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Vanadium lithium iron phosphate anode material and preparation method thereof

A technology of lithium vanadium iron phosphate and positive electrode materials, applied in chemical instruments and methods, phosphorus compounds, battery electrodes, etc., can solve problems such as difficulty in deintercalation and poor cycle performance of materials, and achieve performance improvement, structural stability and cycle performance. good performance

Inactive Publication Date: 2013-04-17
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium vanadium phosphate has a higher voltage platform, and as a fast ion conductor, lithium vanadium phosphate has more lithium ions that can be deintercalated, so its conductivity is better than lithium iron phosphate, but the first lithium vanadium phosphate It is difficult to deintercalate the three lithiums, and a voltage higher than 4.6V is required to deintercalate, but the charging cut-off voltage is too high, which makes the cycle performance of the material worse

Method used

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  • Vanadium lithium iron phosphate anode material and preparation method thereof
  • Vanadium lithium iron phosphate anode material and preparation method thereof
  • Vanadium lithium iron phosphate anode material and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0028] Take Li x Fe 1-3y V 2y PO 4 In / C x=1.06, y=0.1. Weigh Li according to the molar ratio Li:Fe:V:P=1.06:0.7:0.2:1 2 CO 3 , FeC 2 o 4 2H 2 O, NH 4 VO 3 and NH 4 h 2 PO 4, while weighing 10% of the theoretical product mass of citric acid as a carbon source, weighing 0.1% of the starting material mass of polyethylene glycol as a dispersant. Add ethanol as the liquid phase medium according to 1 times the mass of the starting material, and at the same time add zirconium balls with a diameter of 3 μm according to the ball-to-material ratio of 1:1, and ball mill at 175 r / min for 3 hours. After the ball-milled sample was vacuum-dried at 120°C for 10 hours, it was pre-fired at 380°C for 4 hours in a tube furnace fed with nitrogen, and after cooling to room temperature, the sample was ground for a second time and then heated at 650°C , and nitrogen atmosphere for 18h sintering, and then cooled to room temperature, the lithium vanadium iron phosphate positive electrode...

Embodiment 2

[0030] Take Li x Fe 1-3y V 2y PO 4 In / C x=1.02, y=0.1. Weigh LiOH·H according to the molar ratio Li:Fe:V:P=1.02:0.7:0.2:1 2 O, FeC 2 o 4 2H 2 O, NH 4 VO 3 and (NH 4 ) 2 HPO 4 , while weighing 8% of the theoretical product mass of sucrose as a carbon source, weighing 3% of the starting material mass of polyacrylamide as a dispersant. Add acetone as the liquid phase medium according to the mass ratio of the starting material 1.2:1, and add 2 μm steel balls according to the ball-to-material ratio of 4:1, and ball mill at 220r / min for 2h. After the ball milled sample was dried at 50°C for 12 hours, it was pre-fired at a low temperature of 300°C for 6 hours in a tube furnace fed with argon gas, then cooled, and after regrinding, it was sintered at 700°C for 16 hours, and cooled to room temperature to obtain ferrovanadium phosphate Lithium cathode material.

Embodiment 3

[0032] Take Li x Fe 1-3y V 2y PO 4 In / C x=1.1, y=0.2. Weigh LiOH·H according to the molar ratio Li:Fe:V:P=1.1:0.4:0.4:1 2 O, Fe 2 o 3 , V 2 o 5 and (NH 4 ) 2 HPO 4 At the same time, glucose with 15% of the theoretical product mass was weighed as a carbon source. Weigh 1.5% polyethylene glycol by weight of the starting material as a dispersant. Add deionized water as the liquid phase medium according to the mass ratio of starting materials 5:1, and add 3 μm steel balls according to the ball-to-material ratio of 8:1, and ball mill at 300 r / min for 0.5 h. The ball-milled samples were dried in a vacuum oven at 100°C for 24 hours, and then the samples were finely ground. Pre-fire the ground sample in a tube furnace with reducing gas (2% hydrogen + 98% nitrogen) at a low temperature of 300°C for 6 hours, directly raise the temperature to 750°C for sintering for 12 hours, cool to room temperature and grind to obtain ferrovanadium phosphate Lithium cathode material.

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Abstract

The invention discloses a lithium-rich vanadium lithium iron phosphate anode material, aiming to overcome the respective defects of lithium iron phosphate and lithium vanadium phosphate. The material comprises LixFe1-3yV2yPO4 / C, wherein the x is great than or equal to 1.0 and less than or equal to 1.15 and the y is equal to 0.01-0.2. The material simultaneously has the composite crystal structures of olivine lithium iron phosphate and monoclinic lithium vanadium phosphate. The preparation method comprises the following steps of: weighing the initial raw materials, namely a lithium source, an iron source, a vanadium source and a phosphorus source in the molar ratio of x:(1-3y):2y:1, adding a carbon source and a dispersing agent, ball-milling and mixing in a liquid medium, subjecting to low-temperature pre-sintering and high-temperature sintering under the protection of an inert gas or a reducing gas, and cooling to the room temperature, thereby obtaining the vanadium lithium iron phosphate anode material.

Description

technical field [0001] The invention relates to a lithium vanadium iron phosphate cathode material and a preparation method thereof, in particular to a lithium vanadium iron phosphate cathode material for a lithium ion battery and a preparation method thereof, belonging to the field of lithium ion battery materials. Background technique [0002] Since 1987, the World Commission on Environment and Development has formally proposed sustainable development. More and more countries in the world realize that a sustainable society should be a society that can meet social needs without endangering the survival of future generations. The greatest unsustainability in our world today lies in energy and the environment. Therefore, developing new materials and seeking new energy must be one of the major issues that must be solved in the 21st century. The energy problems that human society is facing now include two main contents: one is the development of raw energy materials and the g...

Claims

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Application Information

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IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/10
Inventor 张云邹继洲
Owner SICHUAN UNIV
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