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Method for preparing core-shell composite sulfide material through two-step method

A composite, sulfide technology, applied in chemical instruments and methods, cobalt sulfide, iron sulfide, etc., can solve the problems of difficult controllability of observation and monitoring experimental technology, strong dependence on experimental equipment, high risk, etc. Improved voltage plateau characteristics, improved effective discharge capacity, and reduced risk

Active Publication Date: 2021-10-15
富电新材料(佛山)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Previously, FeS was successfully prepared by hydrothermal method in our laboratory. 2 @CoS 2 Composite materials and hydrothermal preparation materials technology need to be carried out in a high temperature and sealed reactor, the reaction process is highly dependent on the experimental equipment, the observation and monitoring of the experimental reaction process and the control of the experimental technology are difficult, and The batch size is small, the risk is high, and it is difficult to achieve the industrial goal of high cost performance

Method used

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  • Method for preparing core-shell composite sulfide material through two-step method
  • Method for preparing core-shell composite sulfide material through two-step method
  • Method for preparing core-shell composite sulfide material through two-step method

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Experimental program
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Effect test

Embodiment 5

[0060] Sulfurization experiment of precursors with low cobalt concentration;

[0061] The preparation process of precursor is consistent with embodiment 1, and concrete condition parameter is as follows:

[0062] In the experiment, the reaction temperature was set at 75°C, and the concentration was 12g L -1 CoSO 4 54 ml and 20 g acidified pretreated FeS 2 The powder is the raw material, and the pH value is studied at 11; stirring; then in the water bath solution, the temperature is raised to 60-85°C at a heating rate of 5°C / min, stirred and kept for a while; after the plating solution becomes clear; solid-liquid separation; Precursors of core-shell composite sulfide materials. The phase analysis of the obtained electroless cobalt plating product is as follows: Figure 5 Shown in CP-1(Co).

[0063] The prepared product plus elemental sulfur powder undergoes vulcanization reaction (sulfur powder is sufficient), the first stage is 10 ℃ min -1 The heating rate was increased ...

Embodiment 6

[0068] Vulcanization experiment of precursors with high cobalt concentration;

[0069] The preparation process of precursor is consistent with embodiment 1, and concrete condition parameter is as follows:

[0070] In the experiment, the reaction temperature was set at 75°C, and the concentration was 12g L -1 CoSO 4 110 ml and 20 g acidified pretreated FeS 2 The powder is the raw material, and the pH value is studied at 11; stirring; then in the water bath solution, the temperature is raised to 60-85°C at a heating rate of 5°C / min, stirred and kept for a while; after the plating solution becomes clear; solid-liquid separation; Precursors of core-shell composite sulfide materials. The phase analysis of the obtained electroless cobalt plating product is as follows: Figure 5 Shown in CP-2(Co).

[0071] The prepared product plus elemental sulfur powder undergoes vulcanization reaction (sulfur powder is sufficient), the first stage is 10 ℃ min -1 The heating rate was increase...

Embodiment 7

[0073] Vulcanization experiments of precursors with high cobalt concentration;

[0074] The preparation process of precursor is consistent with embodiment 1, and concrete condition parameter is as follows:

[0075] In the experiment, the reaction temperature was set at 75°C, and the concentration was 12g L -1 CoSO 4 170 ml and 20 g of pretreated FeS 2 The powder is the raw material, and the pH value is studied at 11; stirring; then in the water bath solution, the temperature is raised to 60-85°C at a heating rate of 5°C / min, stirred and kept for a while; after the plating solution becomes clear; solid-liquid separation; Precursors of core-shell composite sulfide materials. The phase analysis of the obtained electroless cobalt plating product is as follows: Figure 5 Shown in CP-3(Co).

[0076] The prepared product plus elemental sulfur powder undergoes vulcanization reaction (sulfur powder is sufficient), the first stage is 10 ℃ min -1 The heating rate was increased to 3...

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Abstract

The invention relates to the field of manufacturing of thermal batteries and normal-temperature lithium primary battery electrode materials, in particular to a method for preparing a core-shell composite sulfide material through a two-step method. The method comprises the following steps: forming a metal cobalt layer which is uniformly distributed on the surface of FeS2 powder particles through a chemical plating method to obtain a precursor material; then carrying out vulcanization treatment on the precursor material; and obtaining the core-shell composite sulfide material. When the prepared shell cobalt disulfide accounts for 2.5-14.6% of the total mass of the core-shell composite sulfide material, the core-shell composite positive electrode material is used as a positive electrode material; after a thermal battery is assembled, the thermal battery is subjected to constant-current discharge at the working temperature of 520 DEG C and the current density of 200mA / cm < 2 >, and when the cut-off voltage is 1.6 V, the specific discharge capacity of the thermal battery is up to 331mAh / g. The preparation operation method is reliable, the cost is low, the obtained product has excellent thermal stability and electrochemical performance, and large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to the field of manufacturing electrode materials for thermal batteries and lithium primary batteries at normal temperature, in particular to a two-step method for preparing core-shell composite sulfide materials. [0002] technical background [0003] Thermal battery is a special battery with molten salt as electrolyte. Thermal battery has the characteristics of high power density, high energy density, long storage time, rapid and reliable activation, suitable for various harsh working conditions, and simple and convenient use. Therefore, it is mainly used as a power source for high-tech weapons such as missiles, guided bombs, and torpedoes. In the civilian field, thermal batteries also have broad application prospects as emergency power supplies for aircraft, power supplies for underground high-temperature prospecting equipment, and fire alarm power supplies. The widely used cathode material is mainly natural pyrite iron disulfi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/12C01G51/00H01M4/36H01M4/58H01M6/36
CPCC01G49/12C01G51/30H01M4/366H01M4/5815H01M6/36C01P2004/03C01P2002/72C01P2004/84C01P2006/40Y02E60/10
Inventor 刘志坚宁慧龙
Owner 富电新材料(佛山)有限公司
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