CN100467527C - Carbon fiber reinforced bismalemide resin base composite material, and its preparing method - Google Patents
Carbon fiber reinforced bismalemide resin base composite material, and its preparing method Download PDFInfo
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- CN100467527C CN100467527C CNB2005100964385A CN200510096438A CN100467527C CN 100467527 C CN100467527 C CN 100467527C CN B2005100964385 A CNB2005100964385 A CN B2005100964385A CN 200510096438 A CN200510096438 A CN 200510096438A CN 100467527 C CN100467527 C CN 100467527C
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Abstract
This invention relates a complex material with the group of double Malay imides resin which was enhanced by carbon fiber, and its preparation method. It is characterized in: putting the allylic compounds, inorganic whiskers and double Malay imides resins into reactor, then heated and stirred. When the resins changed transparency, the acetone was then dripped in. The resin glue was obtained after cooling; or putting the double Malay imides resin, dia mines, inorganic whiskers and toluol into reactor, heated and refluxed, then the epoxide resin and the acetone were added, after milled equality, the whiskerizing resin glue was obtained. The two resin glues with the carbon fiber immersed were obtained by the two different methods above and were prepared to produce the complex material according the fashioned technology. Compared with the complex material without whiskers, the flexural strength, shock strength and tensile strength of the complex material in this invention were increased by 5-10% and the shearing strength in layers was increased by 10-30%. The preparation method is simple and feasible, and can be extended easily.
Description
Technical field:
The present invention relates to a kind of carbon fiber reinforced bismalemide resin base composite material and preparation method thereof, prepared the advanced carbon fiber reinforced bismalemide resin base composite material of a kind of novel high interlaminar shear strength by bimaleimide resin, modification by copolymerization body, whisker and carbon fiber.
Background technology:
Advanced polymer matrix composites with its outstanding lightweight, high heat-resisting, height ratio strong, the characteristics of height ratio mould and playing the part of indispensable key player in modern industry.The carbon fiber reinforced bismalemide resin base high performance composite are the typical case's representatives in the advanced polymer matrix composites, and it has obtained widespread use in comprising numerous leading-edge fields of defense and commercial industry.Yet an outstanding shortcoming of carbon fiber enhancement resin base composite material is that interlaminar shear strength is lower, and when carbon fiber was high modulus fibre, this shortcoming was more obvious, seriously restricts it than the more application under the exacting terms of work on hand environment.
Mechanical properties such as (axially) tensile strength of fiber reinforced polymer matrix composite, flexural strength are mainly born most of load by fiber, and the interlaminar shear strength of matrix material is then mainly determined by the intensity of interfacial adhesion strength between fiber and matrix and matrix.Causing between polymeric matrix and the fiber reinforced material interfacial adhesion strength relatively poor mainly is because will pass through the high temperature hot pressing and two processes that cool in composite material forming, resin matrix and fiber have very big difference through the shrinking percentage of heating postcooling, so the difference of the interface between resin matrix behind the curing molding and fiber produces stress, makes interlaminar shear strength relatively poor.Therefore, the shrinking percentage that reduces matrix is to improve the composite material interface bonding strength, and then improves the effective ways of matrix material interlayer shearing resistance.In addition, also can improve the interlayer performance of matrix material greatly by macrofiber being carried out 3 D weaving.But it is bigger that 3 D weaving implements difficulty, and cost is very high.
Summary of the invention:
The technical problem that solves:
For fear of the deficiencies in the prior art part, the present invention proposes a kind of carbon fiber reinforced bismalemide resin base composite material and preparation method thereof.
Technical scheme:
A kind of preparation method of carbon fiber reinforced bismalemide resin base composite material is characterized in that: preparation process is as follows:
A, take by weighing allylic cpd 20-90b, inorganic crystal whisker 1-10b and bimaleimide resin 100b in reactor, be warming up to 120-150 ℃ under heating, agitation condition, wherein b is a weight unit;
B, treat resin transparent afterreaction 30-60min, drip solvent acetone again, reduce to whisker/bimaleimide resin glue that room temperature obtains homogeneous transparent;
C, make unidirectional pre-immersion material with above-mentioned glue and carbon fiber 0-300b on wrapping machine, treat behind fugitive constituent＜5wt% prepreg to make volatile content＜1wt% in 65 ℃ of baking 5-10min down, wherein b is a weight unit;
D, above-mentioned carbon fiber prepreg is laid in the mould that scribbles releasing agent suppresses on platen-press: described pressing process is 130 ℃ and stops 30min and begin pressurization, pressurize heats up then, the heating process parameter is: 150 ℃ 1 hour, connect 180 ℃ 1 hour, connect 200 ℃ 1 hour; Aftertreatment technology be 230 ℃ 1 hour, forming pressure is 1MPa.
A kind of preparation method of carbon fiber reinforced bismalemide resin base composite material is characterized in that: preparation process is as follows:
A, take by weighing diamine, bimaleimide resin 100b, inorganic crystal whisker 1-10b and toluene in reactor, reflux 30min, wherein b is a weight unit;
B, be chilled to 40 ℃ and add Resins, epoxy and acetone, stir and promptly get whisker/bimaleimide resin glue;
C, make unidirectional pre-immersion material with above-mentioned glue and carbon fiber 100-300b on wrapping machine, treat behind fugitive constituent＜5wt% prepreg to make volatile content＜1wt% in 65 ℃ of baking 5-10min down, wherein b is a weight unit;
D, above-mentioned carbon fiber prepreg is laid in the mould that scribbles releasing agent suppresses on platen-press: described pressing process is 130 ℃ and stops 30min and begin pressurization, pressurize heats up then, the heating process parameter is: 150 ℃ 1 hour, connect 180 ℃ 1 hour, connect 200 ℃ 1 hour; Aftertreatment technology be 230 ℃ 1 hour, forming pressure is 1Mpa;
The total amount of described diamine and Resins, epoxy is 20-90b.
Described bimaleimide resin is 4,4 '-dimaleoyl imino ditane, 4,4 '-dimaleoyl imino phenyl ether, 4,4 '-dimaleoyl imino sulfobenzide or N-phenyl substituted maleimide amine or its mixture.
Described inorganic crystal whisker is silicon carbide whisker, silicon nitride crystal whisker, titanium carbide crystal whisker, alumina whisker, aluminium nitride whisker, zirconium white whisker, ZnOw, titanium carbide crystal whisker, potassium titanate crystal whisker, aluminium borate whisker or barium carbonate whisker.
Described carbon fiber is general carbon fiber: T300, T400H, T700, T800, IM6, IM7 or IM8; And high modulus carbon fiber: M40, M40J, M55J or M60J.
Described allylic cpd is diallyl bisphenol or diallyl bisphenol S.
Described diamine is fatty amine or aromatic amine.
Described fatty amine is: quadrol, Diethylenetriaminee (DETA), triethylenetetramine, tetraethylenepentamine, hexanediamine, dimethylaminopropylamine or diethyl amino propylamine or Dyhard RU 100.
Described aromatic amine is Ursol D, mphenylenediamine, 4,4 '-two amido ditanes, 4,4 '-two amido sulfobenzides, 3,3 '-dichloro-4,4,4 '-two amido ditanes or 4,4 '-two amido diphenyl ethers.
Described Resins, epoxy is novolac epoxy or bisphenol A epoxide resin.
Beneficial effect:
The present invention is by being filled in inorganic crystal whisker in the polymkeric substance, and is compound with carbon fiber again, prepares the advanced carbon fiber reinforced bismalemide resin base high performance composite of high interlaminar shear strength.The strong mechanical performance of this matrix material derives from three aspects: one, and the adding of the inorganic crystal whisker that shrinking percentage is lower has improved the shrinking percentage of resin matrix, and it is poor to have reduced the interface that causes because of shrinking percentage between matrix and the fiber.They are two years old, whisker with certain length-to-diameter ratio can be pricked interlayer at polymer matrix composite as the nail riveting, this pinning effect makes the contact between fiber and the resin matrix become the three-dimensional connection with steric effect from original simple bonding interface (two dimension), this structure that is similar to 3 D weaving makes matrix material when being subjected to shearing action, to overcome on the one hand bonding between matrix and the fiber and do work, on the other hand also will be by destroying bonding acting the between inorganic particulate and matrix and the fiber, make crackle when expansion, need consume more energy, thereby improve the interlayer performance of polymer matrix composite.Its three, the characteristic high-strength, Gao Mo of whisker has also further improved the intensity and the modulus of matrix material.
The present invention proposes a kind of carbon fiber reinforced bismalemide resin base composite material and compares with the matrix material that does not add whisker, and its flexural strength, resistance to impact shock, tensile strength have improved 5-10%, and interlaminar shear strength has improved 10-30%.They can be used for the leading-edge field in thermal characteristics and mechanical property (especially interlaminar shear strength) exigent national defence and the civilian industry.Preparation method of the present invention, technology is simple, feasible, is easy to promote.
Embodiment:
Now the present invention is further described:
Embodiment 1
Take by weighing 4,4 '-dimaleoyl imino ditane 100g, diallyl bisphenol 75g, put into three mouthfuls of reaction flasks of 500ml, be heated to 140-150 ℃ of reaction 30min, be cooled to and begin to add acetone 200ml below 100 ℃, add the 5g ZnOw during to room temperature.On wrapping machine, make unidirectional pre-immersion material with above-mentioned glue and M55J carbon fiber, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min down in 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 130 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 230 ℃/5h, and forming pressure is 1MPa.The tensile strength that obtains unidirectional shop layer matrix material is 1050MPa, and flexural strength is 1250MPa, and modulus in flexure is 198GPa, and interlaminar shear strength is 84MPa.Compare with the contrast material that does not add ZnOw, their flexural strength and tensile strength increase rate are 5-7%, and interlaminar shear strength has improved 24%.
Embodiment 2
Take by weighing 4,4 '-dimaleoyl imino ditane 100g, diallyl bisphenol 75g, put into three mouthfuls of reaction flasks of 500ml, be heated to 140-150 ℃ of reaction 30min, be cooled to and begin to add acetone 200ml below 100 ℃, add the 1g ZnOw during to room temperature.On wrapping machine, make unidirectional pre-immersion material with above-mentioned glue and M55J carbon fiber, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min down in 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 130 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 230 ℃/5h, and forming pressure is 1MPa.The tensile strength that obtains unidirectional shop layer matrix material is 1050MPa, and flexural strength is 1250MPa, and modulus in flexure is 198GPa, and interlaminar shear strength is 84MPa.Compare with the contrast material that does not add ZnOw, their flexural strength and tensile strength increase rate are not obvious, and interlaminar shear strength has improved about 10%.
Embodiment 3
Take by weighing 4,4 '-dimaleoyl imino phenyl ether 100g, diallyl bisphenol S 80g, put into three mouthfuls of reaction flasks of 500ml, be heated to 145-155 ℃ of reaction 45min, be cooled to and begin to add acetone 200ml below 100 ℃, add the 10g aluminium borate whisker during to room temperature.On wrapping machine, make unidirectional pre-immersion material with above-mentioned glue and T700 carbon fiber, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min down in 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 130 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 230 ℃/5h, and forming pressure is 1MPa.The tensile strength that obtains unidirectional shop layer matrix material is 1640MPa, flexural strength is 1280MPa, modulus in flexure is 235GPa, interlaminar shear strength is 69MPa, compare with the contrast material that does not add ZnOw, their flexural strength and tensile strength increase rate are 5-8%, and interlaminar shear strength has improved 28%.
Embodiment 4
Take by weighing 4,4 '-dimaleoyl imino ditane 90g, N-phenyl substituted maleimide amine 10g, diallyl bisphenol 80g,, put into three mouthfuls of reaction flasks of 500ml, be heated to 140-150 ℃ of reaction 30min, be cooled to and begin to add acetone 200ml below 100 ℃, adding 8g potassium titanate crystal whisker during to room temperature.On wrapping machine, make unidirectional pre-immersion material with above-mentioned glue and M40 carbon fiber, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min down in 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 130 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 230 ℃/5h, and forming pressure is 1MPa.Obtain unidirectional shop layer performance of composites and compare with the performance of the contrast material that does not add ZnOw, their flexural strength and tensile strength increase rate are 5-7%, and interlaminar shear strength has improved 23%.
Take by weighing 4,4 '-dimaleoyl imino ditane 90g, N-phenyl substituted maleimide amine 10g, 4,4 '-two amido ditane 10g, silicon nitride crystal whisker 6g, toluene 250ml puts into three mouthfuls of reaction flasks of 500ml, reflux 30min, be chilled to 40 ℃ and add bisphenol A type epoxy resin (E-51) 30g and acetone 100ml, stir and promptly get whisker/BMI resin adhesive liquid.Adopt the Wrapping formed unidirectional M60J carbon fiber prepreg of this resin adhesive liquid, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min under 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 115 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 130 ℃/1h+150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 220 ℃/5h, and forming pressure is 1MPa.Obtain unidirectional shop layer performance of composites and compare with the performance of the contrast material that does not add whisker, their flexural strength and tensile strength increase rate are 5%, and interlaminar shear strength has improved 26%.
Embodiment 6
Take by weighing 4,4 '-dimaleoyl imino ditane 60g, 4,4 '-dimaleoyl imino phenyl ether 30g, N-phenyl substituted maleimide amine 10g ' 4,4 '-two amido diphenyl ether 12g, alumina whisker 5g, toluene 250ml, put into three mouthfuls of reaction flasks of 500ml, reflux 30min is chilled to 40 ℃ and adds glycerol epoxy resin (B-63) 22g and acetone 100ml, stirs and promptly gets whisker/BMI resin adhesive liquid.Adopt the Wrapping formed unidirectional IM7 carbon fiber prepreg of this resin adhesive liquid, treat behind fugitive constituent＜5wt% prepreg to be dried by the fire 5-10min under 65 ℃, make volatile content＜1wt%, be laid on compression moulding on platen-press in the mould that scribbles releasing agent on request.Pressing process is 115 ℃ and stops 30min and begin pressurization that pressurize heats up then, and technology is 130 ℃/1h+150 ℃/1h+180 ℃/1h+200 ℃/1h, and aftertreatment technology is 220 ℃/5h, and forming pressure is 1MPa.Obtain unidirectional shop layer performance of composites and compare with the performance of the contrast material that does not add ZnOw, their flexural strength and tensile strength increase rate are 6-8%, and interlaminar shear strength has improved 29%.
Claims (10)
1, a kind of preparation method of carbon fiber reinforced bismalemide resin base composite material, it is characterized in that: preparation process is as follows:
A, take by weighing allylic cpd 20-90b, inorganic crystal whisker 1-10b and bimaleimide resin 100b in reactor, be warming up to 120-150 ℃ under heating, agitation condition, wherein b is a weight unit;
B, treat resin transparent afterreaction 30-60min, drip solvent acetone again, reduce to whisker/bimaleimide resin glue that room temperature obtains homogeneous transparent;
C, make unidirectional pre-immersion material with above-mentioned glue and carbon fiber 0-300b on wrapping machine, treat behind fugitive constituent＜5wt% prepreg to make volatile content＜1wt% in 65 ℃ of baking 5-10min down, wherein b is a weight unit;
D, above-mentioned carbon fiber prepreg is laid in the mould that scribbles releasing agent suppresses on platen-press: described pressing process is 130 ℃ and stops 30min and begin pressurization, pressurize heats up then, the heating process parameter is: 150 ℃ 1 hour, connect 180 ℃ 1 hour, connect 200 ℃ 1 hour; Aftertreatment technology be 230 ℃ 1 hour, forming pressure is 1MPa.
2, a kind of preparation method of carbon fiber reinforced bismalemide resin base composite material, it is characterized in that: preparation process is as follows:
A, take by weighing diamine, bimaleimide resin 100b, inorganic crystal whisker 1-10b and toluene in reactor, reflux 30min, wherein b is a weight unit;
B, be chilled to 40 ℃ and add Resins, epoxy and acetone, stir and promptly get whisker/bimaleimide resin glue;
C, make unidirectional pre-immersion material with above-mentioned glue and carbon fiber 100-300b on wrapping machine, treat behind fugitive constituent＜5wt% prepreg to make volatile content＜1wt% in 65 ℃ of baking 5-10min down, wherein b is a weight unit;
D, above-mentioned carbon fiber prepreg is laid in the mould that scribbles releasing agent suppresses on platen-press: described pressing process is 130 ℃ and stops 30min and begin pressurization, pressurize heats up then, the heating process parameter is: 150 ℃ 1 hour, connect 180 ℃ 1 hour, connect 200 ℃ 1 hour; Aftertreatment technology be 230 ℃ 1 hour, forming pressure is 1Mpa;
The total amount of described diamine and Resins, epoxy is 20-90b.
3, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 1 and 2, it is characterized in that: described bimaleimide resin is 4,4 '-dimaleoyl imino ditane, 4,4 '-dimaleoyl imino phenyl ether, 4,4 '-dimaleoyl imino sulfobenzide or N-phenyl substituted maleimide amine or its mixture.
4, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 1 and 2 is characterized in that: described inorganic crystal whisker is silicon carbide whisker, silicon nitride crystal whisker, titanium carbide crystal whisker, alumina whisker, aluminium nitride whisker, zirconium white whisker, ZnOw, titanium carbide crystal whisker, potassium titanate crystal whisker, aluminium borate whisker or barium carbonate whisker.
5, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 1 and 2 is characterized in that: described carbon fiber is general carbon fiber: T300, T400H, T700, T800, IM6, IM7 or IM8; Or high modulus carbon fiber: M40, M40J, M55J or M60J.
6, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 1 is characterized in that: described allylic cpd is diallyl bisphenol or diallyl bisphenol S.
7, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 2 is characterized in that: described diamine is fatty amine or aromatic amine.
8, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 7 is characterized in that: described fatty amine is: quadrol, Diethylenetriaminee (DETA), triethylenetetramine, tetraethylenepentamine, hexanediamine, dimethylaminopropylamine or diethyl amino propylamine or Dyhard RU 100.
9, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 7, it is characterized in that: described aromatic amine is Ursol D, mphenylenediamine, 4,4 '-two amido ditanes, 4,4 '-two amido sulfobenzides, 3,3 '-dichloro-4,4,4 '-two amido ditanes or 4,4 '-two amido diphenyl ethers.
10, the preparation method of carbon fiber reinforced bismalemide resin base composite material according to claim 2 is characterized in that: described Resins, epoxy is novolac epoxy or bisphenol A epoxide resin.
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| CN101440175B (en) * | 2007-11-23 | 2011-07-20 | 颜立峰 | Cast nylon active heat resisting flexibilizer and preparation thereof |
| CN102507283B (en) * | 2011-11-10 | 2013-09-04 | 西安康本材料有限公司 | Method for preparing 12k multifilament sample and testing stretching performance of sample |
| CN102634208B (en) * | 2012-04-27 | 2014-01-01 | 沈阳航空航天大学 | Nanocomposite modification method applied to bismaleimide resin based composite |
| KR20190035731A (en) * | 2016-08-05 | 2019-04-03 | 닛뽄 가야쿠 가부시키가이샤 | Maleimide resin composition, prepreg, cured product thereof, and semiconductor device |
| CN114656787A (en) * | 2020-12-23 | 2022-06-24 | 中国石油化工股份有限公司 | Wear-resistant high-hardness anticorrosive composition and application thereof |
| CN114213810A (en) * | 2021-12-28 | 2022-03-22 | 宁波美佳速创智能科技有限公司 | High-strength 3D printing photosensitive resin material |
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