CN104191753A - Method for preparing continuous carbon fiber enhanced polyether-ether-ketone matrix fiber metal laminates - Google Patents
Method for preparing continuous carbon fiber enhanced polyether-ether-ketone matrix fiber metal laminates Download PDFInfo
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- CN104191753A CN104191753A CN201410426655.5A CN201410426655A CN104191753A CN 104191753 A CN104191753 A CN 104191753A CN 201410426655 A CN201410426655 A CN 201410426655A CN 104191753 A CN104191753 A CN 104191753A
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Abstract
The invention discloses a method for preparing continuous carbon fiber enhanced polyether-ether-ketone matrix fiber metal laminates and belongs to the field of preparation of composite materials. The method comprises the following steps: by utilizing continuous carbon fibers and a modified polyether-ether-ketone resin solution, preparing a continuous carbon fiber enhanced polyether-ether-ketone prepreg; sequentially performing degreasing treatment, acid pickling and anodic oxidation treatment on metal plates; alternatively laying the treated metal plates and the continuous carbon fiber enhanced polyether-ether-ketone prepreg, performing hot-press curing and forming on the metal plates and the prepreg in a mold, and naturally cooling, thereby obtaining the carbon fiber enhanced polyether-ether-ketone matrix fiber metal laminates. The fiber metal laminates prepared by the invention have the advantages of high toughness, high strength, difficulty in processing, environmental friendliness and no pollution.
Description
Technical field
The preparation method of Fiber Reinforced Metal Laminates of the present invention, is specifically a kind of preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal, belongs to composite preparation field.
Background technology
Fiber Reinforced Metal Laminates (Fiber Metal Laminates, FMLs), it is the material for the exploitation of the high fatigue crack of civil aircraft district in early days, it is to be replaced after laying by fibrous composite and sheet metal, under certain temperature, pressure, solidify a kind of interlayer hybrid composite forming after a period of time, therefore be also called the super laminate (Super Hybrid Laminates) that mixes.
The FMLs applying in Aero-Space is at present generally thermosetting composite layered plate, exists poor toughness, is not easy many defects such as shaping, thereby hindered the application of this type of material in typical products in mass production manufacture process.Foreign scholar research shows, thermoplasticity FMLs has good toughness, is easily shaped and can recycles, and forming technology is simple, can be used for the manufacture of typical products in mass production.
Continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal is the composite layered plate of new generation with more excellent combination property.In this type of Fiber Reinforced Metal Laminates, resin matrix polyether-ether-ketone (PEEK) is a kind of hemicrystalline aromatic thermoplastic engineering plastics, there is high temperature resistant, resistance to chemical attack, high strength, high-fracture toughness, the easy feature such as the excellent properties such as processing and linear expansion coefficient is less, self is fire-retardant, wearability is high, insulation, hydrolysis, being more satisfactory engineering material, is also the study hotspot in current thermoplastic composite field.Fortifying fibre carbon fiber strength is large, and modulus is high, lightweight, high temperature resistant, and chemical stability is good, can guarantee that thermoplastic composite has higher fracture toughness, and meanwhile, when there is layering, carbon fiber can play the effect at bridge joint interface, slows down the expansion of crackle.
On March 27th, 2013, Chinese invention patent application CN102991009A discloses a kind of carbon fiber-metal laminate of interlayer toughened, it selects the thermoplastic nylon nonwoven with high porosity as interlayer toughened/separation layer, make resin matrix can infiltration occur smoothly in toughness reinforcing/separation layer and infiltrate in hot-forming process, but toughness reinforcing/separation layer and matrix resin do not occur to dissolve and phase-splitting, have still kept complete nonwoven fabric construct form.And then, by nylon nonwoven fabrics and matrix resin, mutually run through and form the non-reaction induced three-dimensional net structure being separated, play the effect of interlayer toughened, cut off contacting between carbon fiber reinforcement and plymetal simultaneously, play electrochemistry iris action, eliminated between carbon fiber reinforcement and plymetal the electrochemical corrosion problem that the existence due to potential difference causes.But the fusing point of the thermoplastic nylon nonwoven that this patent of invention is selected is 200 ℃ of left and right, fusing point is lower has limited its application under higher temperature.
Summary of the invention
Technical problem to be solved by this invention is to overcome prior art defect, provides that a kind of resistance to elevated temperatures is good, intensity is high and the preparation method of the continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal of easy processing.
In order to solve the problems of the technologies described above, the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal provided by the invention, comprises the following steps:
1), utilize continuous carbon fibre and modified polyetheretherketonefiber resin solution, prepare continuous carbon fibre reinforced polyether ether ketone prepreg;
2), successively metallic plate is carried out to ungrease treatment, pickling and anodized;
3), by step 2) metallic plate and the step 1 handled well) the continuous carbon fibre reinforced polyether ether ketone prepreg for preparing replaces laying and inserts in mould;
4), by step 3) mould carry out after hot-press solidifying shaping, the naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
In the present invention, described step 1) preparation process is: the speed of service dipping modified polyetheretherketonefiber resin solution by continuous carbon fibre with 15-25m/min, then be evenly arranged on roller, making carbon fiber volume content is the continuous carbon fibre reinforced polyether ether ketone prepreg of 40%-60%.
In the present invention, described step 2) organic solvent that in, ungrease treatment adopts is acetone or isopropyl alcohol.
In the present invention, described step 2) pickle that pickling adopts is the mixed acid solution that 350g/L nitric acid and 60g/L hydrofluoric acid are made into, and pickling temperature is 40
oc, pickling duration 40s.
In the present invention, described step 2) anode oxidation process is: using metallic plate as anode, corrosion resistant plate, as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, imposes 10-20V voltage oxidation 10-20min in the electrolyte that 6g/L sodium metasilicate forms.
In the present invention, described step 3) brushing primer between metallic plate and continuous carbon fibre reinforced polyether ether ketone prepreg in.
In the present invention, described primer is modified polyetheretherketonefiber chloroformic solution, and described modified polyetheretherketonefiber chloroformic solution proportioning is that 105g polyether-ether-ketone powder is dissolved in 1L chloroform.
In the present invention, the carbon fiber arragement direction in described step 3) in metallic plate rolling direction and continuous carbon fibre reinforced polyether ether ketone prepreg can be 0 °, ± 45 ° or 90 °.
In the present invention, the hot pressing solid process in described step 4) is: first by mold heated to 240 ℃, insulation 1h; Subsequently mould is warming up to 370 ℃, is incubated 1h and applies 4-5MPa pressure.
In the present invention, described metallic plate is TA1, TA2, TA18 or TC4, and thickness is 0.1-0.5mm.
Beneficial effect of the present invention is: (1), the present invention combine the metal of lightweight and high-intensity carbon fiber reinforced polyether-ether-ketone prepreg, it not only has the feature that metal easily connects processing, the characteristic also with carbon fiber reinforced polyether-ether-ketone high-strength light, lower with Metal Phase specific density, to compare toughness better with carbon fibre composite, intensity is high, and elastic modelling quantity is high, has excellent heat-resisting quantity; (2), step of the present invention is simple, convenient operation, production cost is low, environment friendly and pollution-free.
Accompanying drawing explanation
Fig. 1 is preparation method's flow chart of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal of the present invention;
Fig. 2 is laying structure chart in embodiment 1.
In figure: 1-patrix, 2-counterdie, 3-sheet metal, 4-prepreg.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
embodiment 1
As shown in Figure 1, the continuous carbon fibre reinforced polyether ether ketone Fiber Reinforced Metal Laminates that embodiment 1 is a kind of five-layer structure, it consists of the thick TA2 titanium plate of three layers of 0.3mm 3, two layers of continuous carbon fibre reinforced polyether ether ketone prepreg 4.
Concrete preparation method is as follows:
The first step, at room temperature continuous carbon fibre is with the speed dipping of 15m/min by modified polyetheretherketonefiber chloroformic solution, and being then evenly arranged in and on roller, making carbon fiber volume content is 50% unidirectional pre-immersion material.
Second step, to 3 surface washings of TA2 titanium plate, removes surface contaminant with distilled water; Then use acetone wiping TA2 thin plate 3 surfaces, remove surperficial grease; Again TA2 titanium plate 3 is put into the mixed acid solution being comprised of the nitric acid of 350g/L and the hydrofluoric acid of 60g/L, 40
ounder C, pickling 40s, removes surface oxide layer; Finally TA2 titanium plate 3 is put into electrolytic cell and carry out anodic oxidation, using TA2 titanium plate 3 as anode, corrosion resistant plate is as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, imposes 10V voltage oxidation 15min in the electrolyte that 6g/L sodium metasilicate forms, make TA2 titanium plate 3 surfaces obtain the oxide-film of one deck even compact.
The 3rd step, the proportioning of usining is dissolved in modified polyetheretherketonefiber chloroformic solution in 1L chloroform as primer TA2 titanium plate 3 surfaces that evenly brushing obtains after second step as 105g polyether-ether-ketone powder, and TA2 titanium plate 3 and carbon fiber reinforced polyether-ether-ketone prepreg are pressed to the sequence alternate laying shown in Fig. 1, wherein the rolling direction angle of the carbon fiber direction in carbon fiber reinforced polyether-ether-ketone prepreg 4 and TA2 titanium plate 3 is 0 °, after laying by patrix 1 and counterdie 2 matched moulds;
The 4th step, mould is placed on hot press, by mold heated to 240 ℃, insulation 1h, again mould is warming up to subsequently to 370 ℃, is incubated 1h and applies 5MPa pressure and make polyether-ether-ketone produce crosslinking curing, the then naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
embodiment 2
The present embodiment is a kind of continuous carbon fibre reinforced polyether ether ketone Fiber Reinforced Metal Laminates of three-decker, and it consists of two layers of thick TA1 titanium plate 3, one deck continuous carbon fibre reinforced polyether ether ketone prepreg 4 of 0.1mm.
Concrete preparation method is as follows:
The first step, at room temperature continuous carbon fibre is with the speed dipping of 18m/min by modified polyetheretherketonefiber powder chloroformic solution, and being then evenly arranged in and on roller, making carbon fiber volume content is 60% unidirectional pre-immersion material.
Second step, to 3 surface washings of TA1 titanium plate, removes surface contaminant with distilled water; Then use isopropyl alcohol TA1 titanium plate 3 surfaces, remove surperficial grease; Again TA1 titanium plate 3 is put into the mixed acid solution being comprised of the nitric acid of 350g/L and the hydrofluoric acid of 60g/L, 40
ounder C, pickling 40s, removes surface oxide layer; Finally TA1 titanium plate 3 is put into electrolytic cell and carry out anodic oxidation, using TA1 titanium plate 3 as anode, corrosion resistant plate is as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, imposes 15V voltage oxidation 20min in the electrolyte that 6g/L sodium metasilicate forms, make TA1 titanium plate 3 surfaces obtain the oxide-film of one deck even compact.
The 3rd step, the proportioning of usining is dissolved in modified polyetheretherketonefiber chloroformic solution in 1L chloroform as primer TA1 titanium plate 3 surfaces that evenly brushing obtains after second step as 105g polyether-ether-ketone powder, and TA1 titanium plate 3 and carbon fiber reinforced polyether-ether-ketone prepreg 4 are pressed to the sequence alternate laying shown in Fig. 1, wherein the carbon fiber direction in carbon fiber reinforced polyether-ether-ketone prepreg 4 and TA1 titanium plate 3 rolling direction angles are 90 °, after laying by patrix 1 and counterdie 2 matched moulds;
The 4th step, mould is placed on hot press, by mold heated to 240 ℃, insulation 1h, again mould is warming up to subsequently to 370 ℃, is incubated 1h and applies 4.5MPa pressure and make polyether-ether-ketone produce crosslinking curing, the then naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
embodiment 3
The present embodiment is a kind of continuous carbon fibre reinforced polyether ether ketone Fiber Reinforced Metal Laminates of five-layer structure, and it consists of the thick TC4 titanium plate of three layers of 0.5mm 3, two layers of continuous carbon fibre reinforced polyether ether ketone prepreg.
The first step, the preparation of prepreg: at room temperature continuous carbon fibre is with the speed dipping of 20m/min by modified polyetheretherketonefiber chloroformic solution, and being then evenly arranged in and making carbon fiber volume content on roller is 60% unidirectional pre-immersion material.
Second step, sheet metal pretreatment: to 3 surface washings of TC4 titanium plate, remove surface contaminant with distilled water; Then use acetone wiping titanium plate surface, remove surperficial grease; Again TC4 titanium plate 3 is put into the mixed acid solution being comprised of the nitric acid of 350g/L and the hydrofluoric acid of 60g/L, 40
ounder C, pickling 40s, removes surface oxide layer; Finally TC4 titanium plate 3 is put into electrolytic cell and carry out anodic oxidation, using TC4 titanium plate 3 as anode, corrosion resistant plate is as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, imposes 20V voltage oxidation 10min in the electrolyte that 6g/L sodium metasilicate forms, make TC4 titanium plate 3 surfaces obtain the oxide-film of one deck even compact.
The 3rd step, the proportioning of usining is dissolved in modified polyetheretherketonefiber chloroformic solution in 1L chloroform as primer TC4 titanium plate 3 surfaces that evenly brushing obtains after second step as 105g polyether-ether-ketone powder, and TC4 titanium plate 3 and carbon fiber reinforced polyether-ether-ketone prepreg 4 are replaced to laying as shown in Figure 1, wherein the carbon fiber direction in carbon fiber reinforced polyether-ether-ketone prepreg 4 and TA1 titanium plate 3 rolling direction angles are 90 °, after laying by patrix 1 and counterdie 2 matched moulds;
The 4th step, mould is placed on hot press, by mold heated to 240 ℃, insulation 1h, again mould is warming up to subsequently to 370 ℃, is incubated 1h and applies 4MPa pressure and make polyether-ether-ketone produce crosslinking curing, the then naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
embodiment 4
The present embodiment is a kind of continuous carbon fibre reinforced polyether ether ketone Fiber Reinforced Metal Laminates of three-decker, and it consists of two layers of thick TA18 titanium plate 3, one deck continuous carbon fibre reinforced polyether ether ketone prepreg 4 of 0.25mm.
Concrete preparation method is as follows:
The first step, at room temperature continuous carbon fibre is with the speed dipping of 25m/min by modified polyetheretherketonefiber powder chloroformic solution, and being then evenly arranged in and on roller, making carbon fiber volume content is 40% unidirectional pre-immersion material.
Second step, to 3 surface washings of TA18 titanium plate, removes surface contaminant with distilled water; Then use acetone wiping TA1 titanium plate 3 surfaces, remove surperficial grease; Again TA18 titanium plate 3 is put into the mixed acid solution being comprised of the nitric acid of 350g/L and the hydrofluoric acid of 60g/L, 40
ounder C, pickling 40s, removes surface oxide layer; Finally TA1 titanium plate 3 is put into electrolytic cell and carry out anodic oxidation, using TA18 titanium plate 3 as anode, corrosion resistant plate is as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, imposes 15V voltage oxidation 15min in the electrolyte that 6g/L sodium metasilicate forms, make TA18 titanium plate 3 surfaces obtain the oxide-film of one deck even compact.
The 3rd step, the proportioning of usining is dissolved in modified polyetheretherketonefiber chloroformic solution in 1L chloroform as primer TA18 titanium plate 3 surfaces that evenly brushing obtains after second step as 105g polyether-ether-ketone powder, and TA18 titanium plate 3 and carbon fiber reinforced polyether-ether-ketone prepreg 4 are pressed to the sequence alternate laying shown in Fig. 1, wherein the carbon fiber direction in carbon fiber reinforced polyether-ether-ketone prepreg 4 and TA18 titanium plate 3 rolling direction angles are 45 °, after laying by patrix 1 and counterdie 2 matched moulds;
The 4th step, mould is placed on hot press, by mold heated to 240 ℃, insulation 1h, again mould is warming up to subsequently to 370 ℃, is incubated 1h and applies 4.3MPa pressure and make polyether-ether-ketone produce crosslinking curing, the then naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make some improvement under the premise without departing from the principles of the invention, and these improvement also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal, is characterized in that comprising the following steps:
1), utilize continuous carbon fibre and modified polyetheretherketonefiber resin solution, prepare continuous carbon fibre reinforced polyether ether ketone prepreg;
2), successively metallic plate is carried out to ungrease treatment, pickling and anodized;
3), by step 2) metallic plate and the step 1 handled well) the continuous carbon fibre reinforced polyether ether ketone prepreg for preparing replaces laying and inserts in mould;
4), by step 3) mould carry out after hot-press solidifying shaping, the naturally cooling carbon fiber reinforced polyether-ether-ketone Fiber Reinforced Metal Laminates that obtains.
2. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 1, it is characterized in that described step 1) preparation process is: the speed of service dipping modified polyetheretherketonefiber resin solution by continuous carbon fibre with 15-25m/min, then be evenly arranged on roller, making carbon fiber volume content is the continuous carbon fibre reinforced polyether ether ketone prepreg of 40%-60%.
3. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 1, is characterized in that: the organic solvent that described step 2), ungrease treatment adopts is acetone or isopropyl alcohol.
4. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 2, it is characterized in that: the pickle that described step 2) pickling adopts is the mixed acid solution that 350g/L nitric acid and 60g/L hydrofluoric acid are made into, and pickling temperature is 40
oc, pickling duration 40s.
5. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 3, it is characterized in that: described step 2) anode oxidation process is: using metallic plate as anode, corrosion resistant plate is as negative electrode, by 300g/L NaOH, 65g/L sodium tartrate, 30g/L ethylenediamine tetra-acetic acid, in the electrolyte that 6g/L sodium metasilicate forms, impose 10-20V voltage oxidation 10-20min.
6. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 1, is characterized in that: brushing primer between metallic plate and continuous carbon fibre reinforced polyether ether ketone prepreg described step 3).
7. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 7, it is characterized in that: described primer is modified polyetheretherketonefiber chloroformic solution, described modified polyetheretherketonefiber chloroformic solution proportioning is that 105g polyether-ether-ketone powder is dissolved in 1L chloroform.
8. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 1, is characterized in that: the carbon fiber arragement direction in described step 3) in metallic plate rolling direction and continuous carbon fibre reinforced polyether ether ketone prepreg prepreg can be 0 °, ± 45 ° or 90 °.
9. according to the preparation method of the continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal described in claim 1 to 8 any one, it is characterized in that the hot pressing solid process in described step 4) is: first by mold heated to 240 ℃, insulation 1h; Subsequently mould is warming up to 370 ℃, is incubated 1h and applies 4-5MPa pressure.
10. the preparation method of continuous carbon fibre reinforced polyether ether ketone matrix fiber plymetal according to claim 9, is characterized in that: described metallic plate is TA1, TA2, TA18 or TC4, and thickness is 0.1-0.5mm.
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Cited By (6)
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| CN106891511A (en) * | 2017-03-01 | 2017-06-27 | 江苏大学 | The warm forming device and method of metal and carbon fiber prepreg composite element |
| CN107283871A (en) * | 2017-08-24 | 2017-10-24 | 哈尔滨工业大学 | A kind of preparation method of thermoplastic resin matrix's carbon fiber titanium/titanium alloy layer plywood |
| CN107379725A (en) * | 2017-07-10 | 2017-11-24 | 南京航空航天大学 | A kind of method and composite for improving titanium/fiber-reinforced composite laminates interface performance |
| CN107599446A (en) * | 2017-09-30 | 2018-01-19 | 威海拓展纤维有限公司 | Carbon fiber prepreg laying device |
| CN108081729A (en) * | 2016-11-23 | 2018-05-29 | 比亚迪股份有限公司 | A kind of metal fiber composite board and preparation method thereof |
| CN113288385A (en) * | 2021-05-17 | 2021-08-24 | 济南大学 | Method for preparing bionic lumbar pedicle screw by continuous carbon fibers |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108081729A (en) * | 2016-11-23 | 2018-05-29 | 比亚迪股份有限公司 | A kind of metal fiber composite board and preparation method thereof |
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| CN107379725A (en) * | 2017-07-10 | 2017-11-24 | 南京航空航天大学 | A kind of method and composite for improving titanium/fiber-reinforced composite laminates interface performance |
| CN107283871A (en) * | 2017-08-24 | 2017-10-24 | 哈尔滨工业大学 | A kind of preparation method of thermoplastic resin matrix's carbon fiber titanium/titanium alloy layer plywood |
| CN107283871B (en) * | 2017-08-24 | 2019-04-09 | 哈尔滨工业大学 | A kind of thermoplastic resin matrix's carbon fiber-titanium/titanium alloy layer plywood preparation method |
| CN107599446A (en) * | 2017-09-30 | 2018-01-19 | 威海拓展纤维有限公司 | Carbon fiber prepreg laying device |
| CN113288385A (en) * | 2021-05-17 | 2021-08-24 | 济南大学 | Method for preparing bionic lumbar pedicle screw by continuous carbon fibers |
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Application publication date: 20141210 |