CN104988736A - Method for improving interface toughness of epoxy resin based carbon fiber composite material - Google Patents
Method for improving interface toughness of epoxy resin based carbon fiber composite material Download PDFInfo
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- CN104988736A CN104988736A CN201510346866.2A CN201510346866A CN104988736A CN 104988736 A CN104988736 A CN 104988736A CN 201510346866 A CN201510346866 A CN 201510346866A CN 104988736 A CN104988736 A CN 104988736A
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Abstract
The invention discloses a method for improving the interface toughness of an epoxy resin based carbon fiber composite material and belongs to the technical field of modification of the epoxy resin based carbon fiber composite material. The method comprises the following steps of 1 dissolving hydroxyl-terminated nitrile rubber in an organic solvent to obtain a hydroxyl-terminated nitrile rubber solution, 2 enabling a carbon fiber fabric to be in contact with the hydroxyl-terminated nitrile rubber solution and performing drying to obtain a woven carbon fiber fabric modified by the hydroxyl-terminated nitrile rubber, 3 using an epoxy resin and curing agent mixed solution to soak the woven carbon fiber fabric modified by the hydroxyl-terminated nitrile rubber and performing curing to obtain the epoxy resin based carbon fiber composite material. The hydroxyl-terminated nitrile rubber is added at the interface position of carbon fiber and epoxy resin so that the interface toughness of the epoxy resin based carbon fiber composite material can be effectively improved on the premise that shear strength is not lost.
Description
Technical field
The present invention relates to epoxy resin base carbon fiber composite material technical field of modification, particularly a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness.
Background technology
Epoxy resin base carbon fiber composite material with its high specific strength, high ratio modulus, high temperature resistant, numerous excellent properties such as corrosion-resistant and being widely used on space flight, automobile, electronics, sports goods and medicine equipment.The performance of epoxy resin/carbon fibre composite is by fiber bodies, and resin matrix and bond strength therebetween determine.But because the thermal coefficient of expansion of epoxy resin and carbon fiber has larger gap, this makes the epoxy resin/carbon fibre composite after solidifying there is larger interface thermal residual strain.In addition, composite material interface also also exists the contraction-remainder stress of resin matrix solidification.Above-mentioned residual stress can make the interfacial toughness of composite reduce.When composite due to Local Property not good and crack time, the existence of interfacial stress can make micro-crack spread rapidly, when the strength of materials be not enough to opposing interfacial stress time, material will destroy.
Current reduction interfacial stress, the method improving composite material interface toughness mainly realize by introducing dilatancy monomer.Volume obvious increase compared with monomer of dilatancy monomer polymerization products therefrom, therefore, it is possible to offset the volume contraction in Curing Process of Epoxy to a certain extent, reduce interfacial stress, improve the impact flexibility of composite, thus improve the interfacial toughness of composite.
Realizing in process of the present invention, the present inventor finds at least there is following problem in prior art: the method for existing raising epoxy resin base carbon fiber composite material interfacial toughness can cause the shear strength of composite to reduce.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of method of the raising epoxy resin base carbon fiber composite material interfacial toughness that shear strength can not be caused to reduce.
Specifically, following technical scheme is comprised:
The invention provides a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness, said method comprising the steps of:
Step 1, is dissolved in hydroxy'terminated butadiene nitrile rubber in organic solvent, obtains hydroxy'terminated butadiene nitrile rubber solution;
Step 2, contacts carbon fibre fabric cloth with described hydroxy'terminated butadiene nitrile rubber solution, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification after drying;
Step 3, infiltrates with the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of epoxy resin and curing agent, namely obtains epoxy resin base carbon fiber composite material after solidification.
Preferably, in step 1,2000 ~ 5000 of described hydroxy'terminated butadiene nitrile rubber.
Preferably, in step 1, the mass ratio of described hydroxy'terminated butadiene nitrile rubber and described organic solvent is 5 ~ 15:100.
Preferably, in step 1, described organic solvent is selected from least one in butanone, cyclohexane and dimethylbenzene.
Preferably, in step 2, the mode that described carbon fibre fabric cloth contacts with described hydroxy'terminated butadiene nitrile rubber solution is: described hydroxy'terminated butadiene nitrile rubber solution is placed in solution tank, more described carbon fiber woven cloth is passed through described solution tank with the speed of 0.05 ~ 0.2m/s.
Preferably, in step 3, the preparation method of the mixed solution of described epoxy resin and curing agent is: epoxy resin and curing agent are mixed according to the ratio of mass ratio 100:20 ~ 30, then to add acetone by mixture diluted to the viscosity of epoxy resin and curing agent be 400 ~ 650mPaS.
Preferably, the bisphenol f type epoxy resin of described epoxy resin to be viscosity be 2500 ~ 4000mPaS.
Preferably, described curing agent is diethylenetriamine, at least one in triethylene tetramine and m-xylene diamine.
Preferably, in step 3, the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of vacuum bag pressure method epoxy resin and curing agent is adopted to infiltrate.
Preferably, in step 3, a solidification point three phases carries out, and is followed successively by: 80 DEG C of heating, 1 hour, 120 DEG C heating are heated 2 hours for 2 hours and 150 DEG C.
The beneficial effect of the technical scheme that the embodiment of the present invention provides:
The method of the raising epoxy resin base carbon fiber composite material interfacial toughness that the embodiment of the present invention provides is by adding hydroxy'terminated butadiene nitrile rubber at carbon fiber and epoxy resin interface place, under the prerequisite of not losing shear strength, epoxy resin base carbon fiber composite material interfacial toughness is made to improve 38% ~ 50%.Hydroxy'terminated butadiene nitrile rubber has good toughness, and when interface is subject to external load and produces micro-crack, hydroxy'terminated butadiene nitrile rubber can hinder the expansion of crackle; When interfacial failure, hydroxy'terminated butadiene nitrile rubber also can absorb energy, and the toughness at epoxy resin base carbon fiber composite material interface is improved.Simultaneously, hydroxyl in hydroxy'terminated butadiene nitrile rubber molecule can react with the group of epoxy resin and carbon fiber surface, hydroxy'terminated butadiene nitrile rubber molecule also can be cross-linked itself, form cross-linking system thus epoxy resin is combined with carbon fiber more firmly, not affecting the shear strength of epoxy resin base carbon fiber composite material.
Detailed description of the invention
For making technical scheme of the present invention and advantage clearly, below embodiment of the present invention is described further in detail.
The invention provides a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness, said method comprising the steps of:
Step 1, is dissolved in hydroxy'terminated butadiene nitrile rubber in organic solvent, obtains hydroxy'terminated butadiene nitrile rubber solution;
Step 2, contacts carbon fibre fabric cloth with described hydroxy'terminated butadiene nitrile rubber solution, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification after drying;
Step 3, infiltrates with the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of epoxy resin and curing agent, namely obtains epoxy resin base carbon fiber composite material after solidification.
Hydroxy'terminated butadiene nitrile rubber is the acrylonitrile-butadiene rubbers of strand two ends with hydroxyl.Hydroxy'terminated butadiene nitrile rubber has good toughness, and after being added to epoxy resin and carbon fiber interface, when interface is subject to external load and produces micro-crack, hydroxy'terminated butadiene nitrile rubber can hinder the expansion of crackle; When interfacial failure, hydroxy'terminated butadiene nitrile rubber also can absorb energy, and the toughness at epoxy resin base carbon fiber composite material interface is improved.Simultaneously, hydroxyl in hydroxy'terminated butadiene nitrile rubber molecule can react with the group of epoxy resin and carbon fiber surface, hydroxy'terminated butadiene nitrile rubber molecule also can be cross-linked itself, form cross-linking system thus epoxy resin is combined with carbon fiber more firmly, not affecting the shear strength of epoxy resin base carbon fiber composite material.Therefore, the method by adding hydroxy'terminated butadiene nitrile rubber at carbon fiber and epoxy resin interface place that the embodiment of the present invention provides, can, under the prerequisite of not losing shear strength, make epoxy resin base carbon fiber composite material interfacial toughness improve 38% ~ 50%.
In the methods described above, the number-average molecular weight of described hydroxy'terminated butadiene nitrile rubber is preferably 2000 ~ 5000, such as, can be 2500,3000,3500,4000,4500 etc.
In the methods described above, in step 1, the mass ratio of described hydroxy'terminated butadiene nitrile rubber and described organic solvent is preferably 5 ~ 15:100, such as, can be 6:100,8:100,10:100,12:100 etc.If the mass ratio of described hydroxy'terminated butadiene nitrile rubber and organic solvent is too small, namely hydroxy'terminated butadiene nitrile rubber solution concentration is too low, the content of hydroxy'terminated butadiene nitrile rubber in the epoxy resin base carbon fiber composite material finally obtained then can be made less, affect the performance of epoxy resin base carbon fiber composite material; If the mass ratio of described hydroxy'terminated butadiene nitrile rubber and organic solvent is excessive, hydroxy'terminated butadiene nitrile rubber solution viscosity can be made excessive, cause hydroxy'terminated butadiene nitrile rubber skewness in gained epoxy resin base carbon fiber composite material, also can affect the performance of epoxy resin base carbon fiber composite material.
In the methods described above, in step 1, organic solvent for dissolving hydroxy'terminated butadiene nitrile rubber does not strictly limit, hydroxy'terminated butadiene nitrile rubber can be made to dissolve, can be such as butanone, cyclohexane or diformazan, can be used alone a kind of organic solvent, also can multiple organic solvent used in combination.In order to make hydroxy'terminated butadiene nitrile rubber be dissolved in better in organic solvent, can at 60 ~ 80 DEG C stirring and dissolving.
In the methods described above, in step 2, the mode that described carbon fibre fabric cloth is contacted with described hydroxy'terminated butadiene nitrile rubber solution does not have considered critical, as long as hydroxy'terminated butadiene nitrile rubber can be made to be evenly distributed on carbon fiber woven cloth.Such as can adopt the method for immersion, also can adopt and hydroxy'terminated butadiene nitrile rubber solution is placed in solution tank, then by described carbon fiber woven cloth with the method for the speed of 0.05 ~ 0.2m/s by described solution tank.
In the methods described above, in step 3, the preparation method of the mixed solution of epoxy resin and curing agent is also not particularly limited, this area routine techniques means.Such as: epoxy resin and curing agent are mixed according to the ratio of mass ratio 100:20 ~ 30, then to add acetone by mixture diluted to the viscosity of epoxy resin and curing agent be 400 ~ 650mPaS.Wherein, the viscosity of the mixed solution of epoxy resin and curing agent can be 450mPaS, 500mPaS or 650mPaS etc.The ratio of the epoxy resin after the acetone added accounts for dilution and the mixed solution of curing agent is preferably 15 ~ 30wt%.
In the methods described above, epoxy resin used can be bisphenol A type epoxy resin, bisphenol f type epoxy resin or bisphenol-s epoxy resin, but preferred bisphenol f type epoxy resin.The viscosity preferably 2500 ~ 4000mPaS of epoxy resin such as, can be 3000mPaS, 3500mPaS etc.
In the methods described above, described curing agent can be the arbitrary epoxy curing agent that this area is commonly used, such as diethylenetriamine, triethylene tetramine and m-xylene diamine etc.Can be used alone a kind of curing agent, also can the composite use of multiple curing agent.
In the methods described above, in step 3, do not have particular/special requirement by the method that the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of epoxy resin and curing agent infiltrates, this area common technology means, such as, can adopt vacuum bag pressure method.
In the methods described above, in step 3, the curing process of epoxy resin does not have particular/special requirement yet, this area common technology means.Such as, three phases can be divided to carry out, be followed successively by: 80 DEG C of heating, 1 hour, 120 DEG C heating 2 hours and 150 DEG C of heating, 2 hours (i.e. 80/1h+120/2h+150/2h).
In the methods described above, in gained epoxy resin base carbon fiber composite material, the percent by volume of carbon fiber can be 50 ~ 58%.
Following examples 1 ~ 3 adopt the method for raising epoxy resin base carbon fiber composite material interfacial toughness provided by the invention to prepare epoxy resin base carbon fiber composite material.To the interfacial toughness of gained epoxy resin base carbon fiber composite material, and compare with the epoxy resin base carbon fiber composite material not adding hydroxy'terminated butadiene nitrile rubber.Wherein, the interfacial toughness interlaminar shear strength of epoxy resin base carbon fiber composite material characterizes, and interlaminar shear strength test is carried out according to the method for " JC/T 773-2010 fibre reinforced plastics short beam method measures interlaminar shear strength ".
Embodiment 1
The present embodiment provides a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness, and the method comprises the following steps:
Number-average molecular weight is that the hydroxy'terminated butadiene nitrile rubber of 2500 mixes with the ratio of dimethylbenzene according to mass ratio 5:100 by step 1, is then stirred to dissolve completely at 60 DEG C to obtain hydroxy'terminated butadiene nitrile rubber solution;
Step 2, is placed in solution tank by above-mentioned hydroxy'terminated butadiene nitrile rubber solution, then is passed through in solution tank with the speed of 0.1m/s by carbon fiber woven cloth, and then drying at room temperature 10min, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification;
Step 3, be the bisphenol F epoxy resin of 3500mPaS and the m-xylene diamine ratio mixing and stirring according to mass ratio 100:20 by viscosity, then the acetone adding 15wt% fully dilutes, obtaining viscosity is the epoxy resin of 520mPaS and the mixed solution of curing agent; Adopt the carbon fiber woven cloth of the hydroxy'terminated butadiene nitrile rubber modification to step 2 gained of the mixed solution of the above-mentioned epoxy resin of vacuum bag pressure method and curing agent to infiltrate, be then cured according to the curing process of 80/1h+120/2h+150/2h.The epoxy resin base carbon fiber composite material that carbon fiber content is 52% (percent by volume) is obtained after the demoulding, deburring, cutting, polishing.
The epoxy resin base carbon fiber composite material not adding hydroxy'terminated butadiene nitrile rubber according to preparation method's preparation of above epoxy resin base carbon fiber composite material contrasts reference as blank sample.
Test result shows, the interfacial toughness of the epoxy resin base carbon fiber composite material adopting the method for the raising epoxy resin base carbon fiber composite material interfacial toughness of the present embodiment to obtain improves 43% compared with blank sample.
Embodiment 2
The present embodiment provides a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness, and the method comprises the following steps:
Number-average molecular weight is that the hydroxy'terminated butadiene nitrile rubber of 2300 mixes with the ratio of butanone according to mass ratio 8.5:100 by step 1, is then stirred to dissolve completely at 75 DEG C to obtain hydroxy'terminated butadiene nitrile rubber solution;
Step 2, is placed in solution tank by above-mentioned hydroxy'terminated butadiene nitrile rubber solution, then is passed through in solution tank with the speed of 0.08m/s by carbon fiber woven cloth, and then drying at room temperature 10min, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification;
Step 3, be the bisphenol F epoxy resin of 2600mPaS and the diethylenetriamine ratio mixing and stirring according to mass ratio 100:26 by viscosity, then the acetone adding 16wt% fully dilutes, obtaining viscosity is the epoxy resin of 420mPaS and the mixed solution of curing agent; Adopt the carbon fiber woven cloth of the hydroxy'terminated butadiene nitrile rubber modification to step 2 gained of the mixed solution of the above-mentioned epoxy resin of vacuum bag pressure method and curing agent to infiltrate, be then cured according to the curing process of 80/1h+120/2h+150/2h.The epoxy resin base carbon fiber composite material that carbon fiber content is 51% (percent by volume) is obtained after the demoulding, deburring, cutting, polishing.
The epoxy resin base carbon fiber composite material not adding hydroxy'terminated butadiene nitrile rubber according to preparation method's preparation of above epoxy resin base carbon fiber composite material contrasts reference as blank sample.
Test result shows, the interfacial toughness of the epoxy resin base carbon fiber composite material adopting the method for the raising epoxy resin base carbon fiber composite material interfacial toughness of the present embodiment to obtain improves 49% compared with blank sample.
Embodiment 3
The present embodiment provides a kind of method improving epoxy resin base carbon fiber composite material interfacial toughness, and the method comprises the following steps:
Number-average molecular weight is that the hydroxy'terminated butadiene nitrile rubber of 3000 mixes with the ratio of cyclohexane according to mass ratio 11.3:100 by step 1, is then stirred to dissolve completely at 77 DEG C to obtain hydroxy'terminated butadiene nitrile rubber solution;
Step 2, is placed in solution tank by above-mentioned hydroxy'terminated butadiene nitrile rubber solution, then is passed through in solution tank with the speed of 0.2m/s by carbon fiber woven cloth, and then drying at room temperature 10min, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification;
Step 3, be the bisphenol F epoxy resin of 3200mPaS and the triethylene tetramine ratio mixing and stirring according to mass ratio 100:28 by viscosity, then the acetone adding 15wt% fully dilutes, obtaining viscosity is the epoxy resin of 560mPaS and the mixed solution of curing agent; Adopt the carbon fiber woven cloth of the hydroxy'terminated butadiene nitrile rubber modification to step 2 gained of the mixed solution of the above-mentioned epoxy resin of vacuum bag pressure method and curing agent to infiltrate, be then cured according to the curing process of 80/1h+120/2h+150/2h.The epoxy resin base carbon fiber composite material that carbon fiber content is 56% (percent by volume) is obtained after the demoulding, deburring, cutting, polishing.
The epoxy resin base carbon fiber composite material not adding hydroxy'terminated butadiene nitrile rubber according to preparation method's preparation of above epoxy resin base carbon fiber composite material contrasts reference as blank sample.
Test result shows, the interfacial toughness of the epoxy resin base carbon fiber composite material adopting the method for the raising epoxy resin base carbon fiber composite material interfacial toughness of the present embodiment to obtain improves 39% compared with blank sample.
To sum up, the embodiment of the present invention, by adding hydroxy'terminated butadiene nitrile rubber at carbon fiber and epoxy resin interface place, makes gained epoxy resin base carbon fiber composite material interfacial toughness improve 38% ~ 50%, and does not lose shear strength.
The above is only understand technical scheme of the present invention for the ease of those skilled in the art, not in order to limit the present invention.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. improve a method for epoxy resin base carbon fiber composite material interfacial toughness, it is characterized in that, said method comprising the steps of:
Step 1, is dissolved in hydroxy'terminated butadiene nitrile rubber in organic solvent, obtains hydroxy'terminated butadiene nitrile rubber solution;
Step 2, contacts carbon fibre fabric cloth with described hydroxy'terminated butadiene nitrile rubber solution, obtains the carbon fiber woven cloth of hydroxy'terminated butadiene nitrile rubber modification after drying;
Step 3, infiltrates with the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of epoxy resin and curing agent, namely obtains epoxy resin base carbon fiber composite material after solidification.
2. method according to claim 1, is characterized in that, in step 1, the number-average molecular weight of described hydroxy'terminated butadiene nitrile rubber is 2000 ~ 5000.
3. method according to claim 1, is characterized in that, in step 1, the mass ratio of described hydroxy'terminated butadiene nitrile rubber and described organic solvent is 5 ~ 15:100.
4. method according to claim 1, is characterized in that, in step 1, described organic solvent is selected from least one in butanone, cyclohexane and dimethylbenzene.
5. method according to claim 1, it is characterized in that, in step 2, the mode that described carbon fibre fabric cloth contacts with described hydroxy'terminated butadiene nitrile rubber solution is: described hydroxy'terminated butadiene nitrile rubber solution is placed in solution tank, more described carbon fiber woven cloth is passed through described solution tank with the speed of 0.05 ~ 0.2m/s.
6. method according to claim 1, it is characterized in that, in step 3, the preparation method of the mixed solution of described epoxy resin and curing agent is: epoxy resin and curing agent are mixed according to the ratio of mass ratio 100:20 ~ 30, then to add acetone by mixture diluted to the viscosity of epoxy resin and curing agent be 400 ~ 650mPaS.
7. method according to claim 6, is characterized in that, the bisphenol f type epoxy resin of described epoxy resin to be viscosity be 2500 ~ 4000mPaS.
8. method according to claim 6, is characterized in that, described curing agent is diethylenetriamine, at least one in triethylene tetramine and m-xylene diamine.
9. method according to claim 1, is characterized in that, in step 3, adopts the carbon fiber woven cloth of mixed solution to described hydroxy'terminated butadiene nitrile rubber modification of vacuum bag pressure method epoxy resin and curing agent to infiltrate.
10. method according to claim 9, is characterized in that, in step 3, a solidification point three phases carries out, and is followed successively by: 80 DEG C of heating, 1 hour, 120 DEG C heating are heated 2 hours for 2 hours and 150 DEG C.
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