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A preparation method of titanium nitride and carbon double-coated lithium manganese iron phosphate composite material

A technology for coating ferromanganese phosphate and composite materials, which is applied in electrochemical generators, structural parts, electrical components, etc. Unsatisfactory effect and other problems, to achieve the effect of improving cycle stability, high tap density, and simple use of equipment

Active Publication Date: 2019-07-12
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it has been reported that nano-scale lithium manganese phosphate materials have been obtained by hydrothermal method, sol-gel and other methods, the preparation method is complicated, the cost is high, and the tap density of the dispersed nanoparticles is very low, resulting in a very low volumetric energy density. , which is not conducive to practical application
In addition, since LiMnPO 4 It does not have a good affinity with carbon, and the effect of carbon coating in the existing preparation methods is generally unsatisfactory. In order to obtain a higher discharge capacity, it is necessary to add a proportion of up to 20-30wt% carbon, which further reduces the power density of the battery.
[0004] LiMnxFe as an olivine structure 1 -xPO 4 The material is in LiMnPO 4 developed on the basis of the modified, LiMnxFe 1 -xPO 4 The material has two charging and discharging platforms, compared to LiFePO 4 The specific energy is higher than that of LiMnPO 4 The conductivity is good, and it has good cycle and rate; however, although Fe 2+ The introduction of lithium manganese phosphate can improve the conductivity of lithium manganese phosphate, but the range of improvement is limited, and it is difficult to make full use of the electrochemical performance of the material.

Method used

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  • A preparation method of titanium nitride and carbon double-coated lithium manganese iron phosphate composite material
  • A preparation method of titanium nitride and carbon double-coated lithium manganese iron phosphate composite material
  • A preparation method of titanium nitride and carbon double-coated lithium manganese iron phosphate composite material

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Embodiment 1

[0030] A preparation method of a titanium nitride and carbon double-coated lithium manganese iron phosphate composite material, specifically comprising the following steps:

[0031] 1) According to the molar ratio of Li:Mn:Fe:P=1.05:0.8:0.2:1, respectively weigh lithium carbonate, manganese acetate, ferrous oxalate and ammonium dihydrogen phosphate for material preparation, and LiMn synthesized according to theory 0.8 Fe 0.2 PO 4 5% of the mass of the material weighed sucrose, lithium carbonate, manganese acetate, ferrous oxalate, ammonium dihydrogen phosphate and sucrose were wet ball milled and dried, and then ball milled to obtain LiMn 0.8 Fe 0.2 PO 4 Precursor;

[0032] 2) Put the above precursors into the tube furnace, under protective N 2 Under the atmosphere, the temperature was raised to 750 °C at a rate of 5 °C / min and calcined for 10 h, and the NH 3 and TiCl preheated to 60°C 4 to N 2 As the carrier gas is passed into the tube furnace, the protective N is con...

Embodiment 2

[0035] A preparation method of a titanium nitride and carbon double-coated lithium manganese iron phosphate composite material, specifically comprising the following steps:

[0036] 1) According to the molar ratio of Li:Mn:Fe:P=1.0:0.5:0.5:1, respectively weigh lithium hydroxide, manganese acetate, ferric oxide and phosphoric acid for preparation, and LiMn synthesized according to theory 0.5 Fe 0.5 PO 4 Weigh glucose at 3% of the mass of the material, wet lithium hydroxide, manganese acetate, ferric oxide, phosphoric acid and glucose through ball milling and drying, and then ball mill to obtain LiMn 0.5 Fe 0.5 PO 4 Precursor;

[0037] 2) Put the above precursor into a tube furnace, raise the temperature to 600°C at a rate of 2°C / min in an argon atmosphere, and heat it for 15 hours, then add NH 3 , TiCl preheated to 60°C 4 to N 2 Pass the carrier gas into the tube furnace separately, control the argon, NH 3 and carrier N 2 The flow rates were 600mL / min, 100mL / min and 2...

Embodiment 3

[0039] A preparation method of a titanium nitride and carbon double-coated lithium manganese iron phosphate composite material, specifically comprising the following steps:

[0040] 1) According to the molar ratio of Li:Mn:Fe:P=1.1:0.6:0.4:1, weigh lithium lithium acetate, manganese oxalate, ferrous oxalate and ammonium dihydrogen phosphate for preparation, and LiMn synthesized according to theory 0.6 Fe 0.4 PO 4 8% of the mass of the material weighs the phenolic resin, and the lithium source, the manganese source, the iron source, the phosphorus source and the carbon source are subjected to wet ball milling and drying, and then ball milled to obtain LiMn 0.6 Fe 0.4 PO 4 Precursor;

[0041] 2) Put the above precursors into the tube furnace, under protective N 2 Under the atmosphere, the temperature was raised to 800 °C at a rate of 8 °C / min for 10 h, and the TiCl preheated to 60 °C was 4 to N 2 as carrier gas, and NH 3 Pass into the tube furnace respectively, control t...

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Abstract

The invention discloses a preparation method for a lithium manganese iron phosphate composite coated by both titanium nitride and carbon. The preparation method comprises the following steps: adding a certain amount of a carbon source during synthesis of a precursor; and then during sintering, introducing NH3 in a protective atmosphere, introducing TiCl4 with N2 as carrying gas and uniformly depositing a layer of a titanium nitride coating on the surface of lithium manganese iron phosphate by using a chemical vapor deposition method so as to prepare the lithium manganese iron phosphate composite uniformly coated by both titanium nitride and carbon. According to the invention, through adjustment of a carbon source addition amount during synthesis and the flow and deposition time of the three gases during vapor deposition, the granularity, thickness and bulk density of the coating can be adjusted, and the lithium manganese iron phosphate composite uniformly coated by both titanium nitride and carbon can be obtained. The coating has good uniformity and consistency; the composite has high tap density and good conductivity; a lithium ion positive electrode material using the composite has good charge and discharge rate and cycle stability; and the preparation method is simple, controllable and easy for industrial production.

Description

technical field [0001] The invention relates to the field of positive electrode materials for lithium ion batteries, in particular to a preparation method of a titanium nitride and carbon double-coated lithium manganese iron phosphate composite material. Background technique [0002] Phosphate-like material LiMPO with olivine structure 4 (M=Fe, Mn, Ni, Co) is used as a lithium-ion battery material, its theoretical capacity is about 170mAh / g, and it has many advantages such as stable structure, low reactivity with electrolyte, high safety, and good battery cycle performance. advantage. Among such phosphate materials, LiFePO 4 The synthesis of materials is relatively simple, and large-scale production and sales have been realized. However, LiFePO 4 Due to the low potential platform (about 3.4V) of lithium deintercalation, the material reduces the overall energy density of the battery and limits its development in electric vehicles. while LiMnPO 4 The working voltage for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M4/136H01M4/1397H01M10/0525
CPCH01M4/136H01M4/1397H01M4/362H01M4/5825H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 郭钰静刘兴亮杨茂萍汪志全
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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