CN115650751B - Fiber-reinforced silicon carbide cladding and method for making same - Google Patents
Fiber-reinforced silicon carbide cladding and method for making same Download PDFInfo
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- CN115650751B CN115650751B CN202211254791.1A CN202211254791A CN115650751B CN 115650751 B CN115650751 B CN 115650751B CN 202211254791 A CN202211254791 A CN 202211254791A CN 115650751 B CN115650751 B CN 115650751B
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 145
- 238000005253 cladding Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000835 fiber Substances 0.000 claims abstract description 78
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 238000005238 degreasing Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000000280 densification Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000011248 coating agent Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000009954 braiding Methods 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
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- 238000001764 infiltration Methods 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
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- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 235000021313 oleic acid Nutrition 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000002775 capsule Substances 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000006243 chemical reaction Methods 0.000 claims 1
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- 238000000197 pyrolysis Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 15
- 238000002156 mixing Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229940083037 simethicone Drugs 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Ceramic Products (AREA)
Abstract
The invention discloses a fiber-reinforced silicon carbide cladding and a preparation method thereof, wherein the preparation method comprises the following steps: s1, preparing slurry; s2, preparing and forming the slurry into a silicon carbide lining pipe green body; s3, degreasing and sintering the silicon carbide lining pipe green body to form a high-density silicon carbide lining pipe; and S4, arranging a fiber woven layer on the outer surface of the silicon carbide lining pipe, and densifying the fiber woven layer. The invention prepares slurry by mixing the silicon carbide fiber powder mixture with organic solvent and the like, then processes and forms a shell green body, combines degreasing and sintering treatment to prepare the silicon carbide lining pipe, and has the characteristics of high strength and high toughness; in the setting of the fiber woven layer and the subsequent densification process, the straightness of the cladding tube is maintained, the requirements of the straightness, roundness and design values of parameters of inner diameter and outer diameter of the cladding can be met, and the processing amount of the subsequent cladding is reduced.
Description
Technical Field
The invention relates to a silicon carbide cladding, in particular to a fiber-reinforced silicon carbide cladding and a preparation method thereof.
Background
The SiC composite cladding is mainly divided into three layers and two layers, and compared with the two-layer structural design, the three-layer design can further ensure the air tightness of cladding materials, so that the safety of the nuclear fuel element is improved.
At present, the preparation process of the three-layer SiC composite cladding comprises the following steps: after the fiber is woven on the lining, the intermediate layer is densified through a CVI or PIP process, and finally, the coating technology is used for realizing the coating of the outermost layer. However, due to the super-length-diameter ratio characteristic of the SiC composite cladding, parameters such as straightness, roundness, inner diameter and outer diameter of the SiC composite cladding are easily affected due to deformation of the lining in the preparation process. Meanwhile, because of the high hardness and the brittle texture of SiC, the processing difficulty of SiC is increased, and therefore, the preparation of a full-size SiC composite cladding is difficult to realize in the prior art.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a fiber-reinforced and toughened silicon carbide cladding.
The technical scheme adopted for solving the technical problems is as follows: a method for preparing a fiber-reinforced silicon carbide cladding is provided, which comprises the following steps:
s1, preparing slurry; the slurry comprises the following raw materials in parts by weight: 45-89.7 parts of silicon carbide fiber powder mixture, 10-40 parts of organic solvent, 0.1-5 parts of dispersing agent, 0.1-5 parts of plasticizer and 0.1-5 parts of defoamer;
s2, preparing and forming the slurry into a silicon carbide lining pipe green body;
s3, degreasing and sintering the silicon carbide lining pipe green body to form a high-density silicon carbide lining pipe;
and S4, arranging a fiber woven layer on the outer surface of the silicon carbide lining pipe, and densifying the fiber woven layer to form a fiber-toughened silicon carbide cladding.
Preferably, in step S1, the silicon carbide fiber powder mixture includes a silicon carbide material; the silicon carbide material comprises silicon carbide fibers and silicon carbide powder, wherein the volume percentage of the silicon carbide fibers in the silicon carbide material is 10-50%;
the diameter of the silicon carbide fiber is 0.01-10 mu m, and the length-diameter ratio of the silicon carbide fiber is 10-1000.
Preferably, in step S1, the silicon carbide fiber powder mixture further includes a sintering aid, and the mass percentage of the sintering aid in the silicon carbide fiber powder mixture is 1-10%.
Preferably, the sintering aid is Al 2 O 3 -Re 2 O 3 Wherein Re is Sc, Y, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb or Lu.
Preferably, in the sintering aid, al 2 O 3 And Re (Re) 2 O 3 The proportion of (2) is 1-99 wt%:99 to 1 weight percent.
Preferably, in step S1, the organic solvent is at least one of absolute ethanol, acetone, xylene, and polyethylene glycol.
Preferably, the dispersing agent is at least one of oleic acid, stearic acid and castor oil.
Preferably, the plasticizer is at least one of carboxymethyl cellulose, phenolic resin and tetramethyl ammonium hydroxide.
Preferably, the defoaming agent is at least one of ethylene glycol, glycerol and dimethyl silicone oil.
Preferably, in step S1, the raw materials are made into a slurry by at least one of roller ball milling, planetary ball milling, magnetic stirring, and mechanical stirring.
Preferably, in step S2, the slurry is made into a silicon carbide inner liner tube green body by a compression molding or extrusion molding process.
Preferably, in step S3, the degreasing treatment is as follows: under vacuum, the temperature is raised to 400-800 ℃ at a heating rate of 1-10 ℃/min, and the temperature is kept for 1-10 h.
Preferably, in step S3, the sintering process is as follows: heating to 800-1200 deg.c at the heating rate of 10-20 deg.c/min; then heating to 1700-2200 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 0.5-4 h.
Preferably, in step S3, the atmosphere of the sintering treatment is vacuum or at least one of argon, helium, and nitrogen.
Preferably, in the step S2, the inner diameter of the silicon carbide lining pipe green body is 7 mm-7.8 mm, the outer diameter is 8.5 mm-9 mm, and the wall thickness is 0.35 mm-1.0 mm; the length of the silicon carbide lining pipe green body is 1000 mm-4000 mm.
Preferably, in the step S3, the inner diameter of the formed high-density silicon carbide lining pipe is 7.1-7.9 mm, the outer diameter is 8.4-9.1 mm, the wall thickness is 0.25-1.0 mm, and the length is 1000-4000 mm.
Preferably, in the step S4, the inner diameter of the silicon carbide composite cladding is 7.1 mm-7.9 mm, the outer diameter is 9.5 mm-10.1 mm, the wall thickness is 0.3 mm-1.5 mm, and the length is 1000 mm-4000 mm; the straightness is 1/2000-1/100.
Preferably, in step S4, the diameter of the silicon carbide fiber used in the fiber braid is 5 μm to 20 μm.
Preferably, in step S4, the densification treatment employs at least one of chemical vapor infiltration, precursor dip-cracking, and reactive infiltration.
Preferably, the method of preparing the fiber-reinforced silicon carbide cladding further comprises the steps of:
s5, a coating is arranged on the outer surface of the silicon carbide composite cladding.
Preferably, the coating comprises at least one of a silicon carbide coating, a metallic chromium coating, a high entropy coating.
The invention also provides a fiber-reinforced silicon carbide cladding which is prepared by adopting the preparation method of any one of the above.
The invention has the beneficial effects that: preparing slurry by using a silicon carbide fiber powder mixture and an organic solvent, and the like, then processing and forming into a shell green body, and preparing the silicon carbide lining pipe by combining degreasing and sintering treatment, wherein the silicon carbide lining pipe has high-strength high-toughness characteristics; in the setting of the fiber woven layer and the subsequent densification process, the straightness of the cladding tube is maintained, the requirements of the straightness, roundness and design values of parameters of inner diameter and outer diameter of the cladding can be met, and the processing amount of the subsequent cladding is reduced.
In addition, the preparation method does not need high-temperature and high-pressure processes, and simplifies the preparation process; the prepared fiber-reinforced and toughened silicon carbide cladding has high density, high heat transfer performance and high mechanical property.
Detailed Description
The preparation method of the fiber-reinforced silicon carbide cladding comprises the following steps:
s1, preparing slurry.
The slurry comprises the following raw materials in parts by weight: 45-89.7 parts of silicon carbide fiber powder mixture, 10-40 parts of organic solvent, 0.1-5 parts of dispersing agent, 0.1-5 parts of plasticizer and 0.1-5 parts of defoamer.
Wherein the silicon carbide fiber powder mixture comprises a silicon carbide material and a sintering aid. The silicon carbide material further comprises silicon carbide fiber and silicon carbide powder, wherein the silicon carbide fiber and the silicon carbide powder are mixed to form the silicon carbide material, and the silicon carbide fiber accounts for 10-50% of the volume percentage.
In the silicon carbide fiber powder mixture, the silicon carbide fiber is used as a short fiber, plays a role in strengthening, is beneficial to meeting requirements on straightness, roundness, inner diameter parameters, outer diameter parameters and the like of the cladding, and can improve the compactness of the cladding. Preferably, the silicon carbide fibers have a diameter of 0.01 μm to 10 μm and an aspect ratio of 10 to 1000.
In the silicon carbide material, the mass percentage of the sintering aid is 1-10%. The sintering aid is Al 2 O 3 -Re 2 O 3 ，Al 2 O 3 And Re (Re) 2 O 3 The proportion of (2) is 1-99 wt%:99wt%About 1wt%. Wherein Re is Sc, Y, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb or Lu.
For other raw materials of the slurry, the organic solvent is at least one of absolute ethyl alcohol, acetone, dimethylbenzene and polyethylene glycol; the dispersing agent is at least one of oleic acid, stearic acid and castor oil; the plasticizer is at least one of carboxymethyl cellulose, phenolic resin and tetramethyl ammonium hydroxide; the defoaming agent is at least one of glycol, glycerol and simethicone.
When the slurry is prepared, the raw materials with required quality are weighed and mixed into the slurry through at least one of roller ball milling, planetary ball milling, magnetic stirring and mechanical stirring.
S2, preparing the slurry into a silicon carbide lining pipe green body with thin wall and super length-diameter ratio through a compression molding or extrusion molding process.
The inner diameter of the silicon carbide lining pipe green body is 7 mm-7.8 mm, the outer diameter is 8.5 mm-9 mm, and the wall thickness is 0.35 mm-1.0 mm; the length of the silicon carbide lining pipe green body is 1000 mm-4000 mm.
And S3, degreasing and sintering the green body of the silicon carbide lining pipe to form the high-density silicon carbide lining pipe.
Wherein, degreasing treatment is as follows: under vacuum, the temperature is raised to 400-800 ℃ at a heating rate of 1-10 ℃/min, and the temperature is kept for 1-10 h.
The sintering treatment is as follows: heating to 800-1200 deg.c at the heating rate of 10-20 deg.c/min; then heating to 1700-2200 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 0.5-4 h. The atmosphere of the sintering treatment is vacuum or at least one of argon, helium and nitrogen.
After degreasing and sintering treatment, the formed high-density silicon carbide lining pipe has the inner diameter of 7.1-7.9 mm, the outer diameter of 8.4-9.1 mm, the wall thickness of 0.25-1.0 mm and the length of 1000-4000 mm.
And S4, arranging a fiber woven layer on the outer surface of the silicon carbide lining pipe, and densifying the fiber woven layer to form a fiber-reinforced silicon carbide cladding.
The fiber braiding layer can be directly formed on the outer surface of the silicon carbide lining pipe through a braiding machine and the like, so that the toughness of the silicon carbide cladding is improved. The fiber braiding layer is formed by braiding silicon carbide fibers. If the fiber diameter is too large, the fiber braiding effect is poor; the diameter of the fiber is too small, and the fiber is easy to break in the weaving process; therefore, to ensure that the formed fiber braid has a preferable effect, the silicon carbide fiber has a diameter of 5 μm to 20 μm.
The densification treatment of the woven fiber layer may be at least one of chemical vapor infiltration, precursor dip-cracking, and reactive infiltration.
The inner diameter of the silicon carbide composite cladding obtained after densification is 7.1 mm-7.9 mm, the outer diameter is 9.5 mm-10.1 mm, the wall thickness is 0.3 mm-1.5 mm, and the length is 1000 mm-4000 mm; the straightness is 1/2000-1/100.
S5, a coating is arranged on the outer surface of the silicon carbide composite cladding.
The coating comprises at least one of a silicon carbide coating, a metallic chromium coating, a high entropy coating, and a metallic chromium coating may be preferred.
The density of the fiber-reinforced silicon carbide cladding prepared by the invention reaches 95-99%, and the cladding leakage rate is 10- 13 ～1×10- 1 0Pa·m 3 And/s, the tensile strength of the alloy is 350-550 MPa at room temperature, and the tensile strength of the alloy is 400-600 MPa at 1200 ℃.
The invention is further illustrated by the following examples.
Example 1
The raw materials comprise: 64.5wt% of silicon carbide fiber powder mixture, 35wt% of organic solvent, 0.15wt% of dispersing agent, 0.2wt% of plasticizer and 0.15wt% of defoamer. Wherein the dispersing agent is oleic acid, the plasticizer is carboxymethyl cellulose, the defoaming agent is ethylene glycol, and the organic solvent is absolute ethyl alcohol; the silicon carbide fiber powder mixture comprises silicon carbide material and sintering aid, wherein the proportion of the sintering aid is 5%, and the sintering aid is Al 2 O 3 -Y 2 O 3 Wherein Al is 2 O 3 And Re (Re) 2 O 3 The proportion of (2) is 45wt%:55wt% of silicon carbide material including silicon carbide fibers and silicon carbideThe volume ratio of the powder and the silicon carbide fiber is 40 percent, the diameter of the silicon carbide fiber is 0.1 mu m, and the length-diameter ratio of the fiber is 500. The raw materials are mixed by adopting roller ball milling, silicon nitride is adopted as a grinding ball, absolute ethyl alcohol is adopted as a ball milling medium, and slurry is prepared by ball milling.
The sizing agent is prepared into a molded lining pipe green body through an extrusion molding preparation process, wherein the inner diameter of the molded lining pipe green body is 7.5mm, the outer diameter of the molded lining pipe green body is 8.5mm, the wall thickness of the molded lining pipe green body is 0.5mm, and the length of the molded lining pipe green body is 4000mm. Degreasing is carried out in a vacuum environment, and the degreasing process is to heat up to 600 ℃ at a heating rate of 2 ℃/min and preserve heat for 5h; continuously sintering at high temperature after degreasing, wherein the sintering process is to raise the temperature to 1200 ℃ at a heating rate of 10 ℃/min; then heating to 1900 ℃ at 5 ℃/min, and preserving heat for 2 hours, wherein the sintering atmosphere is argon. After sintering, a dense lining tube was obtained, which had an inner diameter of 7.9mm, an outer diameter of 8.5mm, a wall thickness of 0.3mm and a length of 4000mm. After the outer surface of the lining pipe is woven by long fibers with the diameter of 10 mu m, densification is carried out at the temperature of 1300 ℃ by adopting a CVI process, and SiC coating deposition is carried out on the outer surface by adopting a CVD process continuously, so that the silicon carbide cladding pipe is prepared.
After the silicon carbide cladding tube is subjected to rough grinding treatment on the inner surface and the outer surface, the inner diameter is 7.9mm, the outer diameter is 9.9mm, the wall thickness is 1mm, and the length is 4000mm. The density of the obtained silicon carbide cladding tube is 99%, and the straightness is 1/100; the leakage rate of the cladding is 10- 13 Pa·m 3 And/s, which has a tensile strength of 400MPa at room temperature and 450MPa at 1200 ℃.
Example 2
The raw materials comprise: 89.7wt percent of silicon carbide fiber powder mixture, 10wt percent of organic solvent, 0.1wt percent of dispersing agent, 0.1wt percent of plasticizer and 0.1wt percent of defoamer. In the silicon carbide fiber powder mixture, the volume ratio of the silicon carbide fibers is 10 percent, the diameter of the silicon carbide fibers is 0.01 mu m, and the length-diameter ratio of the fibers is 1000. A slurry was prepared as in example 1.
The sizing agent is subjected to compression molding preparation technology, and the inner diameter of the formed lining pipe green body is 7.8mm, the outer diameter is 8.5mm, the wall thickness is 0.35mm, and the length is 4000mm. Degreasing is carried out in a vacuum environment, and the degreasing process is to heat up to 700 ℃ at a heating rate of 2 ℃/min and preserve heat for 4 hours; continuously sintering at high temperature after degreasing, wherein the sintering process is to raise the temperature to 1200 ℃ at a heating rate of 10 ℃/min; heating to 1700 ℃ at 5 ℃/min, and preserving heat for 2 hours, wherein the sintering atmosphere is argon. After sintering, a dense lining tube was obtained, which had an inner diameter of 7.9mm, an outer diameter of 8.4mm, a wall thickness of 0.25mm and a length of 4000mm. After the outer surface of the lining pipe is woven by long fibers with the diameter of 20 mu m, densification is carried out at the temperature of 1200 ℃ by adopting a CVI process, and SiC coating deposition is carried out on the outer surface by adopting a CVD process continuously, so that the silicon carbide cladding pipe is prepared.
After the silicon carbide cladding tube is subjected to rough grinding treatment on the inner surface and the outer surface, the inner diameter is 7.9mm, the outer diameter is 10.0mm, the wall thickness is 1.05mm, and the length is 4000mm. The density of the obtained silicon carbide cladding tube is 99%, and the straightness is 1/2000; the leakage rate of the cladding is 10- 13 Pa·m 3 And/s, which has a tensile strength of 350MPa at room temperature and 400MPa at a high temperature of 1200 ℃.
Example 3
The raw materials comprise: 45wt% of silicon carbide fiber powder mixture, 45wt% of organic solvent, 5wt% of dispersing agent, 5wt% of plasticizer and 5wt% of defoamer. In the silicon carbide fiber powder mixture, the volume ratio of the silicon carbide fibers is 50%, the diameter of the silicon carbide fibers is 0.01 mu m, and the length-diameter ratio of the fibers is 1000. A slurry was prepared as in example 1.
The sizing agent is subjected to compression molding preparation technology, and the inner diameter of the formed lining pipe green body is 7.1mm, the outer diameter is 8.4mm, the wall thickness is 0.65mm, and the length is 4000mm. Degreasing is carried out in a vacuum environment, and the degreasing process is to heat up to 800 ℃ at a heating rate of 2 ℃/min and preserve heat for 10h; continuously sintering at high temperature after degreasing, wherein the sintering process is to raise the temperature to 1200 ℃ at a heating rate of 10 ℃/min; heating to 2200 ℃ at 5 ℃/min, and preserving heat for 2 hours, wherein the sintering atmosphere is argon. After sintering, a dense lining tube was obtained, which had an inner diameter of 7.5mm, an outer diameter of 8.2mm, a wall thickness of 0.35mm and a length of 4000mm. After the outer surface of the lining pipe is woven by long fibers with the diameter of 5 mu m, densification is carried out at the temperature of 1100 ℃ by adopting a CVI process, and SiC coating deposition is carried out on the outer surface by adopting a CVD process continuously, so that the silicon carbide cladding pipe is prepared.
After the silicon carbide cladding tube is subjected to rough grinding treatment on the inner surface and the outer surface, the inner diameter is 7.5mm, the outer diameter is 9.5mm, the wall thickness is 1mm, and the length is 4000mm. The density of the obtained silicon carbide cladding tube is 99%, and the straightness is 1/500; the leakage rate of the cladding is 10- 13 Pa·m 3 And/s, which has a tensile strength of 550MPa at room temperature and 600MPa at a high temperature of 1200 ℃.
Example 4
The raw materials comprise: 80wt% of silicon carbide fiber powder mixture, 15wt% of organic solvent, 1.5wt% of dispersing agent, 2wt% of plasticizer and 1.5wt% of defoamer. In the silicon carbide fiber powder mixture, the volume ratio of the silicon carbide fibers is 35%, the diameter of the silicon carbide fibers is 5 mu m, and the length-diameter ratio of the fibers is 10. A slurry was prepared as in example 1.
And (3) carrying out compression molding preparation on the sizing agent to prepare the molded lining pipe green body with the inner diameter of 7.5mm, the outer diameter of 8.5mm, the wall thickness of 0.5mm and the length of 4000mm. Degreasing is carried out in a vacuum environment, and the degreasing process is to heat up to 500 ℃ at a heating rate of 2 ℃/min and preserve heat for 3 hours; continuously sintering at high temperature after degreasing, wherein the sintering process is to raise the temperature to 1200 ℃ at a heating rate of 10 ℃/min; heating to 1800 ℃ at a speed of 5 ℃/min, and preserving heat for 2 hours, wherein the sintering atmosphere is argon. After sintering, a dense lining tube was obtained, which had an inner diameter of 7.7mm, an outer diameter of 8.4mm, a wall thickness of 0.35mm and a length of 4000mm. After the outer surface of the lining pipe is woven by long fibers with the diameter of 15 mu m, densification is carried out at the temperature of 1100 ℃ by adopting a CVI process, and SiC coating deposition is carried out on the outer surface by adopting a CVD process continuously, so that the silicon carbide cladding pipe is prepared.
After the silicon carbide cladding tube is subjected to rough grinding treatment on the inner surface and the outer surface, the inner diameter is 7.7mm, the outer diameter is 9.9mm, the wall thickness is 1.1mm, and the length is 4000mm. The density of the obtained silicon carbide cladding tube is 99%, and the straightness is 1/1000; the leakage rate of the cladding is 10- 13 Pa·m 3 And/s, which has a tensile strength of 400MPa at room temperature and 500MPa at 1200 ℃.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.
Claims (7)
1. A method of making a fiber-reinforced silicon carbide capsule, comprising the steps of:
s1, preparing slurry; the slurry comprises the following raw materials in parts by weight: 45-89.7 parts of silicon carbide fiber powder mixture, 10-40 parts of organic solvent, 0.1-5 parts of dispersing agent, 0.1-5 parts of plasticizer and 0.1-5 parts of defoamer;
the silicon carbide fiber powder mixture comprises a silicon carbide material; the silicon carbide material comprises silicon carbide fibers and silicon carbide powder, wherein the volume percentage of the silicon carbide fibers in the silicon carbide material is 10-50%; the diameter of the silicon carbide fiber is 0.01 mu m-10 mu m, and the length-diameter ratio of the silicon carbide fiber is 10-1000;
s2, preparing and forming the slurry into a silicon carbide lining pipe green body through a compression molding or extrusion molding process; the inner diameter of the silicon carbide lining pipe green body is 7-7.8 mm, the outer diameter is 8.5-9 mm, and the wall thickness is 0.35-1.0 mm; the length of the silicon carbide lining pipe green body is 1000-4000 mm;
s3, degreasing and sintering the silicon carbide lining pipe green body to form a high-density silicon carbide lining pipe; degreasing treatment is as follows: heating to 400-800 ℃ at a heating rate of 1-10 ℃/min under vacuum, and preserving heat for 1-10 h;
the sintering treatment is as follows: heating to 800-1200 deg.c at the heating rate of 10-20 deg.c/min; heating to 1700-2200 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 0.5-4 h;
the inner diameter of the formed high-density silicon carbide lining pipe is 7.1-7.9 mm, the outer diameter is 8.4-9.1 mm, the wall thickness is 0.25-1.0 mm, and the length is 1000-4000 mm;
s4, arranging a fiber woven layer on the outer surface of the silicon carbide lining pipe, and densifying the fiber woven layer to form a fiber-toughened silicon carbide cladding;
the fiber braiding layer is formed by braiding silicon carbide fibers, and the diameter of the silicon carbide fibers is 5-20 mu m; the densification treatment adopts at least one of chemical vapor infiltration, precursor impregnation pyrolysis and reaction infiltration;
the inner diameter of the silicon carbide composite cladding is 7.1-7.9 mm, the outer diameter is 9.5-10.1 mm, the wall thickness is 0.3-1.5 mm, and the length is 1000-4000 mm; the straightness is 1/2000-1/100;
s5, a coating is arranged on the outer surface of the silicon carbide cladding; the coating comprises at least one of a silicon carbide coating, a metallic chromium coating and a high entropy coating.
2. The method for producing a fiber-reinforced silicon carbide cladding according to claim 1, wherein in step S1, said silicon carbide fiber powder mixture further comprises a sintering aid, said sintering aid being 1 to 10% by mass in said silicon carbide fiber powder mixture.
3. The method of preparing a fiber-reinforced silicon carbide capsule according to claim 2, wherein the sintering aid is Al 2 O 3 -Re 2 O 3 Wherein Re is Sc, Y, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb or Lu;
in the sintering aid, al 2 O 3 And Re (Re) 2 O 3 The proportion of (2) is 1-99 wt%:99 The weight percent is 1 percent.
4. The method for preparing a fiber-reinforced silicon carbide cladding according to claim 1, wherein in step S1, said organic solvent is at least one of absolute ethanol, acetone, xylene, polyethylene glycol;
the dispersing agent is at least one of oleic acid, stearic acid and castor oil;
the plasticizer is at least one of carboxymethyl cellulose, phenolic resin and tetramethyl ammonium hydroxide;
the defoaming agent is at least one of glycol, glycerol and dimethyl silicone oil.
5. The method of preparing a fiber-reinforced silicon carbide capsule according to claim 1, wherein in step S1, the raw materials are slurried by at least one of roller ball milling, planetary ball milling, magnetic stirring, and mechanical stirring.
6. The method for producing a fiber-reinforced silicon carbide cladding according to claim 1, wherein in step S3, the atmosphere of the sintering treatment is vacuum or at least one of argon, helium, and nitrogen.
7. A fibre-reinforced silicon carbide cladding produced by the method of any one of claims 1 to 6.
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