CN102658261B - Method for preparing resin-base composite material thermal protection structure from modified resin by vapor deposition process - Google Patents
Method for preparing resin-base composite material thermal protection structure from modified resin by vapor deposition process Download PDFInfo
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- CN102658261B CN102658261B CN 201210163731 CN201210163731A CN102658261B CN 102658261 B CN102658261 B CN 102658261B CN 201210163731 CN201210163731 CN 201210163731 CN 201210163731 A CN201210163731 A CN 201210163731A CN 102658261 B CN102658261 B CN 102658261B
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Abstract
The invention discloses a method for preparing a resin-base composite material thermal protection structure from modified resin by a vapor deposition process, and relates to a preparation method for a resin-base composite material thermal protection structure. The method aims to solve the problem that an existing resin-base composite material cannot meet requirement on super-high temperature, powerful scouring and aerodynamic scouring ablation with short duration. The method includes firstly treating a resin-base composite material protection interface; secondly, preparing the modified resin from epoxy resin with three functional groups, a hardener, a modifier, an accelerator, a dispersing agent and a diluent; thirdly, spraying the modified resin prepared at the second step on the surface, which is treated at the first step, of the resin-base composite base material, and allowing deposition for a certain period; and solidifying by means of gradually increasing the temperature to obtain the resin-base composite material thermal protection structure prepared from the modified resin by the vapor deposition process. The method is mainly used for preparing the thermal protection structure on the surface of the resin-base composite material.
Description
Technical field
The present invention relates to a kind of preparation method of polymer matrix composites thermal protection structure.
Background technology
Mylar, epoxy resin, bismaleimide resin, polyimide resin even the cyanate ester resin of widespread usage in the present tree resin-based composite matrix, Applicable temperature is no more than 400 ℃, far can not satisfy superhigh temperature, washed away by force, the aerodynamics of the journey actual condition of ablating in short-term, cause the destruction rapidly of existing polymer matrix composites matrix generation cracking reaction and structure, and the forfeiture architectural characteristic, thereby lose polymer matrix composites in the application prospect of this specific area.
Summary of the invention
The objective of the invention is to solve existing polymer matrix composites and can not satisfy superhigh temperature, wash away and the aerodynamics of journey washes away ablation in short-term problem by force, and provide a kind of modified resin vapour deposition process to prepare the method for polymer matrix composites thermal protection structure.
A kind of modified resin vapour deposition process prepares the method for polymer matrix composites thermal protection structure, specifically finishes according to the following steps:
One, polymer matrix composites substrate surface treatment: adopt sandblast mode or 80# sand paper uniform grinding polymer matrix composites substrate surface, adopt acetone to clean then 2～4 times, adopt ethyl acetate to clean again 2～4 times, be dried to the polymer matrix composites base material after constant weight namely obtains surface treatment; Two, allotment modified resin: low whipping speed is under 40r/min～80r/min trifunctional epoxy resin, curing agent, modifier, promoter and dispersant to be stirred, low whipping speed is to add diluent under 40r/min～80r/min then, and being diluted to viscosity is 19m
2/ s～25m
2Till/the s, namely obtain modified resin; Three, spray deposited: the modified resin that step 2 is obtained joins in the flush coater, be polymer matrix composites substrate surface after 0.2MPa～0.5MPa, sedimentation rate are under the condition of 0.1mm/min～0.2mm/min the modified resin of step 2 preparation evenly to be sprayed to the surface treatment that step 1 obtains at pressure, deposition 8min～12min, namely obtaining thickness is the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer; Four, solidify: be 8 ℃/min～12 ℃/min with the thickness of step 3 preparation with programming rate be that the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer is warming up to 75 ℃～85 ℃ from room temperature, and at 75 ℃～85 ℃ following isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 135 ℃～145 ℃, and at 135 ℃～145 ℃ isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 160 ℃～170 ℃, and at 160 ℃～170 ℃ following 25min～35min that solidify, after naturally cooling to 20 ℃～60 ℃, namely obtain the modified resin vapour deposition process and prepare the polymer matrix composites thermal protection structure; The mass ratio of the trifunctional epoxy resin described in the step 2 and curing agent is 100: (10～15); The mass ratio of the trifunctional epoxy resin described in the step 2 and modifier is 100: (100～120); The mass ratio of the trifunctional epoxy resin described in the step 2 and promoter is 100: (5～10); The mass ratio of the trifunctional epoxy resin described in the step 2 and dispersant is 100: (5～10).
Advantage of the present invention: one, the present invention adopts vapour deposition process that modified resin successfully is attached to the polymer matrix composites surface, form thermal protection structure, broken through the mylar of widespread usage in the present tree resin-based composite matrix, epoxy resin, bismaleimide resin, polyimide resin even cyanate ester resin, Applicable temperature is no more than 400 ℃, far can not satisfy superhigh temperature, wash away by force, the actual condition of the aerodynamics of journey ablation in short-term, cause the destruction rapidly of existing polymer matrix composites matrix generation cracking reaction and structure, and the forfeiture architectural characteristic, thereby lose polymer matrix composites in the application prospect of this specific area; Two, the invention solves and satisfying and bringing into play the polymer matrix composites structural behaviour and can design, on the basis of the easy grade of moulding process traditional advantage, selection and the moulding process of high temperature resistant antiscour reisn base material have been solved well, improve its heat-resisting quantity and scour resistance greatly, through simulated test checking and actual condition examination, the interface performance of modified resin and matrix material is good, the gas-phase deposition implementation process is stablized controlled, thermal protection usefulness obviously improves, can experience repeatedly washing away of 1000 ℃ and above high temperature blast particle air-flow, become the key link of structure-function integration composite product thermal protection structure preparation process; Three, the present invention preparation have thermal protection structure polymer matrix composites, can satisfy wash away by force and in short-term the aerodynamics of journey wash away ablation; And thermal protection structure is attached to the surface of polymer matrix composites with molecular link and chemical bond, washes away with the aerodynamics of journey in short-term that thermal protection structure can not separate with polymer matrix composites under the situation of ablation washing away by force.
Specific embodiments
The specific embodiment one: present embodiment is the method that a kind of modified resin vapour deposition process prepares the polymer matrix composites thermal protection structure, specifically finishes according to the following steps:
One, polymer matrix composites substrate surface treatment: adopt sandblast mode or 80# sand paper uniform grinding polymer matrix composites substrate surface, adopt acetone to clean then 2～4 times, adopt ethyl acetate to clean again 2～4 times, be dried to the polymer matrix composites base material after constant weight namely obtains surface treatment; Two, allotment modified resin: low whipping speed is under 40r/min～80r/min trifunctional epoxy resin, curing agent, modifier, promoter and dispersant to be stirred, low whipping speed is to add diluent under 40r/min～80r/min then, and being diluted to viscosity is 19m
2/ s～25m
2Till/the s, namely obtain modified resin; Three, spray deposited: the modified resin that step 2 is obtained joins in the flush coater, be polymer matrix composites substrate surface after 0.2MPa～0.5MPa, sedimentation rate are under the condition of 0.1mm/min～0.2mm/min the modified resin of step 2 preparation evenly to be sprayed to the surface treatment that step 1 obtains at pressure, deposition 8min～12min, namely obtaining thickness is the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer; Four, solidify: be 8 ℃/min～12 ℃/min with the thickness of step 3 preparation with programming rate be that the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer is warming up to 75 ℃～85 ℃ from room temperature, and at 75 ℃～85 ℃ following isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 135 ℃～145 ℃, and at 135 ℃～145 ℃ isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 160 ℃～170 ℃, and at 160 ℃～170 ℃ following 25min～35min that solidify, after naturally cooling to 20 ℃～60 ℃, namely obtain the modified resin vapour deposition process and prepare the polymer matrix composites thermal protection structure.
The mass ratio of the trifunctional epoxy resin described in the present embodiment step 2 and curing agent is 100: (10～15); The mass ratio of the trifunctional epoxy resin described in the present embodiment step 2 and modifier is 100: (100～120); The mass ratio of the trifunctional epoxy resin described in the present embodiment step 2 and promoter is 100: (5～10); The mass ratio of the trifunctional epoxy resin described in the present embodiment step 2 and dispersant is 100: (5～10).
Present embodiment adopts vapour deposition process that modified resin successfully is attached to the polymer matrix composites surface, form thermal protection structure, broken through the mylar of widespread usage in the present tree resin-based composite matrix, epoxy resin, bismaleimide resin, polyimide resin even cyanate ester resin, Applicable temperature is no more than 400 ℃, far can not satisfy superhigh temperature, wash away by force, the actual condition of the aerodynamics of journey ablation in short-term, cause the destruction rapidly of existing polymer matrix composites matrix generation cracking reaction and structure, and the forfeiture architectural characteristic, thereby lose polymer matrix composites in the application prospect of this specific area.
Present embodiment has solved and has satisfied and bringing into play the polymer matrix composites structural behaviour and can design, on the basis of the easy grade of moulding process traditional advantage, selection and the moulding process of high temperature resistant antiscour reisn base material have been solved well, improve its heat-resisting quantity and scour resistance greatly, through simulated test checking and actual condition examination, the interface performance of modified resin and matrix material is good, the gas-phase deposition implementation process is stablized controlled, thermal protection usefulness obviously improves, can experience repeatedly washing away of 1000 ℃ and above high temperature blast particle air-flow, become the key link of structure-function integration composite product thermal protection structure preparation process.
Present embodiment preparation have thermal protection structure polymer matrix composites, can satisfy wash away by force and in short-term the aerodynamics of journey wash away ablation; And thermal protection structure is attached to the surface of polymer matrix composites with molecular link and chemical bond, washes away with the aerodynamics of journey in short-term that thermal protection structure can not separate with polymer matrix composites under the situation of ablation washing away by force.
The specific embodiment two: the difference of present embodiment and the specific embodiment one is: the polymer matrix composites base material described in the step 1 is mylar based composites, epoxy resin-base composite material, bimaleimide resin base composite material, polyimide resin based composites or cyanate resin base composite material.Other are identical with the specific embodiment one.
The specific embodiment three: present embodiment and one of the specific embodiment one or two difference are: curing agent described in the step 2 is to adopt m-phenylene diamine (MPD) and DDM curing agent by mass ratio 1: (0.8～1.2) mixes.Other are identical with the specific embodiment one or two.
The described DDM curing agent of present embodiment is bought and is obtained, by 4 of mass fraction 75%, and the mixture that many phenyl polyamino methane blended of 4-diaminodiphenyl-methane and mass fraction 25% forms.
The specific embodiment four: one of present embodiment and specific embodiment one to three difference is: modifier described in the step 2 is nano silicon or silicon carbide whisker, and perhaps nano silicon and silicon carbide whisker are pressed mass ratio 1: the mixture of (1.5～2.0).Other are identical with the specific embodiment one to three.
The specific embodiment five: one of present embodiment and specific embodiment one to four difference is: promoter described in the step 2 is silane coupler.Other are identical with the specific embodiment one to four.
The specific embodiment six: one of present embodiment and specific embodiment one to five difference is: dispersant described in the step 2 is graphite.Other are identical with the specific embodiment one to five.
The specific embodiment seven: one of present embodiment and specific embodiment one to six difference is: diluent described in the step 2 is to adopt toluene and dimethylbenzene by mass ratio 1: (0.8～1.2) mixes.Other are identical with the specific embodiment one to six.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of modified resin vapour deposition process prepares the method for polymer matrix composites thermal protection structure, specifically finishes according to the following steps:
One, polymer matrix composites substrate surface treatment: adopt the sandblast mode polymer matrix composites substrate surface of polishing, adopt acetone to clean then 3 times, adopt ethyl acetate to clean again 3 times, be dried to the polymer matrix composites base material after constant weight namely obtains surface treatment; Two, allotment modified resin: low whipping speed is under the 60r/min trifunctional epoxy resin, curing agent, modifier, promoter and dispersant to be stirred, and low whipping speed is to add diluent under the 60r/min then, and being diluted to viscosity is 21m
2Till/the s, namely obtain modified resin; Three, spray deposited: the modified resin that step 2 is obtained joins in the flush coater, be polymer matrix composites substrate surface after 0.35MPa, sedimentation rate are under the condition of 0.15mm/min the modified resin of step 2 preparation evenly to be sprayed to the surface treatment that step 1 obtains at pressure, deposition 10min, namely obtaining thickness is the curing materials for the treatment of of 2mm modified resin thermal protection structure layer; Four, solidify: be 10 ℃/min with the thickness of step 3 preparation with programming rate be that the curing materials for the treatment of of 2mm modified resin thermal protection structure layer is warming up to 80 ℃ from room temperature, and at 80 ℃ of following isothermal curing 10min, continuing then with programming rate is that 10 ℃/min is warming up to 140 ℃, and at 140 ℃ of isothermal curing 10min, continuing then with programming rate is that 10 ℃/min is warming up to 165 ℃, and at 165 ℃ of following 30min that solidify, after naturally cooling to 40 ℃, namely obtain the modified resin vapour deposition process and prepare the polymer matrix composites thermal protection structure.
Polymer matrix composites base material described in this test procedure one is epoxy resin-base composite material.
The mass ratio of the trifunctional epoxy resin described in this test procedure two and curing agent is 100: 12.5; The mass ratio of the trifunctional epoxy resin described in this test procedure two and modifier is 100: 110; The mass ratio of the trifunctional epoxy resin described in this test procedure two and promoter is 100: 7.5; The mass ratio of the trifunctional epoxy resin described in this test procedure two and dispersant is 100: 7.5.
Trifunctional epoxy resin described in this test procedure two is TPNE epoxy resin.Curing agent described in this test procedure two is to adopt m-phenylene diamine (MPD) and DDM curing agent to mix at 1: 1 by mass ratio.Modifier described in this test procedure two is nano silicon.Promoter described in this test procedure two is silane coupler.Dispersant described in this test procedure two is graphite.Diluent described in this test procedure two is to adopt toluene and dimethylbenzene to mix at 1: 1 by mass ratio.
This is tested described DDM curing agent purchase and obtains, by 4 of mass fraction 75%, and the mixture that many phenyl polyamino methane blended of 4-diaminodiphenyl-methane and mass fraction 25% forms.
Flush coater described in this test procedure three is SNE801 type flush coater.
Method of the present invention is through the checking of composite structure goods thermal protection structure preparation process, the interface performance of modified resin and matrix material is good, the gas-phase deposition implementation process is stablized controlled, thermal protection usefulness is obvious, improve heat-resisting quantity and the scour resistance of composite product greatly, can enough experience repeatedly washing away of 1000 ℃ and above high temperature blast particle air-flow, become the key link that the industry of structure-function integration composite product is made.
Adopt the experiment of high temperature blast particle airflow scouring, detect the polymer matrix composites that have thermal protection structure of this test preparation, wash away 6 times (what wash away is thermal protection structure one side that has the thermal protection structure polymer matrix composites) at 1000 ℃ of experience and above high temperature blast particle air-flow, the polymer matrix composites that have thermal protection structure of this test preparation do not have significant change, so the thermal protection structure polymer matrix composites that have of this test preparation have high temperature resistant as can be known, anti-ly wash away by force, the aerodynamics of anti-journey in short-term washes away advantages such as ablation.
Claims (5)
1. a modified resin vapour deposition process prepares the method for polymer matrix composites thermal protection structure, it is characterized in that the method that the modified resin vapour deposition process prepares the polymer matrix composites thermal protection structure finishes according to the following steps:
One, polymer matrix composites substrate surface treatment: adopt sandblast mode or 80# sand paper uniform grinding polymer matrix composites substrate surface, adopt acetone to clean then 2～4 times, adopt ethyl acetate to clean again 2～4 times, be dried to the polymer matrix composites base material after constant weight namely obtains surface treatment; Two, allotment modified resin: low whipping speed is under 40r/min～80r/min trifunctional epoxy resin, curing agent, modifier, promoter and dispersant to be stirred, low whipping speed is to add diluent under 40r/min～80r/min then, and being diluted to viscosity is 19m
2/ s～25m
2Till/the s, namely obtain modified resin; Three, spray deposited: the modified resin that step 2 is obtained joins in the flush coater, be polymer matrix composites substrate surface after 0.2MPa～0.5MPa, sedimentation rate are under the condition of 0.1mm/min～0.2mm/min the modified resin of step 2 preparation evenly to be sprayed to the surface treatment that step 1 obtains at pressure, deposition 8min～12min, namely obtaining thickness is the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer; Four, solidify: be 8 ℃/min～12 ℃/min with the thickness of step 3 preparation with programming rate be that the curing materials for the treatment of of 1.5mm～2.5mm modified resin thermal protection structure layer is warming up to 75 ℃～85 ℃ from room temperature, and at 75 ℃～85 ℃ following isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 135 ℃～145 ℃, and at 135 ℃～145 ℃ isothermal curing 8min～12min, continuing then with programming rate is that 8 ℃/min～12 ℃/min is warming up to 160 ℃～170 ℃, and at 160 ℃～170 ℃ following 25min～35min that solidify, after naturally cooling to 20 ℃～60 ℃, namely obtain the modified resin vapour deposition process and prepare the polymer matrix composites thermal protection structure; The mass ratio of the trifunctional epoxy resin described in the step 2 and curing agent is 100: (10～15); The mass ratio of the trifunctional epoxy resin described in the step 2 and modifier is 100: (100～120); The mass ratio of the trifunctional epoxy resin described in the step 2 and promoter is 100: (5～10); The mass ratio of the trifunctional epoxy resin described in the step 2 and dispersant is 100: (5～10); Curing agent described in the step 2 is to adopt m-phenylene diamine (MPD) and DDM curing agent by mass ratio 1: (0.8～1.2) mixes; Modifier described in the step 2 is nano silicon or silicon carbide whisker, and perhaps nano silicon and silicon carbide whisker are pressed mass ratio 1: the mixture of (1.5～2.0).
2. a kind of modified resin vapour deposition process according to claim 1 prepares the method for polymer matrix composites thermal protection structure, it is characterized in that the polymer matrix composites base material described in the step 1 is mylar based composites, epoxy resin-base composite material, bimaleimide resin base composite material, polyimide resin based composites or cyanate resin base composite material.
3. a kind of modified resin vapour deposition process according to claim 2 prepares the method for polymer matrix composites thermal protection structure, it is characterized in that promoter described in the step 2 is silane coupler.
4. a kind of modified resin vapour deposition process according to claim 3 prepares the method for polymer matrix composites thermal protection structure, it is characterized in that dispersant described in the step 2 is graphite.
5. the method for preparing the polymer matrix composites thermal protection structure according to claim 1,2,3 or 4 described a kind of modified resin vapour deposition processes, it is characterized in that diluent described in the step 2 is to adopt toluene and dimethylbenzene by mass ratio 1: (0.8～1.2) mixes.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002126618A (en) * | 2000-10-26 | 2002-05-08 | Nippon Paint Co Ltd | Method for forming multilayered coating film and multilayered coating film |
| CN1630581A (en) * | 2001-09-25 | 2005-06-22 | 亨克尔两合股份公司 | Autodeposition compositions |
| CN101198632A (en) * | 2005-05-10 | 2008-06-11 | 新日铁化学株式会社 | Epoxy resin composition and cured product |
| CN101580626A (en) * | 2009-01-24 | 2009-11-18 | 南亚塑胶工业股份有限公司 | Resin composition with high thermal conductivity, no halogen and difficult fire retardance and pre-impregnated body and coating material thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002126619A (en) * | 2000-10-26 | 2002-05-08 | Nippon Paint Co Ltd | Method for forming multilayered coating film and multilayered coating film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002126618A (en) * | 2000-10-26 | 2002-05-08 | Nippon Paint Co Ltd | Method for forming multilayered coating film and multilayered coating film |
| CN1630581A (en) * | 2001-09-25 | 2005-06-22 | 亨克尔两合股份公司 | Autodeposition compositions |
| CN101198632A (en) * | 2005-05-10 | 2008-06-11 | 新日铁化学株式会社 | Epoxy resin composition and cured product |
| CN101580626A (en) * | 2009-01-24 | 2009-11-18 | 南亚塑胶工业股份有限公司 | Resin composition with high thermal conductivity, no halogen and difficult fire retardance and pre-impregnated body and coating material thereof |
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