CN110550963B - Preparation method of thin-wall C/SiC extension section - Google Patents
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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Abstract
The invention disclosesA preparation method of a thin-wall C/SiC extension section comprises the steps of sequentially laying carbon fiber cloth to prepare an extension section preform, carrying out degumming treatment, carrying out chemical vapor infiltration, sucking a mixed solution A into a small end of the preform in a vacuum impregnation mode, sucking a mixed solution B into the extension section preform in a vacuum impregnation mode, placing the cured extension section preform into a furnace for high-temperature treatment, and circulating until the weight of the extension section preform increased in the next round is less than 1% of the weight of the extension section preform increased in the previous round. The density of the prepared extension section does not exceed 2.0g/cm3While the density of the conventional niobium alloy is 8.85g/cm3The quality of the extension section can be effectively reduced, and the performance of the engine is improved; in addition, compared with the conventional niobium alloy extension section, the extension section provided by the invention has good oxidation resistance due to the SiC and Si-O-C materials, does not need to be subjected to complex oxidation resistance treatment, and has a simple preparation process.
Description
Technical Field
The invention belongs to the technical field of C/SiC composite ceramics, and particularly relates to a preparation method of a thin-wall C/SiC extension section.
Background
The liquid rocket engine extension section is used for increasing the area ratio of an engine nozzle and is one of main measures for improving the specific impulse of the engine. The difficult-to-dissolve metal niobium alloy is widely used as the material of the extension section at present. The niobium alloy has good atmospheric corrosion resistance and good processing performance, can keep higher strength at high temperature, but has poor high-temperature oxidation resistance, expensive material price and complex manufacturing process.
Disclosure of Invention
The invention aims to provide a preparation method of a thin-wall C/SiC extension segment, which can effectively reduce the quality of the extension segment, effectively reduce the preparation cost and does not need antioxidant treatment, aiming at the defects of the technology.
In order to realize the purpose, the preparation method of the thin-wall C/SiC extension segment comprises the following steps:
1) sequentially laying carbon fiber cloth, and preparing an extension section prefabricated body along a core mold in a sewing mode;
2) placing the extending section prefabricated body into a furnace, and carrying out degumming treatment;
3) putting the prefabricated body subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration;
4) polycarbosilane and divinylbenzene are mixed according to the mass ratio of 1: 0.4-0.6, preparing a mixed solution A, and putting the mixed solution A into a vacuum impregnation container A; then placing the small end of the extension segment preform into a vacuum impregnation container A, sucking the mixed solution A into the small end of the preform in a vacuum impregnation mode, drying and curing;
5) polysiloxane and divinylbenzene in a mass ratio of 1: 0.5-0.8, preparing a mixed solution B, and putting the mixed solution B into a vacuum impregnation container B; then putting the part of the extending section preform which is not impregnated into a vacuum impregnation container B, sucking the mixed solution B into the extending section preform in a vacuum impregnation mode, drying and curing;
6) placing the solidified extending section prefabricated body into a furnace for high-temperature treatment;
7) and (5) repeating the steps 4) to 6) until the weight increase of the next round is less than 1 percent of the mass increase of the previous round.
Further, in the step 1), the carbon fiber cloth for sewing is T300B-3K plain cloth, the yarn for sewing is carbon fiber T300B-6K, and the sewing distance is 2-4 mm/needle.
Further, in the step 2), the degumming treatment temperature is 600-1100 ℃, the vacuum degree is-70 to-99 KPa, and the time is 5-10 h.
Further, in the step 3), the prefabricated body after the glue removing treatment is placed into a vapor deposition furnace for chemical vapor infiltration to 0.8-1.0 g/cm3The carbon source gas for chemical vapor deposition is methane or propylene, the purity of the methane or the propylene is more than 99.99 percent, the deposition temperature is 800-1200 ℃, the pressure is-0.08-0.09 MPa, and the time is 120-240 hours.
Further, in the step 4), the dipping vacuum degree is-0.08 to-0.09 MPa, the dipping time is 7 to 10 hours, the drying and curing temperature is 80 to 120 ℃, and the time is 8 to 12 hours.
Further, in the step 5), the dipping vacuum degree is-0.08 to-0.09 MPa, the dipping time is 10 to 15 hours, the drying and curing temperature is 100 to 150 ℃, and the time is 4 to 8 hours.
Further, in the step 6), the high-temperature treatment temperature is 800-1200 ℃, the pressure is 0.01-0.03 MPa, and the time is 2-4 h.
Compared with the prior art, the invention has the following advantages: the density of the prepared extension section does not exceed 2.0g/cm3While the density of the conventional niobium alloy is 8.85g/cm3The quality of the extension section can be effectively reduced, and the performance of the engine is improved; in addition, compared with the conventional niobium alloy extension section, the extension section provided by the invention has good oxidation resistance due to the SiC and Si-O-C materials, does not need to be subjected to complex oxidation resistance treatment, and has a simple preparation process; the extension section provided by the invention is composed of different materials according to different axial temperatures of products, the high-temperature small end is made of high-temperature-resistant C/SiC materials, the low-temperature large end is made of C/Si-0-C, and the cost of polysiloxane which is a main raw material for preparing the C/Si-0-C is 60 yuan/KG and is far less than that of polycarboxyoxane (5000 yuan/KG) which is a main raw material for preparing the C/SiC, so that the preparation cost of the extension section can be effectively reduced compared with that of the traditional single-component C/SiC materials.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The preparation method of the thin-wall C/SiC extension segment comprises the following steps:
1) sequentially laying carbon fiber cloth, and preparing an extension section prefabricated body along a core mold in a sewing mode; the carbon fiber cloth for sewing is T300B-3K plain cloth, the yarns for sewing are carbon fiber T300B-6K, and the sewing distance is 2-4 mm/needle;
2) putting the extending section prefabricated body into a furnace, and carrying out degumming treatment, wherein the degumming treatment temperature is 600-1100 ℃, the vacuum degree is-70 to-99 KPa, and the time is 5-10 h;
3) putting the prefabricated body subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration to 0.8-1.0 g/cm3The carbon source gas for chemical vapor deposition is methane or propylene, and the purity of the methane or the propyleneMore than 99.99 percent, the deposition temperature is 800-1200 ℃, the pressure is-0.08-0.09 MPa, and the time is 120-240 hours;
4) polycarbosilane and divinylbenzene are mixed according to the mass ratio of 1: 0.4-0.6, preparing a mixed solution A, and putting the mixed solution A into a vacuum impregnation container A; then placing the small end of the prefabricated body of the extension section into a vacuum impregnation container A, sucking the mixed solution A into the small end of the prefabricated body in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.08 to-0.09 MPa, the impregnation time is 7 to 10 hours, the drying and curing temperature is 80 to 120 ℃, and the time is 8 to 12 hours;
5) polysiloxane and divinylbenzene in a mass ratio of 1: 0.5-0.8, preparing a mixed solution B, and putting the mixed solution B into a vacuum impregnation container B; then putting the part of the un-impregnated extending section preform into a vacuum impregnation container B, sucking the mixed solution B into the extending section preform in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.08 to-0.09 MPa, the impregnation time is 10 to 15 hours, the drying and curing temperature is 100 to 150 ℃, and the time is 4 to 8 hours;
the viscosity of the mixed solution A is determined by the proportion of the mixed solution A, the high-temperature area of the small end of the prefabricated body of the extension section is ensured to be composed of a high-temperature resistant SiC matrix by matching with the dipping process of the mixed solution A, and the dipping time is adjusted according to the height of the high-temperature resistant area of the extension section;
the proportion of the mixed solution B determines the viscosity of the mixed solution B, the impregnation process of the mixed solution B is matched to ensure that the large end is soaked, the mixed solution B consists of an SI-O-C matrix, meanwhile, the proportion of a transition layer from the SI-O-C to the SIC is determined, the two matrix materials have different linear expansion, and large thermal stress is easily generated without good transition, so that the solution at the joint in the subsequent cracking process is cracked and damaged;
6) placing the solidified extending section prefabricated body into a furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 800-1200 ℃, the pressure is 0.01-0.03 MPa, and the time is 2-4 h;
7) repeating the steps 4) to 6) until the weight increase of the next round is less than 1 percent of the mass increase of the previous round;
8) and machining the blank to the required size of the extension section through mechanical machining to finish the preparation of the extension section.
The density of the prepared extension section does not exceed 2.0g/cm3While the density of the conventional niobium alloy is 8.85g/cm3The quality of the extension section can be effectively reduced, and the performance of the engine is improved; in addition, compared with the conventional niobium alloy extension section, the extension section provided by the invention has good oxidation resistance due to the SiC and Si-O-C materials, does not need to be subjected to complex oxidation resistance treatment, and has a simple preparation process; the extension section provided by the invention is composed of different materials according to different axial temperatures of products, the high-temperature small end is made of high-temperature-resistant C/SiC materials, the low-temperature large end is made of C/Si-0-C, and the cost of polysiloxane which is a main raw material for preparing the C/Si-0-C is 60 yuan/KG and is far less than that of polycarboxyoxane (5000 yuan/KG) which is a main raw material for preparing the C/SiC, so that the preparation cost of the extension section can be effectively reduced compared with that of the traditional single-component C/SiC materials.
Example 1
1) After carbon fiber cloth T300B-3K plain cloth is paved to 5mm along a core mould, all layers of carbon fiber cloth are connected into a whole extending section prefabricated body in a sewing mode, and the sewing needle pitch is 3 mm/needle;
2) putting the extending section prefabricated body into a furnace, and carrying out degumming treatment, wherein the degumming treatment temperature is 800 ℃, the vacuum degree is-90 KPa, and the time is 6 h;
3) putting the prefabricated body which is subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration to 0.8g/cm3The carbon source gas for chemical vapor deposition is methane, the deposition temperature is 1000 ℃, the pressure is-0.09 MPa, and the time is 200 h;
4) polycarbosilane and divinylbenzene are mixed according to the mass ratio of 1: 0.5 preparing a mixed solution A, and putting the mixed solution A into a vacuum impregnation container A; then placing the small end of the prefabricated body of the extension section into a vacuum impregnation container A, sucking the mixed solution A into the small end of the prefabricated body in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.09 MPa, the impregnation time is 10 hours, the drying and curing temperature is 100 ℃, and the time is 10 hours;
5) polysiloxane and divinylbenzene in a mass ratio of 1: 0.8, preparing a mixed solution B, and putting the mixed solution B into a vacuum impregnation container B; then putting the part of the un-impregnated preform of the extension section into a vacuum impregnation container B, sucking the mixed solution B into the preform of the extension section in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.09 MPa, the impregnation time is 15h, the drying and curing temperature is 150 ℃, and the impregnation time is 6 h;
the viscosity of the mixed solution A is determined by the proportion of the mixed solution A, the high-temperature area of the small end of the prefabricated body of the extension section is ensured to be composed of a high-temperature resistant SiC matrix by matching with the dipping process of the mixed solution A, and the dipping time is adjusted according to the height of the high-temperature resistant area of the extension section;
the proportion of the mixed solution B determines the viscosity of the mixed solution B, the impregnation process of the mixed solution B is matched to ensure that the large end is soaked, the mixed solution B consists of an SI-O-C matrix, meanwhile, the proportion of a transition layer from the SI-O-C to the SIC is determined, the two matrix materials have different linear expansion, and large thermal stress is easily generated without good transition, so that the solution at the joint in the subsequent cracking process is cracked and damaged;
6) placing the solidified extending section prefabricated body into a furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 1200 ℃, the pressure is 0.02MPa, and the time is 2 hours;
7) repeating the steps 4) to 6) until the weight increase of the next round is less than 1 percent of the mass increase of the previous round;
8) and machining the blank to the required size of the extension section through mechanical machining to finish the preparation of the extension section.
Example 2
1) After carbon fiber cloth T300B-3K plain cloth is paved to 5mm along a core mould, all layers of carbon fiber cloth are connected into a whole extending section prefabricated body in a sewing mode, and the sewing needle pitch is 4 mm/needle;
2) putting the extending section prefabricated body into a furnace, and carrying out degumming treatment, wherein the degumming treatment temperature is 900 ℃, the vacuum degree is-80 KPa, and the time is 8 h;
3) putting the prefabricated body which is subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration to 0.9g/cm3The carbon source gas for chemical vapor deposition is methane, the deposition temperature is 1100 ℃, the pressure is-0.07 MPa, and the time is 180 hours;
4) polycarbosilane and divinylbenzene are mixed according to the mass ratio of 1: 0.6 preparing a mixed solution A, and putting the mixed solution A into a vacuum impregnation container A; then placing the small end of the prefabricated body of the extension section into a vacuum impregnation container A, sucking the mixed solution A into the small end of the prefabricated body in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.08 MPa, the impregnation time is 8 hours, the drying and curing temperature is 90 ℃, and the impregnation time is 12 hours;
5) polysiloxane and divinylbenzene in a mass ratio of 1: 0.5 preparing a mixed solution B, and putting the mixed solution B into a vacuum impregnation container B; then putting the part of the un-impregnated preform of the extension section into a vacuum impregnation container B, sucking the mixed solution B into the preform of the extension section in a vacuum impregnation mode, drying and curing, wherein the impregnation vacuum degree is-0.08 MPa, the impregnation time is 12h, the drying and curing temperature is 130 ℃, and the impregnation time is 8 h;
the viscosity of the mixed solution A is determined by the proportion of the mixed solution A, the high-temperature area of the small end of the prefabricated body of the extension section is ensured to be composed of a high-temperature resistant SiC matrix by matching with the dipping process of the mixed solution A, and the dipping time is adjusted according to the height of the high-temperature resistant area of the extension section;
the proportion of the mixed solution B determines the viscosity of the mixed solution B, the impregnation process of the mixed solution B is matched to ensure that the large end is soaked, the mixed solution B consists of an SI-O-C matrix, meanwhile, the proportion of a transition layer from the SI-O-C to the SIC is determined, the two matrix materials have different linear expansion, and large thermal stress is easily generated without good transition, so that the solution at the joint in the subsequent cracking process is cracked and damaged;
6) placing the solidified extending section prefabricated body into a furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 1000 ℃, the pressure is 0.03MPa, and the time is 4 hours;
7) repeating the steps 4) to 6) until the weight increase of the next round is less than 1 percent of the mass increase of the previous round;
8) and machining the blank to the required size of the extension section through mechanical machining to finish the preparation of the extension section.
Claims (5)
1. A preparation method of a thin-wall C/SiC extension section is characterized by comprising the following steps: the method comprises the following steps:
1) sequentially laying carbon fiber cloth, and preparing an extension section prefabricated body along a core mold in a sewing mode;
2) placing the extending section prefabricated body into a furnace, and carrying out degumming treatment; the degumming treatment temperature is 600-1100 ℃, the vacuum degree is-70 to-99 KPa, and the time is 5-10 h;
3) putting the prefabricated body subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration; putting the prefabricated body subjected to the degumming treatment into a vapor deposition furnace for chemical vapor infiltration to 0.8-1.0 g/cm3The carbon source gas for chemical vapor deposition is methane or propylene, the purity of the methane or the propylene is more than 99.99 percent, the deposition temperature is 800-1200 ℃, the pressure is-0.08-0.09 MPa, and the time is 120-240 hours;
4) polycarbosilane and divinylbenzene are mixed according to the mass ratio of 1: 0.4-0.6, preparing a mixed solution A, and putting the mixed solution A into a vacuum impregnation container A; then placing the small end of the extension segment preform into a vacuum impregnation container A, sucking the mixed solution A into the small end of the preform in a vacuum impregnation mode, drying and curing;
5) polysiloxane and divinylbenzene in a mass ratio of 1: 0.5-0.8, preparing a mixed solution B, and putting the mixed solution B into a vacuum impregnation container B; then putting the part of the extending section preform which is not impregnated into a vacuum impregnation container B, sucking the mixed solution B into the extending section preform in a vacuum impregnation mode, drying and curing;
6) placing the solidified extending section prefabricated body into a furnace for high-temperature treatment;
7) and (5) repeating the steps 4) to 6) until the weight increase of the next round is less than 1 percent of the mass increase of the previous round.
2. The method for preparing the thin-walled C/SiC extension segment according to claim 1, wherein: in the step 1), the carbon fiber cloth for sewing is T300B-3K plain cloth, the yarns for sewing are carbon fibers T300B-6K, and the sewing distance is 2-4 mm per needle.
3. The method for preparing the thin-walled C/SiC extension segment according to claim 1, wherein: in the step 4), the dipping vacuum degree is-0.08 to-0.09 MPa, the dipping time is 7 to 10 hours, the drying and curing temperature is 80 to 120 ℃, and the time is 8 to 12 hours.
4. The method for preparing the thin-walled C/SiC extension segment according to claim 1, wherein: in the step 5), the dipping vacuum degree is-0.08 to-0.09 MPa, the dipping time is 10 to 15 hours, the drying and curing temperature is 100 to 150 ℃, and the time is 4 to 8 hours.
5. The method for preparing the thin-walled C/SiC extension segment according to claim 1, wherein: in the step 6), the high-temperature treatment temperature is 800-1200 ℃, the pressure is 0.01-0.03 MPa, and the time is 2-4 h.
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