Preparation method of pyrite-type ferrous disulfide micron/nano crystalline material with controllable morphology

A technology of ferrous disulfide and nanocrystalline materials, applied in the direction of iron sulfide, nanotechnology, nanotechnology, etc., to achieve low cost, simple preparation process, and reduce production costs

Inactive Publication Date: 2012-11-21
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Marcasite-type ferrous disulfide is an unstable variant of pyrite-type ferrous disulfide, and its direct band gap is 0.51 eV, which is too narrow to be used as a solar cell material.
So far, there is no report on the solvothermal preparation of monodisperse, single phase, controlled morphology and particle size pyrite-type ferrous disulfide micro / nanocrystals

Method used

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  • Preparation method of pyrite-type ferrous disulfide micron/nano crystalline material with controllable morphology
  • Preparation method of pyrite-type ferrous disulfide micron/nano crystalline material with controllable morphology
  • Preparation method of pyrite-type ferrous disulfide micron/nano crystalline material with controllable morphology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 A method for preparing a pyrite-type ferrous disulfide micro / nanocrystalline material with controllable morphology, comprising the following steps:

[0037] (1) Stir the solvent dimethyl sulfoxide (DMSO) and pass nitrogen gas with a purity of 98.5% or more, and then add the compounding agent thioglycolic acid (TGA) at a concentration of 2.4 μl / mL at a concentration of 0.003 g / mL. mL of surfactant polyvinylpyrrolidone (PVP), mixed and stirred to obtain solution A.

[0038] Among them: the volume ratio (mL / mL) of thioglycolic acid and dimethyl sulfoxide is 1:5; the volume ratio (mL / mL) of polyvinylpyrrolidone and dimethyl sulfoxide is 1:2.

[0039] Surfactant polyvinylpyrrolidone has a molecular weight of 10,000.

[0040] (2) In solution A, add iron source with a concentration of 0.01mol / L—ferrous chloride and an aqueous solution of sodium thiosulfate with a concentration of 0.03mol / L in sequence, pass nitrogen with a purity of more than 98.5% and stir vi...

Embodiment 2

[0044] Example 2 A method for preparing a pyrite-type ferrous disulfide micro / nanocrystalline material with controllable morphology, comprising the following steps:

[0045] (1) Stir the solvent dimethyl sulfoxide (DMSO) and pass through the argon gas with a purity of 98.5% or more, and add the compounding agent thioglycolic acid (TGA) at a concentration of 2.4 μl / mL at a concentration of 0.009 g / mL surfactant polyvinylpyrrolidone (PVP), mixed and stirred to obtain solution A.

[0046] Among them: the volume ratio (mL / mL) of thioglycolic acid and dimethyl sulfoxide is 1:10; the volume ratio (mL / mL) of polyvinylpyrrolidone and dimethyl sulfoxide is 1:6.

[0047] Surfactant polyvinylpyrrolidone has a molecular weight of 1,300,000.

[0048] (2) Add iron source with a concentration of 0.02 mol / L—ferrous sulfate and an aqueous sodium thiosulfate solution with a concentration of 0.06 mol / L in sequence in solution A, pass argon gas with a purity of more than 98.5% and stir vi...

Embodiment 3

[0052] Example 3 A method for preparing a pyrite-type ferrous disulfide micro / nanocrystalline material with controllable morphology, comprising the following steps:

[0053] (1) Stir the solvent dimethyl sulfoxide (DMSO) and pass nitrogen gas with a purity of 98.5% or more, and add the compounding agent thioglycolic acid (TGA) at a concentration of 2.4 μl / mL at a concentration of 0.006 g / mL. mL of surfactant polyvinylpyrrolidone (PVP), mixed and stirred to obtain solution A.

[0054] Among them: the volume ratio (mL / mL) of thioglycolic acid and dimethyl sulfoxide is 1:7; the volume ratio (mL / mL) of polyvinylpyrrolidone and dimethyl sulfoxide is 1:4.

[0055] Surfactant polyvinylpyrrolidone has a molecular weight of 100,000.

[0056] (2) In solution A, add iron source with a concentration of 0.015 mol / L—ferrous chloride and an aqueous solution of sodium thiosulfate with a concentration of 0.045 mol / L in sequence, pass nitrogen with a purity of more than 98.5% and stir vi...

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Abstract

The invention relates to a preparation method of a pyrite-type ferrous disulfide micron/nano crystalline material with a controllable morphology. The method comprises the following steps of: (1) respectively adding solvent dimethyl sulfoxide into compounding agent thioglycolic acid and surfactant polyvinylpyrrolidone under the condition of agitating and leading in nitrogen or argon, and obtaining a solution A by mixing and agitating; (2) orderly adding an iron source and a sodium thiosulfate water solution into the solution A, leading in the nitrogen or argon and vigorously stirring to obtain a solution B; (3) transferring the solution B into a reaction kettle and reacting for 4-12 hours at 120-180 DEG C after uniformly agitating, to obtain pyrite-type ferrous disulfide suspension liquid; (4) centrifugally separating, washing for a plurality of times and drying the pyrite-type ferrous disulfide suspension liquid in vacuum to constant weight to obtain the pyrite-type ferrous disulfide micron/nano crystalline material. The product obtained by the method has controllable particle size and morphology, good process repeatability and stable quality, and is expected to be applied to the fields such as photovoltaic conversion and lithium ion battery materials.

Description

technical field [0001] The invention relates to a preparation method of a pyrite-type ferrous disulfide material, in particular to a preparation method of a pyrite-type ferrous disulfide micro / nano crystal material with controllable morphology. Background technique [0002] Ferrous disulfide in nature exists in two forms of pyrite and marcasite. Pyrite-type ferrous disulfide is an excellent semiconductor material with a direct band gap of 0.95 eV, which is close to the requirement of 1.1 eV for ideal solar cell materials (A.Ennaoui, S. Fiechter, C.Pettenkofer, N. Alonso-Vante, K.Buker,, M. Bronold, C.Hopfner, H. Sol. Tributsch; Iron disulphide for solar energy conversion [J]. Energy. Mater. Sol.Cells.1993, 29, 289-370.) . Marcasite-type ferrous disulfide is an unstable variant of pyrite-type ferrous disulfide, and its direct band gap is 0.51 eV, which is too narrow to be used as a solar cell material. The light absorption coefficient of pyrite-type ferrous sulfide is as h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/12B82Y30/00
Inventor 拜永孝包琰邓爱英魏成蓉胡新军
Owner LANZHOU UNIVERSITY
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