CN108485181A - A kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites and preparation method thereof of matrix - Google Patents
A kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites and preparation method thereof of matrix Download PDFInfo
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- CN108485181A CN108485181A CN201810233520.5A CN201810233520A CN108485181A CN 108485181 A CN108485181 A CN 108485181A CN 201810233520 A CN201810233520 A CN 201810233520A CN 108485181 A CN108485181 A CN 108485181A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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Abstract
The invention discloses the fibre reinforced composites that a kind of silicon carbide polyether-ether-ketone is matrix, by fiber preform, boundary layer, silicon carbide substrate and polyether-ether-ketone matrix composition；It is characterized in that boundary layer is coated on the surface of monfil, state of siege in a ring, interfacial layer thickness is 0.3 ~ 10mm, silicon carbide substrate is filled in fibrage, winding, in the hole for the fiber preform that laying is formed, across boundary layer between fiber, microcosmic discrete distribution, silicon-carbide particle, contain stomata between crystal grain, it is thin to see by fiber segmentation, form long strip block between fiber interfascicular irregular bulk and filament, polyether-ether-ketone is filled in the hole of silicon carbide substrate, it is formed continuous, half discontinuous network state, subnetwork runs through, upper and lower surface of the subnetwork not through composite material.
Description
Technical field
The present invention relates to a kind of fibre reinforced composites and preparation method thereof, more particularly to a kind of silicon carbide-polyethers ether
Ketone is the fibre reinforced composites and preparation method thereof of matrix.
Background technology
Fibre reinforced composites, especially silicon carbide fiber reinforced based composites have structure light wt, height higher than strong
Than mould, stability is good, good impact resistance, low thermal coefficient of expansion and the features such as oxidation and corrosion, extensive
Applied to fields such as automobile, sport, electronics and aerospaces.When silicon carbide fiber reinforced based composites are applied in aerospace
Field non high temperature component, such as airline carriers of passengers engine housing, fuselage cover, undercarriage and wing non high temperature component,
Due to material preparation defect, with higher open pore rate（5~15%）, surface roughness is larger and surface brittleness is big, easily
Collapse the shortcomings of broken, which greatly limits silicon carbide fiber reinforced based composites non high temperature component application.
Polyether-ether-ketone is the most important kind in poly(aryl ether ketone) family, is that the most excellent thermoplasticity of comprehensive performance is extraordinary
One of engineering plastics.Polyether-ether-ketone glass transition temperature is 143 DEG C, and the melting temperature of crystallinity PEEK is 343 DEG C.Due to poly-
Ether ether ketone is the polymer of the full armaticity of main chain, and the phenyl ring containing high-content in strand, it is excellent that this just imparts polyether-ether-ketone
Comprehensive performance, including good heat resistance, excellent thermal stability and thermo oxidative stability, anti-flammability, hydrolytic resistance and resistance to
The excellent performance such as radiation property.It, can be apparent right when in the hole that polyether-ether-ketone is filled in silicon carbide substrate as matrix
Silicon carbide fiber reinforced based composites carry out Strengthening and Toughening, hence it is evident that reduce the open pore rate of material（＜ 0.1%）And improve material
The roughness on surface makes silicon carbide fiber reinforced based composites can be applied to the multiple fields such as airplane skin structural material.
Application publication number be CN107310240A Chinese patent disclose carbon fiber reinforced polyetheretherketonecomposite composite material and
Preparation method belongs to the technical field of continuous carbon fibre enhancing composite material.The invention solves existing APC-2 prepregs to answer
Used time prepares the technical problem of existing laying difficulty during complex component.Carbon fiber reinforced polyetheretherketonecomposite composite material be by
Carbon fiber and polyetheretherketonefiber fiber carry out shuffling with control of two-dimensional braided, then clipped, stack paving, hot-forming handle are made successively
's；Wherein, warp thread is carbon fiber, and weft yarn is polyetheretherketonefiber fiber, two layers of Unidirectional of arbitrary neighborhood during stack paving
Fiber is arranged in angle.The method of the present invention remain fiber flexibility and hanging property, laying it is more convenient.Prepared by the invention
It is carbon fiber reinforced polyetheretherketonecomposite composite material, there is no playing, polyether-ether-ketone is excellent to ceramic matric composite surface layer Strengthening and Toughening etc.
Point.
Application No. is 201710483096.5 Chinese patent, to disclose a kind of high temperature resistance and high strength of fibre reinforced light
Matter hybrid ceramic-resin composite materials pipe fitting, using ceramic matric composite as shell, polymer matrix composites are inner casing, shell,
Inner casing formation composite construction nested against one another, inside and outside wall surface is smooth, and ceramic composition is in ladder along pipe thickness direction in composite material
Degree distribution, is gradually reduced, heat resistance is good, prolonged application can be realized at 600 DEG C, compared to conventional aluminum inwards by outer surface of pipe fittings
Alloy shell, thermal coefficient is lower, and high temperature resistant thermal protective performance is more preferable；Resin Composition along pipe thickness direction also distribution gradient,
Gradually reduced outward by inner surface of pipe fitting, and fill certain amount filler, improves resin-based materials heat resistance and impact resistance
Can, vibration damping shock-resistance features are made it have, the two is integrally formed, and is prepared and is integrated high temperature resistant, solar heat protection, heat-insulated, carrying, vibration damping
Lightweight hybrid ceramic-resin composite materials pipe fitting.
Application No. is 201710294190.6 Chinese patents to disclose a kind of novel carbon fiber composite and its manufacture
Method, the novel carbon fiber composite include 60% ~ 80% carbon fiber, 19% ~ 31% thermoplastic resin, 12% ~ 18% ceramic material
With 1% ~ 9% curing agent, the carbon fiber, thermoplastic resin, ceramic material and curing agent mixing match be 14:5:3:1, this hair
Bright while also disclosing a kind of manufacturing method of novel carbon fiber composite, this method includes S1：Carbon fiber bundle is arranged to interconnect
Body structure；S2：Make glycolylurea epoxide resin, pvdf resin or vinylidene fluoride copolymers resin matrix solution, ceramic material
The mixed serum of powder；S3：It pours；S4：Hot forming process, the present invention is by carbon fiber by interconnected body structure setting one
It rises, using thermoplastic resin, ceramic material and curing agent by multigroup carbon fiber thermal pressing formation, is increased in overall structure novel
The intensity, toughness and service life of carbon fibre composite, it is more more stable than traditional carbon fiber composite structure.
There are problems to be for above-mentioned patent：Pure ceramic matric composite density is big, and pure ceramic matric composite brittleness is big, limitation
It is applied in the field that rigidity requirement is high, reliability requirement is high, functionally gradient material (FGM) still cannot solve the above problems.
Invention content
To solve the above problems, the present invention proposes that a kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites of matrix
And preparation method thereof, the advantage of the silicon carbide fiber reinforced based composites of polyether-ether-ketone Strengthening and Toughening is given full play to, fiber has been widened
Enhance the application field of carborundum based material.
A kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites of matrix, by fiber preform, boundary layer, carbonization
Silicon substrate and polyether-ether-ketone matrix composition；Fiber is one kind of carbon fiber, silicon carbide fibre, high silica fiber, alumina fibre
Or two kinds, the volume fraction for accounting for entire composite material is 25 ~ 55%；Boundary layer be pyrolytic carbon, silicon carbide, boron nitride, aluminium oxide,
1 ~ 3 kind in zirconium oxide, phosphate, carbon nanotubes, fullerene, it is arranged as 1 ~ 5 layer, it is characterised in that boundary layer is coated on monofilament
The surface of fiber, in a ring state of siege, interfacial layer thickness are 0.3 ~ 10mm, the volume fraction for accounting for entire composite material is 2 ~
10%；Silicon carbide substrate be filled in fibrage, winding, laying formed fiber preform hole in, between fiber across
Boundary layer, microcosmic discrete distribution, contains stomata between silicon-carbide particle, crystal grain, thin to see by fiber segmentation, forms fibre bundle
Between long strip block between irregular bulk and filament, account for the 25 ~ 45% of entire composite material volume fraction；Polyether-ether-ketone is filled in
In the hole of silicon carbide substrate, continuous, half discontinuous network state is formed, subnetwork runs through the upper and lower surface of composite material,
The volume fraction for accounting for entire composite material is 5 ~ 25%；The density of composite material of the present invention is 1.6 ~ 2.0g/cm3, compound
In material surface area, silicon carbide occupied area is 0 ~ 10%, and polyether-ether-ketone occupied area is 90 ~ 100%.
A kind of silicon carbide-polyether-ether-ketone is the preparation method of the fibre reinforced composites of matrix, it is characterised in that including
The step of following sequences：
（1）Fibrage, winding, lay are prepared into fiber preform, is cleaned by ultrasonic with organic solvent, is dried in baking oven, is dried
Dry temperature is 80 ~ 120 DEG C；
（2）Inert atmosphere or vacuum high temperature by fiber preform in flowing are handled, and carbon fiber precast body is at 1500 ~ 2000 DEG C
High-temperature process, silicon carbide fibre precast body exist in 800 ~ 1000 DEG C of high-temperature process, high silica fiber, alumina fibre precast body
500 ~ 800 DEG C of high-temperature process；
（3）Prepare interface：Pyrolytic carbon, silicon carbide, boron nitride interface are prepared using chemical vapor infiltration, using sol-gal process
Alumina interface is prepared by presoma of aluminium secondary butylate, zirconium oxide interface is prepared using metal zirconium salt chemical vapour deposition technique, is adopted
Phosphate interface is prepared as presoma with sol-gal process using nitrate and phosphoric acid the second light industry bureau amine, using catalysis-chemical vapor deposition
Method or carbon nanotubes solution dipping method prepare carbon nanotubes interface, and carbon tetrachloride is used to prepare fullerene for solution solution modeling method
Interface；
（4）Using trichloromethyl silane, dichloro methyl silane, chloromethyl silane as presoma, by chemical vapor infiltration system
Standby fine and close nanocrystalline beta silicon carbide matrix；To contain vinyl liquid Polycarbosilane as presoma, prepared by infiltration pyrolysis method more
Hole crystallite beta silicon carbide matrix, after the completion of preparation, composite material is semi-finished product, and open porosity is 10 ~ 27%；
（5）Diphenyl sulphone (DPS) is dissolved in acetone, then polyether-ether-ketone is dissolved in diphenyl sulphone (DPS)/acetone soln, diphenyl sulphone (DPS) and polyether-ether-ketone
Mass ratio is 1：4 ~ 10, polyether-ether-ketone-diphenyl sulphone (DPS)/acetone soln is put into baking oven and is dried, diphenyl sulphone (DPS) modified polyether ether is obtained
Ketone；
（6）By step（4）It prepares semi-finished product and is embedded in step（5）In the modified polyetheretherketonefiber prepared, it is warming up to 360 ~ 440
DEG C, it vacuumizes, then 0.5 ~ 5h of pressure heat-preserving, the composite material of the present invention is obtained after demoulding.
Advantageous effect of the present invention：（1）Using polyether-ether-ketone as matrix Strengthening and Toughening fibre reinforced composites, manufacturing cycle
It is short, it is easy to accomplish；（2）Due to the toughening effect of polyether-ether-ketone, reduces fibre reinforced composites stress and collapse broken tendency, carry
The high intensity of fibre reinforced composites；（3）Polyether-ether-ketone can be substantially reduced fibre reinforced composites surface open pore
Rate improves the flatness and smoothness on fibre reinforced composites surface, has widened its application field.
Embodiment
A kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites of matrix, by fiber preform, boundary layer, carbonization
Silicon substrate and polyether-ether-ketone matrix composition；Fiber is carbon fiber, and the volume fraction for accounting for entire composite material is 40%；Boundary layer is
Pyrolytic carbon interface, it is characterised in that boundary layer is coated on the surface of monfil, in a ring state of siege, and interfacial layer thickness is
1mm, the volume fraction for accounting for entire composite material are 3%；Silicon carbide substrate is filled in the hole of the fiber preform of fibrage formation
In gap, contain stomata between silicon-carbide particle, crystal grain across boundary layer, microcosmic discrete distribution between fiber, it is thin to see upper quilt
Fiber segmentation forms long strip block between fiber interfascicular irregular bulk and filament, accounts for entire composite material volume fraction
35%；Polyether-ether-ketone is filled in the hole of silicon carbide substrate, forms continuous, half discontinuous network state, subnetwork runs through,
For subnetwork not through the upper and lower surface of composite material, the volume fraction for accounting for entire composite material is 20%；It is of the present invention multiple
The density of condensation material is 1.85g/cm3, during composite material surface accumulates, silicon carbide occupied area is 5%, polyether-ether-ketone occupied area
It is 95%.
A kind of above-mentioned silicon carbide-polyether-ether-ketone is the preparation method of the fibre reinforced composites of matrix, including following suitable
The step of sequence：
（1）Carbon fiber braiding is prepared into carbon fiber precast body, is cleaned by ultrasonic with absolute ethyl alcohol, is dried in baking oven, drying temperature
It is 80 DEG C；
（2）By carbon fiber precast body in the inert atmosphere of flowing 1800 DEG C of high-temperature process；
（3）Prepare interface：Pyrolytic carbon interface is prepared using chemical vapor infiltration；
（4）Using trichloromethyl silane as presoma, fine and close nanocrystalline beta silicon carbide matrix is prepared by chemical vapor infiltration；
To contain vinyl liquid Polycarbosilane as presoma, porous crystallite beta silicon carbide matrix is prepared by infiltration pyrolysis method, prepares and completes
Afterwards, composite material is semi-finished product, open porosity 20%；
（5）Diphenyl sulphone (DPS) is dissolved in acetone, then polyether-ether-ketone is dissolved in diphenyl sulphone (DPS)/acetone soln, diphenyl sulphone (DPS) and polyether-ether-ketone
Mass ratio is 1：5, polyether-ether-ketone-diphenyl sulphone (DPS)/acetone soln is put into baking oven and is dried, temperature is 80 DEG C, obtains diphenyl sulphone (DPS) and changes
Property polyether-ether-ketone；
（6）By step（4）It prepares semi-finished product and is embedded in step（5）In the modified polyetheretherketonefiber prepared, 400 DEG C are warming up to, is taken out
Vacuum, then pressure heat-preserving 3h, obtains the composite material of the present invention after demoulding.
Composite material compression strength prepared by the present embodiment 1 is more than 550MPa, and bending strength is more than 700MPa, fracture mode
For ductile rupture, fracture toughness 40MPam1/2, elasticity modulus 180GPa, can be used as Aeronautics and Astronautics high rigidity requirement
Workpiece.
The specific implementation mode of the present invention is above are only, but the design concept of the present invention is not limited thereto, it is all to utilize this
Conceive the change for carrying out unsubstantiality to the present invention, the behavior for invading the scope of protection of the invention should all be belonged to.In every case it is not de-
Content from technical solution of the present invention is simply repaiied to any type of made by above example according to the technical essence of the invention
Change, equivalent variations and remodeling, still falls within the protection domain of technical solution of the present invention.
Claims (2)
1. a kind of silicon carbide-polyether-ether-ketone is the fibre reinforced composites of matrix, by fiber preform, boundary layer, silicon carbide
Matrix and polyether-ether-ketone matrix composition；Fiber be carbon fiber, 1 ~ 2 kind of silicon carbide fibre, high silica fiber, alumina fibre,
The volume fraction for accounting for entire composite material is 25 ~ 55%；Boundary layer be pyrolytic carbon, silicon carbide, boron nitride, aluminium oxide, zirconium oxide,
1 ~ 3 kind in phosphate, carbon nanotubes, fullerene, it is arranged as 1 ~ 5 layer, it is characterised in that boundary layer is coated on monfil
Surface, state of siege, interfacial layer thickness are 0.3 ~ 10mm in a ring, and the volume fraction for accounting for entire composite material is 2 ~ 10%；Carbonization
Silicon substrate be filled in fibrage, the fiber preform that winding, laying are formed hole in, across boundary layer between fiber,
Microcosmic discrete distribution, contains stomata between silicon-carbide particle, crystal grain, thin to see by fiber segmentation, forms fiber interfascicular and does not advise
Then long strip block between bulk and filament accounts for the 25 ~ 45% of entire composite material volume fraction；Polyether-ether-ketone is filled in silicon carbide
In the hole of matrix, continuous, half discontinuous network state is formed, subnetwork runs through the upper and lower surface of composite material, accounts for entire
The volume fraction of composite material is 5 ~ 25%；The density of composite material of the present invention is 1.6 ~ 2.0g/cm3, composite material table
In area, silicon carbide occupied area is 0 ~ 10%, and polyether-ether-ketone occupied area is 90 ~ 100%.
2. a kind of silicon carbide-polyether-ether-ketone is the preparation method of the fibre reinforced composites of matrix, it is characterised in that including under
The step of stating sequence：
（1）Fibrage, winding, lay are prepared into fiber preform, is cleaned by ultrasonic with organic solvent, is dried in baking oven, is dried
Dry temperature is 80 ~ 120 DEG C；
（2）Inert atmosphere or vacuum high temperature by fiber preform in flowing are handled, and carbon fiber precast body is at 1500 ~ 2000 DEG C
High-temperature process, silicon carbide fibre precast body exist in 800 ~ 1000 DEG C of high-temperature process, high silica fiber, alumina fibre precast body
500 ~ 800 DEG C of high-temperature process；
（3）Prepare interface：Pyrolytic carbon, silicon carbide, boron nitride interface are prepared using chemical vapor infiltration, using sol-gal process
Alumina interface is prepared by presoma of aluminium secondary butylate, zirconium oxide interface is prepared using metal zirconium salt chemical vapour deposition technique, is adopted
Phosphate interface is prepared as presoma with sol-gal process using nitrate and phosphoric acid the second light industry bureau amine, using catalysis-chemical vapor deposition
Method, carbon nanotubes solution dipping method prepare carbon nanotubes interface, and carbon tetrachloride is used to prepare fullerene for solution solution modeling method
Interface；
（4）Using trichloromethyl silane, dichloro methyl silane, chloromethyl silane as presoma, by chemical vapor infiltration system
Standby fine and close nanocrystalline beta silicon carbide matrix；To contain vinyl liquid Polycarbosilane as presoma, prepared by infiltration pyrolysis method more
Hole crystallite beta silicon carbide matrix, after the completion of preparation, composite material is semi-finished product, and open porosity is 10 ~ 27%；
（5）Diphenyl sulphone (DPS) is dissolved in acetone, then polyether-ether-ketone is dissolved in diphenyl sulphone (DPS)/acetone soln, diphenyl sulphone (DPS) and polyether-ether-ketone
Mass ratio is 1：4 ~ 10, polyether-ether-ketone-diphenyl sulphone (DPS)/acetone soln is put into baking oven and is dried, diphenyl sulphone (DPS) modified polyether ether is obtained
Ketone；
（6）By step（4）It prepares semi-finished product and is embedded in step（5）In the modified polyetheretherketonefiber prepared, it is warming up to 360 ~ 440
DEG C, it vacuumizes, then 0.5 ~ 5h of pressure heat-preserving, the composite material of the present invention is obtained after demoulding.
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| CN111517810A (en) * | 2020-04-23 | 2020-08-11 | 山东工业陶瓷研究设计院有限公司 | High-temperature-resistant ceramic matrix composite interface composite coating and preparation method thereof |
| CN112341204A (en) * | 2020-11-10 | 2021-02-09 | 大连理工大学 | Continuous fiber interweaved and laminated zirconium diboride-based composite material and preparation method thereof |
| CN113683437A (en) * | 2021-08-30 | 2021-11-23 | 江西信达航科新材料科技有限公司 | Carbon-carbon composite material containing refractory metal |
| CN113912405A (en) * | 2020-07-09 | 2022-01-11 | 南京航空航天大学 | Composite material reinforced by hybrid fiber preform and preparation method thereof |
| CN114611782A (en) * | 2022-03-08 | 2022-06-10 | 南京航空航天大学 | Rigidity prediction method for weaving C/C composite material in thermal oxidation environment |
| CN115872760A (en) * | 2022-10-24 | 2023-03-31 | 西安鑫垚陶瓷复合材料股份有限公司 | Filling method of strip holes in ceramic matrix composite prefabricated body |
| CN116425558A (en) * | 2023-05-10 | 2023-07-14 | 中北大学 | Continuous silicon carbide fiber reinforced mullite-based composite material containing interface layer and preparation method thereof |
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| CN111517810A (en) * | 2020-04-23 | 2020-08-11 | 山东工业陶瓷研究设计院有限公司 | High-temperature-resistant ceramic matrix composite interface composite coating and preparation method thereof |
| CN113912405A (en) * | 2020-07-09 | 2022-01-11 | 南京航空航天大学 | Composite material reinforced by hybrid fiber preform and preparation method thereof |
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| CN112341204A (en) * | 2020-11-10 | 2021-02-09 | 大连理工大学 | Continuous fiber interweaved and laminated zirconium diboride-based composite material and preparation method thereof |
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