CN103254572A - Graphene oxide/carbon nano-tube collaboration-modified glass fiber reinforced epoxy composite material and preparation method thereof - Google Patents
Graphene oxide/carbon nano-tube collaboration-modified glass fiber reinforced epoxy composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a graphene/carbon nano-tube collaboration-modified glass fiber reinforced epoxy composite material and a preparation method thereof. The composite material comprises an epoxy resin base material and inorganic nanometer filler which is uniformly dispersed in the epoxy resin base material, wherein the composite nanometer inorganic filler is composed of graphene oxide with thickness of 0.35nm-20nm and diameter of 5 microns-100microns and the carbon nano-tube with the diameter of 30nm-50nm and length of 10 microns-20 microns. The graphene/carbon nano-tube collaboration-modified glass fiber reinforced epoxy composite material can be used for effectively improving the mechanical performances of epoxy resin matrix and interface bonding strength between the matrix and the glass fiber by utilizing the excellent mechanical performances and the surface active functional groups of the graphene oxide and the carbon nano-tube, so that the interlayer shearing strength of the glass fiber composite material is effectively improved.
Description
Technical field
The invention belongs to the preparation field of polymer matrix composite, specifically relate to the preparation method of a kind of graphene oxide/carbon nano-tube modification glass reinforced epoxy based composites.
Background technology
The glass fiber reinforcement epoxy based composites has specific tenacity and specific rigidity height, designability is strong, the fatigue crack-resistant performance is good, corrosion-resistant, scantlings of the structure good stability and be convenient to the integrally formed distinct advantages of big area, now become the important materials that can't replace in national economy, national defense construction and the development in science and technology, as tire cord of bulletproof halmet, bullet proof clothing, vertisplane wing, early warning plane radome, various high pressure vessel, the straight plate of civilian aircraft, sports goods, all kinds of high temperature resistant goods and excellent performance etc.Influence life-span and the security of use but there are shortcomings such as interlayer is easy to crack in glass reinforced epoxy matrix material, thereby need further to improve its mechanical property.
And depending primarily on the intensity of matrix resin and matrix resin, the interlayer shear performance of matrix material is combined situation with the interface of glass fibre.The one dimension carbon nanotube has excellent mechanical property, thereby existing a large amount of research report about the carbon nanotubes reinforced polymer based nano composite material.Yet weak interface makes the reinforced effects of carbon nanotube can not get fine performance in conjunction with causing stress transmission relatively poor between carbon nanotube and the polymeric matrix.Therefore, people carry out functionalization to improve the interface combination between the carbon nano-tube/polymer to carbon nanotube.The two dimensional oxidation Graphene is the same with the one dimension carbon nanotube to have excellent mechanical property, even there are some researches show that graphene oxide has better mechanical property, thereby becomes the focus of recent people's research.There is the scientific research personnel that mechanics and thermomechanical property that graphene oxide improves Resins, epoxy are reported.Studies show that the adding of small amounts Graphene can effectively improve intensity, toughness and the second-order transition temperature of Resins, epoxy.Graphene oxide is better than carbon nanotube aspect the mechanical property of Resins, epoxy improving, and mainly is because graphene oxide has higher specific surface area and graphene oxide uneven surface intermeshes with epoxy matrix and cause stronger interface to be combined.And the graphene oxide surface has functional groups such as hydroxyl, epoxy group(ing) and carboxyl, can react with the hydroxyl of fiberglass surfacing, thereby improves the interface bond strength of matrix and fiber.
Because carbon nanotube is the one dimension carbon material, and Graphene is two-dimentional carbon material, both use simultaneously and are expected to form network structure, and may produce synergy.The research report of at present existing carbon nano-tube modification glass fibre/epoxy matrix composite also has the research of a small amount of Graphene modified glass-fiber/epoxy matrix composite to report.But, the present report that does not also have graphene oxide/carbon nanotube modified synergic glass fiber reinforcement epoxy matrix material.
Summary of the invention
The object of the present invention is to provide a kind of graphene oxide/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites and preparation method thereof.
Technical scheme of the present invention is as follows:
Graphene oxide provided by the invention/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites is to be inorganic nano-filler with graphene oxide and carbon nanotube, be polymeric matrix with Resins, epoxy, pass through solution blended process then earlier inorganic nano-filler and Resins, epoxy are mixed, again the resin matrix that mixes is compound to glass fibre by cladding process, obtains composite product by compression molding curing at last.
The preparation method of graphene oxide provided by the invention/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites, its step is as follows:
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 0.01-20g/L, then, be that the ultrasonic device of 300-1000W carried out supersound process 0.5-5 hour described graphite oxide ethanolic soln with power again, get the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 0.01-20g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 5-30 minute, and then be that the ultrasonic device of 300-1000W carried out supersound process 0.5-5 hour described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 50-80 degree centigrade baking oven, dried by the fire 10-48 hour, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation 10-20 minute, obtain mixture, bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble is only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Advantage of the present invention and characteristics are:
Adopt the interlayer shear performance of carbon nanomaterial (graphene oxide) with carbon nanomaterial (carbon nanotube) the modified synergic glass reinforced epoxy based composites of one dimension of two dimension, when utilizing both separately excellent properties, also use the synergistic effect that they produce together, thereby strengthened matrix resin, also made matrix resin be combined more firmly with the interface of glass fibre.Therefore make the matrix material of preparation have excellent interlayer shear performance.
Embodiment
Embodiment 1
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 0.01g/L, then, is that the ultrasonic device of 1000W carried out supersound process 0.5 hour to described graphite oxide ethanolic soln with power again, gets the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 20g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 30 minutes, and then be that the ultrasonic device of 1000W carried out supersound process 0.5 hour to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 80 degrees centigrade baking oven, dried by the fire 10 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 20 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Embodiment 2
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 1g/L, then, is that the ultrasonic device of 300W carried out supersound process 5 hours to described graphite oxide ethanolic soln with power again, gets the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 19g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 5 minutes, and then be that the ultrasonic device of 300W carried out supersound process 0.5 hour to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 50 degrees centigrade baking oven, dried by the fire 48 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 10 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Embodiment 3
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 0.2g/L, then, is that the ultrasonic device of 600W carried out supersound process 2 hours to described graphite oxide ethanolic soln with power again, gets the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 1.0g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 20 minutes, and then be that the ultrasonic device of 800W carried out supersound process 3 hours to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 80 degrees centigrade baking oven, dried by the fire 30 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 20 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Embodiment 4
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 1.0g/L, then, is that the ultrasonic device of 800W carried out supersound process 4 hours to described graphite oxide ethanolic soln with power again, gets the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 1.0g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 30 minutes, and then be that the ultrasonic device of 1000W carried out supersound process 3 hours to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 80 degrees centigrade baking oven, dried by the fire 24 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 15 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Embodiment 5
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 1.5g/L, then, be that the ultrasonic device of 1000W carried out supersound process 0.5-5 hour described graphite oxide ethanolic soln with power again, get the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 5g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 20 minutes, and then be that the ultrasonic device of 600W carried out supersound process 5 hours to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 80 degrees centigrade baking oven, dried by the fire 48 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 20 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Embodiment 6
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 0.5g/L, then, is that the ultrasonic device of 1000W carried out supersound process 5 hours to described graphite oxide ethanolic soln with power again, gets the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 1.0g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 30 minutes, and then be that the ultrasonic device of 1000W carried out supersound process 5 hours to described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 80 degrees centigrade baking oven, dried by the fire 48 hours, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation is 20 minutes, obtains mixture, and bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
Claims (5)
1. graphene oxide/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites is characterized in that, this matrix material comprises epoxy resin-base material and the nanometer inorganic filler that is dispersed in this epoxy resin-base material.
2. by the described graphene oxide of claim 1/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites, it is characterized in that the body material of described matrix material is Resins, epoxy.
3. by the described graphene oxide of claim 1/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites, it is characterized in that described nanometer inorganic filler is graphene oxide and carbon nanotube.
4. the preparation method of graphene oxide/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites, its step is as follows:
1) graphene oxide is dispersed in the ethanol, compound concentration is the graphene oxide ethanolic soln of 0.01-20g/L, then, be that the ultrasonic device of 300-1000W carried out supersound process 0.5-5 hour described graphite oxide ethanolic soln with power again, get the graphene oxide ethanolic soln;
2) adding carbon nanotube and Resins, epoxy make its concentration be respectively 0.01-20g/L and 200g/L in the graphene oxide ethanolic soln of step 1) gained, obtain mixed solution, and with magnetic stirrer mixed solution 5-30 minute, and then be that the ultrasonic device of 300-1000W carried out supersound process 0.5-5 hour described mixed solution with power;
3) with step 2) to put into temperature through the mixed solution of supersound process be 50-80 degree centigrade baking oven, dried by the fire 10-48 hour, extracts alcohol solvent in the described mixed solution out with vacuum pump again, do not have bubble to mixed solution and end;
4) add stoichiometric solidifying agent in the mixed solution of step 3), at room temperature magnetic agitation 10-20 minute, obtain mixture, bubble in the mixture is extracted with vacuum pump in magnetic agitation limit in limit then, and no bubble is only to the mixture;
5) mixture of step 4) gained is coated in the glasscloth surface, stacked together the glasscloth that was coated with epoxy resin composition then, by the method for mold pressing, forming and hardening obtains composite product.
5. press the preparation method of the described graphene oxide of claim 4/carbon nanotube modified synergic glass fiber reinforcement epoxy based composites, it is characterized in that, earlier graphene oxide, carbon nanotube and the Resins, epoxy matrix resin that obtains admixed together, again matrix resin and the compound matrix material that obtains of glass fibre.
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Application publication date: 20130821 |