CN106189088B - A kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material - Google Patents
A kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material Download PDFInfo
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- CN106189088B CN106189088B CN201610566145.7A CN201610566145A CN106189088B CN 106189088 B CN106189088 B CN 106189088B CN 201610566145 A CN201610566145 A CN 201610566145A CN 106189088 B CN106189088 B CN 106189088B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention belongs to polymer matrix composite manufacturing fields, and in particular to a kind of preparation method of carbon nanotube graphene oxide hybrid reinforced composite material.The present invention by graphene oxide and carbon nanotube by being assembled into high self-maintaining nano-sized carbon hybrid structure reinforcement, it is infiltrated through resin matrix, after polymerization, obtain carbon nanotube graphene oxide hybrid reinforced composite material, using 2 ethyl, 4 methylimidazole as " bridge " between carbon nanotube and graphene oxide, prepare the porous carbon nanotube graphene oxide reinforcement of low-density and high-specific surface area, the reinforcement remains graphene oxide and the reapective features of carbon nanotube simultaneously, as high conductivity, thermal conductivity and the continuous reinforcement of three-dimensional macro and various kinds of resin matrix are compound, manufacturing cost is low, multi-functional carbon nanotube graphene oxide hybrid reinforced composite material.
Description
Technical field
The invention belongs to polymer matrix composite manufacturing fields, and in particular to a kind of carbon nanotube-graphene oxide is mixed
The preparation method of miscellaneous enhancing composite material.
Background technology
In recent years, to polymer matrix composite, more stringent requirements are proposed for scientific and technical rapid development, and collection carrying is led
The advanced composite material (ACM) of the structure functions such as electricity, heat conduction is increasingly subject to people's favor, the novel enhanced of some micro/nano-scales
Body is introduced among various thermoplasticity and thermosetting resin matrix, by constructing multi-level macroscopical continuous structure, is greatly carried
The performance of polymer matrix composite has been risen, its application range has further been widened.Using carbon nanotube and graphene as representative
Nano-carbon material is because with huge specific surface area, excellent mechanical property and heat conductivility in novel energy, biology, electronics
Information and field of functional materials are concerned.Material property fundamentally depends on its internal microstructure, is formed and solid
Change among the forming process of composite material.Currently, the development of nano carbon composite material is maked rapid progress, but still face two sides
The problem of face：First, the formation and control of nanocomposite interior three-dimensional Microscopic order carbon structure；Second is that as function carrier
This body structure of nano-carbon material and property regulation and control.
Why there is nano carbon composite material conductive, heat conductivility key to be it inside resin matrix by taking
It connects, be wound macroscopical contiguous network, this forming process is influenced by a variety of thermodynamics and kinetics factors.Production polymerization
The conventional method of object based composites is melt blending or solution blending, in forming process, by ultrasonic wave or shear action
Realize that nano-carbon material is evenly dispersed in resin matrix, but this dynamic structure in thermodynamics non-equilibrium and its high length
Diameter greatly influences carbon nanotube and graphene oxide than inevitably leading to the aggregation of micro/nano-scale carbon material and piling up
Energy gives full play to.How to realize that nano-carbon material forms structure that is orderly and stablizing inside resin matrix is composite material neck
The general character project that domain faces.
Carbon nanotube or graphene are assembled into three-dimensional continuous nano-sized carbon reinforcement, after compounding with the resin matrix, three
It is a kind of promising process route that continuous nano-sized carbon reinforcement, which is tieed up, as material function conversion and the material base exported.
But the problem of presently, there are following three aspects：（1）Anisotropy in terms of the function of brought by a peacekeeping two-dimensional structure；（2）By
By the carbon nanotube or the self-maintaining difference of graphene reinforcement of π-π interaction assemblings, composite structure and property are seriously affected
The uniformity of energy；（3）Chemical vapor deposition（CVD）The carbon nanotube and graphene of method production have very strong hydrophobicity, are not easy
Fully infiltrated and formed by resin matrix strong interfaces combination.
Invention content
In view of the problems of the existing technology, it is compound to provide a kind of carbon nanotube-graphene oxide hybrid buildup by the present invention
The preparation method of material, it is therefore an objective to by the way that graphene oxide and carbon nanotube are assembled into high self-maintaining nano-sized carbon hybrid structure
Reinforcement obtains carbon nanotube-graphene oxide hybrid reinforced composite material, with 2- second after resin matrix infiltration, polymerization
Base -4-methylimidazole prepares low-density as shown in Figure 1 and Gao Bi as " bridge " between carbon nanotube and graphene oxide
Porous carbon nanotube-graphene oxide reinforcement of surface area, the reinforcement remain graphene oxide and carbon nanometer simultaneously
The reapective features of pipe, it is compound as high conductivity, thermal conductivity and the continuous reinforcement of three-dimensional macro and various kinds of resin matrix, it is prepared into
This low, multi-functional carbon nanotube-graphene oxide hybrid reinforced composite material（As shown in Figure 2）.
Realize that the technical solution of the object of the invention follows the steps below：
（1）By graphene oxide ultrasonic disperse 40 ~ 60 minutes in water, graphene oxide dispersion is obtained；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 40o2-ethyl-4-methylimidazole is added in C, then
Ultrasonic disperse 40 ~ 60 minutes, is added carbon nanotube, and ultrasonic disperse is added ammonium hydroxide after 2 ~ 3 hours, is warming up to 85 ~ 90oC, hydro-thermal are anti-
It answers 7 ~ 10 hours；
（3）By step（2）After gained reaction product carries out liquid-nitrogen freeze drying processing 12 ~ 14 hours, dry 2 ~ 3 hours,
Obtain three dimensional carbon nanotubes-graphene oxide hybrid buildup body；
（4）Three dimensional carbon nanotubes-graphene oxide reinforcement is infiltrated using resin matrix, carbon is obtained after moulding process processing
Nanotube-graphene oxide hybrid reinforced composite material.
Wherein, step（1）A diameter of 20-100 μm of the graphene oxide, graphene oxide dispersion it is a concentration of
0.1mg/ml-2mg/ml。
Step（2）The weight ratio of the 2-ethyl-4-methylimidazole and graphene oxide is 1:1~2.
Step（2）The carbon nanotube is carbon nanotube, surface carboxyl groups are carbon nano-tube modified, surface amino groups modified carbon is received
Mitron or surface hydroxyl are carbon nano-tube modified, are single wall, double-walled or multi-walled carbon nanotube.
Step（2）The ammonia volume is 1 ~ 2ml.
Step（2）The weight ratio of the graphene oxide and carbon nanotube is 2 ~ 1:1.
Step（4）The resin matrix is epoxy resin, bimaleimide resin, unsaturated polyester (UP), vinyl tree
Any one of fat or cyanate ester resin.
Step（4）The moulding process is vacuum assisted resin transfer molding（VARTM）, Resin Film Infusion（RFI）Work
Any one of skill or vacuum immersion/mould pressing process.
Compared with prior art, specific and advantageous effect of the invention is：
（1）The present invention by multiphase, multicomponent, multi-level thought apply to novel nanocomposite materials design among, profit
It is amphipathic with graphene oxide, keep carbon nanotube evenly dispersed in water and the conduction collectively as composite inner, leads
Heat passage.
（2）Carbon nanotube-graphene oxide reinforcement had not only had the polar active group of graphene oxide, but also was received with carbon
The high length-diameter ratio of mitron and the conductive, capacity of heat transmission are conducive to and the compound preparation conduction of various kinds of resin matrix, heat-conductive composite material.
（3）It is acted on using " bridge " of π-π interaction and 2-ethyl-4-methylimidazole, high length-diameter ratio and transverse and longitudinal ratio
Flexible graphene oxide and carbon nanotube are assembled into the good self-maintaining continuous reinforcement of three-dimensional, are conducive to subsequent tree
Fat infiltrates and forming process.
（4）Electric conductivity, the thermal conductivity of carbon nanotube-graphene oxide hybrid reinforced composite material can aoxidize stone by control
Black alkene size is adjusted with carbon nanotube ratio and dosage, and room temperature resistivity reduces by 10 orders of magnitude.
（5）Equipment needed for the present invention is simple, of low cost, and technological operation is convenient, can be used for various kinds of resin based composites
System.
Description of the drawings
Fig. 1 is the stereoscan photograph of the carbon nanotube-graphene oxide reinforcement prepared in embodiment 1；
Fig. 2 is the optical photograph of the carbon nanotube-graphene oxide hybrid reinforced composite material prepared in embodiment 1.
Specific implementation mode
The following examples are further illustrations of the invention, the epoxy resin that is used in embodiment, bismaleimide
Resin, unsaturated polyester (UP), vinylite and cyanate ester resin are commercial products.
The single-walled nanotube specific surface area used in the embodiment of the present invention>140m2/ g, the specific surface area of double-walled nanotubes>
350m2/ g, the specific surface area of multi-walled carbon nanotube>500m2/ g, is commercial products, and a diameter of the 20 of the graphene oxide of use
-100μm。
The ultrasonic field working frequency used in the embodiment of the present invention is 45kHz, power 100W.
Embodiment 1
The preparation method of the carbon nanotube of the present embodiment-graphene oxide hybrid reinforced composite material according to the following steps into
Row：
（1）By 0.5g graphene oxides in 2000ml water ultrasonic disperse 40 minutes, obtain the graphite oxide of 0.25mg/ml
Alkene dispersion liquid；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 40o0.5g 2- ethyl -4- methyl miaows are added in C
0.5g multi-walled carbon nanotubes are added in azoles, re-ultrasonic dispersion 1 hour, and ultrasonic disperse is added 1ml ammonium hydroxide, is warming up to after 2 hours
90oC, hydro-thermal reaction 7 hours；
（3）By step（2）It is small in 105 DEG C of drying 2 after gained reaction product carries out liquid-nitrogen freeze drying processing 14 hours
When, three-dimensional multi-walled carbon nanotube-graphene oxide hybrid buildup body is obtained, scanning electron microscopic picture is as shown in Figure 1, from Fig. 1
It can be seen that obtain carbon nanotube-graphene oxide reinforcement of high porosity, high specific area, can with resin matrix into
Row is compound to prepare polymer matrix composite；
（4）It is molded, multi-walled carbon nanotube-graphene oxide hybrid buildup body is put into a concentration of using mould pressing process
It is infiltrated 4 hours in the epoxy resin of 30wt%/acetone glue, 65 oIt is moved in mold after being dried 2 hours under C, 80 oC is kept
Temperature applies the pressure 1h of 5MPa after twenty minutes, according still further to 80oC/1h, 110oC/2h, 170oC/2h, 200oThe program liter of C/1h
Temperature solidification, is made three-dimensional multi-walled carbon nanotube-graphene oxide hybrid reinforced composite material, and conductivity is 1 × 10-4Scm-1, heat
Conductance is 0.5Wm-1K-1, optical photograph is as shown in Figure 2.
Embodiment 2
The preparation method of the carbon nanotube of the present embodiment-graphene oxide hybrid reinforced composite material according to the following steps into
Row：
（1）By 1g graphene oxides in 2000ml water ultrasonic disperse 60 minutes, obtain the graphene oxide of 0.5mg/ml
Dispersion liquid；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 45o1g 2- ethyl -4- methyl miaows are added in C
1g carboxyl modified multi-walled carbon nanotubes are added in azoles, re-ultrasonic dispersion 1 hour, and 2ml ammonium hydroxide is added in ultrasonic disperse after 2 hours, heat up
To 90oC, hydro-thermal reaction 10 hours；
（3）By step（2）It is small in 105 DEG C of drying 2 after gained reaction product carries out liquid-nitrogen freeze drying processing 14 hours
When, obtain three-dimensional carboxyl modified multi-walled carbon nanotube-graphene oxide hybrid buildup body；
（4）Using vacuum assisted resin transfer molding technological forming, by carboxyl modified multi-walled carbon nanotube-oxygen after cutting
Graphite alkene hybrid buildup body is put into mold, with being preheated to 50oIt is more that the epoxy resin of C infiltrates carboxyl modified under vacuum
After wall carbon nano tube-graphene oxide hybrid buildup body, according to 80oC/1h, 110oC/2h, 170oC/2h, 200oThe program of C/1h
Elevated cure, is made carboxyl modified multi-walled carbon nanotube-graphene oxide hybrid reinforced composite material, and conductivity is 2 × 10- 4Scm-1, thermal conductivity 0.3Wm-1K-1。
Embodiment 3
The preparation method of the carbon nanotube of the present embodiment-graphene oxide hybrid reinforced composite material according to the following steps into
Row：
（1）By 2g graphene oxides, ultrasonic disperse 50 minutes, the graphene oxide for obtaining 1mg/ml divide in 2000ml water
Dispersion liquid；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 42o1g 2- ethyl -4- methyl miaows are added in C
1g hydroxyl modified multi-walled carbon nanotubes are added in azoles, re-ultrasonic dispersion 1 hour, and 1ml ammonium hydroxide is added in ultrasonic disperse after 2 hours, heat up
To 85oC, hydro-thermal reaction 8 hours；
（3）By step（2）It is small in 105 DEG C of drying 2 after gained reaction product carries out liquid-nitrogen freeze drying processing 13 hours
When, obtain three-dimensional hydroxyl modified multi-walled carbon nanotube-graphene oxide hybrid buildup body；
（4）It is molded using Resin film infusion, epoxy resin is placed in mold, then placed in the above after cutting
Hydroxyl modified multi-walled carbon nanotube-graphene oxide reinforcement, be then sealed with vacuum bag, be heated to 50oIt is vacuumized after C,
After epoxy resin infiltrates hydroxyl carbon nano tube-graphene oxide hybrid buildup body, according to 80oC/1h, 110oC/2h, 170oC/
2h, 200oThe temperature programming of C/1h cures, and hydroxylated multi-walled carbon nanotubes-graphene oxide hybrid reinforced composite material is made,
Its conductivity is 1.3 × 10-4Scm-1, thermal conductivity 0.58Wm-1K-1。
Embodiment 4
The preparation method of the carbon nanotube of the present embodiment-graphene oxide hybrid reinforced composite material according to the following steps into
Row：
（1）By 2g graphene oxides, ultrasonic disperse 40 minutes, the graphene oxide for obtaining 1mg/ml divide in 2000ml water
Dispersion liquid；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 40o2g 2- ethyl -4- methyl miaows are added in C
The amido modified multi-walled carbon nanotubes of 2g are added in azoles, re-ultrasonic dispersion 1 hour, and 1ml ammonium hydroxide is added in ultrasonic disperse after 2 hours, heat up
To 85oC, hydro-thermal reaction 8 hours；
（3）By step（2）It is small in 105 DEG C of drying 2 after gained reaction product carries out liquid-nitrogen freeze drying processing 14 hours
When, obtain three-dimensional amino-group modifying multiwall carbon nano-tube-graphene oxide hybrid buildup body；
（4）Using vacuum assisted resin transfer molding technological forming, by amido modified multi-walled carbon nanotube-oxygen after cutting
Graphite alkene hybrid buildup body is put into mold, with being preheated to 40oThe cyanate ester resin of C infiltrates amido modified under vacuum
After multi-walled carbon nanotube-graphene oxide hybrid buildup body, according to 110oC/1h, 170oC/2h, 200oThe temperature programming of C/1h is solid
Change, amido modified multi-walled carbon nanotube-graphene oxide hybrid reinforced composite material is made, conductivity is 3 × 10-4Scm-1, heat
Conductance is 0.25Wm-1K-1。
Claims (4)
1. a kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material, it is characterised in that according to following step
It is rapid to carry out：
（1）By graphene oxide ultrasonic disperse 40 ~ 60 minutes in water, graphene oxide dispersion is obtained；The graphite oxide
A diameter of 20-100 μm of alkene, a concentration of 0.1mg/mL ~ 2mg/mL of graphene oxide dispersion；
（2）By step（1）Obtained graphene oxide dispersion is warming up to 40o2-ethyl-4-methylimidazole, then ultrasound is added in C
Dispersion 40 ~ 60 minutes, is added carbon nanotube, and ultrasonic disperse is added ammonium hydroxide after 2 ~ 3 hours, is warming up to 85 ~ 90oC, hydro-thermal reaction 7 ~
10 hours；The weight ratio of 2-ethyl-4-methylimidazole and graphene oxide is 1:1~2；The weight of graphene oxide and carbon nanotube
Amount is than being 2 ~ 1:1；
（3）By step（2）After gained reaction product carries out liquid-nitrogen freeze drying processing 12 ~ 14 hours, dries 2 ~ 3 hours, obtain
Three dimensional carbon nanotubes-graphene oxide hybrid buildup body；
（4）Three dimensional carbon nanotubes-graphene oxide reinforcement is infiltrated using resin matrix, carbon nanometer is obtained after moulding process processing
Pipe-graphene oxide hybrid reinforced composite material；The resin matrix is epoxy resin, bimaleimide resin, insatiable hunger
Any one of with polyester, vinylite or cyanate ester resin.
2. a kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material according to claim 1,
It is characterized in that step（2）The carbon nanotube is that surface carboxyl groups are carbon nano-tube modified, surface amino groups are carbon nano-tube modified or table
Face hydroxyl modified carbon nanotube is single wall, double-walled or multi-walled carbon nanotube.
3. a kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material according to claim 1,
It is characterized in that step（2）The ammonia volume is 1 ~ 2ml.
4. a kind of preparation method of carbon nanotube-graphene oxide hybrid reinforced composite material according to claim 1,
It is characterized in that step（4）The moulding process be vacuum assisted resin transfer molding, Resin film infusion or vacuum immersion/
Any one of mould pressing process.
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Effective date of registration: 20200219 Address after: No.8, approach road, Airport Industrial Park, Lianshui County, Huai'an City, Jiangsu Province Patentee after: Huai'an Aviation Industry Research Institute Co., Ltd Address before: 110136 Shenyang Province, moral economic development zone, moral, South Street, No. 37, No. Patentee before: Shenyang Aerospace University |