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Ferrous disulfide microspheres and preparation method thereof

A technology of ferrous disulfide and microspheres, applied in iron sulfide and other directions, can solve the problems of non-cubic phase pyrite impurities, difficult process control, uneven morphology, etc., to achieve uniform morphology and size, low cost, The effect of large binding reaction area

Active Publication Date: 2017-05-31
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the first few methods such as chemical vapor deposition require harsh conditions such as high temperature, high vacuum and high pressure during preparation, and the process is complicated and difficult to control.
However, the mechanical ball milling method is difficult to solve the FeS in the reaction process. 2 The problem of being oxidized is easy to produce impurities of non-cubic pyrite, product phase impurity and uneven morphology, etc.

Method used

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  • Ferrous disulfide microspheres and preparation method thereof
  • Ferrous disulfide microspheres and preparation method thereof
  • Ferrous disulfide microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Weigh 2.7g FeCl 3 ·6H 2 O, fully dissolved in 40mL deionized water, stirred to obtain a homogeneous solution;

[0037] (2) Add 0.76g of thiourea to the above solution, fully stir and dissolve;

[0038] (3) Add 10g of polyvinylpyrrolidone (PVP) into the above solution by weighing again, and stir while ultrasonically to obtain a homogeneous transparent solution;

[0039] (4) Transfer the final solution into a polytetrafluoroethylene-lined stainless steel sealed high-temperature and high-pressure reactor, heat it to 240 ° C, and react at constant temperature for 12 hours. After the reaction is completed, cool it, and then wash it with deionized water and absolute ethanol. Centrifuge three times, and finally the target product can be obtained.

[0040] For the FeS prepared above 2 microspheres for detection, figure 1 , figure 2 FeS prepared for this example 2 The scanning electron micrograph of the microsphere shows that the FeS 2 The microspheres are uniformly...

Embodiment 2

[0042] (1) Weigh 2.0g FeCl 3 ·6H 2 O, fully dissolved in 40mL deionized water, stirred to obtain a homogeneous solution;

[0043] (2) Add 0.76g of thiourea to the above solution, fully stir and dissolve;

[0044] (3) Add 10g of polyvinylpyrrolidone (PVP) into the above solution by weighing again, and stir while ultrasonically to obtain a homogeneous transparent solution;

[0045] (4) Transfer the final solution into a polytetrafluoroethylene-lined stainless steel sealed high-temperature and high-pressure reactor, heat it to 240 ° C, and react at constant temperature for 12 hours. After the reaction is completed, cool it, and then wash it with deionized water and absolute ethanol. Centrifuge three times, and finally the target product can be obtained.

Embodiment 3

[0047] (1) Weigh 3.4g FeCl 3 ·6H 2 O, fully dissolved in 40mL deionized water, stirred to obtain a homogeneous solution;

[0048] (2) Add 0.76g of thiourea to the above solution, fully stir and dissolve;

[0049] (3) Add 10g of polyvinylpyrrolidone (PVP) into the above solution by weighing again, and stir while ultrasonically to obtain a homogeneous transparent solution;

[0050] (4) Transfer the final solution into a polytetrafluoroethylene-lined stainless steel sealed high-temperature and high-pressure reactor, heat it to 240 ° C, and react at constant temperature for 12 hours. After the reaction is completed, cool it, and then wash it with deionized water and absolute ethanol. Centrifuge three times, and finally the target product can be obtained.

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Abstract

The invention relates to ferrous disulfide microspheres and a preparation method thereof. The ferrous disulfide microspheres are microspheres with single hole structures and are formed by clustering ferrous disulfide nano particles. The preparation method comprises the following steps: (1) dissolving ferric salt or ferrite into deionized water to obtain a solution; (2) adding thiourea into the solution, and carrying out stirring to dissolve the thiourea to obtain a mixed solution; (3) adding polyvinylpyrrolidone into the mixed solution, and carrying out ultrasonic stirring to obtain reaction liquid; (4) putting the reaction liquid into a reaction kettle, and after the reaction is completed, carrying out cooling, washing and centrifugating to obtain the ferrous disulfide microspheres. Compared with the prior art, the ferrous disulfide microspheres and the preparation method thereof which are disclosed by the invention have the advantages that the microspheres are uniform in particle size, the synthesis process is simple, a few of types of raw materials are needed, and the requirement on equipment is relatively low.

Description

technical field [0001] The invention relates to the field of inorganic chemical industry, in particular to a ferrous disulfide microsphere and a preparation method thereof. Background technique [0002] With the development of human society and science and technology, fossil fuels have been difficult to meet the growing demand, and will bring huge damage to the environment. Therefore, the development and utilization of new energy has become a top priority. The development of rechargeable secondary batteries and the utilization of solar energy have become the focus of new energy sources. Especially with the development of new energy vehicles, the research and development of rechargeable batteries with high energy storage has become a top priority. Researchers have developed various high-energy lithium-ion battery electrode materials (especially negative electrode materials), such as transition metal oxides and sulfides. [0003] Chalcopyrite (FeS 2 ), is a rich mineral, c...

Claims

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Application Information

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IPC IPC(8): C01G49/12
CPCC01G49/12C01P2002/72C01P2004/03C01P2004/34C01P2004/61
Inventor 高国黄鹏尹婷张倩崔大祥
Owner SHANGHAI JIAO TONG UNIV
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