CN102514116A - Method for shaping and toughening fiber reinforced composite material - Google Patents
Method for shaping and toughening fiber reinforced composite material Download PDFInfo
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- CN102514116A CN102514116A CN2011103769479A CN201110376947A CN102514116A CN 102514116 A CN102514116 A CN 102514116A CN 2011103769479 A CN2011103769479 A CN 2011103769479A CN 201110376947 A CN201110376947 A CN 201110376947A CN 102514116 A CN102514116 A CN 102514116A
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Abstract
The invention belongs to the technical field of composite material, and relates to a method for shaping and toughening a fiber reinforced composite material. In the invention, polyimide foam powder (such as poly tetracid diester diamide, polyimide foam precursor) are used for shaping and toughening a continuous fiber reinforced composite material; after the polyimide foam powder is uniformly dispersed on fiber fabric, the powder can be bonded onto the surface of the fabric when heated at a certain temperature; and when the powder is foamed at a higher temperature, the powder and the surface of the fabric can be mutually spliced, penetration bonding can be caused on fiber surface and a bridge structure is formed in situ, thus shaping and toughing effects are realized at the same time. The formed toughening bridge structure has the characteristics of high temperature tolerance and insolubility, and the problem of flowing difficulty in RTM (released to manufacturing) glue injection caused by overhigh viscosity is not caused.
Description
Technical field
The invention belongs to field of compound material, relate to a kind of typing of fibre reinforced composites and toughness reinforcing method.
Background technology
Layer closes the interlayer faults toughness of thermosetting resin based composites mainly through the especially toughness reinforcing realization of interlayer resin matrix of resin matrix.The toughness of material and its chemical constitution, micro-structural are relevant, have four kinds of toughening mechanism to be used in material toughness reinforcing, that is: viscoelastic flow, micro-crack and be full of cracks, crackle grappling bridge, crack deflection.There have following several method to be applied to the chain extension of (1) thermosetting resin in succession to be toughness reinforcing or to form inierpeneirating network structure toughness reinforcing; (2) mix rubber particles, thermoplastic resin, two-phase or multiphase structure of generation that is separated of utilizing chemical reaction to induce is toughness reinforcing, has comprised " offing normal " method for toughening that " original position " and new development are come out; (3) utilize the rigid inorganic particle of micrometer/nanometer yardstick to carry out toughness reinforcing.On international forward position, study often structure fiber and the micro-nano hybrid structure of CNT are arranged, utilize numerator self-assembly technique to form to grow firm bar structure and vermicular texture etc.
At present, for the method for studying often on the international forward position, although some method toughening effect is outstanding especially; But practical application has certain difficulty; As construct fiber and the micro-nano hybrid structure of CNT, and the harsh process time of operating condition is long, and just rod is toughness reinforcing for utilizing numerator self-assembly technique to grow up; System gel after forming the molecule self-organizing structures is difficult to moulding.For traditional method, toughness reinforcing toughness is then relevant with crosslink density with to form inierpeneirating network structure toughness reinforcing like chain extension, and the result that toughness improves system viscosity often becomes big, solidfied material rigidity and descends.The rigid inorganic particle toughening is the ubiquity dispersion problem then, also is unfavorable for being used for the RTM moulding.
With the closely-related technology of the present invention be above-mentioned (2), promptly utilize and mix rubber particles, thermoplastic resin, the heterogeneous structure that utilizes this toughness material to form is toughness reinforcing.For tradition " original position " method for toughening; The system viscosity becomes big after mixing resin; Can not or be difficult to use in the RTM moulding; New development is come out, and (Chinese CN101220561 CN101760965A) has avoided this problem to " offing normal " toughening technology to a certain extent, through adding one deck toughened film in the composite material forming process; Do not reduce other mechanical properties through the multi-level heterogeneous toughness reinforcing phase structure of interlayer behind the curing molding; And impact strength (CAI) improves more than 100% after making the compression of composite, but the dissolubility of thermoplastic resin is required relatively harsher, then in the injecting glue process, causes tackify to be difficult to flow and is washed away and disperse unequal phenomenon if thermoplastic resin has certain solubility in thermosetting resin.Like the patent No. is that WO9009410-A etc. is that particle dispersion is added interlayer toughened; Also closely related with this patent; But thisly dispersed thermoplastic granulates is added the back grain structure change hardly, still be present in the composite interlayer that finally obtains, can not play infiltration or adhesion work to the fiber of levels in order to reach better toughening effect with original pattern with pattern; And most particles are subsphaeroidal polyhedron, and the two-phase interface area of formation is less relatively.
Summary of the invention
The objective of the invention is to propose a kind of typing of the fibre reinforced composites that help promoting composite material toughness and toughness reinforcing method.Technical solution of the present invention is:
Caking property when (1) utilizing the foaming of polyimides foam powder is as the typing of composite;
(2) utilize the foaming of polyimides foam powder interlayer to form the adhesion micro-structural as the interlayer toughened structure; The steps include:
(a) the polyimides foam powder evenly is sprinkling upon fabric surface, surface density is 3～30g/m
2, environment temperature is a room temperature; Through 50～200 ℃ heating, be 1～60s heat time heating time, obtains the fabric of appendix foam powder;
(b) the fabric shop layer with appendix foam powder obtains precast body; The precast body that the shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 250～300 ℃; The polyimides foam powder is fully foamed, and form the TPI portal structure of toughness reinforcing usefulness at interlayer.
Used foam powder can be various tetracid diester di-ammonium salts, the polyamic acid foam precursors of gathering in the polyimides foam powder; Powder particle is 1～50 μ m, and solvent is 1%～40%, and solvent is methyl alcohol, ethanol, N; Dinethylformamide, N, the N-dimethylacetylamide
Advantage and beneficial effect that the present invention has are that the present invention utilizes foam powder to be used for the typing of fibre reinforced composites and toughness reinforcing method.Foam powder is dispersed on the fabric; Powder has caking property when uniform temperature heats; Can obtain the fabric of appendix setting agent, and can be used as the layer typing of material shop, when foam powder foams at higher temperature; Appendix foam powder particle expands, bonding and can the infiltration bonding take place each other at fiber surface, form portal structure at interlayer.This portal structure plays toughening effect at the interlayer of composite, has the high and undissolved characteristics of temperature tolerance, does not cause in the further RTM injecting glue the excessive and problem of flow difficulties of viscosity.
The characteristic that the present invention softens formation micmstructure of polymer when having caking property and foaming when utilizing the foaming powder foaming is as the interlayer toughened agent; With respect to method for toughening in the past; Flexibilizer plays typing and toughness reinforcing effect simultaneously; And be unlikely to flowing of the system that has influence on because of the toughened thermoplastic polymer dissolution being used for the RTM production technology; Foaming forms interlayer thermoplasticity bridge crosslinking structure also has bigger surface area with respect to filling in toughening layer purely, the rigidity of also favourable increase interlayer toughened structure.The used method of method of the present invention is operated fairly simple, and the range of choice of polyimides foam powder is wider, and the polyimides thermoplastic structure heat resistance that obtains after the foaming is high, satisfies the requirement of large-scale application.
The present invention utilizes the polyimides foam powder (as to gather tetracid diester diamides; The polyimide foam presoma), uniform temperature has certain caking property when heating; Can be used as material and tentatively finalize the design, when the higher temperature imidization is foamed, as forming the process of foams behind the common powder foam; The foam powder particle expands, bonding and can the infiltration bonding take place each other at fiber surface, form portal structure at interlayer.Rubber or thermoplastic particles are toughness reinforcing different to be with mixing; Foam powder has the characteristic of caking property and foaming formation structure; What the method for toughening of " offing normal " was different is, thermoplastic resin is need be under specified temp not solvable through the chemical induction formation micro-structural that is separated.
The specific embodiment
Caking property when the present invention (1) utilizes the foaming of polyimides foam powder is as the typing of composite; (2) utilize the foaming of polyimides foam powder interlayer to form the adhesion micro-structural as the interlayer toughened structure;
The steps include:
(a) the polyimides foam powder evenly is sprinkling upon fabric surface, surface density is 3～30g/m
2, environment temperature is a room temperature; Through 50～200 ℃ heating, be 1～60s heat time heating time, obtains the fabric of appendix foam powder;
(b) the fabric shop layer with appendix polyimides foam powder obtains precast body; The precast body that the shop layer is obtained places baking oven; Adopt the method for vacuum bag compression set type; Be heated to 250～300 ℃, the polyimides foam powder is fully foamed, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Below introduce embodiments of the invention:
Embodiment 1:
(1) be that polyimides foam powder as follows is ground into about 5 μ m the Powdered of size with structural formula, methanol content is 10% in the foam powder, is dispersed in the continuous carbon fibre fabric face, and surface density is 10g/m
2, environment temperature is a room temperature; Behind 180 ℃ heating region 5s, obtain the fabric of appendix foam powder.
When (2) the shop layer is finalized the design; The precast body that shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 300 ℃ and kept 1 hour; Make the abundant imidization foaming of polyimides foam powder, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Embodiment 2:
(1) be that polyimides foam powder as follows is ground into about 20 μ m the Powdered of size with structural formula, ethanol content is 30% in the foam powder, is dispersed in the continuous carbon fibre fabric face, and surface density is 25g/m
2, environment temperature is a room temperature; Behind 160 ℃ heating region 15s, obtain the fabric of appendix foam powder.
When (2) the shop layer is finalized the design; The precast body that shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 280 ℃ and kept 1.5 hours; Make the abundant imidization foaming of polyimides foam powder, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Embodiment 3:
(1) be that polyimides foam powder as follows is ground into about 40 μ m the Powdered of size with structural formula, solvent DMF content is 15% in the foam powder, is dispersed in the continuous carbon fibre fabric face, and surface density is 25g/m
2, environment temperature is a room temperature; Behind 180 ℃ heating region 30s, obtain the fabric of appendix foam powder.
When (2) the shop layer is finalized the design; The precast body that shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 250 ℃ and kept 2 hours; Make the abundant imidization foaming of polyimides foam powder, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Embodiment 4:
(1) be that polyimides foam powder as follows is ground into about 2 μ m the Powdered of size with structural formula, methanol content is 40% in the foam powder, is dispersed in the continuous carbon fibre fabric face, and surface density is 5g/m
2, environment temperature is a room temperature; Behind 140 ℃ heating region 10s, obtain the fabric of appendix foam powder.
When (2) the shop layer is finalized the design; The precast body that shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 280 ℃ and kept 0.5 hour; Make the abundant imidization foaming of polyimides foam powder, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Embodiment 5:
(1) be that polyimides foam powder as follows is ground into about 25 μ m the Powdered of size with structural formula, solvent DMAc content is 20% in the foam powder, is dispersed in the continuous carbon fibre fabric face, and surface density is 20g/m
2, environment temperature is a room temperature; Behind 160 ℃ heating region 50s, obtain the fabric of appendix foam powder.
When (2) the shop layer is finalized the design; The precast body that shop layer is obtained places baking oven, adopts the method for vacuum bag compression set type, is heated to 300 ℃ and kept 1 hour; Make the abundant imidization foaming of polyimides foam powder, and form the thermoplastic polymer portal structure of toughness reinforcing usefulness at interlayer.
Claims (2)
1. the typing of fibre reinforced composites and toughness reinforcing method is characterized in that:
Caking property when (1) utilizing the foaming of polyimides foam powder is as the typing of composite;
(2) utilize the foaming of polyimides foam powder interlayer to form the adhesion micro-structural as the interlayer toughened structure; The steps include:
(a) the polyimides foam powder evenly is sprinkling upon fabric surface, surface density is 3～30g/m
2, environment temperature is a room temperature; Through 50～200 ℃ heating, be 1～60s heat time heating time, obtains the fabric of appendix foam powder;
(b) the fabric shop layer with appendix polyimides foam powder obtains precast body; The precast body that the shop layer is obtained places baking oven; Adopt the method for vacuum bag compression set type; Be heated to 250～300 ℃, the polyimides foam powder is fully foamed, and form the TPI portal structure of toughness reinforcing usefulness at interlayer.
2. the typing of a kind of fibre reinforced composites according to claim 1 and toughness reinforcing method; It is characterized in that: used foam powder is various tetracid diester di-ammonium salts, the polyamic acid foam precursors of gathering in the polyimides foam powder, and powder particle is 1～50 μ m, and heating-up temperature is 250～300 ℃; Solvent is 1%～40%; Solvent is methyl alcohol, ethanol, N, dinethylformamide, N, N-dimethylacetylamide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110376947.9A CN102514116B (en) | 2011-11-22 | 2011-11-22 | Method for shaping and toughening fiber reinforced composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110376947.9A CN102514116B (en) | 2011-11-22 | 2011-11-22 | Method for shaping and toughening fiber reinforced composite material |
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| CN102514116A true CN102514116A (en) | 2012-06-27 |
| CN102514116B CN102514116B (en) | 2014-07-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897058A (en) * | 2021-09-10 | 2022-01-07 | 航天材料及工艺研究所 | High-strength polyimide foam and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686696A (en) * | 2005-06-10 | 2005-10-26 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation method of liquid state shaping composite material preshaped body |
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- 2011-11-22 CN CN201110376947.9A patent/CN102514116B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686696A (en) * | 2005-06-10 | 2005-10-26 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation method of liquid state shaping composite material preshaped body |
Non-Patent Citations (2)
| Title |
|---|
| 《POLYMER COMPOSITES》 19990630 V.E.YUDIN，J.U.OTAIGBE，V.N.ARTEMIEVA， "Processing and Properties of New High-Temperature，Lightweight Composites Based on Foam Polyimide Binder" 337-345 1-2 第20卷, 第3期 * |
| V.E.YUDIN，J.U.OTAIGBE，V.N.ARTEMIEVA，: ""Processing and Properties of New High-Temperature，Lightweight Composites Based on Foam Polyimide Binder"", 《POLYMER COMPOSITES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897058A (en) * | 2021-09-10 | 2022-01-07 | 航天材料及工艺研究所 | High-strength polyimide foam and preparation method thereof |
| CN113897058B (en) * | 2021-09-10 | 2023-11-10 | 航天材料及工艺研究所 | High-strength polyimide foam and preparation method thereof |
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| CN102514116B (en) | 2014-07-02 |
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