CN105619916B - A kind of carbon fibre composite of nanometer of toughness reinforcing and preparation method thereof - Google Patents
A kind of carbon fibre composite of nanometer of toughness reinforcing and preparation method thereof Download PDFInfo
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- CN105619916B CN105619916B CN201510994172.XA CN201510994172A CN105619916B CN 105619916 B CN105619916 B CN 105619916B CN 201510994172 A CN201510994172 A CN 201510994172A CN 105619916 B CN105619916 B CN 105619916B
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- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B32B2307/00—Properties of the layers or laminate
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- B32B2307/54—Yield strength; Tensile strength
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- B32B2307/00—Properties of the layers or laminate
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- B32B2307/542—Shear strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
Abstract
The invention provides carbon fibre composite of a kind of nanometer of toughness reinforcing and preparation method thereof, belong to carbon fibre composite technical field.The carbon fibre composite of the present invention is molded with by 16~20 layers of prepreg, 1 layer of Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film molded curing；Wherein, the Activated Graphite alkene/halloysite nanotubes laminated film is by 10~15% amination graphenes, and the halloysite nanotubes of 70~80% benzyl glycidyl ether and 10~15% modified grafting long-chain polymers are made；The Activated Carbon Nanotubes/halloysite nanotubes laminated film is made up of the halloysite nanotubes of the modified grafting long-chain polymer of 10~15% CNT and 70~80% benzyl glycidyl ether and 10~15%.The deficiency overcome in prior art of the present invention, is realized to carbon fibre composite various dimensions, the mechanical property of carbon fibre composite is greatly improved in multiple dimensioned activeness and quietness.
Description
Technical field：
The present invention relates to carbon fibre composite technical field, and in particular to a kind of graphene/halloysite nanotubes film and
The carbon fibre composite of CNT/halloysite nanotubes film coordination plasticizing.
Background technology：
Graphene is that have carbon atom, into the individual layer two-dimension plane structure of honeycomb crystal lattice, to have by regular hexagon close-packed arrays
Stronger electric conductivity, higher intensity.The original lamella of graphene because its low apparent activation energy, tend not to very well and it is poly-
Compound infiltrates and reaches and disperse well, finally causes its enhanced composite property not rise anti-drop.
Since Japanese Scientists find CNT since 1991, its preparation method, performance and application are obtained for extensively
Research.The caliber of CNT is in 2-20nm, and length can reach micron level, and larger draw ratio and specific surface area holds it
Easily reunite, it is difficult to scatter in the base.Meanwhile, surface inertness makes its interface binding power between matrix weaker,
Stress can not be shifted effectively between matrix and CNT during stand under load.
Interface cohesion is bad and bad dispersibility of the nano-particle in resin matrix, is a nanometer reinforcing fiber resin base all the time
Key issue in composite.General simple mechanical mixture is difficult so that nano-particle effectively disperses in resin matrix.
There is fragility height, the low problem of toughness, traditional solution as a kind of high-performance composite materials in carbon fibre composite
Certainly method has thermoplastic resin modified, rubber particles modification etc..However, passing through the conventional methods such as thermoplastic resin and rubber particles
It is modified, although can to improve the toughness of composite, but the heat resistance of composite can be caused to decline, modulus decline etc. one is
Row problem.Carbon fibre composite is prepared present invention employs the toughening carbon fiber reinforced prepreg of nano-particle interlayer, can be significantly
The toughness of material is improved, while can also improve the modulus of composite, high-performance composite materials are obtained.
The content of the invention：
Present invention aims to overcome that there is provided a kind of stone for the characteristics of carbon fibre composite toughness in prior art is not enough
The carbon fibre composite of black alkene/CNT/halloysite nanotubes coordination plasticizing, the carbon fibre composite is by 16~20
Layer prepreg film, 1 layer of Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes
Laminated film molded curing is molded with；Wherein, the Activated Graphite alkene/halloysite nanotubes laminated film is by 10~15% ammonia
The galapectite of base graphite alkene, 70~80% benzyl glycidyl ether and 10~15% modified grafting long-chain polymers is received
Mitron is made；The Activated Carbon Nanotubes/halloysite nanotubes laminated film is by 10~15% CNT and 70~80%
Benzyl glycidyl ether and the halloysite nanotubes of 10~15% modified grafting long-chain polymers be made.
Further, the thickness of the carbon fibre composite is：2~3mm, the prepreg thickness be 0.09~
0.17mm, Activated Graphite alkene/halloysite nanotubes laminated film thickness are 50~80 μm, Activated Carbon Nanotubes/galapectite nanometer
The thickness of pipe laminated film is 50~80 μm.
Further, the ply stacking-sequence of the carbon fibre composite is respectively from top to bottom：8~10 layers of prepreg, 1 layer of work
Property graphene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film and 8~10 layers
Prepreg.
Meanwhile, the present invention also provides a kind of preparation method of carbon fibre composite, and the carbon fibre composite is used
Prepared by die pressing, be specifically by 0.09~0.17mm carbon fiber prepreg, Activated Graphite alkene/halloysite nanotubes laminated film
It is placed in Activated Carbon Nanotubes/halloysite nanotubes laminated film in compression molding instrument, according to the solidification work of carbon fiber prepreg
Skill carries out curing molding, is finally pressed into the unidirectional composite material laminate that thickness is 2~3mm.
Wherein, the preparation method of Activated Graphite alkene/halloysite nanotubes laminated film comprises the following steps：
A) halloysite nanotubes are added in hydrochloric acid solution, remove a layer turbid solution, plus distilled water centrifugal treating, take precipitation
Thing is dried, grinding, obtains powder I；
B) sodium chloride solution is added in powder I, stirred, distilled water centrifugal treating, dried under the conditions of 105 DEG C, grinding is obtained
To powder II；
C) cetyl trimethylammonium bromide is added in powder II, 60 DEG C of oil bath stirrings, ethanol is centrifuged, 90 DEG C of drying,
Grinding, obtains the halloysite nanotubes of modified grafting long-chain polymer；
D) amination graphene is mixed in benzyl glycidyl ether, mechanical agitation obtains mixed liquor I；
E) mixed liquor I is added in ball mill, under nitrogen protection ball milling, obtains mixed liquor II；
F) oil bath under conditions of mixed liquor II being placed in into 150 ± 5 DEG C, then normal temperature standing, obtains the mixing of Activated Graphite alkene
Liquid；
G) halloysite nanotubes of modified grafting long-chain polymer are added in Activated Graphite alkene mixed liquor, are mixed
Close liquid III；
H) mixed liquor III is heated to 90 ± 5 DEG C, and the mechanical agitation under conditions of 90 ± 5 DEG C after being thoroughly mixed, obtained
Mixed liquor IV；
I) by mixed liquor IV under 60W ultrasonic powers ultrasonically treated, obtained Activated Graphite alkene galapectite after normal temperature is stood
Nanotube mixed liquor；
J) by Activated Graphite alkene/halloysite nanotubes mixed liquor film, then normal temperature is stood, and obtains graphene/galapectite
Nanotube composite film.
The preparation method of the Activated Carbon Nanotubes/halloysite nanotubes laminated film comprises the following steps：
A) aminated carbon nano tube is added in benzyl glycidyl ether, stirs, obtain mixed liquor 1.；
B) 1. mixed liquor is added in ball mill, under nitrogen protection ball milling, obtains mixed liquor 2.；
C) by the mixed liquor 2. oil bath under conditions of 150 ± 5 DEG C, then normal temperature is stood, and obtains Activated Carbon Nanotubes mixing
Liquid；
D) the halloysite nanotubes finished product of modified grafting long-chain polymer is added in Activated Carbon Nanotubes mixed liquor,
And it is heated to 90 ± 5 DEG C, 3. the mechanical agitation under conditions of 90 ± 5 DEG C obtains mixed liquor；
E) 3. mixed liquor is placed in ultrasonically treated under 60W ultrasonic powers, then normal temperature is stood, obtained activated carbon nanometer
Pipe/halloysite nanotubes mixed liquor；
F) Activated Carbon Nanotubes/halloysite nanotubes mixed liquor is subjected to film on tetrafluoroethene flat board, normal temperature is stood,
Obtain CNT/halloysite nanotubes laminated film.
Further, the condition of the ball milling is：Interval is needed after 200~500r/min of rotational speed of ball-mill, continuous ball milling 10min
5min, 0.5~4h of Ball-milling Time.
The method of film of the present invention includes：Glass bar film is used, with rejection film machine film, film applicator film is used.
Beneficial effect：
One：
The deficiency overcome in prior art of the present invention, by the mixed processing of Activated Graphite alkene/halloysite nanotubes,
The mixed processing of Activated Carbon Nanotubes/halloysite nanotubes, realizes to composite various dimensions, multiple dimensioned activeness and quietness, leads to
The data for crossing embodiment 1~4 can be seen that the mechanical property for substantially increasing composite.
First, the present invention to amination graphene by pre-processing, by amination graphene with benzyl glycidol
Ether reacts, and is handled by wet ball grinding and obtains Activated Graphite alkene.Secondly, will by being pre-processed to aminated carbon nano tube
Aminated carbon nano tube reacts with benzyl glycidyl ether, is handled by wet ball grinding and obtains Activated Carbon Nanotubes, finally, this hair
It is bright by being pre-processed to halloysite nanotubes, the halloysite nanotubes of purchase and concentration hydrochloric acid reaction are stood.Outwell
Clear liquid, distilled water centrifugal treating to PH=6 is dried, grinding.Then sodium chloride solution reaction is added, distilled water centrifugal treating is straight
To not chloride ion-containing, dry, grinding.Last same cetyl trimethylammonium bromide, ethanol centrifugation, drying, grinding is modified
The halloysite nanotubes of grafting long-chain polymer afterwards.
The present invention is carried out liquid active graphene with modified halloysite nanotubes by above-mentioned three kinds of preprocessing process
Mix processing, obtain Activated Graphite alkene/halloysite nanotubes mixed liquor.Afterwards with conventional coating method by Activated Graphite alkene/angstrom
Lip river stone nanotube mixed liquor carries out film.Liquid active CNT is carried out with modified halloysite nanotubes to mix processing,
Obtain Activated Carbon Nanotubes/halloysite nanotubes mixed liquor.Conventional coating method is used afterwards by CNT/halloysite nanotubes
Mixed liquor carries out film.Finally by two layers of nano composite membrane be layered on prepreg between compression molding prepare composite laminated plate,
Wherein, the conventional coating method includes using glass bar film, with rejection film machine film, with the existing film side such as film applicator film
Method.
Secondly：
The present invention is prepared for two kinds of nano composite membranes for being applied to interlayer toughened.Added in the preparation process of composite membrane
Halloysite nanotubes can improve the dispersiveness of graphene and CNT in resin matrix.It is pre- in composite membrane interlayer toughened
During leaching material, the matrix of composite membrane is studied, the orientation technology of nano-particle is employed so that graphene and carbon
Nanotube can well disperse in composite membrane.Meanwhile, resin control technique is being carried out to composite membrane matrix so that two layers is not
Adding between prepreg, will not be separated at the composite material interface prepared, with prepreg matrix with composite membrane
There is good compatibility.Composite membrane storage period prepared by this method can reach 6 months, be adapted to scientific research and industry is raw
Production.Send elsewhere bright the problem of improve graphene and CNT bad dispersibility, composite material interface performance is greatly improved.Will
The present invention prepare laminate applied to commercialized 977-2/HTS prepregs, obtain composite laminated plate interlaminar shear strength,
Bending strength, bending modulus compare raising more than 20% with the type fracture toughness of laminate I compared with only with one layer of composite film material.
The inventive method is simple, and cost of material is low, and the carbon fibre composite toughness of preparation is significantly increased, with good
Good market prospects.
Embodiment：
By following examples, the present invention is described in detail.Reagent in non-specified otherwise, embodiment is analysis
It is pure, wherein：
The graphene of surface grafting ethylenediamine, the CNT of surface grafting diethyl toluene diamine are by Nanjing Xian Feng nanometers
Material Science and Technology Ltd. buys；
Halloysite nanotubes are bought by Qingdao Yuan Xin nanosecond science and technology Co., Ltd.
Carbon fiber prepreg is provided by Cytec companies of the U.S., trade mark 977-2/HTS.
Embodiment 1
A kind of Activated Graphite alkene halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is by graphite
Alkene, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) will purchase halloysite nanotubes 10g and concentration 1mol/L hydrochloric acid 300ml reaction 24h, standing 1 day.Outwell supernatant
Liquid, distilled water centrifugal treating is dried to PH=6.0, and under conditions of 60 DEG C, and grinding obtains powder I.
B) in powder I add 300ml 1mol/L sodium chloride solutions, stir 48h, then with distilled water centrifugal treating until
Not chloride ion-containing (being examined with silver nitrate), dries under the conditions of 105 DEG C, grinding obtains powder II.
C) 5g powder II is taken to add 250ml, 12h is stirred in 0.014mol/L cetyl trimethylammonium bromides, 60 DEG C of oil baths,
Ethanol is centrifuged, 90 DEG C of drying, grinding, obtains the halloysite nanotubes of modified grafting long-chain polymer.
D) amination graphene 1g is taken, and is mixed with 8g benzyl glycidyl ethers, mechanical agitation 3h obtains mixed liquor I.
E) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 1h, rotational speed of ball-mill is 300r/min, is obtained
To mixed liquor II.
F) oil bath 1h under conditions of mixed liquor II being placed in into 150 DEG C, subsequent normal temperature stands 24h, obtains Activated Graphite alkene and mixes
Close liquid.
G) take the halloysite nanotubes of the modified grafting long-chain polymers of 1g to add in Activated Graphite alkene mixed liquor, obtain
Mixed liquor III.Mixed liquor III is heated to 90 DEG C, and the mechanical agitation under conditions of 90 DEG C after being thoroughly mixed, mixed liquor is obtained
Ⅳ。
H) mixed liquor IV is placed in ultrasonically treated 2h under 60W ultrasonic powers, normal temperature stands 4h, obtained Activated Graphite afterwards
Alkene halloysite nanotubes mixed liquor.
I) Activated Graphite alkene halloysite nanotubes mixed liquor is subjected to film on tetrafluoroethene flat board, coating thickness is 80
μm, normal temperature is stood, and obtains graphene halloysite nanotubes laminated film.
A kind of CNT/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is received by carbon
Mitron, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) aminated carbon nano tube 1g is taken, and is mixed with 8g benzyl glycidyl ethers, mechanical agitation 2h obtains mixed liquor I.
B) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 4h, rotational speed of ball-mill is 300r/min, is obtained
To mixed liquor II.
C) oil bath 1h under conditions of mixed liquor II being placed in into 150 DEG C, subsequent normal temperature stands 24h, obtains Activated Carbon Nanotubes
Mixed liquor.
D) take the halloysite nanotubes finished product of the modified grafting long-chain polymers of 1g to be added to 9g Activated Carbon Nanotubes to mix
Close in liquid, be sufficiently mixed, and mixed liquor is heated to 90 DEG C, the mechanical agitation under conditions of 90 DEG C obtains mixed liquor III.
E) mixed liquor III is placed in ultrasonically treated 3h under 60W ultrasonic powers, normal temperature stands 4h afterwards, obtained activated carbon is received
Mitron/halloysite nanotubes mixed liquor.
F) Activated Carbon Nanotubes/halloysite nanotubes mixed liquor is subjected to film, coating thickness on tetrafluoroethene flat board
For 80 μm, normal temperature is stood, and obtains graphene carbon nanotube composite film.
A kind of high-modulus high tenacity high polymer material, using die pressing by 16 layers of 0.13mm carbon fiber prepreg film, 1
Layer Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film are pressed into
Thickness is 2mm unidirectional composite material laminate, wherein, ply stacking-sequence is from top to bottom：8 layers of carbon fiber prepreg, 1 layer of activity
Graphene/halloysite nanotubes laminated film, 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film is finally 8 layers of carbon
Fiber prepreg material.Above-mentioned prepreg is placed in mould after the completion of laying, it is former according to carbon fiber prepreg using compression molding instrument
Some curing process carry out curing molding, and the carbon fiber for obtaining graphene/carbon nano-tube/halloysite nanotubes coordination plasticizing is combined
Material.
Comparative example 1：A kind of carbon fiber prepreg material, using die pressing by 16 layers of 0.13mm carbon fiber prepreg and 1
Layer Activated Graphite alkene halloysite nanotubes laminated film is pressed into the unidirectional composite material laminate that thickness is 2mm, wherein, laying
Sequentially it is from top to bottom：8 layers of carbon fiber prepreg film, 1 layer of Activated Graphite alkene halloysite nanotubes laminated film, is finally 8
Layer carbon fiber prepreg film.Above-mentioned prepreg is placed in mould after the completion of laying, using compression molding instrument according to carbon fiber
The original curing process of prepreg carries out curing molding, obtains carbon fibre composite I.
Comparative example 2：A kind of carbon fiber prepreg material, using die pressing by 16 layers of 0.13mm carbon fiber prepreg and 1
Layer Activated Carbon Nanotubes/halloysite nanotubes laminated film is pressed into the unidirectional composite material laminate that thickness is 2mm, wherein,
Ply stacking-sequence is from top to bottom：8 layers of carbon fiber prepreg, 1 layer of active stone CNT/halloysite nanotubes laminated film, most
It is afterwards 8 layers of carbon fiber prepreg film.Above-mentioned prepreg is placed in mould after the completion of laying, using compression molding instrument according to carbon
The original curing process of fiber prepreg material carries out curing molding, obtains carbon fibre composite II.
Embodiment 2
A kind of Activated Graphite alkene/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is by stone
Black alkene, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
K) will purchase halloysite nanotubes 10g and concentration 1mol/L hydrochloric acid 300ml reaction 24h, standing 1 day.Outwell supernatant
Liquid, distilled water centrifugal treating is dried to PH=6.0, and under conditions of 60 DEG C, and grinding obtains powder I.
L) in powder I add 300ml 1mol/L sodium chloride solutions, stir 48h, then with distilled water centrifugal treating until
Not chloride ion-containing (being examined with silver nitrate), dries under the conditions of 105 DEG C, grinding obtains powder II.
M) 5g powder II is taken to add 250ml, 12h is stirred in 0.014mol/L cetyl trimethylammonium bromides, 60 DEG C of oil baths,
Ethanol is centrifuged, 90 DEG C of drying, grinding, obtains the halloysite nanotubes of modified grafting long-chain polymer.
N) amination graphene 1.5g is taken, and is mixed with 7g benzyl glycidyl ethers, mechanical agitation 2h obtains mixed liquor I.
O) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 0.5h, rotational speed of ball-mill is 200r/min,
Obtain mixed liquor II.
P) oil bath 1h under conditions of mixed liquor II being placed in into 150 DEG C, subsequent normal temperature stands 5h, obtains the mixing of Activated Graphite alkene
Liquid.
Q) take the halloysite nanotubes of the modified grafting long-chain polymers of 1.5g to add above-mentioned 8.5g Activated Graphites alkene to mix
Close in liquid, obtain mixed liquor III.Mixed liquor III is heated to 90 DEG C, and the mechanical agitation under conditions of 90 DEG C after being thoroughly mixed,
Obtain mixed liquor IV.
R) mixed liquor IV is placed in ultrasonically treated 2h under 60W ultrasonic powers, normal temperature stands 4h, obtained Activated Graphite afterwards
Alkene halloysite nanotubes mixed liquor.
S) by Activated Graphite alkene halloysite nanotubes mixed liquor film applicator film, coating thickness is 50 μm, and normal temperature is stood,
Obtain graphene/halloysite nanotubes laminated film.
A kind of CNT/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is received by carbon
Mitron, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
G) aminated carbon nano tube 1.5g is taken, and is mixed with 7g benzyl glycidyl ethers, mechanical agitation 2h obtains mixed liquor
Ⅰ。
H) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 0.5h, rotational speed of ball-mill is 200r/min,
Obtain mixed liquor II.
I) oil bath 1h under conditions of mixed liquor II being placed in into 150 DEG C, subsequent normal temperature stands 5h, obtains Activated Carbon Nanotubes and mixes
Close liquid.
J) the halloysite nanotubes finished product of the modified grafting long-chain polymers of 1.5g is taken to be added to 8.5g activated carbon nanometer
In pipe mixed liquor, it is sufficiently mixed, and mixed liquor is heated to 90 DEG C, the mechanical agitation under conditions of 90 DEG C obtains mixed liquor III.
K) mixed liquor III is placed in ultrasonically treated 2h under 60W ultrasonic powers, normal temperature stands 1h afterwards, obtained activated carbon is received
Mitron/halloysite nanotubes mixed liquor.
L) by Activated Carbon Nanotubes/halloysite nanotubes mixed liquor film applicator film, coating thickness is 50 μm, and normal temperature is quiet
Put, obtain CNT/halloysite nanotubes laminated film.
A kind of high-modulus high tenacity high polymer material, using die pressing by 16 layers of 0.15mm carbon fiber prepreg, 1 layer of work
Property graphene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film are pressed into thickness
For 2.4mm unidirectional composite material laminate, wherein, ply stacking-sequence is from top to bottom：8 layers of carbon fiber prepreg, 1 layer of active stone
Black alkene/halloysite nanotubes laminated film, 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film is finally 8 layers of carbon fibre
Tie up prepreg.Above-mentioned prepreg is placed in mould after the completion of laying, it is original according to carbon fiber prepreg using compression molding instrument
Curing process carry out curing molding, obtain graphene/halloysite nanotubes and CNT/halloysite nanotubes coordination plasticizing
Carbon fibre composite.
Embodiment 3
A kind of Activated Graphite alkene/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is by stone
Black alkene, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) will purchase halloysite nanotubes 10g and concentration 1mol/L hydrochloric acid 300ml reaction 24h, standing 1 day.Outwell supernatant
Liquid, distilled water centrifugal treating is dried to PH=6.0, and under conditions of 60 DEG C, and grinding obtains powder I.
B) in powder I add 300ml 1mol/L sodium chloride solutions, stir 48h, then with distilled water centrifugal treating until
Not chloride ion-containing (being examined with silver nitrate), dries under the conditions of 105 DEG C, grinding obtains powder II.
C) 5g powder II is taken to add 250ml, 12h is stirred in 0.014mol/L cetyl trimethylammonium bromides, 60 DEG C of oil baths,
Ethanol is centrifuged, 90 DEG C of drying, grinding, obtains the halloysite nanotubes of modified grafting long-chain polymer.
D) amination graphene 1.25g is taken, and is mixed with 7.5g benzyl glycidyl ethers, mechanical agitation 2.5h is mixed
Close liquid I.
E) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 2h, rotational speed of ball-mill is 280r/min, is obtained
To mixed liquor II.
F) oil bath 1h under conditions of mixed liquor II being placed in into 155 DEG C, subsequent normal temperature stands 10h, obtains Activated Graphite alkene and mixes
Close liquid.
G) halloysite nanotubes of the modified grafting long-chain polymers of 1.25g are taken to add in Activated Graphite alkene mixed liquor,
Obtain mixed liquor III.Mixed liquor III is heated to 95 DEG C, and the mechanical agitation under conditions of 95 DEG C after being thoroughly mixed, mixed
Liquid IV.
H) mixed liquor IV is placed in ultrasonically treated 2h under 60W ultrasonic powers, normal temperature stands 4h, obtained Activated Graphite afterwards
Alkene/halloysite nanotubes mixed liquor.
I) Activated Graphite alkene halloysite nanotubes mixed liquor is used into glass bar coating method film, coating thickness is 60 μm,
Normal temperature is stood, and obtains graphene/halloysite nanotubes laminated film.
A kind of CNT/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is received by carbon
Mitron, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) aminated carbon nano tube 1.25g is taken, and is mixed with 7.5g benzyl glycidyl ethers, mechanical agitation 2.5h is obtained
Mixed liquor I.
B) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 2h, rotational speed of ball-mill is 280r/min, is obtained
To mixed liquor II.
C) oil bath 1h under conditions of mixed liquor II being placed in into 155 DEG C, subsequent normal temperature stands 10h, obtains Activated Carbon Nanotubes
Mixed liquor.
D) take the halloysite nanotubes finished product of the modified grafting long-chain polymers of 1.25g to be added to Activated Carbon Nanotubes to mix
Close in liquid, be sufficiently mixed, and mixed liquor is heated to 95 DEG C, the mechanical agitation under conditions of 95 DEG C obtains mixed liquor III.
E) mixed liquor III is placed in ultrasonically treated 2.5h under 60W ultrasonic powers, normal temperature stands 2h, obtained activated carbon afterwards
Nanotube/halloysite nanotubes mixed liquor.
F) Activated Carbon Nanotubes/halloysite nanotubes mixed liquor is used into glass bar coating method film, coating thickness is 60 μ
M, normal temperature is stood, and obtains graphene carbon nanotube composite film.
A kind of high-modulus high tenacity high polymer material, using die pressing by 20 layers of 0.15mm carbon fiber prepreg film, 1
Layer Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film are pressed into
Thickness is 3.0mm unidirectional composite material laminate, wherein, ply stacking-sequence is from top to bottom：10 layers of carbon fiber prepreg, 1 layer
Activated Graphite alkene/halloysite nanotubes laminated film, 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film, is finally 10
Layer carbon fiber prepreg.Above-mentioned prepreg is placed in mould after the completion of laying, using compression molding instrument according to carbon fibre initial rinse
Expect that original curing process carries out curing molding, obtain graphene/halloysite nanotubes and CNT/halloysite nanotubes association
With the carbon fibre composite of toughness reinforcing.
Embodiment 4
A kind of Activated Graphite alkene/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is by stone
Black alkene, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) will purchase halloysite nanotubes 10g and concentration 1mol/L hydrochloric acid 300ml reaction 24h, standing 1 day.Outwell supernatant
Liquid, distilled water centrifugal treating is dried to PH=6.0, and under conditions of 60 DEG C, and grinding obtains powder I.
B) in powder I add 300ml 1mol/L sodium chloride solutions, stir 48h, then with distilled water centrifugal treating until
Not chloride ion-containing (being examined with silver nitrate), dries under the conditions of 105 DEG C, grinding obtains powder II.
C) 5g powder II is taken to add 250ml, 12h is stirred in 0.014mol/L cetyl trimethylammonium bromides, 60 DEG C of oil baths,
Ethanol is centrifuged, 90 DEG C of drying, grinding, obtains the halloysite nanotubes of modified grafting long-chain polymer.
D) amination graphene 1g is taken, and is mixed with 7.5g benzyl glycidyl ethers, mechanical agitation 2h obtains mixed liquor I.
E) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 3h, rotational speed of ball-mill is 240r/min, is obtained
To mixed liquor II.
F) oil bath 1h under conditions of mixed liquor II being placed in into 145 DEG C, subsequent normal temperature stands 20h, obtains Activated Graphite alkene and mixes
Close liquid.
G) take the halloysite nanotubes of the modified grafting long-chain polymers of 1.5g to add in Activated Graphite alkene mixed liquor, obtain
To mixed liquor III.Mixed liquor III is heated to 85 DEG C, and the mechanical agitation under conditions of 85 DEG C after being thoroughly mixed, mixed liquor is obtained
Ⅳ。
H) mixed liquor IV is placed in ultrasonically treated 2h under 60W ultrasonic powers, normal temperature stands 4h, obtained Activated Graphite afterwards
Alkene/halloysite nanotubes mixed liquor.
I) by Activated Graphite alkene halloysite nanotubes mixed liquor rejection film machine film, coating thickness is 70 μm, and normal temperature is stood,
Obtain graphene/halloysite nanotubes laminated film.
A kind of CNT/halloysite nanotubes composite membrane for prepreg interlayer toughened, the composite membrane is received by carbon
Mitron, halloysite nanotubes are composited as steps described below, and specific preparation method is as follows：
A) aminated carbon nano tube 1g is taken, and is mixed with 7.5g benzyl glycidyl ethers, mechanical agitation 2h obtains mixed liquor
Ⅰ。
B) mixed liquor I is added in planetary ball mill, under nitrogen protection ball milling 3h, rotational speed of ball-mill is 240r/min, is obtained
To mixed liquor II.
C) oil bath 1h under conditions of mixed liquor II being placed in into 145 DEG C, subsequent normal temperature stands 20h, obtains Activated Carbon Nanotubes
Mixed liquor.
D) the halloysite nanotubes finished product of the modified grafting long-chain polymers of 1.5g is taken to be added to 8.5g activated carbon nanometer
In pipe mixed liquor, it is sufficiently mixed, and mixed liquor is heated to 85 DEG C, the mechanical agitation under conditions of 85 DEG C obtains mixed liquor III.
E) mixed liquor III is placed in ultrasonically treated 3h under 60W ultrasonic powers, normal temperature stands 2h afterwards, obtained activated carbon is received
Mitron/halloysite nanotubes mixed liquor.
F) by Activated Carbon Nanotubes/halloysite nanotubes mixed liquor rejection film machine film, coating thickness is 70 μm, and normal temperature is quiet
Put, obtain CNT/halloysite nanotubes laminated film.
A kind of high-modulus high tenacity high polymer material, using die pressing by 18 layers of 0.15mm carbon fiber prepreg film, 1
Layer Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film are pressed into
Thickness is 2.7mm unidirectional composite material laminate, wherein, ply stacking-sequence is from top to bottom：9 layers of carbon fiber prepreg, 1 layer of work
Property graphene/halloysite nanotubes laminated film, 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film is finally 9 layers
Carbon fiber prepreg.Above-mentioned prepreg is placed in mould after the completion of laying, using compression molding instrument according to carbon fiber prepreg
Original curing process carries out curing molding, and the carbon fiber for obtaining graphene/carbon nano-tube/halloysite nanotubes coordination plasticizing is answered
Condensation material.
Applicant detected to the performance indications of composite, wherein, the Interlaminar shear strengths of composite
(ILSS) tested according to JC/T 773-2010, bending property is tested according to GB/T 1446-1983, layer
Mode Ⅱ fracture toughness (the G of plywood IⅠc) tested according to ASTM D 5528.
The graphene that embodiment 1~4 is prepared/halloysite nanotubes film and CNT/halloysite nanotubes film association
With the mechanical property such as following table of toughening carbon fiber reinforced composite：
The mechanical property for the carbon fibre composite that comparative example 1~2 is prepared such as following table：
Claims (7)
1. the carbon fibre composite of a kind of nanometer of toughness reinforcing, it is characterised in that：The carbon fibre composite is pre- by 16~20 layers
Leaching material, 1 layer of Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of Activated Carbon Nanotubes/halloysite nanotubes laminated film
Molded curing is molded with；
Wherein, the Activated Graphite alkene/halloysite nanotubes laminated film is by 10~15% amination graphenes, 70~80%
The halloysite nanotubes of benzyl glycidyl ether and 10~15% modified grafting long-chain polymers are made；The activated carbon is received
Mitron/halloysite nanotubes laminated film by 10~15% CNT and 70~80% benzyl glycidyl ether and 10~
The halloysite nanotubes of 15% modified grafting long-chain polymer are made.
2. carbon fibre composite according to claim 1, it is characterised in that：The thickness of the carbon fibre composite
For：2~3mm, the Activated Graphite alkene/halloysite nanotubes laminated film thickness is 50~80 μm, Activated Carbon Nanotubes/Ai Luo
The thickness of stone nanotube composite film is 50~80 μm.
3. carbon fibre composite according to claim 1, it is characterised in that：The laying of the carbon fibre composite is suitable
Sequence is respectively from top to bottom：8~10 layers of prepreg, 1 layer of Activated Graphite alkene/halloysite nanotubes laminated film and 1 layer of activated carbon
Nanotube/halloysite nanotubes laminated film and 8~10 layers of prepreg.
4. a kind of preparation method of carbon fibre composite, it is characterised in that：The carbon fibre composite is using molding legal system
It is standby, it is specifically by 0.09~0.17mm carbon fiber prepreg, 50~80 μm of Activated Graphite alkene/halloysite nanotubes laminated films
It is placed in after 50~80 μm of Activated Carbon Nanotubes/halloysite nanotubes laminated film laying in compression molding instrument, according to carbon fiber
The curing process of prepreg carries out curing molding, is finally pressed into the unidirectional composite material laminate that thickness is 2~3mm；
Wherein, the preparation method of the Activated Graphite alkene/halloysite nanotubes laminated film comprises the following steps：
A) halloysite nanotubes are added in hydrochloric acid solution, remove a layer turbid solution, plus distilled water centrifugal treating, taking precipitate dries
Dry, grinding obtains powder I；
B) sodium chloride solution is added in powder I, stirred, distilled water centrifugal treating, dried under the conditions of 105 DEG C, grinding obtains powder
End II；
C) cetyl trimethylammonium bromide is added in powder II, 60 DEG C of oil bath stirrings, ethanol centrifugation, 90 DEG C of drying are ground,
Obtain the halloysite nanotubes of modified grafting long-chain polymer；
D) amination graphene is mixed in benzyl glycidyl ether, mechanical agitation obtains mixed liquor I；
E) mixed liquor I is added in ball mill, under nitrogen protection ball milling, obtains mixed liquor II；
F) oil bath under conditions of mixed liquor II being placed in into 150 ± 5 DEG C, then normal temperature standing, obtains Activated Graphite alkene mixed liquor；
G) halloysite nanotubes of modified grafting long-chain polymer are added in Activated Graphite alkene mixed liquor, mixed liquor is obtained
Ⅲ；
H) mixed liquor III is heated to 90 ± 5 DEG C, and the mechanical agitation under conditions of 90 ± 5 DEG C after being thoroughly mixed, mixed
Liquid IV；
I) by mixed liquor IV under 60W ultrasonic powers ultrasonically treated, the Activated Graphite alkene/galapectite nanometer that normal temperature is obtained after standing
Pipe mixed liquor；
J) by Activated Graphite alkene/halloysite nanotubes mixed liquor film, then normal temperature is stood, and obtains graphene/galapectite nanometer
Pipe laminated film.
5. the preparation method of carbon fibre composite according to claim 4, it is characterised in that：The activated carbon nanometer
The preparation method of pipe/halloysite nanotubes laminated film comprises the following steps：
A) aminated carbon nano tube is added in benzyl glycidyl ether, stirs, obtain mixed liquor 1.；
B) 1. mixed liquor is added in ball mill, under nitrogen protection ball milling, obtains mixed liquor 2.；
C) by the mixed liquor 2. oil bath under conditions of 150 ± 5 DEG C, then normal temperature is stood, and obtains Activated Carbon Nanotubes mixed liquor；
D) the halloysite nanotubes finished product of modified grafting long-chain polymer is added in Activated Carbon Nanotubes mixed liquor, and added
Heat is to 90 ± 5 DEG C, and 3. the mechanical agitation under conditions of 90 ± 5 DEG C obtains mixed liquor；
E) 3. mixed liquor is placed in it is ultrasonically treated under 60W ultrasonic powers, then normal temperature stand, obtained Activated Carbon Nanotubes/angstrom
Lip river stone nanotube mixed liquor；
F) by Activated Carbon Nanotubes/halloysite nanotubes mixed liquor film, then normal temperature is stood, and obtains CNT/galapectite
Nanotube composite film.
6. a kind of preparation method of carbon fibre composite according to claim 4 or 5, it is characterised in that the ball milling
Condition be：Interval 5min, 0.5~4h of Ball-milling Time are needed after 200~500r/min of rotational speed of ball-mill, continuous ball milling 10min.
7. a kind of preparation method of carbon fibre composite according to claim 4 or 5, it is characterised in that the film
Method include：Glass bar film is used, with rejection film machine film, film applicator film is used.
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