CN102815958B - Preparation method of ceramizable resin matrix composite material - Google Patents
Preparation method of ceramizable resin matrix composite material Download PDFInfo
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- CN102815958B CN102815958B CN 201210309114 CN201210309114A CN102815958B CN 102815958 B CN102815958 B CN 102815958B CN 201210309114 CN201210309114 CN 201210309114 CN 201210309114 A CN201210309114 A CN 201210309114A CN 102815958 B CN102815958 B CN 102815958B
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Abstract
Belonging to the technical field of composite materials, the invention discloses a preparation method of a ceramizable resin matrix composite material. The method includes: selecting an appropriate reinforcing material and ceramizable additive-containing resin, then dipping the reinforcing material into a resin adhesive solution, and when the reinforcing material is evenly dipped, placing the reinforcing material into a die, and conducting heating pressing to mold the composite material. The ceramizable additive within the composite material can have chemical change at a temperature higher than 600DEG C so as to form ceramics, thus greatly improving the ablation resistance of the composite material, reducing the shortcomings of excessive ablation and interlaminar cracking in high temperature resin matrix composite materials, reducing the production cycle and material cost, as well as substantially improving the machining properties of ceramic materials.
Description
Technical field
The invention belongs to technical field of composite materials, but particularly a kind of preparation method of ceramic polymer matrix composites.
Background technology
Aircraft carries out gliding type maneuvering flight on a large scale in the endoatmosphere, environment when its Working environment belongs to typical middle temperature, long boat, the large area region temperature is in 600 ℃～1200 ℃ scopes, common ablative-type protective coating polymer matrix composites ablation amount under this Working environment is excessive, can not satisfy the requirement of aircraft aerodynamic configuration.
But the ceramic polymer matrix composites are a kind of novel heat insulation materials, but it is to add the ceramic additive in the anti-Ablative resin of new type high temperature, the matrix material of the molding mode preparation by dipping and compacting.In low thermophase, rely on the ablation resistance solar heat protection of anti-Ablative resin self; After but envrionment temperature surpassed material ceramic temperature spot, material carried out ceramic and changes, and relied on stupalith self thermotolerance to play the thermal protection effect.But because but the density of present ceramic polymer matrix composites is 1.6g/cm
3～1.7g/cm
3, thermal conductivity is 0.6W(mK
-1), can't satisfy the demand of preventing heat-insulation integrative; Although ceramic matric composite has high temperature resistant, oxidation resistant characteristics simultaneously, its cost is high, thermal conductivity is high, anti-heat insulation structural design is complicated, and large-area applications is subject to certain limitation.
Summary of the invention
The purpose of this invention is to provide a kind of can heat-insulation integrative, but and the preparation method of ceramic polymer matrix composites that can large-area applications.
The technical solution adopted in the present invention is:
But a kind of preparation method of ceramic polymer matrix composites comprises the following steps:
(1) silane coupling agent is dissolved with solvent, but the ceramic additive is added in silane coupler solution, stir under 60～80 ℃, until without reuniting, filter and dry desolventizing, but obtain the ceramic additive of surface modification;
(2) anti-Ablative resin is dissolved with solvent, with step (1) but the ceramic additive of the surface modification that obtains join in the solution of anti-the Ablative resin, both are mixed, but make the ceramic resin adhesive liquid, but but there are not ceramic additive or other visible impurity of reunion in the ceramic resin adhesive liquid;
(3) with step (2) but the ceramic resin adhesive liquid lay-up that obtains dry after thorough strongthener dipping is all even;
(4) strongthener that step (3) dipping is obtained is put in mould, with the mould matched moulds, is to carry out under 0～80 ℃ in temperature by pressuring method during matched moulds;
(5) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h;
(6) solidify complete after, the demoulding when mould is down to room temperature, but and the overlap of polishing ceramic polymer matrix composites.
Preferably, described strongthener is fibre integral fabric.
Further, when described strongthener was the staple length yarn, its preparation method was:
(1) silane coupling agent is dissolved with solvent, but ceramic additive and low density filler are added in silane coupler solution, stir at 60～80 ℃ of temperature, until without till reuniting, carry out dry desolventizing, but obtain the ceramic additive of surface modification;
(2) anti-Ablative resin is dissolved with solvent, with step (1) but ceramic additive and the low density filler of the surface modification that obtains join in the solution of anti-the Ablative resin, both are mixed, but make the ceramic resin adhesive liquid, but but there are not ceramic additive or other visible impurity of reunion in the ceramic resin adhesive liquid;
(3) the staple length yarn is put into step (2) but in the ceramic resin adhesive liquid that obtains, stir and rub, requiring the mix and blend time is 50min～60min, and per minute mixes and is no less than 20 times, needs to guarantee that the staple length yarn is infiltrated evenly by the ceramic resin adhesive liquid but mix after complete;
(4) will flood good staple length yarn and evenly spread out, the silk weight≤100g of group of staple length yarn is fluffy, and the interval that 10mm～20mm should be arranged between silk group, then be placed in 15 ℃～30 ℃, dry in the environment of the ventilation cleaning of humidity≤75%, the time of drying is no less than 24h;
(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and after tearing, maximum pack is no more than 20;
(6) the silk group that step (5) dipping is obtained, with the mould matched moulds, carries out insulation 1h by one one, put in mould uniformly under 60～80 ℃ during matched moulds by pressuring method;
(7) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h;
(8) solidify complete after, naturally cool to the demoulding when being not less than 30 ℃ until mould, but and the overlap of polishing ceramic polymer matrix composites.
Preferably, described solvent is dehydrated alcohol or acetone.
Preferably, described step (3) can be carried out under the environment of vacuum or pressurization.
Further, the mould in described (4) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
Further, the mould in described (6) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
Further, in the process that described intensification is solidified, the mold cavity size does not change.
Preferably, described low density filler is hollow glass micropearl, hollow silicon dioxide microballoon or hollow phenolic aldehyde microballoon.
Further, described step (4) is: will flood good staple length yarn and evenly spread out and be placed on the desk that is covered with clean plastic cloth, silk weight≤the 100g of group of staple length yarn, fluffy, and the interval that 10mm～20mm should be arranged between silk group, then be placed in 15 ℃～30 ℃, dry in the environment of the ventilation cleaning of humidity≤75%, the time of drying is no less than 24h.
The present invention has the following advantages:
But utilize the ceramic polymer matrix composites that method of the present invention prepares to have advantages of light weight, high-strength, anti-ablation and heat insulation, under＞600 ℃ of high temperature aerobic environments, but the ceramic additive is realized the ceramic transformation, and material converting is resistant to elevated temperatures fiber reinforced ceramic composite.But and the ceramic polymer matrix composites by the preparation of this forming method, need not to change existing moulding process, equipment and mould, production cycle, cost, workability and thermal insulation all are better than ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
Description of drawings
The invention will be further described below in conjunction with accompanying drawing.
But the structural representation of mould matched moulds in the preparation method of a kind of ceramic polymer matrix composites that Fig. 1 provides for the embodiment of the present invention 1;
But the structural representation of mould matched moulds in the preparation method of a kind of low density ceramic polymer matrix composites that Fig. 2 provides for the embodiment of the present invention 2.
Embodiment
But the preparation method of ceramic polymer matrix composites 2 comprises the following steps:
(1) silane coupling agent is dissolved with dehydrated alcohol, but the ceramic additive is added in silane coupler solution, stir under 60 ℃, until without reuniting, filter and dry desolventizing, but obtain the ceramic additive of surface modification, but the ceramic additive is the mixture of silicate, nitride, carbide;
(2) anti-Ablative resin is dissolved with dehydrated alcohol, with step (1) but the ceramic additive of the surface modification that obtains join in the solution of anti-the Ablative resin, both are mixed, but make the ceramic resin adhesive liquid, but but there are not ceramic additive or other visible impurity of reunion in the ceramic resin adhesive liquid;
(3) under vacuum environment, with step (2) but the ceramic resin adhesive liquid impregnation of fibers integral fabric that obtains dry after thorough fibre integral fabric dipping is all even;
(4) with reference to Fig. 1, the fibre integral fabric that step (3) dipping obtains is put in mould 1,, at room temperature carry out during matched moulds mould 1 matched moulds by pressuring method, before the dress mould in the die cavity of mould 1 even wiping releasing agent;
(5) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h, heat up in the process of solidifying, the mold cavity size does not change;
(6) solidify complete after, the demoulding when mould 1 is down to room temperature, but and the overlap of polishing ceramic polymer matrix composites 2.
But the ceramic polymer matrix composites of moulding have the high-strength light characteristic of fiber reinforced polymer composites at normal temperatures as stated above, under＞600 ℃ of high temperature aerobic environments, but the ceramic additive is realized the ceramic transformation, and material converting is resistant to elevated temperatures fiber reinforced ceramic composite.But and pass through the ceramic polymer matrix composites that this forming method prepares, and cost is relatively low, and workability and structural safety performance are better than ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
When strongthener is the staple length yarn, but the preparation method of low density ceramic polymer matrix composites 4 is:
(1) silane coupling agent is dissolved with acetone, but ceramic additive and hollow silicon dioxide microballoon are added in silane coupler solution, stir at 80 ℃ of temperature, until without till reuniting, carry out dry desolventizing, but obtain the ceramic additive of surface modification;
(2) anti-Ablative resin is dissolved with acetone, with step (1) but ceramic additive and the hollow silicon dioxide microballoon of the surface modification that obtains join in the solution of anti-the Ablative resin, both are mixed, but make the ceramic resin adhesive liquid, but but there are not ceramic additive or other visible impurity of reunion in the ceramic resin adhesive liquid;
(3) under pressurized conditions, in the ceramic resin adhesive liquid that the staple length yarn is put into step (2) but obtains, stir and rub, requiring the mix and blend time is 50min, per minute mixes and to be no less than 20 times, needs to guarantee that the staple length yarn is infiltrated evenly by the ceramic resin adhesive liquid but mix after complete;
(4) will flood good staple length yarn evenly spreads out and is placed on the desk that is covered with clean plastic cloth, silk weight≤the 100g of group of staple length yarn, fluffy, and the interval that 20mm should be arranged between silk group, then be placed in 15 ℃, dry in the environment of the ventilation cleaning of humidity≤75%, the time of drying is no less than 24h;
(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and after tearing, maximum pack is no more than 20;
(6) with reference to Fig. 2, the silk that step (5) dipping obtains is rolled into a ball, one one, put in mould 3 uniformly, by pressuring method with mould 3 matched moulds, carry out under 60 ℃ during matched moulds, insulation 1h evenly sprays releasing agent in the die cavity of mould 3 before the dress mould, the device of exerting pressure is press 5;
(7) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h;
(8) solidify complete after, naturally cool to the demoulding when being not less than 30 ℃ until mould, but and the overlap of polishing ceramic polymer matrix composites 4.
But the low density ceramic polymer matrix composites of moulding have advantages of light weight, high-strength, anti-ablation and heat insulation as stated above, under＞600 ℃ of high temperature aerobic environments, but the ceramic additive is realized the ceramic transformation, and material converting is that resistant to elevated temperatures staple fibre strengthens ceramic composite.But and the low density ceramic polymer matrix composites by the preparation of this forming method, need not to change existing moulding process, equipment and mould, production cycle, cost, workability and thermal insulation all are better than ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
Above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (10)
1. but the preparation method of ceramic polymer matrix composites, is characterized in that, comprises the following steps:
(1) silane coupling agent is dissolved with solvent, but the ceramic additive is added in silane coupler solution, stir under 60～80 ℃, until without reuniting, filter and dry desolventizing, but obtain the ceramic additive of surface modification;
(2) anti-Ablative resin is dissolved with solvent, with step (1) but the ceramic additive of the surface modification that obtains join in the solution of anti-the Ablative resin, both are mixed, but make the ceramic resin adhesive liquid, but but there are not ceramic additive or other visible impurity of reunion in the ceramic resin adhesive liquid;
(3) with step (2) but the ceramic resin adhesive liquid lay-up that obtains dry after thorough strongthener dipping is all even;
(4) strongthener that step (3) dipping is obtained is put in mould, with the mould matched moulds, is to carry out under 0～80 ℃ in temperature by pressuring method during matched moulds;
(5) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h;
(6) solidify complete after, the demoulding when mould is down to room temperature, but and the overlap of polishing ceramic polymer matrix composites.
2. but the preparation method of ceramic polymer matrix composites according to claim 1, is characterized in that, described strongthener is fibre integral fabric.
3. but the preparation method of ceramic polymer matrix composites according to claim 1, is characterized in that, when described strongthener was the staple length yarn, its preparation method was:
(1) silane coupling agent is dissolved with solvent, but ceramic additive and low density filler are added in silane coupler solution, stir at 60～80 ℃ of temperature, until without till reuniting, carry out dry desolventizing, but obtain the ceramic additive of surface modification;
(2) anti-Ablative resin is dissolved with solvent, with step (1) but ceramic additive and the low density filler of the surface modification that obtains join in the solution of anti-the Ablative resin, the three is mixed, but make the ceramic resin adhesive liquid, but but there is not the ceramic additive of reunion in the ceramic resin adhesive liquid;
(3) the staple length yarn is put into step (2) but in the ceramic resin adhesive liquid that obtains, stir and rub, requiring the mix and blend time is 50min～60min, and per minute mixes and is no less than 20 times, needs to guarantee that the staple length yarn is infiltrated evenly by the ceramic resin adhesive liquid but mix after complete;
(4) will flood good staple length yarn and evenly spread out, the silk weight≤100g of group of staple length yarn is fluffy, and the interval that 10mm～20mm should be arranged between silk group, then be placed in 15 ℃～30 ℃, dry in the environment of the ventilation cleaning of humidity≤75%, the time of drying is no less than 24h;
(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and after tearing, maximum pack is no more than 20;
(6) the silk group that step (5) dipping is obtained, with the mould matched moulds, carries out insulation 1h by one one, put in mould uniformly under 60～80 ℃ during matched moulds by pressuring method;
(7) according to the curing cycle of anti-Ablative resin, the curing that heats up, described curing cycle is: be incubated 1h under 90 ℃, 1h to 110 ℃ of intensification; Be incubated 1h under 110 ℃, 1h to 140 ℃ of intensification; Be incubated 1h under 140 ℃, 1h to 180 ℃ of intensification; Be incubated 2h under 180 ℃, 1h to 200 ℃ of intensification; At 200 ℃ of insulation 1h;
(8) solidify complete after, naturally cool to the demoulding when being not less than 30 ℃ until mould, but and the overlap of polishing ceramic polymer matrix composites.
4. but the preparation method of according to claim 1 or 3 described ceramic polymer matrix composites, is characterized in that, described solvent is dehydrated alcohol or acetone.
5. but the preparation method of according to claim 1 or 3 described ceramic polymer matrix composites, is characterized in that, described step (3) can be carried out under the environment of vacuum or pressurization.
6. but the preparation method of ceramic polymer matrix composites according to claim 1, is characterized in that, the mould in described (4) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
7. but the preparation method of ceramic polymer matrix composites according to claim 3, is characterized in that, the mould in described (6) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
8. but the preparation method of according to claim 1 or 3 described ceramic polymer matrix composites, is characterized in that, in the process that described intensification is solidified, the mold cavity size does not change.
9. but the preparation method of ceramic polymer matrix composites according to claim 3, is characterized in that, described low density filler is hollow glass micropearl, hollow silicon dioxide microballoon or hollow phenolic aldehyde microballoon.
10. but the preparation method of ceramic polymer matrix composites according to claim 3, it is characterized in that, described step (4) is: will flood good staple length yarn and evenly spread out and be placed on the desk that is covered with clean plastic cloth, silk weight≤the 100g of group of staple length yarn, fluffy, and the interval of 10mm～20mm should be arranged between silk group, then be placed in 15 ℃～30 ℃, dry in the environment of the ventilation cleaning of humidity≤75%, the time of drying is no less than 24h.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449825A (en) * | 2013-08-19 | 2013-12-18 | 航天特种材料及工艺技术研究所 | Micro-ablation insulating material and preparation method thereof |
| CN103540155B (en) * | 2013-09-29 | 2016-02-10 | 湖北三江航天红阳机电有限公司 | A kind of preparation method of resistant to elevated temperatures Ablative resin based composites |
| CN109486201B (en) * | 2018-09-13 | 2021-03-23 | 沈阳理工大学 | Self-crosslinking type silicon-boron-containing high polymer-based ablation-resistant heat-insulating material and preparation method thereof |
| CN109294238B (en) * | 2018-09-13 | 2021-03-16 | 沈阳理工大学 | Light high-elastic ablation-resistant heat-insulating material and preparation method thereof |
| CN110194609B (en) * | 2019-04-22 | 2021-07-16 | 湖南远辉新材料研究院有限公司 | High-temperature-resistant and oxidation-resistant ceramizable resin composite material and preparation method thereof |
| CN111349306A (en) * | 2020-03-16 | 2020-06-30 | 武汉理工大学 | Ceramizable phenolic resin and preparation method and application thereof |
| CN112064357B (en) * | 2020-08-27 | 2022-10-14 | 航天特种材料及工艺技术研究所 | Ablation-resistant silicone resin composite material and preparation method thereof |
| CN112662311B (en) * | 2020-12-07 | 2021-10-01 | 上海航天设备制造总厂有限公司 | Light high-silicon ceramic resin coating, ceramic coating and preparation method thereof |
| CN117165248B (en) * | 2023-10-31 | 2024-02-23 | 南京艾布纳新材料股份有限公司 | Multi-curing polyurethane ceramic sealant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101939359A (en) * | 2007-10-22 | 2011-01-05 | 弗莱克斯伯陶器公司 | Fire resistant flexible ceramic resin blend and composite products formed therefrom |
| CN102558666A (en) * | 2010-12-28 | 2012-07-11 | 上海金发科技发展有限公司 | Ceramic fiber reinforced polypropylene complex and preparation method thereof |
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2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101939359A (en) * | 2007-10-22 | 2011-01-05 | 弗莱克斯伯陶器公司 | Fire resistant flexible ceramic resin blend and composite products formed therefrom |
| CN102558666A (en) * | 2010-12-28 | 2012-07-11 | 上海金发科技发展有限公司 | Ceramic fiber reinforced polypropylene complex and preparation method thereof |
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