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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  • 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 lit

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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Example Embodiment

[0027] Example 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 At the same time, weigh 10% of the theoretical product mass of citric acid as a carbon source, and weigh 0.1% of the starting material mass of polyethylene glycol as a dispersant. Ethanol was added as the liquid phase medium according to 1 times the mass of the starting material, and zirconium balls with a diameter of 3 μm were added according to the ball-to-material ratio of 1:1, and the ball milling was performed at 175r / 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 filled with nitrogen. After cooling to room temperature, the sample was subjected to secondary grinding and then at 650°C. , And sintering in a nitrogen atmosphere for 18 hours, and then cooling to room temperature, to obtain li...

Example Embodiment

[0029] Example 2

[0030] Take Li x Fe 1-3y V 2y PO 4 In / C, x=1.02 and 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 At the same time, weigh 8% of the theoretical product mass of sucrose as a carbon source, and weigh 3% of the starting material mass of polyacrylamide as a dispersant. Acetone was added as the liquid medium according to the mass ratio of the starting materials of 1.2:1, and 2μm steel balls were added according to the ball-to-material ratio of 4:1, and ball milled at 220r / min for 2h. After the ball milled sample was dried at 50°C for 12 hours, it was pre-fired at 300°C for 6 hours in a tube furnace with argon gas and then cooled. After grinding again, it was sintered at 700°C for 16 hours and cooled to room temperature to obtain ferrovanadium phosphate. Lithium cathode material.

Example Embodiment

[0031] Example 3

[0032] Take Li x Fe 1-3y V 2y PO 4 In / C, x=1.1 and 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, 15% glucose of theoretical product mass is weighed as the carbon source. Weigh 1.5% polyethylene glycol of the starting material as a dispersant. Add deionized water as the liquid phase medium according to the mass ratio of the starting materials of 5:1, and add 3μm steel balls according to the ball-to-material ratio of 8:1, and ball mill at 300r / min for 0.5h. The ball milled sample was dried in a vacuum drying oven at 100°C for 24 hours, and then the sample was ground. The ground sample was pre-fired at 300°C for 6 hours in a tube furnace filled with reducing gas (2% hydrogen + 98% nitrogen), heated directly to 750°C, sintered for 12 hours, cooled to room temperature, and ground to obtain iron vanadium 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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