CN115958816A - Light and low-ablation nozzle expansion section and preparation method thereof - Google Patents
Light and low-ablation nozzle expansion section and preparation method thereof Download PDFInfo
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- CN115958816A CN115958816A CN202211682342.7A CN202211682342A CN115958816A CN 115958816 A CN115958816 A CN 115958816A CN 202211682342 A CN202211682342 A CN 202211682342A CN 115958816 A CN115958816 A CN 115958816A
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Abstract
The invention provides a preparation method of a light and low ablation spray pipe expansion section, which comprises the steps of mixing high carbon residue phenolic resin, polyacrylonitrile-based chopped carbon fiber and a solvent in proportion to form a premix, after the premix is subjected to solvent removal treatment, filling the premix into an expansion section prefabricated part curing tool, heating and pressurizing the premix by a press to cure the premix into a prefabricated part blank, and adding the prefabricated part blank by a prefabricated part machine to obtain a prefabricated part; weaving the composite expansion section preform outside the preform and at the large end part of the expansion section by adopting a carbon cloth/net tire + needling forming process, impregnating phenolic resin after the preform is manufactured, heating and pressurizing the preform in an expansion section integral die pressing tool by a press to solidify the preform into a composite expansion section product, and locally machining the expansion section blank in the subsequent spray pipe production to be assembled with a spray pipe shell in place. The invention solves the problems of lower material strength, large ablation amount in a high-temperature and high-pressure working environment, heavier weight of the spray pipe and the like of the winding expansion section, and meets the requirement of the solid rocket engine on the performance of the spray pipe with high impact mass ratio.
Description
Technical Field
The invention relates to the field of solid rocket engine nozzles, in particular to a lightweight low-ablation nozzle expansion section and a preparation method thereof.
Background
At present, most of the materials for the expansion section of the solid rocket engine nozzle produced in a sizing batch in China are carbon cloth/high silica cloth reinforced phenolic resin composite winding products. The carbon cloth/high silica cloth reinforced phenolic resin composite winding expansion section has large ablation amount in a high-temperature high-pressure strong working environment, and the ablation resistance in a long-time scouring process is ensured by increasing the design thickness of materials, so that the negative mass of the expansion section is large, and the requirement of the weight reduction index of the spray pipe is not met. Therefore, the expanding section with light weight and long-term low ablation performance becomes the necessary choice of the advanced high-performance spray pipe.
The technical scheme of the existing light and low ablation expansion section mainly comprises the following steps: in patent CN111997781a, a composite material expansion section forming method based on RTM process semi-curing surface is adopted to prepare a double-layer composite material nozzle expansion section, wherein the inner layer is a 2.5D carbon fiber fabric reinforced resin matrix composite material ablation layer, and the outer layer is a high silica fiber cloth tape winding formed thermal insulation layer. In the preparation method of the expansion section, the ablation layer prepared by the 2.5D carbon fiber preform has different ablation resistance stripping capabilities due to different combustion surfaces of warps and wefts exposed in fuel gas in the working process of a high-pressure engine, ablation appearance similar to a wave shape is easy to cause, ablation uniformity is poor, the method relates to a plurality of molding technologies such as RTM tool design, a cloth tape winding technology, autoclave compression curing and the like, different tool matching is required in the molding process, the process is complex, and the product quality influence factors are more; in the patent CN106116623A, aiming at the defects of large weight, high cost and the like of the existing diffusion section, a carbon fiber fabric is impregnated by using a vapor deposition method and then cracked to obtain a C/C blank. And soaking the blank in a xylene solution of polycarbosilane, and finally carrying out a series of operations of physical pressure curing, pyrolysis and machining to obtain the expansion section with the required size. The preparation process needs special equipment such as vapor deposition equipment and a high-temperature cracking furnace, the required product density can be achieved only by repeating the dipping-curing-cracking process for 5-7 times, the whole process is complex, the equipment requirement is high, and the process cost is high; the patent CN209011969U is based on a carbon cloth-high silica cloth/phenolic aldehyde winding expansion section, a carbon/silicon carbide composite winding material with smaller thickness and relatively lighter weight is introduced at the rear section of the expansion section to reduce the overall weight, and the carbon/silicon carbide composite winding material is still the winding expansion section.
Most of the existing expansion section materials are prepared by a carbon cloth/high silica cloth reinforced phenolic resin composite winding technology, and the existing expansion section materials mainly have the following two defects in the practical engine application: firstly, the step effect (butt joint with the throat insert) of the small end of the expansion section is obvious, the ablation rate is high, the specific impact efficiency of the expansion section is reduced, and even the structural damage of the expansion section can be caused; on the other hand, the outlet cone of the expansion section is of a thin-wall structure, the composite material in the traditional winding process has the problem of low interlayer performance, the phenomenon of structural delamination is easy to occur after high-temperature carbonization, and in order to reduce the influence of a carbonization area, a design idea of increasing the wall thickness needs to be adopted, but the negative quality of the expansion section is greatly increased due to the condition.
Disclosure of Invention
One of the purposes of the invention is to provide a light-weight and low-ablation nozzle expansion section, which solves the problems that the existing winding expansion section has lower material strength, large ablation amount in a high-temperature and high-pressure working environment, needs thicker winding thickness to meet the ablation resistance requirement, causes heavier nozzle weight and the like, and meets the requirement of an advanced solid rocket engine on the performance of a nozzle with high impact mass ratio.
In order to solve the technical problem, the invention provides a preparation method of a light-weight low-ablation nozzle expansion section, which comprises the following steps:
s1: preparing the small end of the expansion section: mixing high-carbon-residue phenolic resin, polyacrylonitrile-based chopped carbon fiber and a solvent in proportion to form a premix, carrying out desolvation treatment on the premix, then filling the premix into an expansion section prefabricated part curing tool, heating and pressurizing the premix by a press to cure the premix into a prefabricated part blank, and adding the prefabricated part blank by a prefabricated part machine to obtain a prefabricated part;
s2: preparing the large end of the expansion section: weaving the prefabricated member of the composite expansion section at the outer side of the prefabricated member and the large end part of the expansion section by adopting a carbon cloth/net tire and needling forming process, impregnating phenolic resin after the prefabricated member is manufactured, heating and pressurizing the prefabricated member in an integral die pressing tool of the expansion section by a press to solidify the prefabricated member into a composite expansion section product, and locally machining the expansion section blank and assembling the expansion section blank and a spray pipe shell in place in the subsequent spray pipe production.
Further, the solvent in the S1 is industrial alcohol, wherein the mass ratio of the high-carbon-residue phenolic resin to the polyacrylonitrile-based chopped carbon fiber to the solvent is 1:1.4-1.6:2.8-3.2.
Further, desolventizing the premix in the S1 at 70-80 ℃, and keeping the content of the volatile component x in the premix to be more than or equal to 3.0% and less than or equal to 5.5%.
Further, the heating and curing step of the press in the S1 comprises the following steps: heating from room temperature to 80-90 deg.C within 50-60min, and maintaining for 120-130min; then heating to 100-110 ℃ within 50-60min, and keeping the temperature for 90-100min; finally, heating to 170-180 ℃ within 140-150min, and keeping the temperature for 150-160min; the press pressurization and solidification steps are as follows: pressing at 80-90 deg.C under 1.0-1.5MPa, and closing the mold; pressurizing at 100-110 deg.c to 3.0-3.5MPa; maintaining at 100-110 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 6.0-6.5MPa; keeping the temperature at 100-110 ℃ for 90-100min, deflating for 1-2min, pressurizing for 10.0-10.5MPa, maintaining the pressure until the procedure is finished, naturally cooling the curing tool to room temperature after the curing is finished, and demoulding to take out the small-end prefabricated part blank.
Further, the carbon cloth in the S2 is T800 polyacrylonitrile-based carbon fiber twill cloth, the net tire is T700 polyacrylonitrile-based carbon fiber, the carbon cloth and the carbon fiber net tire are alternately laminated, the layering direction is parallel to the bus direction of the expansion section, and the composite expansion section integral preform with the conical structure is formed by fixedly molding through a needling process.
Further, after the composite expansion segment preform in S2 is molded by compression, the preform is subjected to dehumidification treatment at the temperature of 105-110 ℃/2 h.
Further, the heating and curing step of the press in the S2 comprises the following steps: heating from room temperature to 100-110 deg.C within 80-90min, and maintaining for 240-250min; then heating to 120-130 ℃ within 30-40min, and keeping the temperature for 120-130min; finally heating to 170-180 deg.C within 170-180min, and maintaining for 150-160min; the press pressurization and solidification steps are as follows: heating to 100-110 deg.C, pressurizing to 0.3-0.4MPa, and die assembling; pressurizing to 1.0-1.2MPa after the heat preservation at 100-110 ℃; heating to 120-130 deg.C, discharging gas for 1-2min, and pressurizing at 2.0-2.2MPa; maintaining at 120-130 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 3.0-3.2MPa; keeping the temperature at 120-130 deg.C for 120-130min, deflating for 1-2min, pressurizing at 4.0-4.2MPa, maintaining the pressure until the procedure is finished, curing, naturally cooling the expansion section integral mould pressing tool to room temperature, demoulding and taking out the expansion section product.
Based on the same concept, the invention also provides a light-weight and low-ablation nozzle expansion section.
One or more technical schemes of the invention have the following technical effects:
the embodiment of the invention provides a light-weight low-ablation nozzle expansion section and a preparation method thereof. With traditional carbon cloth/high silica cloth reinforcing phenolic resin complex winding expansion section, and the winding expansion section of modified carbon/carborundum combined material is compared on winding expansion section basis, combined type spray tube expansion section, through subregion functional design, make it have better anti ablation performance in the main ablation district of tip, other non-ablation districts possess good overall structure stability and low density advantage, the whole prefabricated body of expansion section adopts carbon cloth + acupuncture shaping, the interlaminar shear strength has been improved greatly, avoid appearing winding expansion section thin wall structural design and take place the risk of structural stratification easily after high temperature carbonization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
FIG. 1 is a flow diagram of a process for preparing a lightweight, low-ablation nozzle expansion segment;
FIG. 2 is a view of a tooling for curing a small-end prefabricated part of an expansion section;
FIG. 3 is a schematic structural view of a small-end preform of an expansion section;
FIG. 4 is a drawing of an integral preform of the composite expansion segment;
FIG. 5 is a drawing of the composite expansion segment integral molding tooling;
FIG. 6 is a composite expansion segment article view (blank);
the device comprises a male die 1, a collar 2, screws 3, a female die 4, a cushion block 5, a top cover 6, a female die 7, a male die 8, screws 9 and a chassis 10.
Detailed Description
Example 1
As shown in fig. 1, a method for preparing a lightweight, low-ablation nozzle flare includes:
s1: preparing the small end of the expansion section: mixing high carbon residue phenolic resin, polyacrylonitrile-based chopped carbon fiber and a solvent in proportion to form a premix, carrying out desolventizing treatment on the premix, filling the premix into an expansion section prefabricated part curing tool, heating and pressurizing the premix by a press to cure the premix into a prefabricated part blank, and machining the prefabricated part blank to obtain a prefabricated part;
specifically, the solvent is industrial alcohol, wherein the mass ratio of the high-carbon-residue phenolic resin to the polyacrylonitrile-based chopped carbon fiber to the solvent is 1:1.4-1.6:2.8 to 3.2, wherein the mixing sequence is that the high carbon residue phenolic resin and the industrial alcohol are mixed evenly by adopting a mechanical stirring mode according to the proportion, then the polyacrylonitrile-based short carbon fiber is put in,repeatedly kneading and extruding to fully and uniformly mix the resin solution and the carbon fibers to form a premix, desolventizing the premix at 70-80 ℃, putting the premix into an oven for desolventizing, or desolventizing in other modes, keeping the content of the volatile x in the premix between 3.0% and 5.5%, and testing the volatile content of the premix by the method: weighing a certain amount (20-40 g) of premix, putting the premix into a (103-107) DEG C oven after weighing m1, preserving the heat for 29-31 min, taking out the premix, airing the premix to room temperature, weighing m2 again, and calculating the volatile component x as follows:
after the premix is qualified by solvent removal treatment, a proper amount of premix is weighed and is filled into the expansion section small-end prefabricated part curing tool shown in figure 1, and the mold filling of the expansion section small-end prefabricated part is completed. The expansion section small-end prefabricated part curing tool comprises a cushion block, a female die, a male die and a lantern ring. The female die is connected with the lantern ring through screws, and other tools are connected in a matched mode. Before the premix is filled into a mold, the female mold is connected with the cushion block in a matching way, the female mold is connected with the sleeve ring through the screw, a cavity is formed among the cushion block, the female mold and the sleeve ring, the weighed premix is uniformly laid into the cavity, and finally the male mold is covered, so that the mold filling of the small-end prefabricated member of the expansion section is completed; placing the curing tool for the small-end prefabricated part of the expansion section after die filling on a press for curing, wherein the heating and curing steps of the press are as follows: heating from room temperature to 80-90 deg.C within 50-60min, and maintaining for 120-130min; then heating to 100-110 ℃ within 50-60min, and keeping the temperature for 90-100min; finally, heating to 170-180 ℃ within 140-150min, and keeping the temperature for 150-160min; the press pressurization and solidification steps are as follows: pressing at 80-90 deg.c under 1.0-1.5MPa to match the mold; pressurizing at 100-110 deg.c to 3.0-3.5MPa; maintaining at 100-110 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 6.0-6.5MPa; keeping the temperature at 100-110 ℃ for 90-100min, deflating for 1-2min, pressurizing for 10.0-10.5MPa, maintaining the pressure until the procedure is finished, naturally cooling the curing tool to room temperature after curing is finished, demolding and taking out the small-end prefabricated part blank; the preform blank machine was used to obtain the preform product shown in fig. 3.
S2: preparing the large end of the expansion section: weaving a composite expansion section prefabricated body on the outer side of the prefabricated part and the large end part of the expansion section by adopting a carbon cloth/net tire + needling forming process, impregnating phenolic resin after the prefabricated part is manufactured, heating, pressurizing and curing the prefabricated part into a composite expansion section product in an expansion section integral die pressing tool through a press, and locally machining and assembling the expansion section blank and a spray pipe shell in place in the subsequent spray pipe production;
specifically, the carbon cloth is T800 polyacrylonitrile-based carbon fiber twill cloth, the net tire is T700 polyacrylonitrile-based carbon fiber, the carbon cloth and the carbon fiber net tire are alternately laminated, the layering direction is parallel to the bus direction of the expansion section, and the composite expansion section integral preform with a conical structure is fixedly formed by a needling process; after the composite expansion section preform is molded, dehumidifying the preform at the temperature of 105-110 ℃/2 h; after dehumidification, the prefabricated part is covered by a vacuum bag to form a closed space, a vacuumizing port is reserved at the small end, and a plurality of glue inlets are reserved at the large end. The vacuum degree of the vacuum bag is checked before impregnation, and the vacuum degree can be continuously maintained at less than or equal to-0.07 MPa. Weighing a certain amount of phenolic resin, placing the phenolic resin in a clean container, connecting the phenolic resin in the container with a preform glue inlet through a PE glue injection pipe, opening a preform glue inlet valve when the vacuum degree meets the requirement, slowly sucking the phenolic resin into the preform under vacuum suction until the preform is completely soaked by the phenolic resin, and finishing the resin impregnation process of the preform. And (3) placing the prefabricated body impregnated with the resin into a composite expansion section integral mould pressing tool, and heating, pressurizing and curing. The integral die pressing tool is composed of a female die, a male die, a base plate, a top cover and screws as shown in figure 5. Firstly, connecting a male die and a chassis through screws, then installing the impregnated prefabricated body on the male die, and then sequentially closing a female die and a top cover to complete die installation; placing the die-filled tool on a press for curing; the heating and curing steps of the press are as follows: heating from room temperature to 100-110 deg.C within 80-90min, and maintaining for 240-250min; then heating to 120-130 ℃ within 30-40min, and keeping the temperature for 120-130min; finally heating to 170-180 deg.C within 170-180min, and maintaining for 150-160min; the press pressurization and solidification steps are as follows: heating to 100-110 deg.C, pressurizing to 0.3-0.4MPa, and die assembling; pressurizing to 1.0-1.2MPa after the heat preservation at 100-110 ℃; heating to 120-130 deg.C, discharging gas for 1-2min, and pressurizing at 2.0-2.2MPa; maintaining at 120-130 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 3.0-3.2MPa; maintaining at 120-130 deg.C for 120-130min, degassing for 1-2min, pressurizing at 4.0-4.2MPa, maintaining pressure until the procedure is finished, curing, naturally cooling the expansion section integral molding tool to room temperature, demolding, and taking out the expansion section product, as shown in FIG. 6.
The oxyacetylene ablation rate (execution standard GJB 323B) of the polyacrylonitrile-based carbon fiber/high carbon residue phenolic resin material is 0.02-0.03mm/s, which is reduced by 50% compared with the ablation rate (0.05-0.06) of the traditional winding expansion section material, besides, compared with the winding expansion section, the carbon fiber/phenolic resin material has simpler preparation process and greatly improved quality controllability.
Claims (8)
1. A method for preparing a light-weight low-ablation nozzle expansion section is characterized by comprising the following steps:
s1: preparing the small end of the expansion section: mixing high-carbon-residue phenolic resin, polyacrylonitrile-based chopped carbon fiber and a solvent in proportion to form a premix, carrying out desolvation treatment on the premix, then filling the premix into an expansion section prefabricated part curing tool, heating and pressurizing the premix by a press to cure the premix into a prefabricated part blank, and adding the prefabricated part blank by a prefabricated part machine to obtain a prefabricated part;
s2: preparing the large end of the expansion section: weaving the prefabricated member of the composite expansion section at the outer side of the prefabricated member and the large end part of the expansion section by adopting a carbon cloth/net tire and needling forming process, impregnating phenolic resin after the prefabricated member is manufactured, heating and pressurizing the prefabricated member in an integral die pressing tool of the expansion section by a press to solidify the prefabricated member into a composite expansion section product, and locally machining the expansion section blank and assembling the expansion section blank and a spray pipe shell in place in the subsequent spray pipe production.
2. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: the solvent in the S1 is industrial alcohol, wherein the mass ratio of the high-carbon-residue phenolic resin to the polyacrylonitrile-based chopped carbon fiber to the solvent is 1:1.4-1.6:2.8-3.2.
3. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: the solvent of the premix in S1 is removed at 70-80 ℃, and the content of volatile x in the premix is maintained to be 3.0-5.5%.
4. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: the heating and curing step of the press in the S1 comprises the following steps: heating from room temperature to 80-90 deg.C within 50-60min, and maintaining for 120-130min; then heating to 100-110 ℃ within 50-60min, and keeping the temperature for 90-100min; finally, heating to 170-180 ℃ within 140-150min, and keeping the temperature for 150-160min; the press pressurization and solidification steps are as follows: pressing at 80-90 deg.c under 1.0-1.5MPa to match the mold; pressurizing at 100-110 deg.c to 3.0-3.5MPa; maintaining at 100-110 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 6.0-6.5MPa; keeping the temperature at 100-110 ℃ for 90-100min, deflating for 1-2min, pressurizing for 10.0-10.5MPa, maintaining the pressure until the procedure is finished, naturally cooling the curing tool to room temperature after the curing is finished, and demoulding to take out the small-end prefabricated part blank.
5. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: and in S2, the carbon cloth is T800 polyacrylonitrile-based carbon fiber twill cloth, the net tire is T700 polyacrylonitrile-based carbon fiber, the carbon cloth and the carbon fiber net tire are alternately laminated, the layering direction is parallel to the bus direction of the expansion section, and the composite expansion section integral preform with a conical structure is fixedly formed by a needling process.
6. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: and (3) after the composite expansion section prefabricated body in the S2 is subjected to compression molding, dehumidifying the prefabricated body at the temperature of 105-110 ℃/2 h.
7. The method of making a lightweight, low ablation nozzle flare according to claim 1, further comprising: the heating and curing step of the press in the S2 comprises the following steps: heating from room temperature to 100-110 deg.C within 80-90min, and maintaining for 240-250min; then heating to 120-130 ℃ within 30-40min, and keeping the temperature for 120-130min; finally heating to 170-180 deg.C within 170-180min, and maintaining for 150-160min; the press pressurization and solidification steps are as follows: heating to 100-110 deg.C, pressurizing to 0.3-0.4MPa, and die assembling; pressurizing to 1.0-1.2MPa after the heat preservation at 100-110 ℃; heating to 120-130 deg.C, discharging gas for 1-2min, and pressurizing at 2.0-2.2MPa; maintaining at 120-130 deg.C for 60-70min, discharging gas for 1-2min, and pressurizing at 3.0-3.2MPa; keeping the temperature at 120-130 deg.C for 120-130min, deflating for 1-2min, pressurizing at 4.0-4.2MPa, maintaining the pressure until the procedure is finished, curing, naturally cooling the expansion section integral mould pressing tool to room temperature, demoulding and taking out the expansion section product.
8. A light, low ablation nozzle expansion segment, characterized by: the lightweight, low ablation dilation segment is prepared by any one of the methods of claims 1 to 7.
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