CN109354823A - Prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method - Google Patents
Prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method Download PDFInfo
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- CN109354823A CN109354823A CN201811377638.1A CN201811377638A CN109354823A CN 109354823 A CN109354823 A CN 109354823A CN 201811377638 A CN201811377638 A CN 201811377638A CN 109354823 A CN109354823 A CN 109354823A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/14—Modified phenol-aldehyde condensates
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- C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2461/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2461/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C08K7/00—Use of ingredients characterised by shape
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- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08K7/00—Use of ingredients characterised by shape
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Abstract
The invention discloses prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method.Using fiber cloth as reinforced phase, it is immersed in the different dipping solutions that phenolic resin is matrix, ceramic composition and cenosphere content distribution gradient respectively, prepares prepreg；Lamination, molding, at 150 DEG C~200 DEG C heat cure molding be made comprising heat shield, gradient transitional lay, thermal insulation layer gradient composites.For gradient composites produced by the present invention when temperature is up to 1000 DEG C, heat shield can be changed into the ceramic phase with higher-strength, can resist hot-fluid and wash away；Gradient transitional lay can alleviate stress concentration, reduce stress；Addition tiny balloon enables thermal insulation layer to have good thermal matching.
Description
Technical field
The invention belongs to composite materials with regard to technical field, and in particular to one kind prevent it is heat-insulated can ceramic phenolic resin base gradient
The preparation method of composite material.
Background technique
Functionally gradient material (FGM) is that one kind corresponds to its component and microstructure spatially consecutive variations, and ladder is presented in the performance of material
Spend the composite material of variation.Compared with conventional composite materials, due to turning between the phase of composition gradient material with continuous, smooth
Become, so that the thermal mismatching problem between material interface can be made when increasing functionally gradient material (FGM) between two kinds of different materials interfaces
Greatly alleviate, to avoid integral material in the peeling-off destruction in different materials interface.
There are many kinds of the preparation processes for preparing functionally gradient material (FGM) at present, the gradient as disclosed in publication number CN101391895A/anti-
Heat prevention/insulation ceramic base composite material and preparation method thereof is molded by powder and is made: ultrasonic cleaning, ball milling, drying are used to prepare
The raw material powder of each layer is laid in graphite jig in order, under inert atmosphere conditions, 5 points is kept the temperature after mixture is heated up
Clock is made.Since powder molding will receive such as, material weight is uneven, material fluidity is poor, the influence of the uncontrollable factor of operation, can lead
Sample is caused to be easy to produce defect.
Gradient distribution heat insulation material and preparation method thereof as disclosed in publication number CN105294143A, is enhanced by Amorphous GaN O
Porous ceramic matrix, silicon boron glass intermediate and the surface covering made of oxidation material are made.Made from this method
Sample generates larger stress easily at interlayer.
Polymer matrix composite can ceramic technology, be improve polymer matrix composite high temperature resistant, resistance to ablation, anti-impact
One brand-new route of brush.One kind as disclosed in publication number CN 102675822 can Carbon-based polymer composite material capable of being ceramized and
Preparation method, by carbon-based resin, high temperature resistant coupling agent, fibre reinforced materials, aluminium silicate mineral matter powder and non-oxidizable
Ceramic powders are suppressed through mixing.As one kind disclosed in publication number CN104945838A is fire-retardant can ceramic macromolecule composite wood
Material, by New Ablative-resisting polymer/resin add can ceramic additive, through dipping, compression moulding be made.
Summary of the invention
It is an object of that present invention to provide it is a kind of prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method.
Especially under the unilateral high hot-fluid of the components such as aerospace craft shell, the high thermal environment washed away, aircraft endothecium structure is protected
It is not damaged, meets space flight and aviation aircraft component and the needs of anti-heat-insulation integrative, improve advanced space flight boat under high-heat environment
The reliability of empty aircraft component thermal protection.
In order to achieve the above objectives, as follows using technical solution:
It is a kind of prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, include the following steps；
Using fiber cloth as reinforced phase, being immersed in phenolic resin respectively is that matrix, ceramic composition and cenosphere content are in
In the different dipping solutions of gradient distribution, prepreg is prepared；Lamination, molding, heat cure molding is made and includes at 150 DEG C~200 DEG C
Heat shield, gradient transitional lay, thermal insulation layer gradient composites；
Wherein, the mass percent of ceramic composition is reduced according to 50%-0% gradient in the dipping solution, cenosphere
Mass percent is increased according to 0%-4.8% gradient.
According to the above scheme, the fiber cloth includes one of quartz fiber cloth, carbon cloth, high silicon oxygen cloth or several
Kind.
According to the above scheme, the phenolic resin is boron bakelite resin.
According to the above scheme, the tiny balloon is hollow glass micro-ball, hollow ceramic microspheres, phenolic resin tiny balloon
One or more of；Particle size range is 10~250 μm, and bulk density is 0.35~0.45g/cm3。
According to the above scheme, the ceramic composition is silicide based ceramic metal, kaolin, silica, one in mica
Kind is several；D50Partial size is 2~3um, and purity is greater than 99%.
According to the above scheme, the dipping solution ingredient for preparing heat shield is as follows: ceramic composition, tiny balloon, resin, solvent are by matter
Amount is than being 2:0:1:1；The dipping solution ingredient for preparing gradient transitional lay is as follows: ceramic composition, tiny balloon, resin, solvent are by matter
Amount is than being 1.5:0.025:1:1,1:0.05:1:1,0.5:0.075:1:1；The dipping solution ingredient for preparing thermal insulation layer is as follows: ceramics
Component, tiny balloon, resin, solvent are 0:0.1:1:1 in mass ratio.
According to the above scheme, the thickness control of the gradient composites is between 10~11mm.
When temperature is up to 1000 DEG C, heat shield can be changed into higher-strength gradient composites produced by the present invention
Ceramic phase, hot-fluid can be resisted and washed away；Gradient transitional lay can alleviate stress concentration, reduce stress；Addition tiny balloon makes
Thermal insulation layer has good thermal matching energy, can be controlled composite density in 0.7~1.2g/cm according to design3It is real in range
Now anti-heat-insulation integrative.It is provided by the invention prevent it is heat-insulated can ceramic phenolic resin base gradient composite material can unidirectionally be heated
When protection materials not by the destruction of high temperature.
The present invention realizes the function of anti-heat-insulation integrative by preparing the design of prepreg lamination molding, i.e. surface layer is non-ablative
Solar heat protection, inner layer heat-insulation.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
Embodiment 1
Stock: by weight: 0 part of cenosphere, 5 parts, 10 parts, 15 parts, 20 parts, 200 parts of ceramic composition, 150 parts,
100 parts, 50 parts, 0 part, 40 layers of fiber cloth.
100 parts of boron bakelite resins and 100 parts of alcohol 1 to 1 are dissolved, it is 5 groups standby.Cenosphere and ceramic composition are added respectively
Enter wherein, stirs evenly and be made into gradient dipping solution.Regular fiber cloth is cut, dipping solution is equably brushed and is made in fiber cloth
Prepreg, dry in the air is suitable for viscosity.
Prepreg is cut into regular size, according to ceramic composition sequence lamination from high to low, folds 40 layers.It is put in mold
Be placed on hot press, be pressed and molded under 80 DEG C~200 DEG C, pressure 15MPa~19MPa, can be obtained prevent it is heat-insulated can ceramics
Change phenolic resin base gradient composite material.
Embodiment 2
With embodiment 1.
To manufactured one kind prevent it is heat-insulated can ceramic phenolic resin base gradient composite material sample weighed, deburring, cut out
It is measured at regular cube, then to the length of material, obtaining density is 1.1g/cm3。
Embodiment 3
With embodiment 1.
It is analyzed using interface of the electron probe microanalyzer to composite material, it can be observed that ladder is presented in titanium elements
Degree distribution.Show that preparation process of the present invention is good, gradient composites can be made.
Embodiment 4
With embodiment 1.
Sample is machined, and the ablation sample of 30 × 10mm of Φ is processed into.In air atmosphere, it is burnt using oxy-acetylene
Erosion machine carries out ablation test to sample, and 5 samples are one group, and linear ablative rate is averaged.It is tested through oxyacetylene ablation, sample
Linear ablative rate≤0.015mm/s.
Embodiment 5
With embodiment 1.
Manufactured gradient composites sample is put into Muffle furnace by 1200 DEG C of high warm experiments, with insulating brick and gas
Gel protects sample side and internal layer, only exposes surface layer side.After ten minutes, scantling is stablized, and material surface is without bright
Aobvious defect, thickness direction is without crack due to thermal stress, and without obvious ablation, overall performance is good for heat-insulated side layer by layer.Weightless >=70%, from
Heat shield to thermal insulation layer thermal conductivity less than 0.4 [W/mK].
Claims (7)
1. it is a kind of prevent it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, it is characterised in that including following step
Suddenly；
Using fiber cloth as reinforced phase, be immersed in respectively phenolic resin be matrix, ceramic composition and cenosphere content in gradient
In the different dipping solutions of distribution, prepreg is prepared；Lamination, molding, heat cure molding is made at 150 DEG C~200 DEG C includes solar heat protection
Layer, gradient transitional lay, thermal insulation layer gradient composites；
Wherein, the mass percent of ceramic composition is reduced according to 50%-0% gradient in the dipping solution, the quality of cenosphere
Percentage is increased according to 0%-4.8% gradient.
2. it is according to claim 1 prevent it is heat-insulated can ceramic phenolic resin base gradient composite material, it is characterised in that: it is described
Fiber cloth include one or more of quartz fiber cloth, carbon cloth, high silicon oxygen cloth.
3. prevent as described in claim 1 it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, feature exists
In the phenolic resin be boron bakelite resin.
4. prevent as described in claim 1 it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, feature exists
In the tiny balloon be one or more of hollow glass micro-ball, hollow ceramic microspheres, phenolic resin tiny balloon；Grain
Diameter range is 10~250 μm, and bulk density is 0.35~0.45g/cm3。
5. prevent as described in claim 1 it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, feature exists
In the ceramic composition be one or more of montmorillonite, silica, mica, kaolin；D50Partial size is 2~3um, purity
Greater than 99%.
6. prevent as described in claim 1 it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, feature exists
As follows in the dipping solution ingredient for preparing heat shield: ceramic composition, tiny balloon, resin, solvent are 2:0:1:1 in mass ratio；System
The dipping solution ingredient of standby gradient transitional lay is as follows: ceramic composition, tiny balloon, resin, solvent are 1.5:0.025 in mass ratio:
1:1,1:0.05:1:1,0.5:0.075:1:1；The dipping solution ingredient for preparing thermal insulation layer is as follows: ceramic composition, tiny balloon, tree
Rouge, solvent are 0:0.1:1:1 in mass ratio.
7. prevent as described in claim 1 it is heat-insulated can ceramic phenolic resin base gradient composite material preparation method, feature exists
In the gradient composites thickness control between 10~11mm.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910390A (en) * | 2019-03-04 | 2019-06-21 | 湖北菲利华石英玻璃股份有限公司 | A kind of prefabricated preparation of Graded Density resin composite materials |
| CN109968757A (en) * | 2019-04-22 | 2019-07-05 | 中国人民解放军国防科技大学 | Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof |
| CN110194609A (en) * | 2019-04-22 | 2019-09-03 | 湖南远辉新材料研究院有限公司 | A kind of high temperature resistant, it is anti-oxidant can ceramic resin composite materials and preparation method thereof |
| CN110627517A (en) * | 2019-10-25 | 2019-12-31 | 航天特种材料及工艺技术研究所 | Gradient ultrahigh-temperature ceramic matrix composite material and preparation method thereof |
| CN112457039A (en) * | 2020-11-27 | 2021-03-09 | 尚天保 | Carbon fiber heat insulation material and preparation method thereof |
| CN112708240A (en) * | 2019-10-24 | 2021-04-27 | 洛阳双瑞橡塑科技有限公司 | Thermosetting ceramizable phenolic aldehyde composite material and preparation process thereof |
| CN112920442A (en) * | 2021-01-29 | 2021-06-08 | 中国人民解放军国防科技大学 | Resin-based heat-proof composite material with surface coated with high-temperature infrared stealth coating and preparation method thereof |
| CN113276496A (en) * | 2021-06-03 | 2021-08-20 | 北京理工大学 | Light-weight heat-insulation integrated carbon fiber reinforced phenolic resin composite material |
| CN113274963A (en) * | 2021-04-26 | 2021-08-20 | 中国科学院化学研究所 | Reaction device for preparing polymer with high filling ratio and high viscosity and preparation method of polymer |
| CN115447218A (en) * | 2022-09-23 | 2022-12-09 | 湖北航天技术研究院总体设计所 | Light heat-proof and heat-insulating integrated structure with surface layer porcelainized and enhanced and preparation method thereof |
| CN115570852A (en) * | 2021-12-30 | 2023-01-06 | 湖北三江航天红阳机电有限公司 | Design, preparation and test method of low-density high-temperature-resistant heat-insulation-preventing composite material |
| CN115816926A (en) * | 2022-12-22 | 2023-03-21 | 武汉理工大学 | Reusable heat-proof and heat-insulating structure based on ceramic tiles and preparation method thereof |
| CN115181393B (en) * | 2022-07-01 | 2023-06-23 | 蚌埠凌空科技有限公司 | Modified resin matrix composite material for heat insulation and preparation method thereof |
| CN117430912A (en) * | 2023-12-20 | 2024-01-23 | 中国科学院赣江创新研究院 | Expanded microsphere modified fiber reinforced phenolic aerogel composite material and preparation method and application thereof |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910390A (en) * | 2019-03-04 | 2019-06-21 | 湖北菲利华石英玻璃股份有限公司 | A kind of prefabricated preparation of Graded Density resin composite materials |
| CN109968757A (en) * | 2019-04-22 | 2019-07-05 | 中国人民解放军国防科技大学 | Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof |
| CN110194609A (en) * | 2019-04-22 | 2019-09-03 | 湖南远辉新材料研究院有限公司 | A kind of high temperature resistant, it is anti-oxidant can ceramic resin composite materials and preparation method thereof |
| CN109968757B (en) * | 2019-04-22 | 2020-07-07 | 中国人民解放军国防科技大学 | Ablation-resistant light heat-proof heat-insulation integrated composite 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 |
| CN112708240A (en) * | 2019-10-24 | 2021-04-27 | 洛阳双瑞橡塑科技有限公司 | Thermosetting ceramizable phenolic aldehyde composite material and preparation process thereof |
| CN110627517B (en) * | 2019-10-25 | 2022-03-25 | 航天特种材料及工艺技术研究所 | Gradient ultrahigh-temperature ceramic matrix composite material and preparation method thereof |
| CN110627517A (en) * | 2019-10-25 | 2019-12-31 | 航天特种材料及工艺技术研究所 | Gradient ultrahigh-temperature ceramic matrix composite material and preparation method thereof |
| CN112457039A (en) * | 2020-11-27 | 2021-03-09 | 尚天保 | Carbon fiber heat insulation material and preparation method thereof |
| CN112920442B (en) * | 2021-01-29 | 2023-04-07 | 中国人民解放军国防科技大学 | Resin-based heat-proof composite material with surface coated with high-temperature infrared stealth coating and preparation method thereof |
| CN112920442A (en) * | 2021-01-29 | 2021-06-08 | 中国人民解放军国防科技大学 | Resin-based heat-proof composite material with surface coated with high-temperature infrared stealth coating and preparation method thereof |
| CN113274963A (en) * | 2021-04-26 | 2021-08-20 | 中国科学院化学研究所 | Reaction device for preparing polymer with high filling ratio and high viscosity and preparation method of polymer |
| CN113276496A (en) * | 2021-06-03 | 2021-08-20 | 北京理工大学 | Light-weight heat-insulation integrated carbon fiber reinforced phenolic resin composite material |
| CN115570852A (en) * | 2021-12-30 | 2023-01-06 | 湖北三江航天红阳机电有限公司 | Design, preparation and test method of low-density high-temperature-resistant heat-insulation-preventing composite material |
| CN115181393B (en) * | 2022-07-01 | 2023-06-23 | 蚌埠凌空科技有限公司 | Modified resin matrix composite material for heat insulation and preparation method thereof |
| CN115447218A (en) * | 2022-09-23 | 2022-12-09 | 湖北航天技术研究院总体设计所 | Light heat-proof and heat-insulating integrated structure with surface layer porcelainized and enhanced and preparation method thereof |
| CN115447218B (en) * | 2022-09-23 | 2023-11-17 | 湖北航天技术研究院总体设计所 | Surface porcelain reinforced light heat-proof and heat-insulating integrated structure and preparation method thereof |
| CN115816926A (en) * | 2022-12-22 | 2023-03-21 | 武汉理工大学 | Reusable heat-proof and heat-insulating structure based on ceramic tiles and preparation method thereof |
| CN115816926B (en) * | 2022-12-22 | 2023-10-13 | 武汉理工大学 | Reusable heat-proof and heat-proof structure based on ceramic tile and preparation method thereof |
| CN117430912A (en) * | 2023-12-20 | 2024-01-23 | 中国科学院赣江创新研究院 | Expanded microsphere modified fiber reinforced phenolic aerogel composite material and preparation method and application thereof |
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