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A hollow structure ferrous sulfide@carbon in-situ composite material and its preparation method and application

An in-situ composite material, ferrous sulfide technology, used in structural parts, electrochemical generators, active material electrodes, etc., can solve the problem of pulverization and shedding volume changes of graphite anode materials, excessive potassium ion volume, and rapid capacity decay and other problems, to achieve the effect of low cost, cheap and easy-to-obtain raw materials, and maintaining structural integrity

Active Publication Date: 2022-03-25
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When potassium ions are intercalated in graphite, a step change will occur. Although graphite, as a negative electrode material for KIBs, has high reversible capacity and good rate capability, due to the large volume of potassium ions, it is easy to cause deformation of the graphite structure and has the disadvantage of rapid capacity decay.
Although lithium, sodium and potassium are in the same main group, compared with lithium ions and sodium ions, potassium ions with larger radius are more likely to cause pulverization and exfoliation of graphite negative electrode materials (volume caused by potassium ion intercalation / deintercalation process). The change is very huge), thus facing the problems of rapid capacity fading, low initial Coulombic efficiency, and poor cycle stability

Method used

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  • A hollow structure ferrous sulfide@carbon in-situ composite material and its preparation method and application
  • A hollow structure ferrous sulfide@carbon in-situ composite material and its preparation method and application
  • A hollow structure ferrous sulfide@carbon in-situ composite material and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Preparation of hollow structure ferrous sulfide@carbon in situ composite:

[0032] (1) Weigh 1.0g of ferrous sulfate, stir and dissolve in 30mL of water, then add 800mg of glycerin, stir to dissolve, add 1mol / L ammonia water dropwise at a rate of 1mL / min, stop the dropwise addition after white precipitation appears in the solution, and stir at room temperature 2h, suction filtration, washing, and drying at 50°C to obtain a solid nanorod-shaped iron hydroxide-glycerol precursor;

[0033] (2) Weigh 200mg of the precursor of step (1), add 30mL of water, ultrasonically disperse until uniform, add 570mg of cysteine, stir to dissolve, transfer to a hydrothermal kettle, 150°C hydrothermal reaction for 12h, and naturally cool To room temperature, the product was black, centrifuged, washed with ethanol and deionized water, and dried under vacuum at 60°C. The obtained powder was placed in a porcelain boat, placed in a muffle furnace, and calcined at 600°C for 2 hours under nitrog...

Embodiment 2

[0038] The ferrous sulfide@carbon in-situ composite material with a hollow rod-shaped structure prepared in Example 1 was used as an electrode active material in an energy storage battery. Mix 800 mg of ferrous sulfide@carbon in-situ composite material with a hollow rod-like structure, 100 g of acetylene black, and 100 g of polyvinylidene fluoride, add 1 g of nitrogen methyl pyrrolidone, and spread the stirred slurry on aluminum foil at 100 degrees drying. Cut out 1 cm original pieces of dendrites. The diaphragm is made of non-woven fabric, the counter electrode is metal potassium sheet, and the electrolyte is potassium hexafluorophosphate dissolved in diethyl carbonate solvent with a concentration of 1mol / L. A 2016 button battery is assembled in an anhydrous and oxygen-free glove box to obtain potassium Ion button battery.

[0039] The potassium ion button battery prepared in this embodiment was charged and discharged at a rate of 0.1C between 0.1 volts and 3.5 volts. The ...

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Abstract

The invention relates to a hollow structure ferrous sulfide@carbon in-situ composite material and its preparation method and application, comprising the following steps: (1) dissolving ferrous sulfate and glycerin in water, and then adding lye drop by drop until precipitation occurs Then stop dropping, stir at room temperature, then suction filter, wash, and dry to obtain a rod-shaped ferrous precursor; (2) Disperse the ferrous precursor in water, add an organic sulfur source, stir for at least 1 hour, and then heat up to 130°C Perform hydrothermal reaction at ~150°C, then naturally cool to room temperature, filter, wash, and dry to obtain the ferrous sulfide precursor; calcinate the ferrous sulfide precursor, and obtain a hollow structure ferrous sulfide@carbon after cooling In situ composites. The present invention obtains the ferrous sulfide@carbon in-situ composite material with a hollow rod-like structure through a template-free method and applies it to a potassium-ion battery as an electrode active material. The obtained battery has a long cycle life, good potassium storage performance, and a stable negative electrode structure. Chalking does not fall off.

Description

technical field [0001] The invention relates to the technical field of energy storage batteries, in particular to a hollow-structured ferrous sulfide@carbon in-situ composite material and its preparation method and application. Background technique [0002] With the widespread application of lithium-ion batteries (LIBs) in portable energy storage devices and electric energy storage devices, the increasingly scarce and uneven distribution of Li metals has gradually emerged. Therefore, researchers have focused their research on sodium-ion batteries (SIBs) and potassium-ion batteries (KIBs) with similar electrochemical properties to LIBs. Sodium and potassium metals, which are abundant, cheap, and environmentally friendly, are ideal candidates to replace LIBs. However, sodium ions are almost unable to undergo multi-step intercalation reactions with commercial graphite to form graphite intercalation compounds NaC 64 The specific capacity of the crystal structure is very low, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/62H01M4/58H01M4/136H01M10/054
CPCH01M4/5815H01M4/628H01M4/625H01M4/136H01M10/054H01M2004/021H01M2004/027Y02E60/10
Inventor 张蕾侯之国张雪倩
Owner JIANGSU UNIV OF TECH
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