in foam carbon matrix, to obtain the Foam carbon composite material with excellent comprehensive performance.To allow graphene to be uniformly dispersed in foam carbon matrix, the enhancing to Carbon foam comprehensive performance is realized.The method that the present invention prepares grapheme foam carbon composite simultaneously, has the characteristics that the period is short, simple for process, at low cost, easy-operating.
Description
Technical field
The invention belongs to technical field of material, are related to a kind of preparation method of grapheme foam carbon composite.
Background technology
Since 21st century, the fast development in the fields such as science and technology and industry manufacture, while also material is carried
More and more harsh requirement is gone out, the single material of many traditional performances gradually cannot be satisfied growing application and needed
It asks, the material with a variety of excellent performances gradually causes the extensive concern of people.Carbon foam is a kind of with spongy abscess knot
The new carbon of structure has low-density, high intensity, highly conductive, high heat conduction, resistant to chemical etching, damping and inhales many spies such as wave
Property, these excellent properties make Carbon foam be shown in fields such as heat exchange, suction wave noise reduction, absorption, energy stores and biological medicines
Wide application prospect.However, the performance of Carbon foam still has certain gap away from practical application at present, novel foam charcoal is developed
Composite material improves its comprehensive performance, is critical issue urgently to be resolved hurrily in current foam carbon material research field.
The two-dimentional carbon material that graphene is made of single layer of carbon atom has very excellent electrical property, mechanical property, heat
Conductive performance and optical property.It is one of highest material of known strength, and tensile strength is up to 130 parts of pa or more；Its heat
The coefficient of conductivity is between 3000~5000 W/mK；Its resistivity only has 10-6Ω cm are the materials of resistivity minimum.Cause
If this is carried out compound, it will play the association on two kinds of material properties using graphene as additive material with foam carbon material
Same-action greatly improves composite performance of Carbon foam basis material, including mechanical property, electric conductivity and heat-conductive characteristic etc.
Deng.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of grapheme foam carbon composite, solve the prior art
Present in graphene be difficult to disperse the problem general with Carbon foam comprehensive performance in the base.
The present invention uses following technical scheme to achieve the above object：
A kind of preparation method of grapheme foam carbon composite, includes the following steps：
Step 1, the preparation of graphene：
Expanded graphite is added in ethanol solution, then by mixed solution ultrasound 3h~5h, is then placed in 80 DEG C of baking ovens
Middle dry 12h, obtains thin graphene；
Step 2, graphene/mesophase pitch mixed system is prepared：
It will be dissolved in alcohol solvent together with graphene and mesophase pitch that step 1 obtains, then utilize ultrasonic wave stone
Black alkene separating apparatus makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly volatilize；
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through, and reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material；
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized；
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature to get to graphitizable foams carbon composite.
As a further solution of the present invention, in step 1 expanded graphite according to the mass fraction be 1 part~10 parts.
As a further solution of the present invention, in step 2 mesophase pitch be coal measures mesophase pitch, interphase content >=
95%.
As a further solution of the present invention, mesophase pitch is 100 parts~200 parts according to the mass fraction in step 2.
As a further solution of the present invention, heating rate is 2 DEG C/min in step 3.
As a further solution of the present invention, the specific heat temperature raising mode of carbonization process is in step 4：First with 2 DEG C/min
500 DEG C are warming up to, 1h is kept the temperature, then 1000 DEG C are warming up to 5 DEG C/min, keeps the temperature 2h.
As a further solution of the present invention, graphited heating ramp rate is 5 DEG C/min in step 5.
The beneficial effects of the invention are as follows：The present invention can be by improving dispersion of the graphene in presoma mesophase pitch
Property, to allow graphene to be uniformly dispersed in foam carbon matrix, realize the enhancing to Carbon foam comprehensive performance.Simultaneously originally
The method that invention prepares grapheme foam carbon composite has the characteristics that the period is short, simple for process, at low cost, easy-operating.
Description of the drawings
Fig. 1 is the SEM photograph of 1 gained foam carbon material of the embodiment of the present invention.
Specific implementation mode
The present invention is further elaborated in the following with reference to the drawings and specific embodiments.
Embodiment 1
Step 1, the preparation of graphene：
1 part of expanded graphite is added in ethanol solution, then by mixed solution ultrasound 3h~5h, is then placed in 80 DEG C of bakings
Dry 12h, obtains thin graphene in case.
Step 2, graphene/mesophase pitch mixed system is prepared：
The graphene that step 1 obtains is dissolved in together with 100 parts of mesophase pitch in alcohol solvent, ultrasound is then utilized
Wave graphene dispersion instrument makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly wave
Hair.
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through.Reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material.
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized.
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature, you can obtains graphitizable foams carbon composite.
Embodiment 2
Step 1, the preparation of graphene：
3 parts of expanded graphites are added in ethanol solution, then by mixed solution ultrasound 3h~5h, are then placed in 80 DEG C of bakings
Dry 12h, obtains thin graphene in case.
Step 2, graphene/mesophase pitch mixed system is prepared：
The graphene that step 1 obtains is dissolved in together with 120 parts of mesophase pitch in alcohol solvent, ultrasound is then utilized
Wave graphene dispersion instrument makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly wave
Hair.
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through.Reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material.
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized.
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature, you can obtains graphitizable foams carbon composite.
Embodiment 3
Step 1, the preparation of graphene：
5 parts of expanded graphites are added in ethanol solution, then by mixed solution ultrasound 3h~5h, are then placed in 80 DEG C of bakings
Dry 12h, obtains thin graphene in case.
Step 2, graphene/mesophase pitch mixed system is prepared：
The graphene that step 1 obtains is dissolved in together with 140 parts of mesophase pitch in alcohol solvent, ultrasound is then utilized
Wave graphene dispersion instrument makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly wave
Hair.
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through.Reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material.
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized.
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature, you can obtains graphitizable foams carbon composite.
Embodiment 4
Step 1, the preparation of graphene：
7 parts of expanded graphites are added in ethanol solution, then by mixed solution ultrasound 3h~5h, are then placed in 80 DEG C of bakings
Dry 12h, obtains thin graphene in case.
Step 2, graphene/mesophase pitch mixed system is prepared：
The graphene that step 1 obtains is dissolved in together with 160 parts of mesophase pitch in alcohol solvent, ultrasound is then utilized
Wave graphene dispersion instrument makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly wave
Hair.
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through.Reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material.
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized.
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature, you can obtains graphitizable foams carbon composite.
Embodiment 5
Step 1, the preparation of graphene：
9 parts of expanded graphites are added in ethanol solution, then by mixed solution ultrasound 3h~5h, are then placed in 80 DEG C of bakings
Dry 12h, obtains thin graphene in case.
Step 2, graphene/mesophase pitch mixed system is prepared：
The graphene that step 1 obtains is dissolved in together with 180 parts of mesophase pitch in alcohol solvent, ultrasound is then utilized
Wave graphene dispersion instrument makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly wave
Hair.
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, the powder-like that then will be obtained
Product are placed in high-temperature high-pressure reaction kettle, are warming up to 500 DEG C and are kept the temperature 3h, and nitrogen protection, pressure 3MPa are passed through.Reaction terminates
It is cooled to room temperature automatically afterwards, obtains Carbon foam raw material.
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and are protected
Warm 2h, then cooled to room temperature, the Foam carbon composite material after being carbonized.
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2
Gas shielded is finally cooled to room temperature, you can obtains graphitizable foams carbon composite.
The above is present pre-ferred embodiments, for the ordinary skill in the art, according to the present invention
Introduction, in the case where not departing from the principle of the present invention with spirit, changes, modifications, replacement and change that embodiment is carried out
Type still falls within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of grapheme foam carbon composite, which is characterized in that include the following steps：
Step 1, the preparation of graphene：
Expanded graphite is added in ethanol solution, then by mixed solution ultrasound 3h~5h, is then placed in 80 DEG C of baking ovens and does
Dry 12h, obtains thin graphene；
Step 2, graphene/mesophase pitch mixed system is prepared：
It will be dissolved in alcohol solvent together with graphene and mesophase pitch that step 1 obtains, then utilize ultrasonic wave graphene
Separating apparatus makes the two uniformly mixing, and acquisition homogeneous solution, which is placed on drying in 80 DEG C of baking ovens, for 24 hours, makes ethyl alcohol thoroughly volatilize；
Step 3, it foams：
The graphene that step 2 is obtained/mesophase pitch mixed system carries out 12h ball millings, then sets obtained powder sample
It in high-temperature high-pressure reaction kettle, is warming up to 500 DEG C and keeps the temperature 3h, be passed through nitrogen protection, pressure 3MPa, after reaction automatically
It is cooled to room temperature, obtains Carbon foam raw material；
Step 4, it carbonizes：
The Carbon foam raw material that step 3 obtains are placed in CVD tube furnaces, nitrogen protection is passed through, be heated to 1000 DEG C and keep the temperature 2h,
Then cooled to room temperature, the Foam carbon composite material after being carbonized；
Step 5, it is graphitized：
By step 4 to charing Carbon foam be put into high temperature graphitization stove, be heated to 2300 DEG C and keep the temperature 2h, lead to N2Gas shielded,
Room temperature is finally cooled to get to graphitizable foams carbon composite.
2. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 1
Middle expanded graphite is 1 part~10 parts according to the mass fraction.
3. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 2
Middle mesophase pitch is coal measures mesophase pitch, interphase content >=95%.
4. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 2
Middle mesophase pitch is 100 parts~200 parts according to the mass fraction.
5. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 3
Middle heating rate is 2 DEG C/min.
6. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 4
The middle specific heat temperature raising mode of carbonization process is：500 DEG C first are warming up to 2 DEG C/min, keeps the temperature 1h, then be warming up to 5 DEG C/min
1000 DEG C, keep the temperature 2h.
7. a kind of preparation method of grapheme foam carbon composite according to claim 1, which is characterized in that step 5
In graphited heating ramp rate be 5 DEG C/min.
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| CN201810643104.2A CN108584942A (en) | 2018-06-21 | 2018-06-21 | A kind of preparation method of grapheme foam carbon composite |
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| CN201810643104.2A CN108584942A (en) | 2018-06-21 | 2018-06-21 | A kind of preparation method of grapheme foam carbon composite |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437160A (en) * | 2018-11-22 | 2019-03-08 | 陕西延长石油（集团）有限责任公司 | A kind of supercapacitor graphene/carbon composite material and preparation method thereof |
| CN110342488A (en) * | 2019-08-16 | 2019-10-18 | 湖南大学 | A kind of preparation method of high-performance foam carbon |
| CN110615433A (en) * | 2019-10-29 | 2019-12-27 | 北京化工大学 | Preparation method of high-thermal-conductivity mesophase pitch-based foamy carbon |
| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN114074935A (en) * | 2020-08-13 | 2022-02-22 | 国家能源投资集团有限责任公司 | Foam carbon material and preparation method thereof |
| CN114843111A (en) * | 2022-05-17 | 2022-08-02 | 清华大学 | Multilevel-structure carbon nanocomposite and preparation method and application thereof |
| CN116082047A (en) * | 2021-11-05 | 2023-05-09 | 天津大学 | Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method |
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| CN104591131A (en) * | 2015-01-27 | 2015-05-06 | 航天材料及工艺研究所 | Preparation method of high-thermal-conductivity graphene-enhanced foamy carbon |
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| CN104591131A (en) * | 2015-01-27 | 2015-05-06 | 航天材料及工艺研究所 | Preparation method of high-thermal-conductivity graphene-enhanced foamy carbon |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437160A (en) * | 2018-11-22 | 2019-03-08 | 陕西延长石油（集团）有限责任公司 | A kind of supercapacitor graphene/carbon composite material and preparation method thereof |
| CN110342488A (en) * | 2019-08-16 | 2019-10-18 | 湖南大学 | A kind of preparation method of high-performance foam carbon |
| CN110342488B (en) * | 2019-08-16 | 2022-11-11 | 湖南大学 | Preparation method of high-performance foam carbon |
| CN110615433A (en) * | 2019-10-29 | 2019-12-27 | 北京化工大学 | Preparation method of high-thermal-conductivity mesophase pitch-based foamy carbon |
| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN114074935A (en) * | 2020-08-13 | 2022-02-22 | 国家能源投资集团有限责任公司 | Foam carbon material and preparation method thereof |
| CN116082047A (en) * | 2021-11-05 | 2023-05-09 | 天津大学 | Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method |
| CN114843111A (en) * | 2022-05-17 | 2022-08-02 | 清华大学 | Multilevel-structure carbon nanocomposite and preparation method and application thereof |
| CN114843111B (en) * | 2022-05-17 | 2024-01-30 | 清华大学 | Multi-level structure carbon nano composite material and preparation method and application thereof |
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