CN104530653B - A kind of preparation method of epoxy resin/graphite alkene/Nanometer Copper composite - Google Patents
A kind of preparation method of epoxy resin/graphite alkene/Nanometer Copper composite Download PDFInfo
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- CN104530653B CN104530653B CN201410828545.1A CN201410828545A CN104530653B CN 104530653 B CN104530653 B CN 104530653B CN 201410828545 A CN201410828545 A CN 201410828545A CN 104530653 B CN104530653 B CN 104530653B
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Abstract
The preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite, relates to the preparation method of a kind of epoxy resin composite material.The present invention is to solve that current epoxy resin is not provided simultaneously with excellent electric conductivity and the technical problem of excellent mechanical performance.The present invention: one, prepare graphene oxide colloidal sol；Two, graphene oxide-loaded nano copper powder；Three, the Graphene of load copper nanoparticle dispersion in the epoxy；Four, solidification.The invention have the advantages that one, graphene/nanometer copper favorable dispersibility in the epoxy in epoxy resin/graphite alkene/Nanometer Copper composite prepared by the inventive method；Two, compared with pure epoxy resin, the tensile strength of epoxy resin/graphite alkene/Nanometer Copper composite prepared by the present invention increases substantially；The glass transition temperature of epoxy resin/graphite alkene/Nanometer Copper composite that three, prepared by the present invention is improved compared with pure epoxy resin.
Description
Technical field
The present invention relates to the preparation method of a kind of epoxy resin composite material.
Background technology
Containing phenyl ring and ehter bond in epoxy resin (EP) structure, therefore there is excellent electrical insulating property, resistant to chemical media and glue
Connecing property, is widely used in coating, adhesive and engineering material field.EP adhesive gold non-to various metals and major part
Belonging to material and all have good cementability, metal sticks with glue agent requirement, and it has certain electric conductivity, need to be modified EP.
EP matter is crisp, and it is carried out toughening modifying is also necessary.
Graphene has electric conductivity, heat conductivity and the biocompatibility of excellence, and it is the material that mankind's known strength is the highest, than
Diamond is the hardest, and taller upper 300 times of the iron and steel that strength ratio is the most best, being uniformly dispersed in epoxy resin can
To be greatly enhanced the toughness of epoxy resin.Nanometer Copper metal material has good electric conductivity and low electron mobility, as
Electrically-conducting paint, conducting wire material and electrode material are widely used in electronics industry, thus to copper nanoparticle electrically-conducting paint
Research be increasingly subject to people's attention, be uniformly dispersed in epoxy resin and can well be improved epoxy resin
Electric conductivity.
But, current epoxy resin is not provided simultaneously with excellent electric conductivity and excellent mechanical performance.
Summary of the invention
The present invention is to solve that current epoxy resin is not provided simultaneously with excellent electric conductivity and the technology of excellent mechanical performance
Problem, and the preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite is provided.
The preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite of the present invention is carried out according to the following steps:
One, prepare graphene oxide colloidal sol: prepare graphene oxide by traditional Hummers method, by graphene oxide with
Distilled water is ultrasonic after mixing, and obtains graphene oxide colloidal sol；In described graphene oxide colloidal sol, the concentration of graphene oxide is
0.01g/mL；
Two, graphene oxide-loaded nano copper powder: by CuSO4 .5H2O adds in distilled water ultrasonic to being completely dissolved, and obtains
Copper sulfate solution, graphene oxide colloidal sol step one prepared and copper sulfate solution are poured in the there-necked flask of 250mL,
Room temperature sonic oscillation 1h, is then placed within low whipping speed in the water-bath of 70 DEG C and is sequentially added into water under conditions of being 300r/min
Close hydrazine aqueous solution and sodium hydrate aqueous solution, continue low whipping speed in the water-bath of 70 DEG C and stir under conditions of being 300r/min
Mix 45min, be naturally down to room temperature, obtain loading the Graphene of copper nanoparticle；The concentration of described copper sulfate solution is
0.0267g/mL；The concentration of described sodium hydrate aqueous solution is 0.05g/mL；The volume of described hydrazine hydrate aqueous solution is dense
Degree is 61.54%；Described graphene oxide colloidal sol and the volume ratio of copper sulfate solution are 1:2；Described hydrazine hydrate is water-soluble
Liquid is 1:2.3 with the volume ratio of copper sulfate solution；Described sodium hydrate aqueous solution with the volume ratio of copper sulfate solution is
1:3；
Three, the Graphene of load copper nanoparticle dispersion in the epoxy: the stone of the load copper nanoparticle that step 2 is obtained
Ink alkene joins in epoxy resin, disperses 5min～7min with mulser, obtain ring under conditions of rotating speed is 7000r/min
Epoxy resins/graphene/nanometer copper mixture；Described epoxy resin is E-51；The load Nanometer Copper that described step 2 obtains
The Graphene of powder and the mass ratio of epoxy resin are 1:(6.25～200)；
Four, solidification: the inner surface at Teflon mould coats fine vacuum silicone grease, and then inner surface scribbles fine vacuum silicon
Epoxy resin/graphite alkene/Nanometer Copper mixture and firming agent that the Teflon mould of fat, step 3 obtain are respectively put into
The baking oven of 60 DEG C is incubated 2h, then by preheated epoxy resin/graphite alkene/Nanometer Copper mixture and preheated firming agent
Under conditions of rotating speed be 100r/min, stir 4min～5min after mixing, obtain epoxy resin/graphite alkene/Nanometer Copper prepolymer,
Pour epoxy resin/graphite alkene/Nanometer Copper prepolymer into preheated inner surface and scribble the politef mould of fine vacuum silicone grease
In tool, under conditions of temperature is 70 DEG C, it is incubated 2h, is warming up to 125 DEG C and under conditions of temperature is 125 DEG C, is incubated 2.5h,
Be warming up to 150 DEG C and under conditions of temperature is 150 DEG C be incubated 1h, be naturally down to room temperature, obtain epoxy resin/graphite alkene/
Nanometer Copper composite；Described firming agent is polyamide 6 51；Described firming agent and the epoxy resin described in step 3
Mass ratio be 1:2.
The invention have the advantages that
One, in epoxy resin/graphite alkene/Nanometer Copper composite that prepared by the inventive method, graphene/nanometer copper is at epoxy resin
In favorable dispersibility；
Two, compared with pure epoxy resin, the tensile strength of epoxy resin/graphite alkene/Nanometer Copper composite prepared by the present invention
60% can be improved；
Three, as the 10wt% that graphene/nanometer copper content is epoxy resin, epoxy resin/graphite alkene prepared by the present invention/
The glass transition temperature of Nanometer Copper composite improves general 8 DEG C compared with pure epoxy resin.
Accompanying drawing explanation
Fig. 1 is the SEM figure of pure epoxy resin；
Fig. 2 is the SEM figure of the epoxy resin/graphite alkene/Nanometer Copper composite of test two preparation；
Fig. 3 be XRD figure spectrum, curve a is pure epoxy resin, curve b be test two preparation epoxy resin/graphite alkene/
Nanometer Copper composite, curve c is the copper nanoparticle of test three preparation；
Fig. 4 is DMA figure, and curve 1 is pure epoxy resin, and curve 2 is the epoxy resin/graphite alkene/receive of test one preparation
Rice carbon/carbon-copper composite material；
Fig. 5 is mechanical property figure, and it is negative that the mass fraction of transverse axis refers to that the step 2 described in step 3 in the present invention obtains
The Graphene carrying copper nanoparticle accounts for the mass fraction of epoxy resin, and a point is pure epoxy resin, and b point is the ring that test one obtains
Epoxy resins/graphene/nanometer copper composite material, c point is epoxy resin/graphite alkene/Nanometer Copper composite that test two obtains.
Detailed description of the invention
Detailed description of the invention one: present embodiment is the preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite,
Carry out the most according to the following steps:
One, prepare graphene oxide colloidal sol: prepare graphene oxide by traditional Hummers method, by graphene oxide with
Distilled water is ultrasonic after mixing, and obtains graphene oxide colloidal sol；In described graphene oxide colloidal sol, the concentration of graphene oxide is
0.01g/mL；
Two, graphene oxide-loaded nano copper powder: by CuSO4 .5H2O adds in distilled water ultrasonic to being completely dissolved, and obtains
Copper sulfate solution, graphene oxide colloidal sol step one prepared and copper sulfate solution are poured in the there-necked flask of 250mL,
Room temperature sonic oscillation 1h, is then placed within low whipping speed in the water-bath of 70 DEG C and is sequentially added into water under conditions of being 300r/min
Close hydrazine aqueous solution and sodium hydrate aqueous solution, continue low whipping speed in the water-bath of 70 DEG C and stir under conditions of being 300r/min
Mix 45min, be naturally down to room temperature, obtain loading the Graphene of copper nanoparticle；The concentration of described copper sulfate solution is
0.0267g/mL；The concentration of described sodium hydrate aqueous solution is 0.05g/mL；The volume of described hydrazine hydrate aqueous solution is dense
Degree is 61.54%；Described graphene oxide colloidal sol and the volume ratio of copper sulfate solution are 1:2；Described hydrazine hydrate is water-soluble
Liquid is 1:2.3 with the volume ratio of copper sulfate solution；Described sodium hydrate aqueous solution with the volume ratio of copper sulfate solution is
1:3；
Three, the Graphene of load copper nanoparticle dispersion in the epoxy: the stone of the load copper nanoparticle that step 2 is obtained
Ink alkene joins in epoxy resin, disperses 5min～7min with mulser, obtain ring under conditions of rotating speed is 7000r/min
Epoxy resins/graphene/nanometer copper mixture；Described epoxy resin is E-51；The load Nanometer Copper that described step 2 obtains
The Graphene of powder and the mass ratio of epoxy resin are 1:(6.25～200)；
Four, solidification: the inner surface at Teflon mould coats fine vacuum silicone grease, and then inner surface scribbles fine vacuum silicon
Epoxy resin/graphite alkene/Nanometer Copper mixture and firming agent that the Teflon mould of fat, step 3 obtain are respectively put into
The baking oven of 60 DEG C is incubated 2h, then by preheated epoxy resin/graphite alkene/Nanometer Copper mixture and preheated firming agent
Under conditions of rotating speed be 100r/min, stir 4min～5min after mixing, obtain epoxy resin/graphite alkene/Nanometer Copper prepolymer,
Pour epoxy resin/graphite alkene/Nanometer Copper prepolymer into preheated inner surface and scribble the politef mould of fine vacuum silicone grease
In tool, under conditions of temperature is 70 DEG C, it is incubated 2h, is warming up to 125 DEG C and under conditions of temperature is 125 DEG C, is incubated 2.5h,
Be warming up to 150 DEG C and under conditions of temperature is 150 DEG C be incubated 1h, be naturally down to room temperature, obtain epoxy resin/graphite alkene/
Nanometer Copper composite；Described firming agent is polyamide 6 51；Described firming agent and the epoxy resin described in step 3
Mass ratio be 1:2.
Present embodiment advantage:
One, in epoxy resin/graphite alkene/Nanometer Copper composite that prepared by the method for present embodiment, graphene/nanometer copper is at ring
Favorable dispersibility in epoxy resins；
Two, compared with pure epoxy resin, the tension of epoxy resin/graphite alkene/Nanometer Copper composite prepared by present embodiment
Intensity can improve 60%；
Three, as the 10wt% that graphene/nanometer copper content is epoxy resin, epoxy resin/graphite prepared by present embodiment
The glass transition temperature of alkene/Nanometer Copper composite improves general 8 DEG C compared with pure epoxy resin.
Detailed description of the invention two: present embodiment is unlike detailed description of the invention one: traditional described in step one
Hummers method prepares the step of graphene oxide:
The flaky graphite powder taking 1.2g joins in the glass there-necked flask that volume is 500mL, adds the dense sulfur of 50mL
Acid, stirs 30min under conditions of room temperature and mixing speed are 250r/min, is put in ice-water bath by glass there-necked flask, then
Being slowly added to the potassium permanganate of 10g and the sodium nitrate of 1.5g, low whipping speed is to stir under conditions of 200r/min and ice-water bath
Mix 2h, under conditions of room temperature and mixing speed are 250r/min, after being taken out from ice-water bath by glass there-necked flask, stir 2h,
Then it is stirring 24h under conditions of 250r/min with mixing speed in the water-bath that temperature is 35 DEG C, adds
The mass fraction of 10mL～15mL be 30% hydrogen peroxide solution and the hydrochloric acid that mass fraction is 36%～38% of 10mL water-soluble
Liquid, obtains mixed solution, collects lower floor's thick liquid by centrifugal for mixed solution, thick liquid is put in semipermeable membrane dialysis extremely
Solution is neutral, obtains graphene oxide.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is unlike one of detailed description of the invention one to two: described in step 3
The Graphene of load copper nanoparticle that step 2 obtains is 1:10 with the mass ratio of epoxy resin.Other and detailed description of the invention
One of one to two identical.
Detailed description of the invention four: present embodiment is unlike detailed description of the invention two: traditional described in step one
Hummers method prepare glass there-necked flask is taken out from ice-water bath by the step of graphene oxide after in room temperature and mixing speed
For under conditions of 250r/min stir 2h, then in the water-bath that temperature is 35 DEG C and mixing speed be the condition of 250r/min
Lower stirring 24h, adds the hydrogen peroxide solution that mass fraction is 30% of 12mL and the mass fraction of 10mL is 37%
Aqueous hydrochloric acid solution, obtains mixed solution.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is unlike one of detailed description of the invention one to four: described in step 3
The Graphene of load copper nanoparticle that step 2 obtains is 1:6.25 with the mass ratio of epoxy resin.Other and detailed description of the invention
One of one to four identical.
Use following verification experimental verification effect of the present invention:
Test one: this test is the preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite, specifically by following
Step is carried out:
One, prepare graphene oxide colloidal sol: prepare graphene oxide by traditional Hummers method, by graphene oxide with
Distilled water is ultrasonic after mixing, and obtains graphene oxide colloidal sol；In described graphene oxide colloidal sol, the concentration of graphene oxide is
0.01g/mL；
Two, graphene oxide-loaded nano copper powder: by CuSO4 .5H2O adds in distilled water ultrasonic to being completely dissolved, and obtains
Copper sulfate solution, graphene oxide colloidal sol step one prepared and copper sulfate solution are poured in the there-necked flask of 250mL,
Room temperature sonic oscillation 1h, is then placed within low whipping speed in the water-bath of 70 DEG C and is sequentially added into water under conditions of being 300r/min
Close hydrazine aqueous solution and sodium hydrate aqueous solution, continue low whipping speed in the water-bath of 70 DEG C and stir under conditions of being 300r/min
Mix 45min, be naturally down to room temperature, obtain loading the Graphene of copper nanoparticle；The concentration of described copper sulfate solution is
0.0267g/mL；The concentration of described sodium hydrate aqueous solution is 0.05g/mL；The volume of described hydrazine hydrate aqueous solution is dense
Degree is 61.54%；Described graphene oxide colloidal sol and the volume ratio of copper sulfate solution are 1:2；Described hydrazine hydrate is water-soluble
Liquid is 1:2.3 with the volume ratio of copper sulfate solution；Described sodium hydrate aqueous solution with the volume ratio of copper sulfate solution is
1:3；
Three, the Graphene of load copper nanoparticle dispersion in the epoxy: the stone of the load copper nanoparticle that step 2 is obtained
Ink alkene joins in epoxy resin, disperses 5min with mulser, obtain epoxy resin under conditions of rotating speed is 7000r/min
/ graphene/nanometer copper mixture；Described epoxy resin is E-51；The stone of the load copper nanoparticle that described step 2 obtains
Ink alkene is 1:10 with the mass ratio of epoxy resin；
Four, solidification: the inner surface at Teflon mould coats fine vacuum silicone grease, and then inner surface scribbles fine vacuum silicon
Epoxy resin/graphite alkene/Nanometer Copper mixture and firming agent that the Teflon mould of fat, step 3 obtain are respectively put into
The baking oven of 60 DEG C is incubated 2h, then by preheated epoxy resin/graphite alkene/Nanometer Copper mixture and preheated firming agent
Under conditions of rotating speed is 100r/min, stirs 4min after mixing, obtains epoxy resin/graphite alkene/Nanometer Copper prepolymer, will
Epoxy resin/graphite alkene/Nanometer Copper prepolymer is poured preheated inner surface into and is scribbled the Teflon mould of fine vacuum silicone grease
In, under conditions of temperature is 70 DEG C, it is incubated 2h, is warming up to 125 DEG C and under conditions of temperature is 125 DEG C, is incubated 2.5h,
Be warming up to 150 DEG C and under conditions of temperature is 150 DEG C be incubated 1h, be naturally down to room temperature, obtain epoxy resin/graphite alkene/
Nanometer Copper composite；Described firming agent is polyamide 6 51；Described firming agent and the epoxy resin described in step 3
Mass ratio be 1:2.
Test two: this test is the preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite, specifically by following
Step is carried out:
One, prepare graphene oxide colloidal sol: prepare graphene oxide by traditional Hummers method, by graphene oxide with
Distilled water is ultrasonic after mixing, and obtains graphene oxide colloidal sol；In described graphene oxide colloidal sol, the concentration of graphene oxide is
0.01g/mL；
Two, graphene oxide-loaded nano copper powder: by CuSO4 .5H2O adds in distilled water ultrasonic to being completely dissolved, and obtains
Copper sulfate solution, graphene oxide colloidal sol step one prepared and copper sulfate solution are poured in the there-necked flask of 250mL,
Room temperature sonic oscillation 1h, is then placed within low whipping speed in the water-bath of 70 DEG C and is sequentially added into water under conditions of being 300r/min
Close hydrazine aqueous solution and sodium hydrate aqueous solution, continue low whipping speed in the water-bath of 70 DEG C and stir under conditions of being 300r/min
Mix 45min, be naturally down to room temperature, obtain loading the Graphene of copper nanoparticle；The concentration of described copper sulfate solution is
0.0267g/mL；The concentration of described sodium hydrate aqueous solution is 0.05g/mL；The volume of described hydrazine hydrate aqueous solution is dense
Degree is 61.54%；Described graphene oxide colloidal sol and the volume ratio of copper sulfate solution are 1:2；Described hydrazine hydrate is water-soluble
Liquid is 1:2.3 with the volume ratio of copper sulfate solution；Described sodium hydrate aqueous solution with the volume ratio of copper sulfate solution is
1:3；
Three, the Graphene of load copper nanoparticle dispersion in the epoxy: the stone of the load copper nanoparticle that step 2 is obtained
Ink alkene joins in epoxy resin, disperses 5min with mulser, obtain epoxy resin under conditions of rotating speed is 7000r/min
/ graphene/nanometer copper mixture；Described epoxy resin is E-51；The stone of the load copper nanoparticle that described step 2 obtains
Ink alkene is 1:6.25 with the mass ratio of epoxy resin；
Four, solidification: the inner surface at Teflon mould coats fine vacuum silicone grease, and then inner surface scribbles fine vacuum silicon
Epoxy resin/graphite alkene/Nanometer Copper mixture and firming agent that the Teflon mould of fat, step 3 obtain are respectively put into
The baking oven of 60 DEG C is incubated 2h, then by preheated epoxy resin/graphite alkene/Nanometer Copper mixture and preheated firming agent
Under conditions of rotating speed is 100r/min, stirs 4min after mixing, obtains epoxy resin/graphite alkene/Nanometer Copper prepolymer, will
Epoxy resin/graphite alkene/Nanometer Copper prepolymer is poured preheated inner surface into and is scribbled the Teflon mould of fine vacuum silicone grease
In, under conditions of temperature is 70 DEG C, it is incubated 2h, is warming up to 125 DEG C and under conditions of temperature is 125 DEG C, is incubated 2.5h,
Be warming up to 150 DEG C and under conditions of temperature is 150 DEG C be incubated 1h, be naturally down to room temperature, obtain epoxy resin/graphite alkene/
Nanometer Copper composite；Described firming agent is polyamide 6 51；Described firming agent and the epoxy resin described in step 3
Mass ratio be 1:2.
Test three: this test is the method preparing Nanometer Copper powder body:
By the CuSO of 0.8g4.5H2O joins in 30mL distilled water ultrasonic to dissolving, adds the polyethylene ratio of 0.06g
Pyrrolidone (PVP), ultrasonic 30min, pours the CuSO of ultrasonic dissolution the most respectively in three-necked bottle into4.5H2O's Yu PVP
Mixed solution, adds 13mL hydrazine hydrate aqueous solution, is eventually adding the NaOH aqueous solution of 10mL, turns at 70 DEG C
Speed is stirring 45min under conditions of 300r/min, and the product obtained sucking filtration after cooling, with a large amount of distilled water and dehydrated alcohol
After washing, put into and vacuum drying oven is dried 10h at ambient temperature, finally grind and obtain copper nanoparticle；Described hydrogen-oxygen
The concentration changing sodium water solution is 0.05g/mL；The volumetric concentration of described hydrazine hydrate aqueous solution is 61.54%.
Fig. 1 is the SEM figure of pure epoxy resin, and Fig. 2 is the epoxy resin/graphite alkene/Nanometer Copper composite wood of test two preparation
The SEM figure of material, by Fig. 2 it is observed that add graphene/nanometer copper in pure epoxy resin to make this composite section
Becoming irregular, rough, the line pure epoxy resin compared with Fig. 1 in river is compared and is not apparent from, and adds graphene/nanometer
The new surface that copper is formed is many, namely absorbs impact energy many, and this can improve the feature that pure epoxy resin matter is crisp.
Fig. 3 be XRD figure spectrum, curve a is pure epoxy resin, curve b be test two preparation epoxy resin/graphite alkene/
Nanometer Copper composite, curve c is the copper nanoparticle of test three preparation, owing to epoxy resin absworption peak is very big, so graphite
The summit of alkene is fallen by the peak diffraction of epoxy resin, as can be seen from the figure the epoxy resin/graphite alkene/Nanometer Copper of test two preparation
Composite has the absworption peak of graphene/nanometer copper and epoxy resin, illustrate test two prepared epoxy resin/graphite alkene/
Nanometer Copper composite.
Fig. 4 is DMA figure, and curve 1 is pure epoxy resin, and curve 2 is the epoxy resin/graphite alkene/receive of test one preparation
Rice carbon/carbon-copper composite material, it can be seen that compared with pure epoxy resin, the epoxy resin/graphite alkene of test two preparation/
The fissipation factor peak position of Nanometer Copper composite is substantially moved to high temperature direction, i.e. the addition of Nanometer Copper improves epoxy resin
Tg, improve general 8 DEG C.
Fig. 5 is mechanical property figure, and it is negative that the mass fraction of transverse axis refers to that the step 2 described in step 3 in the present invention obtains
The Graphene carrying copper nanoparticle accounts for the mass fraction of epoxy resin, and a point is pure epoxy resin, and b point is the ring that test one obtains
Epoxy resins/graphene/nanometer copper composite material, c point is epoxy resin/graphite alkene/Nanometer Copper composite that test two obtains,
As can be seen from the figure the tensile strength of pure epoxy resin is 31.14Mpa, but is as the addition mechanics of graphene/nanometer copper
Performance is remarkably reinforced, the mechanics of epoxy resin/graphite alkene/Nanometer Copper composite that this explanation test one and test two are prepared
Performance is than the excellence of pure epoxy resin, the tensile strength of the epoxy resin/graphite alkene/Nanometer Copper composite of test one preparation
Being 47.82Mpa, the tensile strength of the epoxy resin/graphite alkene/Nanometer Copper composite of test two preparation is 54.56Mpa,
60% is improve compared with pure epoxy resin.
Claims (4)
1. the preparation method of epoxy resin/graphite alkene/Nanometer Copper composite, it is characterised in that epoxy resin/graphite alkene/
The preparation method of Nanometer Copper composite is carried out according to the following steps:
One, graphene oxide colloidal sol is prepared: prepare graphene oxide by traditional Hummers method, by graphene oxide and steaming
Distilled water is ultrasonic after mixing, and obtains graphene oxide colloidal sol；In described graphene oxide colloidal sol, the concentration of graphene oxide is
0.01g/mL；
Two, graphene oxide-loaded nano copper powder: by CuSO4.5H2O adds in distilled water ultrasonic to being completely dissolved, and obtains
Copper sulfate solution, graphene oxide colloidal sol step one prepared and copper sulfate solution are poured in the there-necked flask of 250mL,
Room temperature sonic oscillation 1h, is then placed within low whipping speed in the water-bath of 70 DEG C and is sequentially added into hydration under conditions of being 300r/min
Hydrazine aqueous solution and sodium hydrate aqueous solution, continue to stir under conditions of in the water-bath of 70 DEG C, low whipping speed is 300r/min
45min, is down to room temperature naturally, obtains loading the Graphene of copper nanoparticle；The concentration of described copper sulfate solution is
0.0267g/mL；The concentration of described sodium hydrate aqueous solution is 0.05g/mL；The volumetric concentration of described hydrazine hydrate aqueous solution
It is 61.54%；Described graphene oxide colloidal sol and the volume ratio of copper sulfate solution are 1:2；Described hydrazine hydrate aqueous solution
It is 1:2.3 with the volume ratio of copper sulfate solution；Described sodium hydrate aqueous solution is 1:3 with the volume ratio of copper sulfate solution；
Three, the Graphene of load copper nanoparticle dispersion in the epoxy: the stone of the load copper nanoparticle that step 2 is obtained
Ink alkene joins in epoxy resin, disperses 5min～7min with mulser, obtain epoxy under conditions of rotating speed is 7000r/min
Resin/graphite alkene/Nanometer Copper mixture；Described epoxy resin is E-51；The load copper nanoparticle that described step 2 obtains
The mass ratio of Graphene and epoxy resin be 1:(6.25～200)；
Four, solidification: the inner surface at Teflon mould coats fine vacuum silicone grease, and then inner surface scribbles fine vacuum silicon
Epoxy resin/graphite alkene/Nanometer Copper mixture and firming agent that the Teflon mould of fat, step 3 obtain are respectively put into
The baking oven of 60 DEG C is incubated 2h, then by preheated epoxy resin/graphite alkene/Nanometer Copper mixture and preheated firming agent
Under conditions of rotating speed be 100r/min, stir 4min～5min after mixing, obtain epoxy resin/graphite alkene/Nanometer Copper prepolymer,
Pour epoxy resin/graphite alkene/Nanometer Copper prepolymer into preheated inner surface and scribble the Teflon mould of fine vacuum silicone grease
In, under conditions of temperature is 70 DEG C, it is incubated 2h, is warming up to 125 DEG C and under conditions of temperature is 125 DEG C, is incubated 2.5h,
It is warming up to 150 DEG C and under conditions of temperature is 150 DEG C, is incubated 1h, being naturally down to room temperature, obtain epoxy resin/graphite alkene/receive
Rice carbon/carbon-copper composite material；Described firming agent is polyamide 6 51；Described firming agent and the epoxy resin described in step 3
Mass ratio is 1:2；
Traditional Hummers method described in step one prepares the step of graphene oxide:
The flaky graphite powder taking 1.2g joins in the glass there-necked flask that volume is 500mL, adds the concentrated sulphuric acid of 50mL,
Under conditions of room temperature and mixing speed are 250r/min, stir 30min, glass there-necked flask is put in ice-water bath, more slowly
Adding potassium permanganate and the sodium nitrate of 1.5g of 10g, low whipping speed is stirring 2h under conditions of 200r/min and ice-water bath,
Under conditions of room temperature and mixing speed are 250r/min, 2h is stirred, then in temperature after being taken out from ice-water bath by glass there-necked flask
Degree is in the water-bath of 35 DEG C and mixing speed is to stir 24h under conditions of 250r/min, adds the quality of 10mL～15mL
Mark is hydrogen peroxide solution and the aqueous hydrochloric acid solution that mass fraction is 36%～38% of 10mL of 30%, obtains mixed solution,
Collecting lower floor's thick liquid by centrifugal for mixed solution, it is neutrality to solution that thick liquid is put into dialysis in semipermeable membrane, obtains oxygen
Functionalized graphene.
The preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite the most according to claim 1, its feature
Under conditions of room temperature and mixing speed are 250r/min, 2h is stirred, then after being to take out glass there-necked flask from ice-water bath
Being stirring 24h under conditions of 250r/min with mixing speed in the water-bath that temperature is 35 DEG C, the quality adding 12mL is divided
Number is hydrogen peroxide solution and the aqueous hydrochloric acid solution that mass fraction is 37% of 10mL of 30%, obtains mixed solution.
The preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite the most according to claim 1, its feature
It is that the Graphene of load copper nanoparticle that the step 2 described in step 3 obtains is 1:10 with the mass ratio of epoxy resin.
The preparation method of a kind of epoxy resin/graphite alkene/Nanometer Copper composite the most according to claim 1, its feature
It is that the Graphene of load copper nanoparticle that the step 2 described in step 3 obtains is 1:6.25 with the mass ratio of epoxy resin.
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| CN105850984B (en) * | 2016-05-23 | 2019-04-16 | 新乡医学院第三附属医院 | A kind of brain slice in vitro electric signal recording device based on novel stimulating electrode |
| CN106670501B (en) * | 2016-12-29 | 2020-04-10 | 陕西理工大学 | Preparation method of graphene-metal matrix composite powder |
| CN107814507B (en) * | 2017-10-25 | 2020-09-25 | 江***醇新材料科技有限公司 | Graphene-based heat-conducting composite material and preparation method and application thereof |
| CN108342177B (en) * | 2018-03-28 | 2020-09-01 | 黑龙江省科学院石油化学研究院 | Preparation method of high-dispersion graphene oxide reinforced epoxy resin adhesive |
| CN109593322A (en) * | 2018-12-04 | 2019-04-09 | 黑龙江大学 | The preparation method of graphene-supported corronil reinforced epoxy composite material |
| CN110655755A (en) * | 2019-10-09 | 2020-01-07 | 荆楚理工学院 | Preparation method of silver nanoparticle loaded graphene-based epoxy resin composite material |
| CN112408868A (en) * | 2019-12-23 | 2021-02-26 | 鲍欢 | Preparation method of wear-resistant impact-resistant epoxy mortar repair material |
| CN111269536A (en) * | 2020-04-16 | 2020-06-12 | 扬州金霞塑胶有限公司 | Nano cellulose/copper composite material modified resin and preparation method thereof |
| CN111995978B (en) * | 2020-09-08 | 2022-03-15 | 株洲飞鹿高新材料技术股份有限公司 | Low-temperature quick-drying polymer-based conductive adhesive and preparation method thereof |
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| CN102286189B (en) * | 2011-06-24 | 2012-11-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| CN102581295A (en) * | 2012-01-10 | 2012-07-18 | 黑龙江大学 | Method of using liquid-phase reduction method to prepare nano copper powder loaded graphene |
| CN103374207B (en) * | 2012-04-18 | 2017-04-19 | 国家纳米科学中心 | Epoxy composite material and preparation method thereof |
| CN103408895A (en) * | 2013-04-18 | 2013-11-27 | 北京化工大学常州先进材料研究院 | Preparation method of graphene/epoxy resin composite material |
| CN103193978B (en) * | 2013-04-24 | 2015-07-08 | 黑龙江大学 | Preparation method for polyaniline/graphene/nano-copper composite material |
| CN103408897A (en) * | 2013-07-08 | 2013-11-27 | 陆静 | Graphene nano composite material |
| CN103525013A (en) * | 2013-10-17 | 2014-01-22 | 嘉兴市隆鑫碳纤维制品有限公司 | Conducting carbon fiber composite material as well as preparation method thereof |
| CN103554861B (en) * | 2013-11-04 | 2015-09-09 | 哈尔滨市都邦节能科技有限公司 | A kind of preparation method of Graphene polymer sheet material |
| CN103724938B (en) * | 2013-12-06 | 2015-10-21 | 黑龙江大学 | A kind of preparation method of nano-copper/epoxy resin composite material |
| CN104140639B (en) * | 2014-08-01 | 2016-08-24 | 黑龙江大学 | A kind of preparation method of Graphene/epoxy resin composite material |
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