WO2024077567A1 - Gainage de matériau composite de carbure de silicium à haute densité et son procédé de préparation - Google Patents

Gainage de matériau composite de carbure de silicium à haute densité et son procédé de préparation Download PDF

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Publication number
WO2024077567A1
WO2024077567A1 PCT/CN2022/125203 CN2022125203W WO2024077567A1 WO 2024077567 A1 WO2024077567 A1 WO 2024077567A1 CN 2022125203 W CN2022125203 W CN 2022125203W WO 2024077567 A1 WO2024077567 A1 WO 2024077567A1
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silicon carbide
cladding
preparing
density
composite material
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PCT/CN2022/125203
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English (en)
Chinese (zh)
Inventor
薛佳祥
吴利翔
廖业宏
任啟森
杨荣坤
Original Assignee
中广核研究院有限公司
岭东核电有限公司
中国广核集团有限公司
中国广核电力股份有限公司
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Priority to PCT/CN2022/125203 priority Critical patent/WO2024077567A1/fr
Publication of WO2024077567A1 publication Critical patent/WO2024077567A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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

Definitions

  • the invention relates to the technical field of nuclear fuel elements, and in particular to a high-density silicon carbide composite material cladding and a preparation method thereof.
  • the existing commercial Zr alloy cladding has poor high temperature resistance and corrosion resistance, and has a high hydrogen production rate when reacting with water at high temperature.
  • the above disadvantages of Zr alloy reduce the safety of nuclear power plants.
  • SiC can be used as a new cladding material to replace the existing Zr alloy because of its high melting point, corrosion resistance, resistance to neutron irradiation, low neutron absorption cross section, and low hydrogen production rate when reacting with water at high temperature.
  • the preparation methods of SiC cladding materials include NITE (nano-impregnation transient liquid phase) method, CVI (chemical vapor infiltration) method, PIP (precursor impregnation pyrolysis) method and RI (reactive infiltration) method.
  • the NITE method for preparing SiC cladding proposes that SiC fibers containing an interface layer (usually pyrolysis carbon) be impregnated into a slurry made by mixing nano-SiC particles with an oxidative sintering aid, and then hot-pressed and sintered under an inert gas (usually argon) to prepare a SiC-based composite material.
  • the SiC composite cladding prepared by the NITE method has the advantages of low porosity, high thermal conductivity, dense matrix, high crystallinity, and no residual Si.
  • this technology needs to be prepared under high temperature ( ⁇ 1750°C) and high pressure ( ⁇ 10 MPa) conditions, and cannot achieve the preparation of meter-level thin-walled and ultra-aspect ratio cladding materials.
  • the CVI/PIP method proposes to weave SiC fibers containing an interface layer (usually pyrolysis carbon) and then further densify them through the CVI/PIP process to prepare SiC cladding materials.
  • the above process can achieve the preparation of meter-level thin-walled and ultra-aspect ratio SiC composite claddings, but the prepared claddings have many pore defects, and the PIP process preparation process is lengthy.
  • the RI method proposes a reaction infiltration process to prepare continuous fiber reinforced SiC-based composites.
  • the SiC cladding prepared by this process contains a lot of residual Si, which reduces its high temperature performance and corrosion resistance.
  • the technical problem to be solved by the present invention is to provide a method for preparing a high-density silicon carbide composite material cladding and the prepared silicon carbide composite material cladding.
  • the technical solution adopted by the present invention to solve the technical problem is: to provide a method for preparing a high-density silicon carbide composite material cladding, comprising the following steps:
  • the slurry includes raw materials and their weight proportions are as follows: 45-89.7 parts of silicon carbide fiber powder mixture, 10-40 parts of organic solvent, 0.1-5 parts of dispersant, 0.1-5 parts of plasticizer and 0.1-5 parts of defoamer;
  • the silicon carbide fiber powder mixture includes silicon carbide material
  • the silicon carbide material comprises silicon carbide fibers and silicon carbide powder, and the volume percentage of the silicon carbide fibers in the silicon carbide material is 10 to 50%;
  • the diameter of the silicon carbide fiber is 0.01 ⁇ m to 10 ⁇ m, and the aspect ratio of the silicon carbide fiber is 10 to 1000.
  • the silicon carbide fiber powder mixture further includes a sintering aid.
  • the mass percentage of the sintering aid in the silicon carbide fiber powder mixture is 1-10%.
  • 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.
  • the ratio of Al 2 O 3 to Re 2 O 3 is 1 wt% to 99 wt%: 99 wt% to 1 wt%.
  • the organic solvent is at least one of anhydrous ethanol, acetone, xylene and polyethylene glycol.
  • the dispersant 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 ethylene glycol, glycerin and dimethyl silicone oil.
  • the raw material is made into slurry by at least one of roller ball milling, planetary ball milling, magnetic stirring and mechanical stirring.
  • step S2 the slurry is formed into a silicon carbide cladding green body by compression molding or extrusion molding.
  • the degreasing treatment is as follows: under vacuum, the temperature is increased to 400°C to 800°C at a heating rate of 1°C/min to 10°C/min, and the temperature is kept for 1 to 10 hours.
  • the sintering treatment is as follows: heating to 800°C-1200°C at a heating rate of 10°C/min-20°C/min; then heating to 1700°C-2200°C at a heating rate of 5°C/min-10°C/min, and keeping warm for 0.5-4h.
  • the atmosphere of the sintering treatment is vacuum, or at least one of argon, helium and nitrogen.
  • the inner diameter of the silicon carbide green body is 6 mm to 9 mm, the outer diameter is 9.5 mm to 12 mm, and the wall thickness is 0.5 mm to 1.5 mm; the length of the silicon carbide green body is 1000 mm to 4000 mm.
  • the formed high-density silicon carbide cladding has an inner diameter of 7 mm to 8 mm, an outer diameter of 9.5 mm to 10 mm, a wall thickness of 0.5 mm to 1 mm, and a length of 1000 mm to 4000 mm.
  • the density of the silicon carbide cladding is 95-99%
  • the cladding leakage rate is 10 -13 -1 ⁇ 10 -10 Pa ⁇ m 3 /s
  • the tensile strength is 200 MPa-350 MPa at room temperature
  • the tensile strength is 250 MPa-400 MPa at a high temperature of 1200°C.
  • the method for preparing the high-density silicon carbide composite material cladding further comprises the following steps:
  • the protective coating includes at least one of a silicon carbide coating, a metal chromium coating, and a high entropy coating.
  • the present invention also provides a high-density silicon carbide composite material cladding, which is prepared by any of the preparation methods described above.
  • a silicon carbide fiber powder mixture is combined with an organic solvent to form a slurry, which is then processed into a cladding green body, and combined with degreasing and sintering treatment to obtain a meter-scale, ultra-aspect ratio silicon carbide cladding, thereby improving the density of the silicon carbide cladding, reducing pore defects and reducing its harmful by-products; simplifying the cladding preparation process, improving production efficiency; and reducing preparation costs.
  • the method for preparing the high-density silicon carbide composite material cladding of the present invention may include the following steps:
  • the slurry includes raw materials and their weight proportions are as follows: 45-89.7 parts of silicon carbide fiber powder mixture, 10-40 parts of organic solvent, 0.1-5 parts of dispersant, 0.1-5 parts of plasticizer and 0.1-5 parts of defoamer.
  • the silicon carbide fiber powder mixture includes silicon carbide material and sintering aid.
  • the silicon carbide material may further include silicon carbide fiber and silicon carbide powder, which are mixed together, and the volume percentage of silicon carbide fiber is 10-50%.
  • the silicon carbide fiber is a short fiber that plays a reinforcing role and improves the compactness of the prepared cladding.
  • the diameter of the silicon carbide fiber is 0.01 ⁇ m to 10 ⁇ m, and the aspect ratio of the silicon carbide fiber is 10 to 1000.
  • the mass percentage of the sintering aid is 1-10%.
  • the sintering aid is Al 2 O 3 -Re 2 O 3 , and the ratio of Al 2 O 3 to Re 2 O 3 is 1wt%-99wt%:99wt%-1wt%.
  • Re is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu.
  • the organic solvent is selected from at least one of anhydrous ethanol, acetone, xylene, and polyethylene glycol;
  • the dispersant is at least one of oleic acid, stearic acid, and castor oil;
  • the plasticizer is at least one of carboxymethyl cellulose, phenolic resin, and tetramethylammonium hydroxide;
  • the defoaming agent is at least one of ethylene glycol, glycerin, and dimethyl silicone oil.
  • the required weight of each raw material is weighed, and then the raw materials are mixed into the slurry by at least one of roller ball milling, planetary ball milling, magnetic stirring, and mechanical stirring.
  • the slurry is formed into a thin-walled, ultra-length-diameter ratio silicon carbide cladding green body by molding, extrusion or other processing methods.
  • the inner diameter of the silicon carbide green body is 6 mm to 9 mm, the outer diameter is 9.5 mm to 12 mm, and the wall thickness is 0.5 mm to 1.5 mm; the length of the silicon carbide green body is 1000 mm to 4000 mm.
  • the degreasing treatment is as follows: under vacuum, the temperature is increased to 400°C to 800°C at a heating rate of 1°C/min to 10°C/min, and the temperature is kept for 1 to 10 hours.
  • the sintering treatment is as follows: heating to 800°C to 1200°C at a heating rate of 10°C/min to 20°C/min; then heating to 1700°C to 2200°C at a heating rate of 5°C/min to 10°C/min, and keeping the temperature for 0.5 to 4 hours.
  • the sintering treatment atmosphere is vacuum, or at least one of argon, helium, and nitrogen.
  • the formed high-density silicon carbide cladding has an inner diameter of 7mm to 8mm, an outer diameter of 9.5mm to 10mm, a wall thickness of 0.5mm to 1mm, and a length of 1000mm to 4000mm.
  • the corrosion resistance of the silicon carbide cladding is improved by setting a protective coating.
  • the protective coating includes at least one of a silicon carbide coating, a metal chromium coating, and a high entropy coating, and the protective coating may preferably be a metal chromium coating.
  • the silicon carbide composite material cladding prepared by the present invention has a density of 95-99%, a cladding leakage rate of 10 -13 to 1 ⁇ 10 -10 Pa ⁇ m 3 /s, a tensile strength of 200MPa to 350MPa at room temperature, and a tensile strength of 250MPa to 400MPa at a high temperature of 1200°C.
  • the raw materials of the slurry are: 80wt% silicon carbide fiber powder mixture, 10wt% organic solvent, 2.5wt% dispersant, 5wt% plasticizer, 2.5wt% defoamer; the dispersant is oleic acid, the plasticizer is carboxymethyl cellulose, the defoamer is ethylene glycol, and the organic solvent is anhydrous ethanol.
  • the proportion of sintering aid in the silicon carbide fiber powder mixture is 10%, and the sintering aid is Al 2 O 3 -Y 2 O 3 , wherein the ratio of Al 2 O 3 to Y 2 O 3 is 45wt%:55wt%, and the silicon carbide material includes silicon carbide fiber and silicon carbide powder, the volume ratio of silicon carbide fiber is 40%, the diameter of silicon carbide fiber is 0.1 ⁇ m, and the fiber aspect ratio is 500.
  • the above raw materials are mixed by roller ball milling, silicon nitride is used as grinding ball, anhydrous ethanol is used as ball milling medium, and the slurry is prepared by ball milling.
  • the above slurry was prepared into a cladding green body by extrusion molding process, with an inner diameter of 7.9 mm, an outer diameter of 10 mm, a wall thickness of 1.05 mm, and a length of 4000 mm.
  • Degreasing was carried out in a vacuum environment, and the degreasing process was heated to 600°C at a heating rate of 2°C/min and kept warm for 5 hours; after degreasing, high-temperature sintering was continued, and the sintering process was heated to 1200°C at a heating rate of 10°C/min; then heated to 1900°C at 5°C/min, kept warm for 2 hours, and the sintering atmosphere was argon. After sintering, a dense silicon carbide composite cladding was formed, with an inner diameter of 8.0 mm, an outer diameter of 10.0 mm, a wall thickness of 1.0 mm, and a length of 4000 mm.
  • the density of the silicon carbide composite material cladding prepared in this embodiment is 99%, the cladding leakage rate is 10 -13 Pa ⁇ m 3 /s, the tensile strength is 300 MPa at room temperature, and the tensile strength is 350 MPa at a high temperature of 1200°C.
  • the raw materials of the slurry are: 89.7wt% silicon carbide fiber powder mixture, 10wt% organic solvent, 0.1wt% dispersant, 0.1wt% plasticizer, and 0.1wt% defoamer; the volume ratio of silicon carbide fiber in the silicon carbide fiber powder mixture is 10%, the diameter of the silicon carbide fiber is 0.01 ⁇ m, and the fiber aspect ratio is 1000.
  • the rest is the same as in Example 1, and the slurry is prepared.
  • the above slurry was prepared into a cladding green body by extrusion molding process, with an inner diameter of 7.9 mm, an outer diameter of 9.5 mm, a wall thickness of 0.8 mm, and a length of 4000 mm.
  • Degreasing was carried out under vacuum environment, and the degreasing process was heated to 500 ° C at a heating rate of 2 ° C / min and kept warm for 2 hours; after degreasing, high-temperature sintering was continued, and the sintering process was heated to 1200 ° C at a heating rate of 10 ° C / min; then heated to 1800 ° C at 5 ° C / min, kept warm for 2 hours, and the sintering atmosphere was argon. After sintering, a dense silicon carbide composite cladding was formed, with an inner diameter of 7.95 mm, an outer diameter of 9.5 mm, a wall thickness of 0.775 mm, and a length of 4000 mm.
  • the density of the silicon carbide composite material cladding prepared in this embodiment is 99%, the cladding leakage rate is 10 -12 Pa ⁇ m 3 /s, the tensile strength is 350 MPa at room temperature, and the tensile strength is 400 MPa at a high temperature of 1200°C.
  • the raw materials of the slurry are: 50wt% silicon carbide fiber powder mixture, 40wt% organic solvent, 2.5wt% dispersant, 3.5wt% plasticizer, 4.0wt% defoamer; the volume ratio of silicon carbide fiber in the silicon carbide fiber powder mixture is 50%, the diameter of the silicon carbide fiber is 1 ⁇ m, and the fiber aspect ratio is 10.
  • the rest is the same as in Example 1, and the slurry is prepared.
  • the above slurry was prepared into a cladding green body by extrusion molding process, with an inner diameter of 8.2 mm, an outer diameter of 11.0 mm, a wall thickness of 1.4 mm, and a length of 4000 mm.
  • Degreasing was carried out in a vacuum environment, and the degreasing process was heated to 800 ° C at a heating rate of 2 ° C / min and kept warm for 10 hours; after degreasing, high-temperature sintering was continued, and the sintering process was heated to 1200 ° C at a heating rate of 10 ° C / min; then heated to 2200 ° C at 5 ° C / min, kept warm for 2 hours, and the sintering atmosphere was argon. After sintering, a dense silicon carbide composite cladding was formed, with an inner diameter of 7.9 mm, an outer diameter of 9.9 mm, a wall thickness of 1.0 mm, and a length of 4000 mm.
  • the density of the silicon carbide composite material cladding prepared in this embodiment is 99%, the cladding leakage rate is 10 -13 Pa ⁇ m 3 /s, the tensile strength is 350 MPa at room temperature, and the tensile strength is 400 MPa at a high temperature of 1200°C.
  • the raw materials of the slurry are: 70wt% silicon carbide fiber powder mixture, 20wt% organic solvent, 3.5wt% dispersant, 3.5wt% plasticizer, and 3.0wt% defoamer; the volume ratio of silicon carbide fiber in the silicon carbide fiber powder mixture is 35%, the diameter of the silicon carbide fiber is 5 ⁇ m, and the fiber aspect ratio is 10.
  • the rest is the same as in Example 1, and the slurry is prepared.
  • the above slurry is prepared into a cladding green body through an extrusion molding process, with an inner diameter of 8.1mm, an outer diameter of 10.1mm, a wall thickness of 1.0mm, and a length of 4000mm.
  • Degreasing is carried out in a vacuum environment, and the degreasing process is to heat up to 600°C at a heating rate of 2°C/min and keep warm for 3h; after degreasing, high-temperature sintering is continued, and the sintering process is to heat up to 1200°C at a heating rate of 10°C/min; then heat up to 1850°C at 5°C/min, keep warm for 2h, and the sintering atmosphere is argon.
  • a dense silicon carbide composite cladding is formed, with an inner diameter of 8.0mm, an outer diameter of 9.8mm, a wall thickness of 0.9mm, and a length of 4000mm.
  • the density of the silicon carbide composite material cladding prepared in this embodiment is 99%, the cladding leakage rate is 10 -13 Pa ⁇ m 3 /s, the tensile strength is 325 MPa at room temperature, and the tensile strength is 350 MPa at a high temperature of 1200°C.

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
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Abstract

La présente invention concerne un gainage de matériau composite de carbure de silicium à haute densité et son procédé de préparation. Le procédé de préparation comprend les étapes suivantes : S1, préparation d'une bouillie ; S2, traitement et transformation de la bouillie en un corps cru de gainage de carbure de silicium ; et S3, dégraissage et frittage du corps cru de gainage de carbure de silicium pour former un gainage de carbure de silicium à haute densité. Dans le procédé de préparation du gainage de matériau composite de carbure de silicium à haute densité selon la présente invention, un mélange de poudre de fibre de carbure de silicium est coordonné avec un solvant organique, etc, pour préparer une bouillie, la bouillie est ensuite traitée et transformée en un corps cru de gainage, et des traitements de dégraissage et de frittage sont effectués pour préparer un gainage de carbure de silicium nanométrique ayant un super rapport longueur-diamètre, de telle sorte que la densité du gainage de carbure de silicium est améliorée, les défauts de pores sont réduits, et les sous-produits nocifs du gainage de carbure de silicium sont diminués ; un procédé de préparation du gainage est simplifié, et le rendement de production est amélioré ; et le coût de préparation est réduit.
PCT/CN2022/125203 2022-10-13 2022-10-13 Gainage de matériau composite de carbure de silicium à haute densité et son procédé de préparation WO2024077567A1 (fr)

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JP2002293636A (ja) * 2001-04-03 2002-10-09 Japan Science & Technology Corp ＳｉＣ繊維強化型ＳｉＣ複合材料のホットプレス製造方法
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CN103922746A (zh) * 2014-04-21 2014-07-16 哈尔滨工业大学 一种水基流延成型制备致密氮化硅陶瓷材料及致密异形氮化硅陶瓷材料的方法
CN106904984A (zh) * 2017-02-27 2017-06-30 中国核动力研究设计院 一种SiC短纤维复合材料及复合包壳管及其制备方法
CN106977217A (zh) * 2016-06-03 2017-07-25 北京航空航天大学 一种高强高韧性碳化硅纤维增强碳化硅陶瓷基复合材料的制备方法
JP2018199588A (ja) * 2017-05-25 2018-12-20 イビデン株式会社 ＳｉＣ／ＳｉＣ複合材の製造方法
CN113563082A (zh) * 2021-08-06 2021-10-29 中国建筑材料科学研究总院有限公司 薄壁碳化硅陶瓷换热管及其制备方法和应用

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002293636A (ja) * 2001-04-03 2002-10-09 Japan Science & Technology Corp ＳｉＣ繊維強化型ＳｉＣ複合材料のホットプレス製造方法
CN1600744A (zh) * 2004-10-13 2005-03-30 中国科学院上海硅酸盐研究所 短纤维增强碳化硅基复合材料的制备方法
CN101580390A (zh) * 2008-05-15 2009-11-18 中国科学院金属研究所 一种碳化硅陶瓷管状制品及其制备方法
CN103922746A (zh) * 2014-04-21 2014-07-16 哈尔滨工业大学 一种水基流延成型制备致密氮化硅陶瓷材料及致密异形氮化硅陶瓷材料的方法
CN106977217A (zh) * 2016-06-03 2017-07-25 北京航空航天大学 一种高强高韧性碳化硅纤维增强碳化硅陶瓷基复合材料的制备方法
CN106904984A (zh) * 2017-02-27 2017-06-30 中国核动力研究设计院 一种SiC短纤维复合材料及复合包壳管及其制备方法
JP2018199588A (ja) * 2017-05-25 2018-12-20 イビデン株式会社 ＳｉＣ／ＳｉＣ複合材の製造方法
CN113563082A (zh) * 2021-08-06 2021-10-29 中国建筑材料科学研究总院有限公司 薄壁碳化硅陶瓷换热管及其制备方法和应用

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