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Preparation method and application of carbon or transition metal doped iron-sulfur compound composite material

A technology of iron-sulfur compounds and transition metals, which is applied in the field of preparation of iron-sulfur compound composite materials, and can solve problems such as volume expansion, decay, and cracks

Pending Publication Date: 2021-06-15
TIANMU LAKE INST OF ADVANCED ENERGY STORAGE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But FeS Z (Z≥1) The conductivity is poor, and the problem of volume expansion is prone to occur during charging and discharging, which affects the capacity decline, cycle performance and rate performance of the battery
There are two reasons for this: on the one hand, once the lithiation reaction occurs in the battery, the electron migration speed on the surface of the element Li is much faster than the electron migration speed inside the element, and the electron migration speed of FeS Z (Z≥1) The material cannot bear such a large volume change at all, and finally cracks appear from the bottom, and the material appears pulverized; on the other hand, some studies have shown that FeS Z (Z≥1) After the first cycle of charge and discharge, free iron ions and sulfur ions will be generated, both of which are easily soluble in the electrolyte to bring about the "double shuttle effect", causing capacity decline, and iron ions are also easy to deposit on the surface of the positive electrode , which hinders the contact between the SEI film on the surface of the positive electrode and the electrolyte, and the free iron ions and FeS 2 A reaction occurs that lowers the potential of the battery
[0004] For this reason, some researchers proposed to combine carbon network structure or transition metal oxide (Fe x o y ) and FeS Z (Z≥1) materials are recombined by means of compounding, doping or coating to alleviate the FeS Z (Z≥1) volume change, but still unable to relieve FeS Z (Z≥1) The problem caused by the generation of free iron ions after charging and discharging, and Fe x o y Medium Fe will aggravate the existence of this problem

Method used

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  • Preparation method and application of carbon or transition metal doped iron-sulfur compound composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Fe 2 o 3 / MoS 2 / FeS 2 Preparation of composite materials

[0037] (1) Add 45mL of ethylene glycol and 5mL of deionized water together and mix well;

[0038] (2) Add 1.2 mol iron acetylacetonate and 0.3 mol molybdenum acetylacetonate to the system in step (1), stir and sonicate evenly, pour it into a high-pressure reactor with polytetrafluoroethylene as the inner tank, heat at 150°C for 8 hours, and take it out Filter, wash the precipitate with ethanol, and finally dry it in an oven at 60°C for 12 hours;

[0039] (3) The product of step (2) and 1.2 mol of sublimed sulfur were placed in an argon protective atmosphere and calcined at 450°C for 4 hours, and Fe was obtained after natural cooling. 2 o 3 / MoS 2 / FeS 2 composite material. The XRD pattern of the product is attached figure 1 shown, from the attached figure 1 The presence of Mo oxides (or hydroxides) was not detected in the composite materials, and it can be seen that the Mo in the composite material i...

Embodiment 2

[0055] Fe 2 o 3 / NiS / FeS composites

[0056] (1) Add 40mL of N-methylpyrrolidone and 5mL of deionized water together and mix well;

[0057] (2) Add 0.4 mol iron acetylacetonate and 0.08 mol nickel acetylacetonate to the system in step (1), stir and sonicate evenly, pour it into a high-pressure reactor whose inner tank is polytetrafluoroethylene, heat at 140°C for 10 hours, and take it out Filter, wash the precipitate with ethanol, and finally dry it in an oven at 70°C for 10 hours;

[0058] (3) The product of step (2) was calcined at 400°C for 6 hours in a sublimated sulfur atmosphere, and Fe was obtained after natural cooling. 2 o 3 / NiS / FeS composites.

[0059] Fe prepared by embodiment 2 2 o 3 / NiS / FeS composite material, acetylene black, and polytetrafluoroethylene are stirred and mixed at high speed in N-methylpyrrolidone at a mass ratio of 94:3:3 to fully obtain a slurry with a solid content of 66.22%. The slurry is coated on aluminum foil, then vacuum-dried at 1...

Embodiment 3

[0064] Fe 2 o 3 Preparation of / C / FeS composites

[0065] (1) Add 60mL of isopropanol and 6mL of ethylenediamine aqueous solution together and mix well;

[0066] (2) Add 0.4 mol iron acetylacetonate and 0.12 mol superconducting carbon black to the system of step (1), stir and ultrasonically evenly, pour it into a high-pressure reactor whose inner tank is polytetrafluoroethylene and heat at 135°C for 16 hours Take out and filter, wash the precipitate with ethanol, and finally dry it in an oven at 85°C for 7 hours;

[0067] (3) Mix and grind the product of step (2) with 1.2 mol of ferrous sulfide thoroughly, then place them together in a nitrogen protective atmosphere for calcination at 420°C for 6 hours, and obtain Fe after natural cooling. 2 o 3 / C / FeS composites.

[0068] Fe prepared by embodiment 3 2 o 3 / C / FeS composite material, superconducting carbon black, and polytetrafluoroethylene are stirred and mixed at high speed in N-methylpyrrolidone at a mass ratio of 7:2...

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Abstract

The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method and application of a carbon or transition metal doped iron-sulfur compound composite material. The preparation method comprises the following steps: full mixing an organic solvent and an inorganic solvent to obtain a mixed solvent, adding an iron source, a transition metal source or a carbon source into the mixed solvent, heating to carry out organic-inorganic hybridization reaction, filtering, washing a filter cake, drying, and calcining the dried filter cake in a sulfur source environment to obtain the target product. The prepared carbon or transition metal doped iron-sulfur compound composite material is used as an active substance of a positive electrode material in an alkali metal ion battery.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a preparation method and application of an iron-sulfur compound composite material doped with carbon or transition metal. Background technique [0002] With the advancement of technology and the improvement of people's living standards, more and more high-tech products appear in our daily life, such as Bluetooth headsets, mobile chargers, remote control aircraft, robots and electric lock access control, etc. One of the commonly used chemical power sources for these products is lithium-ion batteries due to their advantages of no memory effect, environmental friendliness and long life. However, at present, ternary materials, lithium iron phosphate, lithium cobalt oxide, etc. are commonly used commercially as positive electrode materials for lithium-ion batteries, and their theoretical specific capacity is low (<300mAh g -1 ), these have been unable to meet people'...

Claims

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Application Information

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IPC IPC(8): C01G49/12C01G39/06C01G49/06C01G53/11C01B32/00C01G23/00H01M4/58H01M4/52H01M4/36H01M4/62H01M10/0525H01M10/054
CPCC01G49/12C01G39/06C01G49/06C01G53/11C01B32/00C01G23/007H01M4/5815H01M4/523H01M4/362H01M4/626H01M4/625H01M10/0525H01M10/054C01P2004/80C01P2006/40Y02E60/10
Inventor 朱甜冯凯冯辉灿邱玲娅
Owner TIANMU LAKE INST OF ADVANCED ENERGY STORAGE TECH CO LTD
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