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Preparation method of alumina-zirconia composite staple fibers and preparation method thereof

A technology of zirconia and alumina, which is applied in the field of alumina-zirconia composite short fiber and its preparation, can solve the problems of high price, difficulty in mixing aluminum and zirconium, and unsuitability for industrial production, so as to ensure stability , the effect of improving stability

Active Publication Date: 2020-04-28
山东鲁阳浩特高技术纤维有限公司
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Problems solved by technology

[0004] The aluminum source and zirconium source used in the above-mentioned alumina / zirconia composite fiber are both organic matter, which is expensive and not suitable for industrial production
USP5002906A discloses a method for preparing alumina-zirconia ceramic fibers. In this method, alumina powder and aluminum chloride are polymerized at 30-60°C, then zirconium aqueous solution is added, stirred evenly, concentrated and spun , heat treatment to obtain alumina-zirconia composite ceramic fibers, the mixing of aluminum and zirconium in this method is difficult to achieve uniformity, making the properties of the sol unstable; CN1379130A discloses a preparation method of alumina-zirconia ceramic fibers, which uses inorganic Aluminum salt, zirconium salt and metal aluminum are the main raw materials. The precursor sol is prepared under reflux conditions. Water-soluble polymers are added as spinning aids. After concentration, the silk stock solution is obtained, and the gel fiber (sol- Gel one-step method, spraying into fiber, this method is difficult to achieve uniform mixing of aluminum and zirconium, making the properties of the sol unstable); Qiao Jian et al. used inorganic aluminum chloride, aluminum powder, basic zirconium carbonate, yttrium acetate and acetic acid As raw materials, AlO was prepared by sol-gel method and centrifugal spinning technique 3 -ZrO 2 (3mol%Y2O3) composite ceramic fiber, the maximum length of the gel fiber is up to 70cm, after treatment at 1200 ℃, it is completely transformed into α-alumina (α-Al2O3) and tetragonal zirconia (t-ZrO2) (see: Journal of Synthetic Crystals) 2014, 43, 3163), the above-mentioned preparation method has the existence of aluminum powder to produce hydrogen, and the phenomenon of sol instability occurs, and a crystal phase stabilizer needs to be added

Method used

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preparation example Construction

[0025] The preparation method of alumina-zirconia composite fibers in the prior art uses organic aluminum sources and organic zirconium salts to prepare alumina-zirconia composite sols, which is expensive and not suitable for industrial production. Instead, inorganic aluminum sources and inorganic zirconium salts are used. The sol prepared by the sol-gel one-step method is unstable. In view of the above-mentioned technical problems, the application provides a method for preparing alumina-zirconia composite short fibers. The preparation method adopts a single inorganic aluminum source and an inorganic zirconium salt. Moreover, the stability of the sol spinning solution is improved by using the method of first gelling and then degumming. Specifically, the application provides a method for preparing alumina-zirconia composite short fibers, comprising the following steps:

[0026] A) heating the aluminum powder, hydrochloric acid and water to reflux to obtain a polyaluminum chlori...

Embodiment 1

[0044] (1) Heat aluminum powder, hydrochloric acid and distilled water at a molar ratio of 1.7:1:19.5 to reflux at 100°C to obtain Al 2 o 3 The polyaluminum chloride sol with a content of 22wt% was cooled to room temperature for later use; zirconium oxychloride (35.5% zirconia content) was prepared as a solution with a mass fraction of 50%; at room temperature, the mass ratio of alumina to zirconia was 1.5:1 , pour the zirconium oxychloride solution into the polymerized alumina sol, and with the increase of the added amount of the zirconium oxychloride solution, the zirconium-aluminum gel will appear slowly; When the glue is complete, heat it in a water bath at 40°C;

[0045] (2) Acetic acid is configured as a 50% solution, and acetic acid is added to the above-mentioned gel to degelatinize according to 6% of the sum of the quality of aluminum oxide in polyaluminium chloride and zirconium oxide in the zirconium source;

[0046] (3) slowly dissolving the spinning aid (polyvin...

Embodiment 2

[0052] (1) Heat aluminum powder, hydrochloric acid and distilled water at a molar ratio of 1.7:1:19.5 to reflux at 100°C to obtain Al 2 o 3 The polyaluminum chloride sol with a content of 22wt% was cooled to room temperature for later use; zirconium oxychloride (35.5% zirconia content) was prepared as a solution with a mass fraction of 50%; at room temperature, the mass ratio of alumina to zirconia was 1.5:1 , pour the zirconium oxychloride solution into the polymerized alumina sol, and with the increase of the added amount of the zirconium oxychloride solution, the zirconium-aluminum gel will appear slowly; When the glue is complete, heat it in a water bath at 40°C;

[0053] (2) Acetic acid is configured as a 50% solution, and acetic acid is added to the above-mentioned gel to degelatinize according to 6% of the sum of the quality of aluminum oxide in polyaluminium chloride and zirconium oxide in the zirconium source;

[0054] (3) slowly dissolving the spinning aid (polyvin...

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Abstract

The invention provides a preparation method of alumina-zirconia composite staple fibers. The preparation method comprises the following steps of A) preparing poly aluminum chloride sol; mixing a zirconium oxychloride solution and the poly aluminum chloride sol to obtain zirconium-aluminum gel; B) peptizing the zirconium-aluminum gel to obtain a zirconium-aluminum solution; C) mixing the zirconium-aluminum solution with an aqueous solution of a spinning auxiliary agent, and performing distilling and concentrating to obtain a zirconium-aluminum composite spinning solution; D) aging the zirconium-aluminum composite spinning solution, and then throwing threads to form fibers to obtain precursor fibers; and E) carrying out heat treatment on the precursor fibers to obtain the alumina-zirconia composite staple fibers. According to the preparation method of the alumina-zirconia composite staple fibers in the invention, a single inorganic aluminum source and an inorganic zirconium salt are usedfor reaction, and the characteristics of firstly gelling and then peptizing are utilized, so that the stability of the sol spinning solution is improved without the need of adding an additional stabilizing auxiliary agent an crystal grain inhibitor, and the method is simple and safe and is suitable for preparing the alumina-zirconia composite staple fibers in industrial production.

Description

technical field [0001] The invention relates to the technical field of composite fibers, in particular to an alumina-zirconia composite short fiber and a preparation method thereof. Background technique [0002] Alumina / zirconia composite fiber (hereinafter referred to as Al 2 o 3 / ZrO 2 Fiber) has higher temperature resistance than alumina fiber, higher flexural strength and fracture toughness than zirconia fiber; and has been developed and commercialized by DuPont of the United States, named PRD-166 fiber, which contains 80% oxide Aluminum, 20% zirconia and a small amount of yttrium. After testing, the high temperature resistance, mechanical and physical properties of alumina / zirconia composite fibers are superior to other metal and ceramic materials. [0003] In view of the above-mentioned advantages of alumina / zirconia composite fibers, researchers have started extensive research. In the presence of nitric acid, J.Chandradass et al. dissolved aluminum isopropoxide i...

Claims

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Application Information

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IPC IPC(8): D01F9/08
CPCD01F9/08
Inventor 傅超郑维金岳耀辉鹿明王成龙
Owner 山东鲁阳浩特高技术纤维有限公司
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