CN110357080A - A kind of three-dimensional grapheme and preparation method thereof - Google Patents
A kind of three-dimensional grapheme and preparation method thereof Download PDFInfo
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- CN110357080A CN110357080A CN201910794169.1A CN201910794169A CN110357080A CN 110357080 A CN110357080 A CN 110357080A CN 201910794169 A CN201910794169 A CN 201910794169A CN 110357080 A CN110357080 A CN 110357080A
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- dimensional grapheme
- nickel foam
- nickel
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- foam
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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
- C01B32/186—Preparation by chemical vapour deposition [CVD]
Abstract
The invention discloses a kind of three-dimensional graphemes, the graphene sheet layer of nickel sheet and tight outside nickel foam including show bubble, and the graphene sheet layer outside foam nickel skeleton constitutes three-dimensional grapheme.Also disclose a kind of preparation method of three-dimensional grapheme, comprising: dehydrated alcohol is fitted into volatilization room, heating volatilization, while being passed through argon hydrogen mixture as carrying gas, the alcohol vapour that carrying gas takes away volatilization, which enters, to be placed in the CVD tube furnace of nickel foam.Wherein (1) dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；(2) nickel foam is cut into circle that diameter is 1.5 ㎝ as substrate, puts several copper foils as catalyst near nickel foam；(3) three-dimensional grapheme can be obtained on nickel foam substrate by reacting 30-90 minutes in CVD tube furnace.The present invention uses chemical vapour deposition technique, and raw material sources are easy to get, and cost is relatively low, and three-dimensional grapheme obtained has excellent engineering properties, higher flexibility.
Description
Technical field
The present invention relates to a kind of three-dimensional graphemes and preparation method thereof.
Background technique
Big specific surface area, high conductivity and the high chemical stability of three-dimensional grapheme make graphene become electrification
Learn the electrode material for having very much a potentiality of double layer capacitor (EDLC).The stacking of graphene makes its 2600m2The specific surface area of/g is not
It can full utilization and corresponding 550F.g-1Intrinsic specific capacitance also fail to give full play to.3D graphene increases electrode
Can and specific surface area, improve the conductivity of graphene network and have and be conducive to the porous logical of electrolyte intermediate ion transmission
Road, these features allow graphene to become a kind of good electrode material for super capacitor.
Graphene due to its high conductivity, big specific surface area, high chemical stability and to catalyst granules it is strong
Adhesive force be also considered as fuel-cell catalyst application a strong candidate.Graphene or the surface GO are a large amount of
Functional group can provide more chances for the nucleation of catalyst nano-particles and attachment.The promising graphene of these features is in fuel
Application in terms of battery provides condition.
The graphene and graphene oxide of three-dimensional structure possess huge specific surface area, it is thus possible to provide a large amount of absorption
Active site: this porous material has very big porosity, therefore has huge absorption space.3D grapheme material tool
There is good gas sorption ability, and is proved to be to remove water pollutant (such as organic solvent, oil, heavy metal ion and dye
Colour solid) it is effective absorption and absorbing material.Therefore graphene 3D material can be used for adsorbing pernicious gas and water in air
Resource purification.In addition, hydrogen molecule due to that can be adsorbed on two sides thus be expected to have very high hydrogen storage capability by graphene.Base
Pass through the electrical conductance, shape and the volume that change itself in terms of as the sensor of various analytes in the porous structure of graphene
With very big application potential.
Summary of the invention
The present invention uses ethyl alcohol as carbon source by CVD method, nickel foam as substrate, and copper foil is as catalyst, at 1050 DEG C
Temperature under the conditions of in foam nickel surface prepare high quality three-dimensional grapheme, wherein foam nickel base is easy in certain item
It is etched under part, to obtain the higher three-dimensional grapheme of purity.
The technical problems to be solved by the present invention are: overcome the deficiencies of the prior art and provide a kind of three-dimensional grapheme and its
Preparation method, the graphene have excellent engineering properties and higher flexibility, and the preparation method step is simple, to metal substrate
It is required that low.
In order to solve the above-mentioned technical problem, the technical scheme is that a kind of three-dimensional grapheme, including nickel foam and
Graphene sheet layer of the tight outside nickel foam, the graphene sheet layer outside nickel foam constitute three-dimensional grapheme.
The present invention also provides a kind of preparation methods of three-dimensional grapheme, comprising the following steps:
Step S1: dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；Step S2: nickel foam is cut into diameter and is
The circle of 1.5 ㎝ is as substrate, and copper foil is as catalyst；Step S3: reacting 30-90 minutes in CVD tube furnace can steep
Three-dimensional grapheme is obtained on foam nickel substrate.
Further, in the step S1, the capacity for room of volatilizing is 250 milliliters, is equipped with 100 milliliters of dehydrated alcohol, volatilization temperature
Degree is 80 DEG C.
Further, in the step S2, nickel foam is cut into the circle that diameter is 1.5 ㎝, is placed in quartz boat, nickel foam is attached
Several copper foils are closely put as catalyst, quartz boat are put into the quartz ampoule of CVD tube furnace.
Further, in the step S3, nickel foam is heated to 1050 DEG C in non-oxidizing gas environment, is finally passed through
The argon hydrogen mixture for carrying alcohol vapour of 5sccm reacts 30-90 minutes.
After above-mentioned technical proposal, the invention has the following advantages: 1) three-dimensional grapheme of the invention has
Excellent engineering properties, higher flexibility have huge application prospect in energy storage device, photovoltaic device, sensor field；
2) method that the present invention is combined using chemical vapor deposition, raw material sources are easy to get, and cost is relatively low；3) using copper foil as catalysis
Agent substantially increases the success rate of experiment；4) preparation method of the invention is simple, and the chemical reagent integrally used is less, right
Environmental pollution is smaller.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of three-dimensional grapheme of the invention；Fig. 2 is three-dimensional grapheme of the invention
Raman characterization figure.
Specific embodiment
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment one
A kind of three-dimensional grapheme, the graphene sheet layer of nickel screen and tight outside nickel foam including show bubble, stone
Black alkene lamella constitutes three-dimensional grapheme.
It can be seen from the electron scanning micrograph of the graphene fiber of Fig. 1, graphene is in the form of sheets；From the Raman of Fig. 2
Phenogram can be seen that graphene fiber has the characteristic peak of the graphenes such as the peak D, the peak G and the peak 2D, the intensity ratio at the peak 2D and the peak G
(I2D/IG) thickness of graphene sheet layer is represented, intensity ratio is bigger, and thickness is smaller, and for intensity than smaller, thickness is bigger.
Embodiment two
The present invention also provides a kind of preparation methods of three-dimensional grapheme, comprising the following steps:
Step S1: dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；Step S2: nickel foam is cut into diameter and is
The circle of 1.5 ㎝ is as substrate, and copper foil is as catalyst；Step S3: reacting 30-90 minutes in CVD tube furnace can steep
Three-dimensional grapheme is obtained on foam nickel substrate.
Preferably, in the step S1, the capacity for room of volatilizing is 250 milliliters, is equipped with 100 milliliters of dehydrated alcohol, volatilization temperature
Degree is 80 DEG C.
Preferably, in the step S2, nickel foam is cut into the circle that diameter is 1.5 ㎝, is placed in quartz boat, nickel foam is attached
Several copper foils are closely put as catalyst, quartz boat are put into the quartz ampoule of CVD tube furnace.
Preferably, in the step S3, nickel foam is heated to 1050 DEG C in non-oxidizing gas environment, is finally passed through
The argon hydrogen mixture for carrying alcohol vapour of 5sccm reacts 30 minutes.
Optionally, the non-oxidizing gas is Ar gas.
Preferably, the preparation method further includes the steps that etching, etch step are as follows: will obtain on nickel foam substrate
Three-dimensional grapheme, be put into sodium peroxydisulfate solution, substrate etching fallen, then cleaned repeatedly for several times with deionized water, Ji Kezhuan
It moves on in any required substrate.
Embodiment three
A kind of preparation method of three-dimensional grapheme, comprising the following steps:
Step S1: dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；Step S2: nickel foam is cut into diameter and is
The circle of 1.5 ㎝ is as substrate, and copper foil is as catalyst；Step S3: reacting 30-90 minutes in CVD tube furnace can steep
Three-dimensional grapheme is obtained on foam nickel substrate.
Preferably, in the step S1, the capacity for room of volatilizing is 250 milliliters, is equipped with 100 milliliters of dehydrated alcohol, volatilization temperature
Degree is 80 DEG C.
Preferably, in the step S2, nickel foam is cut into the circle that diameter is 1.5 ㎝, is placed in quartz boat, nickel foam is attached
Several copper foils are closely put as catalyst, quartz boat are put into the quartz ampoule of CVD tube furnace.
Preferably, in the step S3, nickel foam is heated to 1050 DEG C in non-oxidizing gas environment, is finally passed through
The argon hydrogen mixture for carrying alcohol vapour of 5sccm reacts 60 minutes.
Optionally, the non-oxidizing gas is H2And N2The mixed mixed gas of arbitrary proportion.
Example IV
A kind of preparation method of three-dimensional grapheme, comprising the following steps:
Step S1: dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；Step S2: nickel foam is cut into diameter and is
The circle of 1.5 ㎝ is as substrate, and copper foil is as catalyst；Step S3: reacting 30-90 minutes in CVD tube furnace can steep
Three-dimensional grapheme is obtained on foam nickel substrate.
Preferably, in the step S1, the capacity for room of volatilizing is 250 milliliters, is equipped with 100 milliliters of dehydrated alcohol, volatilization temperature
Degree is 80 DEG C.
Preferably, in the step S2, nickel foam is cut into the circle that diameter is 1.5 ㎝, is placed in quartz boat, nickel foam is attached
Several copper foils are closely put as catalyst, quartz boat are put into the quartz ampoule of CVD tube furnace.
Preferably, in the step S3, nickel foam is heated to 1050 DEG C in non-oxidizing gas environment, is finally passed through
The argon hydrogen mixture for carrying alcohol vapour of 5sccm reacts 90 minutes.
Optionally, the non-oxidizing gas is N2Gas.
Three-dimensional grapheme of the invention is that one layer of graphene sheet layer has been wrapped up outside the preferable nickel foam of electric conductivity, these
Graphene sheet layer is combined closely with internal nickel foam, so that the three-dimensional grapheme has excellent engineering properties, it is higher soft
Property, there is huge application prospect in energy storage device, photovoltaic device, sensor field.
The present invention uses chemical vapour deposition technique, and raw material sources are easy to get, and cost is relatively low.
For the present invention using nickel foam as substrate, copper foil largely improves the success rate of experiment as catalyst.It adopts
It uses nickel foam as substrate, but also the three-dimensional grapheme toughness prepared is strong, and the reaction time can be led to adjust graphite
The number of plies of alkene.
Preparation method of the invention is simple, and the chemical reagent integrally used is less, and environmental pollution is smaller.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of three-dimensional grapheme, it is characterised in that: nickel sheet and tight including show bubble are outside nickel foam
Graphene sheet layer, the graphene sheet layer outside nickel foam constitute three-dimensional grapheme, and the three-dimensional grapheme of this method preparation has
Good mechanical performance and flexibility have good electric conductivity, biggish specific surface area.
2. a kind of preparation method of three-dimensional grapheme according to claim 1, which comprises the following steps:
Step S1: dehydrated alcohol volatilizees under the conditions of 80 DEG C, and alcohol vapour is as carbon source；Step S2: nickel foam is cut into diameter and is
The circle of 1.5 ㎝ is as substrate, and copper foil is as catalyst；Step S3: reacting 30-90 minutes in CVD tube furnace can steep
Three-dimensional grapheme is obtained on foam nickel substrate.
3. the preparation method of three-dimensional grapheme fiber according to claim 2, it is characterised in that: in the step S1, wave
The capacity for sending out room is 250 milliliters, is equipped with 100 milliliters of dehydrated alcohol, volatilization temperature is 80 DEG C.
4. the preparation method of three-dimensional grapheme according to claim 2, it is characterised in that: in the step S2, nickel foam
It is cut into the circle that diameter is 1.5 ㎝, is placed in quartz boat, nickel foam nearby puts several copper foils as catalyst, and quartz boat is put
In the quartz ampoule for entering CVD tube furnace.
5. the preparation method of three-dimensional grapheme according to claim 2, it is characterised in that: in the step S3, nickel foam
It is heated to 1050 DEG C in non-oxidizing gas environment, is finally passed through the argon hydrogen mixture for carrying alcohol vapour of 5sccm,
Reaction 30-90 minutes.
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| CN201910794169.1A CN110357080A (en) | 2019-08-27 | 2019-08-27 | A kind of three-dimensional grapheme and preparation method thereof |
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| CN201910794169.1A CN110357080A (en) | 2019-08-27 | 2019-08-27 | A kind of three-dimensional grapheme and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111675209A (en) * | 2020-06-02 | 2020-09-18 | 天津理工大学 | Method for growing vertical graphene film by using nitrogen and ethanol |
| CN115403800A (en) * | 2022-09-28 | 2022-11-29 | 佳木斯大学 | Preparation method of polyimide/three-dimensional graphene composite film with high dielectric constant |
-
2019
- 2019-08-27 CN CN201910794169.1A patent/CN110357080A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111675209A (en) * | 2020-06-02 | 2020-09-18 | 天津理工大学 | Method for growing vertical graphene film by using nitrogen and ethanol |
| CN115403800A (en) * | 2022-09-28 | 2022-11-29 | 佳木斯大学 | Preparation method of polyimide/three-dimensional graphene composite film with high dielectric constant |
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Application publication date: 20191022 |