WO2019019365A1 - Procédé pour la préparation de fibre céramique continue composite d'alumine-zircone - Google Patents

Procédé pour la préparation de fibre céramique continue composite d'alumine-zircone Download PDF

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WO2019019365A1
WO2019019365A1 PCT/CN2017/104315 CN2017104315W WO2019019365A1 WO 2019019365 A1 WO2019019365 A1 WO 2019019365A1 CN 2017104315 W CN2017104315 W CN 2017104315W WO 2019019365 A1 WO2019019365 A1 WO 2019019365A1
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alumina
temperature
composite ceramic
fiber
continuous fiber
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English (en)
Chinese (zh)
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陈代荣
孟强
贾玉娜
焦秀玲
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Shandong University
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Shandong University
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C04B35/62236—Fibres based on aluminium oxide
    • 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
    • C04B35/624—Sol-gel processing
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • USP 5002906 reports an alumina-zirconia ceramic
  • the method for preparing fiber the method firstly polymerizing alumina powder and aluminum chloride at 30-60 ° C, then adding zirconium salt aqueous solution, stirring uniformly, and then concentrating, spinning and heat-treating to obtain alumina-zirconia composite ceramic Fiber, the method is difficult to achieve uniformity in the mixing of aluminum and zirconium, and the properties of the sol are unstable;
  • CN1379130A discloses a method for preparing an alumina-zirconia ceramic fiber, which is mainly composed of inorganic aluminum salt, zirconium salt and metal aluminum.
  • Zirconium acetate and zirconium oxychloride were used as raw materials, polyvinyl alcohol was used as spinning aid, alumina-zirconia precursor fiber spinning solution was prepared by sol-gel method, and gel fiber was prepared by high speed centrifugal twisting machine. (See: Material Guide B 2015, 29, 68).
  • the above three methods adopt the blowing method or the centrifugal spinning technology, and the prepared ceramic fibers are all short fibers, and the preparation of continuous fibers cannot be realized.
  • Tan Hongbin et al. used aluminum nitrate, zirconium oxychloride and tartaric acid as raw materials, and polyvinylpyrrolidone as a spinning aid.
  • the zirconia/alumina composite ceramic fiber was prepared by sol-gel method.
  • the present invention provides a high strength, uniform diameter, and length
  • the method for preparing the alumina-zirconia composite ceramic continuous fiber comprises the following steps:
  • the gel fiber obtained in the step (2) is dried at 50-70 ° C, and then heated to a temperature of 400-500 ° C at a rate of 0.5-3 ° C / min, at this temperature for 0.5-2 h; and then at 2-5 ° C /
  • the speed of min is raised to 700-850 ° C, and the temperature is kept at 0.5-1 h.
  • the temperature is raised to 1200-1400 ° C at a rate of 8-10 ° C / min, and the temperature is maintained at 0.5-2 h to obtain Al 2 O 3 -ZrO. 2 composite ceramic continuous fiber.
  • the cerium nitrate of the present invention is added in order to prevent the fiber crystal grains from rapidly increasing at a high temperature, resulting in a decrease in fiber strength.
  • the addition of cerium nitrate too low or too high is detrimental to the increase in fiber strength.
  • the alumina-zirconia composite ceramic continuous fiber prepared by the invention has uniform diameter, small thermal conductivity, compact internal structure, good flexibility, high bending strength and fracture toughness, and high temperature treatment.
  • the tensile strength of the fiber monofilament can reach 2.54 GPa.
  • Figure 4 is a high magnification SEM photograph of an alumina-zirconia composite ceramic continuous fiber obtained in Example 4 of the present invention.
  • Step (2) is the same as in Embodiment 2.
  • the SEM photograph of the Al 2 O 3 -ZrO 2 composite ceramic continuous fiber obtained in this example is shown in Fig. 3, and the SEM photograph of the high magnification is shown in Fig. 4, and the SEM photograph of the fiber cross section is shown in Fig. 5.
  • the fiber diameter is uniform and the internal structure is tight, and the number of pores between the crystal grains is small, which is advantageous for improving the mechanical strength of the fiber.
  • a method for preparing an alumina-zirconia composite ceramic continuous fiber comprises the following steps:
  • the spinning solution was added to a rotary steaming flask, the aging temperature was set to 45 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the aging was carried out to a viscosity of 395 Pa ⁇ s to obtain a spinnable precursor sol.
  • Step (2) is the same as in Embodiment 2.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Fibers (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

L'invention concerne un procédé pour la préparation d'une fibre céramique continue composite d'alumine-zircone. Le procédé consiste à préparer un sol de précurseur filable à l'aide d'un sol d'alumine contenant des particules colloïdales d'Al13, une nanodispersion de γ-AlOOH, de l'acétate de zirconium, du nitrate d'yttrium et du poly(alcool vinylique) (PVA) ; préparer une fibre gélatineuse à l'aide d'une technique de filage à sec ; et la soumettre à un traitement thermique pour obtenir la fibre céramique continue composite d'alumine-zircone.
PCT/CN2017/104315 2017-07-28 2017-09-29 Procédé pour la préparation de fibre céramique continue composite d'alumine-zircone Ceased WO2019019365A1 (fr)

Applications Claiming Priority (2)

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CN201710632579.7 2017-07-28
CN201710632579.7A CN107266081B (zh) 2017-07-28 2017-07-28 一种氧化铝-氧化锆复合陶瓷连续纤维的制备方法

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110863265A (zh) * 2019-09-06 2020-03-06 青岛中科星熠高新技术研究院有限公司 一种连续陶瓷纤维的制备方法

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CN107986797A (zh) * 2017-12-11 2018-05-04 苏州图纳新材料科技有限公司 固态复合陶瓷前驱体、复合纤维棉及其制备方法
CN111001399A (zh) * 2019-12-23 2020-04-14 武汉纺织大学 一种用于窗纱纱网的具有光催化功能的陶瓷纤维及其制备方法
CN111074426B (zh) * 2019-12-26 2024-01-19 山东鲁阳浩特高技术纤维有限公司 一种氧化铝-氧化锆复合纤维毯及其制备方法
CN113968974B (zh) * 2020-07-22 2022-07-19 中国科学院化学研究所 一种Al-Zr共聚氧化物陶瓷前驱体及其制备方法
CN112779674B (zh) * 2020-12-28 2023-01-24 山东鲁阳浩特高技术纤维有限公司 一种氧化锆-氧化铝纤维复合纤维毯及其制备方法
CN114687007A (zh) * 2022-03-25 2022-07-01 中国民航大学 一种静电纺丝制备氧化铝-氧化锆气凝胶纤维的生产方法
CN115073151A (zh) * 2022-06-21 2022-09-20 重庆德强化工有限公司 陶瓷纤维气凝胶及其制备方法
CN115262033B (zh) * 2022-06-27 2024-06-28 东华大学 一种致密连续α-氧化铝纤维材料的制备方法
CN115233336B (zh) * 2022-06-27 2024-07-23 东华大学 一种均匀致密的高温连续氧化锆长丝的制备方法
CN115852528B (zh) * 2022-06-27 2024-05-31 东华大学 一种规模化生产连续钇铝石榴石长丝的方法
CN116178024B (zh) * 2023-02-28 2024-07-05 山东创新精密科技有限公司 一种复合多孔陶瓷增强铝合金材料
CN117265696B (zh) * 2023-09-05 2025-08-12 南京邮电大学 一种锆原位掺杂的连续式氧化铝陶瓷纤维的制备方法
CN117702306A (zh) * 2023-12-13 2024-03-15 中南大学 一种连续氧化铝-氧化锆复合陶瓷纤维及其制备方法

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EP0257969A2 (fr) * 1986-08-20 1988-03-02 E.I. Du Pont De Nemours And Company Fibre d'oxyde d'aluminium modifié par l'oxyde de zirconium
US5002906A (en) * 1989-09-29 1991-03-26 E. I. Du Pont De Nemours And Company Process for making modified alumina fibers
US5244477A (en) * 1989-04-28 1993-09-14 Norton Company Sintered sol gel alumina abrasive filaments
JPH09291421A (ja) * 1996-04-22 1997-11-11 Isolite Kogyo Kk アルミナジルコニア繊維及びその製造方法
CN106927808A (zh) * 2017-04-10 2017-07-07 山东大学 一种钇铝石榴石连续纤维的制备方法

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CN1137297C (zh) * 2001-04-09 2004-02-04 中国科学院山西煤炭化学研究所 一种氧化铝-氧化锆纤维的制备方法
CN103408292B (zh) * 2013-07-26 2014-11-05 山东大学 一种氧化铝-氧化锆陶瓷纤维的制备方法
JP6238286B2 (ja) * 2013-11-14 2017-11-29 国立研究開発法人物質・材料研究機構 ジルコニア連続繊維とその製造方法

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EP0257969A2 (fr) * 1986-08-20 1988-03-02 E.I. Du Pont De Nemours And Company Fibre d'oxyde d'aluminium modifié par l'oxyde de zirconium
US5244477A (en) * 1989-04-28 1993-09-14 Norton Company Sintered sol gel alumina abrasive filaments
US5002906A (en) * 1989-09-29 1991-03-26 E. I. Du Pont De Nemours And Company Process for making modified alumina fibers
JPH09291421A (ja) * 1996-04-22 1997-11-11 Isolite Kogyo Kk アルミナジルコニア繊維及びその製造方法
CN106927808A (zh) * 2017-04-10 2017-07-07 山东大学 一种钇铝石榴石连续纤维的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110863265A (zh) * 2019-09-06 2020-03-06 青岛中科星熠高新技术研究院有限公司 一种连续陶瓷纤维的制备方法

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