CN114953507A - Preparation method of ablation-resistant local thermal protection material for surface continuous braid - Google Patents
Preparation method of ablation-resistant local thermal protection material for surface continuous braid Download PDFInfo
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- CN114953507A CN114953507A CN202210582597.XA CN202210582597A CN114953507A CN 114953507 A CN114953507 A CN 114953507A CN 202210582597 A CN202210582597 A CN 202210582597A CN 114953507 A CN114953507 A CN 114953507A
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- 238000002679 ablation Methods 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 76
- 239000011347 resin Substances 0.000 claims abstract description 76
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000005011 phenolic resin Substances 0.000 claims abstract description 69
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 69
- 239000000835 fiber Substances 0.000 claims abstract description 50
- 239000000919 ceramic Substances 0.000 claims abstract description 29
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 26
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 239000002344 surface layer Substances 0.000 claims abstract description 16
- 239000010410 layer Substances 0.000 claims abstract description 11
- 238000012805 post-processing Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 42
- 239000010453 quartz Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000003292 glue Substances 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000011161 development Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000006748 scratching Methods 0.000 claims description 2
- 230000002393 scratching effect Effects 0.000 claims description 2
- 238000009954 braiding Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000003754 machining Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- -1 phenolic aldehyde Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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- 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
- B29C70/34—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 and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
- B29C70/342—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 and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation using isostatic pressure
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/40—Weight reduction
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
A surface layer continuous braid body ablation-resistant local thermal protection material preparation method, the surface layer uses the medium porcelain resin to presoak 2.5D braid body to make the prepreg of medium porcelain resin, use the vacuum bag to press and make prepreg and die cavity laminate closely after the mould preheats; the inner layer is made into a phenolic resin premix by adopting ablation-resistant phenolic resin mixed chopped fibers, and a layer of medium-ceramic resin prepreg is laid on the surface of the premix to finish final pressing when the last filling is pre-pressed by three times of filling on a press; after the bolts are fastened, the bolts are cured, and finally, the local thermal protection material structural member is prepared by demolding and post-processing; after being cured, the invention greatly improves the ablation resistance and has higher rigidity; the toughness of the local thermal protection material is greatly improved; and the net size of the prepared local thermal protection component is formed, so that the damage of machining to the overall strength of the component is avoided, the material waste is reduced, and the manufacturing period is shortened.
Description
Technical Field
The invention relates to the technical field of local thermal protection materials for aircrafts, in particular to a preparation method of an ablation-resistant local thermal protection material for a surface continuous woven body.
Background
Localized thermal protective materials are important materials to protect aircraft from burnout or overheating in high temperature thermal environments. At present, the heat-proof materials outside aircrafts at home and abroad are generally resin-based ablation heat-proof materials, and standard-density ablation materials represented by carbon cloth/phenolic aldehyde, glass cloth/phenolic aldehyde and high-silica cloth/phenolic aldehyde are mainly applied to remote aircrafts which are in service in extremely severe thermal environments such as high heat flow, ultrahigh temperature, high stagnation pressure, high-speed particle scouring and the like in a short time.
The traditional preparation method has high material cost and processing cost, and the surface fiber of the composite material is cut by a cutter in the processing process, so that the mechanical property and the ablation and erosion resistance of the composite material are reduced, the Chinese patent 'a heat insulation composite material formed by winding a prepreg tape and a preparation method thereof' describes a preparation method for winding and forming a heat protection material, the preparation method needs machining after preparation, the surface fiber is discontinuous, the ablation resistance is greatly reduced, and the heat protection composite material prepared by the traditional method under the thermal environment conditions of high Mach number, high heat flow and high pressure cannot meet the requirement of the aerodynamic appearance of an aircraft due to excessive local ablation.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of an ablation-resistant local thermal protection material for a surface layer continuous braided body, wherein the ablation resistance of the surface layer is greatly improved after a medium-ceramic resin preimpregnated 2.5D braided body is solidified, and the surface layer continuous braided body has higher rigidity; the interior of the thermal protective material is filled with a phenolic resin premix prepared by mixing chopped fibers with ablation-resistant phenolic resin, so that the thermal protective material has high ablation resistance and the toughness of the local thermal protective material is greatly improved; and the net size of the prepared local thermal protection component is formed, so that the damage of machining to the overall strength of the component is avoided, the material waste is reduced, and the manufacturing period is shortened.
In order to achieve the purpose, the invention adopts the following technical scheme:
a surface layer continuous braid body ablation-resistant local thermal protection material preparation method, the surface layer uses the medium porcelain resin to presoak 2.5D braid body to make the prepreg of medium porcelain resin, use the vacuum bag to press and make prepreg and die cavity laminate closely after the mould preheats; the inner layer is made into a phenolic resin premix by adopting ablation-resistant phenolic resin mixed chopped fibers, and a layer of medium-ceramic resin prepreg is laid on the surface of the premix to complete final pressing when the last filling is prepressed by filling for three times on a press; and (4) solidifying after fastening the bolts, and finally preparing the local thermal protection material structural member by demolding and post-processing.
A preparation method of a local ablation-resistant thermal protection material of a surface continuous woven body comprises the following steps:
s1, preparing a medium porcelain resin prepreg: spreading release paper on a heating platform, spreading a quartz fiber woven body on the release paper after the preheating temperature of the heating platform reaches 50-60 ℃, and fixing the edge by adopting a clamp; after the fixation is finished, drying the quartz fiber braided body for 30-60min at the temperature of 50-60 ℃; weighing ablation-resistant medium-porcelain resin according to 1-1.5 times of the mass of the quartz fiber woven body, dividing the ablation-resistant medium-porcelain resin into two parts, pouring one part of the ablation-resistant medium-porcelain phenolic resin into the center of the quartz fiber woven body, driving the glue from the central area to the periphery, and uniformly rolling and turning over by using a tetrafluoro roller; driving the other part of the ablation-resistant medium-ceramic resin to glue from the central area to the periphery again, and uniformly rolling by using a tetrafluoro roller; in the process of using a tetrafluoro roller to roll glue, the glue rolling direction must be parallel to the warp direction or the weft direction; after the ablation-resistant mesoceramic resin is uniformly rolled, keeping the temperature of a heating platform at 70-80 ℃, and drying for 30-120min to prepare mesoceramic resin prepreg;
s2, preparation of phenolic resin premix: putting the quartz fiber fixed-length yarn into an oven, and drying for 30-60min at 50-60 ℃; weighing ablation-resistant phenolic resin according to 1-1.5 times of the mass of the quartz fiber fixed-length yarn, and mixing the ablation-resistant phenolic resin and the quartz fiber fixed-length yarn in a basin; uniformly mixing ablation-resistant resin and quartz fiber fixed-length yarns to obtain a premix, grabbing the premix by using a close-tooth rake, putting the loose premix to a heating platform, keeping the temperature of the heating platform at 70-80 ℃, and preserving heat for 30-90min to obtain a phenolic resin premix;
s3, cutting the vitrified resin prepreg in the step S1 according to the surface layer development picture of the composite material member, and weighing the mass m after cutting; multiplying the volume of the die cavity by the target density to be 1.4-1.6g/cm 3 Calculating to obtain the total mass M; weighing the mass M-M of the phenolic resin premix in the step S2;
s4, filler: spraying a release agent for 1-3 times on the surface of the mold and the inside of the mold cavity, placing the mold in an oven, baking at the temperature of 70-90 ℃ for 60-120min, maintaining the temperature of the mold at 70-90 ℃, fixing the mold on a press, installing an upper mold at the upper end of the press, installing a lower mold at the lower end of the press, laying the cut mesoceramic resin prepreg in the step S3 on the inner molded surface of the mold, tightly attaching the cut mesoceramic resin prepreg to the surface of the mold by using vacuum bag pressure, keeping the vacuum degree of the vacuum bag pressure to be not less than-0.085 MPa, and keeping the pressure for 10-50 min; filling the phenolic resin premix weighed in the step S3 into a cavity formed by the medium-ceramic resin prepreg for three times, wherein the first filling amount is 70-80% of the total amount, pre-pressing for 5-10min after filling, the pre-pressing pressure is 1-5MPa, then opening, and using a dense tooth rake to loosen the phenolic resin premix on the surface; then adding 10-15% of the total amount of the phenolic resin premix for secondary prepressing, opening the prepressing for 5-10min, and continuously using a dense tooth rake to loosen the phenolic resin premix on the surface; then filling the rest of the phenolic resin premix, paving a layer of medium-ceramic resin prepreg on the surface of the phenolic resin premix, and then finishing final pressure, wherein the final pressure is 5-10min and is 1-5 Mpa;
s5, mold closing: fastening the die after the final pressing by using bolts, and taking down the die from the press after the fastening is finished;
s6, curing: putting the mould into an oven, and heating and curing according to a curing system of the medium-ceramic resin;
s7, demolding: after the curing is finished, taking out the mold when the temperature of the oven is reduced to be within 60 ℃, and demolding when the temperature of the mold is reduced to be within 40 ℃;
s8, post-processing: and (5) polishing the burrs on the edge of the product by using sand paper.
Compared with the prior art, the invention has at least the following beneficial effects
The clean-type forming local thermal protection composite material of the continuous surface-layer braided body is prepared by adopting a die pressing process clean-type forming mode through structural design and process optimization, has an ablation-resistant structure of the continuous surface-layer quartz fiber braided body, and has the advantages of excellent pneumatic appearance and portable installation function. The design of adopting the surface continuous fabric has the advantage of improving and enhancing the ablation performance; the net-shaped forming process is adopted, so that the material waste caused by machining is avoided, and the production cost is reduced; the product density is properly reduced by controlling the proportion of the filler, the mechanical toughness is improved, and the method has the advantages of controllable material density and improved material toughness; in conclusion, the invention has the advantages of improving the ablation performance of the product, shortening the production period, reducing the manufacturing cost and the like.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Referring to fig. 1, embodiment 1, a method for preparing an ablation-resistant local thermal protection material for a surface layer continuous woven body comprises the following steps:
s1, preparing a medium porcelain resin prepreg: spreading release paper on a heating platform, spreading a quartz fiber woven body on the release paper after the preheating temperature of the heating platform reaches 50 ℃, and fixing the edge by adopting a clamp; after the fixation is finished, drying the quartz fiber braided body for 60min at the temperature of 50 ℃ to promote the volatilization of water in the fiber; weighing ablation-resistant medium-porcelain resin according to 1 time of the mass of the quartz fiber woven body, dividing the ablation-resistant medium-porcelain resin into two parts, pouring one part of the ablation-resistant medium-porcelain phenolic resin into the center of the quartz fiber woven body, driving the glue from the central area to the periphery, and uniformly rolling by using a tetrafluoro roller and then turning over; driving the other part of the ablation-resistant medium-ceramic resin to glue from the central area to the periphery again, and uniformly rolling by using a tetrafluoro roller; in the process of using a tetrafluoro roller to roll glue, the glue rolling direction must be parallel to the warp direction or the weft direction; after the ablation-resistant mesoceramic resin is uniformly rolled, keeping the temperature of the heating platform at 70 ℃, and drying for 120min to prepare mesoceramic resin prepreg;
s2, preparation of phenolic resin premix: putting the quartz fiber fixed-length yarn into an oven, and drying for 60min at 50 ℃; weighing ablation-resistant phenolic resin according to 1 time of the mass of the quartz fiber fixed-length yarn, and mixing the ablation-resistant phenolic resin and the quartz fiber fixed-length yarn in a basin; uniformly mixing ablation-resistant resin and quartz fiber fixed-length yarns to obtain a premix, grabbing the premix by using a close-tooth rake, putting the grabbed and loosened premix on a heating platform, keeping the temperature of the heating platform at 70 ℃, and keeping the temperature for 90min to obtain a phenolic resin premix;
s3, cutting the vitrified resin prepreg in the step S1 according to the surface layer development picture of the composite material member, and weighing the mass m after cutting; multiplying the volume of the mold cavity by the target density of 1.4g/cm 3 Calculating to obtain the total mass M; weighing the mass M-M of the phenolic resin premix in the step S2;
s4, filler: spraying a release agent for 1 time on the surface of the mold and the inside of the mold cavity, placing the mold in an oven, setting the temperature at 70 ℃, baking for 120min, keeping the temperature of the mold at 70 ℃, fixing the mold on a press, installing an upper mold at the upper end of the press, installing a lower mold at the lower end of the press, laying the cut medium-ceramic resin prepreg in the step S3 on the inner surface of the mold, tightly attaching the cut medium-ceramic resin prepreg to the surface of the mold by using vacuum bag pressing, keeping the edge angle of the prepared outer surface clear, keeping the vacuum degree of the vacuum bag pressing at not less than-0.085 MPa, and keeping the pressure for 10 min; filling the phenolic resin premix weighed in the step S3 into a cavity formed by the medium-ceramic resin prepreg for three times, wherein the first filling amount is 70% of the total amount, prepressing for 5min after filling, and prepressing under 5MPa, then opening, and using a dense tooth rake to rake loose the phenolic resin premix on the surface; then adding 15% of the total amount of the phenolic resin premix for filling, performing secondary prepressing, opening after 5min of prepressing, and continuously using a dense tooth rake to scrape the phenolic resin premix on the surface of the pine; then filling the rest of the phenolic resin premix, paving a layer of medium-ceramic resin prepreg on the surface of the phenolic resin premix, and then finishing final pressure, wherein the final pressure is 5min and 5 Mpa;
s5, mold closing: fastening the die after the final pressing by using bolts, and taking down the die from the press after the fastening is finished;
s6, curing: putting the mould into an oven, and heating and curing according to a curing system of the medium-ceramic resin;
s7, demolding: after the curing is finished, taking out the mold when the temperature of the oven is reduced to be within 60 ℃, and demolding when the temperature of the mold is reduced to be within 40 ℃;
s8, post-processing: and (5) polishing the burrs on the edge of the product by using sand paper.
Embodiment 2, a method for preparing an ablation-resistant local thermal protection material for a surface continuous woven body, comprising the following steps:
s1, preparing a medium porcelain resin prepreg: spreading release paper on a heating platform, spreading a quartz fiber woven body on the release paper after the preheating temperature of the heating platform reaches 60 ℃, and fixing the edge by adopting a clamp; after the fixation is finished, drying the quartz fiber braided body for 30min at the temperature of 60 ℃ to promote the volatilization of water in the fiber; weighing ablation-resistant medium-porcelain resin according to 1.5 times of the mass of the quartz fiber woven body, dividing the ablation-resistant medium-porcelain resin into two parts, pouring one part of the ablation-resistant medium-porcelain phenolic resin into the center of the quartz fiber woven body, driving the glue from the central area to the periphery, and uniformly rolling by using a tetrafluoro roller and then turning over; driving the other part of the ablation-resistant medium-ceramic resin to glue from the central area to the periphery again, and uniformly rolling by using a tetrafluoro roller; in the process of using a tetrafluoro roller to roll glue, the glue rolling direction must be parallel to the warp direction or the weft direction; after the ablation-resistant mesoceramic resin is uniformly rolled, keeping the temperature of the heating platform at 80 ℃, and drying for 30min to prepare mesoceramic resin prepreg;
s2, preparation of phenolic resin premix: putting the quartz fiber fixed-length yarn into an oven, and drying for 30min at the temperature of 60 ℃; weighing ablation-resistant phenolic resin according to the mass which is 1.5 times of the quartz fiber fixed-length yarn, and putting the ablation-resistant phenolic resin and the quartz fiber fixed-length yarn into a basin for mixing; uniformly mixing ablation-resistant resin and quartz fiber fixed-length yarns to obtain a premix, grabbing the premix by using a close-tooth rake, putting the grabbed and loosened premix to a heating platform, keeping the temperature of the heating platform at 80 ℃, and keeping the temperature for 30min to obtain a phenolic resin premix;
s3, cutting the vitrified resin prepreg in the step S1 according to the surface layer development picture of the composite material member, and weighing the mass m after cutting; multiplying the volume of the mold cavity by the target density of 1.6g/cm 3 Calculating to obtain the total mass M; weighing the mass M-M of the phenolic resin premix in the step S2;
s4, filler: spraying a release agent for 3 times on the surface of the mold and the inside of the mold cavity, placing the mold in an oven, setting the temperature to 90 ℃, baking for 60min, keeping the temperature of the mold at 90 ℃, fixing the mold on a press, installing an upper mold at the upper end of the press, installing a lower mold at the lower end of the press, laying the cut medium-ceramic resin prepreg in the step S3 on the inner surface of the mold, tightly attaching the cut medium-ceramic resin prepreg to the surface of the mold by using vacuum pressure, keeping the edge angle of the prepared outer surface clear, keeping the vacuum degree of the vacuum pressure at not less than-0.085 MPa, and keeping the pressure for 50 min; filling the phenolic resin premix weighed in the step S3 into a cavity formed by the medium-ceramic resin prepreg for three times, wherein the first filling amount is 80% of the total amount, prepressing for 10min after filling, and opening the cavity under the prepressing pressure of 1MPa, and using a dense-tooth rake to rake loose the phenolic resin premix on the surface; then adding 10% of the total amount of the phenolic resin premix for filling, performing secondary pre-pressing, opening the pre-pressing for 10min, and continuously using a dense-tooth rake to rake loose the phenolic resin premix on the surface; then filling the rest of the phenolic resin premix, paving a layer of medium-ceramic resin prepreg on the surface of the phenolic resin premix, and then finishing final pressure, wherein the final pressure is 10min and is 1 Mpa;
s5, mold closing: fastening the die after the final pressing by using bolts, and taking down the die from the press after the fastening is finished;
s6, curing: putting the mould into an oven, and heating and curing according to a curing system of the medium-ceramic resin;
s7, demolding: after the curing is finished, taking out the mold when the temperature of the oven is reduced to be within 60 ℃, and demolding when the temperature of the mold is reduced to be within 40 ℃;
s8, post-processing: and (5) polishing the burrs on the edge of the product by using sand paper.
Embodiment 3, a method for preparing an ablation-resistant local thermal protection material for a surface continuous woven body, comprising the following steps:
s1, preparing a medium porcelain resin prepreg: spreading release paper on a heating platform, spreading a quartz fiber woven body on the release paper after the preheating temperature of the heating platform reaches 55 ℃, and fixing the edge by adopting a clamp; drying the quartz fiber braided body at 55 ℃ for 45min after the fixation is finished, and promoting the water in the fiber to volatilize; weighing ablation-resistant medium-porcelain resin according to 1.3 times of the mass of the quartz fiber woven body, dividing the ablation-resistant medium-porcelain resin into two parts, pouring one part of the ablation-resistant medium-porcelain phenolic resin into the center of the quartz fiber woven body, driving the glue from the central area to the periphery, and uniformly rolling by using a tetrafluoro roller and then turning over; driving the other part of the residual ablation-resistant middle-ceramic resin to glue from the central area to the periphery again, and uniformly rolling by using a tetrafluoro roller; in the process of using a tetrafluoro roller to roll glue, the glue rolling direction must be parallel to the warp direction or the weft direction; after the ablation-resistant mesoceramic resin is uniformly rolled, keeping the temperature of a heating platform at 75 ℃, and drying for 65min to prepare mesoceramic resin prepreg;
s2, preparation of phenolic resin premix: putting the quartz fiber fixed-length yarn into an oven, and drying for 45min at the temperature of 55 ℃; weighing ablation-resistant phenolic resin according to 1.3 times of the mass of the quartz fiber fixed-length yarn, and mixing the ablation-resistant phenolic resin and the quartz fiber fixed-length yarn in a basin; uniformly mixing ablation-resistant resin and quartz fiber fixed-length yarns, scratching loose the premix by using a close-teeth rake, putting the scratched and loosened premix on a heating platform, keeping the temperature of the heating platform at 75 ℃, and preserving the heat for 65min to prepare a phenolic resin premix;
s3, cutting the vitrified resin prepreg in the step S1 according to the surface layer development picture of the composite material member, and weighing the mass m after cutting; multiplying the volume of the mold cavity by the target density of 1.5g/cm 3 Calculating to obtain a total mass M; weighing the mass M-M of the phenolic resin premix in the step S2;
s4, filler: spraying a release agent for 2 times on the surface of the mold and the inside of the mold cavity, placing the mold in an oven, setting the temperature at 80 ℃, baking for 90min, keeping the temperature of the mold at 80 ℃, fixing the mold on a press, installing an upper mold at the upper end of the press, installing a lower mold at the lower end of the press, laying the cut medium-ceramic resin prepreg in the step S3 on the inner surface of the mold, tightly attaching the cut medium-ceramic resin prepreg to the surface of the mold by using vacuum pressure, keeping the edge angle of the prepared outer surface clear, keeping the vacuum degree of the vacuum pressure at not less than-0.085 MPa, and keeping the pressure for 30 min; filling the phenolic resin premix weighed in the step S3 into a cavity formed by the medium-ceramic resin prepreg for three times, wherein the first filling amount is 75% of the total amount, prepressing for 7min after filling, and opening the cavity under the prepressing pressure of 3MPa, and using a dense tooth rake to rake loose the phenolic resin premix on the surface; then adding 13% of the total amount of the phenolic resin premix for filling, performing secondary pre-pressing, opening the pre-pressing for 7min, and continuously using a dense-tooth rake to rake loose the phenolic resin premix on the surface; then filling the rest of the phenolic resin premix, paving a layer of middle-porcelainized resin prepreg on the surface of the phenolic resin premix, and then finishing final pressure for 7min, wherein the final pressure is 3 Mpa;
s5, mold closing: fastening the die after the final pressing by using bolts, and taking down the die from the press after the fastening is finished;
s6, curing: putting the mould into an oven, and heating and curing according to a curing system of the medium-ceramic resin;
s7, demolding: after the curing is finished, taking out the mold when the temperature of the oven is reduced to be within 60 ℃, and demolding when the temperature of the mold is reduced to be within 40 ℃;
s8, post-processing: and (5) polishing the burrs on the edge of the product by using sand paper.
The composite materials prepared in the embodiments 1, 2 and 3 are tested, the ablation experiment condition is that the ablation condition of a medium-long-distance high-Mach aircraft is subjected to a test of a micro wind tunnel simulation real state, and the obtained result is shown in a table I;
watch 1
It can be seen that: the composite material prepared in the embodiment 1 has the advantages of low density, moderate tensile strength, moderate ablation performance and the like, but the composite material prepared by the composite material has the phenomenon of material shortage locally, and the filling of the phenolic resin premix is insufficient. The composite material prepared in example 2 has high density, but has the advantages of high tensile strength and ablation performance, clear surface edges and corners and good apparent quality. The composite material prepared in the embodiment 3 has the advantages of moderate density, high tensile strength, high ablation performance and the like, and the material has good apparent quality and qualified size.
Claims (2)
1. A preparation method of ablation-resistant local thermal protection material of a surface continuous braiding body is characterized by comprising the following steps: the surface layer is made into a medium porcelain resin prepreg by adopting a medium porcelain resin prepreg 2.5D woven body, and the prepreg is tightly attached to the die cavity by using vacuum bag pressing after the die is preheated; the inner layer is made into a phenolic resin premix by adopting ablation-resistant phenolic resin mixed chopped fibers, and a layer of medium-ceramic resin prepreg is laid on the surface of the premix to finish final pressing when the last filling is pre-pressed by three times of filling on a press; and (4) solidifying after fastening the bolts, and finally preparing the local thermal protection material structural member by demolding and post-processing.
2. The method for preparing the ablation-resistant local thermal protection material of the surface layer continuous woven body according to the claim 1, is characterized by comprising the following steps of:
s1, preparing a medium porcelain resin prepreg: spreading release paper on a heating platform, spreading a quartz fiber woven body on the release paper after the preheating temperature of the heating platform reaches 50-60 ℃, and fixing the edge by adopting a clamp; after the fixation is finished, drying the quartz fiber braided body for 30-60min at the temperature of 50-60 ℃; weighing ablation-resistant medium-porcelain resin according to 1-1.5 times of the mass of the quartz fiber woven body, dividing the ablation-resistant medium-porcelain resin into two parts, pouring one part of the ablation-resistant medium-porcelain phenolic resin into the center of the quartz fiber woven body, driving the glue from the central area to the periphery, and uniformly rolling and turning over by using a tetrafluoro roller; driving the other part of the ablation-resistant medium-ceramic resin to glue from the central area to the periphery again, and uniformly rolling by using a tetrafluoro roller; in the process of using a tetrafluoro roller to roll glue, the glue rolling direction must be parallel to the warp direction or the weft direction; after the ablation-resistant mesoceramic resin is uniformly rolled, keeping the temperature of a heating platform at 70-80 ℃, and drying for 30-120min to prepare mesoceramic resin prepreg;
s2, preparation of phenolic resin premix: putting the quartz fiber fixed-length yarn into an oven, and drying for 30-60min at 50-60 ℃; weighing ablation-resistant phenolic resin according to 1-1.5 times of the mass of the quartz fiber fixed-length yarn, and mixing the ablation-resistant phenolic resin and the quartz fiber fixed-length yarn in a basin; uniformly mixing ablation-resistant resin and quartz fiber fixed-length yarns, scratching loose the premix by using a close-teeth rake, putting the scratched and loosened premix on a heating platform, keeping the temperature of the heating platform at 70-80 ℃, and preserving heat for 30-90min to prepare a phenolic resin premix;
s3, cutting the vitrified resin prepreg in the step S1 according to the surface development picture of the composite material member, and weighing the mass m after cutting; multiplying the volume of the die cavity by the target density to be 1.4-1.6g/cm 3 Calculating to obtain a total mass M; weighing the mass M-M of the phenolic resin premix in the step S2;
s4, filler: spraying a release agent for 1-3 times on the surface of the mold and the inside of the mold cavity, placing the mold in an oven, baking at the temperature of 70-90 ℃ for 60-120min, maintaining the temperature of the mold at 70-90 ℃, fixing the mold on a press, installing an upper mold at the upper end of the press, installing a lower mold at the lower end of the press, laying the cut mesoceramic resin prepreg in the step S3 on the inner molded surface of the mold, tightly attaching the cut mesoceramic resin prepreg to the surface of the mold by using vacuum bag pressure, keeping the vacuum degree of the vacuum bag pressure to be not less than-0.085 MPa, and keeping the pressure for 10-50 min; filling the phenolic resin premix weighed in the step S3 into a cavity formed by the medium-ceramic resin prepreg for three times, wherein the first filling amount is 70-80% of the total amount, pre-pressing for 5-10min after filling, the pre-pressing pressure is 1-5MPa, then opening, and using a dense tooth rake to loosen the phenolic resin premix on the surface; then adding 10-15% of the total amount of the phenolic resin premix for secondary prepressing, opening the prepressing for 5-10min, and continuously using a dense tooth rake to loosen the phenolic resin premix on the surface; then filling the rest of the phenolic resin premix, paving a layer of medium-ceramic resin prepreg on the surface of the phenolic resin premix, and then finishing final pressure, wherein the final pressure is 5-10min and is 1-5 Mpa;
s5, mold closing: fastening the die after the final pressing by using bolts, and taking down the die from the press after the fastening is finished;
s6, curing: putting the mould into an oven, and heating and curing according to a curing system of the medium-ceramic resin;
s7, demolding: after the curing is finished, taking out the mold when the temperature of the oven is reduced to be within 60 ℃, and demolding when the temperature of the mold is reduced to be within 40 ℃;
s8, post-processing: and (5) polishing the burrs on the edge of the product by using sand paper.
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