CN106219524A - A kind of low temperature prepares the method for shelly texture elastic graphite alkene foam - Google Patents
A kind of low temperature prepares the method for shelly texture elastic graphite alkene foam Download PDFInfo
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- CN106219524A CN106219524A CN201610555379.1A CN201610555379A CN106219524A CN 106219524 A CN106219524 A CN 106219524A CN 201610555379 A CN201610555379 A CN 201610555379A CN 106219524 A CN106219524 A CN 106219524A
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- foam
- graphite alkene
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- graphite oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
- C01P2006/40—Electric properties
Abstract
The present invention relates to a kind of method that low temperature prepares shelly texture elastic graphite alkene foam, including: graphite oxide at room temperature, is added deionized water and is made into graphite oxide dispersion, ultrasonic agitation by (1), carry out vacuum lyophilization by after solution freezing, obtain graphite oxide foam；(2) above-mentioned graphite oxide foam is immersed reduction in hydroiodic acid, then clean and again freezing, obtain frozen sample；Frozen sample is carried out vacuum lyophilization, to obtain final product.Preparation method of the present invention is simple, it is not necessary to the complicated technologies such as high temperature, and cost of manufacture is cheap；The shelly texture elastic graphite alkene foam of preparation has high surface, light weight, excellent elasticity, high adsorption, has broad application prospects at aspects such as pollutant absorption and circuit devcies.
Description
Technical field
The invention belongs to graphene aerogel field, prepare shelly texture elastic graphite alkene bubble particularly to a kind of low temperature
The method of foam.
Background technology
Graphene (Graphene) is made up of sp2 hydbridized carbon atoms, presents regular hexagon cycle honeycomb dot matrix knot
Structure, its thickness is the least.Graphene has the physical properties such as good conduction, heat conduction, mechanics, is become by scientist first from 2004
The two-dimensional structure of (Novoselov, K.S.et al.Science.2004,3006,666) its uniqueness and excellence since merit is prepared
Performance by the extensive concern of numerous scholars.Mechanical performance, electric property and the thermodynamic property that Graphene is excellent, at electricity
The aspects such as pond, ultracapacitor, drug delivery have a wide range of applications.
Aeroge (Aerogel), also known as xerogel, is the solid material of a kind of porous foam shape, have the lightest density with
And the highest specific surface area.Its appearance is solid-state, and in-house network cavernous structure is filled with gas medium.Graphene aerogel is with stone
The ink aeroge that formed as skeleton of alkene, has been provided simultaneously with the characteristic of Graphene and aeroge, has high porosity, ultralight
Density, good mechanical strength, and the performance such as the electrical conductivity of excellence.It has the special two-dimensional structure of Graphene and excellence
Physico-chemical property make the preparation of graphene aerogel and performance study receive publicity.
At present, there is a variety of method preparing elastic graphite alkene foam.Sink including hydro-thermal method self assembly, chemical gaseous phase
Area method, sol-gel process etc..Hydro-thermal method typically requires higher temperature and pressure；Chemical vapour deposition technique is generally with the nickel of 3D
Foam as substrate, deposited graphite alkene the most thereon, but this method needs high temperature, and cost ratio
Higher.Said method obtains the condition harshness that elastic graphite alkene foam needs, and preparation flow is complicated, and cost is high.
Summary of the invention
The technical problem to be solved is to provide a kind of low temperature and prepares shelly texture elastic graphite alkene foam
Method, the method preparation method is simple, it is not necessary to the complicated technologies such as high temperature, and cost of manufacture is cheap；The shelly texture of preparation is elastic
Grapheme foam has high surface, light weight, excellent elasticity, high adsorption, in sides such as pollutant absorption and circuit devcies
Face has broad application prospects.
A kind of low temperature of the present invention prepares the method for shelly texture elastic graphite alkene foam, including:
(1) at room temperature, graphite oxide adding deionized water and is made into graphite oxide dispersion, ultrasonic agitation, by solution
Carry out vacuum lyophilization after freezing, obtain graphite oxide foam；
(2) above-mentioned graphite oxide foam is immersed reduction in hydroiodic acid, then clean and again freezing, obtain freezing sample
Product；Frozen sample is carried out vacuum lyophilization, obtains shelly texture elastic graphite alkene foam.
The concentration of the graphite oxide dispersion in described step (1) is 15～50mg/mL；Ultrasonic time is 15～72h；Stir
The time of mixing is 24～72h.
Cryogenic temperature in described step (1) is-200 DEG C～-5 DEG C, and cooling time is 1～5h.
Vacuum lyophilization temperature in described step (1) is-60 DEG C～-40 DEG C, the vacuum lyophilization time be 24～
72h, vacuum is 20～200Pa.
During in described step (2), graphite oxide foam immerses hydroiodic acid, the time of reduction is 1～4h.
Cleaning in described step (2) is for cleaning with ethanol and deionized water.
Cryogenic temperature in described step (2) is-200 DEG C～-5 DEG C, and cooling time is 1～5h.
The temperature of the vacuum lyophilization in described step (2) is-60 DEG C～-40 DEG C, and the vacuum lyophilization time is 24
～96h, vacuum is 20～200Pa.
Beneficial effect
(1) preparation method of the present invention is simple, it is not necessary to the complicated technologies such as high temperature, and cost of manufacture is cheap.
(2) present invention directly obtains elastic graphite alkene foam by graphite oxide foam, keeps the original structure of Graphene
Feature, has the mechanical property of excellence, it is possible to bear through many second compression and recover rapidly initial complexion, having good conduction
Property, its resistance changes along with the change of elastic graphite alkene foam shape, can serve as having resilient electronic device.
(3) the shelly texture elastic graphite alkene foam prepared by the present invention has high surface, light weight, excellent bullet
Property, high adsorption, have broad application prospects in pollutant absorption and the aspect such as circuit devcie.
Accompanying drawing explanation
Fig. 1 is the digital photograph that embodiment 1 prepares shelly texture elastic graphite alkene foam；
Fig. 2 is the scanning electron microscope (SEM) photograph that embodiment 1 prepares shelly texture elastic graphite alkene foam；
Fig. 3 is the Raman spectrogram that embodiment 1 prepares shelly texture elastic graphite alkene foam；
Fig. 4 is that embodiment 1 prepares shelly texture elastic graphite alkene foam time m-electricity under cyclic strain 40% acts on
Flow curve.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
At room temperature, weigh graphite oxide 800mg, be placed in the beaker of 50mL, then add deionized water 20mL and be made into dense
Degree is the graphite oxide dispersion of 40mg/mL, then beaker is put into supersound process 24h in Ultrasound Instrument, then adds in beaker
After entering magneton, beaker is placed on magnetic stirring apparatus process 24h, places into supersound process 24h in Ultrasound Instrument.
Dispersion liquid elder generation freezing processing 3h after processing, the temperature of freezing processing is-8 DEG C, then at vacuum lyophilization
Reason 48h, in processing procedure, vacustat is-45 DEG C in about 50Pa, temperature.To the graphite oxide foam hydroiodic acid obtained
Reduction, the time is 2h.Foam ethanol after reduction and deionized water are repeatedly washed, then freezing processing 3h, freezing
The temperature processed be-8 DEG C, then vacuum lyophilization process 48h, and in processing procedure, vacustat is at about 50Pa, temperature is-
45℃.Fig. 1 is the digital photograph of shelly texture elastic graphite alkene foam prepared by the present embodiment, it will thus be seen that elastic graphite
The quality of alkene foam is very light, and calculating density is 0.028g/cm3.Fig. 2 is elastic graphite alkene foam prepared by the present embodiment
Scanning electron microscope (SEM) photograph, it can be seen that foam inside is shelly texture so that it is have the highest porosity.Fig. 3 is the present embodiment system
The Raman spectrogram of standby elastic graphite alkene foam, it will thus be seen that the most bimodal in figure (D peak and G peak) has before and after reduction
Significantly change, the ratio I of peak valued/IgIt is increased to 1.43 after reduction by 0.98 before reducing, shows that reduction reaction makes its structure
Having opened bigger change, reduction degree is the biggest.Fig. 4 is that the time current of elastic graphite alkene foam prepared by the present embodiment is bent
Line, each peak value of appearance shows that now elastic graphite alkene foam is compressed 40%, can be clear and definite in figure find out elastic graphite
When alkene foam occurs quantitative deformation, the electric current of its correspondence becomes the most constant multiple, it can be said that this elastic graphite alkene bright steeps
Foam is when deformation, and its resistance also changes.
Embodiment 2
At room temperature, weigh graphite oxide 600mg, be placed in the beaker of 50mL, then add deionized water 20mL and be made into dense
Degree is the graphite oxide dispersion of 30mg/mL, then beaker is put into supersound process 36h in Ultrasound Instrument, then adds in beaker
After entering magneton, beaker is placed on magnetic stirring apparatus process 36h, places into supersound process 36h in Ultrasound Instrument.
Dispersion liquid elder generation freezing processing 3h after processing, the temperature of freezing processing is-8 DEG C, then at vacuum lyophilization
Reason 48h, in processing procedure, vacustat is-45 DEG C in about 50Pa, temperature.To the graphite oxide foam hydroiodic acid obtained
Reduction, the time is 2h.Foam ethanol after reduction and deionized water are repeatedly washed, then freezing processing 3h, freezing
The temperature processed be-8 DEG C, then vacuum lyophilization process 48h, and in processing procedure, vacustat is at about 50Pa, temperature is-
45℃.The elastic graphite alkene foam obtained is tested, finds that its intensity decreases 10% relative to embodiment 1, survey its Raman
Spectrum, it can be observed that reducing degree keeps consistent with the sample in embodiment 1 substantially.
Embodiment 3
At room temperature, weigh graphite oxide 1000mg, be placed in the beaker of 50mL, then add deionized water 20mL and be made into dense
Degree is the graphite oxide dispersion of 50mg/mL, then beaker is put into supersound process 36h in Ultrasound Instrument, then adds in beaker
After entering magneton, beaker is placed on magnetic stirring apparatus process 36h, places into supersound process 36h in Ultrasound Instrument.
Dispersion liquid elder generation freezing processing 3h after processing, the temperature of freezing processing is-8 DEG C, then at vacuum lyophilization
Reason 48h, in processing procedure, vacustat is-45 DEG C in about 50Pa, temperature.To the graphite oxide foam hydroiodic acid obtained
Reduction, the time is 2h.Foam ethanol after reduction and deionized water are repeatedly washed, then freezing processing 3h, freezing
The temperature processed be-8 DEG C, then vacuum lyophilization process 48h, and in processing procedure, vacustat is at about 50Pa, temperature is-
45℃.The elastic graphite alkene foam obtained is tested, finds that intensity adds 12% relative to embodiment 1.Survey its Raman light
Spectrum, it can be observed that reducing degree is lower slightly compared with the sample in embodiment 1.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (8)
1. the method that low temperature prepares shelly texture elastic graphite alkene foam, including:
(1) at room temperature, graphite oxide adding deionized water and is made into graphite oxide dispersion, ultrasonic agitation, by solution freezing
After carry out vacuum lyophilization, obtain graphite oxide foam；
(2) above-mentioned graphite oxide foam is immersed reduction in hydroiodic acid, then clean and again freezing, obtain frozen sample；Will
Frozen sample carries out vacuum lyophilization, obtains shelly texture elastic graphite alkene foam.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the concentration of the graphite oxide dispersion in described step (1) is 15～50mg/mL；Ultrasonic time is 15～72h；During stirring
Between be 24～72h.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the cryogenic temperature in described step (1) is-200 DEG C～-5 DEG C, and cooling time is 1～5h.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the vacuum lyophilization temperature in described step (1) is-60 DEG C～-40 DEG C, and the vacuum lyophilization time is 24～72h, very
Reciprocal of duty cycle is 20～200Pa.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: during in described step (2), graphite oxide foam immerses hydroiodic acid, the time of reduction is 1～4h.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the cleaning in described step (2) is for cleaning with ethanol and deionized water.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the cryogenic temperature in described step (2) is-200 DEG C～-5 DEG C, and cooling time is 1～5h.
A kind of low temperature the most according to claim 1 prepares the method for shelly texture elastic graphite alkene foam, and its feature exists
In: the temperature of the vacuum lyophilization in described step (2) is-60 DEG C～-40 DEG C, and the vacuum lyophilization time is 24～96h,
Vacuum is 20～200Pa.
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| CN201610555379.1A CN106219524A (en) | 2016-07-15 | 2016-07-15 | A kind of low temperature prepares the method for shelly texture elastic graphite alkene foam |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517162A (en) * | 2016-12-15 | 2017-03-22 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of nitrogen/ sulphur co-doping three-dimensional graphene sponge |
| CN108002366A (en) * | 2017-11-10 | 2018-05-08 | 清华大学 | Graphene solar energy water cleaning foam and its preparation method and application |
| CN110002434A (en) * | 2019-03-26 | 2019-07-12 | 北京理工大学 | A kind of ultralight grapheme foam material of sqouynd absorption lowering noise and preparation method thereof |
Citations (2)
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| CN102674315A (en) * | 2012-04-25 | 2012-09-19 | 浙江大学 | Graphene-carbon nano tube composite all-carbon ultra-light elastic aerogel and preparation method thereof |
| CN103086371A (en) * | 2013-01-24 | 2013-05-08 | 东南大学 | Method for preparing hydrophobic graphene sponge |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674315A (en) * | 2012-04-25 | 2012-09-19 | 浙江大学 | Graphene-carbon nano tube composite all-carbon ultra-light elastic aerogel and preparation method thereof |
| CN103086371A (en) * | 2013-01-24 | 2013-05-08 | 东南大学 | Method for preparing hydrophobic graphene sponge |
Non-Patent Citations (1)
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| 徐方强: "氧化石墨泡沫材料的制备及其对气体的吸附性能研究", 《万方数据库》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517162A (en) * | 2016-12-15 | 2017-03-22 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of nitrogen/ sulphur co-doping three-dimensional graphene sponge |
| CN108002366A (en) * | 2017-11-10 | 2018-05-08 | 清华大学 | Graphene solar energy water cleaning foam and its preparation method and application |
| CN110002434A (en) * | 2019-03-26 | 2019-07-12 | 北京理工大学 | A kind of ultralight grapheme foam material of sqouynd absorption lowering noise and preparation method thereof |
| CN110002434B (en) * | 2019-03-26 | 2021-05-04 | 北京理工大学 | Sound-absorbing noise-reducing ultra-light graphene foam material and preparation method thereof |
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Application publication date: 20161214 |