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Pompon bismuthous sulfide and preparation method thereof

A technology of bismuth trisulfide and bismuth sulfide, applied in chemical instruments and methods, inorganic chemistry, bismuth compounds, etc., can solve problems such as difficult bismuth sulfide materials, and achieve the effects of large specific surface area, good crystallization and uniform size

Inactive Publication Date: 2012-08-01
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, "Journal of Inorganic Chemistry" (2008, Vol.24No.4, 547-552) reported that Zhang Qi of Xiangtan University and others used polyethylene glycol octylphenyl ether + alkylphenol polyoxyethylene ether, alkyl Different surfactants such as phenol polyoxyethylene ether, polyethylene glycol octyl phenyl ether, and bismuth sulfide nanoflower materials synthesized by the reflux method can be seen from the scanning electron microscope diagram given. The bismuth sulfide aggregates into bundles to form a flower-like bismuth sulfide nanoflower material, which has a larger surface area than granular and rod-shaped bismuth sulfide materials; but it is difficult to obtain Bismuth sulfide materials with higher surface area
So far, we haven’t seen any fluffy bismuth sulfide materials with larger specific surface area, good crystallization, uniform size, and better application prospects in the fields of catalysis and sensing, and polyparaphenylene sulfides that have been carboxylated by solvothermal / hydrothermal methods. Published report on the preparation method of bismuth sulfide materials with uniform size and pompous shape synthesized from acetylene (PPV)

Method used

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  • Pompon bismuthous sulfide and preparation method thereof
  • Pompon bismuthous sulfide and preparation method thereof
  • Pompon bismuthous sulfide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0012] First, bismuth nitrate was dissolved in DMF to prepare a 0.2mol / L solution; and carboxylated PPV was dissolved in methanol or water to prepare a 0.2mol / L solution; 1 volume ratio mixed, stirred at room temperature for 30 minutes to obtain a mixed solution; thioacetamide was dissolved in methanol to prepare a 0.2mol / L solution, according to the molar ratio Bi:S=3:2, added to the mixed solution obtained above After stirring evenly at room temperature, place it in a hydrothermal kettle and heat at a constant temperature of 120°C for 12 hours; take out the hydrothermal kettle, cool it to room temperature, and centrifuge at a speed of 5000 rpm to obtain a black solid, then Repeatedly wash with deionized water and ethanol until the centrifuged liquid is colorless, clear and transparent; then extract the centrifuged solid with ethanol, and finally place the solid obtained by ethanol extraction in a vacuum drying oven at 60°C Dry to obtain the product fluffy bismuth sulfide mat...

Embodiment 2

[0017] First, the Bi(NO 3 ) 3 ·5H 2 O was dissolved in DMF to prepare a 2mol / L solution; and the carboxylated PPV was dissolved in methanol or water to prepare a 0.001mol / L solution; the two solutions configured above were mixed in a volume ratio of 1:10, Stir at room temperature for 30 minutes to obtain a mixed solution; then dissolve thiourea in methanol to prepare a 0.01mol / L solution, add it to the mixed solution obtained above according to the molar ratio Bi:S=3:2, and stir evenly at room temperature After that, put it in a hydrothermal kettle and heat at a constant temperature of 80°C for 24 hours; take out the hydrothermal kettle, cool it to room temperature, and centrifuge at a speed of 8000 rpm to obtain a black solid, and then use deionized water to obtain a black solid. Repeated washing with ethanol until the centrifuged liquid is colorless, clear and transparent, and the solid separated by centrifugation; then the solid separated by centrifugation is extracted wi...

Embodiment 3

[0020] First, the Bi(NO 3 ) 3 ·5H 2 O was dissolved in DMF to prepare a 0.01mol / L solution; and the carboxylated PPV was dissolved in methanol or water to prepare a 2mol / L solution; the two solutions configured above were mixed in a volume ratio of 1:0.01, Stir at room temperature for 30 minutes to obtain a mixed solution; dissolve thiourea in methanol to prepare a 0.2mol / L solution, add it to the mixed solution obtained above according to the molar ratio Bi:S=3:2, and stir evenly at room temperature , placed in a hydrothermal kettle, and heated at a constant temperature of 160°C for 8 hours; the hydrothermal kettle was taken out, cooled to room temperature, and centrifuged at a speed of 3000 rpm to obtain a black solid, and then deionized water and ethanol were used respectively Alternately and repeatedly washed until the centrifuged liquid is colorless, clear and transparent, the solid separated by centrifugation; then the solid separated by centrifugation is extracted wit...

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Abstract

The invention discloses pompon bismuthous sulfide and a preparation method thereof. The preparation method is characterized in that bismuth nitrate serves as a bismuth source, thiourea or thioacetamide serves as a sulfur source, and hydrothermal / solvothermal reaction is preformed on the bismuth source and the sulfur source under the action of carboxylated polyphenylvinylene surfactant. Prepared bismuth sulfide pompon has an orthorhombic system structure, and cell parameters of crystals in the directions of coordinate axes X, Y and Z are respectively 11.149nm, 11.304nm and 3.981nm; and nanoribbon sliver-shaped pompon formed by the crystals of the bismuthous sulfide is subjected to agglomeration to generate bismuthous sulfide pompon, the diameter of the bismuthous sulfide pompon is 2 plus / minus 0.3 mu m, the length of the single nanoribbon sliver-shaped pompon is 0.3 plus / minus 0.1 mu m, the width of the pompon sliver is 300 plus / minus 10 nm, and the thickness of the pompon sliver is 100 plus / minus 10 nm. Compared with bismuth sulfide materials prepared by the convention method, the bismuth sulfide material prepared by the method disclosed by the invention has larger specific surface area and is good in crystallization and uniform in size, thus having better application prospect in the fields of catalysis and sensing.

Description

technical field [0001] The invention belongs to the technical field of bismuth sulfide preparation methods, and in particular relates to a pompom-shaped bismuth trisulfide and a method for preparing pompom-shaped bismuth trisulfide by a solvothermal / hydrothermal method. Background technique [0002] Bi 2 S 3 It is a direct narrow bandgap semiconductor material with an energy gap of 1.3eV, which is widely used in the fields of photovoltaic materials, photodiode materials, sensors and catalysis. In recent years, granular, rod-like, hedgehog-like and flower-like bismuth sulfides have been prepared by using solvothermal / hydrothermal methods, microwave methods, and template methods. For example, "Journal of Inorganic Chemistry" (2008, Vol.24No.4, 547-552) reported that Zhang Qi of Xiangtan University and others used polyethylene glycol octylphenyl ether + alkylphenol polyoxyethylene ether, alkyl Different surfactants such as phenol polyoxyethylene ether, polyethylene glycol oc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G29/00B82Y40/00
Inventor 徐卫兵孙海燕庄晓萌吕洪香马海红周正发
Owner HEFEI UNIV OF TECH
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