CN105295373A - Preparation method for carbon fiber reinforced polyimide composite material - Google Patents
Preparation method for carbon fiber reinforced polyimide composite material Download PDFInfo
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- CN105295373A CN105295373A CN201410326641.6A CN201410326641A CN105295373A CN 105295373 A CN105295373 A CN 105295373A CN 201410326641 A CN201410326641 A CN 201410326641A CN 105295373 A CN105295373 A CN 105295373A
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Abstract
The invention relates to a preparation method for a carbon fiber reinforced polyimide (PI) composite material. According to the method, a concentrated nitric acid oxidation and polyimide cladding composite method is adopted to perform surface modification on chopped carbon fiber (CF), so that the mechanical property of the CF reinforced thermoplastic polyimide composite material (CF/TPI) is improved.
Description
Technical field
The invention belongs to polyimide special engineering plastics technical field, relate to a kind of preparation of carbon fiber reinforcement polyimide composite material.
Background technology
Polyimide (PI) generally refers to the class high-performance polymer containing aromatic nucleus and imide ring structure in repeating unit, usually there is high-modulus, high strength, low water absorption, hydrolysis, radiation hardness, the engineering plastics of superior insulation and resistance to thermo-oxidative stability.
At present, polyimide (PI) principal item is divided into thermoset and thermoplastic polyimide.
(1) Thermocurable polyimide: this polyimide resin is opaque solid, insoluble infusibility high molecular polymer, its moulding process does not relate to imidization, relative density is 1.50, without fusing point and glass transition point below 500 DEG C, stablize in less than 450 DEG C, and be insoluble to most organic solvent, there is outstanding high thermal resistance, can use continuously under the comparatively high temps of 260 DEG C, and can good mechanical property and electrical property be kept, itself impact and good stability of the dimension, do not ftracture, not cold flow, there is excellent resistance to heat emission, good chemical-resistant resistance and wear resistance and self lubricity, himself good flame resistance, at high temperature only burn Sum decomposition, missing of ignition.
(2) thermoplastic polyimide: low than heat curing-type PI molecule of the rigidity of thermoplasticity PI molecule, and while increase is flexible, keep mechanical property and thermo-oxidative stability, the solvent resistance etc. of heat curing-type PI excellence as far as possible.This resin has comprehensive physical and mechanical properties, relative density is 1.38, glass transition temperature about 270 DEG C, there is good wear resistance, radiation resistance and electrical insulating property, as as aromatic nucleus special engineering plastics, it occupies the status of very vital role in heat-resistant plastic, is one of kind that in current special engineering plastics, thermotolerance is best, is also the maximum polyimide resin of consumption.But thermotolerance is not as Thermocurable polyimide.
But pure PI is because of lower tension, ultimate compression strength, is not suitable for using as friction materials separately, and the PI matrix material of mechanical property and frictional behaviour excellence after adding fortifying fibre, can be obtained.
Fiber has high strength, high-modulus, the advantage such as high temperature resistant, can increase the mechanical property of PI, improve its dimensional stability, intensity, toughness and thermotolerance etc.Fiber at present for enhancing by polymer modification mainly contains carbon fiber, glass fibre, aramid fiber and various whisker.But undressed fiber surface presents inertia, its specific activity area is little, and surface energy is low, and poor with the interface cohesion of resin, reinforced effects is limited, even can cause the self-defect of matrix material.Therefore, need to carry out surface modification to fiber, to improve the Interface adhesive strength of fiber reinforcement PI matrix material, thus obtain the PI matrix material of mechanical property excellence.
Summary of the invention
The object of the invention is the preparation method providing a kind of fibre reinforced polyimide (PI) matrix material, adopt concentrated nitric acid oxidation and polyimide covered composite yarn method to carry out surface modification to chopped carbon fiber (CF), improve CF and strengthen thermoplastic polyimide composite material (CF/TPI) mechanical property.
The present invention relates to a kind of preparation method of fibre reinforced polyimide (PI) matrix material, it comprises the following steps:
1). carbon fiber surface modification
At normal temperatures, concentrated nitric acid is adopted to carry out etching 1h, drying for standby.
2). the preparation of polyamic acid (PPA)
A certain amount of aromatic series alkyldiamine (DAMI) is dissolved in equal benzene tetramethyl-dianhydride (PMDA), take Tetra hydro Phthalic anhydride as end-capping reagent, and preparation PAA massfraction is the solution of 20%, designs coated PI relative molecular mass 40000.
3). polyimide is coated
Use N, N ˊ-N,N-DIMETHYLACETAMIDE (DMAc) to dilute the PPA solution prepared, its viscosity is reduced, then according to the mass ratio 1:10 of PPA:CF, PPA and CF mixing is stirred evenly, desolventizing DMAc under vacuum.For preventing CF from reuniting in imidization, first remove excessive solvent in mixture, then hot imidization process 2h at 250 DEG C, obtains the CF being coated with PI, then uses agitator to beat evenly.
4) .PI the Molding Forming of Composites
Die press technology for forming is adopted to prepare 30%(massfraction) the TPI matrix material of CF.The CF mechanically mixing of PI powder is even, join in mould and be warmed up to 280 DEG C, apply pressure 10MPa, heat-insulation pressure keeping 1h; Then 340 DEG C are warming up to, pressurize 1h; Be cooled to 100 DEG C, namely the demoulding obtains matrix material.
As no specific instructions, various raw material of the present invention all can be obtained by commercially available, or prepares according to the ordinary method of this area.Unless otherwise defined or described herein, all specialties used herein and scientific words and those skilled in the art the same meaning be familiar with.In addition any method similar or impartial to described content and material all can be applicable in this illustration method.
[embodiment] further illustrates the present invention below by example
At normal temperatures, adopt concentrated nitric acid to carry out etching 1h to CF-1 in advance, be designated as CF-2, drying for standby.A certain amount of aromatic series alkyldiamine (DAMI) is dissolved in equal benzene tetramethyl-dianhydride (PMDA), take Tetra hydro Phthalic anhydride as end-capping reagent, and preparation PAA massfraction is the solution of 20%, designs coated PI relative molecular mass 40000.Use N, N ˊ-N,N-DIMETHYLACETAMIDE (DMAc) to dilute the PPA solution prepared, its viscosity is reduced, then according to the mass ratio 1:10 of PPA:CF, PPA and CF mixing is stirred evenly, desolventizing DMAc under vacuum.For preventing CF from reuniting in imidization, first remove excessive solvent in mixture, then hot imidization process 2h at 250 DEG C, obtains the CF being coated with PI, then uses agitator to beat and evenly (is designated as CF-3).Die press technology for forming is adopted to prepare 30%(massfraction) the TPI matrix material of CF.The CF mechanically mixing of PI powder is even, join in mould and be warmed up to 280 DEG C, apply pressure 10MPa, heat-insulation pressure keeping 1h; Then 340 DEG C are warming up to, pressurize 1h; Be cooled to 100 DEG C, namely the demoulding obtains composite material moulded.Adopt testing standard: tensile strength testing standard is GB/T1040-92, and flexural strength testing standard is GB/T1042-92, impact property test sample shape adopts non-notch standard pilot plant sample, and test result is as shown in table 1.
Table 1CF/TPI composite materials property
| CF-1 | CF-2 | CF-3 | |
| Tensile strength (MPa) | 96 | 91 | 106 |
| Tensile modulus (GPa) | 3.1 | 3.0 | 6.5 |
| Shock strength (KJ/ m 2) | 10.8 | 12.4 | 18.8 |
| Flexural strength (MPa) | 136 | 143 | 161 |
It can thus be appreciated that, the PI layer of concentrated nitric acid to CF surface treatment and coated process can strengthen the interfacial adhesion effect between TPI and CF, and the tensile strength of matrix material improves 10.4%, and Young's modulus improves 109.7%, shock strength improves 74.07%, and flexural strength improves 18.38%.
Below be only embody rule example of the present invention, protection scope of the present invention is not constituted any limitation.The technical scheme that all employings convert on an equal basis or equivalence is replaced and formed, all drops within scope.
Claims (4)
1. the preparation method of fibre reinforced polyimide (PI) matrix material, adopt concentrated nitric acid oxidation and polyimide covered composite yarn method to carry out surface modification to chopped carbon fiber (CF), improve CF and strengthen thermoplastic polyimide composite material (CF/TPI) mechanical property.
2. a kind of fibre reinforced polyimide (PI) matrix material according to claim 1, it is characterized in that, selected carbon fiber diameter is 7 ~ 10 μm, and length is about 100 μm.
3. a kind of fibre reinforced polyimide (PI) matrix material according to claim 1, it is characterized in that, what carbon fiber surface modification was selected is concentrated nitric acid.
4. the preparation method of a kind of fibre reinforced polyimide (PI) matrix material according to claim 1, it comprises step below:
1) carbon fiber surface modification
At normal temperatures, concentrated nitric acid is adopted to carry out etching 1h, drying for standby;
2) preparation of polyamic acid (PPA)
A certain amount of aromatic series alkyldiamine (DAMI) is dissolved in equal benzene tetramethyl-dianhydride (PMDA), take Tetra hydro Phthalic anhydride as end-capping reagent, and preparation PAA massfraction is the solution of 20%, designs coated PI relative molecular mass 40000;
3) polyimide is coated
Use N, N ˊ-N,N-DIMETHYLACETAMIDE (DMAc) dilutes the PPA solution prepared, its viscosity is reduced, then according to the mass ratio 1:10 of PPA:CF, PPA and CF mixing is stirred evenly, desolventizing DMAc under vacuum, for preventing CF from reuniting in imidization, first remove excessive solvent in mixture, then hot imidization process 2h at 250 DEG C, obtain the CF being coated with PI, then use agitator to beat evenly;
4) PI the Molding Forming of Composites
Die press technology for forming is adopted to prepare 30%(massfraction) the TPI matrix material of CF, the CF mechanically mixing of PI powder is even, join in mould and be warmed up to 280 DEG C, apply pressure 10MPa, heat-insulation pressure keeping 1h; Then 340 DEG C are warming up to, pressurize 1h; Be cooled to 100 DEG C, namely the demoulding obtains matrix material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410326641.6A CN105295373A (en) | 2014-07-10 | 2014-07-10 | Preparation method for carbon fiber reinforced polyimide composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410326641.6A CN105295373A (en) | 2014-07-10 | 2014-07-10 | Preparation method for carbon fiber reinforced polyimide composite material |
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| CN105295373A true CN105295373A (en) | 2016-02-03 |
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| CN201410326641.6A Pending CN105295373A (en) | 2014-07-10 | 2014-07-10 | Preparation method for carbon fiber reinforced polyimide composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909477A (en) * | 2020-09-08 | 2020-11-10 | 山东东岳高分子材料有限公司 | High-performance carbon oxide fiber/graphite/polyimide modified polytetrafluoroethylene high-molecular composite material and preparation method thereof |
-
2014
- 2014-07-10 CN CN201410326641.6A patent/CN105295373A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 高鑫 等: "复合处理碳纤维增强聚酰亚胺复合材料力学性能", 《复合材料学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909477A (en) * | 2020-09-08 | 2020-11-10 | 山东东岳高分子材料有限公司 | High-performance carbon oxide fiber/graphite/polyimide modified polytetrafluoroethylene high-molecular composite material and preparation method thereof |
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Application publication date: 20160203 |
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