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Preparation method of tin oxide fiber precursor and tin oxide crystal fibers

A precursor fiber and crystal fiber technology, applied in the direction of tin oxide, inorganic raw material artificial filament, etc., can solve the problems of poor fiber strength, easy pulverization, loose and porous, etc., and achieve high mass production efficiency, soft luster, and uniform diameter Effect

Active Publication Date: 2015-06-10
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the preparation of tin oxide fibers by electrospinning has relatively low requirements for the precursors of the target elements, but the molar content of the target elements in the spinning solution is low. In the existing literature reports, the precursor fibers are simply subjected to high temperature Aerobic treatment causes problems such as poor morphology, uneven crystal grains, loose and porous fibers, poor fiber strength, and easy pulverization of existing tin oxide fibers. It is difficult to realize industrial production, which limits the application of tin oxide fibers

Method used

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  • Preparation method of tin oxide fiber precursor and tin oxide crystal fibers
  • Preparation method of tin oxide fiber precursor and tin oxide crystal fibers
  • Preparation method of tin oxide fiber precursor and tin oxide crystal fibers

Examples

Experimental program
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Effect test

Embodiment 1

[0053] (1) Synthesis of tin oxide fiber precursor

[0054] Weigh 100.0 g of anhydrous tin tetrachloride, dissolve it in 400 ml of methanol, stir until fully dissolved, and mark the resulting solution as liquid A. Weigh 96.0g of sodium acetate, dissolve it in 450ml of methanol, add 10g of deionized water, stir until fully dissolved, and mark the resulting solution as B solution. Add solution A dropwise to solution B at 30°C The time is 30min. Stir continuously during the dropwise addition and continue to stir for 1h after the dropwise addition. After stopping the stirring, let the reaction solution stand at room temperature for 12h, filter, the precipitate is sodium chloride, and the filtrate is the tin oxide fiber precursor solution .

[0055] (2) Concentration of fiber spinning solution

[0056] The tin oxide fiber precursor solution was distilled under reduced pressure at 38°C, concentrated to obtain a uniform light yellow spinning solution with a viscosity of 40 Pa·S, and...

Embodiment 2

[0063] As described in Example 1, the difference is that the methanol solvent in step (1) was replaced with absolute ethanol. That is, weigh 100.0 g of anhydrous tin tetrachloride, dissolve it in 300 ml of absolute ethanol, add 7.0 g of water, stir until fully dissolved, and mark the resulting solution as liquid A. Weigh 110.0g of sodium acetate and dissolve it in 350ml of absolute ethanol. The resulting solution is marked as solution B. Add solution B dropwise to solution A at a temperature of 70°C for 40 minutes. Stir continuously during the dropwise addition. And continue to stir for 1 h after the dropwise addition, stop the stirring and let the reaction solution stand at room temperature for 12 h. Adjust the viscosity of the spinning solution in step (2) to 25Pa·S, and adjust the standing time to 2h. In step (3), the motor speed is 16000r / min, the temperature in the spinning room is 28°C, and the relative humidity is adjusted to 40%. Set the heating rate under the water ...

Embodiment 3

[0066] As described in Example 1, the difference is that the methanol solvent in step (1) is replaced by n-propanol. Dissolve 100g of anhydrous tin tetrachloride in 600ml of propanol, dissolve 110.0g of sodium acetate in 750ml of propanol, weigh 100.0g of anhydrous tin tetrachloride, dissolve it in 600ml of propanol, and add 7.8g water, stirred until fully dissolved, and the resulting solution was marked as liquid A. Weigh 110.0g of sodium acetate, dissolve it in 750ml of propanol, and stir until fully dissolved. The resulting solution is marked as B solution. At 30°C, drop solution B and solution A into the container at the same time, and the dropping time is 30min. , Stir continuously during the dropwise addition and continue to stir for 1h after the dropwise addition, stop stirring and let the reaction solution stand at room temperature for 11h.

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Abstract

The invention relates to a preparation method of a tin oxide fiber precursor and tin oxide crystal fibers. The preparation method comprises the following steps: carrying out a replacement reaction on halides of tin and potassium (sodium) acetate to synthesize the tin oxide fiber precursor which takes acetic acid as a ligand; concentrating a precursor solution to obtain a spinning solution and carrying out centrifugal silk spinning to obtain tin oxide precursor fibers; and carrying out procedures of special atmosphere pre-treatment, high-temperature heat treatment and the like on the precursor fibers to obtain the tin oxide crystal fibers. According to the preparation method, the long-diameter ratio of the tin oxide crystal fibers is greater than 1000, the tensile strength of the fibers is 0.8GPa-1.1GPa, the whiteness of the fibers is good and the color and luster of the fibers are soft. The preparation method is simple in preparation process, moderate in condition and stable in quality of fibers in batches; spinning sol does not go bad after being placed for a long time. The tin oxide crystal fibers can be applied to the fields of photocatalysis, air sensitivity, humidity sensitivity and the like. The tin oxide fiber precursor can also be used for preparing oxide thin films, nano powder and nano wires or preparing tin-containing functional materials including nano tin oxide fibers and the like by an electrostatic spinning method.

Description

technical field [0001] The invention relates to a tin oxide fiber precursor and a tin oxide crystal fiber preparation method, belonging to the technical field of semiconductor oxide material preparation. Background technique [0002] Tin dioxide is a wide bandgap semiconductor oxide with a bandgap width of 3.6eV, and its tetragonal crystal system is also called rutile type. The stable crystalline tin dioxide belongs to the rutile structure and is tetragonal P4 2 / mnm space group, a 0 =0.4738nm, c 0 =0.3188nm, Z=2. In the actual synthesis process, tin dioxide material has oxygen vacancies due to oxygen deficiency, so it exhibits the nature of n-type semiconductor. Tin dioxide material has been widely used because of its excellent performance in optics, electricity, catalysis, gas sensitivity, pressure sensitivity, heat sensitivity and humidity sensitivity. [0003] Tin oxide crystal fiber is a kind of fiber material with polycrystalline structure. Its crystal grain size ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08C01G19/02
Inventor 林学军许东王新强朱陆益张光辉刘雪松刘本学蔡宁宁
Owner SHANDONG UNIV
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