CN103724040A - Preparation method of SiC-ZrC segmented ceramic matrix composite spray pipe - Google Patents
Preparation method of SiC-ZrC segmented ceramic matrix composite spray pipe Download PDFInfo
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- CN103724040A CN103724040A CN201310412185.2A CN201310412185A CN103724040A CN 103724040 A CN103724040 A CN 103724040A CN 201310412185 A CN201310412185 A CN 201310412185A CN 103724040 A CN103724040 A CN 103724040A
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Abstract
A preparation method of a SiC-ZrC segmented ceramic matrix composite spray pipe is characterized in that the ceramic matrix composite comprises a porous C/C composite framework, a SiC coating and a ZrC coating. A CVI (chemical vapor infiltration) method is adopted to prepare a porous C/C precast body which is placed into absolute ethyl alcohol for ultrasonic oscillation and cleaning and placed into a graphite crucible after drying; Si is placed on the surfaces of a straight section and a skirt part of the porous C/C precast body, the porous C/C precast body with Si is then embedded by SiC powder, and the porous C/C precast body embedded by the Sic powder is placed into a tube furnace and heated to a high temperature; Zr is placed at the skirt section of the porous C/C precast body, and the porous C/C precast body with Zr is then placed into the tube furnace and heated to the high temperature; a melt is infiltrated into the porous body through capillary force and reacts to obtain the SiC-ZrC segmented ceramic matrix composite spray pipe. Obtained ceramic matrix composite has the advantages of light weight, high strength, low porosity, high antioxidant and ablation-resistant capacities, short preparation period and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of polymer matrix composites jet pipe, particularly relate to a kind of preparation method of ceramic matric composite jet pipe of SiC-ZrC segmentation distribution.
Background technology
Carbon/carbon (hereinafter to be referred as C/C) matrix material, because it has the characteristic that under low density and excellent mechanical behavior under high temperature, particularly high temperature, mechanical property goes up not down, becomes the preferred material of the thermojunction member of advanced aircraft.Yet, very easily oxidation under C/C matrix material high temperature, oxidation can make its hole increase, structure weaken, cause the rapid reduction of intensity and other mechanical propertys, and oxidation weight loss 1%, its strength degradation reaches 10%, and (as the Throat Materials for Solid Rocket Motors of Gao Chongzhi ratio, guided missile nose cone etc.) C/C matrix material does not have required high temperature resistance ablation energy ability in extreme environment.Therefore, the high-temp antioxidizing ablation problem of C/C matrix material is the bottleneck of realizing its practical application.Good heat, the chemical stability of mechanical property by comprehensive carbon fiber excellence and ceramic matrix, prepares a kind of by thermal protection, structural bearing and the anti-oxidant new function integrated composite combining for this reason.
Application number is the preparation method that 200910022719.4 Chinese patent discloses a kind of Improvement of The Oxidation Protective Coating For C/c Composites, treated C/C matrix material is embedded in powder, put into plumbago crucible, at 1800～2200 ℃, carry out processing for 1～3 hour, utilize Supersonic Plasma Spraying equipment by MoSi
2powder sprays to the C/C composite material surface with SiC transition layer, will be prepared with SiC/MoSi
2the C/C matrix material of coating is put into High Temperature Furnaces Heating Apparatus, at 1200～1400 ℃, heat-treats 2～6 hours.The C/C matrix material that the method prepares anti-oxidization time in more than 1650 ℃ still air is brought up to 300～400 hours in 200 hours by prior art.
Document " the reaction infiltration method preparation of C/C-SiC matrix material and microtexture, Zhao Yanwei, Sun Wenting, Li Junping, Liu Hongrui, Zhang Guobing, aerospace material technique report, the 2nd phase in 2013 " disclose a kind of reaction infiltration method with no pressure at 1550 ℃ by melt of si or Si
0.9zr
0.1be impregnated into the C/C-SiC matrix material of having prepared high densification in porous C/C precast body.Adopt reaction infiltration method with no pressure to prepare C/C-SiC matrix material, after infiltration Si, in matrix material, be mainly the SiC phase that reaction generates, also have a small amount of free Si residual; Infiltration Si
0.9zr
0.1siC, ZrSi in rear matrix material, have mainly been generated
2with ZrC phase, do not find that free Si exists.
Summary of the invention
1, the technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, a kind of preparation method of ceramic matric composite jet pipe of SiC-ZrC segmentation distribution is provided, it is characterized in that described ceramic matric composite comprises porous C/C matrix material skeleton, SiC coating and ZrC coating.First adopt chemical Vapor deposition process to prepare C/C porous preform, the two ends of precast body are that straight section and skirt portion are infiltrated Si, two ends are imbedded in SiC powder, Zr infiltrates in middle throat, then successively separately at high temperature Si and Zr react generation SiC and ZrC with C after, make, it is characterized in that including the preparation process of following order:
(1) adopt the cloth lamination of plain weave to prepare Two-dimensional Carbon fiber preform;
(2) adopt CVI on carbon fabric perform, to deposit pyrolysis C, through high temperature graphitization, process and make porous C/C precast body;
(3) porous C/C precast body is put into dehydrated alcohol cleaned by ultrasonic vibration 2～4 times, in air dry oven, 80～120 ℃ are dried 3～5h, until mass conservation;
(4) porous C/C precast body of having dried is put into plumbago crucible;
(5) Si is placed on the surface in porous C/C precast body straight section and skirt section, and with the embedding of SiC powder, puts into tube furnace, tube furnace temperature rise rate is 8～10 ℃/min, heats to 1400～1600 ℃, furnace cooling after insulation 1～3h;
(6) Zr is placed on the middle throat of porous C/C precast body surface, puts into tube furnace, tube furnace temperature rise rate is 8～10 ℃/min, heats to 1900～2100 ℃, furnace cooling after insulation 0.5～1.5h;
(7) take out matrix material and obtain the ceramic matric composite jet pipe that SiC-ZrC segmentation distributes after by surface working.
The present invention has advantages of: (1) can not cause Carbon Fiber Damage after adopting the standby porous C/C precast body infiltration Si of CVI legal system and Zr, has guaranteed composite material strength; (2) in the matrix material making, can not remain free Si, anti-oxidant and anti-ablation ability is strong; (3) preparation cycle is short, cost is low, residual clearance rate is low and can dead size be shaped.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Embodiment 1
(1) adopt the cloth lamination of plain weave to prepare Two-dimensional Carbon fiber preform;
(2) adopt CVI on carbon fabric perform, to deposit pyrolysis C, through high temperature graphitization, process and make porous C/C precast body;
(3) porous C/C precast body is put into dehydrated alcohol cleaned by ultrasonic vibration 2 times, in air dry oven, 100 ℃ are dried 3h, until mass conservation;
(4) porous C/C precast body of having dried is put into plumbago crucible;
(5) Si is placed on the surface in porous C/C precast body straight section and skirt section, and with the embedding of SiC powder, puts into tube furnace, tube furnace temperature rise rate is 8 ℃/min, heats to 1500 ℃, furnace cooling after insulation 2h;
(6) Zr is placed on the middle throat of porous C/C precast body surface, puts into tube furnace, tube furnace temperature rise rate is 8 ℃/min, heats to 1900 ℃, furnace cooling after insulation 1h;
(7) take out matrix material and obtain the ceramic matric composite jet pipe that SiC-ZrC segmentation distributes after by surface working.
Embodiment 2
(1) adopt the cloth lamination of plain weave to prepare Two-dimensional Carbon fiber preform;
(2) adopt CVI on carbon fabric perform, to deposit pyrolysis C, through high temperature graphitization, process and make porous C/C precast body;
(3) porous C/C precast body is put into dehydrated alcohol cleaned by ultrasonic vibration 3 times, in air dry oven, 120 ℃ are dried 4h, until mass conservation;
(4) porous C/C precast body of having dried is put into plumbago crucible;
(5) Si is placed on the surface in porous C/C precast body straight section and skirt section, and with the embedding of SiC powder, puts into tube furnace, tube furnace temperature rise rate is 10 ℃/min, heats to 1600 ℃, furnace cooling after insulation 3h;
(6) Zr is placed on the middle throat of porous C/C precast body surface, puts into tube furnace, tube furnace temperature rise rate is 10 ℃/min, heats to 2000 ℃, furnace cooling after insulation 1.5h;
(7) take out matrix material and obtain the ceramic matric composite jet pipe that SiC-ZrC segmentation distributes after by surface working.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for the ceramic matric composite jet pipe that SiC-ZrC segmentation distributes, is characterized in that comprising the preparation process of following order:
(1) adopt the cloth lamination of plain weave to prepare Two-dimensional Carbon fiber preform;
(2) adopt CVI on carbon fabric perform, to deposit pyrolysis C, through high temperature graphitization, process and make porous C/C precast body;
(3) porous C/C precast body is put into dehydrated alcohol cleaned by ultrasonic vibration 2～4 times, in air dry oven, 80～120 ℃ are dried 3～5h, until mass conservation;
(4) porous C/C precast body of having dried is put into plumbago crucible;
(5) Si is placed on the surface in porous C/C precast body straight section and skirt section, and with the embedding of SiC powder, puts into tube furnace, tube furnace temperature rise rate is 8～10 ℃/min, heats to 1400～1600 ℃, furnace cooling after insulation 1～3h;
(6) Zr is placed on the middle throat of porous C/C precast body surface, puts into tube furnace, tube furnace temperature rise rate is 8～10 ℃/min, heats to 1900～2100 ℃, furnace cooling after insulation 0.5～1.5h;
(7) take out matrix material and obtain the ceramic matric composite jet pipe that SiC-ZrC segmentation distributes after by surface working.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190932A (en) * | 2014-09-10 | 2014-12-10 | 太仓派欧技术咨询服务有限公司 | Manufacturing method of ceramic matrix composite nozzle throat nickel alloy strengthening ring |
| CN104402525A (en) * | 2014-10-30 | 2015-03-11 | 中国人民解放军国防科学技术大学 | Graphite surface ablation-resistant layer and preparation method thereof |
| CN111377749A (en) * | 2020-02-24 | 2020-07-07 | 哈尔滨工业大学 | Method for realizing transportation of ceramic slurry in carbon fiber woven body by imitating transpiration effect |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515870A (en) * | 2011-12-10 | 2012-06-27 | 西北工业大学 | Preparation method of C/SiC-ZrB2-ZrC ultrahigh-temperature ceramic-based composite material |
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- 2013-09-11 CN CN201310412185.2A patent/CN103724040B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515870A (en) * | 2011-12-10 | 2012-06-27 | 西北工业大学 | Preparation method of C/SiC-ZrB2-ZrC ultrahigh-temperature ceramic-based composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190932A (en) * | 2014-09-10 | 2014-12-10 | 太仓派欧技术咨询服务有限公司 | Manufacturing method of ceramic matrix composite nozzle throat nickel alloy strengthening ring |
| CN104402525A (en) * | 2014-10-30 | 2015-03-11 | 中国人民解放军国防科学技术大学 | Graphite surface ablation-resistant layer and preparation method thereof |
| CN104402525B (en) * | 2014-10-30 | 2016-08-24 | 中国人民解放军国防科学技术大学 | Graphite surface anti-yaw damper layer and preparation method thereof |
| CN111377749A (en) * | 2020-02-24 | 2020-07-07 | 哈尔滨工业大学 | Method for realizing transportation of ceramic slurry in carbon fiber woven body by imitating transpiration effect |
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Address after: 215400 Chengxiang City, Taicang Province town of the People South Road, No. 162, No. Patentee after: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. Address before: 215400 people's road, Jiangsu, Taicang Hua Xu apartment C412 Patentee before: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. |