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Mixed-valence iron-based fluoride positive electrode material and preparation method thereof

A positive electrode material, fluoride technology, applied in the field of electrochemistry and material chemistry, can solve problems such as poor conductivity, achieve the effect of improving electronic conductivity, low operating labor intensity, and good flexibility

Active Publication Date: 2021-03-26
SHANGHAI INST OF SPACE POWER SOURCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the existing FeF3 and FeF2 for the electrical conductivity of battery cathode materials In order to solve the problem of poor performance, by preparing mixed valence iron-based fluorides, some ferric ions are reduced to ferrous ions by high temperature reduction method, and the mixed valence FexF3 (1 xF3(1<x≤1.2) the electronic conductivity of the cathode material itself

Method used

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  • Mixed-valence iron-based fluoride positive electrode material and preparation method thereof

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Effect test

Embodiment 1

[0019] Weigh FeF 3 ·3H 2 O raw materials were placed in a high-temperature reaction furnace, heated to 200°C under the protection of argon, and then kept for 2 hours; heated again to 400°C, kept for 2 hours, and then naturally cooled to room temperature to obtain the precursor. Mix the precursor with oxalic acid at a mass ratio of 1:1.5, high-speed ball milling and ensure that the particle size D90≤10μm, place it in a high-temperature and high-pressure reaction furnace, and feed hydrogen-argon mixed gas (hydrogen concentration is 10%), After heating up to 420° C. and keeping it warm for 20 minutes, the hydrogen-argon gas mixture was stopped, and the argon gas was injected again to rapidly cool to room temperature to obtain the mixed valent iron-based fluoride positive electrode material. After the cathode material is assembled into a single battery with LiCl spacer powder and lithium-boron alloy, the discharge curve at 650 ° C is as follows: figure 1 As shown, the open circu...

Embodiment 2

[0021] Weigh FeF 3 ·3H 2 O raw materials were placed in a high-temperature reaction furnace, heated to 200°C under the protection of argon, and then kept for 2 hours; heated again to 400°C, kept for 2 hours, and then naturally cooled to room temperature to obtain the precursor. Mix the precursor with oxalic acid at a mass ratio of 1:2, and after high-speed ball milling to ensure that D90≤10 μm, place it in a high-temperature and high-pressure reaction furnace, feed hydrogen-argon mixed gas (hydrogen concentration is 10%), and heat up to After holding at 420°C for 30 minutes, stop feeding the hydrogen-argon gas mixture, and then feed the argon gas again to quickly cool to room temperature to obtain the mixed valence iron-based fluoride positive electrode material.

Embodiment 3

[0023] Weigh FeF 3 ·3H 2 O raw materials were placed in a high-temperature reaction furnace, heated to 200°C under the protection of argon, and then kept for 2 hours; heated again to 400°C, kept for 2 hours, and then naturally cooled to room temperature to obtain the precursor. Mix the precursor with oxalic acid at a mass ratio of 1:1, and after high-speed ball milling to ensure that D90≤10 μm, place it in a high-temperature and high-pressure reaction furnace, feed hydrogen-argon mixed gas (hydrogen concentration is 10%), and heat up to After holding at 420°C for 10 minutes, stop feeding the hydrogen-argon gas mixture, and then feed the argon gas again to rapidly cool to room temperature, and then obtain the mixed valence iron-based fluoride positive electrode material.

[0024] In summary, the present invention creatively proposes a mixed valence Fe x f 3 (1≤x≤1.2) The preparation method of the positive electrode material controls the content of ferrous iron in the positiv...

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Abstract

The invention discloses a mixed-valence iron-based fluoride positive electrode material and a preparation method thereof. The method comprises the steps that 1, newly-prepared FeF3.3H2O is weighed, heated to 180-220 DEG C under the argon protection condition and then subjected to heat preservation for 2 h; raising the temperature to 400-420 DEG C again, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain a precursor; 2, mixing the precursor with oxalic acid, and carrying out high-speed ball milling and drying treatment; and 3, putting the mixture of the precursor and oxalic acid into a high-temperature reactor, introducing hydrogen-argon mixed gas, heating to 420 DEG C, keeping the temperature for 10-30 minutes, stopping introducing the hydrogen-argon mixed gas, introducing argon again, and quickly cooling to room temperature to obtain the mixed-valence iron-based fluoride positive electrode material of which the structural general formula is FexF3,wherein x is more than 1 and less than or equal to 1.2. The preparation method of the positive electrode material is good in flexibility, the content of ferrous iron in the positive electrode material can be controlled by adjusting the addition amount of oxalic acid and the reaction time, the technological method is simple, the operation labor intensity is low, and the requirement of large-scaleindustrial production is met.

Description

technical field [0001] The invention relates to the fields of electrochemistry and material chemistry, in particular to a mixed-valent iron-based fluoride cathode material and a preparation method thereof. Background technique [0002] The thermal battery is a primary reserve battery that uses the heating system of the battery itself to heat and melt the non-conductive solid-state salt electrolyte into an ionic conductor and enter the working state. Because of its long storage period, high specific power and fast activation time, it is widely used in missiles, rockets, bombs and other weapon systems. [0003] At present, one of the research focuses in the field of thermal battery technology is the development of a new generation of high-voltage cathode materials, subject to the influence of the decomposition voltage of the alkali metal halide electrolyte used in thermal batteries, NiCl 2 , FeF 3 Cathode materials with a lithium potential in the range of 2.5V-3.0V have rece...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M6/36
CPCH01M4/582H01M6/36H01M2004/028Y02E60/10
Inventor 罗重霄胡冉季柳燕王晓敏洪俊林
Owner SHANGHAI INST OF SPACE POWER SOURCES
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