CN112358298A - Rapid preparation method of C/SiC composite material engine nozzle - Google Patents
Rapid preparation method of C/SiC composite material engine nozzle Download PDFInfo
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- CN112358298A CN112358298A CN202011150119.9A CN202011150119A CN112358298A CN 112358298 A CN112358298 A CN 112358298A CN 202011150119 A CN202011150119 A CN 202011150119A CN 112358298 A CN112358298 A CN 112358298A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02K—JET-PROPULSION PLANTS
- F02K1/00—Plants characterised by the form or arrangement of the jet pipe or nozzle; Jet pipes or nozzles peculiar thereto
- F02K1/78—Other construction of jet pipes
- F02K1/82—Jet pipe walls, e.g. liners
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B21/00—Methods or machines specially adapted for the production of tubular articles
- B28B21/42—Methods or machines specially adapted for the production of tubular articles by shaping on or against mandrels or like moulding surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B21/00—Methods or machines specially adapted for the production of tubular articles
- B28B21/42—Methods or machines specially adapted for the production of tubular articles by shaping on or against mandrels or like moulding surfaces
- B28B21/48—Methods or machines specially adapted for the production of tubular articles by shaping on or against mandrels or like moulding surfaces by wrapping, e.g. winding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B21/00—Methods or machines specially adapted for the production of tubular articles
- B28B21/92—Methods or apparatus for treating or reshaping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B21/00—Methods or machines specially adapted for the production of tubular articles
- B28B21/92—Methods or apparatus for treating or reshaping
- B28B21/94—Methods or apparatus for treating or reshaping for impregnating or coating by applying liquids or semi-liquids
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- D06M2101/40—Fibres of carbon
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Abstract
The invention provides a rapid preparation method of a C/SiC composite engine nozzle, belonging to the technical field of ceramic matrix composites and comprising the following steps: preparing a carbon fiber cloth pyrolytic carbon interface layer, preparing an engine spray pipe preform, densifying a matrix and densifying a spray pipe blank. According to the invention, the spray pipe preform is prepared by adopting a layer stitching process, a high-temperature compression molding cracking process and a precursor dipping cracking process are adopted, and profile modeling graphite core mold tooling dimension assist is combined, so that the rapid densification of the matrix is realized, the preparation period is effectively shortened, meanwhile, the allowance processing is positioned in the densification process, the blank closed hole rate can be reduced, the blank densification degree is favorably improved, and the processed bare fibers are wrapped to a certain degree in the subsequent densification process, so that the product quality is improved. The spray pipe prepared by the preparation method disclosed by the invention is stable in forming quality, controllable in fiber density, low in equipment and control technical requirements in the preparation process, low in cost and beneficial to popularization and large-scale production.
Description
Technical Field
The invention relates to a preparation method of an engine spray pipe, in particular to a rapid preparation method of a thin-wall C/SiC composite engine spray pipe, and belongs to the technical field of ceramic matrix composites.
Background
The jet pipe (including convergent section, throat insert and diffusion section) is an energy conversion device in the engine, and it converts the heat energy of combustion products in the shell into kinetic energy of high-speed jet flow, and after convergence and diffusion, it is sprayed out as high-temperature gas. The jet pipe is required to bear heat and force applied by complex high-temperature gas flow, mechanical load of vibration and swing of the jet pipe and the like in work, the service environment is very severe, and the jet pipe is a complex part with most faults in engine development. The severe service environment requires that the material for the spray pipe has high ablation resistance, high pressure resistance, scouring resistance and thermal shock resistance. In addition, the structure should have the characteristics of light weight, high reliability, good processing performance, low cost and the like.
The engine nozzle material scheme mainly comprises a high-temperature alloy material, a titanium alloy material, a C/C composite material, a C/SiC composite material and the like. Although the high-temperature alloy material has high melting point, the density is high, and the weight reduction purpose is not facilitated. The titanium alloy material has reduced strength in a high-temperature environment and is easily oxidized. The C/C and C/SiC composite materials have the characteristics of high specific strength, high specific modulus, excellent thermal shock resistance and the like. However, the C/C composite material is not oxidation-resistant and has overlarge ablation amount, and the C/SiC composite material has a series of excellent performances of low density, high strength, high temperature resistance, ablation resistance, scouring resistance and the like and simultaneously has better oxidation resistance than the C/C composite material.
At present, the preparation of C/SiC composite material engine nozzle prefabricated bodies mainly comprises winding forming and three-dimensional weaving forming processes. The three-dimensional weaving method is low in automation degree and low in production efficiency; in the three-dimensional weaving method, the fiber winding is discontinuous, the winding tension is not uniform, and the forming quality is not stable; the fiber is bent, and the thin-wall spray pipe is not beneficial to maintaining the strength and the sealing property of the component for a long time; the carbon fiber content of the preform is not easy to control, and the fiber density cannot be controlled through tension adjustment. The winding forming method has small adaptability, can not wind products with any structural form, and for products with concave surfaces, fibers can not cling to the surface of a core mould to be overhead during winding. In addition, the molding process has high requirements on equipment and control technology and higher cost.
The SiC ceramic matrix composite densification process mainly comprises Reaction Melt Infiltration (RMI), Chemical Vapor Infiltration (CVI), nano-impregnation and instantaneous eutectic phase (NITE), slurry impregnation Hot Pressing (HP) and precursor impregnation cracking (PIP). Among them, the NITE, RMI and HP processes require a high temperature environment, and damage may be caused to the fibers during the preparation process, affecting the overall performance. The CVI process can prepare the silicon carbide substrate under the conditions of low temperature and low pressure, has small damage to fibers and meets the requirement of near net size molding of a component with a complex shape, but the process has long preparation period and high preparation cost, and is not easy to prepare a composite material with thicker thickness. The traditional PIP process has low requirement on equipment, is simple, is suitable for near-net-shape preparation of large-scale components with complex shapes, can realize the preparation of ceramic matrixes with specific components by designing and regulating the molecular structure of an organic precursor, but has the disadvantages of long preparation period, low purity of the matrixes and reduction of the densification efficiency due to low yield of ceramic precursors.
Disclosure of Invention
In order to solve at least one problem of low production efficiency, unstable forming quality, uncontrollable fiber density, high requirements on equipment and control technology and high cost in the existing spray pipe preparation, the inventor of the invention carries out intensive research and provides a rapid preparation method of a C/SiC composite material engine spray pipe. The spray pipe prepared by the preparation method has stable forming quality, controllable fiber density, low requirements on equipment and control technology in the preparation process and low cost, thereby completing the invention.
The technical scheme provided by the invention is as follows:
a method for quickly preparing a C/SiC composite engine nozzle comprises the following steps:
step (1), adopting a chemical vapor deposition process, taking hydrocarbon gas as a carbon source gas, taking inert gas or nitrogen as diluent gas, arranging carbon fibers in a carbon deposition furnace for deposition, preparing carbon fiber cloth containing a pyrolytic carbon interface layer, and then carrying out graphitization treatment on the carbon fiber cloth containing the pyrolytic carbon interface layer;
step (2), uniformly coating silicon carbide precursor slurry on the surface of the carbon fiber cloth obtained in the step (1), combining a profiling graphite core mold tool, adopting a layer sewing process to enable the carbon fiber cloth to be tightly attached to the surface of the profiling graphite core mold tool and to be formed in a surrounding mode, and preparing a spray pipe prefabricated body;
step (3), densifying the spray pipe preform prepared in the step (2) by adopting a high-temperature compression molding and cracking process to prepare a C/SiC composite spray pipe blank;
and (4) machining the spray pipe blank in the step (3) by adopting a machining method, removing machining allowance, and then continuously densifying the machined spray pipe blank by adopting a precursor impregnation cracking process to obtain the C/SiC composite material engine spray pipe.
The rapid preparation method of the C/SiC composite material engine nozzle provided by the invention has the following beneficial effects:
(1) according to the invention, the carbon fiber cloth laying sewing process is adopted to prepare the spray pipe preform, and the obtained spray pipe preform structure is mainly characterized by high fiber volume fraction, high density, low void ratio and good in-plane performance; meanwhile, the carbon fiber cloth is not bent in the plane direction and keeps a vertical parallel state, so that the mechanical property in the axial direction of the fiber is fully exerted;
(2) in the invention, a high-temperature compression molding cracking process and a precursor impregnation cracking process (PIP) are adopted, and a copying graphite core mold tool is used for assisting in shape maintenance, so that the rapid densification of a matrix is realized, and the preparation period is effectively shortened; meanwhile, the high-temperature compression molding cracking process can effectively improve the volume content of the blank fibers and play a role in maintaining the shape;
(3) according to the invention, the spray pipe blank is processed when reaching a certain density, and then densification is continued until reaching the density design requirement, the closed hole rate of the blank can be reduced by processing in the process, and the densification degree of the blank is improved; meanwhile, the processed bare fibers are wrapped to a certain degree in the subsequent densification process, so that the product quality is improved;
(4) in the high-temperature compression molding cracking process, a layer of graphite paper is filled between the graphite core mold tool and the prefabricated body, so that the graphite core mold tool is conveniently reloaded, the graphite core mold tool is fully and closely attached to the prefabricated body in the molding process, and pressure is uniformly applied; and the damage of the graphite core mold tool to the fibers in the processes of loading and subsequent pressing is reduced.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The invention provides a rapid preparation method of a C/SiC composite material engine nozzle, which comprises the following steps:
step 1, preparing a carbon fiber cloth pyrolytic carbon interface layer: the method comprises the steps of adopting a chemical vapor deposition process, taking hydrocarbon gas as a carbon source gas, taking inert gas or nitrogen as diluent gas, arranging carbon fibers in a carbon deposition furnace for deposition, preparing carbon fiber cloth containing a pyrolytic carbon interface layer, and then carrying out graphitization treatment on the carbon fiber cloth containing the pyrolytic carbon interface layer.
In step 1, the hydrocarbon gas may be methane, propane, acetylene, or the like.
In the step 1, in the chemical vapor deposition process, the deposition pressure is 1-15 KPa, the deposition temperature is 800-1200 ℃, and the deposition time is 40-60 hours. Preferably, the deposition pressure is 1-5 KPa, the deposition temperature is 900-1200 ℃, and the deposition time is 40-60 hours.
In the step 1, in the graphitization treatment, the graphitization treatment temperature is 1900-2200 ℃, and the graphitization treatment time is 2-4 hours. In the graphitization temperature and time range, the carbon fiber cloth is graphitized, so that the ductility of the carbon fiber cloth can be enhanced, and the subsequent profiling laying layer is convenient. If the graphitization treatment temperature or the treatment time is lower than the required range, the disordered carbon content in the interface layer is higher, the interlayer slip probability is lower, and the fiber toughening is not facilitated; if the graphitization treatment temperature or the graphitization treatment time is higher than the above-described required range, the structure of the carbon fiber itself is changed, and the fiber reinforcement effect is weakened.
In the step 1, the thickness of the pyrolytic carbon interface layer deposited on the carbon fiber cloth containing the pyrolytic carbon interface layer is 0.2-1.0 μm.
Step 2, preparing an engine spray pipe preform: uniformly coating silicon carbide precursor slurry on the surface of the carbon fiber cloth containing the pyrolytic carbon interface layer obtained in the step 1), combining a profiling graphite core mold tool, adopting a layer-spreading sewing process to enable the carbon fiber cloth to be tightly attached to the surface of the profiling graphite core mold tool and to be formed in a surrounding mode, and preparing the spray pipe preform.
In the step 2, the concrete steps of preparing the spray pipe preform by adopting the layer-laying sewing process are as follows:
(i) adopting a split type profiling graphite core mold tool, and coating a release agent on the surface of the split type profiling graphite core mold tool; clinging the carbon fiber cloth coated with the silicon carbide precursor slurry and containing the pyrolytic carbon interface layer to the surface of the graphite core mold tool, forming in a surrounding mode, butting the edge seams of the layers, and finishing the first layer of layers of the spray pipe preform;
(ii) laying other layers sequentially by the same first layer laying method, wherein the edge seams of each layer of carbon fiber cloth are staggered sequentially in the laying process, the distance between the edge seams of the front layer of carbon fiber cloth and the edge seams of the rear layer of carbon fiber cloth is larger than 10mm, and the layers are tightly attached until the design wall thickness requirement is met;
(iii) and demolding the jet pipe prefabricated body, and then sewing the carbon fiber prefabricated body, wherein the width and the interval of the sewing lines are less than 5 mm. By adopting a layer laying sewing scheme, the size of the thread bundle of the sewing thread and the sewing distance are controlled, and the bonding strength between layers of the fabric of the spraying pipe can be effectively improved.
In the invention, the carbon fiber cloth is used for preparing the jet pipe preform by adopting a layer-laying sewing process, so that the near-net-size preparation can be realized, the fiber volume fraction of the preform is effectively improved, the porosity is reduced, and the mechanical property in the axial direction of the fiber is fully exerted.
Meanwhile, precursor slurry containing SiC nanoparticles is uniformly coated on the surface of the carbon fiber cloth, and then the carbon fiber cloth is attached to a spray pipe graphite core mold tool for laying, so that the viscosity of the precursor slurry is fully utilized, the use of extra organic glue solution is avoided, and the impurity components are reduced.
In the step 2, the silicon carbide precursor slurry comprises the following components: solid Polycarbosilane (PCS), liquid PCS and inert filler SiC nanoparticles are blended by wet ball milling blending or solution mechanical stirring blending, and can also be heated in a water bath or an oil bath to assist in mixing. Wherein, liquid PCS is used as a solvent, and the mass ratio of the liquid PCS to the solid PCS is 0.5-2: 1, SiC nano particles account for 0.5-20% of the total mass of the precursor slurry.
The inventors of the present invention have found through studies that the addition of SiC nanoparticles contributes to the improvement of toughness of the composite material, however, if the addition amount of SiC nanoparticles is too small, the toughening effect is not significant, and if the addition amount of SiC nanoparticles is too large, the growth of silicon carbide crystal grains is excessively inhibited, and the above ratio is a preferable range. Meanwhile, the mass ratio of the liquid PCS to the solid PCS has an influence on the viscosity of the ceramic precursor slurry, if the addition amount of the solid PCS is too small, the viscosity of the slurry is lower, the promotion of the components of the ceramic matrix is not facilitated, and if the addition amount of the solid PCS is too large, the viscosity of the slurry is higher, and the porosity and the size in the matrix are larger.
Step 3, densifying the matrix: and (3) densifying the spray pipe preform prepared in the step 2) by adopting a high-temperature compression molding and cracking process to prepare the C/SiC composite spray pipe blank.
In the step 3, the process of densifying the nozzle preform prepared in the step 2) includes:
laying graphite paper on the surface of a graphite core mold tool, clamping and maintaining the spray pipe preform by the graphite core mold tool, putting the whole spray pipe preform into a hot pressing furnace, and performing pyrolysis in an inert atmosphere.
In the step 3, in the high-temperature compression molding cracking process, the cracking temperature is 1000-1800 ℃, the pressure is 2-10 MPa, and the time is 0.5-2 hours; preferably, the cracking temperature is 1000-1500 ℃, the pressure is 2-6 MPa, and the time is 1-2 hours.
Step 4, densification of the spray pipe blank: and (3) machining the spray pipe blank in the step 3) by adopting a machining method to remove machining allowance, and then continuously densifying the machined spray pipe blank by adopting a precursor impregnation cracking (PIP) process to obtain the C/SiC composite material engine spray pipe.
In the step 4, the PIP process includes the steps of: and (3) performing pressure impregnation on the processed spray pipe blank, then performing solidification and cracking, and finally circulating the impregnation and cracking process until the density requirement is met. Wherein the density is required to be 1.8-2.2 g/cm3。
In the PIP process, the dipping pressure is 1-10 MPa, the dipping temperature is 50-100 ℃, and the dipping time is 1-5 hours; the curing temperature is 150-550 ℃, and the curing time is 1-15 hours; the cracking temperature is 900-1550 ℃, and the cracking time is 1-5 hours.
Preferably, in the PIP process, the dipping pressure is 1-5 MPa, the dipping temperature is 60-80 ℃, and the dipping time is 1-4 hours; the curing temperature is 150-350 ℃, and the curing time is 1-5 hours; the cracking temperature is 1000-1200 ℃, and the cracking time is 2-4 hours.
In the step 4, the precursor solution for pressure impregnation includes: solid-state PCS and liquid-state PCS, the mass ratio of the solid-state PCS to the liquid-state PCS is 0-1: 1.
examples
Example 1
A preparation method of a C/SiC composite material engine nozzle comprises the following steps:
1) the method comprises the steps of weaving satin cloth by using continuous carbon fibers as raw materials, and then arranging the carbon fibers in a deposition furnace by using methane as a carbon source gas for deposition treatment of a pyrolytic carbon interface layer. The process conditions of the chemical vapor deposition are as follows: the deposition temperature was 950 ℃, the deposition pressure was 1.5KPa, and the deposition time was 50 hours. The thickness of the pyrolytic carbon interface layer after deposition is about 0.24 μm. Finally, placing the deposited carbon fiber cloth in a high-temperature furnace for graphitization treatment, wherein the graphitization treatment temperature is 1950 ℃, and the graphitization treatment time is 2.5 hours;
2) uniformly coating the precursor slurry on the surface of the carbon fiber cloth obtained in the step 1), then combining with a profiling graphite core mold tool, adopting a layer sewing process to enable the carbon fiber cloth to be tightly attached to the surface of the graphite core mold tool for surrounding forming, and preparing a spray pipe prefabricated body. Wherein the mass ratio of liquid PCS to solid PCS in the precursor slurry is 1: 1, SiC nano particles account for 3 percent of the total mass of the precursor slurry. The distance between the front layer carbon fiber cloth edge seam and the rear layer carbon fiber cloth edge seam is 10mm, and the width and the distance of the sewing thread are 5 mm;
3) clamping and maintaining the spray pipe preform obtained in the step 2) by using a graphite core mold tool, filling a layer of graphite paper between the graphite core mold tool and the spray pipe preform, putting the whole spray pipe preform into a hot pressing furnace, and performing compression molding and rapid cracking in an inert gas Ar atmosphere, wherein the cracking temperature is 1200 ℃, the pressure is 5MPa, and the time is 1 hour;
4) machining the spray pipe blank obtained in the step 3) by adopting a machining method, then continuously densifying the machined spray pipe blank by adopting a PIP (poly-p-phenylene-imide) process for 2 times, and finally obtaining the spray pipe blank with the density of 2.03g/cm3The C/SiC composite nozzle of (1). Wherein, the mass ratio of the solid PCS to the liquid PCS in the impregnation phase is 1: 1, the dipping pressure is 1.5MPa, the dipping time is 2 hours, and the dipping temperature is 60 ℃; the curing temperature is 200 ℃, and the curing time is 2 hours; the cracking temperature is 1050 ℃ and the cracking time is 3 hours.
Example 2
A preparation method of a C/SiC composite material engine nozzle comprises the following steps:
1) continuous carbon fibers are used as raw materials, firstly woven into plain cloth, and then propane is used as a carbon source gas, and the carbon fibers are arranged in a deposition furnace for pyrolytic carbon interface layer deposition treatment. The process conditions of the chemical vapor deposition are as follows: the deposition temperature was 1150 ℃, the deposition pressure was 1.0KPa, and the deposition time was 50 hours. The thickness of the pyrolytic carbon interface layer after deposition is about 0.35 μm. Finally, placing the deposited carbon fiber cloth in a high-temperature furnace for graphitization treatment, wherein the graphitization treatment temperature is 2000 ℃, and the graphitization treatment time is 3 hours;
2) uniformly coating the precursor slurry on the surface of the carbon fiber cloth obtained in the step 1), then combining with a profiling graphite core mold tool, and adopting a layer sewing process to enable the carbon fiber cloth to be tightly attached to the surface of the graphite core mold tool to be formed around the surface to prepare a spray pipe prefabricated part. Wherein the mass ratio of liquid PCS to solid PCS in the precursor slurry is 1.2: 1, SiC nano particles account for 4 percent of the total mass of the precursor slurry. The distance between the front layer carbon fiber cloth edge seam and the rear layer carbon fiber cloth edge seam is 10mm, and the width and the distance of the sewing thread are 10 mm;
3) and (3) carrying out graphite core mold tool clamping and dimensional maintaining on the spray pipe preform obtained in the step 2), then putting the whole spray pipe preform into a hot pressing furnace, and carrying out compression molding and rapid cracking in an inert gas Ar atmosphere. The cracking temperature is 1300 ℃, the pressure is 5MPa, and the time is 1 hour;
4) by machinesProcessing the spray pipe blank obtained in the step 3) by using a processing method, then continuously densifying the processed spray pipe blank by using a PIP (poly-p-phenylene-imide) process for 2 times, and finally obtaining the spray pipe blank with the density of 2.15g/cm3The C/SiC composite nozzle member of (1). Wherein, the mass ratio of the solid PCS to the liquid PCS in the impregnation phase is 1: 1.5, the dipping pressure is 2MPa, the dipping time is 1 hour, and the dipping temperature is 70 ℃; the curing temperature is 250 ℃, and the curing time is 1.5 hours; the cracking temperature is 1200 ℃ and the cracking time is 4 hours.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (10)
1. A rapid preparation method of a C/SiC composite material engine nozzle is characterized by comprising the following steps:
step (1), adopting a chemical vapor deposition process, taking hydrocarbon gas as a carbon source gas, taking inert gas or nitrogen as diluent gas, arranging carbon fibers in a carbon deposition furnace for deposition, preparing carbon fiber cloth containing a pyrolytic carbon interface layer, and then carrying out graphitization treatment on the carbon fiber cloth containing the pyrolytic carbon interface layer;
step (2), uniformly coating silicon carbide precursor slurry on the surface of the carbon fiber cloth obtained in the step (1), combining a profiling graphite core mold tool, adopting a layer sewing process to enable the carbon fiber cloth to be tightly attached to the surface of the profiling graphite core mold tool and to be formed in a surrounding mode, and preparing a spray pipe prefabricated body;
step (3), densifying the spray pipe preform prepared in the step (2) by adopting a high-temperature compression molding and cracking process to prepare a C/SiC composite spray pipe blank;
and (4) machining the spray pipe blank in the step (3) by adopting a machining method, removing machining allowance, and then continuously densifying the machined spray pipe blank by adopting a precursor impregnation cracking process to obtain the C/SiC composite material engine spray pipe.
2. The preparation method according to claim 1, wherein in the step (1), in the chemical vapor deposition process, the deposition pressure is 1 to 15KPa, the deposition temperature is 800 to 1200 ℃, and the deposition time is 40 to 60 hours; and/or
In the graphitization treatment, the graphitization treatment temperature is 1900-2200 ℃, and the graphitization treatment time is 2-4 hours.
3. The method according to claim 1, wherein in the step (1), the thickness of the pyrolytic carbon interface layer deposited on the carbon fiber cloth containing the pyrolytic carbon interface layer is 0.2-1.0 μm.
4. The preparation method of claim 1, wherein in the step (2), the step of preparing the nozzle preform by adopting a ply sewing process comprises the following specific steps:
(i) adopting a split type profiling graphite core mold tool, and coating a release agent on the surface of the split type profiling graphite core mold tool; clinging the carbon fiber cloth coated with the silicon carbide precursor slurry and containing the pyrolytic carbon interface layer to the surface of the graphite core mold tool, forming in a surrounding mode, butting the edge seams of the layers, and finishing the first layer of layers of the spray pipe preform;
(ii) laying other layers sequentially by the same first layer laying method, wherein the edge seams of each layer of carbon fiber cloth are staggered sequentially in the laying process, the distance between the edge seams of the front layer of carbon fiber cloth and the edge seams of the rear layer of carbon fiber cloth is larger than 10mm, and the layers are tightly attached until the design wall thickness requirement is met;
(iii) and demolding the jet pipe prefabricated body, and then sewing the carbon fiber prefabricated body, wherein the width and the interval of the sewing lines are less than 5 mm.
5. The preparation method according to claim 1, wherein in the step (2), the components of the silicon carbide precursor slurry comprise solid polycarbosilane, liquid polycarbosilane and SiC nanoparticles, wherein the mass ratio of the liquid polycarbosilane to the solid polycarbosilane is 0.5-2: 1, SiC nano particles account for 0.5-20% of the total mass of the precursor slurry.
6. The method of claim 1, wherein in step (3), the densifying the nozzle preform prepared in step (2) comprises: laying graphite paper on the surface of a graphite core mold tool, clamping and maintaining the spray pipe preform by the graphite core mold tool, putting the whole spray pipe preform into a hot pressing furnace, and performing pyrolysis in an inert atmosphere.
7. The preparation method according to claim 1, wherein in the step (3), in the high-temperature compression molding cracking process, the cracking temperature is 1000 ℃ to 1800 ℃, the pressure is 2MPa to 10MPa, and the time is 0.5 hour to 2 hours.
8. The method according to claim 1, wherein in the step (4), the step of the precursor impregnation cracking process comprises: pressure impregnation is carried out on the processed spray pipe blank, then solidification and cracking are carried out, and finally the impregnation cracking process is circulated until the density reaches 1.8-2.2 g/cm3。
9. The preparation method of claim 8, wherein in the precursor impregnation cracking process, the impregnation pressure is 1-10 MPa, the impregnation temperature is 50-100 ℃, and the impregnation time is 1-5 hours; the curing temperature is 150-550 ℃, and the curing time is 1-15 hours; the cracking temperature is 900-1550 ℃ and the cracking time is 1-5 hours.
10. The preparation method according to claim 8, wherein the precursor solution for pressure impregnation comprises solid polycarbosilane and liquid polycarbosilane, and the mass ratio of the solid polycarbosilane to the liquid polycarbosilane is 0-1: 1.
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