CN101417516A - Bearing/insulating/ablating all-in-one sandwich structure composite material and preparation method thereof - Google Patents
Bearing/insulating/ablating all-in-one sandwich structure composite material and preparation method thereof Download PDFInfo
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- CN101417516A CN101417516A CNA2008100307279A CN200810030727A CN101417516A CN 101417516 A CN101417516 A CN 101417516A CN A2008100307279 A CNA2008100307279 A CN A2008100307279A CN 200810030727 A CN200810030727 A CN 200810030727A CN 101417516 A CN101417516 A CN 101417516A
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Abstract
A composite material of sandwich structure integrating loading, heat insulation and ablation and the manufacturing method are characterized in that an integrated pre-forming body is acquired by puncture and suture of the reinforcing material of a bearing layer, the reinforcing material of an ablating cover, and a heating insulation layer positioned between the two layers; an epoxy resin system and a phenolic resin system are injected simultaneously into a vacuum-pumped mould, in which the integrated forming body is pre-placed, by two sets of RTM injection systems respectively, then, the reinforcing materials of the bearing layer and the ablating layer are soaked by epoxy resin and phenolic resin respectively; and the composite material of sandwich structure integrating loading, heat insulation and ablation can be obtained by solidified molding after mould filling. The invention has the advantages that the composite material of sandwich structure integrating loading, heat insulation and ablation is put forward and can be integrally formed by one-time operation, the function of the interlayer between every layer of the composite material is enhanced greatly, the integrality is good; the stratifying and peeling of the composite can be reduced effectively, and the products have good designable property and can be widely applied to the structural parts of aerospace which need heating insulation and thermal protection.
Description
Technical field
The present invention relates to a kind of Aero-Space composite, be specifically related to a kind of ablate bearing/insulating/ablating all-in-one sandwich structure composite and preparation method thereof of main force support structure spare of heat insulation requirement of Aero-Space that is used for satisfying, this composite can be Integratively formed.
Background technology
When high performance delivery vehicle of reentrying and hypersonic aircraft fly in atmosphere, the air of aircraft front is subjected to strong compression and rubbing action, most of kinetic energy is converted into heat energy, cause the ambient air temperature sharply to raise, and heat energy is rapidly to the aircraft surface transmission.This owing to object in the heating phenomena that atmosphere high speed flight produces, be called " pneumatic heating ".Aircraft position difference, its pneumatic heating environment is also inequality.The aircraft that continues to cruise with Ma6-10 is an example, its pneumatic heating of nose cone portion is the most serious, can reach 2800～3200 ℃, its nose of wing temperature generally also is more than 2000 ℃, and for large-area cabin body, pneumatic heating is not very serious, but maximum heating temperature generally also can reach 1000 ℃, increase along with flight Mach number, pneumatic heating will get over seriously, and the air themperature of stagnation region is with the increase that square is directly proportional of Mach number, and high temperature gas flow might cause guided missile surface modification profile, and the structural strength of change of flight device and rigidity have caused very the normal flight of aircraft to seriously influence.
Under the condition of High Temperature And Velocity airflow scouring, a kind of ablation thermal protection composite material is generally adopted on the structure surface, it be issue in the hot-fluid effect by material estrangedly separate, melt, the physics and the chemical change of multiple heat absorption such as evaporation, distillation and heat radiation, a large amount of heat energy are taken away in quality consumption with self, prevent that heat from importing internal structure into, thereby reach the heat insulation purpose of solar heat protection.
Existing application is prepared into heat shroud in the primary load bearing layer structure and the general preparation technology who adopts of thermal protection structure of aircraft and delivery vehicle with phenolic resin-base composite, by adhesive it is bonded in primary load bearing layer outer surface or Wrapping formed anti-ablation layer on the main force support structure layer of preparing again.This kind process is difficult to introduce thermal insulation layer between ablation layer and structure sheaf, to such an extent as to overall structure heat-proof quality difference and influenced the thermal protection effect of structure sheaf; And interface performance is poor between ablation layer and the structure sheaf, thereby has influenced its result of use.Ablation layer is taken away a large amount of heats except peeling off by ablation, and remaining thickness also will be used for heat insulationly being no more than its normal working temperature scope with the temperature that guarantees bearing bed.The ablation layer material also is that the thermal conductivity factor under the room temperature of phenolic resin-base composite is generally 0.2～0.6W/ (m.k), and density is generally 1100～1700kg/m
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Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes above-mentioned prior art, interlayer performance raising greatly between a kind of each layer, good integrity are provided, can effectively reduce Composites Delamination and peel off, the product designability is good, can be widely used in bearing/insulating/ablating all-in-one sandwich structure composite on the aerospace structure spare of the heat insulation and solar heat protection of needs and preparation method thereof.
For solving the problems of the technologies described above, the present invention adopts following technical proposals.
A kind of bearing/insulating/ablating all-in-one sandwich structure composite, it is characterized in that this composite is by the bearing bed with primary load bearing function, the ablation layer composition that has the thermal insulation layer of heat insulating function and have anti-ablation function, described thermal insulation layer is between bearing bed and ablation layer, this composite specifically is with the bearing bed reinforcing material, ablation layer reinforcing material and place thermal insulation layer puncture between two-layer reinforcing material to sew up to obtain integrated preform, inject separately resin system simultaneously to bearing bed reinforcing material and ablation layer reinforcing material again, Integratively formed and get.
Described bearing bed reinforcing material and ablation layer reinforcing material all are to be applied by the multi-layer fiber cloth shop to form, and described bearing bed resin system comprises epoxy resin, curing agent and promoter; The ablation layer resin system is a phenolic resins, or phenolic resins and catalyst.
Described bearing bed reinforcing material is a carbon fiber-free weft fabric, the carbon fiber plain, the carbon fiber twill, carbon fiber is forged a kind of in the line cloth, epoxy resin in the described bearing bed resin system is E-44 epoxy resin, E-51 epoxy resin, TDE-85 epoxy resin, bisphenol f type epoxy resin, a kind of in the AG-80 epoxy resin, described curing agent is a kind of of acid anhydride type curing agent, promoter is a kind of in the tertiary amine, wherein the consumption of curing agent is 60%～200% of an epoxy resin quality, the consumption of promoter is 0.1%～5% of an epoxy resin quality, the fiber volume fraction of bearing bed reinforcing material is 35～55%, and the volume content of resin system is 65%～45% accordingly.
Bearing bed also is the main force support structure layer, mainly is to prevent that aircraft or delivery vehicle from destroying owing to high overload and high pneumatic pressure during flying, and its thickness can carry out designing and calculating according to the service condition of aircraft and delivery vehicle.
Described thermal insulation layer is a light porous material, and described light porous material is a kind of in aeroge, PEI foam, polyimide foam, the polymethacrylimide foam.
Thermal insulation layer is a sandwich structure, and the main isolated heat that transmits to bearing bed by ablation layer requires to have lower thermal conductivity and lower density.Because bearing bed is the carbocyclic ring O compoiste material, general the upper limit temperature of heat tolerance is no more than 150 ℃, and the gross thickness of thermal insulation layer will guarantee that aircraft or delivery vehicle bearing bed temperature during flying is no more than 150 ℃.The thickness of thermal insulation layer can and obtain according to material properties and service condition calculating.
Described ablation layer reinforcing material is a carbon fiber, glass fibre, the plain of high silica fiber or quartz fibre, twill, forge a kind of in the line cloth, the phenolic resins of its resin system is bismaleimide modified phenolic resins benzoxazine colophony, the low pressure ba phenolic resin, a kind of in poly-aryl ethane resin or the cyanate modified phenolic resins, phenolic resins directly is heating and curing, or the adding catalyst is heating and curing, catalyst system therefor is imidazoles catalyst or tertiary amine catalyst, wherein the imidazoles catalyst consumption is 1%～10% of a phenolic resins quality, the consumption of tertiary amine catalyst is 0.1%～5% of a phenolic resins quality, the fiber volume fraction of ablation layer reinforcing material is 35～55%, and the corresponding volume content of resin system is 65%～45%.
Ablator be issue in the hot-fluid effect by material estrangedly separate, melt, the physics and the chemical change of multiple heat absorption such as evaporation, distillation and heat radiation, take away a large amount of heat energy with the quality consumption of self, thereby reach the purpose of solar heat protection.The ablation resistance of ablation layer is to calculate according to the thickness loss of ablation layer or the loss in weight, its gross thickness will prevent that aircraft or delivery vehicle from suffering a loss owing to overheated during flying, optimal situation is that aircraft or delivery vehicle ablation layer during flying all consume, and the basic structure of aircraft or delivery vehicle (bearing bed) is not suffered a loss.
Peel off for fear of ablation layer layer of cloth layering in ablation process, simultaneously also for fear of the changing of the relative positions between ablation layer and thermal insulation layer and the bearing bed, the process program that the present invention has adopted the reinforcing material to three-decker to puncture and sew up.The suture that described puncture is sewed up is a kind of in carbon fiber yarn, aramid fiber yarn, quartz fibre yarn, glass fiber yarn or the high silica fiber yarn, and it is chain sewing stitching or lock-stitch stitching that stitching is sewed up in puncture.Sewing density can be selected from the interval of 3mm * 3mm～15mm * 15mm, sews up stitching at interval evenly, promptly obtains integrated preform after stitching is finished.
When the integrated preform of preparation, the edge of thermal insulation layer is than the protruding 3～10mm in edge of corresponding bearing bed reinforcing material and ablation layer reinforcing material, do like this is in order by thermal insulation layer two kinds of glues that inject die cavity to be isolated, so that two kinds of glues soak into different separately reinforcing materials respectively.
Above-mentioned composite is prepared according to following step:
(1), cutting bearing bed reinforcing material, insulating layer material and ablation layer reinforcing material, and the edge that makes thermal insulation layer stretches out 3～10mm than the edge of corresponding bearing bed reinforcing material and ablation layer reinforcing material;
(2), bearing bed reinforcing material, insulating layer material and ablation layer reinforcing material are applied in the shop successively, according to the stitching of puncturing of given sewing density and stitching stitching, obtain integrated preform with suture;
(3), integrated preform is put into mould, matched moulds is preheated to 60 ℃～100 ℃; Described mould is the boundary with half of thermal insulation layer thickness in the integrated preform, is divided into former and formpiston two parts, and every part corresponds respectively to bearing bed one side and ablation layer one side to a cover gum-injecting port and a gum outlet should be arranged; Die cavity geomery that formpiston and former constituted and integrated preform measure-alike;
(4), after preheating is finished, two cover pumped vacuum systems are inserted set two gum outlets on the mould respectively, two cover RTM injecting systems are inserted two gum-injecting ports respectively, open pumped vacuum systems mould is vacuumized, require the vacuum of mould to reach-0.05MPa～-0.1MPa;
(5), epoxy resin and phenolic resins are put into a cover RTM injecting systems respectively, preheating ring epoxy resins and phenolic resins to 60 ℃～100 ℃, open two cover RTM injecting systems simultaneously, epoxy resin adhesive liquid and curing agent and promoter are mixed the back inject bearing bed one side, simultaneously with the phenolic resins glue, or add catalyst in the phenolic resins glue and mix back injection ablation layer one side, and adjust the injection pressures of two cover RTM injecting systems synchronously, soak into bearing bed reinforcing material and ablation layer reinforcing material to guarantee epoxy resin adhesive liquid and phenolic resins glue basic synchronization in mould, wherein, the injection pressure of epoxy resin is 0.01MPa～0.1MPa, and the injection pressure of phenolic resins is 0.05MPa～0.5MPa; Described curing agent is a kind of of acid anhydride type curing agent, and promoter is a kind of in the tertiary amine, and wherein the consumption of curing agent is 60%～200% of an epoxy resin quality, and the consumption of promoter is 0.1%～5% of an epoxy resin quality; After two gum outlets of mould begin to have two kinds of glues to flow out, stop injection;
(6), remove pumped vacuum systems and RTM injecting systems, mould is put into baking oven is cured;
(7), solidify finish after, the demoulding, finishing, the edge that thermal insulation layer is had more removes, get final product composite of the present invention.
Catalyst in the described step (5) is imidazoles catalyst or tertiary amine catalyst, and wherein the imidazoles catalyst consumption is 1%～10% of a phenolic resins quality, and the consumption of tertiary amine catalyst is 0.1%～5% of a phenolic resins quality.
Described curing operation is that epoxy resin and phenolic resins are cured under same curing system, be exactly to be incubated 2～4 hours down specifically at 100 ℃～120 ℃, be incubated 2～4 hours down at 130 ℃～150 ℃ then, be incubated 2～4 hours down at 160 ℃～200 ℃ then.
Compared with prior art, the present invention's proposition has also prepared the bearing/insulating/ablating all-in-one sandwich structure composite, thermal insulation layer light weight, advantage that thermal conductivity factor is low have been given full play to, under identical service condition, the present invention can prepare the integrated composite that quality significantly reduces, this is significant for the preparation of the space flight part of " is target to reduce each gram mass ".The present invention can design each layer of goods preform according to different service conditions, the product designability is good, realized the Integratively formed of bearing bed, thermal insulation layer, ablation layer three-decker, the composite product good integrity helps enhancing productivity.Introduced thermal insulation layer between bearing bed and ablation layer, thermal insulation layer is a porous material, and the thermal conductivity factor under its room temperature is generally 0.01～0.6W/ (m.k), and density is 40～200kg/m
3, so the integrated composite for preparing of the present invention can loss of weight under identical service condition more than 30%, application on the space flight part has positive effect for this composite for this.Stitching can significantly improve the interlayer performance of composite, the present invention adopts the puncture sewing process that three layers of reinforcing material are prepared into integrated preform and finally prepare integrated composite, the interlaminar shear strength of composite can improve more than 40%, and Composites Delamination reduces greatly with peeling off also.
Description of drawings
Fig. 1 implements the sectional view of example for composite of the present invention;
The integrated preform schematic diagram of Fig. 2;
Fig. 3 is a moulding process flow chart of the present invention;
Fig. 4 is the moulding process system diagram;
Fig. 5 is the formpiston schematic diagram;
Fig. 6 is the former schematic diagram.
Wherein
A, ablation layer B, thermal insulation layer
C, bearing bed D, suture
A, ablation layer reinforcing material b, insulating layer material
C, bearing bed reinforcing material e, integrated preform
1, epoxy resin container 2, curing agent container
3, resin meter 4, curing agent meter
5, resin transmits pipeline 6, curing agent transmits pipeline
7, pneumatics pump 8, Pressure gauge
9, resin and curing agent mixing point 10, epoxy-resin systems injection pipeline
11, phenolic resins container 12, curing agent container
13, resin meter 14, curing agent meter
15, resin transmits pipeline 16, curing agent transmits pipeline
17, pneumatics pump 18, Pressure gauge
19, mixing point 20, phenolic resin system injection pipeline
21, gum-injecting port 22, gum outlet
23, gum-injecting port 24, gum outlet
25, formpiston 26, former
27, epoxy-resin systems collection container 28, vavuum pump
29, vacuum meter 30, epoxy-resin systems vacuumize/the plastic emitting pipeline
31, phenolic resin system collection container 32, vavuum pump
33, vacuum meter 34, phenolic resin system vacuumize/the plastic emitting pipeline
35, fastening screw hole 36, seal groove.
The specific embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.
As shown in Figure 1, bearing/insulating/ablating all-in-one sandwich structure composite of the present invention, be made up of the bearing bed C with primary load bearing function, the ablation layer A that has the thermal insulation layer B of heat insulating function and have an anti-ablation function, thermal insulation layer B is between bearing bed C and ablation layer A.It is bearing bed reinforcing material c, insulating layer material b and ablation layer reinforcing material a to be sewed up by suture D puncture obtain (as shown in Figure 2) behind the integrated preform e, inject separately resin system simultaneously to bearing bed reinforcing material c and ablation layer reinforcing material a, Integratively formed and get.The bearing bed resin system comprises epoxy resin, curing agent and promoter; The ablation layer resin system is a phenolic resins, or phenolic resins and catalyst.
Embodiment one: prepare certain bearing/insulating/ablating all-in-one sandwich structure composite
Shown in Fig. 3,4, the concrete processing step for preparing composite of the present invention is as follows:
Cutting bearing bed reinforcing material c.Used reinforcing material is the carbon fiber twill, and available from toray company, the trade mark is T300 3K, centre plane density 200g/m
2, according to the stack shop is deposited successively behind 10 layers of carbon fiber twill of formpiston 25 geomery cuttings as shown in Figure 5, the fiber volume fraction of reinforcing material is 45%.
Cutting insulating layer material b.Used insulating layer material is the PEI foam that Switzerland AIREX company produces, and the trade mark is AIREX R82.80, and thermal conductivity is 0.037W/mk, and density is 80kg/m
3The thickness of foam is 20mm, the edge of insulating layer material b has more 5mm than the edge of corresponding ablation layer reinforcing material a and bearing bed reinforcing material c, and (see Fig. 2,5,6 illustrated dimension " f ", f can be 3～10mm), and the shop was applied on bearing bed reinforcing material c after cutting was finished.
Cutting ablation layer reinforcing material a.Used reinforcing material is that quartz fibre is forged line cloth, and available from the Qianjiang friendly special fibre of crowd Materials Co., Ltd, the trade mark is ZY/QW140-92, and centre plane density is 150g/m
2, according to after 35 layers of as shown in Figure 6 the former 26 geomery cuttings successively the stack shop apply on insulating layer material b, the fiber volume fraction of reinforcing material is 45%.
Adopt suture D with ablation layer reinforcing material a, insulating layer material b and the bearing bed reinforcing material c stitching of puncturing.Used suture D is the aramid fiber yarn that du pont company produces, the trade mark is Kevlar-29 (3200 dawn), sewing density is that 4mm * 4mm (can be 3mm * 3mm～15mm * 15mm), after puncturing stitching, Singer-11 type industrial sewing machine obtains integrated preform e according to the lock-stitch stitching, as shown in Figure 2.
Shown in Fig. 4,5 and 6, the mould of preparation composite of the present invention is made up of formpiston 25 and former 26 two parts, and two parts mould is to be the boundary with half of insulating layer material b thickness among the integrated preform e.Formpiston 25 has gum-injecting port 21 and the gum outlet 22 of a cover corresponding to the epoxy-resin systems of bearing bed one side, former 26 has gum-injecting port 23 and the gum outlet 24 of a cover corresponding to the phenolic resin system of ablation layer one side, wherein the runner that constituted of the gum-injecting port 21 of formpiston 25 and gum outlet 22 is used for soaking into bearing bed reinforcing material c, and the runner that the gum-injecting port 23 of former 26 and gum outlet 24 are constituted is used for soaking into ablation layer reinforcing material a.Formpiston 25 is identical with integrated preform e geomery with the die cavity geomery that former 26 is constituted, and is processed with seal groove 36 in the former 26 therein, is used for the sealing of mould.
Integrated preform e is put into mould, bearing bed one side is in formpiston 25, and ablation layer one side is put into sealing rubber ring in seal groove 36 in former 26, formpiston 25 and former 26 is fastening with screw rod by fastening screw hole 35 as shown in Figure 5 and Figure 6, check the mould air-tightness.
Mould inserted be preheated to 80 ℃ in the baking oven.
As shown in Figure 4, the used RTM injecting systems of the present invention comprises plastic holding device (being respectively epoxy resin container 1 and phenolic resins container 11), curing agent container 2 (12) and resin system injection pipeline (being respectively epoxy-resin systems injection pipeline 10 and phenolic resin system injection pipeline 20), plastic holding device transmits pipeline 5 (15) via resin meter 3 (13) and curing agent meter 4 (14) and resin respectively with curing agent container 2 (12) and links to each other with curing agent transmission pipeline 6 (16), through mixing point 9 (19) the threaded tree resin systems injection pipeline (being respectively epoxy-resin systems injection pipeline 10 and phenolic resin system injection pipeline 20) of two pipelines, be provided with pneumatics pump 7 (17) and Pressure gauge 8 (18) again in resin transmission pipeline 5 (15) and curing agent transmission pipeline 6 (16).The used pumped vacuum systems of the present invention comprises vavuum pump 28 (32), resin system collection container (being respectively epoxy-resin systems collection container 27 and phenolic resin system collection container 31) and resin system vacuumize/plastic emitting pipeline (be respectively epoxy-resin systems vacuumize/plastic emitting pipeline 30 and phenolic resin system vacuumize/plastic emitting pipeline 34), vavuum pump 28 links to each other with epoxy-resin systems collection container 27 by pipeline, 32 in vavuum pump links to each other with phenolic resin system collection container 31 by pipeline, epoxy-resin systems collection container 27 vacuumizes with epoxy-resin systems/and plastic emitting pipeline 30 joins, phenolic resin system collection container 31 vacuumizes with phenolic resin system/and plastic emitting pipeline 34 joins, epoxy-resin systems collection container 27 is connected with vacuum meter 29, and phenolic resin system collection container 31 is connected with vacuum meter 33.
As shown in Figure 4, TDE-85 epoxy resin in the bearing bed resin system is put into the epoxy resin container 1 of a cover RTM injecting systems, and, curing agent 70 acid anhydrides and altax P-30 are put into curing agent container 2 according to 114: 0.7 proportionings with TDE-85 epoxy resin preheating to 80 ℃.Regulate resin meter 3 and curing agent meter 4, the mass ratio of TDE-85 epoxy resin, 70 acid anhydrides and DMP-30 is 100: 114: 0.7 in the bearing bed resin system when guaranteeing injection.
The low pressure ba phenolic resin of ablation layer resin system is put into the phenolic resins container 11 of another set of RTM injecting systems, and the low pressure ba phenolic resin is preheated to 80 ℃.
After mould and die preheating is finished, mould is taken out from baking oven.The epoxy-resin systems of one cover pumped vacuum systems is vacuumized/plastic emitting pipeline 30 inserts the gum outlet 22 of formpistons 25, the epoxy-resin systems injection pipeline 10 that fills a cover RTM injecting systems of epoxy resin inserted the gum-injecting port 21 of formpistons 25; The phenolic resin system of another set of pumped vacuum systems is vacuumized/plastic emitting pipeline 34 inserts the gum outlet 24 of formers 26, the phenolic resin system injection pipeline 20 that fills a cover RTM injecting systems of phenolic resins inserted the gum-injecting port 23 of formers 26.
Closed loop epoxy resins injection pipeline 10 and phenolic resins injection pipeline 20, open the vavuum pump 28 and the vavuum pump 32 of two cover pumped vacuum systems, mould is vacuumized, checking system vacuum, and keeping the system vacuum degree to be-0.08MPa, the system vacuum degree can obtain from vacuum meter 29 and vacuum meter 33 readings.
Open epoxy resin injection pipeline 10, regulate pneumatics pump 7, the registration that makes Pressure gauge 8 is 0.01MPa, and epoxy resin and curing agent thereof and promoter are just transmitted pipeline 5 and curing agent by resin and transmitted pipeline 6 and mix the back at resin and curing agent mixing point 9 and inject moulds by epoxy-resin systems injection pipeline 10 and soak into bearing bed reinforcing material c.
When opening epoxy resin injection pipeline 10, also open phenolic resin system injection pipeline 20, regulate pneumatics pump 17, the registration that makes Pressure gauge 18 is 0.1MPa, and phenolic resins just transmits pipeline 15 by resin and soaks into ablation layer reinforcing material a through mixing point 19 along phenolic resin system injection pipeline 20 injection moulds.
After the gum outlet 22 and 24 of mould began to have glue to flow out, closed loop epoxy resins injection pipeline 10 and phenolic resins injection pipeline 20 stopped injection; Close vavuum pump 28 and vavuum pump 32, stop to vacuumize.The epoxy glue solution that flows out mould can vacuumize by epoxy-resin systems/and plastic emitting pipeline 30 flows in the epoxy-resin systems collection containers 27, and the phenolic aldehyde glue that flows out mould can vacuumize by phenolic resin system/and plastic emitting pipeline 34 flows in the phenolic resin system collection containers 31.The volume content of gained bearing bed resin system is 55%, and the volume content of ablation layer resin system is 55%.
Epoxy resin is injected pipeline 10 and phenolic resins injection pipeline 20, epoxy-resin systems vacuumizes/plastic emitting pipeline 30 and phenolic resin system vacuumize/and plastic emitting pipeline 34 removes from mould respectively, and mould is put into baking oven.
Set oven temperature, according to 100 ℃ of 2h, 130 ℃ of 2h, the curing system of 160 ℃ of 4h is cured operation simultaneously to epoxy-resin systems and phenolic resin system.
After curing is finished, mould is taken out from baking oven, the demoulding, finishing, cleaning, the edge that thermal insulation layer is had more removes, and obtains composite product of the present invention.
Embodiment two: use the present invention and prepare certain bearing/insulating/ablation integral composite structure
Cutting bearing bed reinforcing material c.Used reinforcing material is the carbon fiber plain, and available from toray company, the trade mark is T300 3K, centre plane density 200g/m
2, the stack shop is deposited successively behind 12 layers of carbon cloth of cutting, and the fiber volume fraction of reinforcing material is 50%.
Cutting insulating layer material b.Used insulating layer material b is the polymethacrylimide foam of German goldschmidt chemical corporation, the trade mark is ROHACELL 71XT, the thickness of foam is 25mm, the edge of thermal insulation layer b will have more 6mm (seeing Fig. 2,5,6 illustrated dimension " f ") than the edge of corresponding ablation layer reinforcing material a and bearing bed reinforcing material c, and the shop was applied on bearing bed reinforcing material c after cutting was finished.
Cutting ablation layer reinforcing material a.Used ablation layer reinforcing material a is the carbon fiber twill, and available from toray company, the trade mark is T300 3K, centre plane density 200g/m
2, after 35 layers of the cuttings successively the stack shop apply on insulating layer material b, the fiber content of reinforcing material is 50%.
Adopt suture D with ablation layer reinforcing material a, insulating layer material B and the bearing bed reinforcing material c stitching of puncturing.Used suture is the aramid fiber yarn that du pont company produces, the trade mark is Kevlar-29 (3200 dawn), sewing density is 6mm * 6mm, obtains integrated preform e (see figure 2) according to the lock-stitch stitching after Singer-11 type industrial sewing machine punctures stitching.
Shown in Fig. 4,5 and 6, the mould of preparation composite of the present invention is made up of formpiston 25 and former 26 two parts, and two parts mould is to be the boundary with half of integrated preform e insulating layer material b thickness.Formpiston 25 has gum-injecting port 21 and the gum outlet 22 of a cover corresponding to the epoxy-resin systems of bearing bed one side, former 26 has gum-injecting port 23 and the gum outlet 24 of a cover corresponding to the phenolic resin system of ablation layer one side, wherein the runner that constituted of the gum-injecting port 21 of formpiston 25 and gum outlet 22 is used for soaking into bearing bed reinforcing material c, and the runner that the gum-injecting port 23 of former 26 and gum outlet 24 are constituted is used for soaking into ablation layer reinforcing material a.Formpiston 25 is identical with integrated preform e geomery with the die cavity geomery that former 26 is constituted, and is processed with seal groove 36 in the former 26 therein, is used for the sealing of mould.
Integrated preform e is put into mould, bearing bed one side is in formpiston 25, and ablation layer one side is put into sealing rubber ring in seal groove 36 in former 26, formpiston 25 and former 26 is fastening with screw rod by fastening screw hole 35 as shown in Figure 5 and Figure 6, check the mould air-tightness.
Mould inserted be preheated to 90 ℃ in the baking oven.
As shown in Figure 4, the E-51 epoxy resin in the bearing bed resin system is put into epoxy resin container 1, and with E-51 epoxy resin preheating to 90 ℃.According to 78: 0.7 proportionings curing agent 70 acid anhydrides and altax P-30 are put into curing agent container 2.Regulate resin meter 3 and curing agent meter 4, the mass ratio of TDE-85 epoxy resin, 70 acid anhydrides and DMP-30 is 100: 78: 0.7 during with the assurance injection.
The benzoxazine colophony of ablation layer resin system is put into phenolic resins container 11, and benzoxazine colophony is preheated to 90 ℃.The catalyst 2-ethyl-4-methylimidazole is put into curing agent container 12, regulate resin meter 13 and curing agent meter 14, the mass ratio of benzoxazine colophony and 2-ethyl-4-methylimidazole is 100: 8 during with the assurance injection.
After mould and die preheating is finished, mould is taken out from baking oven.Epoxy-resin systems is vacuumized/plastic emitting pipeline 30 access gum outlets 22, epoxy-resin systems injection pipeline 10 inserts gum-injecting ports 21; Phenolic resin system is vacuumized/plastic emitting pipeline 34 access gum outlets 24, phenolic resin system injection pipeline 20 inserts gum-injecting ports 23.
Closed loop epoxy resins injection pipeline 10 and phenolic resins injection pipeline 20, open vavuum pump 28 and vavuum pump 32, mould is vacuumized checking system vacuum, and keeping system vacuum degree-0.09MPa, the system vacuum degree can obtain from vacuum meter 29 and vacuum meter 33 readings.
Open epoxy resin injection pipeline 10, regulate pneumatics pump 7, the registration that makes Pressure gauge 8 is 0.015MPa, epoxy resin and curing agent thereof and promoter are just transmitted pipeline 5 and curing agent by resin and are transmitted pipeline 6 after resin and curing agent mixing point 9 mix, and inject moulds by epoxy-resin systems injection pipeline 10 and soak into bearing bed reinforcing material c.
When opening epoxy resin injection pipeline 10, also open phenolic resin system injection pipeline 20, regulate pneumatics pump 17, the registration that makes Pressure gauge 18 is 0.2MPa, and benzoxazine colophony and 2-ethyl-4-methylimidazole just transmit pipeline 15 by resin and curing agent transmission pipeline 16 soaks into ablation layer reinforcing material a through mixing points 19 along phenolic resin system injection pipeline 20 injection moulds.
After the gum outlet 22 and 24 of mould began to have glue to flow out, closed loop epoxy resins injection pipeline 10 and phenolic resins injection pipeline 20 stopped injection; Close vavuum pump 28 and vavuum pump 32, stop to vacuumize.The epoxy glue solution that flows out mould can vacuumize by epoxy-resin systems/and plastic emitting pipeline 30 flows in the epoxy-resin systems collection containers 27, and the phenolic aldehyde glue that flows out mould can vacuumize by phenolic resin system/and plastic emitting pipeline 34 flows in the phenolic resin system collection containers 31.The volume content of gained bearing bed resin system is 50%, and the volume content of ablation layer resin system is 50%.
Epoxy resin is injected pipeline 10 and phenolic resins injection pipeline 20, epoxy-resin systems vacuumizes/plastic emitting pipeline 30 and phenolic resin system vacuumize/and plastic emitting pipeline 34 removes from mould respectively, and mould is put into baking oven.
Set oven temperature, according to 100 ℃ of 2h, 140 ℃ of 2h, the curing system of 180 ℃ of 4h comes epoxy-resin systems and phenolic resin system are cured operation simultaneously.
After curing is finished, mould is taken out from baking oven, the demoulding, finishing, cleaning, the edge that thermal insulation layer is had more removes, and obtains composite product of the present invention.
The bearing/insulating/ablating all-in-one sandwich structure composite that the present invention proposes and prepares, the interlayer performance improves greatly between each layer of composite, can effectively reduce Composites Delamination and peel off, the product designability is good, can be widely used on the aerospace structure spare of the heat insulation and solar heat protection of needs, the product good integrity of preparing, product quality significantly reduces, excellent combination property.Conceive identical various process programs all among claims protection domain of the present invention with the present invention.
Claims (10)
1, a kind of bearing/insulating/ablating all-in-one sandwich structure composite, it is characterized in that this composite is by the bearing bed with primary load bearing function, the ablation layer composition that has the thermal insulation layer of heat insulating function and have anti-ablation function, described thermal insulation layer is between bearing bed and ablation layer, this composite specifically is with the bearing bed reinforcing material, ablation layer reinforcing material and place thermal insulation layer puncture between two-layer reinforcing material to sew up to obtain integrated preform, inject separately resin system simultaneously to bearing bed reinforcing material and ablation layer reinforcing material again, Integratively formed and get.
2, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 1, it is characterized in that described bearing bed reinforcing material and ablation layer reinforcing material all are to be applied by the multi-layer fiber cloth shop to form, described bearing bed resin system comprises epoxy resin, curing agent and promoter; The ablation layer resin system is a phenolic resins, or phenolic resins and catalyst.
3, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 2, it is characterized in that described bearing bed reinforcing material is a carbon fiber-free weft fabric, the carbon fiber plain, the carbon fiber twill, carbon fiber is forged a kind of in the line cloth, epoxy resin in the described bearing bed resin system is E-44 epoxy resin, E-51 epoxy resin, TDE-85 epoxy resin, bisphenol f type epoxy resin, a kind of in the AG-80 epoxy resin, described curing agent is a kind of of acid anhydride type curing agent, promoter is a kind of in the tertiary amine, wherein the consumption of curing agent is 60%～200% of an epoxy resin quality, the consumption of promoter is 0.1%～5% of an epoxy resin quality, the fiber volume fraction of bearing bed reinforcing material is 35～55%, and the volume content of resin system is 65%～45% accordingly.
4, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 2, it is characterized in that described thermal insulation layer is a light porous material, described light porous material is a kind of in aeroge, PEI foam, polyimide foam, the polymethacrylimide foam.
5, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 2, it is characterized in that described ablation layer reinforcing material is a carbon fiber, glass fibre, the plain of high silica fiber or quartz fibre, twill, forge a kind of in the line cloth, phenolic resins in its resin system is bismaleimide modified phenolic resins benzoxazine colophony, the low pressure ba phenolic resin, a kind of in poly-aryl ethane resin or the cyanate modified phenolic resins, phenolic resins directly is heating and curing, or the adding catalyst is heating and curing, catalyst system therefor is imidazoles catalyst or tertiary amine catalyst, wherein the imidazoles catalyst consumption is 1%～10% of a phenolic resins quality, the consumption of tertiary amine catalyst is 0.1%～5% of a phenolic resins quality, the fiber volume fraction of ablation layer reinforcing material is 35～55%, and the corresponding volume content of resin system is 65%～45%.
6, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 1 and 2; it is characterized in that suture that described puncture is sewed up is a kind of in carbon fiber yarn, aramid fiber yarn, quartz fibre yarn, glass fiber yarn or the high silica fiber yarn, it is chain sewing stitching or lock-stitch stitching that stitching is sewed up in puncture.
7, bearing/insulating/ablating all-in-one sandwich structure composite according to claim 1 and 2, it is characterized in that: when the integrated preform of preparation, the edge of thermal insulation layer is than the protruding 3～10mm in edge of corresponding bearing bed reinforcing material and ablation layer reinforcing material.
8, a kind of preparation method of the composite of bearing/insulating/ablating all-in-one sandwich structure according to claim 1 is characterized in that being prepared according to following step:
(1), cutting bearing bed reinforcing material, insulating layer material and ablation layer reinforcing material, and the edge that makes thermal insulation layer stretches out 3～10mm than the edge of corresponding bearing bed reinforcing material and ablation layer reinforcing material;
(2), bearing bed reinforcing material, insulating layer material and ablation layer reinforcing material are applied in the shop successively, according to the stitching of puncturing of given sewing density and stitching stitching, obtain integrated preform with suture;
(3), integrated preform is put into mould, matched moulds is preheated to 60 ℃～100 ℃; Described mould is the boundary with half of thermal insulation layer thickness in the integrated preform, is divided into former and formpiston two parts, and every part corresponds respectively to bearing bed one side and ablation layer one side to a cover gum-injecting port and a gum outlet should be arranged; Die cavity geomery that formpiston and former constituted and integrated preform measure-alike;
(4), after preheating is finished, two cover pumped vacuum systems are inserted set two gum outlets on the mould respectively, two cover RTM injecting systems are inserted two gum-injecting ports respectively, open pumped vacuum systems mould is vacuumized, require the vacuum of mould to reach-0.05MPa～-0.1MPa;
(5), epoxy resin and phenolic resins are put into a cover RTM injecting systems respectively, preheating ring epoxy resins and phenolic resins, to 60 ℃～100 ℃, open two cover RTM injecting systems simultaneously, epoxy resin adhesive liquid and curing agent and promoter are mixed the back inject bearing bed one side, simultaneously with the phenolic resins glue, or add catalyst in the phenolic resins glue and mix back injection ablation layer one side, and adjust the injection pressures of two cover RTM injecting systems synchronously, wherein, the injection pressure of epoxy resin is 0.01MPa～0.1MPa, and the injection pressure of phenolic resins is 0.05MPa～0.5MPa; Described curing agent is a kind of of acid anhydride type curing agent, and promoter is a kind of in the tertiary amine, and wherein the consumption of curing agent is 60%～200% of an epoxy resin quality, and the consumption of promoter is 0.1%～5% of an epoxy resin quality; After two gum outlets of mould begin to have two kinds of glues to flow out, stop injection;
(6), remove pumped vacuum systems and RTM injecting systems, mould is put into baking oven is cured;
(7), solidify finish after, the demoulding, finishing can obtain this composite.
9, the preparation method of composite according to claim 8, it is characterized in that catalyst is imidazoles catalyst or tertiary amine catalyst in the described step (5), wherein the imidazoles catalyst consumption is 1%～10% of a phenolic resins quality, and the consumption of tertiary amine catalyst is 0.1%～5% of a phenolic resins quality.
10, according to Claim 8 or the preparation method of 9 described composites, it is characterized in that described curing operation is that epoxy resin and phenolic resins are cured under same curing system, be incubated 2～4 hours down at 100 ℃～120 ℃, be incubated 2～4 hours down at 130 ℃～150 ℃ then, be incubated 2～4 hours down at 160 ℃～200 ℃ then.
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