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Preparation method for ZrO2 fiber with SiO2 doped

A fiber and continuous fiber technology, which is applied in the field of preparation of ZrO2 polycrystalline continuous fiber, can solve the problems of difficulty in preparation of inorganic polyzirconium solution, insufficient density of zirconia fiber, and decrease in fiber strength, so as to expand the use temperature range and spinning performance Excellent, good high temperature mechanical properties

Active Publication Date: 2014-11-12
南京理工宇龙新材料科技股份有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the preparation of inorganic polyzirconium solution is difficult
[0017] In the process of preparing zirconia fiber precursors by impregnation method, organic polyzirconium method, sol-gel method, etc., a large amount of organic matter and water are contained. During the sintering process, a large amount of volatile matter is discharged, resulting in insufficient density of zirconia fibers and tensile strength. The strength is low, and the fiber strength of zirconia fiber drops sharply as the temperature rises (above 900°C).

Method used

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  • Preparation method for ZrO2 fiber with SiO2 doped
  • Preparation method for ZrO2 fiber with SiO2 doped
  • Preparation method for ZrO2 fiber with SiO2 doped

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 400g basic zirconium carbonate with an electronic scale and pour it into the reaction kettle. Measure 160ml of glacial acetic acid with a graduated cylinder (100g of basic zirconium carbonate is dissolved in 40ml of glacial acetic acid), pour it into the reaction kettle, and add 250ml of distilled water, the reaction produces a lot of bubbles, after a period of time, filter to obtain a colorless and transparent zirconium acetate solution .

[0034] According to ZrO 2 :SiO2 2 The mass ratio of the chemical composition is 95:5. Measure 31ml of tetraethyl orthosilicate (TEOS), add the blend of TEOS and absolute ethanol to the mixed solution of nitric acid and acetic acid, and TEOS will be hydrolyzed rapidly under acidic conditions. , to obtain a silicic acid solution. The volume ratio of TEOS, absolute ethanol, concentrated nitric acid, acetic acid and water is 10:5:1:1:15. At the same time, the silicic acid solution should be used as soon as possible, so as not ...

Embodiment 2

[0039] Weigh 200g basic zirconium carbonate with an electronic scale and pour it into the reaction kettle. Measure 72ml of glacial acetic acid with a graduated cylinder (100g of basic zirconium carbonate is dissolved in 36ml of glacial acetic acid), pour it into the reaction kettle, and add 150ml of distilled water. The reaction produced a large number of bubbles, and after a period of time, a colorless and transparent zirconium acetate solution was obtained by filtration.

[0040] According to ZrO 2 :SiO2 2 The chemical composition of the mass ratio is 92.2:7.8, measure 25ml of tetraethyl orthosilicate (TEOS), add the blend of TEOS and absolute ethanol to the mixed solution of concentrated nitric acid and acetic acid, stir for 0.5h, TEOS Rapid hydrolysis under acidic conditions to obtain silicic acid solution. The volume ratio of TEOS, absolute ethanol, concentrated nitric acid, acetic acid and water is 10:5:1:1:15. Add the obtained silicon solution to the prepared zircon...

Embodiment 3

[0044] Prepare colorless and transparent zirconium acetate solution and silicic acid solution according to Example 1. Follow Y 2 o 3 The amount of ZrO 2 2mol% of the content, measure 17.6g of yttrium acetate (molecular formula is Y(Ac) 3 4H 2 O), in ZrO 2 During the phase transition process, using Y 2 o 3 as ZrO 2 stabilizer. Add the silicic acid sol to the prepared zirconium acetate solution, then add yttrium acetate to the mixed solution of the two, and finally add 20ml of glacial acetic acid as a colloidal stabilizer and spinning aid, and stir the acetic acid with a magnetic stirrer. Yttrium dissolves completely. After vacuum concentration at 67°C for 2-2.5 hours, a precursor colloid with a viscosity of about 23-32 Pa.s is produced.

[0045]Centrifugal spinning on a self-made centrifugal spinning machine. Under the action of centrifugal force, the precursor colloid is centrifugally thrown out from a small hole with a diameter of 0.5mm at high speed, and then secon...

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Abstract

The invention discloses a preparation method for a ZrO2 fiber with SiO2 doped. A ZrO2-SiO2 fiber is prepared with basic zirconium carbonate (>=40%ZrO2) as a zirconium source, TEOS as a silicon source and acetic acid as stabilizers and spinning auxiliaries by means of a sol-gel method and a centrifugal spinning technology. The method is characterized in that a preparation method for a complex fiber includes the steps of precursor colloid preparation, centrifugal spinning and thermal treatment, so that the ZrO2-SiO2 composite fiber is obtained. The ZrO2-SiO2 fiber has the lowest heat conductivity coefficient, ZrO2 has high melting point, and therefore the ZrO2-SiO2 fiber can be used as a novel high-temperature thermal insulation material. Because the Y2O3 stabilized high-purity ZrO2 fiber is high in high temperature (>=1000 DEG C) pulverization rate and poor in fiber strength, growth of ZrO2 grains can be restrained by adding of a proper amount of SiO2, compared with those of pure YSZ fibers, high temperature mechanical properties of the ZrO2-SiO2 fiber are better, and the using temperature range of the YSZ fibers is expanded. Meanwhile, fiber density is lowered, so that the ZrO2 fiber has good shrinkage resistance and thermal shock resistance and is an ideal light high-temperature thermal insulation material.

Description

technical field [0001] The invention belongs to the technical field of heat insulation of refractory materials, in particular to a 2 Doped ZrO 2 Process for the preparation of polycrystalline continuous fibers. Background technique [0002] Refractory ceramic fiber has become a research and development hotspot because of its excellent thermal insulation performance. C fiber is a kind of thermal insulation material with excellent performance. In non-oxidizing atmosphere, the service temperature can reach 1400℃, but it cannot be used in redox atmosphere for a long time. Alumina or mullite fiber is also an excellent fire-resistant and heat-insulating material. Can be reused in redox atmosphere. Compared with other oxide fibers, zirconia ceramic fiber has the advantages of high melting point (2710±15°C), minimum thermal conductivity, low high-temperature vapor pressure, and chemical corrosion resistance. It is a new type of high-temperature heat-resistant insulation material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08C04B35/48C04B35/622
Inventor 刘和义乔健朱玉龙黄振进崔宏亮
Owner 南京理工宇龙新材料科技股份有限公司
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