CN107458066A - A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites - Google Patents

A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites Download PDF

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Publication number
CN107458066A
CN107458066A CN201710600809.1A CN201710600809A CN107458066A CN 107458066 A CN107458066 A CN 107458066A CN 201710600809 A CN201710600809 A CN 201710600809A CN 107458066 A CN107458066 A CN 107458066A
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carbon fiber
preparation
fiber reinforced
polymer matrix
reinforced polymer
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CN201710600809.1A
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CN107458066B (en
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余木火
程超
张辉
周金利
蒋民强
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Donghua University
National Dong Hwa University
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Donghua University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0036—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0076—Curing, vulcanising, cross-linking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2270/00—Resin or rubber layer containing a blend of at least two different polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/54—Yield strength; Tensile strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2605/00—Vehicles
    • B32B2605/18—Aircraft

Abstract

The present invention relates to a kind of preparation method of toughening carbon fiber reinforced polymer matrix composites, including：(1) epoxy resin is added in polyethers sulfolane solution, obtains mixed solution, it is stand-by finally to carry out deaeration processing；(2) mixed solution is scraped on identical in surface pore aperture and equally distributed flat board with knifing rod, the film forming in deionized water coagulating bath, obtained primary membrane obtains composite membrane after washing and drying；(3) composite membrane and carbon cloth are subjected to laying, resin is irrigated under negative pressure of vacuum, it is cured to obtain toughening carbon fiber reinforced polymer matrix composites.Preparation technology of the present invention is simple, operable row is strong, is adapted to industrialized production；The composite materials property of preparation is lifted by a small margin, and interlaminar fracture toughness lifting is more notable, has a good application prospect.

Description

A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites
Technical field
The invention belongs to carbon fibre composite field, more particularly to a kind of system of toughening carbon fiber reinforced polymer matrix composites Preparation Method.
Background technology
With the demand for development of aircraft industry material lightweight, carbon fiber resin matrix composite (Carbon Fiber Reinforced Polymer CFRP) master/secondary structure material of aircraft is increasingly being applied to, therefore develop high-ductility The carbon fiber/epoxy resin composite material of property is the great research direction of current field of compound material.
The toughness reinforcing of carbon fiber/epoxy resin composite material mainly has two ways：When epoxy resin toughened matrix, second, Interlayer toughened is carried out to composite.Interlayer toughened is that thin toughening material layer is added between composite plys, multiple to improve The fracture toughness and damage tolerance of condensation material；It can be described as the second discrete phase material layer with particle, fiber or film Form is inserted between composite plys.The common implementation of interlayer film toughness reinforcing is by certain thickness thin polymer film It is placed between laying, solidifies laminate according to the curing cycle of resin.
But the phenomenon that resin can not permeate completely often occurs for the method for interlayer toughened at present, causes carbon fibre resin The intensity of based composites is still not high enough, limits its application development.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of toughening carbon fiber reinforced polymer matrix composites, This method preparation technology is simple, operable row is strong, is adapted to industrialized production；The composite materials property of preparation obtains by a small margin Lifting, interlaminar fracture toughness lifting is more notable, has a good application prospect.
The invention provides a kind of preparation method of toughening carbon fiber reinforced polymer matrix composites, including：
(1) polyether sulfone is uniformly mixed at 60 DEG C -80 DEG C with solvent, obtains polyethers sulfolane solution；Then by epoxy resin It is added in polyethers sulfolane solution, is uniformly mixed at 30~50 DEG C, obtain mixed solution, it is stand-by finally carries out deaeration processing；Its In, the mass ratio of polyether sulfone and epoxy resin is 7.5:2.5~9.5:0.5；
(2) mixed solution in step (1) is scraped into identical in surface pore aperture and equally distributed flat board with knifing rod On, film forming, obtained primary membrane obtain composite membrane after washing and drying in deionized water coagulating bath after prevapourising；
(3) composite membrane in step (2) is pressed into the number of plies than 9~19:10~20 carry out laying with carbon cloth, are born in vacuum Pressure perfusion resin, it is cured to obtain toughening carbon fiber reinforced polymer matrix composites (VARI moulding process).
Solvent in the step (1) is dimethyl sulfoxide (DMSO), dimethylformamide or dimethyl acetamide；Polyether sulfone with it is molten The mass ratio of agent is 1:3~6.Polyether sulfone used is hydroxy-end capped.
Epoxy resin in the step (1) is glycidyl ether type epoxy resin.
The glycidyl ether type epoxy resin is E51 epoxy resin.
A width of 100~200 μm between knifing rod in the step (2).The material of flat board is tetrafluoroethene.
The aperture of compound membrane pores in the step (2) is 1~2mm, and surface hole density is 0.3~0.5 hole/cm2。
Perfusion resin in the step (3) is specially：E51 epoxy resin is irrigated, filling temperature is 60~80 DEG C, viscosity For 0.1~0.2Pas.
Curing process parameter in the step (3) is：Solidification temperature is 120~140 DEG C, and hardening time is 2~4h；Institute The curing agent used is amine curing agent.
The present invention using phase inversion prepares polyether sulfone/epoxy resin composite membrane, by composite membrane be laid in carbon cloth it Between, laminate is made using VARI moulding process.By the addition of casting solution epoxy resin additive, composite membrane is compared to pure PES films got a promotion in the dissolution velocity of epoxy resin, and pass through to support flat board punching handle, the composite membrane of gained The surface hole that is evenly distributed with same apertures also have the uniform hole of certain density, when resin is irrigated, hole pair The infiltration of resin plays positive role, effectively solves the problems, such as that it hinders infiltration between carbon cloth.
Ratio of the invention by controlling polyether sulfone and epoxy resin, controllable composite membrane are not dissolved under filling temperature Epoxy resin, at curing temperatures rapid dissolving.After solidification, PES microballoons are mutually separated from matrix phase, these PES microballoon phases The developing direction of crackle when can change resin matrix brittle fracture, and the extension of crackle is hindered, establish a kind of interlayer toughened New method.
Beneficial effect
(1) preparation technology of the present invention is simple, operable row is strong, is adapted to industrialized production；The Compound Material Engineering of preparation It can be lifted by a small margin, interlaminar fracture toughness lifting is more notable, has a good application prospect；
(2) carbon fibre composite after toughness reinforcing is compared to non-toughness reinforcing, its tensile strength, stretch modulus, bending strength And stretch modulus improves, compressive strength lifting 13%, modulus of compressibility lifting 18%, interlaminar fracture toughness lifting 25%.
Brief description of the drawings
Fig. 1 is the mode of appearance of primary membrane of the present invention；
Fig. 2 is the laminate SEM sectional drawings that the present invention is prepared.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Scope.
Embodiment 1
(1) take 19g PES powder to be placed in beaker, add the dimethyl sulfoxide (DMSO) of 4 times of PES mass, 60 DEG C are stirred to equal After even, 1g E51 epoxy resin is added, 30 DEG C stir, and obtain mixed solution, and deaeration processing is stand-by in 30 DEG C of baking ovens.
(2) surface is had to diameter 2mm hole, 0.36 hole of hole density/cm2Tetrafluoroethene plate carry out cleaning drying, and protect Hold that its temperature is identical with mixed solution temperature, mixed solution is poured on to one end of flat board, make its shape with wide knifing rod between 120 μm Into one layer of uniform liquid film, after prevapourising 30s, it is immersed in pure deionized water, primary membrane is obtained after 2min, it is nascent by what is obtained It is stand-by that film obtains composite membrane after washing and drying.
(3) composite membrane is put into continuous carbon cloth interlayer, according to VARI techniques, lays carbon cloth, release cloth, lead Drift net, vacuum bag sealing whole system.Then the gas of mold cavity, 60 DEG C of perfusion E51 asphalt mixtures modified by epoxy resin are extracted out under negative pressure of vacuum Fat, resin viscosity 0.2Pas, wherein composite membrane and carbon cloth number of plies ratio are 9:11.After 120 DEG C/2h+180 DEG C The curing process of processing, obtain the compound phase inversion membrane interlayer toughened resin-based carbon fiber composite wood of polyether sulfone/E51 epoxy resin Material.
Sample correlation mechanical property is detected using microcomputer controlled electronic universal tester
Non- toughening material The present embodiment
Tensile strength (MPa) 602 636
Stretch modulus (GPa) 100 111
Bending strength (MPa) 1203 1165
Bending modulus (GPa) 1165 176
Compressive strength (MPa) 621 694
Modulus of compressibility (GPa) 91 108
GIIC(KJ/m2) 1.227 1.534
It can be drawn the following conclusions by upper table：The compound phase inversion membrane interlayer toughened of the polyether sulfone of the present embodiment/E51 epoxy resin Resin-based carbon fiber composite, non-toughening material tensile strength can be made, stretch modulus, bending strength, bending modulus is by a small margin Improve, compressive strength, modulus, interlaminar fracture toughness improves more obvious, lifting 25%.

Claims (8)

1. a kind of preparation method of toughening carbon fiber reinforced polymer matrix composites, including：
(1) polyether sulfone is uniformly mixed at 60 DEG C -80 DEG C with solvent, obtains polyethers sulfolane solution；Then epoxy resin is added Into polyethers sulfolane solution, uniformly mixed at 30~50 DEG C, obtain mixed solution, it is stand-by finally to carry out deaeration processing；Wherein, gather The mass ratio of ether sulfone and epoxy resin is 7.5:2.5~9.5:0.5；
(2) mixed solution in step (1) is scraped on identical in surface pore aperture and equally distributed flat board with knifing rod, in advance Film forming, obtained primary membrane obtain composite membrane after washing and drying in deionized water coagulating bath after evaporation；
(3) composite membrane in step (2) is pressed into the number of plies than 9~19:10~20 carry out laying with carbon cloth, under negative pressure of vacuum Resin is irrigated, it is cured to obtain toughening carbon fiber reinforced polymer matrix composites.
A kind of 2. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute It is dimethyl sulfoxide (DMSO), dimethylformamide or dimethyl acetamide to state the solvent in step (1)；The mass ratio of polyether sulfone and solvent For 1:3~6.
A kind of 3. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute It is glycidyl ether type epoxy resin to state the epoxy resin in step (1).
A kind of 4. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 3, it is characterised in that：Institute It is E51 epoxy resin to state glycidyl ether type epoxy resin.
A kind of 5. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute A width of 100~200 μm are stated between the knifing rod in step (2).
A kind of 6. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute The aperture for stating the compound membrane pores in step (2) is 1~2mm, and surface hole density is 0.3~0.5 hole/cm2。
A kind of 7. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute The perfusion resin stated in step (3) is specially：Irrigate E51 epoxy resin, filling temperature be 60~80 DEG C, viscosity be 0.1~ 0.2Pa·s。
A kind of 8. preparation method of toughening carbon fiber reinforced polymer matrix composites according to claim 1, it is characterised in that：Institute The curing process parameter stated in step (3) is：Solidification temperature is 120~140 DEG C, and hardening time is 2~4h；Used solidification Agent is amine curing agent.
CN201710600809.1A 2017-07-21 2017-07-21 A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites Active CN107458066B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110370680A (en) * 2019-06-28 2019-10-25 东华大学 A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites
CN113287583A (en) * 2021-06-18 2021-08-24 威海亿美运动器械有限公司 Enhanced fishing rod and manufacturing method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104553177A (en) * 2014-12-15 2015-04-29 中航复合材料有限责任公司 Flame-retardant modified carbon fiber prepreg and composite material product
CN104624061A (en) * 2015-02-02 2015-05-20 曾生 Production method of flat sheet membrane

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104553177A (en) * 2014-12-15 2015-04-29 中航复合材料有限责任公司 Flame-retardant modified carbon fiber prepreg and composite material product
CN104624061A (en) * 2015-02-02 2015-05-20 曾生 Production method of flat sheet membrane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110370680A (en) * 2019-06-28 2019-10-25 东华大学 A kind of preparation method of toughening carbon fiber reinforced polymer matrix composites
CN113287583A (en) * 2021-06-18 2021-08-24 威海亿美运动器械有限公司 Enhanced fishing rod and manufacturing method thereof

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