CN110342498A - A kind of graphene-based elastic structure and preparation method thereof - Google Patents
A kind of graphene-based elastic structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene-based elastic structures and preparation method thereof, and graphene elastic structure is made of graphene-structured unit, and it is 100~40000 μm that graphene-structured unit, which is with a thickness of 30-100nm, area,2Graphene nano film, the graphene nano film crosslinks with adjacent graphene-structured unit, constitutes stereochemical structure.The content of heteroatoms of the graphene nano film is in 10wt% hereinafter, defect concentration ID/IG0.02 or more.This structural unit enhances the intensity and deformation modulus of graphene, greatly maintain the integrality and highly conductive characteristic in aeroge application process, it ensure that the high resiliency of graphene, still there is good deformation behavior at low temperatures, it ensures its cryogenic property stability, provides good thinking for the folding extension under the low volume lift-off of space equipment and space.
Description
Technical field
The invention belongs to field of new materials more particularly to a kind of graphene-based elastic structure and preparation method thereof.
Background technique
2010, two professor Andre GeiM and Konstantin Novoselov of Univ Manchester UK because
It is successfully separated out stable graphene for the first time and obtains Nobel Prize in physics, has started the upsurge that graphene is studied in the whole world.
Graphene has excellent electric property (electron mobility is up to 2 × 105cM2/Vs at room temperature), heating conduction outstanding
(5000W/ (MK), extraordinary specific surface area (2630M2/g), Young's modulus (1100GPa) and breaking strength (125GPa).Stone
The excellent electrical and thermal conductivity performance of black alkene is well beyond metal, while graphene has the advantages that corrosion-and high-temp-resistant, and it is good
Mechanical performance and lower density more allow it to have the potentiality in thermo electric material field substituted metal.
Graphene aerogel is one of the important application form of graphene macroscopic view assembled material, is widely used in solar energy receipts
The key areas such as collection, energy storage, mechanics sensor, optical sensor, sewage treatment, air cleaning, oil leak.But at present
Conventional aeroge has following disadvantage: first, lower crosslinking area and structural unit thickness hold so that its intensity is low
It is easily scaling-off, and poorly conductive；Second, lower structural strength makes its elastic recovery time slow；Third, lower structure are strong
Degree cannot bear bending and tensile deformation so that it can only bear compressive deformation.Three of the above disadvantage, so that its practical application
Receive great obstruction.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of graphene-based elastic structure and its preparation
Method.
The present invention adopts the following technical scheme: a kind of graphene-based elastic structure, is made of graphene-structured unit, institute
Graphene-structured unit is stated to be 100~40000 μm with a thickness of 30-100nm, area2Graphene nano film, the graphite
Alkene nanometer film edge is crosslinked with adjacent graphene-structured unit, constitutes three-dimensional porous structure.The graphene nano film
Content of heteroatoms in 10wt% hereinafter, defect concentration ID/IG0.02 or more.
Further, the three-dimensional porous structure is aerogel structure.
A method of above-mentioned elastic structure is prepared, is included the following steps:
(1) graphene oxide membrane of the degree of orientation 95% or more, the oxidation stone are cast into using graphene oxide solution
Then black alkene size carries out electronation with hydroiodic acid at 20 μm or more, so that oxygen content is in 10wt% or less；
(2) 1400~1800 DEG C or more are warming up to 2-20 DEG C/min and carry out high-temperature process, obtain three-dimensional porous structure
Aerogel film.
A method of preparing above-mentioned elastic structure, this method are as follows:
(1) stannic oxide/graphene nano film is prepared, the number of plies of thickness direction is between 90~300, and area is 100~40000 μ
m2；
(2) nanometer film described in multiple steps 1 is put into poor solvent, after being uniformly dispersed, solid-state is obtained after freeze-drying
Aerogel film of the density in 50mg/mL or more.
Further, in the step 2, concentration of the graphene nano film in poor solvent is 50mg/mL or more.
The beneficial effects of the present invention are: first, the present invention greatly maintains the integrality of aeroge and highly conductive
Characteristic；Second, the thickness and suitable lateral dimension of graphene construction unit 30-100nm, on the one hand ensure that graphene
On the other hand high resiliency improves its cryogenic property stability；Third, the design feature of the structure, imparts its three dimensional elasticity,
It stretches, compress and folds, the 4th, stronger structural unit intensity and appropriate lateral dimension ensure that graphene film
Compression rigidity is bent, its faster elastic recovery time is imparted.This theory is low volume lift-off and the space of space equipment
Under folding extension provide good thinking.
Detailed description of the invention
Fig. 1 is the backfin recovery process figure in situ of the graphene nano film of different-thickness；
Fig. 2 is the partial schematic diagram of graphene aerogel film；
Fig. 3 a is to fold test process schematic diagram, and 3b is the recovery process schematic diagram of aeroge batten；
Fig. 4 is graphene aerogel film sectional view；
Fig. 5 is DMA compression verification result figure.
Specific embodiment
Conventional aeroge has following disadvantage: first, lower crosslinking area and structural unit thickness, so that it is strong
It spends low, is easy scaling-off, and poorly conductive；Second, lower structural strength makes its elastic recovery time slow；Third, it is lower
Structural strength make it that can only bear compressive deformation, cannot bear bending and tensile deformation.
The present invention is mainly the improvement to graphene elastic structure, and graphene elastic structure is by graphene-structured unit
Composition, it is 100~40000 μm that graphene-structured unit, which is with a thickness of 30-100nm, area,2Graphene nano film, it is described
Graphene nano film is crosslinked with adjacent graphene-structured unit, constitutes stereochemical structure.The graphene nano film it is miscellaneous
Atom content is in 10wt% hereinafter, defect concentration ID/IG0.02 or more.
The superiority of above structure is embodied in the following: first, the high thickness of structural unit and strong large area
Crosslinking, enhances the intensity and deformation modulus of graphene, greatly maintain integrality in aeroge application process and
Highly conductive characteristic；Second, the thickness of 30-100nm and the graphene construction unit of suitable lateral dimension itself have it is fabulous
Flexibility and elasticity, ensure that the high resiliency of graphene, meanwhile, relatively thin structural unit thickness, so that it is in low temperature
In the case of still have good deformation behavior, it is ensured that its cryogenic property stability；Third, the cross-linked structure of class rubber designs
(being cross-linked with each other for elastomeric segments) imparts its three dimensional elasticity, stretching, compression and folded elastic；4th, stronger structure list
First intensity and appropriate lateral dimension ensure that the bending compression rigidity of graphene film, impart its faster elasticity and restore
Time.This theory provides good thinking for the folding extension under the low volume lift-off of space equipment and space.
The degree of orientation of heretofore described graphene are as follows: along the quality of the graphene film of planar orientation where graphene film
Content.
The present invention also provides the two methods for obtaining above described structure.
One are as follows:
(1) graphene oxide membrane of the degree of orientation 95% or more, the oxidation stone are cast into using graphene oxide solution
Then black alkene size carries out electronation with hydroiodic acid at 20 μm or more, so that oxygen content is in 10wt% or less；
(2) 1400~1800 DEG C or more are warming up to 2-20 DEG C/min and carry out high-temperature process, obtain three-dimensional porous structure
Aerogel film.
In temperature-rise period, hetero atom gradually falls off, and the defect of graphene oxide sheet is gradually repaired, and leads to gas escape
It is blocked, while nonsynchronous structure repair occurs on different graphene films, so that reaction force attenuation between graphene sheet layer, shape
Stratification from；It is heteroatomic fall off, the leafing of graphene and graphene repair the barrier to be formed, competition is formed between three, when
In the graphene oxide membrane being initially formed, graphene size be can be obtained when 20 μm or more, the degree of orientation are 95% or more by thickness
Degree is 30-100nm, area is 100~40000 μm2Graphene-structured unit constitute three-dimensional porous aerogel film.Instead
It, in the graphene oxide membrane being initially formed, graphene size, then can mistake when 20 μm or less or the degree of orientation are below 95%
More introducing holes assists gas escape, the thickness of structural unit is caused to increase.
Secondly are as follows:
(1) stannic oxide/graphene nano film is prepared, the number of plies of thickness direction is between 90~300, and area is 100~40000 μ
m2；
(2) nanometer film described in multiple steps 1 is put into poor solvent, after being uniformly dispersed, solid-state is obtained after freeze-drying
Aerogel film of the density in 50mg/mL or more.Correspondingly, concentration of the graphene nano film in poor solvent be 50mg/mL with
On.
In the graphene nano film poor solvent dispersion liquid of high concentration, graphene nano film is stacked with, and is formed preliminary
Porous network structure；In freeze-drying process, more closely, contact area increases the stacking between film, to be formed relatively secured
Physical crosslinking.
Below with reference to being that the invention will be further described for embodiment:
Embodiment 1: structural unit research
It is formed a film in substrate using curtain coating or the method filtered, then uses the method for solid transfer agent transfer by graphene
Film stripping is got off, and the graphene nano film that the lateral dimension of different-thickness is 200 μm is respectively obtained, by the graphene of different-thickness
Nanometer film carries out original position TEM compression test, as a result as shown in Figure 1.
It can be seen from the figure that in thickness 30nm hereinafter, graphene film only shows flexibility without elasticity；In 30-
Under the thickness of 100nm, graphene film demonstrates flexibility and flexibility.It is demonstrated experimentally that being more than 100nm or more in graphene film thickness
When, macroscopical assembling film stress easy to form is concentrated and damaged, while the being mutually bonded property of structural unit can also be deteriorated, and be unfavorable for macro
See the stability of material property.
Embodiment 2: the preparation of graphene elastic structure
(1) graphene oxide membrane of the degree of orientation 95% or more, the oxidation stone are cast into using graphene oxide solution
Then black alkene size carries out electronation with hydroiodic acid at 20~40 μm, so that oxygen content is 10wt%；
(2) 1400 DEG C or more are warming up to 2 DEG C/min and carry out high-temperature process, obtain the aerogel film of three-dimensional porous structure.
The aerogel film with a thickness of 100 μm or so.Its partial schematic diagram is as shown in Fig. 2, it can be seen from the figure that constitute aerogel film
Graphene-structured unit be with a thickness of 30-100nm, area be 100~40000 μm2Graphene nano film, graphene receives
Rice film is crosslinked with adjacent graphene-structured unit, constitutes stereochemical structure.Wherein, the content of heteroatoms of graphene nano film
In 10wt% hereinafter, defect concentration ID/IG0.02 or more.
The graphene aerogel film being prepared is carried out to folding test as shown in Figure 3a, it can be seen from the figure that institute
The graphene aerogel film of design preparation can be resistant to prolonged compression bending, can equally bear responsible bending accumulation,
And keep structure constant, can be quick and complete be restored to intrinsic shape.Fig. 3 b characterizes 1cm long, the aeroge batten of 1mm wide
Recovery time, be short to 59ms.
The aerogel film is subjected to DMA compression verification, as a result as shown in figure 5, the aerogel film of this structure can be resistant to zero
Iterative cycles compression under 150 degree to 400 degree above freezing lower, and performance does not occur significantly to change.
Embodiment 3: the preparation of graphene elastic structure
(1) graphene oxide membrane of the degree of orientation 95% or more, the oxidation stone are cast into using graphene oxide solution
Then black alkene size carries out electronation with hydroiodic acid at 60~100 μm, so that oxygen content is 7.6%；
(2) 1800 DEG C or more are warming up to 20 DEG C/min and carry out high-temperature process, obtain the aerogel film of three-dimensional porous structure.
The aerogel film with a thickness of 150 μm or so.By sweep test, the graphene-structured unit for constituting aerogel film is thickness
It is 100~40000 μm for 30-100nm, area2Graphene nano film, graphene nano film and adjacent graphene-structured list
Member crosslinks, and constitutes stereochemical structure.Wherein, the content of heteroatoms of graphene nano film is in 10wt% hereinafter, defect concentration ID/
IG0.02 or more.
The graphene aerogel film being prepared is carried out the test method of Fig. 3 a such as to test, the results showed that, graphite
Alkene aerogel film can be resistant to prolonged compression bending, can equally bear responsible bending accumulation, and keep structure constant,
Can be quick and complete be restored to intrinsic shape.The recovery time of the aeroge batten of 1cm long, 1mm wide, it is short to 47ms.
The aerogel film is subjected to DMA compression verification, the results show that the aerogel film of this structure can be resistant to subzero 150
The iterative cycles compression under 400 degree above freezing is spent, and performance does not occur significantly to change.
Embodiment 4: the preparation of graphene elastic structure
(1) stannic oxide/graphene nano film is prepared using the method for spin coating, the number of plies of thickness direction is 180~300, and area is
100μm2；
(2) nanometer film described in step 1 is put into acetone, concentration 50mg/mL, after being uniformly dispersed, freeze-drying is obtained
Aerogel film.
The aerogel film with a thickness of 250 μm or so.By sweep test, the graphene-structured unit of aerogel film is constituted
It is with a thickness of 60-100nm, area is 100~40000 μm2Graphene nano film, graphene nano film and adjacent graphite
Alkene structural unit crosslinks, and constitutes stereochemical structure.Wherein, the content of heteroatoms of graphene nano film is in 10wt% hereinafter, lacking
Fall into density ID/IG0.02 or more.
The graphene aerogel film being prepared is carried out the test method of Fig. 3 a such as to test, the results showed that, graphite
Alkene aerogel film can be resistant to prolonged compression bending, can equally bear responsible bending accumulation, and keep structure constant,
Can be quick and complete be restored to intrinsic shape.The recovery time of the aeroge batten of 1cm long, 1mm wide, it is short to 37ms.
The aerogel film is subjected to DMA compression verification, the results show that the aerogel film of this structure can be resistant to subzero 150
The iterative cycles compression under 400 degree above freezing is spent, and performance does not occur significantly to change.
Embodiment 5: the preparation of graphene elastic structure
(1) stannic oxide/graphene nano film is prepared using the method filtered, the number of plies of thickness direction is 90~200, and area is
40000μm2；
(2) nanometer film described in multiple steps 1 is put into acetone, concentration 50mg/mL, after being uniformly dispersed, freeze-drying
Obtain aerogel film.
The aerogel film with a thickness of 180 μm or so.By sweep test, the graphene-structured unit of aerogel film is constituted
It is with a thickness of 30-60nm, area is 30000~40000 μm2Graphene nano film, graphene nano film and adjacent stone
Black alkene structural unit crosslinks, and constitutes stereochemical structure.The area of the graphene film obtained due to suction filtration method is more uniform,
It is approximate that and the site of graphene nano film crosslinking is usually in the marginal position of film with the area for filtering film, therefore, the stereochemical structure
In hole size it is more uniform, as shown in Figure 4.The content of heteroatoms of the graphene nano film is in 10wt% hereinafter, defect is close
Spend ID/IG0.02 or more.
The graphene aerogel film being prepared is carried out the test method of Fig. 3 a such as to test, the results showed that, graphite
Alkene aerogel film can be resistant to prolonged compression bending, can equally bear responsible bending accumulation, and keep structure constant,
Can be quick and complete be restored to intrinsic shape.The recovery time of the aeroge batten of 1cm long, 1mm wide, it is short to 44ms.
The aerogel film is subjected to DMA compression verification, the results show that the aerogel film of this structure can be resistant to subzero 150
The iterative cycles compression under 400 degree above freezing is spent, and performance does not occur significantly to change.
Claims (5)
1. a kind of graphene-based elastic structure, which is characterized in that be made of graphene-structured unit, the graphene-structured list
It is 100~40000 μm that member, which is with a thickness of 30-100nm, area,2Graphene nano film, the graphene nano film edge with
Adjacent graphene-structured unit crosslinks, and constitutes three-dimensional porous structure.The content of heteroatoms of the graphene nano film exists
10wt% is hereinafter, defect concentration ID/IG0.02 or more.
2. elastic structure according to claim 1, which is characterized in that the three-dimensional porous structure is aerogel structure.
3. a kind of method for preparing elastic structure described in claim 1, which comprises the steps of:
(1) graphene oxide membrane of the degree of orientation 95% or more, the graphene oxide are cast into using graphene oxide solution
Then size carries out electronation with hydroiodic acid at 20 μm or more, so that oxygen content is in 10wt% or less；
(2) 1400~1800 DEG C or more are warming up to 2-20 DEG C/min and carry out high-temperature process, obtain the airsetting of three-dimensional porous structure
Glue film.
4. a kind of method for preparing elastic structure described in claim 1, which is characterized in that this method are as follows:
(1) stannic oxide/graphene nano film is prepared, the number of plies of thickness direction is between 90~300, and area is 100~40000 μm2；
(2) nanometer film described in multiple steps 1 is put into poor solvent, after being uniformly dispersed, solid state density is obtained after freeze-drying
In the aerogel film of 50mg/mL or more.
5. according to the method described in claim 4, it is characterized in that, graphene nano film is in poor solvent in the step 2
Concentration be 50mg/mL or more.
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