CN102888007B - Toughening membrane with surface bump microstructure and preparation method thereof - Google Patents
Toughening membrane with surface bump microstructure and preparation method thereof Download PDFInfo
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- CN102888007B CN102888007B CN201210342254.2A CN201210342254A CN102888007B CN 102888007 B CN102888007 B CN 102888007B CN 201210342254 A CN201210342254 A CN 201210342254A CN 102888007 B CN102888007 B CN 102888007B
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Abstract
The invention belongs to a toughening technology of a laminated composite material of a continuous carbon fiber reinforced resin matrix and relates to a toughening membrane with a surface bump microstructure and a preparation method of the toughening membrane. The toughening membrane is mainly characterized in that a proper toughening macromolecule is selected to obtain a self-support film with the surface bump microstructure for toughening the laminated composite material by a soft template printing (soft lithography) method. According to the toughening membrane and the preparation method of the toughening membrane, the preparation method is simple, and the preparation method is suitable for various thermoplastic resin systems. The toughening membrane may includes various complicated macromolecule surface bump microstructures and different material matrixes to match with various requirements for toughening the laminated composite material.
Description
Technical field
The invention belongs to the toughening technology that a kind of continuous carbon fibre strengthens resin base laminated composite materials, relate to a kind of toughened film with rat microstructure and preparation method thereof.
Background technology
For aviation matrix material, owing to being generally thermosetting resin, high crosslink density after it is curing causes molecule segment to have very low reactivity, thereby show as the fragility of resin intrinsic, be presented as that for matrix material interlaminal toughness deficiency, shock resistance damage problem limited in one's ability, how to have become important studying a question by the shock resistance damage performance of toughness reinforcing raising matrix material, be also that advanced composite material is applied the greatest problem facing to aircraft structure.
Method for composite material toughening is varied; as directly carried out toughness reinforcing for thermoset substrate resin; but need to or add solubility toughness material by thermosetting resin chain extension, the decline that therefore usually can bring thermotolerance and rigidity, or the problem such as processing technology variation." intercalation " method of introducing ductile structure at laminated composite materials interlayer especially receives publicity, manufacturability and other mechanical property of moulding when improving matrix material shock resistance bed resolution because of it, are kept, most typical example inserts the independently pure thermoplastic resin of high tenacity or thermoset glue-line and " offing normal " toughening technology (referenced patent CN101220561 that grows up thereof at interlayer, CN101760965A, WO2011148111-A1, DE19918079-A1 etc.).
The suitable intercalation film of preparation for the key problem in technology of the solvable or insoluble thermoplasticity intercalation of interlayer intercalation.Technology is before all that independently insoluble thermoplastic film or intercalation film are changed into solvable and can further be formed micron-scale phase separation structure to improve toughness of material by insoluble at resin solidification temperature at intercalation between composite layer, the former can bring the poor consequence in interface, and latter has proposed very high requirement to the solvability of thermoplastic film.And these intercalation films are not more from the consideration of getting on of the microscopic pattern of film, control as improved the microtexture of film may be able to make film promote the effect of bonding not needing to dissolve or only need appropriateness to dissolve or just possess physics bridging when swelling, this point is utilizing non-woven fabrics to be embodied on toughness reinforcing, but the fiber in non-woven fabrics more may present the distribution that is parallel to non-woven fabrics plane or matrix material interlayer, physics bridge linking effect while having reduced I type and II type interlayer faults between fault interface, because fault interface is parallel to the planar extension between laying conventionally.
Soft lithography is a kind of simple method of preparing microstructure, can utilize simply to impress-uncover and copy various microtextures, and its fineness even can arrive Nano grade.But this method is only prepared functional microstructure at substrate surface conventionally, as CN201110205508.1 prepares conductive graphene microstructure for semi-conductor product, as CN1702527 prepares oriented layer for LCD, CN1544308 colloidal crystal patterning is applied to design and the preparation of the optics based on colloidal crystal, but there are no pertinent literature and the patent report by toughened film for the preparation of laminated composite intercalation.
Summary of the invention
Object of the present invention: the object of the invention is to propose a kind of matrix material intercalation toughened film with rat microstructure and preparation method thereof, this toughened film possesses rat microstructure, make not need in matrix material to have preferably and bonding interface and the Reinforced structure of resin matrix through dissolving phase-splitting, and protruding microstructure goes up perpendicular to interlayer and distribute largely, finally have laminated composite is had to good toughening effect, improve the shock resistance bed resolution of laminated composite.
Technical scheme of the present invention is:
Toughened film polymkeric substance used comprises nylon, polyaryletherketone, polyimide, polyetherimide, polyethersulfone or polyether-ether-ketone, and two faces of toughened film have a face or two masks to have rat microstructure, and toughened film area density is at 5g/m
2to 40g/m
2between, the hill height of rat microstructure is between 1 μ m to 150 μ m, and hill height and ledge width size are than being 1:1 to 10:1, toughened film substrate thickness is between 1 ~ 30 μ m, in toughened film, be distributed with penetrating hole, aperture is 50 μ m to 2mm, and porosity is 2% to 50%.
Prepare the method for toughened film, comprise following step:
(1) preparation final state polymers soln, joins final state polymkeric substance in the solvent of this final state polymkeric substance of solubilized and dissolves, and the mass percent concentration of final state polymers soln is 0.2% ~ 25%; Or the polymer precursor of the solubility of final state polymkeric substance is joined in the solvent of this precursor of solubilized and dissolve, the mass percent concentration of precursor solution is 0.2% ~ 25%;
(2) soft seal obtains having the film of rat microstructure, and the method for soft seal is one of following three kinds of methods:
(2-1) one side that has structure of soft template with microstructure is adhered to the solution of one deck final state polymers soln or polymer precursor, again two soft template are forced together relatively with the one side of solution, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain having the two-sided film that has rat microstructure; The one side that has structure of soft template is adhered to the solution of one deck final state polymers soln or polymer precursor, again by this sheet soft template and the smooth soft template of a slice to forcing together, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain one side and have the film of rat microstructure;
(2-2) one side that has structure of soft template with microstructure is adhered to the solution of one deck final state polymers soln or polymer precursor, again two soft template are pressed in relatively to the two sides of the matrix film that a composition is final state polymkeric substance or polymer precursor with the one side of solution, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain having the two-sided film that has rat microstructure; The one side that has structure of this sheet soft template is adhered to the solution of one deck final state polymers soln or polymer precursor, again by this sheet soft template and the smooth soft template of a slice to being pressed in the two sides of the matrix film that a composition is final state polymkeric substance or polymer precursor, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain one side and have the film of rat microstructure;
(2-3) one side that has structure of the soft template with microstructure is adhered to one deck solvent, again by two soft template to being pressed in the two sides of a film, the composition of film is final state polymkeric substance or polymer precursor, solvent-soluble solution used forms polymkeric substance or the polymer precursor of this film, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain the two-sided film that has rat microstructure; The one side that has structure of this sheet soft template is adhered to one deck solvent, then by this sheet soft template and the smooth soft template of a slice to being pressed in the two sides of this film, at room temperature to 120 DEG C, keep 1s ~ 10min, after taking off, obtain one side and have the film of rat microstructure;
(3) for composition be the film with rat microstructure of final state polymkeric substance, film is dried and removed residual solvent; The film with rat microstructure that contains polymer precursor for composition, the processing condition that are first corresponding final state polymkeric substance by this precursor conversion are processed film, then residual solvent is removed in oven dry.By film perforating, aperture is 50 μ m to 2mm, and hole is evenly distributed on film, and porosity is 2 ~ 50%, is had accordingly the toughened film of rat microstructure.
Solvent for use is tetrahydrofuran (THF), acetone, methyl alcohol, water, dimethyl formamide, formic acid, final state polymkeric substance used is nylon, polyaryletherketone, polyimide, polyetherimide, polyethersulfone, polyether-ether-ketone, and polymer precursor used is polyamic acid, polyetheramides acid, polyesteramide, polyetheramides ester.
Soft template material used is PDMS.
Used comprises the roll extrusion of soft template being made to roll form to pressing.
Advantage and disadvantage of the present invention is:
The present invention utilizes the method for simple soft printing to prepare two-sided or one side to have the toughened film of rat microstructure, and the purposes of this film is for the interlayer intercalation of laminated composite toughness reinforcing, to promote the shock resistance bed resolution of matrix material.The present invention has the toughened film of rat microstructure with simple method preparation table mask, preparation method is simple, toughened film prepared by this method can possess various rat microstructures complicated and changeable and differing materials composition, to mate the demand of laminated composite material toughening.This preparation method and obtain toughened film and not only there is larger meaning for the application of scientific research, and the toughened film of the ad hoc structure obtaining can play good toughening effect to laminated composite.
Brief description of the drawings
Fig. 1 is exterior view and the sectional view of the two-sided toughened film all with lotus leaf mastoid process structure prepared by the embodiment of the present invention 1, the structural mastoid process structure of lotus leaf copying is the rat microstructure perpendicular to integral membrane surface, and basilar membrane refers to passive film in the middle of mastoid process structure.
Embodiment
Below by embodiment, design of the present invention and technology of preparing are described in further details.
Rat microstructure described in enforcement refers to the projection having in toughened film perpendicular to the macromolecule material of thin film planar, this projection can be to be similar to the same strip that presents of grating to distribute on thin film planar, there is ripple struction or optical grating construction as two-sided, also can be the projection of spot distribution in the plane, as four directions or the hexagonal lattice structure of mastoid process structure, rule.It is toughness reinforcing that the saying of so-called toughened film comes from laminated composite " intercalation ", be placed in laminated composite interlayer by one deck thermal plastic high polymer film, after solidifying, can effectively improve the interlayer faults toughness of matrix material, thereby improve the anti-low-velocity impact damage performance of matrix material.
Consider the toughness reinforcing application on advanced composite material, the preferred nylon of type of polymer of this layer of toughened film, polyaryletherketone, polyimide, polyetherimide, polyethersulfone, these High performance plastic resins of polyether-ether-ketone, should there is suitable area density, when making it reach toughness reinforcing, keep fiber volume fraction to be unlikely to reduce too much, therefore its area density is at 5g/m
2to 40g/m
2between, more preferably 10g/m
2to 30g/m
2between; The vertical macromolecular structure hill height on film surface is too large and too little all unfavorable, it is too large that hill height is too greatly prepared difficulty, and after laying compacting, presenting calm distribution is unfavorable for toughness reinforcing on the contrary, hill height is too little toughness reinforcing not obvious, therefore be preferably between 1 to 150 μ m, more preferably between 5 to 100 μ m; Facilitate practical application and convenient take off from template in order to keep toughened film to there is certain intensity, also needing there is certain thickness in the film substrate of the centre of microstructured layers, preferably between 1 ~ 30 μ m.More preferably between 3 ~ 10 μ m.
In order to make toughened film not affect flowing of resin in resin injection process and the prepreg course of processing, need to carry out drilling to film, drilling scheme can be selected diversified scheme, controls suitable porosity and meets resin flows requirement, little on the character impact of film itself.This is also the feature with rat microstructure film in other field application that is different from of toughened film needs.
Soft lithography is a kind of method of widely used printing microstructure, but described in document, conventionally all by polymkeric substance wiring solution-forming, then on a substrate, print one deck microstructure film, to utilize the surface properties of microstructure, as optics, environment sensitive etc., and majority is not to obtain a self-supported membrane, more not for the preparation of toughened film.The present invention proposes thus this preparation method of toughened film for the intercalation of rat microstructure that has, its key step has following:
Embodiment 1:
(1-1) by the polyaryletherketone of a PEK-C(phenolphthalein modification) or PES be dissolved in wiring solution-forming in tetrahydrofuran (THF), the mass percent concentration of solution is 5% or 20%;
(1-2) soft seal obtains having the film of rat microstructure: the one side that has structure that solution is added drop-wise to the PDMS soft template that has anti-carved lotus leaf surface microstructure, the hill height of lotus leaf structure is 10 ~ 15 μ m, width is 5 μ m, be that depth-width ratio is 2 ~ 3, again two one sides that all added the microstructure of the soft template of solution are forced together face-to-face, at 30 DEG C, keep 3min, after taking off, obtain having the two-sided film that has lotus leaf structure;
(1-3) aftertreatment obtains toughened film: film is dried to the toughened film of removing residual solvent and obtain having rat microstructure;
(1-4) film is got to about diameter 0.5mm or 0.1mm by the method that machinery is pricked hole or laser boring, every square centimeter is uniformly distributed respectively approximately 25 or 1000 s' aperture.
Embodiment 2:
(2-1) polyamic acid or polyetheramides acid or the polyimide of polyesteramide or polyetheramides ester and so on or the precursor polymer of polyetherimide are dissolved in to wiring solution-forming in methyl alcohol, the mass percent concentration of polymer precursor solution is 1% or 2%;
(2-2) soft seal obtains having the film of rat microstructure: the one side that has structure that solution is added drop-wise to the PDMS soft template that has anti-carved grating surface microstructure, the hill height of grating is 5 μ m or 10 μ m, cycle is 2 μ m, be that depth-width ratio is 2.5 or 5, separately getting the thickness that this kind of polymer precursor of a slice make is the film of 7 μ m, again by the microstructure of two soft template that all added solution together face-to-face to being pressed in the two sides of film, at 40 DEG C, keep 5min, after taking off, obtain having the two-sided polymer precursor film that has rat microstructure;
(2-3) aftertreatment obtains toughened film: film is heated under nitrogen protection to 300 DEG C and keep one hour, obtains two-sided polyimide or the polyetherimide toughened film that has rat microstructure.
(2-4) film is got to diameter 0.5mm by the method that machinery is pricked hole or laser boring, every square centimeter is uniformly distributed the aperture of approximately 100.
Embodiment 3:
(3-1) polyethersulfone or polyetherimide are dissolved in to DMF wiring solution-forming, the mass percent concentration of polymers soln is 15%;
(3-2) soft seal obtains having the film of rat microstructure: the one side that has structure that solution is added drop-wise to the soft template of four directions, the surface dot matrix microstructure having anti-carved, the hill height of four directions dot matrix is 50 μ m or 90 μ m, width is 10 μ m, be that depth-width ratio is 5 or 9, between projection, spacing is 30 microns, this sheet template is pressed on a PEK-C film in the soft template that is placed on surfacing, film thickness is 15 μ m again.At 110 DEG C, keep 10min subsequently, after taking off, obtain thering is one side and have PES/PEK-C or the PEI/PEK-C laminated film of cubic dot matrix;
(3-3) aftertreatment obtains toughened film: film is dried to the toughened film of removing residual solvent and obtain having rat microstructure;
(3-4) film is pricked out to about diameter 1mm by the method that machinery is pricked hole, every square centimeter is uniformly distributed the aperture of approximately 36.
Embodiment 4:
(4-1) get DMF for subsequent use;
(4-2) soft seal obtains having the film of rat microstructure: DMF is added drop-wise to the PDMS soft template of the random protruding microstructure in surface having anti-carved and the one side that has structure of the PDMS soft template of the surperficial hexagonal lattice structure that anti-carved (PDMS that obtains is actually the former of the dot matrix that surface falls in), hill height is 9 μ m or 5 μ m, width is 5 μ m, be that depth-width ratio is 1.4 or 1, between projection, spacing is 10 microns, again two microstructures that all added the soft template of DMF solvent are faced to the relative two sides that is pressed in polyetherimide film, film thickness is 25 μ m.At 90 DEG C, keep 10min subsequently, after solvent evaporates is closely dry, after taking off, obtains having one side and there is the random protruding polyetherimide film simultaneously with hexagonal lattice;
(4-3) aftertreatment obtains toughened film: film is dried to the toughened film of removing residual solvent and obtain having rat microstructure;
(4-4) film is pricked out to about diameter 0.2mm by the method for laser boring, every square centimeter is uniformly distributed the aperture of approximately 800.
Embodiment 5:
(5-1) by the polyaryletherketone of a PEK-C(phenolphthalein modification) be dissolved in wiring solution-forming in tetrahydrofuran (THF), the mass percent concentration of polymers soln is 0.8%; Or nylon is dissolved in in formic acid, to be made into mass percent concentration be 2% polymers soln;
(5-2) soft seal obtains having the toughened film of rat microstructure: the one side that has structure that solution is added drop-wise to the soft template that has anti-carved hexagonal lattice structure, hill height is 10 μ m or 6 μ m, width is 4 μ m, be that depth-width ratio is 2.5 or 1.5, between projection, spacing is 12 microns, again two microstructures that all added the soft template of PEK-C solution are pressed on the PEK-C film that a thickness is 4 μ m face-to-face, respectively at 60 DEG C (THF solution of PEK-C) lower 1s of maintenance and 70 DEG C (formic acid solution of nylon) lower 20s that keeps, after taking off, obtain having the two-sided film that has hexagonal lattice structure,
(5-3) aftertreatment obtains toughened film: film is dried and removed the toughened film with rat microstructure that obtains PEK-C or nylon material after residual solvent;
(5-4) film is pricked out to about diameter 1.5mm by the method that machinery is pricked hole, every square centimeter is uniformly distributed the aperture of approximately 15.
Claims (5)
1. one kind has the toughened film of rat microstructure, it is characterized in that, toughened film polymkeric substance used comprises nylon, polyaryletherketone, polyimide, polyetherimide, polyethersulfone or polyether-ether-ketone, two faces of toughened film have a face or two masks to have rat microstructure, and toughened film area density is at 5g/m
2to 40g/m
2between, the hill height of rat microstructure is between 1 to 150 μ m, and hill height and ledge width size are than being 1:1 to 10:1, toughened film substrate thickness is between 1~30 μ m, in toughened film, be distributed with penetrating hole, aperture is 50 μ m to 2mm, and porosity is 2% to 50%.
2. a method of preparing the toughened film with rat microstructure claimed in claim 1, is characterized in that,
The method comprises following step:
(1) preparation final state polymers soln, joins final state polymkeric substance in the solvent of this final state polymkeric substance of solubilized and dissolves, and the mass percent concentration of final state polymers soln is 0.2%~25%; Or the polymer precursor of the solubility of final state polymkeric substance is joined in the solvent of this precursor of solubilized and dissolve, the mass percent concentration of precursor solution is 0.2%~25%;
(2) soft seal obtains having the film of rat microstructure, and the method for soft seal is one of following three kinds of methods:
(2-1) one side that has structure of soft template with microstructure is adhered to the solution of one deck final state polymers soln or polymer precursor, again two soft template are forced together relatively with the one side of solution, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain having the two-sided film that has rat microstructure; The one side that has structure of soft template is adhered to the solution of one deck final state polymers soln or polymer precursor, again by this sheet soft template and the smooth soft template of a slice to forcing together, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain one side and have the film of rat microstructure;
(2-2) one side that has structure of soft template with microstructure is adhered to the solution of one deck final state polymers soln or polymer precursor, again two soft template are pressed in relatively to the two sides of the matrix film that a composition is final state polymkeric substance or polymer precursor with the one side of solution, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain having the two-sided film that has rat microstructure; The one side that has structure of this sheet soft template is adhered to the solution of one deck final state polymers soln or polymer precursor, again by this sheet soft template and the smooth soft template of a slice to being pressed in the two sides of the matrix film that a composition is final state polymkeric substance or polymer precursor, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain one side and have the film of rat microstructure;
(2-3) one side that has structure of the soft template with microstructure is adhered to one deck solvent, again by two soft template to being pressed in the two sides of a film, the composition of film is final state polymkeric substance or polymer precursor, solvent-soluble solution used forms polymkeric substance or the polymer precursor of this film, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain the two-sided film that has rat microstructure; The one side that has structure of this sheet soft template is adhered to one deck solvent, then by this sheet soft template and the smooth soft template of a slice to being pressed in the two sides of this film, at room temperature to 120 DEG C, keep 1s~10min, after taking off, obtain one side and have the film of rat microstructure;
(3) for composition be the film with rat microstructure of final state polymkeric substance, film is dried and removed residual solvent; The film with rat microstructure that contains polymer precursor for composition, the processing condition that are first corresponding final state polymkeric substance by this precursor conversion are processed film, dry and remove residual solvent again, by film perforating, aperture is 50 μ m to 2mm, hole is evenly distributed on film, and porosity is 2~50%, is had accordingly the toughened film of rat microstructure.
3. a kind of described method of preparing the toughened film with rat microstructure claimed in claim 1 as claimed in claim 2, it is characterized in that, solvent for use is tetrahydrofuran (THF), acetone, methyl alcohol, water, dimethyl formamide, formic acid, final state polymkeric substance used is nylon, polyaryletherketone, polyimide, polyetherimide, polyethersulfone, polyether-ether-ketone, and polymer precursor used is polyamic acid, polyetheramides acid, polyesteramide, polyetheramides ester.
4. a kind of described method of preparing the toughened film with rat microstructure claimed in claim 1 as claimed in claim 2, is characterized in that, soft template material used is PDMS.
5. a kind of described method of preparing the toughened film with rat microstructure claimed in claim 1 as claimed in claim 2, is characterized in that, used comprises the roll extrusion of soft template being made to roll form to pressing.
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CN101220561A (en) * | 2008-01-04 | 2008-07-16 | 中国航空工业第一集团公司北京航空材料研究院 | Prefabricated fabric for liquid condition shaping composite material and preparation thereof |
CN101414119A (en) * | 2008-10-28 | 2009-04-22 | 吉林大学 | Method for building sub-micron or nano-scale formwork by micrometre scale formwork |
CN101537682A (en) * | 2009-03-16 | 2009-09-23 | 浙江工业大学 | Method for preparing superhydrophobic surface by using nano-particles for assisting micromolding |
CN102324279A (en) * | 2011-07-21 | 2012-01-18 | 哈尔滨工业大学 | Method for preparing graphene conductive film based on nanometer soft printing technology |
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CN101220561A (en) * | 2008-01-04 | 2008-07-16 | 中国航空工业第一集团公司北京航空材料研究院 | Prefabricated fabric for liquid condition shaping composite material and preparation thereof |
CN101414119A (en) * | 2008-10-28 | 2009-04-22 | 吉林大学 | Method for building sub-micron or nano-scale formwork by micrometre scale formwork |
CN101537682A (en) * | 2009-03-16 | 2009-09-23 | 浙江工业大学 | Method for preparing superhydrophobic surface by using nano-particles for assisting micromolding |
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