CN106044752A - Method for preparing high orientation graphene aerogel - Google Patents
Method for preparing high orientation graphene aerogel Download PDFInfo
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- CN106044752A CN106044752A CN201610362004.3A CN201610362004A CN106044752A CN 106044752 A CN106044752 A CN 106044752A CN 201610362004 A CN201610362004 A CN 201610362004A CN 106044752 A CN106044752 A CN 106044752A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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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
Abstract
The invention discloses a high orientation graphene aerogel and a preparation method thereof. The method comprises the steps of first preparing a dispersion liquid of graphene or graphene oxide, placing the dispersion liquid of graphene or graphene oxide in a container with an electrode, obtaining a high orientation graphene or graphene oxide dispersion liquid through an additional electric field orientation method, continuing to maintain an electric field effect, performing freeze freezing in liquid nitrogen, and obtaining the high orientation graphene aerogel after freeze drying or supercritical drying. The high orientation graphene aerogel is high in porosity, pores have a very high degree of orientation in an electric field direction, the pore size is controllable, and the high orientation graphene aerogel can be used for electrode materials of batteries and super capacitors, electron field emission sources, heat insulating and radiating materials, adsorbing materials, high flux water filter materials and catalyst carriers and the like.
Description
Technical field
The present invention relates to the preparation field of graphene aerogel, especially relate to the system of a kind of highly oriented graphene aerogel
Preparation Method.
Background technology
Graphene (Graphene) is a kind of monolayer two dimensional crystal, has the highest intensity of known materials and excellence
Electric conductivity and heat conductivity, be current optimal two-dimension nano materials, have extensively in fields such as material, chemistry, biology, the energy
Wealthy application prospect.2010, two professor Andre Geim and Konstantin of Univ Manchester UK
Novoselov obtains Nobel Prize in physics because being successfully separated out stable Graphene first, has started the whole world to graphite
The upsurge of alkene research.The graphene aerogel of macroscopic view is one of main application form of nanoscale graphite alkene.Because it gives full play to
Graphene specific surface area is big, and chemical stability is good, the advantage that electrical and thermal conductivity is good, graphene aerogel can serve as battery and
The electrode material of ultracapacitor, electronic field emission source, heat insulation and dissipation material, adsorbing material, high flux filtering material and catalysis
Agent carrier etc..
Three-dimensional grapheme can be prepared by methods such as chemical vapor infiltration, ice template method, self-assembly method and hydro-thermal methods
Aeroge.Chemical vapor infiltration is highly dependent on the metal form of three dimensional structure, complex steps, operation complexity, it is difficult to realize
Prepared by large-scale industrialization；Ice template method is with the ice crystal in Graphene or graphene oxide water solution refrigerating process as template
The method preparing aeroge；Self-assembly method and hydro-thermal method utilize liquid crystal liquid crystal property and the anisotropy of Graphene, obtain under certain condition
Must have the aeroge of certain degree of orientation.
Above method lacks the pretreatment to graphene dispersion system and preorientation, it is thus achieved that product structure order is poor.System
The graphene aerogel of height-oriented structure of getting everything ready remains a huge challenge.
Summary of the invention
The problems referred to above existed for prior art, the applicant provides the preparation of a kind of highly oriented graphene aerogel
Method.Gained of the present invention highly oriented graphene aerogel porosity is high, and hole has the highest degree of orientation, hole along direction of an electric field
Size is controlled, can be used for battery and the electrode material of ultracapacitor, electronic field emission source, heat insulation and dissipation material, adsorbing material,
High flux filtering material and catalyst carrier etc..
Technical scheme is as follows:
The applicant provides the preparation method of a kind of highly oriented graphene aerogel, specifically comprises the following steps that
(1) by Graphene and the water mixing of 20～100g of 1g, graphene dispersing solution after ultrasonic disperse, is obtained；
(2) graphene dispersing solution that step (1) prepares is placed in electroded container, by extra electric field to molten
Liquid is orientated 1～100 minute, obtains highly oriented graphene dispersing solution；The frequency of described applied alternating field is 10～1000Hz,
Intensity is 50～5000V/m；
(3) highly oriented graphene dispersing solution step (2) obtained, continues to keep electric field action, freezing in liquid nitrogen
Solidification, further lyophilization or critical lyophilization, obtain highly oriented graphene aerogel.
Preferably, the time of step (1) described ultrasonic disperse is: 10～100 minutes.
Preferably, solution is orientated 1～100 minute by step (2) by extra electric field, obtains highly oriented graphene dispersion
Liquid；The frequency of described applied alternating field is 10～500Hz, and intensity is 10～2000V/m.
The applicant additionally provides the preparation method of a kind of highly oriented graphite oxide aerogel, specifically comprises the following steps that
(1) by graphene oxide and the water mixing of 10～100g of 1g, graphene oxide dispersion after ultrasonic disperse, is obtained；
(2) graphene oxide dispersion that step (1) prepares is placed in electroded container, passes through extra electric field
Solution is orientated 1～100 minute, obtains highly oriented graphene oxide dispersion；The frequency of described applied alternating field is 10
～1000Hz, intensity is 50～5000V/m；
(3) highly oriented graphene oxide dispersion step (2) obtained, continues to keep electric field action, in liquid nitrogen
Cryocoagulation, further lyophilization or critical lyophilization, obtain highly oriented graphite oxide aerogel.
Highly oriented graphite oxide aerogel step (3) obtained obtains ordered porous oxidation by heat treatment reduction
Graphene aerogel；Or the highly oriented graphite oxide aerogel that step (3) obtains is reduced by chemical reducing agent, passes through
Washing is dried to obtain ordered porous graphite oxide aerogel.
Preferably, the time of step (1) described ultrasonic disperse is: 5～50 minutes.
Preferably, solution is orientated 1～100 minute by step (2) by extra electric field, obtains highly oriented graphene dispersion
Liquid；The frequency of described applied alternating field is 10～500Hz, and intensity is 10～2000V/m.
Preferably, step (3) lyophilization or critical cryodesiccated time are 2-40h.
Described reducing agent is selected from:
Mass fraction be the hydrazine hydrate of 1%-40%, mass fraction be that the sodium borohydride aqueous solution of 1%-40%, quality are divided
Number is the vitamin C aqueous solution of 5%-50%, mass fraction is the D/W of 1%-40%, mass fraction is 1%-
The hydriodic acid aqueous solution of 40%, mass fraction be the aqueous acetic acid of 1%-40%, mass fraction be the phenylhydrazine water of 1%-40%
Solution, mass fraction be the hydrobromic acid aqueous solution of 1%-40%, mass fraction be that the tea polyphenols aqueous solution of 1%-40%, quality are divided
Number is the aqueous solution of urea of 1%-40%, mass fraction is the sodium thiosulfate solution of 1%-20%, mass fraction is 1%-
The sodium hydrate aqueous solution of 5%, mass fraction are the potassium hydroxide aqueous solution of 1%-40% or mass fraction is 1%-40%'s
Phenol solution.
Useful the having the technical effect that of the present invention
(1) using Graphene or graphene oxide is raw material, prepared by applicable heavy industrialization；
(2) preparation method makes full use of Graphene liquid crystal attribute, easy and simple to handle, environmental protection, it is not necessary to add other auxiliary
Helping property material；
(3) extra electric field frequency and intensity are controlled, and the graphene aerogel degree of orientation of preparation can freely control；
(4) the highly oriented graphene aerogel density prepared can regulate, and the direction being perpendicular to be orientated electric field has good
Elasticity, has thermal conductance and the electric conductivity of excellence simultaneously.
Accompanying drawing explanation
Fig. 1 is electric field induced orientation Graphene or the principle schematic of graphene oxide dispersion；
Fig. 2 is the electron scanning micrograph of graphene aerogel section.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the present invention is specifically described.
As it is shown in figure 1, utilize Graphene liquid crystal that prepared by the response of extra electric field three-dimensional graphene aerogel.
The highly oriented graphene aerogel that this method obtains, Graphene orientations is formed along direction of an electric field through hole, density
For 0.02-0.5g/cm3, the compressive strength being perpendicular to be orientated direction of an electric field is 1-15MPa, and conductivity is more than 1000S/m, hole
Rate is 80%-99.5%.This graphene aerogel with macrovoid through-hole structure can serve as the structural wood of high surface area
Material, is conducive to the diffusion of ion as electrode material, can filter pollutant with rapid adsorption as material for water treatment and keep big
Flux, can realize several functions by the different guest materials of load.
Being described specifically the present invention below in conjunction with embodiment, the present embodiment is served only for being the present invention further
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment, belong to protection scope of the present invention.
Embodiment 1:
(1) add the Graphene of 1g, the water of 6g, in 24 DEG C with the supersound process 1 hour of 12KHz, obtain graphene dispersion
Liquid；
(2) graphene dispersing solution that step (1) obtains is placed in electroded container, is 1000Hz by frequency, by force
Solution is orientated 100 minutes by the extra electric field that degree is 2000V/m, it is thus achieved that highly oriented graphene dispersing solution；
(3) highly oriented graphene dispersing solution step (2) obtained, continues to keep electric field action, freezing in liquid nitrogen
Solidification, further lyophilization or critical lyophilization 40h, obtain highly oriented graphene aerogel；
As in figure 2 it is shown, the highly oriented graphene aerogel of gained, Graphene orientations is formed along direction of an electric field through hole,
Density is 0.2g/cm3, the compressive strength being perpendicular to be orientated direction of an electric field is 15MPa, and the degree of orientation is more than 80%, and conductivity is more than
1000S/m, porosity is 90%, can be as efficient material for water treatment, and when pollutant levels are less than 20mg/mL, adsorption rate can
To reach 95%.
Embodiment 2:
(1) add the Graphene of 1g, the water of 100g, in 60 DEG C with the supersound process 10 hours of 5KHz, obtain Graphene and divide
Dissipate liquid；
(2) graphene dispersing solution prepared by step (1) is placed in electroded container, is 50Hz by frequency, intensity
Solution is orientated 80 minutes by the extra electric field for 1000V/m, it is thus achieved that highly oriented graphene dispersing solution；
(3) highly oriented graphene dispersing solution step (2) obtained, continues to keep electric field action, freezing in liquid nitrogen
Solidification, further lyophilization or critical lyophilization 3h, obtain highly oriented graphene aerogel；
The highly oriented graphene aerogel of gained, Graphene orientations is formed along direction of an electric field through hole, and density is
0.01g/cm3, the compressive strength being perpendicular to be orientated direction of an electric field is 1MPa, and the degree of orientation is more than 90%, and conductivity is more than 1000S/
M, porosity is 99%.
Embodiment 3:
(1) add the graphene oxide of 1g, the water of 30g, in 40 DEG C with the supersound process 5 hours of 10KHz, obtain aoxidizing stone
Ink alkene dispersion liquid；
(2) graphene oxide dispersion prepared by step (1) is placed in electroded container, is 500Hz by frequency,
Intensity is that solution is orientated 50 minutes by the extra electric field of 2000V/m, it is thus achieved that highly oriented graphene oxide dispersion；
(3) highly oriented graphene oxide dispersion step (2) obtained, continues to keep electric field action, in liquid nitrogen
Cryocoagulation, further lyophilization 25h, obtain highly oriented graphite oxide aerogel；
(4) ordered porous oxidation graphite oxide aerogel step (3) obtained is obtained in order by heat treatment reduction
The graphite oxide aerogel of porous；
The highly oriented graphene aerogel of gained, Graphene orientations is formed along direction of an electric field through hole, and density is 0.5g/
cm3, the compressive strength being perpendicular to be orientated direction of an electric field is 6MPa, and the degree of orientation is more than 85%, and conductivity is more than 1000S/m, hole
Rate is 95.8%.
Embodiment 4:
(1) add the graphene oxide of 1g, the water of 5g, in 35 DEG C with the supersound process 1 hour of 15KHz, obtain aoxidizing stone
Ink alkene dispersion liquid；
(2) graphene oxide dispersion prepared by step 1 is placed in electroded container, is 50Hz by frequency, by force
Solution is orientated 75 minutes by the extra electric field that degree is 2000V/m, it is thus achieved that highly oriented graphene oxide dispersion；
(3) highly oriented graphene oxide dispersion step (2) obtained, continues to keep electric field action, in liquid nitrogen
Cryocoagulation, the most critical lyophilization 25h, obtain highly oriented graphite oxide aerogel；
(4) it is reduction 8 in 10% hydrazine hydrate that the ordered porous graphene oxide membrane that step (3) obtains is placed in mass fraction
Hour, washing is dried to obtain Graphene porous Ordered Film.
The highly oriented graphene aerogel of gained, Graphene orientations is formed along direction of an electric field through hole, and density is 0.03-
0.07g/cm3, the compressive strength being perpendicular to be orientated direction of an electric field is 2-4MPa, and the degree of orientation is more than 85%, and conductivity is more than
1000S/m, porosity is 94%, can be as efficient material for water treatment, and when pollutant levels are less than 20mg/mL, adsorption rate can
To reach 98%.
Claims (9)
1. the preparation method of a highly oriented graphene aerogel, it is characterised in that specifically comprise the following steps that
(1) by Graphene and the water mixing of 20～100g of 1g, graphene dispersing solution after ultrasonic disperse, is obtained；
(2) graphene dispersing solution that step (1) prepares is placed in electroded container, by extra electric field, solution is taken
To 1～100 minute, obtain highly oriented graphene dispersing solution；The frequency of described applied alternating field is 10～1000Hz, intensity
It is 50～5000V/m；
(3) the highly oriented graphene dispersing solution that step (2) is obtained, continuation holding electric field action, cryocoagulation in liquid nitrogen,
Further lyophilization or critical lyophilization, obtain highly oriented graphene aerogel.
Preparation method the most according to claim 1, it is characterised in that the time of step (1) described ultrasonic disperse is: 10～
100 minutes.
Preparation method the most according to claim 1, it is characterised in that step (2) by extra electric field to solution orientation 1～
100 minutes, obtain highly oriented graphene dispersing solution；The frequency of described applied alternating field is 10～500Hz, intensity be 10～
2000V/m。
4. the preparation method of a highly oriented graphite oxide aerogel, it is characterised in that specifically comprise the following steps that
(1) by graphene oxide and the water mixing of 10～100g of 1g, graphene oxide dispersion after ultrasonic disperse, is obtained；
(2) graphene oxide dispersion that step (1) prepares is placed in electroded container, by extra electric field to molten
Liquid is orientated 1～100 minute, obtains highly oriented graphene oxide dispersion；The frequency of described applied alternating field be 10～
1000Hz, intensity is 50～5000V/m；
(3) highly oriented graphene oxide dispersion step (2) obtained, continues to keep electric field action, freezing in liquid nitrogen
Solidification, further lyophilization or critical lyophilization, obtain highly oriented graphite oxide aerogel.
Preparation method the most according to claim 4, it is characterised in that the highly oriented graphene oxide gas that step (3) is obtained
Gel obtains ordered porous graphite oxide aerogel by heat treatment reduction；Or the highly oriented oxygen that step (3) is obtained
Functionalized graphene aeroge is reduced by chemical reducing agent, is dried to obtain ordered porous graphite oxide aerogel through washing.
Preparation method the most according to claim 4, it is characterised in that the time of step (1) described ultrasonic disperse is: 5～50
Minute.
Preparation method the most according to claim 4, it is characterised in that step (2) by extra electric field to solution orientation 1～
100 minutes, obtain highly oriented graphene dispersing solution；The frequency of described applied alternating field is 10～500Hz, intensity be 10～
2000V/m。
8. according to the preparation method described in claim 1 or 4, it is characterised in that step (3) lyophilization or critical freezing are done
The dry time is 2-40h.
Preparation method the most according to claim 5, it is characterised in that described reducing agent is selected from:
Mass fraction be the hydrazine hydrate of 1%-40%, mass fraction be that the sodium borohydride aqueous solution of 1%-40%, mass fraction are
The vitamin C aqueous solution of 5%-50%, mass fraction be the D/W of 1%-40%, mass fraction be 1%-40%'s
Hydriodic acid aqueous solution, mass fraction be the aqueous acetic acid of 1%-40%, mass fraction be the phenylhydrazine aqueous solution of 1%-40%, matter
Amount mark be the hydrobromic acid aqueous solution of 1%-40%, mass fraction be that the tea polyphenols aqueous solution of 1%-40%, mass fraction are
The aqueous solution of urea of 1%-40%, mass fraction be the sodium thiosulfate solution of 1%-20%, mass fraction be 1%-5%'s
Sodium hydrate aqueous solution, mass fraction are the potassium hydroxide aqueous solution of 1%-40% or mass fraction is the phenol of 1%-40%
Aqueous solution.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108262012A (en) * | 2018-01-24 | 2018-07-10 | 上海理工大学 | A kind of preparation method of graphene aerogel air purifying filter mesh |
| CN109320286A (en) * | 2018-11-14 | 2019-02-12 | 武汉纺织大学 | The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure |
| CN110010364A (en) * | 2019-04-28 | 2019-07-12 | 清华大学 | Graphene-based orderly high density porous carbon and its preparation method and application |
| CN110857894A (en) * | 2018-08-24 | 2020-03-03 | 中山大学 | Flexible mechanical sensor capable of detecting stress direction based on ordered graphene and preparation method thereof |
| CN111204852A (en) * | 2020-01-17 | 2020-05-29 | 四川农业大学 | Livestock and poultry wastewater tail water treatment system |
| CN111591978A (en) * | 2020-05-29 | 2020-08-28 | 成都理工大学 | Preparation method for preparing graphene air filter element on large scale |
| CN112852386A (en) * | 2021-01-25 | 2021-05-28 | 武汉科技大学 | High-orientation layered graphene aerogel phase-change composite material and preparation method thereof |
| WO2022120712A1 (en) * | 2020-12-10 | 2022-06-16 | 中国科学院深圳先进技术研究院 | Size-controllable aerogel ball and preparation method and application thereof |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN115341306A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | Graphene aerogel fiber and preparation method thereof |
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| CN108262012A (en) * | 2018-01-24 | 2018-07-10 | 上海理工大学 | A kind of preparation method of graphene aerogel air purifying filter mesh |
| CN110857894A (en) * | 2018-08-24 | 2020-03-03 | 中山大学 | Flexible mechanical sensor capable of detecting stress direction based on ordered graphene and preparation method thereof |
| CN110857894B (en) * | 2018-08-24 | 2021-06-04 | 中山大学 | Flexible mechanical sensor capable of detecting stress direction based on ordered graphene and preparation method thereof |
| CN109320286B (en) * | 2018-11-14 | 2021-08-20 | 武汉纺织大学 | Magnetic graphene-based aerogel material with ordered structure and preparation method thereof |
| CN109320286A (en) * | 2018-11-14 | 2019-02-12 | 武汉纺织大学 | The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure |
| CN110010364A (en) * | 2019-04-28 | 2019-07-12 | 清华大学 | Graphene-based orderly high density porous carbon and its preparation method and application |
| CN111204852A (en) * | 2020-01-17 | 2020-05-29 | 四川农业大学 | Livestock and poultry wastewater tail water treatment system |
| CN111591978A (en) * | 2020-05-29 | 2020-08-28 | 成都理工大学 | Preparation method for preparing graphene air filter element on large scale |
| WO2022120712A1 (en) * | 2020-12-10 | 2022-06-16 | 中国科学院深圳先进技术研究院 | Size-controllable aerogel ball and preparation method and application thereof |
| CN112852386A (en) * | 2021-01-25 | 2021-05-28 | 武汉科技大学 | High-orientation layered graphene aerogel phase-change composite material and preparation method thereof |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN114853502B (en) * | 2022-05-26 | 2023-05-12 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN115341306A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | Graphene aerogel fiber and preparation method thereof |
| CN115341306B (en) * | 2022-09-23 | 2023-04-28 | 内蒙古大学 | Graphene aerogel fiber and preparation method thereof |
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Inventor after: Liu Zheng Inventor after: Wang Qinsheng Inventor after: Yang Yongqiang Inventor after: Liu Yuan Inventor after: Jin Ling Inventor after: Cheng Xiaobao Inventor before: Liu Zheng Inventor before: Wang Qinsheng Inventor before: Yang Yongqiang Inventor before: Liu Yuan Inventor before: Jin Ling Inventor before: Chen Xiaobao |
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