CN100418720C - Preparation method of liquid state shaping composite material preshaped body - Google Patents
Preparation method of liquid state shaping composite material preshaped body Download PDFInfo
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- CN100418720C CN100418720C CNB2005100752767A CN200510075276A CN100418720C CN 100418720 C CN100418720 C CN 100418720C CN B2005100752767 A CNB2005100752767 A CN B2005100752767A CN 200510075276 A CN200510075276 A CN 200510075276A CN 100418720 C CN100418720 C CN 100418720C
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Abstract
The present invention relates to a method for preparing a preforming body of liquid state forming composite materials. The method comprises the following steps: a setting agent is dissolved in a certain solvent according to technology dosage; another solvent in which the setting agent can not be dissolved is coated on the surface of a fabric before performing; the solution of the setting agent is coated on the surface of the fabric, and the setting agent mainly disperses on the surface of the fabric after reversed phase precipitation. The present invention can greatly reduce the dosage of the setting agent, overcome the compatibility problem of the setting agent and basal body resin; simultaneously, the present invention can reduce the dosage of harmful solvent, which is favorable to environmental protection; the coating performance of the preforming fabric can not be influenced. Except for satisfying the forming requirement that composite materials is clean or close to clean and making the preforming body obtain a certain degree of integrity, the present invention can satisfy the requirement of enhancing composite material performance, uses thermoplastic resin or setting agent materials containing thermoplastic resin to improve interlaminar toughness, and greatly enhance the compression strength of composite materials after impact.
Description
Invention field: the present invention relates to a kind of preparation method who is used for liquid state shaping composite material preshaped body.
Background of invention: the wing cover structure as aircraft in the aviation main force support structure is big owing to planar dimension, and the toughness reguirements height adopts resin molding osmosis (RFI) moulding usually.And, adopt resin transfer moulding method (RTM) moulding usually in relative size small construction such as the beam of aircraft, bulkheads.The path that corpus fibrosum flows owing to the required dipping of resin in resin molding infusion forming (RFI) process a thickness direction at product, belonging to short distance flows, the shaping viscosity of resin can be higher, and can under higher pressure environment, be shaped when being shaped, thereby both can accomplish higher fiber volume fraction, can adopt viscosity high relatively a lot of again, thereby its toughness may reach the resin system shaping of high tenacity.And resin transfer moulding method (RTM) conduct is a kind of flexible technology, and it can make the part of the large complicated configuration of high fiber volume fraction under lower pressure, and keeps higher structural design efficient.Two kinds of technologies have good complementarity.
Resin transfer molding and resin molding infusion forming are as two kinds of typical process of liquid condition shaping, and wherein a critical process is clean or near clean preform preparation.
Generally speaking, use the main purpose of setting agent to have two: 1. by apply a spot of setting agent at interlayer, make preform have certain globality; 2. to the composite product of complex appearance, must make it before matched moulds, have the shape approaching substantially by presetting technology with end article.
Generally, setting agent is a kind of thermosetting resin, and its consumption accounts for 2～15% of matrix resin consumption, therefore, the compatibility of setting agent and matrix resin is had relatively high expectations.Setting agent is divided into two kinds of forms: powder type and solution form, the pre-setting springback angle that the pre-setting springback angle of powder type is used greater than the solution form, the pre-setting effect is more a bit weaker than the latter, but, setting agent can improve bigger interlayer adhesion when powder type was used, therefore might under the prerequisite that satisfies the pre-setting effect, reduce the consumption of setting agent.Its implementation method is, in certain thermosetting resin (as high molecular expoxy resin), make the setting agent of modification behind a certain proportion of elastomer of adding, then the setting agent of different amounts is coated the one side that strengthens fabric with solution or powder type, fabric is heated make the setting agent fusion and combine with fabric; The fabric that multilayer was handled keeps certain hour after by the rule lay under suitable temperature, pressure condition, make preform become as a whole, and have the profile consistent with die cavity, goes into mould at last, solidifies after injecting resin.Also can adopt thermoplastic resin or elastomeric material to realize the setting agent functionalization as required as shaping material.But no matter be to adopt the solwution method or the typing mode of powder method, all respectively have different pluses and minuses.The former need use a large amount of solvents, and owing to the high osmosis of solution to the pre-setting fabric, most of setting agent mainly is distributed in the fibre bundle, though helping shape like this keeps, but the interlaminar bonding effect is not enough, need to improve the consumption of setting agent, will bring the composite property decline due to setting agent and the matrix resin compatibility thus.And use the powder rule to need expensive pre-setting equipment, and the shop property covered of preformed fabric is relatively poor, can not be well and the die surface attaching.
Because the important function of preform preparation, and presetting technology and matrix injection technology are closely related, studies have shown that: except that satisfy the pre-setting purpose and with matrix resin preferably the compatibility, the vitrification point Tg of setting agent itself also is an important parameter.At first require Tg to be higher than room temperature, guarantee that setting agent is solid-state at normal temperatures, be convenient to preform is carried out technological operation; Tg again can not be too high simultaneously, otherwise be unfavorable for preform is heat-treated to obtain required shape.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of liquid state shaping composite material preshaped body.This method has the advantage of powder method and solwution method concurrently, can obtain satisfied ply adhesion effect under the prerequisite of a large amount of minimizing setting agent consumptions.
Technical solution of the present invention is that setting agent is dissolved in certain solvent by the technology consumption, when pre-setting, apply another kind of solvent at fabric face in advance, this solvent can not dissolve setting agent, then with the setting agent solution coat at fabric face, after anti-phase the separating out, setting agent will mainly be distributed in fabric face.Finish preform shop layer and follow-up liquid condition shaping process based on this.
Its contour machining procedure process is as follows:
1. setting agent formulations prepared from solutions: with setting agent material such as thermosetting resin (unsaturated polyester resin, epoxy resin, cyanate ester resin, bismaleimide resin, polyimide resin, phenolic resins and the curing agent that optionally adds, promoter and other modifier), or thermoplastic resin, or the prepolymer of rubber or thermosetting resin and thermoplastic resin or rubber, or mixture etc. is dissolved in corresponding solvent or solvent system such as dichloroethanes, or carrene, or oxolane, or cyclic ethers, or dioxolane, or dioxane, or acetone, or N-methyl pyrrolidone, or dimethyl formamide, or dimethylacetylamide and composition thereof, obtain finely disseminated solution through stirring or adding thermal agitation, standby after filtering;
2. pre-setting fabric preliminary treatment: according to the dissolution characteristics of setting agent material, select one or more solvents that can not dissolve the setting agent material as the preliminary treatment solvent, the preliminary treatment solvent is distilled water or ethanol or distilled water and ethanolic solution or serves as main contain a small amount of dichloroethanes or carrene or oxolane or cyclic ethers or dioxolane or dioxane or acetone or N-methyl pyrrolidone or dimethyl formamide or dimethylacetylamide and composition thereof with above-mentioned solvent; With the preliminary treatment solvent with spray, pad, mode such as roller coat, brushing soaks into fabric, the used fiber of fabric is composite fortifying fibres commonly used such as carbon fiber, glass fibre, aramid fiber, superhigh molecular weight polyethylene fibers, form of fabric can be woven fabrics such as plain weave, twill, satin weave, through volume, weft-knitted and axial, multidirectional enhancing knitted fabric, non-woven fabric, two dimension two is to, two-dimentional three-dimensional braid;
3. pre-setting fabric setting agent is handled: setting agent solution is distributed in the pre-setting fabric face with sprinkling or modes such as roller coat or brushing, and amount ranges accounts for 1%～15% of fabric side density, decides on fabric construction.Remove solvent or the solvent system that uses in 1 and 2 in modes such as hot plate or drying cylinder or hot-air channel or natural air dryings;
4. preform preparation: the fabric of the 3 surface distributed setting agent materials that obtain is cut, spreads layer by designing requirement, adopt the vacuum bag pressure method moulding, obtain preform.The pre-setting temperature is suitable with the setting agent material melting point.
Advantage of the present invention is:
1. adopted harmless or harmless substantially distilled water, ethanol or the two mixture or based on the mixed solvent of above-mentioned solvent as the preliminary treatment solvent; Fabric is soaked into processing back fabric hole with the preliminary treatment solvent and the pretreated substantially solvent of fabric face occupies, setting agent solution is suppressed the process of osmosis of fabric, can improve the concentration of setting agent solution greatly, reduce the consumption of harmful or slight hazardous solvent;
2. cover above the preliminary treatment solvent owing to setting agent solution, the directional diffusion effect of solvent makes setting agent separate out in that fabric face is anti-phase, thereby mainly be dispersed in fabric face, to improving the adhesive effect between the preform tissue layer and then keeping its globality useful;
3. compare with solwution method, under the suitable condition of the ply adhesion effect of preform, adopt the present invention can reduce the consumption of setting agent, avoid because of degradation problem under the matrix resin performance that the setting agent consumption is big, compatibility causes;
4. because setting agent mainly is distributed in interlayer, comparatively unobstructed in the tissue layer with the interior resin flow channel of fibre bundle, and hole is relatively large between tissue layer, setting agent is not obvious to the influence of interlayer hole, help resin flows, overcome because of the product defect due to the sealing of constricted flow, runner;
5. the requirement of bonded composite performance improvement, part or all of functional modifier such as thermoplastic resin polyether sulfone, polysulfones, polyether-ketone, PEI, polyester, polyamide or elastomeric material or inorganic nano-particle, CNT etc. can be placed the preform interlayer in this way, realize directional profile.
The non-dissolution characteristics that the present invention utilizes setting agent to separate out in the dissolution characteristics and the precipitation of the phase reversal in the non-solvent system of dicyandiamide solution, ingenious will the dissolving with anti-phase two processes is put to process practice on the surface that strengthens fabric, can reduce the setting agent consumption in a large number, overcome the consistency problem of setting agent and matrix resin; Can reduce simultaneously the consumption of hazardous solvent again, help environmental protection; It is unaffected that performance is covered in the shop of preformed fabric.
The specific embodiment
Example one
Setting agent material: epoxy resin and nbr carboxyl terminal performed polymer
Fabric type: 8 pieces of satin weave carbon cloths, fabric side density are 370g/m
2, fiber dimensious: T3003K, solvent: acetone, fabric preliminary treatment solvent: 95% ethanol
It is the 100g/L acetone soln that setting agent is mixed with concentration, after with 200 milliliter of 95% ethanol fabric being carried out preliminary treatment, get 50 milliliters of setting agent solution coat in fabric face, because the fabric hole is that ethanol occupies, the webbing liquid measure is tending towards saturated, therefore the 50ml acetone soln can satisfy the coating needs, after solvent is removed with hot blast, the pre-setting fabric is cut into 200mm * 300mm size, get 6 layers of pre-setting fabric and prepare tabular preform with vacuum bag pressure method, vacuum is-0.08～-0.09Mpa, technological temperature is 85 ℃, cooling and mould unloading after 2 hours, and the preform ply adhesion is good, have certain globality, can carry out burr to it and prune, operations such as dress mould.
Example two
Adopt the present invention and conventional soln legal system to be equipped with preform, condition is with example one.Strengthening fabric type is the G827 one-way fabric, and surface density is 170g/m
2, fiber type is T300 3K.
The closed mould of respectively preform being packed into, connect pressure injection and vacuum system, resin system is the 3266RTM epoxy resin that the Beijing Research Inst. of Aeronautic Material produces, to carrying out pressure injection after resin, mould and the preform deaeration degasification, injection temperature is 60 ℃, finishes curing by 80 ℃, 8 hours+120 ℃, 4 hours technology after finishing.Because setting agent mainly is distributed between tissue layer in the preform of the present invention's preparation, less in the fibre bundle, setting agent is not obvious to the influence of resin flows, adopts the preform of the present invention's preparation the resin mould-filling time can be shortened to 4 hours, and contrast technology is 5.5 hours.The composite property test sees the following form.
| Test event | The present invention | Prior art |
| Bending strength MPa | 1608 | 1599 |
| Bending modulus Gpa | 108 | 109 |
| Interlaminar shear strength MPa | 72.1 | 64.8 |
As can be seen, two kinds of methods are basic identical on bending property, but adopt behind the present invention because setting agent mainly is distributed in interlayer, to improving interlaminal toughness certain help arranged, and interlaminar shear strength increases.
Example three
The setting agent material: polysulfones, solvent: dimethyl formamide, the preliminary treatment solvent: 80% distilled water+20% dimethyl formamide, fabric type are 827 one-way fabrics, and fiber is T3003K, and the RTM resin system is 3266 epoxy resin.Polysulfones is made into 30% (mass percent concentration) solution.After brushing the preliminary treatment solvent on the fabric (consumption is by every square meter fabric 200ml), get 50g polysulfones solution and be coated on fabric face, owing to contain a part of dimethyl formamide in the preliminary treatment solvent, the anti-phase velocity ratio of separating out of polysulfones is slower, can spread operations such as layer, dress mould, closed mould in conjunction with this process, carry out mould immediately and heat up, vacuumize, desolventize, finish the pre-setting operation.Be cooled to 60 ℃, the beginning resin injects, and curing process is with example two.
The composite property test sees the following form.
| Test event | The present invention | Prior art |
| Bending strength MPa | 1567 | 1599 |
| Bending modulus GPa | 102 | 109 |
| Interlaminar shear strength MPa | 86 | 64.8 |
| Impact back compressive strength MPa | 210 | 120 |
From experimental result, employing the present invention can take into account pre-setting and toughening modifying, and compressive strength had significantly raising after the interlaminar shear strength and the impact back compressive strength of composite were especially impacted.
Example four
Setting agent material: 20 parts of 50 parts+modified polyarylether ketone of bisphenol-A epoxy (epoxide number 0.54N/100g) 40 parts+diphenyl-methane, four glycidyl amines (epoxide number 0.80N/100g), solvent: 80% acetone+20% oxolane, be made into 30% (mass percent concentration), fabric preliminary treatment solvent: 80% distilled water+20% oxolane, press example three preparation preforms.The resin molding material is formed: 50 parts of 50 parts+modified polyarylether ketone of bisphenol-A epoxy (epoxide number 0.54N/100g) 40 parts+diphenyl-methane, four glycidyl amines (epoxide number 0.80N/100g), 20 parts+two amido diphenyl sulphone (DPS)s mix the back with each component and prepare resin molding with hot melt.
Reinforcing material: 827 unidirectional carbon cloths, fiber type: T300-3K
The laying in mould with resin molding and fiber preform, (vacuum keeps to make resin fusing and impregnation of fibers preform under heating (120 ℃) pressurization (0.5MPa), vacuum-0.08～-0.09Mpa), be heated to 180 ℃ under (0.5MPa) condition in pressurization and be cooled to 60 ℃ of exoneration moulds down after making resin solidification 2h.
Composite materials property (V
f=55%) sees the following form.
| Bending strength MPa | 1600 |
| Bending modulus Gpa | 132 |
| Interlaminar shear strength MPa | 88 |
| Impact back compressive strength MPa | 256 |
Claims (5)
1. the preparation method of a liquid state shaping composite material preshaped body is characterized in that, preparation technology's method is,
(1) preparation setting agent solution, it is 5%～30% solution that thermosetting resin or thermoplastic resin and corresponding solvent are mixed into mass percent concentration, standby;
(2) fabric preliminary treatment is chosen the solvent that can not dissolve the setting agent material and is soaked at fabric face;
(3) with setting agent spray solution or roller coat or brush on the fabric that has soaked into the preliminary treatment solvent, amount ranges accounts for 1%～15% of fabric side density;
(4) fabric with surface distributed setting agent material cuts, spreads layer by designing requirement, adopts the vacuum bag pressure method moulding, obtains preform.
2. the preparation method of liquid state shaping composite material preshaped body according to claim 1, it is characterized in that the preliminary treatment solvent one of is meant in distilled water and the ethanol and the mixing of dichloroethanes or carrene or oxolane or cyclic ethers or dioxolane or dioxane or acetone or N-methyl pyrrolidone or dimethyl formamide or dimethylacetylamide.
3. the preparation method of liquid state shaping composite material preshaped body according to claim 1, it is characterized in that the thermosetting resin of setting agent material is unsaturated polyester resin, epoxy resin, cyanate ester resin, bismaleimide resin, polyimide resin or phenolic resins.
4. the preparation method of the liquid state shaping composite material preshaped body that requires according to right 1, it is characterized in that, the requirement of bonded composite performance improvement, with part or all of functional modifier promptly: thermoplastic resin or elastomeric material or inorganic nano-particle or CNT place the preform interlayer, improve the anti-low velocity impact performance of composite interlayer toughness and composite, wherein, thermoplastic resin is meant, polyether sulfone, polysulfones, polyether-ketone, PEI, polyester or polyamide.
5. the preparation method of the liquid state shaping composite material preshaped body that requires according to right 1, it is characterized in that, the preform form of fabric is following arbitrary form of fabric: (1) plain weave or twill or satin weave woven fabric, (2) through volume, weft-knitted and axial, multidirectional enhancing knitted fabric, (3) non-woven fabric, (4) two dimension two is to, two-dimentional three-dimensional braid, and the used fiber of fabric is carbon fiber, glass fibre, aramid fiber, superhigh molecular weight polyethylene fibers composite fortifying fibre commonly used.
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| CN101220561B (en) * | 2008-01-04 | 2010-09-08 | 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 |
| CN101775151B (en) * | 2009-01-13 | 2012-01-11 | 姜白燕 | Composite sheet consisting of thermoplastic resin and fiber and manufacturing method thereof |
| CN102707373A (en) * | 2010-12-10 | 2012-10-03 | 中国航空工业集团公司北京航空材料研究院 | Composite-material braided prefabricated filling belt and preparation method of composite-material braided prefabricated filling belt |
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| CN102514116B (en) * | 2011-11-22 | 2014-07-02 | 中国航空工业集团公司北京航空材料研究院 | Method for shaping and toughening fiber reinforced composite material |
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| CN104816491B (en) * | 2015-02-04 | 2017-02-22 | 中航复合材料有限责任公司 | Preparation method for RTM preforms with angular structures |
| CN107160709B (en) * | 2017-06-30 | 2019-08-13 | 沈阳航空航天大学 | A kind of method and rudder face of composite liquid molding ultra light aircraft rudder face |
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