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Method for preparing nano-micronlamellar chalcopyrite microcrystal polymerunder hydrothermal conditions

A technology of micron flakes and chalcopyrite, which is applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve the problems that synthetic chalcopyrite is difficult to control and the products are not environmentally friendly, and achieves the control of chalcopyrite formation , suitable for large-scale production, mild reaction and environmental protection

Inactive Publication Date: 2018-05-29
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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for preparing nano-micron sheet-like chalcopyrite microcrystalline aggregates under hydrothermal conditions. Aiming at problems such as the difficulty in controlling the formation of chalcopyrite synthesized under hydrothermal conditions, and the products are not environmentally friendly, organic complexation is selected. As the source of sulfur, thiourea is used as a strong ligand, and its sulfur atoms will selectively complex with transition metal ions to form Cu and Fe complex cation complexes, which can promote hydrothermal reactions and reduce impurity phases.

Method used

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  • Method for preparing nano-micronlamellar chalcopyrite microcrystal polymerunder hydrothermal conditions
  • Method for preparing nano-micronlamellar chalcopyrite microcrystal polymerunder hydrothermal conditions
  • Method for preparing nano-micronlamellar chalcopyrite microcrystal polymerunder hydrothermal conditions

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Experimental program
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Effect test

Embodiment 1

[0028] Choose thiourea (H 2 NCSNH 2 ), ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) and copper sulfate pentahydrate (CuSO 4 ·5H 2 O) as raw materials, respectively placed in volumetric flasks to prepare solutions of equal volume. Measure the thiourea solution, ferrous sulfate solution and copper sulfate solution respectively, place them in a beaker and mix them thoroughly so that S:Fe:Cu=1:0.5:0.5 (amount of substance), and stir with a glass rod to fully mix them. Add the mixed solution into the reactor so that the solution accounts for 80% of the volume of the reactor. Control the temperature at 180°C and heat for 12h. Cool down to room temperature at a rate of 10°C / 10min, filter with absolute ethanol, and finally obtain a black powder. Chalcopyrite crystal samples were obtained after drying. The morphology of the experimental sample was observed by the Ultra Plus field emission analysis scanning electron microscope. At this time, the chalcopyrite crystals were well ...

Embodiment 2

[0030] Choose thiourea (H 2 NCSNH 2 ), ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) and copper sulfate pentahydrate (CuSO 4 ·5H 2 O) as raw materials, respectively placed in volumetric flasks to prepare solutions of equal volume. Measure the thiourea solution, ferrous sulfate solution and copper sulfate solution respectively, place them in a beaker and mix them thoroughly so that S:Fe:Cu=0.9:0.5:0.5 (quantity of substances), and stir with a glass rod to fully mix them. Add the mixed solution to the reactor so that the solution accounts for about 80% of the volume of the reactor. Control the temperature at 200°C and heat for 24h. Cool down to room temperature at a rate of 10°C / 10min, filter with absolute ethanol, and finally obtain a black powder. Chalcopyrite crystal samples were obtained after drying. The morphology of the experimental samples was observed by the Ultra Plus field emission analysis scanning electron microscope. At this time, the lamellar chalcopyrite ...

Embodiment 3

[0032] Choose thiourea (H 2 NCSNH 2 ), ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) and copper sulfate pentahydrate (CuSO 4 ·5H 2 O) as raw materials, respectively placed in volumetric flasks to prepare solutions of equal volume. Measure the thiourea solution, ferrous sulfate solution and copper sulfate solution respectively, place them in a beaker and mix them thoroughly so that S:Fe:Cu=1:0.5:0.5 (amount of substance), and stir with a glass rod to fully mix them. Add the mixed solution to the reactor so that the solution accounts for about 80% of the volume of the reactor. Control the temperature at 200°C and heat for 24h. Cool down to room temperature at a rate of 10°C / 10min, filter with absolute ethanol, and finally obtain a black powder. Chalcopyrite crystal samples were obtained after drying. The morphology of the experimental sample was observed by the Ultra Plus field emission analysis scanning electron microscope. At this time, the lamellar chalcopyrite crysta...

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Abstract

The invention relates to a method for artificially synthesizing natural minerals, in particular to a method for preparing a nano-micronlamellar chalcopyrite microcrystal polymerunderhydrothermal conditions. The method for preparing the nano-micronlamellar chalcopyrite microcrystal polymerunder the hydrothermal conditions is characterized by using ferrous sulfate heptahydrate (FeSO<4> 7H<2>O), copper sulfate pentahydrate (CuSO<4> 5H<2>O) and thiourea (H<2>NCSNH<2>) as raw materials. The method includes the following steps of a, preparing mixed solution; b,heating; c,cooling; d,filtering; e,drying and preserving to obtain the nano-micronlamellar chalcopyrite microcrystal polymer. By aiming at the problems that the molding of the synthesized chalcopyrite is not easy to control under the hydrothermal conditions, and a product is not environmentally friendly, and the like, the thiourea as an organic complexing agent is selected as a source of sulfur, the thiourea is used as a strong ligand,and sulfur atoms of the thioureaare selectively complexed with transition metal ions to form Cu, Fe complex cation complexes for promoting hydrothermal reaction and reducing impurity phases.

Description

technical field [0001] The invention relates to an artificial synthesis method of natural minerals, in particular to a method for preparing nano-micron sheet-like chalcopyrite microcrystalline aggregates under hydrothermal conditions. Background technique [0002] As a relatively common copper-iron sulfide mineral, natural chalcopyrite can be formed in a variety of environments, and contact metasomatism and hydrothermal origin are the most common. It is produced all over the world, with abundant reserves and low cost, and is the main raw material for industrial copper smelting; [0003] At the same time, Cu in chalcopyrite is a good conductor. As a ternary transition metal sulfide, chalcopyrite has better electrical, magnetic and chemical properties than pyrite, and can be applied to many fields such as semiconductor materials, photoelectric cells, lithium battery cathode materials, and sensors. However, natural chalcopyrite has high impurity content, large and uneven part...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B7/10
CPCC30B29/46C30B7/10
Inventor 黄菲刘开君王学求李光禄黎永丽赵福德张宝匀
Owner 中国地质科学院地球物理地球化学勘查研究所
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