CN106348282A - Double helix carbon fiber graphene composite material and preparation method thereof - Google Patents
Double helix carbon fiber graphene composite material and preparation method thereof Download PDFInfo
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- CN106348282A CN106348282A CN201610707861.2A CN201610707861A CN106348282A CN 106348282 A CN106348282 A CN 106348282A CN 201610707861 A CN201610707861 A CN 201610707861A CN 106348282 A CN106348282 A CN 106348282A
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention discloses a double helix carbon fiber graphene composite material and a preparation method thereof, wherein the double helix carbon fiber graphene composite material is formed by compounding double helix carbon fiber and graphene, wherein the double helix carbon fiber accounts for 1 to 99 percent of the total mass; the fiber diameter of the double helix carbon fiber is 0.1 to 1mu m, the helix diameter is 5 to 10mu m, and the helix length is 10 to 100mu m; the graphene is in a single-sheet or multi-sheet stacked shape, the sheet diameter is 1 to 200mu m, and the thickness is 1 to 50nm. The double helix carbon fiber graphene composite material, particularly the double helix carbon fiber graphene composite material prepared by a hydrothermal compounding method has the characteristics of porosity, large specific surface, good electric conductibility and the like; wide application prospects are realized in aspects of supercapacitor electrode materials, electromagnetic wave absorption/shielding materials, hydrogen storage materials, the improvement of the electroconductibility of the composite material and the like.
Description
Technical field
The invention belongs to technical field of composite materials and in particular to a kind of Double helix carbon fiber and graphite alkene composite and its
Preparation method.
Background technology
Nineteen ninety Gifu, Japan university s.motojima etc. under the conditions of 800 DEG C about, using metal ni as catalyst,
Carbon fiber double-stranded similar to dna is prepared using catalysis pyrolysis acetylene gas method, the Double helix carbon of acquisition is fine
A diameter of 0.1～0.3 μm of dimension (carbon microcoils), screw diameter is 2～8 μm, and helix length is 0.1～5mm, should
Method favorable reproducibility, is that optimum can enable to prepare one of method of Double helix carbon fiber in a large number.Nineteen ninety-five is further in employingization
It is passed through a small amount of sulfur-containing compound (h during learning vapour deposition process (cvd) preparation2S or thiophene) obtain double spiral shells of regular appearance
The carbon fiber of rotation structure.Double helix carbon fiber because of itself special three-dimensional double-spiral structure similar to dna and has Gao Bimo
Amount, super-elasticity, high-specific surface area, of a relatively high electric conductivity and typically chiral the features such as, absorb/screen in new electromagnetic wave
Cover material, Microspring, the detecting element of touch sensor, hydrogen storage material, catalyst carrier, improve the electric conductivity of composite with
And the aspect such as biomedical material has very wide application prospect.
Graphene is with sp by carbon atom2The tightly packed two-dimensional structure green wood with honeycomb lattice obtaining of hybrid form
Material, be at present in the world known the thinnest be also monolayer laminated structure new material the hardest.Carbon atom in Graphene leads to
The strong σ key of overstability simultaneously combines the π key effect hexagon planar structure stable with 3 adjacent carbon atoms compositions, can not only
Enough bear high pressure and pulling force, and there is excellent electric conductivity；Its heat conductivility is significantly larger than most common gold
Belong to, excellent heat conductivity makes it have very big potentiality as the nanometer heat sink material of super large-scale integration.Additionally, graphite
Alkene also has the features such as higher light transmission and good gas barrier property, therefore, carries out extensive and deep base to it
Plinth and applied research, have important scientific meaning.Prepare the conventional method of Graphene at present to be mechanical stripping method, aoxidize also
Former method, carborundum pyrolysismethod and chemical vapour deposition technique.
Content of the invention
It is an object of the invention to provide a kind of Double helix carbon fiber and graphite alkene composite.
Another object of the present invention is to providing the preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite.
The concrete technical scheme of the present invention is as follows:
A kind of Double helix carbon fiber and graphite alkene composite, it is composited by Double helix carbon fiber and Graphene, wherein
Double helix carbon fiber accounts for the 1～99% of gross mass；The fibre diameter of Double helix carbon fiber is 0.1～1 μm, screw diameter 5～10 μ
M, helix length is 10～100 μm；Graphene be single sheet or multi-disc stacked, piece footpath be 1～200 μm, thickness be 1～
50nm.
In a preferred embodiment of the invention, described Double helix carbon fiber accounts for the 1～50% of gross mass.
One of preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprises the steps:
(1) obtain Graphene；
(2) above-mentioned Graphene is added in organic solvent, ultrasonic disperse 0.5～2h, obtains graphene suspension；Above-mentioned
Organic solvent is n- methyl pyrrolidone, n, at least one in n- dimethylformamide, ethanol, chloroform and oxolane.
(3) Double helix carbon fiber is added in above-mentioned graphene suspension, Double helix carbon is made by magnetic agitation effect
Fiber is mixed further with Graphene, after removing solvent, described Double helix carbon fiber and graphite alkene composite is obtained.
In a preferred embodiment of the invention, described step (1) is: by graphene oxide be dispersed in from
In sub- water, ultrasonic stripping obtains graphene oxide solution, is subsequently added into 0.5～5 times of graphene oxide quality of reducing agent,
React 2～48h at a temperature of 50～100 DEG C, filter to obtain filter cake after completion of the reaction, this filter cake is carried out removing by detergent
Unreacted reducing agent, last lyophilization, described Graphene is obtained.
It is further preferred that described reducing agent is hydrazine hydrate, phenylhydrazine, sodium borohydride, sodium citrate, hydroquinone and Wei Sheng
At least one of plain c；Described detergent is water, ethanol and n, at least one in n- dimethylformamide.
In a preferred embodiment of the invention, described step (1) is: graphene oxide is dispersed in deionized water
In, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide solution, then by this graphene oxide solution in 120～200
DEG C carry out reduction reaction 12～48h, last lyophilization, described Graphene is obtained.
The two of the preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprise the steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide
Solution；
(2) in above-mentioned graphene oxide solution, 0.5～5 times of reducing agent of graphene oxide quality and double spiral shell are added
Mix homogeneously after rotation carbon fiber, reacts 2～48h at 50～100 DEG C, filters to obtain filter cake after completion of the reaction, and this filter cake passes through to wash
Wash agent to be carried out, to remove unreacted reducing agent, last lyophilization, described Double helix carbon fiber and graphite alkene being obtained and being combined
Material.
In a preferred embodiment of the invention, described reducing agent is hydrazine hydrate, phenylhydrazine, sodium borohydride, citric acid
At least one of sodium, hydroquinone and vitamin c；Described detergent is water, ethanol and n, in n- dimethylformamide at least
A kind of.
The three of the preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprise the steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide
Solution；
(2) in above-mentioned graphene oxide solution, after adding Double helix carbon fiber, mix homogeneously obtains mixed liquor, then should
Mixed liquor carries out reduction reaction 12～48h, last lyophilization in 120～200 DEG C, and described Double helix carbon fiber and graphite alkene is obtained
Composite.
The invention has the beneficial effects as follows: the Double helix carbon fiber and graphite alkene composite of the present invention, especially by hydro-thermal
The Double helix carbon fiber and graphite alkene composite that composite algorithm prepares has porous, Large ratio surface and good electric conductivity etc.
Feature, in electrode material for super capacitor, electro-magnetic wave absorption/shielding material, hydrogen storage material, improves electric conductivity of composite etc.
Aspect has broad application prospects.
Brief description
Fig. 1 be the embodiment of the present invention 5 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
One.
Fig. 2 be the embodiment of the present invention 5 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
Two.
Fig. 3 be the embodiment of the present invention 5 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
Three.
Fig. 4 be the embodiment of the present invention 6 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
One.
Fig. 5 be the embodiment of the present invention 6 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
Two.
Fig. 6 be the embodiment of the present invention 6 prepared by Double helix carbon fiber and graphite alkene composite stereoscan photograph it
Three.
Specific embodiment
Combine accompanying drawing below by way of specific embodiment technical scheme is further detailed and to describe.
Graphene oxide described in following embodiments is to be prepared by improved hummer method, specific as follows::
Selection granularity is 8000 mesh and the natural flaky graphite of 150 purposes is raw material respectively, dense in about 100ml 98%
In sulphuric acid, it is slowly added to this natural flake graphite of 2g under condition of ice bath, is stirred using magnetic stirring apparatuss low speed, weighs 10g
kmno4It is slowly added in above-mentioned mixed liquor, proceed to reaction 120min in 35 DEG C of water-baths after ice bath reaction 30min, enable graphite
Enough fully oxidized.Reaction terminate after again deionized water reactant liquor is diluted to 500ml, be subsequently adding appropriate 30% peroxide
Change hydrogen solution to mixed liquor no longer effervescent；Add 10ml 5%hcl solution, and with a large amount of deionized waters fully wash in
Property；Finally by the graphene oxide obtaining lyophilization.
Embodiment 1:
Weigh 99mg Graphene to be added in 20ml alcohol solvent, ultrasonic disperse 1h, obtain graphene suspension, by 1mg
Double helix carbon fiber is added in graphene suspension, so that Double helix carbon fiber and Graphene is entered by the effect of low speed magnetic agitation
One step uniformly mixes, and mixed liquor is placed on 24h in 60 DEG C of vacuum drying ovens, removes alcohol solvent, prepares Double helix carbon fine
Dimension graphene composite material, the quality of wherein Double helix carbon fiber accounts for the 1% of the gross mass of Double helix carbon fiber and Graphene.
Embodiment 2
Weigh 50mg Graphene to be added in 20ml alcohol solvent, ultrasonic disperse 1h, obtain graphene suspension, by 50mg
Double helix carbon fiber is added in graphene suspension, so that Double helix carbon fiber and Graphene is entered by the effect of low speed magnetic agitation
One step uniformly mixes, and mixed liquor is placed on 24h in 60 DEG C of vacuum drying ovens, removes alcohol solvent, prepares Double helix carbon fine
Dimension graphene composite material, the quality of wherein Double helix carbon fiber accounts for the 50% of the gross mass of Double helix carbon fiber and Graphene.
Embodiment 3
Weigh 1mg Graphene to be added in 20ml alcohol solvent, ultrasonic disperse 1h, obtain graphene suspension, by 99mg
Double helix carbon fiber is added in graphene suspension, so that Double helix carbon fiber and Graphene is entered by the effect of low speed magnetic agitation
One step uniformly mixes, and mixed liquor is placed on 24h in 60 DEG C of vacuum drying ovens, removes alcohol solvent, prepares Double helix carbon fine
Dimension graphene composite material, the quality of wherein Double helix carbon fiber accounts for the 99% of the gross mass of Double helix carbon fiber and Graphene.
Embodiment 4
After weighing 100mg lyophilization, the graphene oxide of 8000 mesh, is carried out molten in 50ml beaker with 30ml distilled water
Solution, high-speed stirred 12h ultrasonic 1h peels off to graphene oxide, prepare graphene oxide water solution.By Double helix
Carbon fiber: after graphene oxide mass ratio is 1: 25 addition 4mg Double helix carbon fiber, then press graphene oxide: vitamin c quality
Add after 100mg vitamin c stirring at low speed 1h than for 1: 1 so as to mix homogeneously.React 3h, mistake at a temperature of 80 DEG C after sealing
Filter, filter cake is carried out removing unreacted reducing agent by ethanol, prepares described Double helix carbon fine after lyophilization
Dimension graphene composite material.
Embodiment 5
After weighing 100mg lyophilization, the graphene oxide of 8000 mesh, is carried out molten in 50ml beaker with 30ml distilled water
Solution, high-speed stirred 12h ultrasonic 1h peels off to graphene oxide, prepare graphene oxide water solution.By Double helix
Carbon fiber: graphene oxide mass ratio be 1: 25 add 4mg Double helix carbon fiber after, stirring at low speed 1h is so as to mix homogeneously.Will
Mixture is added in hydrothermal reaction kettle, reacts 12h in box atmosphere furnace, and reaction temperature is 180 DEG C.Sample is taken out after cooling
Filter, after filter cake lyophilization, obtain Double helix carbon fiber and graphite alkene composite.Gained Double helix carbon fiber and graphite alkene is combined
Material microscopic appearance is shown in Fig. 1 to Fig. 3.
Embodiment 6
After weighing 100mg lyophilization, the graphene oxide of 150 mesh, is carried out molten in 50ml beaker with 30ml distilled water
Solution, high-speed stirred 12h ultrasonic 2h peels off to graphene oxide, prepare graphene oxide water solution.By Double helix
Carbon fiber: graphene oxide mass ratio be 1: 25 add 4mg Double helix carbon fiber after, stirring at low speed 1h is so as to mix homogeneously.Will
Mixture is added in hydrothermal reaction kettle, reacts 12h in box atmosphere furnace, and reaction temperature is 180 DEG C.Sample is taken out after cooling
Filter, after filter cake lyophilization, obtain Double helix carbon fiber and graphite alkene composite.Gained Double helix carbon fiber and graphite alkene is combined
Material microscopic appearance is shown in Fig. 4 to Fig. 6.
Those of ordinary skill in the art understand, when technical scheme changes in following ranges, remain able to
To same as the previously described embodiments or close technique effect, still fall within protection scope of the present invention:
A kind of Double helix carbon fiber and graphite alkene composite, it is composited by Double helix carbon fiber and Graphene, wherein
Double helix carbon fiber accounts for the 1～99% of gross mass it is preferable that described Double helix carbon fiber accounts for the 1～50% of gross mass；Double helix carbon
The fibre diameter of fiber is 0.1～1 μm, 5～10 μm of screw diameter, and helix length is 10～100 μm；Graphene be single sheet or
Multi-disc stacked, piece footpath is 1～200 μm, and thickness is 1～50nm.
One of preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprises the steps:
(1) obtain Graphene；
(2) above-mentioned Graphene is added in organic solvent, ultrasonic disperse 0.5～2h, obtains graphene suspension；Above-mentioned
Organic solvent is n- methyl pyrrolidone, n, at least one in n- dimethylformamide, ethanol, chloroform and oxolane.
(3) Double helix carbon fiber is added in above-mentioned graphene suspension, Double helix carbon is made by magnetic agitation effect
Fiber is mixed further with Graphene, after removing solvent, described Double helix carbon fiber and graphite alkene composite is obtained.
Described step (1) is: by dispersed for graphene oxide in deionized water, ultrasonic stripping obtains graphene oxide
Solution, is subsequently added into 0.5～5 times of graphene oxide quality of reducing agent, reacts 2～48h, instead at a temperature of 50～100 DEG C
Filter cake should be filtered to obtain, this filter cake is carried out removing unreacted reducing agent by detergent, last lyophilization after finishing,
Described Graphene is obtained.Described reducing agent is in hydrazine hydrate, phenylhydrazine, sodium borohydride, sodium citrate, hydroquinone and vitamin c
At least one；Described detergent is water, ethanol and n, at least one in n- dimethylformamide.
Or described step (1) is: graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, ultrasonic stripping
Obtain graphene oxide solution, then this graphene oxide solution is carried out reduction reaction 12～48h in 120～200 DEG C, finally
Lyophilization, is obtained described Graphene.
The two of the preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprise the steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide
Solution；
(2) in above-mentioned graphene oxide solution, 0.5～5 times of reducing agent of graphene oxide quality and double spiral shell are added
Mix homogeneously after rotation carbon fiber, reacts 2～48h at 50～100 DEG C, filters to obtain filter cake after completion of the reaction, and this filter cake passes through to wash
Wash agent to be carried out, to remove unreacted reducing agent, last lyophilization, described Double helix carbon fiber and graphite alkene being obtained and being combined
Material.
Described reducing agent is at least one in hydrazine hydrate, phenylhydrazine, sodium borohydride, sodium citrate, hydroquinone and vitamin c
Kind；Described detergent is water, ethanol and n, at least one in n- dimethylformamide.
The three of the preparation method of above-mentioned Double helix carbon fiber and graphite alkene composite, comprise the steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide
Solution；
(2) in above-mentioned graphene oxide solution, after adding Double helix carbon fiber, mix homogeneously obtains mixed liquor, then should
Mixed liquor carries out reduction reaction 12～48h, last lyophilization in 120～200 DEG C, and described Double helix carbon fiber and graphite alkene is obtained
Composite.
The above, only presently preferred embodiments of the present invention, therefore the scope of present invention enforcement can not be limited according to this, that is,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.
Claims (9)
1. a kind of Double helix carbon fiber and graphite alkene composite it is characterised in that: it is combined by Double helix carbon fiber and Graphene
Form, wherein Double helix carbon fiber accounts for the 1～99% of gross mass；The fibre diameter of Double helix carbon fiber is 0.1～1 μm, spiral
5～10 μm of diameter, helix length is 10～100 μm；Graphene is single sheet or multi-disc stacked, and piece footpath is 1～200 μm, thick
Spend for 1～50nm.
2. Double helix carbon fiber and graphite alkene composite as claimed in claim 1 it is characterised in that: described Double helix carbon fiber
Account for the 1～50% of gross mass.
3. the Double helix carbon fiber and graphite alkene composite described in claim 1 or 2 preparation method it is characterised in that: include
Following steps:
(1) obtain Graphene；
(2) above-mentioned Graphene is added in organic solvent, ultrasonic disperse 0.5～2h, obtains graphene suspension；Above-mentioned organic
Solvent is n- methyl pyrrolidone, n, at least one in n- dimethylformamide, ethanol, chloroform and oxolane.
(3) Double helix carbon fiber is added in above-mentioned graphene suspension, Double helix carbon fiber is made by magnetic agitation effect
Mix further with Graphene, after removing solvent, described Double helix carbon fiber and graphite alkene composite is obtained.
4. preparation method as claimed in claim 3 it is characterised in that: described step (1) is: graphene oxide is dispersed
In deionized water, ultrasonic stripping obtains graphene oxide solution, be subsequently added into 0.5～5 times of graphene oxide quality also
Former dose, react 2～48h at a temperature of 50～100 DEG C, filter to obtain filter cake after completion of the reaction, this filter cake is carried out clearly by detergent
Wash to remove unreacted reducing agent, last lyophilization, described Graphene is obtained.
5. preparation method as claimed in claim 4 it is characterised in that: described reducing agent be hydrazine hydrate, phenylhydrazine, hydroboration
At least one of sodium, sodium citrate, hydroquinone and vitamin c；Described detergent is water, ethanol and n, n- dimethylformamide
In at least one.
6. preparation method as claimed in claim 3 it is characterised in that: described step (1) is: graphene oxide is dispersed in
In ionized water, after dispersed with stirring is uniform, ultrasonic stripping obtains graphene oxide solution, then by this graphene oxide solution in
120～200 DEG C carry out reduction reaction 12～48h, last lyophilization, and described Graphene is obtained.
7. the Double helix carbon fiber and graphite alkene composite described in claim 1 or 2 preparation method it is characterised in that: include
Following steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, it is molten that ultrasonic stripping obtains graphene oxide
Liquid；
(2) 0.5～5 times of reducing agent and the Double helix carbon of graphene oxide quality in above-mentioned graphene oxide solution, are added
Mix homogeneously after fiber, reacts 2～48h at 50～100 DEG C, filters to obtain filter cake after completion of the reaction, and this filter cake passes through detergent
It is carried out, to remove unreacted reducing agent, last lyophilization, described Double helix carbon fiber and graphite alkene composite being obtained.
8. preparation method as claimed in claim 7 it is characterised in that: described reducing agent be hydrazine hydrate, phenylhydrazine, sodium borohydride,
At least one of sodium citrate, hydroquinone and vitamin c；Described detergent is water, ethanol and n, in n- dimethylformamide
At least one.
9. the Double helix carbon fiber and graphite alkene composite described in claim 1 or 2 preparation method it is characterised in that: include
Following steps:
(1) graphene oxide is disperseed in deionized water, after dispersed with stirring is uniform, it is molten that ultrasonic stripping obtains graphene oxide
Liquid；
(2) in above-mentioned graphene oxide solution, after adding Double helix carbon fiber, mix homogeneously obtains mixed liquor, then mixes this
Liquid carries out reduction reaction 12～48h, last lyophilization in 120～200 DEG C, described Double helix carbon fiber and graphite alkene is obtained and is combined
Material.
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| CN108165078A (en) * | 2018-01-26 | 2018-06-15 | 北京欧美中科学技术研究院 | A kind of preparation method of conductive coating graphene additive |
| CN111588243A (en) * | 2020-06-01 | 2020-08-28 | 深圳市苏仁智能科技有限公司 | Sleeping pillow |
| CN115260559A (en) * | 2022-07-25 | 2022-11-01 | 电子科技大学长三角研究院(湖州) | Flexible mechanical sensor based on graphene in-situ growth spiral carbon fiber and preparation method thereof |
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| CN115260559A (en) * | 2022-07-25 | 2022-11-01 | 电子科技大学长三角研究院(湖州) | Flexible mechanical sensor based on graphene in-situ growth spiral carbon fiber and preparation method thereof |
| CN115260559B (en) * | 2022-07-25 | 2023-06-27 | 电子科技大学长三角研究院(湖州) | Flexible mechanical sensor based on graphene in-situ growth spiral carbon fiber and preparation method thereof |
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Application publication date: 20170125 |