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Low-temperature nano lithium iron phosphate, and preparation method and application thereof

A low-temperature lithium iron phosphate technology, applied in the field of its preparation, low-temperature nano-lithium iron phosphate, can solve problems such as environmental pollution, large amounts of waste water, increased equipment investment and manufacturing costs, and shorten the diffusion distance and reduce primary particles The effect of particle size

Active Publication Date: 2013-10-16
江苏贝特瑞纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The low-temperature discharge performance of lithium iron phosphate nanocrystals prepared by this liquid-phase synthesis method is not good, and in order to obtain a well-crystallized nano-lithium iron phosphate material, a reaction kettle with high temperature resistance and high pressure is required by this liquid-phase synthesis method, and during the synthesis process A large amount of waste water is generated, which virtually increases equipment investment and manufacturing costs, and causes serious environmental pollution

Method used

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  • Low-temperature nano lithium iron phosphate, and preparation method and application thereof
  • Low-temperature nano lithium iron phosphate, and preparation method and application thereof
  • Low-temperature nano lithium iron phosphate, and preparation method and application thereof

Examples

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Embodiment 1

[0052] Lithium hydroxide, iron phosphate, ferrous oxalate and magnesium acetate are used in a molar ratio of 0.9:0.9:0.1:0.01 (equivalent to a molar ratio of lithium source, iron source, phosphorus source and doping elements of 0.9:1:0.9:0.01) Mix, and add ethanol according to 50% of the total mass of the material for ball milling, take out the slurry after 5 hours, and test the slurry particle size D 50 =1.8μm, dry the slurry at 80°C, put the dried powder in H 2 and N 2 (Constituent gas volume ratio H 2 :N 2 =0.1:0.9) in a mixed gas composed of 450 °C constant temperature roasting for 6 hours to obtain a precursor material with a particle size of 50-100 nm; add lithium hydroxide and phosphoric acid (85%) to this precursor material to make lithium source, iron The final molar ratio of phosphorus source and phosphorus source is 1:1:1, and 10% glucose by weight of the precursor material is added for mixing, and 50% of the total mass of the material is added with ethanol for b...

Embodiment 2

[0054] Lithium carbonate, ferrous oxalate, and ammonium dihydrogen phosphate are mixed according to the molar ratio of 0.95:1:0.95 (equivalent to the molar ratio of lithium source, iron source, phosphorus source and doping element is 0.95:1:0.95:0), and Add ethanol to 50% of the total mass of the material for ball milling, take out the slurry after 5 hours, and test the particle size D of the slurry 50 =2.1μm, dry the slurry at 80°C, and roast the dried powder at a constant temperature of 400°C for 3 hours in a protective atmosphere composed of argon to obtain a precursor material with a particle size of 100-150nm; Add lithium dihydrogen phosphate to the material so that the final molar ratio of lithium source, iron source and phosphorus source is 1.05:1:1.05, and add 8% sucrose by weight of the precursor material for mixing, and add ethanol according to 50% of the total mass of the material Perform ball milling, take out the slurry after 5 hours, dry at 80°C, and roast the dr...

Embodiment 3

[0056] Lithium dihydrogen phosphate, ferric oxide, and vanadium pentoxide are prepared at a molar ratio of 0.98:1:0.015 (equivalent to a molar ratio of lithium source, iron source, phosphorus source, and doping element of 0.98:1:0.98:003). Mix, and add ethanol according to 50% of the total mass of the material for ball milling, take out the slurry after 5 hours, and test the particle size D of the slurry 50 =1.2μm, dry the slurry at 80°C, put the dried powder in H 2 Roasting at a constant temperature of 600°C for 10 hours in a reducing atmosphere to obtain a precursor material with a particle size of 150-200 nm; add lithium acetate and diammonium hydrogen phosphate to the precursor material so that the final molar ratio of lithium source, iron source and phosphorus source is 1.1:1:1.1, and add polyvinyl alcohol with 15% of the weight of the precursor material for mixing, and add ethanol for ball milling according to 50% of the total mass of the material, take out the slurry af...

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Abstract

The invention discloses a low-temperature nano lithium iron phosphate, and a preparation method and application thereof. The low-temperature nano lithium iron phosphate is produced through the following steps of: carrying out self-division of a lithium source, an iron source and a phosphorus source in the sintering process through nonstoichiometric induction, thereby forming particles which are at non-perfect crystalline state and have primary grain size ranging from 20 to 300nm; and then performing stoichiometric regulation and sintering by supplementing the lithium source and the phosphorus source, thereby forming particles which are at perfect crystalline state and have a primary grain size ranging from 20 to 300nm, thus obtaining the low-temperature nano lithium iron phosphate. The low-temperature nano lithium iron phosphate provided by the invention has high specific capacity and excellent low-temperature discharge performance; and the method for preparing the low-temperature nano lithium iron phosphate does not need grinding equipment or a high-pressure kettle, so that the unit energy consumption and the equipment investment are greatly reduced; and the method is low in wastewater emission and environmental pollution; besides, the method is simple in production flow, does not need severe conditions and is easily industrialized.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a low-temperature nano-lithium iron phosphate, its preparation method and application. Background technique [0002] LiFePO with olivine structure since 1997 4 Since its discovery, because of its stable discharge voltage platform at 3.4V, wide source of raw materials, good thermal stability, and environmental friendliness, its application as a cathode material for lithium-ion batteries has attracted much attention. But LiFePO 4 The ionic conductivity and electronic conductivity of Li are low, and when charging and discharging, Li + In LiFePO 4 -FePO 4 The diffusion channel between the two phases is a one-dimensional channel, resulting in LiFePO 4 There are deficiencies in low temperature. [0003] Currently improved LiFePO 4 The method of low temperature performance is mainly reflected in the following three aspects: [0004] (1) Improve the conductivity of ...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M10/0525
CPCY02E60/122Y02E60/10
Inventor 席小兵黄友元岳敏杨顺毅任建国
Owner 江苏贝特瑞纳米科技有限公司
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