CN109454894A - A kind of compound layer of resistance to ablative thermal protection of effectively insulating and preparation method thereof - Google Patents
A kind of compound layer of resistance to ablative thermal protection of effectively insulating and preparation method thereof Download PDFInfo
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- CN109454894A CN109454894A CN201811282537.6A CN201811282537A CN109454894A CN 109454894 A CN109454894 A CN 109454894A CN 201811282537 A CN201811282537 A CN 201811282537A CN 109454894 A CN109454894 A CN 109454894A
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- resin
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- 238000002360 preparation method Methods 0.000 title claims abstract description 50
- 150000001875 compounds Chemical class 0.000 title claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 80
- 239000011347 resin Substances 0.000 claims abstract description 80
- 239000004744 fabric Substances 0.000 claims abstract description 53
- 229910052751 metal Inorganic materials 0.000 claims abstract description 44
- 239000002184 metal Substances 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000011049 filling Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims description 35
- 239000003292 glue Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000835 fiber Substances 0.000 claims description 23
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 18
- 229920001568 phenolic resin Polymers 0.000 claims description 18
- 239000003365 glass fiber Substances 0.000 claims description 17
- 238000004804 winding Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000007711 solidification Methods 0.000 claims description 14
- 230000008023 solidification Effects 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 13
- -1 phenolic aldehyde Chemical class 0.000 claims description 13
- 239000005011 phenolic resin Substances 0.000 claims description 13
- 238000010276 construction Methods 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000007598 dipping method Methods 0.000 claims description 9
- 239000004568 cement Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- 239000012943 hotmelt Substances 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000004005 microsphere Substances 0.000 claims description 4
- 229920001709 polysilazane Polymers 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical class O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 claims 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000004907 flux Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000009413 insulation Methods 0.000 description 15
- 238000002679 ablation Methods 0.000 description 11
- 239000002131 composite material Substances 0.000 description 9
- 230000001681 protective effect Effects 0.000 description 7
- 229910052788 barium Inorganic materials 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000009941 weaving Methods 0.000 description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 239000013065 commercial product Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- RCHKEJKUUXXBSM-UHFFFAOYSA-N n-benzyl-2-(3-formylindol-1-yl)acetamide Chemical compound C12=CC=CC=C2C(C=O)=CN1CC(=O)NCC1=CC=CC=C1 RCHKEJKUUXXBSM-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000003981 vehicle Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000002529 flux (metallurgy) Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000012783 reinforcing fiber Substances 0.000 description 2
- 230000009102 absorption Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000013036 cure process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000005439 thermosphere Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/071—Preforms or parisons characterised by their configuration, e.g. geometry, dimensions or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/32—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core on a rotating mould, former or core
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
- B29B15/122—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
- B29B15/125—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2949/00—Indexing scheme relating to blow-moulding
- B29C2949/07—Preforms or parisons characterised by their configuration
- B29C2949/0715—Preforms or parisons characterised by their configuration the preform having one end closed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/30—Vehicles, e.g. ships or aircraft, or body parts thereof
- B29L2031/3076—Aircrafts
Abstract
The present invention relates to compound layers of resistance to ablative thermal protection of a kind of effectively insulating and preparation method thereof.The preparation method include: the first resin comprising low heat filling and the first fabric is compound, obtain internal layer prepreg；Second resin and the second fabric is compound, obtain outer layer prepreg；Metal die is provided；In metal die surface wrap internal layer prepreg, then wind outer layer prepreg；The mold for being wound with internal layer prepreg and outer layer prepreg is solidified, internal layer prepreg and outer layer prepreg is formed, obtains the heat shield.Obtained solar heat protection layer material takes into account solar heat protection and heat-insulated double effects, and according to heat flux, designability is strong, has good anti-heat-proof quality, meets structure-function combining design technology target.
Description
Technical field
The present invention relates to functional composite material technical field more particularly to a kind of compound layers of resistance to ablative thermal protection of effectively insulating
And preparation method thereof.
Background technique
Thermally protective materials are a kind of composite materials by extensive concern at present.In recent years, near space vehicle and it is long when
Between aerocraft cause the extensive concerns of countries in the world, the type aircraft flying for long time, middle low-heat current density, medium enthalpy
Military service feature thermally protective materials and its structure are proposed with new application environment and requirement, including long-time solar heat protection, efficiently every
Heat, high bearing capacity, high reliability etc..External pneumatic heating is serious, under conditions of High Temperature And Velocity airflow scouring, structural body
Surface generallys use a kind of ablation thermal protection composite material, is decomposed under hot-fluid effect by material, melts, evaporates, distilling
Etc. the physical and chemical changes of a variety of heat absorptions and heat dissipation, a large amount of thermal energy are taken away with the quality consumption of itself, prevent heat incoming interior
Portion's structure, to achieve the purpose that solar heat protection is heat-insulated.
Traditional heat insulation material thermal conductivity is higher, to reach certain insulation requirement, it is necessary to increase heat shield thickness.But material
Expect that density is higher, heat shield is thicker, is not able to satisfy lightweight, lower thermal conductivity, high many requirements such as heat-insulated.Single thermal protection shield material
Material is difficult to meet hypersonic lower anti-ablation, double technique requirement heat-insulated for a long time, therefore thermal protection system uses composite junction
Structure, outer surface is anti-ablation layer, inside is thermal insulation layer.
Inventors have found that being difficult to see in the relevant report about the thermally protective materials of this composite construction in the prior art
The report of substantive key technology.It is carried out in research process in the thermally protective materials to this composite construction, there are following
One or more technical problem needs overcome:
(1) do not carry out the research of applicability material system and preparation process for different heat fluxes and section structure,
Cause material and technique that there is certain limitation；
(2) globality of compound thermally protective materials is poor；
(3) lightweight, resistance to ablation and effectively insulating be cannot be considered in terms of.
In view of this, inventor proposes the present invention according to research achievement.
Summary of the invention
(1) technical problems to be solved
The technical problem to be solved by the present invention is the correlation about the thermally protective materials of this composite construction in the prior art
It is difficult to see the report of substantive key technology in report, existing thermal protection sandwich is existing as next or more
A defect:
(1) do not carry out the research of applicability material system and preparation process for different heat fluxes and section structure,
Cause material and technique that there is certain limitation；
(2) globality of compound thermally protective materials is poor；
(3) lightweight, resistance to ablation and effectively insulating be cannot be considered in terms of.
(2) technical solution
In order to solve the above-mentioned technical problems, the present invention provides following technical solutions:
1, a kind of preparation method of the compound layer of resistance to ablative thermal protection of effectively insulating, the preparation method include the following steps:
(1) the first resin comprising low heat filling and the first fabric is compound, obtain internal layer prepreg；
(2) the second resin and the second fabric is compound, obtain outer layer prepreg；
(3) metal die is provided；
(4) in metal die surface wrap internal layer prepreg, then outer layer prepreg is wound；
(5) mold for being wound with internal layer prepreg and outer layer prepreg is solidified, keeps internal layer prepreg and outer layer pre-
Leaching material molding, obtains the heat shield.
2, the preparation method according to 1, the low heat filling are selected from hollow glass micropearl, hollow ceramic microspheres, sky
Heart phenolic aldehyde microballoon is any one or more of；
First resin is selected from phenolic resin, phenol-formaldehyde resin modified, benzoxazine resin, poly- aryl ethane resin, gathers
Siloxane resin is any one or more of；And/or
Fiber used in first fabric is in carbon fiber, glass fibre, high silica fiber, quartz fibre
It is any one or more；Preferably, first fabric has plain weave structure, satin construction or twill structure.
3, the preparation method according to 2, the low heat filling have 10~500 microns of partial size and 0.6~0.1g/
cm3Density.
4, the mass ratio of the preparation method according to 2, the low heat filling and first resin is 0.1~1.
5, the preparation method according to 2, the internal layer prepreg have 50%~70% resin content.
6, preparation method according to technical solution 1, second resin be selected from phenolic resin, phenol-formaldehyde resin modified,
Benzoxazine resin, poly- aryl ethane resin, polysilazane resin are any one or more of；And/or
Fiber used in second fabric is selected from quartz glass fibre, high silica fiber, high-strength glass fibre, nothing
Alkali containing glass fibre, polyacrylonitrile-based carbon fibre, adhesive carbon fiber are any one or more of.
7, the preparation method according to technical solution 6, second fabric have plain weave structure, twill structure,
Satin construction or warp knit inlaid thread structure.
8, the preparation method according to technical solution 6, the outer layer prepreg have 30%~60% resin content.
9, the preparation method according to technical solution 2 prepares the internal layer prepreg using hot melt or glue film method.
10, the preparation method according to technical solution 9, the hot melt carry out as follows:
Low heat filling is added in ethanol solution and is stirred evenly, then mixes, is uniformly dispersed with the first resin, obtains the
One glue；
First glue is poured into glue groove, the first fabric is impregnated using cement dipping machine, obtains the internal layer prepreg.
11, the preparation method according to technical solution 9, the glue film method carry out as follows:
Low heat filling, the first resin and film forming agent are uniformly mixed, resin glue film is made in mixture, then by resin
Glue film is combined on two surfaces up and down of the first fabric, obtains the internal layer prepreg.
12, preparation method according to technical solution 3, the outer layer prepreg are prepared as follows:
Second resin is heated into liquid, is diluted with solvent, impregnates the second fabric using cement dipping machine, is obtained described outer
Layer prepreg.
13, preparation method according to technical solution 1, the width of the internal layer prepreg are 40~80mm；And/or
The width of the outer layer prepreg is 50~110mm.
14, preparation method according to technical solution 1, the internal layer prepreg is using wound in parallel or overlap wrapping
Mode is wound, winding with a thickness of 4~8mm.
15, preparation method according to technical solution 1, the outer layer prepreg are twined by the way of tiltedly folded winding
Around, winding with a thickness of 8~9mm.
16, preparation method according to technical solution 1, the solidification use vacuum pressed solidification method, cured technique
Condition are as follows: vacuum degree -0.085MPa hereinafter, 120~180 DEG C of solidification temperature, 3~8h of curing time, solidifying pressure 0.8~
10MPa。
17, the compound layer of resistance to ablative thermal protection of a kind of effectively insulating, using the described in any item preparation sides of technical solution 1~16
Method is prepared.
(3) beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
(1) preparation method provided by the invention by the inner layer heat-insulation layer and the integrated molding of outer layer heat shield in heat shield and is consolidated
Change, simple process, reliability are high, particularly suitable for batch production.
(2) the solar heat protection layer material that the present invention obtains takes into account solar heat protection and heat-insulated double effects, according to heat flux, can design
Property it is strong, have good anti-heat-proof quality, meet structure-function combining design technology target.
(3) it can get the compound heat shield of the anti-heat type of effectively insulating using the preparation method, synthesis can be down to 1.0g/cm3It is left
The right side significantly reduces whole solar heat protection layer weight, improves aerial flight load.
(4) solar heat protection layer material of the invention is suitable for control cabinet, load cabin, the instrument room, warhead cabin of high-speed aircraft
Etc. metal structures skin-material large area solar heat protection.
Detailed description of the invention
Fig. 1 is the flow diagram of the heat shield preparation method provided by the invention；
Fig. 2 is structural schematic diagram when heat shield and metal cabin are assembled together；
1: metal cabin；2: inner layer heat-insulation layer；3: outer layer heat shield.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of preparation method of compound layer of resistance to ablative thermal protection of effectively insulating, such as Fig. 1 in first aspect
Shown, the preparation method includes the following steps:
(1) the first resin comprising low heat filling and the first fabric is compound, obtain internal layer prepreg；
In some embodiments, the low heat filling can select hollow glass micropearl, hollow ceramic microspheres, hollow phenol
Aldehyde microballoon is any one or more of.Clearly, the low heat filling refer to 10~500 microns partial size and
0.6~0.1g/cm3Density hollow glass micropearl, hollow ceramic microspheres, hollow phenolic aldehyde microballoon it is any one or more of.
The low heat filling of mentioned kind is spherical thin wall cavity structure, and the gas in cavity can play good heat insulation,
To help to improve the resistance to ablation ability of heat shield.It is further preferred that the low heat filling selected has specific partial size,
Its partial size is limited to 10~500 microns by the present invention, for example, can for 10 microns, 20 microns, 30 microns, 40 microns, it is 50 micro-
Rice, 60 microns, 70 microns, 80 microns, 90 microns, 100 microns, 150 microns, 200 microns, 250 microns, 300 microns, it is 350 micro-
Rice, 400 microns, 450 microns or 500 microns.When preparation, it can select with any one or more partial size in above range
Low heat filling.The low heat filling of mentioned kind is commercial product or the product that use existing method can obtain, this hair
It is bright not limit its source or preparation method.
In some embodiments, first resin can select phenolic resin, phenol-formaldehyde resin modified, benzoxazine tree
Rouge, poly- aryl ethane resin, polysilazane resin are any one or more of；The resin of mentioned kind is commercial product or adopts
The product that can be obtained with existing method, the present invention do not limit its source or preparation method.
The fiber for being used to prepare first fabric can select carbon fiber, glass fibre, high silica fiber, quartz
Fiber is any one or more of.For the structure of the first fabric, plain weave structure, satin construction or twill knot can be used
Structure.The method for weaving of the fabric of above-mentioned three kinds of structures is the prior art, this is no longer described in detail in the present invention, and people can root
The fabric of corresponding method for weaving acquisition corresponding construction is selected according to demand.
In some embodiments, the mass ratio of the low heat filling and first resin is 0.1~1.
In some embodiments, the internal layer prepreg has 50%~70% resin content (mass percentage),
For example, can for 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%,
63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%.
For the complex method in the step, hot melt or glue film method can be used, first comprising low heat filling is made
Resin and the first fabric are compound, to obtain internal layer prepreg.
Specifically, the hot melt can carry out as follows:
Low heat filling is added in ethanol solution and is stirred evenly, so that the surface of low heat filling is soaked, then
It is mixed with the first resin, when mixing, can become and stir the mixture change of low heat filling and ethanol solution and add it to first
In resin；Then the mixture comprising low heat filling, ethanol solution and resin is uniformly dispersed, obtains the first glue, dispersed
When the mixture can be dispersed using high-speed mixer；
Then the first glue is poured into glue groove, impregnates the first fabric using cement dipping machine, obtain the internal layer preimpregnation
Material.
Specifically, the glue film method can carry out as follows:
Low heat filling, the first resin and film forming agent are uniformly mixed, resin glue film is made in mixture, then by resin
Glue film is combined on two surfaces up and down of the first fabric, obtains the internal layer prepreg.In this step, film forming agent can
To select product known in the art, the present invention is not specifically limited it herein, and the dosage of film forming agent can also be according to existing skill
Art is tested and is determined.The preparation method of resin glue film is the prior art.
(2) the second resin and the second fabric is compound, obtain outer layer prepreg；
In some embodiments, second resin can select phenolic resin, phenol-formaldehyde resin modified, benzoxazine tree
Rouge, poly- aryl ethane resin, polysilazane resin are any one or more of；The resin of mentioned kind is commercial product or adopts
The product that can be obtained with existing method, the present invention do not limit its source or preparation method.
The fiber for being used to prepare second fabric can select quartz glass fibre, high silica fiber, high-strength glass
Glass fiber, alkali-free glass fibre, polyacrylonitrile-based carbon fibre, adhesive carbon fiber are any one or more of.For described
The structure of two fabrics can use plain weave structure, twill structure, satin construction or warp knit inlaid thread structure.Above-mentioned several knots
The method for weaving of the fabric of structure is the prior art, this is no longer described in detail in the present invention, and people can select phase according to demand
The method for weaving answered obtains the fabric of corresponding construction.
In some embodiments, in the outer layer prepreg obtained, resin content is that 30~60% (quality percentage contains
Amount), for example, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%,
43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%,
58%, 59% or 60%.
For the complex method in the step, can carry out with the following method:
Second resin is heated into liquid, is diluted with solvent, impregnates the second fabric using cement dipping machine, is obtained described outer
Layer prepreg.It should be noted that the present invention is not defined the dosage of solvent and the technique of dipping, as long as can finally obtain
Obtain the outer layer prepreg that resin content meets 30~60%.
(3) metal die is provided；
The structure of metal die is manufactured according to the structure for the metal cabin assembled with heat shield, so as to obtain
It obtains and assembles the heat shield used with metal cabin of different shapes.
Surface clean can be carried out before use to metal die, cleaning agent can be with water and/or other are volatile and right
The nontoxic organic reagent of human body (such as ethyl alcohol).Cleaning can uniformly smear release agent on the surface of metal die after drying, and take off
Mould agent can select the common release agent in all kinds of cure process being currently known, and the present invention does not do specifically its type
It limits.It when smearing release agent, can repeatedly smear, such as 3~4 release agents can be smeared, can be waited after being often painted with once
(for example, 10~20 minutes) are smeared again for a period of time.
(4) in metal die surface wrap internal layer prepreg, then outer layer prepreg is wound；
In this step, when being wound, the width of internal layer prepreg used is preferably 40~80mm, for example, can be with
For 40mm, 45mm, 50mm, 55mm, 60mm, 65mm, 70mm, 75mm or 80mm.If the internal layer preimpregnation obtained in step (1)
The width of material meets above-mentioned condition, then the internal layer prepreg can be used directly；If the internal layer preimpregnation obtained in step (1)
Material is unsatisfactory for above-mentioned condition, then needs to cut internal layer prepreg, its width is made to meet above-mentioned width requirement.
In this step, when being wound, the width of outer layer prepreg used is preferably 50~110mm, for example, can be with
For 50mm, 55mm, 60mm, 65mm, 70mm, 75mm, 80mm, 85mm, 90mm, 95mm, 100mm, 105mm or 110mm.If
The width of outer layer prepreg obtained meets above-mentioned condition in step (2), then the outer layer prepreg can be used directly；If
Outer layer prepreg obtained is unsatisfactory for above-mentioned condition in step (2), then needs to cut outer layer prepreg, meet its width
Above-mentioned width requirement.
In this step, the internal layer prepreg can be wound by the way of wound in parallel or overlap wrapping, be twined
Around thickness be preferably 4~8mm, for example, can be 4mm, 4.5mm, 5mm, 5.5mm, 6mm, 6.5mm, 7mm, 7.5mm or 8mm.
In this step, the outer layer prepreg can be wound by the way of tiltedly folded winding, winding with a thickness of 8
~9mm, for example, can be 8.1mm, 8.2mm, 8.3mm, 8.4mm, 8.5mm, 8.6mm, 8.7mm, 8.8mm, 8.9mm or 9mm.
(5) mold for being wound with internal layer prepreg and outer layer prepreg is solidified, keeps internal layer prepreg and outer layer pre-
Leaching material molding, obtains the heat shield.
In some embodiments, solidification can use vacuum pressed solidification method, can be wound with internal layer preimpregnation when solidification
Expect and the surface of the mold of outer layer prepreg is successively coated with isolation film, inhales rubber mat, vacuum bag sealing vacuumizes, and then heating adds
Pressure is solidified, and internal layer prepreg and outer layer prepreg, internal layer prepreg and resin in outer layer prepreg and fabric are multiple
Integrator；Cured process conditions are preferred are as follows: vacuum degree -0.085MPa hereinafter, 120~180 DEG C of solidification temperature (for example, can
Think 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 150 DEG C, 155 DEG C, 160 DEG C, 165 DEG C, 170 DEG C, 175 DEG C or
180 DEG C), 3~8h of curing time (for example, can be 3h, 4h, 5h, 6h, 7h or 8h), 0.8~10MPa of solidifying pressure (for example,
Can for 0.8MPa, 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, 5MPa, 5.5MPa,
6MPa, 6.5MPa, 7MPa, 7.5MPa, 8MPa, 8.5MPa, 9MPa, 9.5MPa or 10MPa).
The present invention provides a kind of compound layer of resistance to ablative thermal protection of effectively insulating in second aspect, using any of the above-described institute
The preparation method stated is prepared.
The heat shield includes inner layer heat-insulation layer and outer layer heat shield, and inner layer heat-insulation layer is the fabric of resistance to ablation/resistance to ablation
The light composite material that resin/low heat filling is combined, can by wound in parallel or overlap wrapping on molding die,
Outer layer heat shield is the fabric of resistance to ablation/composite material of resistance to Ablative resin, can be wrapped on the thermal insulation layer of inside by tiltedly folding,
Then integrated heat-pressure curing, it is Nian Jie with metal cabin suit after processing demoulding.The solar heat protection layer material takes into account solar heat protection and heat-insulated
Double effects, according to heat flux, designability is strong, has good anti-heat-proof quality, meets structure-function combining design technology
Target is highly suitable for the metal structures skin-materials such as control cabinet, load cabin, instrument room, the warhead cabin of high-speed aircraft
Large area solar heat protection.In addition, the combined density of the solar heat protection layer material can be down to 1.0g/cm3Left and right significantly reduces whole heat shield weight
Amount improves aerial flight load.
In short, the heat shield good integrity, can be used as heat-barrier material, it is also used as thermal-protect ablation material, product can
Design is good, is able to satisfy the heat-insulated requirement of long-time ablation, can be widely applied to heat-insulated and solar heat protection aerospace field with again
Condensation material.
In use, needing to assemble heat shield in metal cabin, the schematic diagram after assembly is shown in Fig. 2.In Fig. 2,1 is metal
Cabin, 2 be inner layer heat-insulation layer, and 3 be outer layer heat shield.
Specifically, after above-mentioned steps (5), installation step can carry out as follows:
(a) preliminary working: the vehicle for carrying out outer circle to the heat shield after curing molding with mold is ground, in mold corresponding position to anti-
Thermosphere both ends are cut, outer circle and the reserved machining allowance of both ends length；
(b) trial assembly is matched: the heat shield processed being demoulded, is removed from the mold, then with metal bay section pre-assembled, is observed
Fit clearance and length surplus；
(c) Nian Jie with metal cabin suit: by the bonding region blasting treatment of heat shield and metal cabin, homogeneous modulation set
Assembling structure glue uniformly smears the structure glue in heat shield and metal cabin bonding region respectively, slowly by heat shield from metal
Metal bay section is inserted in above cabin, heat shield is pressurized to metal cabin using positioning pressurization tooling by equal control fit clearance
Predetermined position guarantees bonding layer uniformity, the structure glue of extrusion is cleaned, and solidifies；
(d) it finishes: the positions such as heat shield shape, aperture and both ends being finished using numerical control device, meet
Drawing requirement, i.e. referable after detection is qualified.
It is the embodiment that the present invention enumerates below.
Embodiment 1
The compound layer of resistance to ablative thermal protection of effectively insulating that embodiment 1 provides has inner layer heat-insulation layer and outer layer heat shield；
Enhanced fabrics in inner layer heat-insulation layer are alkali-free Non-twisting glass fibre grid cloth, and resistance to Ablative resin is barium phenolic aldehyde
Resin, low heat filling are hollow glass micropearl, and partial size is 10 microns, density 0.6g/cm3；
Enhanced fabrics in outer layer heat shield are high silica fiber plain cloth, and resistance to Ablative resin is ba phenolic resin.
Preparation method specifically comprises the following steps:
(1) internal layer prepreg is prepared
Hollow glass micropearl, ba phenolic resin and film forming agent are uniformly mixed, wherein hollow glass micropearl and barium phenolic aldehyde tree
The mass ratio of rouge is 1, and resin glue film is made in mixture, resin glue film is then combined to alkali-free Non-twisting glass fibre grid cloth
Two surfaces up and down on, obtain internal layer prepreg and ensure resin content therein be 70%.
(2) outer layer prepreg is prepared
Ba phenolic resin is heated into liquid, is diluted with solvent, high silica fiber plain cloth is impregnated using cement dipping machine, obtains
Outer layer prepreg simultaneously ensures that resin content therein is 30%.
(3) metal die is provided
Surface clean is carried out to metal die, uniformly smears release agent on metal die surface after drying, is smeared every time
It applies next time, applies 4 times after 15min.
(4) Wrapping formed
In metal die surface wrap internal layer prepreg, winding method is wound in parallel ply sequence, then to wind outer layer pre-
Leaching material, winding method are tiltedly to fold winding ply sequence；Wherein, the width of internal layer prepreg used be 60mm, winding with a thickness of
6mm；The width of outer layer prepreg used is 80mm, is wound with a thickness of 8mm.
(5) vacuum pressed solidifies
Mold outer surface after Wrapping formed is successively coated with isolation film, inhales rubber mat, vacuum bag sealing, it vacuumizes, passes through
Heating pressurization is solidified, and so that resin is combined into one with reinforcing fiber, internal layer prepreg and outer layer prepreg, wherein vacuum
Degree control is in -0.085MPa hereinafter, solidification temperature, which is 150 DEG C, curing time 3h, solidifying pressure 0.8MPa, obtains solar heat protection
Layer.
Above-mentioned heat shield and metal cabin are assembled, specifically comprised the following steps:
(6) preliminary working
The vehicle for carrying out outer circle to the heat shield being cured with mold is ground, and is divided in mold corresponding position heat shield both ends
It cuts, outer circle and the reserved machining allowance of both ends length；
(7) trial assembly is matched
By the heat shield processed demould, remove from the mold, then with metal bay section pre-assembled, observe fit clearance and
Length surplus；
(8) Nian Jie with metal cabin suit
By the bonding region blasting treatment of heat shield and metal cabin, homogeneous modulation sleeve structure glue, respectively in heat shield
The structure glue is uniformly smeared with metal cabin bonding region, heat shield is slowly inserted in metal bay section above metal cabin,
Heat shield is pressurized to metal cabin predetermined position using positioning pressurization tooling, guarantees that bonding layer is equal by equal control fit clearance
It is even consistent, the structure glue of extrusion is cleaned, is solidified；
(9) it finishes
The positions such as heat shield shape, aperture and both ends are finished using numerical control device, meet drawing requirement, are examined
I.e. referable after survey is qualified.
Embodiment 2
The compound layer of resistance to ablative thermal protection of effectively insulating that embodiment 2 provides has inner layer heat-insulation layer and outer layer heat shield；
Enhanced fabrics in inner layer heat-insulation layer are alkali-free Non-twisting glass fibre grid cloth, and resistance to Ablative resin is barium phenolic aldehyde
Resin, low heat filling are hollow glass micropearl, and partial size is 500 microns, density 0.1g/cm3；
Enhanced fabrics in outer layer heat shield are high silica fiber plain cloth, and resistance to Ablative resin is ba phenolic resin.
Preparation method specifically comprises the following steps:
(1) internal layer prepreg is prepared
Hollow glass micropearl, ba phenolic resin and film forming agent are uniformly mixed, wherein hollow glass micropearl and barium phenolic aldehyde tree
The mass ratio of rouge is 0.1, and resin glue film is made in mixture, resin glue film is then combined to alkali-free Non-twisting glass fibre grid
On two surfaces up and down of cloth, obtains internal layer prepreg and ensure that resin content therein is 50%.
(2) outer layer prepreg is prepared
Ba phenolic resin is heated into liquid, is diluted with solvent, high silica fiber plain cloth is impregnated using cement dipping machine, obtains
Outer layer prepreg simultaneously ensures that resin content therein is 50%.
(3) metal die is provided
Surface clean is carried out to metal die, uniformly smears release agent on metal die surface after drying, is smeared every time
It applies next time, applies 3 times after 15min.
(4) Wrapping formed
In metal die surface wrap internal layer prepreg, winding method is wound in parallel ply sequence, then to wind outer layer pre-
Leaching material, winding method are tiltedly to fold winding ply sequence；Wherein, the width of internal layer prepreg used be 40mm, winding with a thickness of
4mm；The width of outer layer prepreg used is 110mm, is wound with a thickness of 9mm.
(5) vacuum pressed solidifies
Mold outer surface after Wrapping formed is successively coated with isolation film, inhales rubber mat, and vacuum bag sealing vacuumizes, passes through
Heating pressurization is solidified, and so that resin is combined into one with reinforcing fiber, internal layer prepreg and outer layer prepreg, wherein vacuum
Degree control is in -0.085MPa hereinafter, solidification temperature, which is 180 DEG C, curing time 3h, solidifying pressure 10MPa, obtains solar heat protection
Layer.
Above-mentioned heat shield and metal cabin are assembled, specific method is the same as embodiment 1.
Embodiment 3
The compound layer of resistance to ablative thermal protection of effectively insulating that embodiment 3 provides has inner layer heat-insulation layer and outer layer heat shield；
Enhanced fabrics in inner layer heat-insulation layer are alkali-free Non-twisting glass fibre grid cloth, and resistance to Ablative resin is barium phenolic aldehyde
Resin, low heat filling are hollow glass micropearl, and partial size is 100 microns, density 0.3g/cm3；
Enhanced fabrics in outer layer heat shield are high silica fiber plain cloth, and resistance to Ablative resin is ba phenolic resin.
It is substantially the same that the preparation method is the same as that of Example 1, the difference is that:
In step (4), the width of internal layer prepreg used is 80mm, is wound with a thickness of 8mm；Outer layer preimpregnation used
The width of material is 50mm, is wound with a thickness of 6mm.
In step (5), solidification temperature is 160 DEG C, curing time 4h, solidifying pressure 5MPa.
Table 1 is the performance test results of solar heat protection layer material made from above-mentioned each embodiment.
Table 1
| Project | Density/(g/cm3) | Linear ablative rate/(mm/s) | Thermal conductivity/(W/mK) |
| Embodiment 1 | 1.0 | 0.32 | 0.26 |
| Embodiment 2 | 1.1 | 0.31 | 0.30 |
| Embodiment 3 | 0.95 | 0.33 | 0.25 |
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of the compound layer of resistance to ablative thermal protection of effectively insulating, which is characterized in that the preparation method includes such as
Lower step:
(1) the first resin comprising low heat filling and the first fabric is compound, obtain internal layer prepreg；
(2) the second resin and the second fabric is compound, obtain outer layer prepreg；
(3) metal die is provided；
(4) in metal die surface wrap internal layer prepreg, then outer layer prepreg is wound；
(5) mold for being wound with internal layer prepreg and outer layer prepreg is solidified, makes internal layer prepreg and outer layer prepreg
Molding, obtains the heat shield.
2. preparation method according to claim 1, which is characterized in that the low heat filling be selected from hollow glass micropearl,
Hollow ceramic microspheres, hollow phenolic aldehyde microballoon are any one or more of；Preferably, the low heat filling is micro- with 10~500
The partial size and 0.6~0.1g/cm of rice3Density；
First resin is selected from phenolic resin, phenol-formaldehyde resin modified, benzoxazine resin, poly- aryl ethane resin, poly- silicon nitrogen
Alkane resin is any one or more of；And/or
Any of fiber in carbon fiber, glass fibre, high silica fiber, quartz fibre used in first fabric
Kind is a variety of；Preferably, first fabric has plain weave structure, satin construction or twill structure；
Preferably, the mass ratio of the low heat filling and first resin is 0.1~1；
Preferably, the internal layer prepreg has 50%~70% resin content.
3. preparation method according to claim 1, which is characterized in that second resin is selected from phenolic resin, modified phenol
Urea formaldehyde, benzoxazine resin, poly- aryl ethane resin, polysilazane resin are any one or more of；And/or
Fiber used in second fabric is selected from quartz glass fibre, high silica fiber, high-strength glass fibre, alkali-free glass
Glass fiber, polyacrylonitrile-based carbon fibre, adhesive carbon fiber are any one or more of；Preferably, second fabric
With plain weave structure, twill structure, satin construction or warp knit inlaid thread structure；
Preferably, the outer layer prepreg has 30%~60% resin content.
4. preparation method according to claim 2, which is characterized in that it is pre- to prepare the internal layer using hot melt or glue film method
Leaching material；
Preferably, the hot melt carries out as follows:
Low heat filling is added in ethanol solution and is stirred evenly, then mixes, is uniformly dispersed with the first resin, obtain the first glue
Liquid；
First glue is poured into glue groove, the first fabric is impregnated using cement dipping machine, obtains the internal layer prepreg；Or
Preferably, the glue film method carries out as follows:
Low heat filling, the first resin and film forming agent are uniformly mixed, resin glue film is made in mixture, then by resin glue film
It is combined on two surfaces up and down of the first fabric, obtains the internal layer prepreg.
5. preparation method according to claim 3, which is characterized in that the outer layer prepreg is made as follows
It is standby:
Second resin is heated into liquid, is diluted with solvent, the second fabric is impregnated using cement dipping machine, it is pre- to obtain the outer layer
Leaching material.
6. preparation method according to claim 1, which is characterized in that the width of the internal layer prepreg is 40~80mm；
And/or
The width of the outer layer prepreg is 50~110mm.
7. preparation method according to claim 1, which is characterized in that the internal layer prepreg uses wound in parallel or overlapping
The mode of winding is wound, winding with a thickness of 4~8mm.
8. preparation method according to claim 1, which is characterized in that the outer layer prepreg is by the way of tiltedly folded winding
Be wound, winding with a thickness of 8~9mm.
9. preparation method according to claim 1, which is characterized in that the solidification uses vacuum pressed solidification method, solidification
Process conditions are as follows: vacuum degree -0.085MPa is hereinafter, 120~180 DEG C of solidification temperature, 3~8h of curing time, solidifying pressure 0.8
~10MPa.
10. a kind of compound layer of resistance to ablative thermal protection of effectively insulating, which is characterized in that using according to any one of claims 1 to 9
Preparation method is prepared.
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| CN109927943A (en) * | 2019-04-04 | 2019-06-25 | 北京卫星制造厂有限公司 | Recoverable airship solar heat protection and carrying integral structure |
| 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 |
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| CN113024157A (en) * | 2021-03-25 | 2021-06-25 | 山东桐强防务科技有限公司 | Heat-proof material and preparation method thereof |
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