Preparation method of chalcogenide tubular material

A chalcogenide, tubular technology, used in the preparation of sulfide/polysulfide, tin compounds, chemical instruments and methods, etc., can solve the problems of large specific surface area of ​​tubular materials, poor transport and separation of photogenerated carriers, etc. To achieve the effect of compact structure, environmentally friendly process, and accelerated transmission rate

Pending Publication Date: 2021-11-19
KUNMING UNIV OF SCI & TECH
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  • Claims
  • Application Information

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Problems solved by technology

[0004] However, most of the chalcogenides obtained by the existing preparation methods are thin films or irregular particle shapes, and the application in the field of optoelectronic semiconductors does not have the advantage of large specific surface area of ​​tubular materials, so the transport and separation of photogenerated carriers is poor.

Method used

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  • Preparation method of chalcogenide tubular material
  • Preparation method of chalcogenide tubular material
  • Preparation method of chalcogenide tubular material

Examples

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Effect test

Embodiment 1

[0036] Embodiment 1: In this embodiment, a tube furnace with dual temperature zones is used to prepare ZnS tubular material;

[0037] A kind of preparation method of ZnS tubular material, concrete steps are as follows:

[0038](1) Place 0.4mol sublimated sulfur (99.9% in purity) in the low-temperature heating zone of a dual-temperature zone tube furnace, and place 0.2mol metallic zinc powder in the high-temperature vulcanization heating zone of a dual-temperature zone tube furnace; wherein the metal zinc Powder purity ≥ 98%;

[0039] (2) Turn on the vacuum pump, pump the pressure in the reaction system to 10Pa and below, then close the pumping valve, open the intake valve, fill in high-purity argon (purity is 99.99%) until the pressure gauge is 100KPa and close Inlet valve, open the inlet valve to re-pump the pressure in the reaction system to 10Pa or below, repeat the gas washing three times to exhaust the impurity gas in the system, and avoid the formation of oxide impuriti...

Embodiment 2

[0043] Embodiment 2: This embodiment adopts double-temperature zone vertical furnace to prepare tin sulfide tubular material;

[0044] A kind of preparation method of tin sulfide tubular material, concrete steps are as follows:

[0045] (1) 1.0mol sublimated sulfur (purity is 99.9%) is placed in the low-temperature heating zone of the double-temperature zone vertical furnace, and 0.4mol tin powder is placed in the high-temperature vulcanization heating zone of the double-temperature zone vertical furnace; wherein the tin powder Purity≥98%;

[0046] (2) Turn on the vacuum pump, pump the pressure in the reaction system to 10Pa and below, then close the pumping valve, open the intake valve, fill in high-purity argon (purity is 99.99%) until the pressure gauge is 100KPa and close Inlet valve, open the inlet valve to re-pump the pressure in the reaction system to 10Pa or below, repeat the gas washing three times to exhaust the impurity gas in the system, and avoid the formation of...

Embodiment 3

[0050] Embodiment 3: In this embodiment, a tubular furnace with dual temperature zones is used to prepare antimony selenide tubular material;

[0051] A kind of preparation method of antimony selenide tubular material, concrete steps are as follows:

[0052] (1) 0.8mol selenium powder (purity greater than 99.9%) is placed in the low-temperature heating zone of the dual-temperature zone tube furnace, and 0.3mol metal antimony powder is placed in the high-temperature vulcanization heating zone of the dual-temperature zone tube furnace; wherein metal antimony Powder purity ≥ 98%;

[0053] (2) Turn on the vacuum pump, pump the pressure in the reaction system to 10Pa and below, then close the pumping valve, open the intake valve, fill in high-purity argon (purity is 99.99%) until the pressure gauge is 100KPa and close Inlet valve, open the inlet valve to re-pump the pressure in the reaction system to 10Pa or below, repeat the gas washing three times to exhaust the impurity gas in ...

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Abstract

The invention relates to a preparation method of a chalcogenide tubular material, and belongs to the technical field of photoelectric material preparation. A solid chalcogenide raw material is placed in a low-temperature heating zone of a double-temperature-zone furnace reactor, a metal raw material is placed in a high-temperature vulcanization reaction zone of the double-temperature-zone furnace reactor, inert gas is adopted for gas washing, then the solid chalcogenide raw material in the low-temperature heating zone and the metal raw material in the high-temperature vulcanization reaction zone are heated, the solid chalcogenide raw material in the low-temperature heating zone releases gaseous chalcogenide to react with the metal raw material in the high-temperature vulcanization reaction zone to generate a gas-phase chalcogenide, and the gas-phase chalcogenide is condensed on the substrate to obtain the chalcogenide tubular material. The chalcogenide tubular material is simple in preparation process, large-scale production can be achieved, the specific surface area of the chalcogenide tubular material is large, photons can be better captured, the transmission rate of photon-generated carriers is increased, and the chalcogenide tubular material is suitable for being applied to the field of photoelectric semiconductors.

Description

technical field [0001] The invention relates to a preparation method of a chalcogen compound tubular material, belonging to the technical field of photoelectric material preparation. Background technique [0002] Metal chalcogenides are important raw materials for industrial production and are widely used in various fields. Among them, most metal chalcogenides have semiconductor properties and are often used in photovoltaic and photoelectrocatalytic materials. Copper sulfide (CuS) thin film has good photoelectric effect, and is an ideal photoelectrochemical material with photosensitivity and light absorption; antimony selenide (Sb 2 Se 3 ) is a binary single-phase compound with a suitable band gap (~1.15eV) and a large absorption coefficient (>10 5 cm -1 ), very suitable for making new low-cost and low-toxic solar cells; tin disulfide (SnS 2 ) is a two-dimensional structure material, SnS 2 It is a layered material with a band gap of 2.2eV. It has a narrow band gap a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/20C01G9/08C01B19/04C01G19/00C01G21/21B82Y40/00
CPCC01B17/20C01G9/08C01B19/007C01G19/00C01G21/21B82Y40/00C01P2004/10C01P2004/13
Inventor 杨佳张君王薇侯堪文黄滔张雅婷杨海艳曹成松徐宝强李绍元杨斌马文会熊恒蒋文龙李一夫田阳刘大春戴永年
Owner KUNMING UNIV OF SCI & TECH
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