CN102166862B - Preparation method of high-performance prefabricated reinforced fabric for facilitating resin flow - Google Patents
Preparation method of high-performance prefabricated reinforced fabric for facilitating resin flow Download PDFInfo
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Abstract
The invention belongs to a prefabricating technology of a preparation method of a resin-based composite material, and relates to a novel prefabricated reinforced fabric for a multifunctional composite material, which is used for facilitating interlaminar quick impregnation and flow of resin and has shaping and composite material toughening functions, and an application technology thereof. The invention aims to provide a material preparation technology and an application technology of a functional reinforced fabric with quick diversion, material toughening and shaping functions by using the shaping function of a high molecular porous medium at a prefabricating stage, the function of a flow distributor at a mold filling molding stage, the function of a toughening agent at a curing stage and the like on the basis of the conventional multi-layer and multi-directional warp-knitted reinforced fabric; and by means of the material preparation technology and the application technology, the prefabricating and shaping performance of a liquid molded composite material is enhanced, the impregnating and flowing properties of resin inside the prefabricated fabric is enhanced, the manufacturing quality of a product is improved, the manufacturing cost is improved and the toughness and basic performance of the obtained solid composite material are improved.
Description
Technical field
The invention belongs to the polymer matrix composites prefabricating technique, relate to resin between a kind of novel, promoting layer fast the dipping multifunctional composite that flows, have concurrently typing and composite material toughening with prefabricated enhancing process for making such fabric.
Background technology
Resin transfer moulding (the RTM of liquid condition shaping, Resin Transfer Molding) and various vacuum aided infiltration forming technique etc. be the main flow of current advanced composite material low-cost technologies, this mainly comprises Seaman resin dip forming (SCRIMP, Seaman ' s Composite Resin Infusion Molding Process), soft mode resin impregnated moulding (RIFT, Resin Infusion under Flexible Tooling) and VA RTM (VARTM, Vacuum Assistant) forming technique etc.In these vacuum assisted resin infusion technology, flow distribution medium or the distributor (Resin Distribution Media or Fabric) of one deck flexibility have all been laid on the surface of composite prefabricated fabric, its effect is that (X-Y direction) forms quick flow channel in the face parallel with the prefabricated fabric contact, promotes resin flowing and dipping at prefabricated fabric thickness direction (Z-direction).Facts have proved that this mobile expedite is very obvious for improving the effect that flows with impregnating speed.
The Chinese invention patent of referenced patent " a kind of prefabricated fabric for liquid condition shaping composite material and preparation method thereof " (application number 200810000135.2; being called for short the ES fabric is ES-Fabrics) a kind of prefabricated method that has the selective toughness reinforcing and typing function fabric of interlayer concurrently proposed; its structural principle all is toughening layer and/or the setting layer that has certain surface density at surperficial appendix one deck of enhanced fabrics; its configuration of surface is discrete particle or perforated membrane etc.; cure stage after mold filling process is finished, the appendix layer of this macromolecule material is entered composite and not multiple independent the existence by the matrix resin dissolving.Facts have proved that this patented technology all has effect aspect the typing and toughness reinforcing two of liquid condition shaping composite material.But its prefabricated fabric causes when carrying out liquid condition shaping because the porous of the toughening layer self that interlayer adds is relatively poor, has weakened the interflow of composite precast construction.
Summary of the invention
The objective of the invention is: propose a kind of at existing multilayer, multidirectional fiber lay down layer through compiling on the basis that strengthens fabric prefabricated enhancing fabric of high-performance of the promotion resin flows of the interflow of reinforced composite precast construction and preparation method thereof.
Technical scheme of the present invention is:
(1) preparation of porous polymeric medium: a) with the mixture of thermoplastic resin or thermosetting resin and thermoplastic resin, method according to solution spinning or melt spinning or electrospinning silk is carried out spinning, weaving then becomes fabric, and porosity is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is 10 μ m～50 μ m; B) maybe will use between the similar and different individual layer porous polymeric medium of above-mentioned a) preparation by at the molten 1min～30min of 100 ℃～450 ℃ following low-grade fevers, the bonding porosity that becomes is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is the layer high molecule porous media of 10 μ m～50 μ m; Or to sew into density be 30 pins/m
2～500 pins/m
2, porosity is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is the layer high molecule porous media of 10 μ m～50 μ m;
(2) porous polymeric medium adheres to setting agent: the single or multiple lift porous polymeric medium is immersed in the setting agent solution, and at the low-melting setting agent of porous polymeric medium surface appendix; Or become the setting agent of chopped strand or particle shape at the surperficial hot melt appendix of the porous polymeric medium of single or multiple lift, and the hot melting process condition is that temperature is 100 ℃～350 ℃, the duration is 1min～30min; The surface density of setting agent material on porous polymeric medium is at 4g/m
2～8g/m
2Between;
(3) preparation of prefabricated enhancing fabric: will adhere to behind the setting agent porous polymeric medium as the appendix material directly be laid in strengthen the fabric shop layer by layer between, its centre plane contact rate is greater than 40%; Be prepared according to non-flexing process for making such fabric then, or sew at thickness direction, sewing density is 30 pins/m
2～500 pins/m
2Or by hot melting mode little each the shop layer that coheres of the porous polymeric medium of reinforcing material shop interlayer, its technology makes prefabricated enhancing fabric realize that the prefabricated layer-layer with the shop interlayer of whole typing is connected for being the molten 1min～30min of 100 ℃～450 ℃ following low-grade fevers in heating-up temperature.
The material of described setting agent is used resin matrix composition, and its melting range is 40 ℃～150 ℃.
Described porous polymeric medium is no latitude cloth, grid yarn or felt.
Advantage of the present invention is:
It is multi-functional in one that the assembling typing that prefabricated enhancing fabric of the present invention (be called for short MESF fabric) has the multi-layer and multi-directional fabric concurrently is connected with lamination, the promotion of interlayer resin flows and solid composite material are toughness reinforcing etc., in use, can improve the processing performance of composite liquid condition shaping and the good prefabricated shaping performance of fabric, realize high tenacityization and the high performance of solid composite material simultaneously.
Preparation method of the present invention, material and structural form thereof by preferred porous polymeric medium, make this appendix material be not only the toughness reinforcing component of shaping material and the solid composite material of the prefabricated process of composite, also utilize the liquid infiltration of interlayer porous media especially dexterously and flowed and promoted function, omitted the flexible resin flow distributor in the traditional vacuum assistant formation, the permeability of prefabricated fabric structure and the uniformity of infiltration have been improved, the technological effect of liquid condition shaping and the workmanship of composite have been improved, shortened preparation time, reduced manufacturing cost, realized multi-functional, integrated, integrate cheaply.
Preparation method of the present invention, since the appendix material can designs fix at specific interlayer, so laminated construction that can manufacturing cycle also can prepare aperiodic laminated construction, the laminated construction that gradient distributes be can also prepare, thereby the huge modification of composite and design freedom given.
The specific embodiment
A kind of by at the composite liquid condition shaping that strengthens the fabric shop interlayer unidirectional non-fold of lay (Non-Crimp) or multi-layer and multi-directional porous polymeric medium with prefabricated enhancing fabric-abbreviations MESF fabric, it has concurrently, and fabric is finalized the design, interlayer resin flows promotion and solid composite material is toughness reinforcing and high performance etc. is multi-functional.
The used reinforcing fiber materials of described MESF fabric is one of following fiber: glass fibre, carbon fiber, aramid fiber, basalt fibre and organic fiber, the tow number of its fiber and woven thickness thereof comprise and use big tow without limits.
The material of the porous polymeric medium that described MESF fabric is used is one of following material: polyether-ketone, polysulfones, polyether sulfone, TPI, PEI, polyphenylene oxide, polyamide, polyolefin; Or one of them mixture of following thermosetting resin one of them and above-mentioned thermoplastic resin: epoxy resin, bimaleimide resin, thermoset polyimide resin, Polybenzoxazine resin, phenolic resins, cyanate ester resin, unsaturated polyester resin.The mixed proportion of above-mentioned thermoplastic resin and thermosetting resin is not limit, as long as can be prepared into the flexible porous media of serialization.The mass mixing ratio example of general above-mentioned thermoplastic resin and thermosetting resin is 1:20～20:1.
The used flexible porous media of this fabric is one of following form: the fabric of various single or multiple lifts, no latitude cloth, grid yarn or felt, be included in appendix on these fabrics, no latitude cloth, grid yarn or felt surface thermoplastic resin recited above or thermosetting resin and thermoplastic resin intermixture's coating or particle, and the material of the material of coating or particle and above-mentioned fabrics, no latitude cloth, grid yarn or felt is identical or different.
The architectural feature of this MESF fabric integral body is unidirectional non-fold and multi-layer and multi-directional, that is to say, strengthen porous media that fabric can utilize macromolecule material and realize typing and do not loose, rely on simultaneously the porous media of macromolecule material realize unidirectional non-fold lay and layer with layer be connected.
For this type of prefabricated enhancing process for making such fabric of high-performance that promotes resin flows, it is characterized in that the step of preparation is as follows:
(1) preparation of porous polymeric medium: 1) with above-mentioned porous polymeric medium material thermoplastic resin or the mixture of thermosetting resin and thermoplastic resin, weave the individual layer porous polymeric medium of the high porosity that becomes fabric, no latitude cloth, grid yarn or felt according to routine techniques (solution spinning or melt spinning or electrospinning silk) spinning; Maybe will be with above-mentioned 1) between the similar and different individual layer macromolecule material porous media of preparation by at the molten 1min～30min of 100 ℃～450 ℃ following low-grade fevers, or sewing becomes low-density, and (sewing density is 30 pins/m
2～500 pins/m
2) the layer high molecule porous media; Porous polymeric medium three-dimensional porosity by method for preparing is greater than 50%, and its surface density is 4g/m
2～20g/m
2, its thickness is 10 μ m～50 μ m.
(2) porous polymeric medium adheres to setting agent: the described high porosity porous polymeric medium of point (1) is immersed in the setting agent solution, and at the low-melting setting agent of porous polymeric medium surface appendix; Or at the chopped strand of the surperficial hot melt appendix of the high porosity porous polymeric medium of the described single or multiple lift of point (1) or the setting agent of particle shape, the hot melting process condition is that temperature is 100 ℃～350 ℃, and the duration is 1min～30min; No matter adopt which kind of method, the surface density of setting agent material on porous polymeric medium is at 4g/m
2～8g/m
2Between.
(3) preparation of prefabricated enhancing fabric: according to the design of MESF prefabricated fabric, will have flexible porous polymeric medium as the appendix material directly be laid in strengthen the fabric shop layer by layer between, its centre plane contact rate is greater than 40%; (with reference to Europatent " Non-Crimp Fabrics " (WO/2002/057527)) preparation method carries out multi-layer and multi-directional lamination lay preparation, or sews at thickness direction that (sewing density is 30 pins/m according to non-flexing fabric then
2～500 pins/m
2) connect, or by hot melting mode (heating-up temperature is the molten 1min of 100 ℃～450 ℃ following low-grade fevers～30min) little each the shop layer that coheres of the porous polymeric medium of reinforcing material shop interlayer, makes the MESF fabric realize the layer of the prefabricated and shop interlayer of whole typing-layer be connected.
(4) composite liquid condition shaping: be lower than under the feature solution temperature of porous polymeric medium (60 ℃～280 ℃) and vacuum aided under, resin matrix is expelled in the MESF fabric, finish quick mold filling and dipping; And at the curing window of higher temperature (60 ℃～350 ℃), finish dissolving or the diffusion of this flexible macromolecule porous media in resin matrix, realize thermoplastic resin toughness reinforcing to the thermosetting matrix.
According to a kind of prefabricated enhancing process for making such fabric of high-performance that promotes resin flows recited above, it is characterized in that, the material of described setting agent is the component of used resin matrix composition or porous polymeric medium, its fusing point is lower than the glass transition temperature of porous polymeric medium, and scope is 40 ℃～150 ℃;
Embodiment 1
Prepare porous appendix medium: commercially available conventional copolyamide (nylon) chemical fibre is weaved becomes hollow plain, and surface density is 8.48g/m
2, porosity 60%.
Prepare (the about 900mm of fabric width) preparation carbon fiber shop layer structure on the Zhuan Ge, [+45 °/0 °/90 °/-45 °] at general NCF
3SLay; Entirely Fang Ge is at the interlayer of each layer unidirectional fiber layers with the hollow plain of above-mentioned polyamide (nylon), and the face contact rate of hollow plain and carbon fiber shop layer is about 40%, forms the alternative stacked precast construction of carbon fiber shop layer and hollow plain.
It is little molten to wherein the hollow plain of polyamide to heat whole fabric, suitably exerts pressure, namely obtained this multidirectional multilayer, appendix the hollow plain of polyamide strengthen the body fabric as the plane MESF multifunctional precast of dipping and mobile promoting layer.
The processing and forming of MESF multifunctional precast fabric: this plane prefabricated fabric is assembled into mould according to the method for conventional vacuum assisted resin infusion, be matrix resin with the E54 epoxy, about 50 ° of C, adopt VARI technology to suck in the mould, and solidify according to the standard technology of E54 resin system.
The porosity of surveying this solid composite material laminate approaches zero, surveys compressive strength 253MPa after the impact of this composite, illustrates that the liquid condition shaping technological property of this MESF multifunctional precast fabric and impact injury tolerance limit are well-behaved.
Embodiment 2
The chemical fibre line porous appendix medium of typing function is with in preparation: commercially available conventional polyether sulfone (PES) chemical fibre is weaved according to the method for embodiment 1 becomes hollow plain, adopt the B-rank to solidify bismaleimide resin as setting agent, after it is dissolved in acetone, flood this hollow plain, obtain the hollow plain of pre-appendix setting agent after the drying, its surface density is 12g/m2, porosity 60%.
Manual preparation [± 45 °]
2SMultilayer unidirectional carbon fiber dimension shop layer, with the hollow plain of above-mentioned pre-appendix setting agent entirely Fang Ge between each unidirectional carbon fiber dimension layer, the face contact rate of hollow plain and carbon fiber shop layer is about 40%, forms the alternative stacked precast construction of carbon fiber shop layer and hollow plain.
The typing of this prefabricated fabric: above-mentioned prefabricated fabric is abutted on the right angle mould, with electric iron it was carried out about even local heat to 120 ° C about 1 minute, it is softening little molten to cause pre-appendix to solidify bismaleimide resin on the B-rank on this hollow plain surface, bonding adjacent carbon fiber layer, conformal cooling then namely obtains the quadruple cloth precast body of finalizing the design in the right angle.
The processing and forming of this right angle precast body: this precast body is gone into mould according to the Fang Fa Ge of conventional high-temperature vacuum assistant formation, be matrix resin with 6421 bismaleimide resins, about 105 ° of C, adopt VARI technology to suck in the mould, and solidify according to the standard technology of 6421 resin systems, namely obtain the composite product at required right angle.
The porosity of surveying this solid right angle composite product approaches zero, illustrates that the setting process of this MESF multifunctional precast fabric and liquid condition shaping technological property are good.
Embodiment 3
Prepare porous appendix medium: commercially available conventional PAEK (PAEK) chemical fibre is weaved becomes nonwoven, again standard setting agent powder ES-T321 is spread in uniform in this nonwoven surface, heating makes its little melting and coheres on this nonwoven, and namely obtaining surface density is 10g/m
2About, the nonwoven porous flow moving medium of voidage 55%, pre-appendix setting agent powder.
The lay structure is [+45 °/0 °/90 °/-45 °] on general NCF preparation dress Ge
2SMultilayer unidirectional carbon fiber dimensional fabric, with the nonwoven porous flow moving medium Fang Ge of the above-mentioned pre-appendix setting agent powder interlayer at the unidirectional fiber lay down layer of each individual layer, namely obtain the prefabricated enhancing fabric of needed MESF.
The typing of this prefabricated fabric: this prefabricated fabric is abutted on the curve mold, roll bonding each the adjacent carbon fiber layer in the softening back of the ES-T321 powder sizing agent that is heated to pre-appendix repeatedly with the electrical heating roller, namely obtain the precast body of a curved surface typing.
The processing and forming of this curved surface precast body: this precast body is gone into mould according to the Fang Fa Ge of conventional vacuum assisted resin infusion, be matrix resin with commercially available benzoxazine, adopt the standard VaRTM technology of this benzoxazine to carry out processing and forming, and be cured according to the standard technology of this resin system, namely obtain required curved surface composite product.
The porosity of surveying this solid koji surface composite material product approaches zero, illustrates that the curved surface setting process of this MESF multifunctional precast fabric and liquid condition shaping technological property are good.
Embodiment 4
Prepare porous appendix medium: commercially available conventional PEI (PEI) chemical fibre is weaved becomes loose grid yarn, its surface density 8g/m
2About, voidage about 65%; With commercially available conventional copolyamide (nylon) dissolving, adopt the electrostatic spinning process preparation to have the nylon nonwoven fabrics of loose and porous structure in the upper and lower surface of this PEI grid cloth, make its little being bonded on this PEI grid yarn, obtain centre plane density 12g/m
2About, the composite multi-layer porous appendix medium of voidage 60%.
Prepare MESF prefabricated fabric and composite laminated plate thereof according to embodiment 1 same method, the porosity of surveying this solid composite material laminate approaches zero, survey compressive strength 260MPa after the impact of this composite, illustrate that the liquid condition shaping technological property of this MESF multifunctional precast fabric and impact injury tolerance limit are well-behaved.
Embodiment 5
Preparation porous appendix medium: according to method index PAEK (PAEK) nonwoven of embodiment 3, carboxy blocking acrylonitrile-butadiene rubber (CTBN) particle is mixed by the weight ratio of 5:100 with AG80 epoxy resin, cryogenic freezing is pulverized and is made the setting agent particle, on horizontal back and forth duster by vibratory sieve with this setting agent uniform particles spreading, heating makes its little melting and coheres on this PAEK nonwoven then, and namely obtaining surface density is 10g/m
2About, voidage 55%, pre-appendix be toughness reinforcing-the nonwoven porous flow moving medium of setting agent powder.
General NCF prepare on the Zhuan Ge (the about 900mm of fabric width) respectively the lay structure be [+45 °/0 °/90 °/-45 °]
2S[+45 °/0 °/90 °/-45 °]
3SMultilayer unidirectional carbon fiber dimensional fabric, with the nonwoven porous flow moving medium Fang Ge of the above-mentioned pre-appendix setting agent powder interlayer at the unidirectional fiber lay down layer of each individual layer, because [+45 °/0 °/90 °/-45 °]
3SPrecast body is thicker, therefore sews with the rare density of glass wire at this prefabricated fabric thickness direction according to conventional NCF method, namely obtains the prefabricated enhancing fabric of needed MESF.
The typing of this prefabricated fabric: this prefabricated fabric is abutted on the plane mould, be heated to the bonding adjacent carbon fiber layer in the softening back of powder sizing agent of pre-appendix, namely obtain the composite preform of a plane typing.
The processing and forming of this unilateral precast body: this precast body is assembled into mould according to the method for conventional vacuum assisted resin infusion, VaRTM technology with 3266 epoxy resin of standard is carried out processing and forming, and be cured according to the standard technology of 3266 resins, namely obtain the plane composite material laminate that this MESF fabric strengthens.
The porosity of surveying this solid composite material laminate approaches zero, illustrates that the liquid condition shaping technological property of this MESF multifunctional precast fabric is good; [+45 °/0 °/90 °/-45 °] is somebody's turn to do in actual measurement
2SThe opening hot strength 500MPa of composite, opening compressive strength 310MPa illustrates because the non-fold one-way orientation character of carbon fiber shop layer causes the basic property of composite laminated plate very high; Survey this composite ([+45 °/0 °/90 °/-45 °]
3S) impact after compressive strength 252MPa, illustrate that the impact injury tolerance limit of this composite laminated plate is well-behaved.
Claims (3)
1. prefabricated enhancing process for making such fabric of high-performance that promotes resin flows is characterized in that the step of preparation is as follows:
(1) preparation of porous polymeric medium: a) with the mixture of thermoplastic resin or thermosetting resin and thermoplastic resin, method according to solution spinning or melt spinning or electrospinning silk is carried out spinning, weaving then becomes fabric, and porosity is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is 10 μ m～50 μ m; B) maybe will use between the similar and different individual layer porous polymeric medium of above-mentioned a) preparation by at the molten 1min～30min of 100 ℃～450 ℃ following low-grade fevers, the bonding porosity that becomes is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is the layer high molecule porous media of 10 μ m～50 μ m; Or to sew into density be 30 pins/m
2～500 pins/m
2, porosity is greater than 50%, and surface density is 4g/m
2～20g/m
2, thickness is the layer high molecule porous media of 10 μ m～50 μ m;
(2) porous polymeric medium adheres to setting agent: the single or multiple lift porous polymeric medium is immersed in the setting agent solution, and at the low-melting setting agent of porous polymeric medium surface appendix; Or become the setting agent of chopped strand or particle shape at the surperficial hot melt appendix of the porous polymeric medium of single or multiple lift, and the hot melting process condition is that temperature is 100 ℃～350 ℃, the duration is 1min～30min; The surface density of setting agent material on porous polymeric medium is at 4g/m
2～8g/m
2Between;
(3) preparation of prefabricated enhancing fabric: will adhere to behind the setting agent porous polymeric medium as the appendix material directly be laid in strengthen the fabric shop layer by layer between, its centre plane contact rate is greater than 40%; Be prepared according to non-flexing process for making such fabric then, or sew at thickness direction, sewing density is 30 pins/m
2～500 pins/m
2Or by hot melting mode little each the shop layer that coheres of the porous polymeric medium of reinforcing material shop interlayer, its technology makes prefabricated enhancing fabric realize that the prefabricated layer-layer with the shop interlayer of whole typing is connected for being the molten 1min～30min of 100 ℃～450 ℃ following low-grade fevers in heating-up temperature.
2. a kind of prefabricated enhancing process for making such fabric of high-performance that promotes resin flows according to claim 1 is characterized in that the material of described setting agent is used resin matrix composition, and its melting range is 40 ℃～150 ℃.
3. a kind of prefabricated enhancing process for making such fabric of high-performance that promotes resin flows according to claim 1 is characterized in that described porous polymeric medium is no latitude cloth, grid yarn or felt.
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| CN102166862A (en) | 2011-08-31 |
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