CN104723577A - Preparation method for carbon fibre fabric-reinforced polyetheretherketone polymer composite material - Google Patents
Preparation method for carbon fibre fabric-reinforced polyetheretherketone polymer composite material Download PDFInfo
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- CN104723577A CN104723577A CN201510111874.9A CN201510111874A CN104723577A CN 104723577 A CN104723577 A CN 104723577A CN 201510111874 A CN201510111874 A CN 201510111874A CN 104723577 A CN104723577 A CN 104723577A
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Abstract
The invention discloses a preparation method for a carbon fibre fabric-reinforced polyetheretherketone polymer composite material, and belongs to the technical field of composite material preparation. The preparation method comprises the following steps: carrying out slurry remover treatment on the surface of a carbon fibre fabric; dissolving polyarylsulfone powder in chloroform or N,N-dimethyl formamide to prepare polymer solution with a certain concentration, then adding polyetheretherketone ultrafine powder, and stirring to obtain a suspension; flatly paving the treated carbon fibre fabric in a cloth-type funnel, pouring the suspension on the carbon fibre fabric, and carrying out low-pressure suction filtration; melting, pressurizing and maintaining a pressure in a hot press; then cooling to a room temperature and demoulding. The preparation method disclosed by the invention solves the problems of high process control difficulty, too high equipment and energy consumption costs, poor adhesive property of polyetheretherketone and carbon fibres, and the like of the existing polyetheretherketone resin during a carbon fibre soaking process, so that preparation for the large fibre fabric-reinforced polyetheretherketone composite material is realized by using simple equipment and a simple and convenient process method.
Description
Technical field
The invention belongs to technical field prepared by fabric polymer matrix composites, be specifically related to a kind of preparation method of carbon fibre fabric reinforced polyether ether ketone composite.
Background technology
Fabric strengthens High Performance FRTP Composites and is used in the nearly all senior engineering structure of aircraft, helicopter, space shuttle, naval vessels, steamer, ocean platform, automobile, sports apparatus, bridge, building etc.The use amount that fabric strengthens High performance plastic resin composite constantly increases, and not only on traditional industry field, application is more and more, and also establishes its status on some emerging fields (as biomedicine).But the domestic report of the research about this respect is few.
The feature that carbon fiber is given prominence to is that high strength, high-modulus, low-density, its specific strength, specific modulus are far above steel alloy, aluminium alloy and titanium alloy.Also have that anti-fatigue performance is good simultaneously, abrasion performance and the feature such as lubricity excellence, good damping capacity, good energy-obsorbing and damping performance.And its profile has significant anisotropy, soft, various fabric can be processed into, continuous-filament woven fabric is compared short fiber and is had higher structural order and tight ness rating, therefore compare short fiber reinforced composite, fabric reinforced composite has more excellent specific strength, bearing capacity and wearability.
Polyether-ether-ketone (PEEK) is a kind of typical thermoplasticity high-performance polymer, and having high strength, high-modulus, high-fracture toughness and excellent dimensional stability, is the most outstanding in all plastics to the excellent fatigue durability of alternate stress.Because high-temperature resistant thermoplastic resin generally has good solvent resistant and oil resistivity, be insoluble to conventional organic solvent, at present mainly adopt hot melt dipping, but due to the melt viscosity of thermoplastic resin matrix larger.Sweat connecting is higher to equipment requirement, and technology and technique controlling difficulty greatly, make it apply and are very limited.Therefore, the biggest problem that the application expanding polyether-ether-ketone composite material faces is exactly solve resin matrix to the infiltration of fiber, and the adhesive power of resin and fortifying fibre is also the key factor determining its energy of playing superiority simultaneously.
At present, some patents disclose three-dimensional establishment carbon fiber/PEEK composite material and preparation method thereof (as Chinese patent 201110022682.2), its knitting skill difficulty is large, and Mechanical Properties of Products not high (bending strength 500-900MPa), simple, the easy and simple to handle development and requirement meeting multiple field of this method production equipment.
Summary of the invention
The object of this invention is to provide a kind of preparation method of carbon fibre fabric reinforced polyether ether ketone composite to solve polyether-ether-ketone resin matrix to the infiltration of fiber and adhesive power; And production equipment is simple, easy and simple to handle, be applicable to the preparation of large-scale fabric reinforced polyether ether ketone composite.
Carbon fibre fabric reinforced polyether ether ketone polymer composites of the present invention is the woven preformed member of carbon fiber through the carbon fiber mass fraction that with the addition of the polyarylsulfone (PAS) solution submergence suction filtration of polyether-ether-ketone superfine powder, hot repressing process obtains be the composite of 50% ~ 61.1%.
Technical scheme of the present invention is as follows.
A preparation method for carbon fibre fabric reinforced polyether ether ketone polymer composites, has following steps:
1) plain weave of angle of weave θ=90 °, twill 2D carbon fibre fabric (that is, the woven preformed member of carbon fiber) are soaked and heat ultrasonic 48 ~ 72 hours in acetone, then spend distilled water and clean, dry;
2) by polyarylsulfone (PAS) powder dissolution at chloroform or N, in dinethylformamide (DMF), the mass concentration of solution is made to be 2.2% ~ 3.2%, stir, after polyarylsulfone (PAS) powder fully dissolves, add polyether-ether-ketone (PEEK) powder, polyether-ether-ketone and carbon fiber mass ratio are 0.45 ~ 0.5: 0.5 ~ 0.55, and stirring makes it Homogeneous phase mixing and obtains suspension;
3) carbon fibre fabric handled well in step 1 is laid in cloth funnel, the suspension configured in step 2 is poured on carbon fibre fabric, low pressure suction filtration, solvent is volatilized completely;
4) carbon fibre fabric obtained in step 3 is placed in hot press, is warming up to 380 DEG C, melting 60min, is then forced into 15 ~ 20MPa, pressurize 30min; Room temperature is down to again with the speed of 20 ~ 30 DEG C/min.
Described polyarylsulfone (PAS), preferred, polyethers sulfone (PES) or biphenyl polyether ether sulfone (PPSU).
The kind of described carbon fiber comprises polyacrylonitrile-based carbon fibre, viscose-based carbon fiber or asphalt base carbon fiber.Carbon fiber bundle comprises 1K, 3K, 6K, 12K or 24K.
Described polyether-ether-ketone (PEEK) powder, order number is 100 ~ 600 orders, and melt index is 60 ~ 150g/10min.
Described low pressure suction filtration, can under vacuum is 0.01MPa suction filtration.
Compared with prior art, the invention solves existing polyether-ether-ketone resin some problems in infiltration carbon fiber process, such as technology and technique controlling difficulty be large, equipment and the problem such as energy consumption cost is too high, the adhesive property of polyether-ether-ketone and carbon fiber is bad.Obviously can find out that composite of the present invention has by the composite pattern electromicroscopic photograph prepared to infiltrate preferably and bond properties.The equipment that the present invention adopts is simple, process is easy, and the composite prepared has good mechanical property, and hot strength can reach 512MPa, bending strength can reach 940MPa.
Accompanying drawing explanation
Fig. 1 is the composite material surface pattern electromicroscopic photograph prepared in the process of the present invention.
Fig. 2 is the composite cross-section morphology electromicroscopic photograph prepared in the process of the present invention.
Detailed description of the invention
Different embodiments is obtained by change polyarylsulfone (PAS) solution concentration, carbon fiber content, hot pressing pressure.Polyether-ether-ketone (PEEK) superfine powder of the high fusion index described in embodiment, 100 ~ 600 orders, melt index are polyether-ether-ketone (PEEK) powder of 60 ~ 150g/10min exactly.
Embodiment 1:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Biphenyl polyether ether sulfone (PPSU) powder dissolution is configured to the polymer solution that mass concentration is 3.2% in appropriate chloroform, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after chloroform volatilization completely.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 15MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 50.2%, and its hot strength is 331MPa, and bending strength is 663MPa.
Embodiment 2:
The woven preformed member of twill 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Biphenyl polyether ether sulfone (PPSU) powder dissolution is configured to the polymer solution that mass concentration is 3.2% in appropriate chloroform, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after chloroform volatilization completely.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 15MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 50.2%, and its hot strength is 311MPa, and bending strength is 641MPa.
Embodiment 3:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Polyether sulfone (PES) powder dissolution is configured to the polymer solution that mass concentration is 3.2% in appropriate DMF, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after drying.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 15MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 50.0%, and its hot strength is 307MPa, and bending strength is 619MPa.
Embodiment 4:
The woven preformed member of twill 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Polyether sulfone (PES) powder dissolution is configured to the polymer solution that mass concentration is 3.2% in appropriate DMF, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after drying.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 15MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 50.0%, and its hot strength is 316MPa, and bending strength is 611MPa.
Embodiment 5:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Biphenyl polyether ether sulfone (PPSU) powder dissolution is configured to the polymer solution that mass concentration is 2.6% in appropriate chloroform, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after chloroform volatilization completely.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 18MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 51.9%, and its hot strength is 411MPa, and bending strength is 726MPa.
Embodiment 6:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Polyether sulfone (PES) powder dissolution is configured to the polymer solution that mass concentration is 2.6% in appropriate DMF, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after drying.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 18MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 52.1%, and its hot strength is 387MPa, and bending strength is 702MPa.
Embodiment 7:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Biphenyl polyether ether sulfone (PPSU) powder dissolution is configured to the polymer solution that mass concentration is 2.2% in appropriate chloroform, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.45: 0.55 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after chloroform volatilization completely.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 18MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 52.5%, and its hot strength is 423MPa, and bending strength is 733MPa.
Embodiment 8:
The woven preformed member of plain weave 2D carbon fiber of angle of weave θ=90 ° is soaked and heats ultrasonic 48 ~ 72 hours in acetone, removing carbon fiber surface sizing agent, then spend distilled water and clean, dry, weigh.Biphenyl polyether ether sulfone (PPSU) powder dissolution is configured to the polymer solution that mass concentration is 2.2% in appropriate chloroform, carbon fiber (CF) in mass ratio in the solution afterwards: the ratio of polyether-ether-ketone superfine powder (PEEK)=0.5: 0.5 adds polyether-ether-ketone (PEEK) superfine powder of high fusion index, abundant stirring, makes it Homogeneous phase mixing and obtains suspension.The carbon fibre fabric handled well is laid in cloth funnel, the suspension configured is poured on carbon fibre fabric, low pressure suction filtration, take out after chloroform volatilization completely.Be placed in hot press, be warming up to 380 DEG C, melting 60min, then pressurize 20MPa, pressurize 30min.Afterwards with the medium cooling rate cooling of 20 ~ 30 DEG C/min, after being cooled to room temperature, the demoulding obtains the composite that carbon fiber mass fraction is 61.1%, and its hot strength is 512MPa, and bending strength is 940MPa.
Claims (6)
1. a preparation method for carbon fibre fabric reinforced polyether ether ketone polymer composites, has following steps:
1) plain weave of angle of weave θ=90 °, twill 2D carbon fibre fabric are soaked and heat ultrasonic 48 ~ 72 hours in acetone, then spend distilled water and clean, dry;
2) by polyarylsulfone (PAS) powder dissolution at chloroform or N, in dinethylformamide, the mass concentration of solution is made to be 2.2% ~ 3.2%, stir, after polyarylsulfone (PAS) powder fully dissolves, add polyether-ether-ketone powder, polyether-ether-ketone and carbon fibre fabric mass ratio are 0.45 ~ 0.5: 0.5 ~ 0.55, stir and obtain suspension;
3) carbon fibre fabric handled well in step 1 is laid in cloth funnel, the suspension configured in step 2 is poured on carbon fibre fabric, low pressure suction filtration, solvent is volatilized completely;
4) carbon fibre fabric obtained in step 3 is placed in hot press, is warming up to 380 DEG C, melting 60min, is then forced into 15 ~ 20MPa, pressurize 30min; Room temperature is down to again with the speed of 20 ~ 30 DEG C/min.
2. the preparation method of carbon fibre fabric reinforced polyether ether ketone polymer composites according to claim 1, is characterized in that, described polyarylsulfone (PAS), is polyether sulfone or biphenyl polyether ether sulfone.
3. the preparation method of carbon fibre fabric reinforced polyether ether ketone polymer composites according to claim 1, is characterized in that, described carbon fibre fabric, is polyacrylonitrile-based carbon fibre, viscose-based carbon fiber or asphalt base carbon fiber.
4. the preparation method of carbon fibre fabric reinforced polyether ether ketone polymer composites according to claim 1, is characterized in that, described polyether-ether-ketone powder, and order number is 100 ~ 600 orders, and melt index is 60 ~ 150g/10min.
5. the preparation method of the carbon fibre fabric reinforced polyether ether ketone polymer composites according to claim 1,2 or 3, is characterized in that, described low pressure suction filtration is suction filtration under vacuum is 0.01MPa.
6. the preparation method of the carbon fibre fabric reinforced polyether ether ketone polymer composites according to claim 1 or 3, is characterized in that described carbon fibre fabric is 1K, 3K, 6K, 12K or 24K.
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| CN105538577A (en) * | 2015-12-21 | 2016-05-04 | 华中科技大学 | Hot press molding device for carbon fiber enhanced polyether-ether-ketone (PEEK) composite material and technological method thereof |
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| CN107237002A (en) * | 2017-06-08 | 2017-10-10 | 广东银禧科技股份有限公司 | A kind of polyether-ether-ketone/chopped fiber composite wire material and preparation method thereof |
| CN111732815A (en) * | 2020-07-13 | 2020-10-02 | 扬州市维纳复合材料科技有限公司 | Preparation method of functional polyether-ether-ketone carbon fiber composite material |
| CN115850741A (en) * | 2023-02-23 | 2023-03-28 | 中国人民解放军军事科学院系统工程研究院 | Carbon fiber reinforced composite material and preparation method thereof |
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Application publication date: 20150624 |