CN103602039B - Preparation method of carbon fiber reinforced polyether ether ketone composite material - Google Patents
Preparation method of carbon fiber reinforced polyether ether ketone composite material Download PDFInfo
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- CN103602039B CN103602039B CN201310570942.9A CN201310570942A CN103602039B CN 103602039 B CN103602039 B CN 103602039B CN 201310570942 A CN201310570942 A CN 201310570942A CN 103602039 B CN103602039 B CN 103602039B
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Abstract
The invention discloses a preparation method of a carbon fiber reinforced polyether ether ketone composite material. The method disclosed by the invention comprises: weaving carbon fibers to a 2D (Two-Dimensional) woven plain or twill preform, then, soaking the woven preform in acetone for 48 hours, ultrasonically treating the preform for 20 minutes through a mixed acid of sulfuric acid and nitric acid, cleaning the preform through deionized water and drying the preform; dissolving diphenyl sulfone in a proper amount of acetone, then adding polyether ether ketone powder, evaporating out the acetone and drying the powder to obtain a polyether ether ketone/diphenyl sulfone mixture; weighing a proper amount of mixture, carrying out hot pressing on the mixture to obtain a pure thin polyether ether ketone rein slice at a temperature of 390 DEG C and at a pressure of 3-4 MPa; alternatively paving the dry preform and the thin polyether ether ketone rein slice in a mold according to such a proportion that the carbon fiber volume fraction is 30-70%, heating up to 380-390 DEG C at a speed of 10-15 DEG C/min, preserving heat for 30 minutes, then, pressurizing to 2-3 MPa, and preserving heat for 30 minutes; and cooling a product in the mold at a moderate cooling speed of 10-15 DEG C/min, meanwhile, pressurizing to 4-5 MPa, further maintaining the pressure for 3 hours, and demolding to obtain a woven carbon fiber/polyether ether ketone composite material.
Description
Technical field
The present invention relates to a kind of preparation method of 2D carbon fiber reinforced polyetheretherketonecomposite composite material.
Technical background
Metallic anchors tool has high strength because of it, can provide the multiple advantages such as Initial stability for fracture, has been widely used in clinical.But the histocompatibility that metal inside-fixture is lower reduces its mechanical stability in bone; Metal material shielding ray causes many critical defects such as checking visual field disappearance.
Carbon fiber is higher by carbon content, has the characteristic of general carbon materials, as high temperature resistant, antifriction scrape along is corrosion-resistant, simultaneously its profile has significant anisotropy, softness, can be processed into various fabric, shows very high intensity along fibre axis direction.Carbon fiber combines with its excellent histocompatibility, firmly fibre substrate and higher anti-compression properties becomes the most frequently used reinforcement material.PEEK is a kind of novel semi-crystalline state, its dimensional stability is better, coefficient of linear expansion is little, resistance to chemical attack, capability of resistance to radiation is strong, good toughness, resistance to fatigue outstanding, rub resistance, the super heat-resisting thermoplastic resin of fragrant family of resistance to skimming wear and Fretting excellence.Recent research finds, the Young's modulus of this material, between cortex bone and spongy bone, can produce fine motion, reduces stress shielding, promotes knitting.Weaving carbon fiber/polyether-ether-ketone composite material is a kind of material being suitable for exter-nal fixer.Application number be 200910051159.5 application for a patent for invention disclose the matrix material injection molding forming method of a kind of short carbon fiber reinforced PEEK, but PEEK resin viscosity is high, wash machine difficulty is required large, its mould and die preheating complex procedures, and short fiber product strength not high (flexural strength 400 ~ 800MPa), application aspect can limit to some extent.Open 3 D weaving carbon fiber/PEEK the composite material and preparation method thereof of some patents at present, but three dimensional weaving technique difficulty is large, and PEEK fiber is generally import, and cost is high, Mechanical Properties of Products not high (500 ~ 1100MPa).Present method adopts hot press moulding method, and its technique is simple, the processing of complex body shape is flexible, product strength high (flexural strength can reach 1783MPa), can be used widely in aviation, industry, building, medical field and develop.
Summary of the invention
The object of this invention is to provide a kind of preparation method of carbon fiber reinforced polyetheretherketonecomposite composite material.
The method of the present invention comprises the following steps:
(1) 2D woven plain weave or twill preformed member, by carbon fiber textile is become, angle of weave θ=90 °; Then, after woven preformed member being soaked 48 hours in acetone, with ultrasonic 20 minutes of nitration mixture (sulfuric acid: nitric acid=3:2), then post-drying is cleaned with deionized water;
(2), sulfobenzide (DPS) is dissolved in proper amount of acetone, stir, after sulfobenzide (DPS) fully dissolves, 80% ratio adds polyether-ether-ketone (PEEK) powder by weight percentage, abundant stirring, after steaming acetone, powder is dried, and obtains polyether-ether-ketone/sulfobenzide (PEEK/DPS) mixture; Weigh up appropriate mixture, with 390 DEG C, pressure 3 ~ 4MPa is hot pressed into pure polyether-ether-ketone resin thin slice, sulfobenzide (DPS) distillation in hot pressing;
(3) be, the ratio of 30% ~ 70% in carbon fiber volume fraction, polyether-ether-ketone (PEEK) resin flake prepared by the dry preformed member obtain step (1) and step (2) is alternately laid in mould, 380 DEG C ~ 390 DEG C are raised to the heat-up rate of 10 ~ 15 DEG C/min, stop 30min, then pressurize 2 ~ 3MPa, insulation 30min.
(4) goods in the mould of step (3) are lowered the temperature with the medium cooling rate of 10 ~ 15 DEG C/min, pressure is mentioned 4 ~ 5MPa simultaneously, continue pressurize 3h, obtain weaving carbon fiber/polyether-ether-ketone (CF/PEEK) matrix material through demoulding process.
Described carbon fiber is PAN-based carbon fiber.
The model of described carbon fiber is T300.
Described carbon fiber bundle comprises 1K, 3K, 6K, 12K and 24K.
Described polyether-ether-ketone (PEEK) is powder or particle.
Beneficial effect of the present invention:
1, the method technique of the present invention is simple, the processing of complex body shape is flexible, product strength high (flexural strength can reach 1783MPa), can be used widely in aviation, industry, building, medical field and develop.
2, use under the carbon fiber reinforced polyetheretherketonecomposite composite material that the present invention produces is suitable for high loading, long lifetime and severe condition
3, the present invention's carbon fiber reinforced polyetheretherketonecomposite composite material intensity of producing is high, and Young's modulus is low, and having can X-ray thoroughly, and histocompatibility better, can alternative metals material be applied to clinical, fix by the interface of strengthening in bone.
4, the impregnation difficulties problem that the viscosity effectively overcoming polyether-ether-ketone (PEEK) is brought greatly, the hot press forming technology condition of carbon fiber knit preformed member and uniqueness is adopted to improve composite materials property, goods flexural strength can reach 1783MPa, decomposition temperature reaches 578 DEG C, has excellent mechanical property and thermal stability.
Accompanying drawing explanation
Fig. 1 is carbon fibre fabric preformed member after soaking 48 hours in acetone, with nitration mixture (sulfuric acid: nitric acid=3:2) carbon fiber surface etching degree electromicroscopic photograph after ultrasonic 20 minutes.
The morphology of the fracture surface electromicroscopic photograph of the CF/PEEK matrix material that Fig. 2 is carbon fiber volume fraction to be prepared when being 60% in the process of the present invention.
Embodiment
Embodiment 1:
Carbon fiber textile is become 2D woven plain weave preformed member, angle of weave θ=90 °, after then woven preformed member being soaked 48 hours in acetone, with nitration mixture: (sulfuric acid: nitric acid=3:2) ultrasonic 20 minutes, its microgram looks as shown in Figure 1, then clean post-drying with deionized water.Sulfobenzide (DPS) is dissolved in proper amount of acetone, stirs, after sulfobenzide (DPS) fully dissolves, polyether-ether-ketone (PEEK) powder is added by 80% mass ratio, abundant stirring, after steaming acetone, powder is dried, and obtains polyether-ether-ketone/sulfobenzide (PEEK/DPS) mixture.Weigh up appropriate mixture, with 390 DEG C, pressure 3MPa is hot pressed into pure polyether-ether-ketone resin thin slice, sulfobenzide (DPS) distillation in hot pressing.By carbon fiber (CF) volume fraction 45%, polyether-ether-ketone (PEEK) volume fraction is 65%, polyether-ether-ketone (PEEK) resin flake of the dry preformed member obtained and preparation is alternately laid in mould, 380 DEG C are raised to the heat-up rate of 10 DEG C/min, stop 30min, then pressurize 2MPa, insulation 30min.By goods in mould with the medium cooling rate cooling of 10 DEG C/min, pressure is mentioned 5MPa simultaneously, continue pressurize 3h, obtain V through demoulding process
cFbe carbon fiber/polyetheretherketonecomposite (CF/PEEK) matrix material of 45%, this goods flexural strength can reach 789MPa, tensile strength 165MPa.
Embodiment 2:
Carbon fiber textile is become 2D woven plain weave preformed member, angle of weave θ=90 °, after then woven preformed member being soaked 48 hours in acetone, with ultrasonic 20 minutes of nitration mixture (sulfuric acid: nitric acid=3:2), then clean post-drying with deionized water.Sulfobenzide (DPS) is dissolved in proper amount of acetone, stirs, after sulfobenzide (DPS) fully dissolves, polyether-ether-ketone (PEEK) powder is added by 80% mass ratio, abundant stirring, after steaming acetone, powder is dried, and obtains polyether-ether-ketone/sulfobenzide (PEEK/DPS) mixture.Weigh up appropriate mixture, with 390 DEG C, pressure 4MPa is hot pressed into pure polyether-ether-ketone (PEEK) resin flake, sulfobenzide distillation in hot pressing.Be 40% by carbon fiber (CF) volume fraction 60% polyether-ether-ketone (PEEK) volume fraction, polyether-ether-ketone (PEEK) resin flake of the dry preformed member obtained and preparation is alternately laid in mould, 385 DEG C are raised to the heat-up rate of 15 DEG C/min, stop 30min, then pressurize 2.5MPa, insulation 30min.By goods in mould with the medium cooling rate cooling of 15 DEG C/min, pressure is mentioned 4.5MPa simultaneously, continue pressurize 3h, obtain V through demoulding process
cFbe carbon fiber/polyetheretherketonecomposite (CF/PEEK) matrix material of 60%, this goods flexural strength can reach 1783MPa, tensile strength 291MPa.
Embodiment 3:
Carbon fiber textile is become 2D woven plain weave preformed member, angle of weave θ=90 °, after then woven preformed member being soaked 48 hours in acetone, with ultrasonic 20 minutes of nitration mixture (sulfuric acid: nitric acid=3:2), then clean post-drying with deionized water.Sulfobenzide (DPS) is dissolved in proper amount of acetone, stirs, after sulfobenzide (DPS) fully dissolves, polyether-ether-ketone (PEEK) powder is added by 80% mass ratio, abundant stirring, after steaming acetone, powder is dried, and obtains polyether-ether-ketone/sulfobenzide (PEEK/DPS) mixture.Weigh up appropriate mixture, with 390 DEG C, pressure 4MPa is hot pressed into pure polyether-ether-ketone (PEEK) resin flake, sulfobenzide distillation in process.By carbon fiber (CF) volume fraction 70%, polyether-ether-ketone (PEEK) volume fraction is 30%, polyether-ether-ketone (PEEK) resin flake of the dry preformed member obtained and preparation is alternately laid in mould, 390 DEG C are raised to the heat-up rate of 10 DEG C/min, stop 30min, then pressurize 3MPa, insulation 30min.By goods in mould with the medium cooling rate cooling of 15 DEG C/min, pressure is mentioned 5MPa simultaneously, continue pressurize 3h, obtain V through demoulding process
cFbe carbon fiber/polyetheretherketonecomposite (CF/PEEK) matrix material of 70%, this matrix material flexural strength can reach 1164MPa, tensile strength 216MPa.
V
cFrepresent the volume shared by carbon fiber.
The microscopic pattern of carbon fiber/polyetheretherketonecomposite (CF/PEEK) matrix material as shown in Figure 2.
Claims (3)
1. a preparation method for carbon fiber reinforced polyetheretherketonecomposite composite material, the method comprises the following steps:
(1) 2D woven plain weave or twill preformed member, by carbon fiber textile is become, angle of weave θ=90 °; Then after woven preformed member being soaked 48 hours in acetone, with nitration mixture ultrasonic 20 minutes, then clean post-drying with deionized water; Described nitration mixture is the mixture of sulfuric acid and nitric acid, sulfuric acid: nitric acid=3:2;
(2), by sulfobenzide be dissolved in proper amount of acetone, stir, after sulfobenzide fully dissolves, 80% ratio adds polyether-ether-ketone powder by weight percentage, fully stirs, and after steaming acetone, powder is dried, and obtains polyether-ether-ketone/sulfobenzide mixture; Weigh up appropriate mixture, with 390 DEG C, pressure 3 ~ 4MPa is hot pressed into pure polyether-ether-ketone resin thin slice, sulfobenzide distillation in hot pressing;
(3) be, the ratio of 30% ~ 70% in carbon fiber volume fraction, polyether-ether-ketone resin thin slice prepared by the dry preformed member obtain step (1) and step (2) is alternately laid in mould, 380 DEG C ~ 390 DEG C are raised to the heat-up rate of 10 ~ 15 DEG C/min, stop 30min, then pressurize 2 ~ 3MPa, insulation 30min;
(4) goods in the mould of step (3) are lowered the temperature with the medium cooling rate of 10 ~ 15 DEG C/min, pressure is mentioned 4 ~ 5MPa simultaneously, continue pressurize 3h, obtain weaving carbon fiber/polyether-ether-ketone composite material through demoulding process.
2. the preparation method of a kind of carbon fiber reinforced polyetheretherketonecomposite composite material according to claim 1, is characterized in that: described carbon fiber is PAN-based carbon fiber.
3. the preparation method of a kind of carbon fiber reinforced polyetheretherketonecomposite composite material according to claim 1 and 2, is characterized in that: the model of described carbon fiber is T300.
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| CN105315649A (en) * | 2014-07-10 | 2016-02-10 | 黑龙江鑫达企业集团有限公司 | Preparation method of PEEK composite material with high tensile strength |
| CN105538577B (en) * | 2015-12-21 | 2016-11-16 | 华中科技大学 | A kind of carbon fiber reinforced polyetheretherketonecomposite composite material hot-press molding method |
| CN106221123A (en) * | 2016-08-08 | 2016-12-14 | 陆志强 | A kind of vehicle frame carbon fiber/polyetheretherketonecomposite composite material and preparation method thereof |
| CN108995335A (en) * | 2017-06-07 | 2018-12-14 | 桂林市庆通有色金属工艺材料开发有限公司 | A kind of carbon fibre fabric reinforced polyether ether ketone base aviation composite and preparation method thereof |
| CN108250671A (en) * | 2018-01-09 | 2018-07-06 | 南京航空航天大学 | A kind of cenosphere reinforced polyether ether ketone wearing composite material and preparation method thereof |
| CN109705525A (en) * | 2019-01-07 | 2019-05-03 | 南京航空航天大学 | A kind of modified carbon fiber reinforced polyether ether ketone polymer matrix composites and preparation method thereof |
| CN110201224A (en) * | 2019-05-24 | 2019-09-06 | 山西医科大学第一医院 | A kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite and preparation method thereof |
| CN110732837A (en) * | 2019-08-21 | 2020-01-31 | 扬中市三利石化机械有限公司 | Centrifugal machine shaft end labyrinth seal transformation process |
| CN110774699A (en) * | 2019-11-04 | 2020-02-11 | 江苏澳盛复合材料科技有限公司 | Sandwich-structured carbon fiber composite material and preparation method thereof |
| CN112519070A (en) * | 2020-11-23 | 2021-03-19 | 太仓市磁力驱动泵有限公司 | Carbon fiber cloth composite polyether-ether-ketone separation sleeve |
| CN113288385A (en) * | 2021-05-17 | 2021-08-24 | 济南大学 | Method for preparing bionic lumbar pedicle screw by continuous carbon fibers |
| CN115071166B (en) * | 2022-08-04 | 2023-05-30 | 中复神鹰(上海)科技有限公司 | Modified continuous carbon fiber reinforced polyether-ether-ketone composite material laminated plate and preparation method thereof |
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| GB0322598D0 (en) * | 2003-09-26 | 2003-10-29 | Victrex Mfg Ltd | Polymeric material |
| CN1267158C (en) * | 2004-06-24 | 2006-08-02 | 上海交通大学 | Polyetheretherketone total hip femoral head prosthesis material and preparation method thereof |
| CN101220196B (en) * | 2008-01-22 | 2010-08-11 | 南京肯特复合材料有限公司 | Poly(ether-ether-ketone) composite material, production method and application of sealing member |
| CN101555342A (en) * | 2009-05-14 | 2009-10-14 | 上海第二工业大学 | Preparation method of carbon fiber/polyetheretherketone composite material |
| CN102167884A (en) * | 2011-01-19 | 2011-08-31 | 天津大学 | Preparation method of three-dimensional woven carbon fiber reinforced polyetheretherketone composite material |
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