CN104926345A - Alumina fiber-reinforced silicon carbide-aluminum silicate ceramic and preparation method thereof - Google Patents

Alumina fiber-reinforced silicon carbide-aluminum silicate ceramic and preparation method thereof Download PDF

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CN104926345A
CN104926345A CN201510266750.8A CN201510266750A CN104926345A CN 104926345 A CN104926345 A CN 104926345A CN 201510266750 A CN201510266750 A CN 201510266750A CN 104926345 A CN104926345 A CN 104926345A
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silicon carbide
aluminum silicate
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CN104926345B (en
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王�义
程海峰
刘海韬
王军
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National University of Defense Technology
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Abstract

The invention discloses alumina fiber-reinforced silicon carbide-aluminum silicate ceramic. An alumina fiber fabric serves as a reinforcement body, silicon carbide ceramic and aluminum silicate ceramic serve as a base body, the silicon carbide ceramic is mainly molded by using a chemical gas-phase permeation method, and the aluminum silicate ceramic is introduced through a sol-gel process. A preparation method comprises the following steps: preparing an Al2O3f/SiC ceramic blank from raw materials including the alumina fiber fabric, trichloromethyl silane, hydrogen and argon by using the chemical gas-phase permeation method; machining the surface of the prepared ceramic blank, and changing a great number of closed holes in the surface into open holes; performing vacuum impregnation on the ceramic blank by using silicon-aluminum composite sol, and transforming the ceramic blank into an intermediate product through gelation and high-temperature ceramization; repeatedly executing the steps for at least four times to obtain the alumina fiber-reinforced silicon carbide-aluminum silicate ceramic finally. The mechanical property, the high temperature resistance and the oxidation resistance of the alumina fiber-reinforced silicon carbide-aluminum silicate ceramic are excellent, the preparation period is short, the cost is low, and clear dimension molding can be achieved.

Description

A kind of sapphire whisker strengthens silicon carbide-aluminum silicate ceramic and preparation method thereof
Technical field
The present invention relates to fiber reinforcedceramics field, particularly relate to a kind of silicon carbide fiber reinforced-aluminum silicate ceramic and preparation method thereof.
Background technology
Oxide fibre strengthens silicon carbide ceramics and has excellent mechanical property, dielectric properties, antioxidant property and environmental resistance, is the important thermal structure functional materials of a class.But the high temperature environmental resistance of silicon carbide is poor, losing efficacy as easily there is oxidation in the water vapour environment of high temperature aerobic, significantly limit its application.
At present, the preparation technology of oxide fibre enhancing silicon carbide ceramics mainly contains precursor pyrolysis and hot pressing (PIP) and chemical vapor infiltration (CVI).PIP method sintering temperature is low, matrix designability is strong, can near-net-shape, but material porosity prepared by PIP is higher, fibre-tendering is comparatively large and fiber/matrix interface cohesion is stronger.In addition, usually containing uncombined carbon and glassy phase SiO in the SiC ceramic that PIP legal system is standby xc ydeng impurity, its antioxidant property is not as good as pure SiC ceramic.CVI method preparation temperature SiC matrix purity that is low, that obtain is higher, also can near-net-shape.But in CVI preparation process, the matrix cracking that generation and thermal mismatching due to defect cause can make its antioxidant property greatly reduce.By matrix modification and rear densification, improve matrix material density further, the antioxidant property of SiC matrix can be improved to a certain extent.
We utilize PIP technique to prepare sapphire whisker enhancing silicon carbide (Al in earlier stage 2o 3f/ SiC) ceramic matric composite, be studied its mechanical property and microscopic appearance, result shows: without the Al of interface modification 2o 3fin/SiC ceramic matrix composite material, fiber/matrix interface cohesion is comparatively strong, and show brittle rupture behavior, flexural strength is only 42.8MPa.In addition, CVI technique is also utilized to prepare Al 2o 3f/ SiC ceramic matrix composite material, result of study shows: original position can form skim carbon coating between sapphire whisker and SiC matrix, thus weaken interface cohesion, the mechanical property of matrix material is more excellent, and flexural strength reaches 92.1MPa.But, owing to there is more hole and crackle in matrix, cause the antioxidant property of matrix material undesirable.
Summary of the invention
Technical problem to be solved by this invention is, overcome the deficiency and defect mentioned in above background technology, there is provided a kind of mechanical property, the sapphire whisker that high temperature resistant and antioxidant property is excellent to strengthen silicon carbide-aluminum silicate ceramic, and correspondingly provide that a kind of preparation cycle is short, cost is low, this sapphire whisker of near-net-shape can strengthen the preparation method of silicon carbide-aluminum silicate ceramic.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is that a kind of sapphire whisker strengthens silicon carbide-aluminum silicate ceramic (abbreviation Al 2o 3f/ SiC-AS), described pottery is with sapphire whisker fabric (Al 2o 3f) as reinforcement, using silicon carbide ceramics (SiC) and aluminum silicate ceramic (AS) as matrix, described silicon carbide ceramics mainly adopts that chemical vapor infiltration is shaping to be obtained, and described aluminum silicate ceramic is introduced by sol-gel technology.
Above-mentioned sapphire whisker strengthens silicon carbide-aluminum silicate ceramic, preferred: described matrix comprises the silicon carbide ceramics of 20% ~ 40% volume fraction (accounting for the volume fraction that whole sapphire whisker strengthens silicon carbide-aluminum silicate ceramic, lower same) and the aluminum silicate ceramic (remaining volumetric spaces is mainly hole) of 10% ~ 20% volume fraction.
Above-mentioned sapphire whisker strengthens silicon carbide-aluminum silicate ceramic, preferred: the flexural strength of described pottery is at more than 125MPa, and the flexural strength after the high temperature oxidation 100h of 1000 DEG C is at more than 110MPa; The Young's modulus of described pottery is at more than 70GPa, and the Young's modulus after the high temperature oxidation 100h of 1000 DEG C is at more than 60GPa.
As a total technical conceive, the present invention also provides a kind of above-mentioned sapphire whisker to strengthen the preparation method of silicon carbide-aluminum silicate ceramic, comprises following processing step:
(1) Al 2o 3fthe preparation of/SiC ceramic base substrate: with sapphire whisker fabric, trichloromethyl silane, hydrogen, argon gas for raw material, adopts chemical vapor infiltration (CVI) to prepare Al 2o 3f/ SiC ceramic base substrate;
(2) Al 2o 3fthe processing of/SiC ceramic base substrate: the Al obtained to above-mentioned steps (1) 2o 3f/ SiC ceramic base substrate carries out surface working, and a large amount of closed pores on surface are become perforate so that carry out subsequent densification;
(3) AS pottery subsequent densification: utilize the Al after sial complex sol vacuum impregnation above-mentioned steps (2) 2o 3f/ SiC ceramic base substrate, changes intermediates into after gelation, pyroceramic;
(4) repeat the process at least 4 times (preferably 4 ~ 8 times) of above-mentioned steps (3), final obtained sapphire whisker strengthens silicon carbide-aluminum silicate ceramic.
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% ~ 45%.
Above-mentioned preparation method, preferably, in described step (1), the processing parameter condition of described chemical vapor infiltration comprises: depositing temperature is 1000 DEG C ~ 1200 DEG C, deposition pressure is 1kPa ~ 5kPa, and hydrogen and argon gas stream speed ratio are 3:1 ~ 1:1, and depositing time is 6h ~ 10h.
Above-mentioned preparation method, preferably, in described step (3), described vacuum-impregnated technological process comprises: utilize Al described in the vacuum impregnation of sial complex sol 2o 3f/ SiC ceramic base substrate 4h ~ 8h, then takes out and hangs 1h ~ 2h in atmosphere; The solid content of described sial complex sol is 18.2wt% ~ 25.3wt%.
Above-mentioned preparation method, preferably, in described step (3), described gelation adopts drying mode to complete, its drying process comprises: the ceramic body after vacuum impregnation is put into baking oven, be warming up to 150 DEG C ~ 200 DEG C, dry 4h ~ 6h with the temperature rise rate of 2 DEG C/min ~ 3 DEG C/min, then naturally cool to room temperature and take out.
Above-mentioned preparation method, preferably, in described step (3), described pyroceramic adopts the mode of Pintsch process to complete, its concrete technological process comprises: the ceramic body after described gelation is put into pyrolyzer, rise to 900 DEG C ~ 1100 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min in atmosphere, insulation 0.5h ~ 1.5h, naturally cools to less than 100 DEG C taking-ups.
The present invention mainly follows following technical thought: the Al not changing CVI technique and prepare 2o 3funder the prerequisite of/SiC ceramic matrix composite material performance, by carrying out modification and subsequent densification process to matrix, to make the crack defect in matrix further up, and then promote mechanical property and the antioxidant property of matrix material.In concrete preparation process, first we prepare Al by CVI technique 2o 3f/ SiC ceramic base substrate, then with sial complex sol for precursor, adopt sol-gel technology to Al 2o 3f/ SiC ceramic base substrate carries out rear densification, and the sapphire whisker of obtained mechanical property and antioxidant property excellence strengthens silicon carbide-aluminum silicate ceramic.
Compared with prior art, the invention has the advantages that:
1. Al of the present invention 2o 3fthe preparation method of/SiC-AS pottery be vapor phase process in conjunction with liquid phase method, pressureless sintering at a lower temperature can prepare SiC-AS ceramic matrix, preparation cycle is short;
2. method of the present invention prepares baroque component by fibrage mode, and product design size controls by numerically-controlled machine precision machining; The raw material chosen extensively is easy to get, and can be widely used in suitability for industrialized production.
Al of the present invention 2o 3f/ SiC-AS pottery, has the common advantage of general ceramic matric composite, as high specific strength and specific modulus, excellent thermal shock resistance etc.In addition, with C f/ SiC, SiC f/ SiC and Al 2o 3f/ SiC ceramic based composites is compared, Al of the present invention 2o 3f/ SiC-AS pottery has more excellent antioxidant property and environmental resistance.
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 3fthe optical photograph of/SiC-AS pottery.
Fig. 2 is Al obtained in the embodiment of the present invention 1 2o 3fthe energy spectrum analysis of matrix in/SiC-AS pottery.
Fig. 3 is Al obtained in the embodiment of the present invention 1 2o 3fthe microscopic appearance figure of/SiC-AS pottery.
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:
One as shown in Figure 1 sapphire whisker enhancing silicon carbide-aluminum silicate ceramic of the present invention (is abbreviated as Al 2o 3f/ SiC-AS), comprise the sapphire whisker of 41% volume fraction of having an appointment, the SiC ceramic of about 33% volume fraction and the AS pottery of about 12% volume fraction.
One prepares above-mentioned the present embodiment Al 2o 3fthe method of/SiC-AS pottery, specifically comprises the following steps:
(1) Al 2o 3fthe preparation of/SiC ceramic base substrate: with three-dimensional orthogonal sapphire whisker fabric be reinforcement, trichloromethyl silane-hydrogen-argon for raw material, adopt CVI prepare Al 2o 3f/ SiC ceramic base substrate; CVI processing parameter is: depositing temperature is 1100 DEG C, deposition pressure is 1.5kPa, hydrogen and argon gas stream speed ratio are 1.5: 1, depositing time is 10h;
(2) Al 2o 3fthe processing of/SiC ceramic base substrate: the Al obtained to above-mentioned steps (1) 2o 3f/ SiC ceramic base substrate carries out surface working, and a large amount of closed pores on surface are become perforate so that carry out subsequent densification;
(3) AS pottery subsequent densification: first, be that the sial complex sol of 19.5wt% is precursor with solid content, the Al obtained to above-mentioned steps (2) 2o 3f/ SiC ceramic base substrate carries out vacuum impregnation 6h, takes out and hangs 2h in atmosphere; Then, the ceramic body after vacuum impregnation is put into baking oven and carries out gelation process, be warming up to 200 DEG C with the temperature rise rate of 2 DEG C/min, dry 5h, naturally cool to room temperature and take out; Finally, the ceramic body after gelation is put into pyrolyzer, rise to 1000 DEG C in atmosphere with the temperature rise rate of 8 DEG C/min, insulation 1h, naturally cools to less than 100 DEG C taking-ups;
(4) above-mentioned steps (3) 4 times are repeated, obtained Al 2o 3f/ SiC-AS pottery.
Through the Al of the present embodiment that above-mentioned steps obtains 2o 3fthe optical photograph of/SiC-AS pottery as shown in Figure 1, its matrix energy spectrum analysis as shown in Figure 2, as seen from Figure 2, Al prepared by the present embodiment 2o 3fcontaining C, Si, Al and O element in/SiC-AS ceramic matrix, consistent with element contained by SiC and AS.
Al prepared by the present embodiment 2o 3fthe Cross Section Morphology of/SiC-AS pottery as shown in Figure 3, as seen from Figure 3, Al 2o 3fin/SiC-AS ceramic composite there is a small amount of micropore in synnema inside, and hole between synnema is larger; In addition, the interface between fiber and matrix is comparatively clear, shows that the consistency of fiber and matrix is better.
With reference to the processing parameter condition of above-mentioned the present embodiment, CVI technique is adopted to prepare Al 2o 3f/ SiC ceramic is sample 1 in contrast; Meanwhile, utilize sial complex sol densify aluminum fiber fabric, preparation Al 2o 3f/ AS pottery is sample 2 in contrast.To the Al that above-mentioned the present embodiment obtains 2o 3f/ SiC-AS pottery and control sample carry out mechanical property contrast test, obtain Specifeca tion speeification as shown in table 1 below.
Table 1: the Specifeca tion speeification of three kinds of matrix materials that contrast test obtains in embodiment 1
Embodiment 2:
A kind of sapphire whisker of the present invention strengthens silicon carbide-aluminum silicate ceramic and (is abbreviated as Al 2o 3f/ SiC-AS), comprise the sapphire whisker of 43% volume fraction of having an appointment, the SiC ceramic of about 25% volume fraction and the AS pottery of about 18% volume fraction.
One prepares above-mentioned the present embodiment Al 2o 3fthe method of/SiC-AS pottery, specifically comprises the following steps:
(1) Al 2o 3fthe preparation of/SiC ceramic base substrate: with three-dimensional orthogonal sapphire whisker fabric be reinforcement, trichloromethyl silane-hydrogen-argon for raw material, adopt CVI prepare Al 2o 3f/ SiC ceramic base substrate; CVI processing parameter is: depositing temperature is 1050 DEG C, deposition pressure is 2kPa, hydrogen and argon gas stream speed ratio are 2: 1, depositing time is 8h;
(2) Al 2o 3fthe processing of/SiC ceramic base substrate: the Al obtained to above-mentioned steps (1) 2o 3f/ SiC ceramic base substrate carries out surface working, and a large amount of closed pores on surface are become perforate so that carry out subsequent densification;
(3) AS pottery subsequent densification: first, be that the sial complex sol of 21.2wt% is precursor with solid content, the Al obtained to above-mentioned steps (2) 2o 3f/ SiC ceramic base substrate carries out vacuum impregnation 7h, takes out and hangs 1.5h in atmosphere; Then, the ceramic body after vacuum impregnation is put into baking oven and carries out gelation process, be warming up to 180 DEG C with the temperature rise rate of 2.5 DEG C/min, dry 6h, naturally cool to room temperature and take out; Finally, the ceramic body after gelation is put into pyrolyzer, rise to 1050 DEG C in atmosphere with the temperature rise rate of 10 DEG C/min, insulation 0.5h, naturally cools to less than 100 DEG C taking-ups;
(4) above-mentioned steps (3) 6 times are repeated, obtained Al 2o 3f/ SiC-AS pottery.
With reference to the processing parameter condition of above-mentioned the present embodiment, CVI technique is adopted to prepare Al 2o 3f/ SiC ceramic is sample 1 in contrast; Meanwhile, utilize sial complex sol densify aluminum fiber fabric, preparation Al 2o 3f/ AS pottery is sample 2 in contrast.To the Al that above-mentioned the present embodiment obtains 2o 3f/ SiC-AS pottery and control sample carry out mechanical property contrast test, obtain Specifeca tion speeification as shown in table 2 below.
Table 2: the Specifeca tion speeification of three kinds of matrix materials that contrast test obtains in embodiment 2
Therefore the sapphire whisker that the invention described above obtains strengthens the flexural strength of silicon carbide-aluminum silicate ceramic at more than 129MPa, and the flexural strength after the high temperature oxidation 100h of 1000 DEG C is still at more than 115MPa; The Young's modulus of pottery is at more than 72GPa, and the Young's modulus after the high temperature oxidation 100h of 1000 DEG C is still at more than 61GPa.

Claims (9)

1. a sapphire whisker strengthens silicon carbide-aluminum silicate ceramic, it is characterized in that: described pottery is using sapphire whisker fabric as reinforcement, using silicon carbide ceramics and aluminum silicate ceramic as matrix, described silicon carbide ceramics mainly adopts that chemical vapor infiltration is shaping to be obtained, and described aluminum silicate ceramic is introduced by sol-gel technology.
2. sapphire whisker according to claim 1 strengthens silicon carbide-aluminum silicate ceramic, it is characterized in that: described matrix comprises the silicon carbide ceramics of 20% ~ 40% volume fraction and the aluminum silicate ceramic of 10% ~ 20% volume fraction.
3. sapphire whisker according to claim 1 and 2 strengthens silicon carbide-aluminum silicate ceramic, it is characterized in that: the flexural strength of described pottery is at more than 125MPa, and the flexural strength after the high temperature oxidation 100h of 1000 DEG C is at more than 110MPa; The Young's modulus of described pottery is at more than 70GPa, and the Young's modulus after the high temperature oxidation 100h of 1000 DEG C is at more than 60GPa.
4. as described in claim 1 or 2 or 3, sapphire whisker strengthens a preparation method for silicon carbide-aluminum silicate ceramic, comprises following processing step:
(1) Al 2o 3fthe preparation of/SiC ceramic base substrate: with sapphire whisker fabric, trichloromethyl silane, hydrogen, argon gas for raw material, adopts chemical vapor infiltration to prepare Al 2o 3f/ SiC ceramic base substrate;
(2) Al 2o 3fthe processing of/SiC ceramic base substrate: the Al obtained to above-mentioned steps (1) 2o 3f/ SiC ceramic base substrate carries out surface working, and a large amount of closed pores on surface are become perforate so that carry out subsequent densification;
(3) AS pottery subsequent densification: utilize the Al after sial complex sol vacuum impregnation above-mentioned steps (2) 2o 3f/ SiC ceramic base substrate, changes intermediates into after gelation, pyroceramic;
(4) repeat the process at least 4 times of above-mentioned steps (3), final obtained sapphire whisker strengthens silicon carbide-aluminum silicate ceramic.
5. preparation method according to claim 4, 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% ~ 45%.
6. the preparation method according to claim 4 or 5, it is characterized in that, in described step (1), the processing parameter condition of described chemical vapor infiltration comprises: depositing temperature is 1000 DEG C ~ 1200 DEG C, deposition pressure is 1kPa ~ 5kPa, hydrogen and argon gas stream speed ratio are 3: 1 ~ 1: 1, and depositing time is 6h ~ 10h.
7. preparation method according to claim 4, is characterized in that, in described step (3), described vacuum-impregnated technological process comprises: utilize Al described in the vacuum impregnation of sial complex sol 2o 3f/ SiC ceramic base substrate 4h ~ 8h, then takes out and hangs 1h ~ 2h in atmosphere; The solid content of described sial complex sol is 18.2wt% ~ 25.3wt%.
8. the preparation method according to claim 4 or 7, it is characterized in that, in described step (3), described gelation adopts drying mode to complete, its drying process comprises: the ceramic body after vacuum impregnation is put into baking oven, be warming up to 150 DEG C ~ 200 DEG C, dry 4h ~ 6h with the temperature rise rate of 2 DEG C/min ~ 3 DEG C/min, then naturally cool to room temperature and take out.
9. the preparation method according to claim 4 or 7, it is characterized in that, in described step (3), described pyroceramic adopts the mode of Pintsch process to complete, its concrete technological process comprises: the ceramic body after described gelation is put into pyrolyzer, rise to 900 DEG C ~ 1100 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min in atmosphere, insulation 0.5h ~ 1.5h, naturally cools to less than 100 DEG C taking-ups.
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CN105367105A (en) * 2015-11-27 2016-03-02 西北工业大学 Method for preparing thick-walled ceramic-matrix composite material through mechanical processing assisted CVI (Chemical Vapor Infiltration)
CN106977217A (en) * 2016-06-03 2017-07-25 北京航空航天大学 A kind of preparation method of high-strength and high-ductility silicon carbide fiber reinforced silicon carbide ceramic matric composite
CN107540385A (en) * 2017-09-01 2018-01-05 安徽青花坊瓷业股份有限公司 A kind of green compact leaching liquid for improving ceramics strength
CN115073212A (en) * 2022-06-02 2022-09-20 陕西美兰德炭素有限责任公司 Aluminum silicate-silicon carbide high-temperature-resistant and silicon vapor corrosion-resistant coating and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105367105A (en) * 2015-11-27 2016-03-02 西北工业大学 Method for preparing thick-walled ceramic-matrix composite material through mechanical processing assisted CVI (Chemical Vapor Infiltration)
CN106977217A (en) * 2016-06-03 2017-07-25 北京航空航天大学 A kind of preparation method of high-strength and high-ductility silicon carbide fiber reinforced silicon carbide ceramic matric composite
CN106977217B (en) * 2016-06-03 2018-05-04 北京航空航天大学 A kind of preparation method of high-strength and high-ductility silicon carbide fiber reinforced silicon carbide ceramic matric composite
CN107540385A (en) * 2017-09-01 2018-01-05 安徽青花坊瓷业股份有限公司 A kind of green compact leaching liquid for improving ceramics strength
CN115073212A (en) * 2022-06-02 2022-09-20 陕西美兰德炭素有限责任公司 Aluminum silicate-silicon carbide high-temperature-resistant and silicon vapor corrosion-resistant coating and preparation method thereof

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