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

A technology of precursor fiber and crystal fiber, which is applied in the direction of tin oxide, artificial filament of inorganic raw materials, etc., can solve the problems of poor fiber strength, uneven grain, easy pulverization, etc., and achieve high mass production efficiency and good whiteness , the effect of uniform diameter

Active Publication Date: 2014-02-05
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 the obtained solution is marked as liquid A. Weigh 96.0g of sodium acetate, dissolve it in 450ml of methanol, add 10g of deionized water, stir until fully dissolved, the obtained solution is marked as B solution, at 30 ℃ temperature, solution A is added dropwise to solution B, dropwise added The time is 30min, the stirring is continued during the dropping process and the stirring is continued for 1 h after the dropping is completed. After the stirring is stopped, the reaction solution is allowed to stand at room temperature for 12 h, and filtered. 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 and concentrated t...

Embodiment 2

[0063] As described in Example 1, the difference is that the methanol solvent in step (1) is replaced with anhydrous ethanol. That is, weigh 100.0 g of anhydrous tin tetrachloride, dissolve it in 300 ml of anhydrous ethanol, add 7.0 g of water, stir until fully dissolved, and the resulting solution is marked as liquid A. Weigh 110.0g of sodium acetate and dissolve it in 350ml of absolute ethanol. The obtained solution is marked as solution B. At 70°C, add solution B dropwise to solution A for 40min, and keep stirring during the dropwise addition. And after the dropwise addition was completed, stirring was continued for 1 hour, and after the stirring was stopped, the reaction solution was allowed to stand at room temperature for 12 hours. The viscosity of the spinning solution in step (2) was adjusted to 25 Pa·S, and the standing time was adjusted to 2 h. In step (3), the speed of the motor is 16000r / min, the temperature of the spinning room is 28°C, and the relative humidity ...

Embodiment 3

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

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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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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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