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Method for preparing multi-hollow zirconium oxide fiber by using cotton fiber

A technology of zirconia fiber and cotton fiber, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of easy formation of broken filaments, inconsistent hollow structure, and many gaps between zirconia grains, so as to prevent infrared energy. The effect of loss, excellent thermal insulation performance, and excellent thermal insulation performance

Inactive Publication Date: 2017-06-13
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the preparation of zirconia fibers by impregnation method is simple and easy to realize, but its disadvantage is that the zirconium content in the zirconium precursor is too low, while the content of organic components is very high, so it will be in the whole sintering process. The volume shrinkage is large, and the decomposition of organic matter leads to more gaps between the grains of zirconia, so the prepared fiber structure is relatively loose, the strength is also low, and the prepared fiber only has a small number of hollow structures.
The zirconia fiber is prepared by electrospinning, and the fiber length is guaranteed, but due to the different process parameters of the experimental equipment, it is easy to form broken filaments during the production process, and the process of making glue is also cumbersome and complicated, and the hollow structure appears Inconsistent, uneven wall thickness
Sol-gel method, due to the high content of zirconium in the precursor, the defects of fiber performance caused by the decomposition of organic matter will be relatively small, and the strength of zirconia fibers prepared by this method is relatively high, but in this method, The sol system is relatively unstable, and it is easy to spontaneously turn into a gel, which will lose the spinning performance and affect the quality of the obtained fiber. Moreover, no zirconia fiber with a hollow structure has been prepared by the sol-gel method for the time being.

Method used

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  • Method for preparing multi-hollow zirconium oxide fiber by using cotton fiber
  • Method for preparing multi-hollow zirconium oxide fiber by using cotton fiber
  • Method for preparing multi-hollow zirconium oxide fiber by using cotton fiber

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation mass percent concentration is 4% zirconium oxychloride solution, namely zirconium oxychloride solid (ZrOCl2 8H2O) 4.71g, yttrium nitrate (Y(NO3)3 6H2O) 0.353g, tin chloride (SnCl4 5H2O) 0.3 g, polyvinylpyrrolidone (PVPK-30) 0.375g, i.e. tin tetrachloride: polyvinylpyrrolidone (S / P value) is 0.8:1, the zirconium oxychloride impregnation salt solution that solvent distilled water 60ml configures, after drying Soak the cotton fibers in the solution for 10 minutes, and stir slightly to speed up the dispersion of the solution in the cotton. The soaked cotton fibers are squeezed out of the excess solution in the filter screen, and then put into a drying box at 50 Dry in the temperature range of ℃ for 12 hours, put the dried cotton in a crucible, sinter in an electric furnace at a temperature of 1300 ℃ with a heating rate of 10 ℃ / min, and keep it warm for 2 hours to obtain a cotton fiber-like ZrO2 multi-hollow fiber Material.

[0030] figure 1 It is the result of...

Embodiment 2

[0032]Preparation mass percent concentration is 6% zirconium oxychloride solution, namely zirconium oxychloride solid (ZrOCl2 8H2O) 7.35g, yttrium nitrate (Y(NO3)3 6H2O) 0.551g, tin chloride (SnCl4 5H2O) 0.3 g, polyvinylpyrrolidone (PVPK-30) 0.60g, that is, the S / P value is 0.5:1, the zirconium oxychloride impregnated salt solution prepared by solvent distilled water 60ml, soak the dried cotton fibers in the solution for 20 minutes, And add slight stirring to speed up the dispersion speed of the solution in the cotton. Squeeze the soaked cotton fibers to remove the excess solution in the filter screen, then put them into a drying oven and dry them at a temperature range of 70°C for 12 hours. The finished cotton was placed in a crucible, sintered in an electric furnace at a temperature of 700°C with a heating rate of 3°C / min, and kept for 1 hour to obtain a cotton fiber-like ZrO2 multi-hollow fiber material.

[0033] Figure 6 Shown is the zirconia X-ray diffraction pattern ob...

Embodiment 3

[0035] Preparation mass percent concentration is 8% zirconium oxychloride solution, namely zirconium oxychloride solid (ZrOCl2 8H2O) 10.21g, yttrium nitrate (Y(NO3)3 6H2O) 0.735g, tin chloride (SnCl4 5H2O) 0.5 g, polyvinylpyrrolidone (PVPK-30) 0.25g, that is, the S / P value is 2.4:1, the zirconium oxychloride impregnated salt solution prepared by solvent distilled water 60ml, soak the dried cotton fibers in the solution for 30 minutes, And add slight stirring to speed up the dispersion speed of the solution in the cotton. Squeeze the soaked cotton fibers to remove the excess solution in the filter screen, then put them into a drying oven and dry them at a temperature range of 70°C for 12 hours. The finished cotton was placed in a crucible, sintered in an electric furnace at a temperature of 800°C with a heating rate of 1°C / min, and kept at a temperature of 2 hours to obtain a cotton fiber-like ZrO2 multi-hollow fiber material.

[0036] Figure 8 Shown is that the mass concentr...

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Abstract

The invention discloses a method for preparing multiple hollow zirconia fibers from cotton fibers. The method uses natural cotton fiber as a template, and zirconium oxychloride-based zirconium-containing salt solution as an impregnating solution. By controlling the ratio of the additive tin tetrachloride in the salt solution to the active agent polyvinylpyrrolidone, the cotton fiber is soaked The multi-hollow zirconia fiber material maintaining the cotton fiber structure is prepared by immersing in the impregnating solution, drying and sintering at high temperature. The method of the invention is simple and low in cost, and can effectively control the size and shape of the hollow fiber. The prepared zirconia fiber has the fiber morphology of cotton, and most of them are hollow fibers. The prepared hollow zirconia fiber material is beneficial to prevent air Convection prevents the loss of infrared energy of objects and has more excellent heat insulation performance.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a method for preparing zirconia fibers, in particular to a method for preparing multi-hollow zirconia fibers with cotton fibers. Background technique [0002] Zirconium dioxide (ZrO2) has good chemical and thermal stability, excellent high-temperature electrical conductivity, high high-temperature strength and toughness, good corrosion resistance and stability. Among them, fibrous ZrO2 is mainly used in aerospace, national defense, atomic energy and other fields, for ultra-high temperature heat insulation protection materials and ceramic matrix composite reinforcement materials; in ceramic sintering, metal smelting, pyrolysis, semiconductor manufacturing, quartz melting and other fields , used to manufacture ultra-high temperature industrial kilns, ultra-high temperature experimental electric furnaces and other ultra-high temperature heating devices that can withstand ...

Claims

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Application Information

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IPC IPC(8): D01F9/10
CPCD01F9/10
Inventor 王天驰李金金余沁堃彭芃司楠李晓彤
Owner NANJING UNIV OF SCI & TECH
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