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Method for preparing nano-chalcopyrite tetrahedral crystals under hydrothermal conditions

A technology of chalcopyrite and tetrahedron, which is applied in chemical instruments and methods, iron compounds, inorganic chemistry, etc., can solve the problems of complex steps, high equipment requirements, and unsuitability for batch preparation, and achieve simple operation, uniform particle size, and improved Effect of Photoelectric Conversion Efficiency

Active Publication Date: 2021-11-30
中国地质科学院地球物理地球化学勘查研究所 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chalcopyrite materials with different morphologies have been synthesized by previous methods, including the preparation of chalcopyrite films by atomic layering, the synthesis of hexagonal chalcopyrite by solvothermal method and the synthesis of nanorods, fibers, and sheets by hydrothermal synthesis. Shaped chalcopyrite, etc., the steps are complicated and require high equipment, so it is not suitable for batch preparation

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  • Method for preparing nano-chalcopyrite tetrahedral crystals under hydrothermal conditions
  • Method for preparing nano-chalcopyrite tetrahedral crystals under hydrothermal conditions
  • Method for preparing nano-chalcopyrite tetrahedral crystals under hydrothermal conditions

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Effect test

Embodiment 1

[0064] Choose thiourea (H 2 NCSNH 2 ), anhydrous ferric chloride (FeCl 3 ) and copper sulfide (CuS)) as precursors, mixed according to the molar ratio of S: Fe: Cu=2.2: 1: 1, mixed powder by mass volume ratio: water = 50: 1, unit g: L, The mixed powder is added into water, and after the inorganic salt of iron and the compound of sulfur are completely dissolved, a suspension is obtained, and a surfactant polyethylene glycol (PEG) is added to the obtained suspension to control its concentration in the solution to 0.02mol / L, after being uniformly vibrated by ultrasonic waves, placed in a polytetrafluoroethylene reactor, heated from room temperature to 220 °C at a rate of 5 °C / min, continued to react for 22 hours, and cooled naturally to room temperature. After the resultant is centrifuged, washed and filtered with absolute ethanol, a black powder is obtained, and after drying, nano chalcopyrite tetrahedral crystals are obtained. The morphology of the experimental sample was ob...

Embodiment 2

[0066] Choose thiourea (H 2 NCSNH 2 ), anhydrous ferric chloride (FeCl 3 ) and copper sulfide (CuS) as precursors, mixed according to the material ratio of S: Fe: Cu=1.8: 0.6: 1, mixed powder by mass volume ratio: water = 47: 1, unit g: L, will Add the mixed powder into water, and after the inorganic salt of iron and the compound of sulfur are completely dissolved, add the surfactant polyethylene glycol (PEG) to the resulting suspension to control its concentration in the solution to be 0.018mol / L. After uniform ultrasonic vibration, place in a polytetrafluoroethylene reactor, heat from room temperature to 230 °C at a rate of 10 °C / min, continue to react for 23 hours, and cool naturally to room temperature. After the resultant is centrifuged, washed and filtered with absolute ethanol, a black powder is obtained, and after drying, nano chalcopyrite tetrahedral crystals are obtained. The morphology of the experimental sample was observed with a field emission analysis scannin...

Embodiment 3

[0068] Choose thiourea (H 2 NCSNH 2 ), anhydrous ferric chloride (FeCl 3 ) and copper sulfide (CuS) as precursors, mixed according to the mass ratio of S: Fe: Cu=2.2: 1.2: 1, mixed powder by mass volume ratio: water = 50: 1, unit g: L, the Add the mixed powder into water, and after the inorganic salt of iron and the compound of sulfur are completely dissolved, add surfactant polyethylene glycol (PEG) to the obtained suspension to control its concentration in the solution to be 0.022mol / L. After uniform ultrasonic vibration, place in a polytetrafluoroethylene reactor, heat from room temperature to 230 °C at a rate of 8 °C / min, continue to react for 22 hours, and cool naturally to room temperature. After the resultant is centrifuged, washed and filtered with absolute ethanol, a black powder is obtained, and after drying, nano chalcopyrite tetrahedral crystals are obtained. The morphology of the experimental sample was observed with a field emission analysis scanning electron ...

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Abstract

The invention discloses a method for preparing nano-chalcopyrite tetrahedral crystals under hydrothermal conditions. Take copper sulfide, water-soluble ferric inorganic salt and sulfur compound as precursors, add an appropriate amount of solvent, then add surfactant, put it in a reaction kettle after ultrasonic vibration, and react in a closed hydrothermal environment; Heating at a certain temperature for a period of time can obtain tetrahedral chalcopyrite with better crystal development. The method has the advantages of mild and environment-friendly conditions, simple operation, easier and sufficient reaction of raw materials, and low cost of required equipment and raw materials. The obtained chalcopyrite has consistent morphology and uniform particle size, and realizes the controllable preparation of chalcopyrite tetrahedral crystals, which provides technical support for photovoltaic performance research. Compared with the existing rod-shaped, fibrous, and flaky chalcopyrite, the chalcopyrite tetrahedron structure of the present invention has smaller splitting energy, which can greatly improve the photoelectric conversion efficiency when applied to photovoltaic materials, which has practical significance.

Description

Technical field: [0001] The invention belongs to the technical field of chalcopyrite preparation, specifically relates to a method for preparing natural minerals, and specifically provides a method for preparing nano chalcopyrite tetrahedral crystals under hydrothermal conditions. Background technique: [0002] As a ternary transition metal sulfide, chalcopyrite has excellent electrical, magnetic and chemical properties. However, natural chalcopyrite has high impurity content, large and uneven particle size, and it is difficult to meet the needs of many fields. The artificially synthesized chalcopyrite structure material has uniform morphology and high purity, and can be applied to many fields such as semiconductor materials, photoelectric cells, and lithium battery cathode materials, and has attracted much attention in recent years. [0003] Chalcopyrite materials with different morphologies have been synthesized by a variety of methods, including the preparation of chalco...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/00
CPCC01G49/009C01P2002/72C01P2004/03C01P2004/61C01P2004/62C01P2006/60
Inventor 黄菲刘开君王学求张志彬李光禄任亚群
Owner 中国地质科学院地球物理地球化学勘查研究所