CN104926346A - Interface-phase-including alumina fibrous fabric reinforced silicon carbide ceramic and preparation method thereof - Google Patents
Interface-phase-including alumina fibrous fabric reinforced silicon carbide ceramic and preparation method thereof Download PDFInfo
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- CN104926346A CN104926346A CN201510266810.6A CN201510266810A CN104926346A CN 104926346 A CN104926346 A CN 104926346A CN 201510266810 A CN201510266810 A CN 201510266810A CN 104926346 A CN104926346 A CN 104926346A
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Abstract
The invention discloses an interface-phase-including alumina fibrous fabric reinforced silicon carbide ceramic. The interface-phase-including alumina fibrous fabric reinforced silicon carbide ceramic uses alumina fibrous fabric as a reinforcement and a silicon carbide ceramic as a matrix, and further, a sacrificial carbon interface phase is formed between the reinforcement and the matrix. A preparation method of the interface-phase-including alumina fibrous fabric reinforced silicon carbide ceramic comprises the following technical steps of first, putting the alumina fibrous fabric into a muffle furnace for carrying out high-temperature oxidation, and depositing a cracking carbon coating on the surface of the fibrous fabric by utilizing a chemical vapor deposition technique; preparing a precursor solution, carrying out vacuum impregnation on the fibrous fabric with the precursor solution, and completing one-time compaction and multi-time repeated compaction through low-temperature crosslinking and high-temperature ceramization, to prepare an alumina fibrous fabric reinforced silicon carbide ceramic including a cracking carbon interface phase; finally, sacrificing the cracking carbon interface phase through high-temperature heat treatment, to prepare a final product. The product provided by the invention is excellent in all mechanical property, antioxygenic property and high-temperature property, further, is short in preparation period and low in cost, and can be molded in a near-net-size manner.
Description
Technical field
The present invention relates to fiber reinforcedceramics field, particularly relate to a kind of sapphire whisker fabric and strengthen silicon carbide ceramics and preparation method thereof.
Background technology
Continuous Fiber Reinforced Ceramic Matrix Composites (CFCC) has the advantages such as high specific strength, high ratio modulus, high tenacity, anti-yaw damper, resistance to oxidation, be the main flow of novel fire resistant, the development of low density heat structured material, have broad application prospects at aerospace field.According to the difference of matrix variety, CFCC can be divided into glass-based, oxide-base and non-oxidized substance based composites three class.At present, study the more and wider material system of application and mainly contain carbon, silicon carbide and oxide ceramics based composites, the fortifying fibre of employing mainly contains carbon fiber, silicon carbide fiber and oxide fibre three class.Wherein, carbon fibre reinforced ceramics based composites has excellent over-all properties, but its antioxidant property is poor; Silicon carbide fiber strengthens ceramic matric composite and has excellent over-all properties equally, but it is practical temperature limited in silicon carbide fiber and high-performance silicon carbide fiber (as Hi-Nicalon etc.) expensive, is difficult to large-scale promotion application; Oxide fibre enhancing ceramic matric composite has excellent antioxidant property and use temperature is higher, becomes the focus of Novel hot structured material research.In addition, oxide ceramics based composites median surface chemistry and ermal physics poor compatibility, and fiber easily damages and causes mechanical property not high; And carbon/silicon carbide ceramic matrix composite has excellent high temperature resistant, anti-oxidant and creep-resistant property, high temperature absorbing material field can also be applied to simultaneously.Thus, oxide fibre strengthens the extensive concern that carbon/silicon carbide ceramic matrix composite causes researchist.
The preparation technology that oxide fibre strengthens carbon/silicon carbide ceramic matrix composite mainly contains: precursor infiltration and pyrolysis method (PIP), chemical vapor infiltration (CVI), liquid-phase silicone method of impregnation (LSI) and mud heat of immersion platen press (SI-HP) etc.Wherein, the application of PIP technique and CVI technique is comparatively extensive.Silicon carbide good crystallinity prepared by CVI technique, purity is higher, but this technique densification rate is low, the cycle is long, requires higher, need special equipment, and matrix composition designability is poor to technical process control; And PIP technique preparation temperature is lower, without the need to pressurization, less to the thermomechanical damage of fiber, operating process is simple, not high to equipment requirements, and matrix the Nomenclature Composition and Structure of Complexes designability is strong, the main shortcoming of this technique is that fiber and matrix surface reaction easily occur and form strong interfacial bond, usually needs to carry out interface modification.
Current, there is no and prepare about PIP technique the research report that oxide fibre strengthens carbon/silicon carbide ceramic matrix composite, only have and prepare about CVI technique the research report that oxide fibre strengthens carbon/silicon carbide ceramic matrix composite on a small quantity, result shows: this material system has excellent mechanical property and antioxidant property, but CVI technique preparation cycle reaches hundreds of hours usually, and production efficiency is lower.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the deficiency and defect mentioned in above background technology, provides all excellent sapphire whisker fabric containing interfacial phase of a kind of mechanical property, antioxidant property and high-temperature behavior to strengthen silicon carbide and (is abbreviated as Al
2o
3f/ SiC) pottery, and correspondingly provide that a kind of preparation cycle is short, cost is low, can the preparation method of this pottery of near-net-shape.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is that a kind of sapphire whisker fabric containing interfacial phase strengthens silicon carbide ceramics, described pottery is using sapphire whisker fabric as reinforcement, using silicon carbide ceramics as matrix, and between reinforcement and matrix, be formed with sacrifice carbon interfacial phase.Have more feature, sacrifice carbon interfacial phase of the present invention is that first the obtained sapphire whisker fabric containing cracking carbon interfacial phase strengthens silicon carbide ceramics after precursor infiltration and pyrolysis technique, then obtain after high-temperature heat treatment sacrifice cracking carbon interfacial phase.
The above-mentioned sapphire whisker fabric containing interfacial phase strengthens silicon carbide ceramics, preferred: the flexural strength of described pottery is at more than 150MPa, and the flexural strength rangeability after 1000 DEG C of high temperature oxidation 2h is no more than 5%; The Young's modulus of described pottery is at more than 75GPa, and the elastic modulus change amplitude after 1000 DEG C of high temperature oxidation 2h is no more than 5%.
As a total technical conceive, the present invention also provides a kind of above-mentioned sapphire whisker fabric containing interfacial phase to strengthen the preparation method of silicon carbide ceramics, comprises following processing step:
(1) fabric pre-treatment: sapphire whisker fabric is placed in retort furnace and carries out high temperature oxidation, to remove surface glue and impurity;
(2) fabric surface Pyrolytic carbon coating preparation: utilize the sapphire whisker fabric face deposition Pyrolytic carbon coating that chemical vapour deposition (CVD) technique obtains in step (1);
(3) precursor solution preparation: take Polycarbosilane and dimethylbenzene by proportioning, for subsequent use after mixing and stirring;
(4) matrix densification: the sapphire whisker fabric obtained after the precursor solution vacuum impregnation step (2) obtained with step (3), then takes out and dries, complete a densification process after crosslinked at low temperature and pyroceramic;
(5) densification repeatedly: repeat above-mentioned steps (4) at least 10 times (preferably 10 ~ 15 times), the obtained sapphire whisker fabric containing cracking carbon interfacial phase strengthens silicon carbide ceramics;
(6) oxide treatment: the sapphire whisker fabric containing cracking carbon interfacial phase above-mentioned steps (5) obtained strengthens silicon carbide ceramics and is placed in retort furnace, by high temperature oxidation to sacrifice cracking carbon interfacial phase, between sapphire whisker fabric and silicon carbide ceramics matrix, form gap, the obtained sapphire whisker fabric containing interfacial phase strengthens silicon carbide ceramics.
Above-mentioned preparation method, preferably, in described step (1), described sapphire whisker fabric is that 2.5D structure, three-dimensional four-way structure, three-dimensional five are to structure, three-dimensional six to structure or three-dimensional orthogonal structure; In described sapphire whisker fabric, fiber volume fraction is 35% ~ 50%.The more fabrics that can only be suitable for one dimension, two dimension of existing most of technique, and adopt the preparation method of invention can realize the near-net-shape of three-dimensional aluminum oxide fabric enhancing silicon carbide ceramics better.
Above-mentioned preparation method, preferably, in described step (1), the technological process of described high temperature oxidation is: sapphire whisker fabric is put into retort furnace, 600 DEG C ~ 800 DEG C are risen in atmosphere with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min, insulation 1h ~ 3h, naturally cools to less than 100 DEG C taking-ups.
Above-mentioned preparation method, preferably, in described step (2), the Parameter Conditions of institute's chemical vapor deposition method comprises: unstripped gas is propylene and argon gas, depositing temperature is 900 DEG C ~ 1100 DEG C, deposition pressure is 1kPa ~ 3kPa, and propylene and argon gas stream speed ratio are 1: 1 ~ 1: 3, and depositing time is 1h ~ 5h.
Above-mentioned preparation method, preferably, in described step (3), the mass ratio of described Polycarbosilane and dimethylbenzene is 1: 0.8 ~ 1: 1.2.
Above-mentioned preparation method, preferably, in described step (4), the described vacuum impregnation time is 4h ~ 8h, and flash-off time is 2h ~ 5h.
Above-mentioned preparation method, preferably, in described step (4), described crosslinked at low temperature adopts oven drying mode to complete, its technological process is: the sapphire whisker fabric after drying is put into convection oven, rise to 160 DEG C ~ 200 DEG C with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min in atmosphere, insulation 3h ~ 6h, naturally cools to room temperature.
Above-mentioned preparation method, preferably, in described step (4), described pyroceramic adopts the mode of Pintsch process to complete, its technological process is: the sapphire whisker fabric after crosslinked at low temperature is put into pyrolyzer, in argon gas, rise to 900 DEG C ~ 1100 DEG C with the temperature rise rate of 10 DEG C/min ~ 15 DEG C/min, insulation 0.5h ~ 2h, naturally cools to less than 100 DEG C taking-ups.
Above-mentioned preparation method, preferably, in described step (6), described high-temperature heat treatment refers to: rise to 600 DEG C ~ 800 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min in atmosphere, and insulation 1h ~ 2h, naturally cools to less than 100 DEG C taking-ups.
Technique scheme of the present invention passes through reasonably INTERFACE DESIGN, and high performance sapphire whisker fabric strengthens carbon/silicon carbide ceramic matrix composite to have adopted PIP technique to prepare, and this is for the expansion of high-temperature hot structure function material, and tool is of great significance.
Compared with prior art, the invention has the advantages that:
1. the Al containing interfacial phase of the present invention
2o
3fthe preparation method of/SiC ceramic be vapor phase process in conjunction with liquid phase method, pressureless sintering can prepare SiC ceramic matrix at a lower temperature, preparation cycle is shorter;
2. in preparation method of the present invention, adopt that CVD technique is high in sapphire whisker fabric face pre-deposition Pyrolytic carbon coating degree of crystallinity, thickness evenness good, can effectively inhibited oxidation aluminum fiber and the diffusion reaction of matrix in matrix material preparation process, thus weaken interface cohesion; And oxidation can leave uniform gap after sacrificing between sapphire whisker and matrix, effectively improve the Al containing interfacial phase
2o
3fthe thermal structure stability of/SiC ceramic;
3. preparation method of the present invention is by the appropriate design of fibrage mode, can also prepare baroque component, and product design size controls by numerically-controlled machine precision machining.
All in all, the present invention obtain containing the Al of interfacial phase
2o
3f/ SiC ceramic, has the common advantage of general ceramic matric composite, as low density and excellent mechanical property etc.In addition, with C
f/ SiC and SiC
f/ SiC ceramic is compared, the Al containing interfacial phase of the present invention
2o
3f/ SiC ceramic has more excellent antioxidant property; The Al prepared with CVI technique
2o
3f/ SiC ceramic is compared, the Al containing interfacial phase of the present invention
2o
3fthe pyroprocessing time of/SiC ceramic is shorter, less to the thermal damage of fiber, and without the need to special equipment, production efficiency is higher and cost is lower.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is Al obtained in the embodiment of the present invention 1
2o
3fexemplary bent intensity-the displacement curve of/SiC ceramic.
Fig. 2 is the section microscopic appearance figure of control sample obtained in the embodiment of the present invention 1.
Fig. 3 is Al obtained in the embodiment of the present invention 1
2o
3fthe section microscopic appearance figure of/SiC ceramic.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Unless otherwise specified, the various starting material, reagent, instrument and equipment etc. used in the present invention are all bought by market and are obtained or prepare by existing method.
Embodiment 1:
Sapphire whisker fabric containing interfacial phase of the present invention strengthens a silicon carbide ceramics, and it is using sapphire whisker fabric as reinforcement, using silicon carbide ceramics as matrix, and is formed with sacrifice carbon interfacial phase between reinforcement and matrix.
The present embodiment, containing the preparation method of the sapphire whisker fabric enhancing silicon carbide ceramics of interfacial phase, specifically comprises following processing step:
(1) fabric pre-treatment: by fiber volume fraction be 40% three-dimensional orthogonal sapphire whisker fabric be placed in retort furnace, 600 DEG C are risen in atmosphere with the temperature rise rate of 10 DEG C/min, insulation 2h, naturally cools to less than 100 DEG C taking-ups, to remove surface glue and impurity;
(2) fabric surface Pyrolytic carbon coating preparation: utilize the fabric surface deposition Pyrolytic carbon coating that chemical vapor deposition method (CVD) obtains in step (1), CVD processing parameter comprises: unstripped gas is propylene and argon gas, depositing temperature is 960 DEG C, deposition pressure is 1kPa, propylene and argon gas stream speed ratio are 1: 1, and depositing time is 5h;
(3) precursor solution preparation: take Polycarbosilane and dimethylbenzene at 1: 1 in mass ratio, for subsequent use after mixing and stirring;
(4) matrix densification: the sapphire whisker fabric that the precursor solution vacuum impregnation step (2) obtained with step (3) obtains, takes out after vacuum impregnation 6h and hangs 3h; Sapphire whisker fabric after drying is put into convection oven and carries out crosslinked at low temperature, rise to 180 DEG C in atmosphere with the temperature rise rate of 3 DEG C/min, insulation 4h, naturally cools to room temperature; Sapphire whisker fabric after crosslinked at low temperature is put into pyrolyzer, in argon gas, rises to 1000 DEG C with the temperature rise rate of 10 DEG C/min, insulation 1h, naturally cools to less than 100 DEG C taking-ups; Complete a densification process;
(5) densification repeatedly: repeat above-mentioned steps (4) 13 times, the obtained sapphire whisker fabric containing cracking carbon interfacial phase strengthens silicon carbide ceramics;
(6) high-temperature heat treatment: the sapphire whisker fabric containing cracking carbon interfacial phase above-mentioned steps (5) obtained strengthens silicon carbide ceramics and is placed in retort furnace, 600 DEG C are risen in atmosphere with the temperature rise rate of 8 DEG C/min, insulation 2h, naturally cool to less than 100 DEG C taking-ups, the obtained sapphire whisker fabric containing sacrificing carbon interfacial phase strengthens silicon carbide ceramics.
The Al sacrificing carbon interfacial phase is not contained according to the method preparation of the present embodiment
2o
3f/ SiC ceramic is sample (namely without the need to preparing Pyrolytic carbon coating on sapphire whisker fabric, also without the need to carrying out follow-up high-temperature heat treatment to sacrifice cracking carbon interfacial phase) in contrast, to the Al containing interfacial phase that above-mentioned the present embodiment obtains
2o
3f/ SiC ceramic and aforementioned control sample carry out mechanical property contrast test, and typical load-displacement curves as shown in Figure 1.As seen from Figure 1, control sample shows brittle rupture behavior, and the Al containing interfacial phase of the present embodiment
2o
3f/ SiC ceramic shows obvious ductile rupture behavior, when load reach maximum after reduce gradually, the present embodiment containing the Al of interfacial phase
2o
3fthe flexural strength of/SiC ceramic is about 4 times of control sample.
In addition, as shown in Figure 2, as seen from Figure 2, section is comparatively smooth for the section microscopic appearance of control sample prepared by the present embodiment, does not observe interfacial detachment and spike protein gene phenomenon, and show that in control sample, fiber/matrix interface cohesion is comparatively strong, the reinforced effects of fiber is not remarkable.And the Al containing interfacial phase prepared by the present embodiment
2o
3fthe section microscopic appearance of/SiC ceramic as shown in Figure 3, obvious interfacial detachment and spike protein gene phenomenon can be observed by Fig. 3, this shows that the introducing of sacrificing carbon interfacial phase can weaken fiber/matrix interface cohesion, and the reinforced effects of fiber is comparatively remarkable, and this is also the Al containing interfacial phase prepared by the present invention
2o
3fthe essential reason of/SiC ceramic excellent in mechanical performance.
Al containing interfacial phase obtained above
2o
3fthe Specifeca tion speeification of/SiC ceramic is as shown in table 1.
Table 1: the Al of preparation in embodiment 1
2o
3fthe Specifeca tion speeification of/SiC ceramic
Embodiment 2:
Sapphire whisker fabric containing interfacial phase of the present invention strengthens a silicon carbide ceramics, and it is using sapphire whisker fabric as reinforcement, using silicon carbide ceramics as matrix, and is formed with sacrifice carbon interfacial phase between reinforcement and matrix.
The present embodiment, containing the preparation method of the sapphire whisker fabric enhancing silicon carbide ceramics of interfacial phase, specifically comprises following processing step:
(1) fabric pre-treatment: by fiber volume fraction be 45% three-dimensional four-way sapphire whisker fabric be placed in retort furnace, 700 DEG C are risen in atmosphere with the temperature rise rate of 8 DEG C/min, insulation 1h, naturally cools to less than 100 DEG C taking-ups, to remove surface glue and impurity;
(2) fabric surface Pyrolytic carbon coating preparation: utilize the fabric surface deposition Pyrolytic carbon coating that chemical vapor deposition method (CVD) obtains in step (1), CVD processing parameter comprises: unstripped gas is propylene and argon gas, depositing temperature is 1050 DEG C, deposition pressure is 2kPa, propylene and argon gas stream speed ratio are 1: 2, and depositing time is 2h;
(3) precursor solution preparation: take Polycarbosilane and dimethylbenzene at 1: 0.8 in mass ratio, for subsequent use after mixing and stirring;
(4) matrix densification: the sapphire whisker fabric that the precursor solution vacuum impregnation step (2) obtained with step (3) obtains, takes out after vacuum impregnation 4h and hangs 4h; Sapphire whisker fabric after drying is put into convection oven and carries out crosslinked at low temperature, rise to 160 DEG C in atmosphere with the temperature rise rate of 5 DEG C/min, insulation 6h, naturally cools to room temperature; Sapphire whisker fabric after crosslinked at low temperature is put into pyrolyzer, in argon gas, rises to 1050 DEG C with the temperature rise rate of 15 DEG C/min, insulation 0.5h, naturally cools to less than 100 DEG C taking-ups; Complete a densification process;
(5) densification repeatedly: repeat above-mentioned steps (4) 10 times, the obtained sapphire whisker fabric containing cracking carbon interfacial phase strengthens silicon carbide ceramics;
(6) high-temperature heat treatment: the sapphire whisker fabric containing cracking carbon interfacial phase above-mentioned steps (5) obtained strengthens silicon carbide ceramics and is placed in retort furnace, 700 DEG C are risen in atmosphere with the temperature rise rate of 10 DEG C/min, insulation 1h, naturally cool to less than 100 DEG C taking-ups, the obtained sapphire whisker fabric containing sacrificing carbon interfacial phase strengthens silicon carbide ceramics.
The Al sacrificing carbon interfacial phase is not contained according to the method preparation of the present embodiment
2o
3f/ SiC ceramic is sample (namely without the need to preparing Pyrolytic carbon coating on sapphire whisker fabric, also without the need to carrying out follow-up high-temperature heat treatment to sacrifice cracking carbon interfacial phase) in contrast, to the Al containing interfacial phase that above-mentioned the present embodiment obtains
2o
3f/ SiC ceramic and aforementioned control sample carry out mechanical property contrast test, the Al containing interfacial phase obtained
2o
3fthe Specifeca tion speeification of/SiC ceramic is as shown in table 2.
Table 2: the Al of preparation in embodiment 2
2o
3fthe Specifeca tion speeification of/SiC ceramic
In addition, the section microscopic appearance display section of above-mentioned control sample is comparatively smooth, does not observe interfacial detachment and spike protein gene phenomenon, and show that in control sample, fiber/matrix interface cohesion is comparatively strong, the reinforced effects of fiber is not remarkable.And the Al containing interfacial phase prepared by the present embodiment
2o
3fobvious interfacial detachment and spike protein gene phenomenon can be observed in the section microscopic appearance of/SiC ceramic, this shows that the introducing of sacrificing carbon interfacial phase can weaken fiber/matrix interface cohesion, the reinforced effects of fiber is comparatively remarkable, and this is also the Al containing interfacial phase prepared by the present invention
2o
3fthe essential reason of/SiC ceramic excellent in mechanical performance.
Therefore the sapphire whisker fabric containing interfacial phase of the present invention strengthens the flexural strength of silicon carbide ceramics at more than 150MPa, and the flexural strength rangeability after 1000 DEG C of high temperature oxidation 2h is no more than 5%; The Young's modulus of pottery is at more than 75GPa, and the elastic modulus change amplitude after 1000 DEG C of high temperature oxidation 2h is no more than 5%.
Claims (10)
1. the sapphire whisker fabric containing interfacial phase strengthens a silicon carbide ceramics, it is characterized in that: described pottery is using sapphire whisker fabric as reinforcement, using silicon carbide ceramics as matrix, and is formed with sacrifice carbon interfacial phase between reinforcement and matrix.
2. the sapphire whisker fabric containing interfacial phase according to claim 1 strengthens silicon carbide ceramics, it is characterized in that: the flexural strength of described pottery is at more than 150MPa, and the flexural strength rangeability after 1000 DEG C of high temperature oxidation 2h is no more than 5%; The Young's modulus of described pottery is at more than 75GPa, and the elastic modulus change amplitude after 1000 DEG C of high temperature oxidation 2h is no more than 5%.
3., as claimed in claim 1 or 2 containing a preparation method for the sapphire whisker fabric enhancing silicon carbide ceramics of interfacial phase, comprise following processing step:
(1) fabric pre-treatment: sapphire whisker fabric is placed in retort furnace and carries out high temperature oxidation, to remove surface glue and impurity;
(2) fabric surface Pyrolytic carbon coating preparation: utilize the sapphire whisker fabric face deposition Pyrolytic carbon coating that chemical vapor deposition method obtains in step (1);
(3) precursor solution preparation: take Polycarbosilane and dimethylbenzene by proportioning, for subsequent use after mixing and stirring;
(4) matrix densification: the sapphire whisker fabric obtained after the precursor solution vacuum impregnation step (2) obtained with step (3), then takes out and dries, complete a densification process after crosslinked at low temperature and pyroceramic;
(5) densification repeatedly: repeat above-mentioned steps (4) at least 10 times, the obtained sapphire whisker fabric containing cracking carbon interfacial phase strengthens silicon carbide ceramics;
(6) high-temperature heat treatment: the sapphire whisker fabric containing cracking carbon interfacial phase above-mentioned steps (5) obtained strengthens silicon carbide ceramics and is placed in retort furnace, by high-temperature heat treatment to sacrifice cracking carbon interfacial phase, between sapphire whisker fabric and silicon carbide ceramics matrix, form gap, the obtained sapphire whisker fabric containing interfacial phase strengthens silicon carbide ceramics.
4. preparation method according to claim 3, is characterized in that, in described step (1): described sapphire whisker fabric is that 2.5D structure, three-dimensional four-way structure, three-dimensional five are to structure, three-dimensional six to structure or three-dimensional orthogonal structure; In described sapphire whisker fabric, fiber volume fraction is 35% ~ 50%.
5. preparation method according to claim 3, it is characterized in that, in described step (1): the technological process of described high temperature oxidation is: sapphire whisker fabric is put into retort furnace, 600 DEG C ~ 800 DEG C are risen in atmosphere with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min, insulation 1h ~ 3h, naturally cools to less than 100 DEG C taking-ups.
6. preparation method according to claim 3, it is characterized in that, in described step (2): the Parameter Conditions of institute's chemical vapor deposition method comprises: unstripped gas is propylene and argon gas, depositing temperature is 900 DEG C ~ 1100 DEG C, deposition pressure is 1kPa ~ 3kPa, propylene and argon gas stream speed ratio are 1: 1 ~ 1: 3, and depositing time is 1h ~ 5h.
7. preparation method according to claim 3, is characterized in that, in described step (3): the mass ratio of described Polycarbosilane and dimethylbenzene is 1: 0.8 ~ 1: 1.2.
8. the preparation method according to any one of claim 3 ~ 7, is characterized in that, in described step (4): the described vacuum impregnation time is 4h ~ 8h, and flash-off time is 2h ~ 5h; Described crosslinked at low temperature adopts oven drying mode to complete, its technological process is: the sapphire whisker fabric after drying is put into convection oven, rise to 160 DEG C ~ 200 DEG C with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min in atmosphere, insulation 3h ~ 6h, naturally cools to room temperature.
9. the preparation method according to any one of claim 3 ~ 7, it is characterized in that, in described step (4): described pyroceramic adopts the mode of Pintsch process to complete, its technological process is: the sapphire whisker fabric after crosslinked at low temperature is put into pyrolyzer, 900 DEG C ~ 1100 DEG C are risen to the temperature rise rate of 10 DEG C/min ~ 15 DEG C/min in argon gas, insulation 0.5h ~ 2h, naturally cools to less than 100 DEG C taking-ups.
10. the preparation method according to any one of claim 3 ~ 7, it is characterized in that, in described step (6), described high-temperature heat treatment refers to: rise to 600 DEG C ~ 800 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min in atmosphere, insulation 1h ~ 2h, naturally cools to less than 100 DEG C taking-ups.
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| CN106966743A (en) * | 2016-06-03 | 2017-07-21 | 北京航空航天大学 | A kind of preparation method of continuous lod thermal structure material compound interface layer |
| CN108484135A (en) * | 2018-04-17 | 2018-09-04 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ ceramics reinforcing fiber resin composite materials |
| CN110282993A (en) * | 2019-08-06 | 2019-09-27 | 山东道普安制动材料有限公司 | A kind of preparation method of the ceramic matric composite of the phase containing interface |
| CN110983757A (en) * | 2019-12-04 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Method for modifying fiber interface of alumina fiber cloth and modified alumina fiber cloth prepared by method |
| CN114853490A (en) * | 2022-03-20 | 2022-08-05 | 西北工业大学 | SiC/SiC ceramic composite material with excellent formability and good mechanical property and preparation method thereof |
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