CN107698269A - Infiltrate the method for silicones intensified ceramic core - Google Patents
Infiltrate the method for silicones intensified ceramic core Download PDFInfo
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- CN107698269A CN107698269A CN201710841786.3A CN201710841786A CN107698269A CN 107698269 A CN107698269 A CN 107698269A CN 201710841786 A CN201710841786 A CN 201710841786A CN 107698269 A CN107698269 A CN 107698269A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
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- B22C9/00—Moulds or cores; Moulding processes
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/52—Constituents or additives characterised by their shapes
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- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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Abstract
The invention discloses a kind of method for infiltrating silicones intensified ceramic core, the ceramic core for needing to strengthen is subjected to vacuum drying treatment, dried ceramic core is immersed in silicon resin solution, it is positioned in vacuum drying chamber and carries out being soaked in vacuum processing under room temperature condition, untill no longer bubble is produced in silicon resin solution, obtain the ceramic core after immersion treatment, the ceramic core of acquisition is subjected to low-temperature setting processing under atmospheric environment, high-temperature heat treatment is carried out under inert atmosphere conditions, obtains the fiber reinforced ceramic core cracked by silicones.The present invention changes to form SiOC fibers and SiC fibers under inert atmosphere conditions using silicones, due to this kind of fiber reinforcement phase be present in ceramic core matrix, its room temperature and high temperature power can be greatly enhanced, preparation technology of the present invention is simple, it is workable, with short production cycle, cost is cheap, and the ceramic core material strengthened has excellent room temperature and mechanical behavior under high temperature.
Description
Technical field
, should more particularly to a kind of method of intensified ceramic core the present invention relates to a kind of preparation method of ceramic core
For model casting, ceramic material prepares and high polymer material research field.
Background technology
It is well known that ceramic core material is the critical component for preparing hollow casting, the quality of its performance determines casting
Yield rate and performance.In particular with the development of aero-turbine and gas turbine, hollow high-temperature alloy blades are carried
Go out higher requirement, that is, require to prepare the high temperature blade of resistance to higher temperature, and one of key that this kind of blade is successfully prepared
It is to need to obtain the ceramic core with excellent performance.During the use of ceramic core, ceramic core needs to bear low
The high speed impact and mechanical external force of warm wax liquor are acted on and are not damaged by, it is also desirable to bear the impact of high-temperature liquid metal and high temperature gas flow
Effect is without deforming or damaged.This requires ceramic core to have very excellent room temperature and mechanical behavior under high temperature.
At present, the ceramic core that can be applied to prepare high-temperature alloy hollow blade is mainly based on silicon substrate and aluminium base.Silicon
Base ceramic core with excellent follow-up removing performance in terms of hollow blade preparation due to being widely applied, aluminium base pottery
Porcelain core with mechanical property more preferable than silicon substrate due to being used to prepare the higher high-temperature alloy hollow blade of temperature in use.
In order to further obtain the high temperature alloy or single crystal hollow blade with more operation at high temperature, by being injection moulded the silicon substrate prepared
Its performance still has much room for improvement with Al-base ceramic core.Therefore, room temperature and High-Temperature Strengthening are processed into further improve silicon substrate
With the necessary ways of Al-base ceramic core performance.Solidification can occur under cryogenic conditions and strengthen its room temperature power so as to play for silicones
The effect of performance is learned, because it has higher ceramic conversion rate, for example the ceramic conversion rate of methyl phenyl silicone resin can reach
More than 80wt%, ceramic core is remained in as the rise of heat treatment temperature can gradually be cracked into silica in air atmosphere
In material, and can plays the mechanical behavior under high temperature of intensified ceramic core.These advantages cause silicones to become ceramic mould core
Expect one of optimal selection of reinforcing.Silicones is in air atmosphere because the product of cracking is silica so that ceramic core
Though mechanical property under the high temperature conditions is improved, but still limited.
The content of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The method of silicones intensified ceramic core is infiltrated, the fiber reinforced ceramic core material as obtained from infiltrating silicones, can be carried
High ceramic core room temperature and mechanical behavior under high temperature, to obtain the ceramic core with excellent room temperature and high-temperature behavior.The present invention
The method technique of offer is simple, prepares the ceramic core excellent performance that cost is relatively low and strengthens.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that:
A kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the ceramic core strengthened will be needed to carry out vacuum drying treatment in vacuum drying chamber, drying temperature is 80~
120 DEG C, drying time is 12~24h, obtains dry ceramic core;Need the preferred silicon-base ceramic core of ceramic core strengthened
Or Al-base ceramic core;
B. it dried ceramic core will be immersed in the step a in silicon resin solution, and be positioned over vacuum drying chamber
In carry out being soaked in vacuum processing at ambient temperature, untill no longer bubble is produced in silicon resin solution, obtain immersion treatment
Ceramic core afterwards;
C. the ceramic core after the step b immersion treatments is subjected to low-temperature setting processing under atmospheric environment, Gu
It is 250~300 DEG C to change temperature, and soaking time is 4~6h, and heating rate is 1~3 DEG C/min;
D. the ceramic core that low-temperature setting is completed in the step c is carried out at high warm under inert atmosphere conditions
Reason, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
600~700 DEG C are warming up to 1~3 DEG C/min speed progress first stage first, 4~6h of insulation carries out silicon tree
The cracking of fat;Second stage is carried out with 1~3 DEG C/min speed again and is warming up to 1200~1500 DEG C, 4~6h is incubated, makes cracking
Product forms fibre reinforcement, so that ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by ceramics
After core cooling but, that is, obtain increasing fiber composite phase intensified ceramic core.The inert atmosphere for carrying out high-temperature heat treatment is preferably adopted
With nitrogen or argon gas.It is preferred that carrying out second stage is warming up to 1250~1500 DEG C.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the silicones that the present invention uses can be changed into fibre reinforcement such as SiOC fibers under an inert atmosphere or SiC is fine
Dimension, they are present in the intercrystalline gap of ceramic core, play the room temperature of enhancing ceramic core and the work of mechanical behavior under high temperature
With;
2. the method for present invention fiber reinforced ceramic core material as obtained from infiltrating silicones, is applicable not only to business
Wide variety of silicon substrate and Al-base ceramic core in industry, it can be extended to other oxide and non-oxidized substance base ceramic moulds
Core;
3. the inventive method technique is simple, workable, production cost is low and can accomplish scale production.
Brief description of the drawings
Fig. 1 is the thing phase micro-structure diagram for the method that the embodiment of the present invention one infiltrates silicones intensified ceramic core.
Embodiment
Such scheme is described further below in conjunction with specific examples of the implementation, the preferred embodiments of the present invention are described in detail such as
Under:
Embodiment one:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the silicon-base ceramic core for needing to strengthen is subjected to vacuum drying treatment in vacuum drying chamber, drying temperature is
120 DEG C, drying time 12h, obtain dry ceramic core;
B. it dried ceramic core will be immersed in the step a in silicon resin solution, and be positioned over vacuum drying chamber
In carry out being soaked in vacuum processing at ambient temperature, untill no longer bubble is produced in silicon resin solution, obtain immersion treatment
Ceramic core afterwards;
C. the ceramic core after the step b immersion treatments is subjected to low-temperature setting processing under atmospheric environment, Gu
It is 250 DEG C, soaking time 4h to change temperature, and heating rate is 1 DEG C/min;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in nitrogen atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
600 DEG C are warming up to the 1 DEG C/min speed progress first stage first, insulation 4h carries out the cracking of silicones;Again
Second stage is carried out with 1 DEG C/min speed and is warming up to 1250 DEG C, is incubated 4h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.Fig. 1 is the thing phase for the method that the embodiment of the present invention one infiltrates silicones intensified ceramic core
Micro-structure diagram.In the present embodiment, silicones changes to form SiOC fibers and SiC fibers, such as Fig. 1 under inert atmosphere conditions
Shown, SiOC fibers or SiC fibers have splendid mechanical behavior under high temperature, increase in ceramic core matrix due to this fiber be present
Qiang Xiang, its room temperature and high temperature power can be greatly enhanced.Therefore, the present embodiment uses silicones as hardening agent to made
Standby ceramic core carries out intensive treatment, carries out heat treatment under inert atmosphere conditions so as to obtain with room temperature and high temperature power
Learn the ceramic core material of excellent performance.
The present embodiment is by infiltrating silicones intensified ceramic core room temperature and mechanical behavior under high temperature, it would be desirable to the ceramics of reinforcing
Core carries out vacuum drying treatment, dried ceramic core is immersed in silicon resin solution, under vacuum and room temperature condition
Carry out being soaked in vacuum processing, obtain the ceramic core after immersion treatment, the ceramic core of acquisition is carried out under atmospheric environment low
Warm curing process, high-temperature heat treatment is carried out under inert atmosphere conditions, obtain the fiber reinforced ceramic cracked by silicones
Core.The preparation technology that the present embodiment is provided is simple, workable, with short production cycle, and cost is cheap, the ceramics strengthened
Core material has excellent room temperature and mechanical behavior under high temperature.
Embodiment two:
The present embodiment and embodiment one are essentially identical, are particular in that:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. this step is identical with embodiment one;
B. this step is identical with embodiment one;
C. this step is identical with embodiment one;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in nitrogen atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
600 DEG C are warming up to the 1 DEG C/min speed progress first stage first, insulation 4h carries out the cracking of silicones;Again
Second stage is carried out with 1 DEG C/min speed and is warming up to 1300 DEG C, is incubated 4h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.In the present embodiment, silicones change under inert atmosphere conditions to be formed SiOC fibers and
SiC fibers, SiOC fibers or SiC fibers have a splendid mechanical behavior under high temperature, due to this kind of fibre be present in ceramic core matrix
Dimension enhancing phase, its room temperature and high temperature power can be greatly enhanced.Therefore, the present embodiment uses silicones as hardening agent pair
Prepared ceramic core carries out intensive treatment, carries out heat treatment under inert atmosphere conditions so as to obtain with room temperature and height
The ceramic core material of warm excellent in mechanical performance.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the Al-base ceramic core for needing to strengthen is subjected to vacuum drying treatment in vacuum drying chamber, drying temperature is
120 DEG C, drying time 12h, obtain dry ceramic core;
B. this step is identical with embodiment one;
C. this step is identical with embodiment one;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in nitrogen atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
600 DEG C are warming up to the 1 DEG C/min speed progress first stage first, insulation 4h carries out the cracking of silicones;Again
Second stage is carried out with 1 DEG C/min speed and is warming up to 1400 DEG C, is incubated 4h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.In the present embodiment, silicones change under inert atmosphere conditions to be formed SiOC fibers and
SiC fibers, SiOC fibers or SiC fibers have a splendid mechanical behavior under high temperature, due to this kind of fibre be present in ceramic core matrix
Dimension enhancing phase, its room temperature and high temperature power can be greatly enhanced.Therefore, the present embodiment uses silicones as hardening agent pair
Prepared ceramic core carries out intensive treatment, carries out heat treatment under inert atmosphere conditions so as to obtain with room temperature and height
The ceramic core material of warm excellent in mechanical performance.
Example IV:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the silicon-base ceramic core for needing to strengthen is subjected to vacuum drying treatment in vacuum drying chamber, drying temperature is
120 DEG C, drying time 12h, obtain dry ceramic core;
B. this step is identical with embodiment one;
C. this step is identical with embodiment one;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in nitrogen atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
600 DEG C are warming up to the 1 DEG C/min speed progress first stage first, insulation 4h carries out the cracking of silicones;Again
Second stage is carried out with 1 DEG C/min speed and is warming up to 1500 DEG C, is incubated 4h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.In the present embodiment, silicones change under inert atmosphere conditions to be formed SiOC fibers and
SiC fibers, SiOC fibers or SiC fibers have a splendid mechanical behavior under high temperature, due to this kind of fibre be present in ceramic core matrix
Dimension enhancing phase, its room temperature and high temperature power can be greatly enhanced.Therefore, the present embodiment uses silicones as hardening agent pair
Prepared ceramic core carries out intensive treatment, carries out heat treatment under inert atmosphere conditions so as to obtain with room temperature and height
The ceramic core material of warm excellent in mechanical performance.
Embodiment five:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the silicon-base ceramic core for needing to strengthen is subjected to vacuum drying treatment, drying temperature 80 in vacuum drying chamber
DEG C, drying time 24h, obtain dry ceramic core;
B. this step is identical with embodiment one;
C. the ceramic core after the step b immersion treatments is subjected to low-temperature setting processing under atmospheric environment, Gu
It is 300 DEG C, soaking time 6h to change temperature, and heating rate is 3 DEG C/min;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in argon gas atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
700 DEG C are warming up to the 3 DEG C/min speed progress first stage first, insulation 6h carries out the cracking of silicones;Again
Second stage is carried out with 3 DEG C/min speed and is warming up to 1200 DEG C, is incubated 6h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.In the present embodiment, silicones change under inert atmosphere conditions to be formed SiOC fibers and
SiC fibers, SiOC fibers or SiC fibers have a splendid mechanical behavior under high temperature, due to this kind of fibre be present in ceramic core matrix
Dimension enhancing phase, its room temperature and high temperature power can be greatly enhanced.Therefore, the present embodiment uses silicones as hardening agent pair
Prepared ceramic core carries out intensive treatment, carries out heat treatment under inert atmosphere conditions so as to obtain with room temperature and height
The ceramic core material of warm excellent in mechanical performance.
Embodiment six:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of method for infiltrating silicones intensified ceramic core, comprises the following steps:
A. the Al-base ceramic core for needing to strengthen is subjected to vacuum drying treatment, drying temperature 80 in vacuum drying chamber
DEG C, drying time 24h, obtain dry ceramic core;
B. this step is identical with embodiment one;
C. the ceramic core after the step b immersion treatments is subjected to low-temperature setting processing under atmospheric environment, Gu
It is 300 DEG C, soaking time 6h to change temperature, and heating rate is 3 DEG C/min;
D. will complete to carry out under inert atmosphere conditions of the ceramic core of low-temperature setting in argon gas atmosphere in the step c
High-temperature heat treatment, the fiber reinforced ceramic core cracked by silicones is obtained, controls the high-temperature heat treatment system to be:
700 DEG C are warming up to the 3 DEG C/min speed progress first stage first, insulation 6h carries out the cracking of silicones;Again
Second stage is carried out with 3 DEG C/min speed and is warming up to 1400 DEG C, is incubated 6h, pyrolysis product is formed fibre reinforcement, so as to
Ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by after ceramic core cooling but, that is, increased
Fiber composite phase intensified ceramic core.In the present embodiment, fiber reinforcement silicon-base ceramic core is obtained by infiltrating silicones,
Silicones changes to form SiOC fibers and SiC fibers under inert atmosphere conditions, and SiOC fibers or SiC fibers have splendid height
Warm mechanical property, due to this kind of fiber reinforcement phase be present in ceramic core matrix, its room temperature and high temperature power can obtain significantly
Improve.Therefore, the present embodiment uses silicones to carry out intensive treatment to prepared ceramic core as hardening agent, in indifferent gas
Heat treatment is carried out under the conditions of atmosphere so as to obtain with the excellent ceramic core material of room temperature and mechanical behavior under high temperature.
The embodiment of the present invention is illustrated above in conjunction with accompanying drawing, but the invention is not restricted to above-described embodiment, can be with
A variety of changes are made according to the purpose of the innovation and creation of the present invention, under all Spirit Essence and principle according to technical solution of the present invention
Change, modification, replacement, combination or the simplification made, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Technical principle and inventive concept without departing from the method for present invention infiltration silicones intensified ceramic core, belong to the present invention
Protection domain.
Claims (4)
- A kind of 1. method for infiltrating silicones intensified ceramic core, it is characterised in that comprise the following steps:A. the ceramic core for needing to strengthen being subjected to vacuum drying treatment in vacuum drying chamber, drying temperature is 80~120 DEG C, Drying time is 12~24h, obtains dry ceramic core;B. it dried ceramic core will be immersed in silicon resin solution, be positioned in vacuum drying chamber in the step a Carry out being soaked in vacuum processing under room temperature condition, untill no longer bubble is produced in silicon resin solution, after obtaining immersion treatment Ceramic core;C. the ceramic core after the step b immersion treatments is subjected to low-temperature setting processing, solidification temperature under atmospheric environment Spend for 250~300 DEG C, soaking time is 4~6h, and heating rate is 1~3 DEG C/min;D. the ceramic core that low-temperature setting is completed in the step c is subjected to high-temperature heat treatment under inert atmosphere conditions, obtained To the fiber reinforced ceramic core by silicones cracking, the high-temperature heat treatment system is controlled to be:600~700 DEG C are warming up to 1~3 DEG C/min speed progress first stage first, 4~6h of insulation carries out silicones Cracking;Second stage is carried out with 1~3 DEG C/min speed again and is warming up to 1200~1500 DEG C, 4~6h is incubated, makes pyrolysis product Fibre reinforcement is formed, so that ceramic core matrix ceramic core intercrystalline is full of fiber reinforcement phase, then by ceramic core After cooling but, that is, obtain increasing fiber composite phase intensified ceramic core.
- 2. the method for silicones intensified ceramic core is infiltrated according to claim 1, it is characterised in that:In the step a, The ceramic core for needing to strengthen selects silicon-base ceramic core or Al-base ceramic core.
- 3. the method for silicones intensified ceramic core is infiltrated according to claim 1, it is characterised in that:In the step d, The inert atmosphere for carrying out high-temperature heat treatment is nitrogen or argon gas.
- 4. the method for silicones intensified ceramic core is infiltrated according to claim 1, it is characterised in that:In the step d, Carry out second stage and be warming up to 1250~1500 DEG C.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111995435A (en) * | 2020-09-02 | 2020-11-27 | 中国石油化工股份有限公司 | Method for filling pores in ceramic heat transfer element, and infiltration device |
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Cited By (8)
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CN110790586A (en) * | 2019-10-31 | 2020-02-14 | 中国科学院长春光学精密机械与物理研究所 | Densification method for reactive sintering of SiC ceramic loose core |
CN111995435A (en) * | 2020-09-02 | 2020-11-27 | 中国石油化工股份有限公司 | Method for filling pores in ceramic heat transfer element, and infiltration device |
CN111995435B (en) * | 2020-09-02 | 2022-05-03 | 中国石油化工股份有限公司 | Method for filling pores in ceramic heat transfer element, and infiltration device |
CN112851383A (en) * | 2021-01-27 | 2021-05-28 | 哈尔滨工业大学 | Infrared radiation resistant light ablation resistant composite material added with opacifier and preparation method thereof |
CN113667162A (en) * | 2021-09-18 | 2021-11-19 | 哈尔滨工业大学 | Method for improving high-temperature resistance of silicone resin and composite material thereof |
CN113667162B (en) * | 2021-09-18 | 2024-03-12 | 哈尔滨工业大学 | Method for improving high temperature resistance of silicone resin and composite material thereof |
CN115947606A (en) * | 2022-12-16 | 2023-04-11 | 中航装甲科技有限公司 | Water-soluble enhancer for silicon-based ceramic core and enhancing method |
CN115947606B (en) * | 2022-12-16 | 2024-03-12 | 中航装甲科技有限公司 | Water-soluble strengthening agent and strengthening method for silicon-based ceramic core |
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