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Preparation method of phosphorus position partly substituted iron lithium phosphate powder

A technology of lithium iron phosphate and powder, which is applied in the field of electrochemical power material preparation, can solve the problems of weakening Fe-O bond, reducing open circuit voltage, and crystal structure without lithium insertion-storage, etc., and achieves good crystallization performance and high composition Uniform, broad-spectrum effect

Inactive Publication Date: 2006-06-14
TSINGHUA UNIV
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Problems solved by technology

However, S, As, Mo, and W all replace P, which will weaken the bond of Fe-O and reduce its open circuit voltage. On the other hand, the formed crystal structure does not have the properties of lithium insertion-storage, and this patent is not implemented. Example as a feasibility verification and support for compounds that fully replace P

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  • Preparation method of phosphorus position partly substituted iron lithium phosphate powder
  • Preparation method of phosphorus position partly substituted iron lithium phosphate powder
  • Preparation method of phosphorus position partly substituted iron lithium phosphate powder

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[0025] The present invention provides a partially substituted phosphorus lithium iron phosphate lithium ion battery positive electrode material that significantly improves the performance of the matrix basic battery by partially replacing the phosphorus element in the phosphorus position in lithium iron phosphate with boron, tungsten, sulfur and silicon elements Powder preparation method. Said lithium ion battery cathode material lithium iron phosphate uses molecular formula LiFeP 1-y D. y o 4 Indicates that D is a substitute, 0<y≤0.5;

[0026] The specific preparation method of the phosphorus partially substituted lithium iron phosphate powder is as follows:

[0027] Lithium salt, ferrous salt, phosphate and substituents are mixed once at a molar ratio of Li:Fe:P:D=1:1:(1-y):y, and then deionized water, industrial alcohol and no At least one of water and ethanol is used as a mixing medium for ball milling for 6 to 12 hours, and dried at 40 to 70°C; after drying, the powde...

Embodiment 1

[0040] 0.05 mol lithium carbonate Li 2 CO 3 , 0.1 mole ferrous oxalate Fe(C 2 o 4 )·2H 2 O and 0.0975 moles of ammonium dihydrogen phosphate NH 4 h 2 PO 4 and 0.0025 moles of boric acid H 3 BO 4 Mix, add to a polyester tank, add 55ml of absolute alcohol, seal and mix on a planetary ball mill for 10 hours, discharge and dry under a nitrogen atmosphere of 0.3 liters / minute, and raise the temperature to 400°C, keep warm for 8 hours, cool down to room temperature with the furnace to obtain pre-burned material; then use industrial alcohol as the medium for ball milling for 6 hours, and after drying the material, in a nitrogen atmosphere of 0.3 liters / min, the temperature rises at a rate of 4°C / min The rate was raised to 700°C, kept at this temperature for 8 hours, and cooled to room temperature with the furnace, and the obtained positive electrode material LiFe(P 0.975 B 0.025 o 4 ) is recorded as sample A. figure 1 In A is the resulting LiFe(P 0.975 B 0.025 o 4 ) XR...

Embodiment 2

[0043] 0.1 lithium hydroxide LiOH·H 2 O, 0.1 mole of ferrous oxalate and 0.07 mole of diammonium hydrogen phosphate (NH 4 ) 2 HPO 4 and 0.03 mole of trimethyl borate (CH 3 O) 3 B is mixed, put into a polyester tank, add 40ml of absolute alcohol, seal it and mix it on a planetary ball mill for 6 hours. to 430°C, keep at this temperature for 7.5 hours, and cool to room temperature with the furnace. Take out the calcined material, add an appropriate amount of deionized water, and seal the ball mill for 10 hours. After the discharge is dried, in a nitrogen-hydrogen mixed atmosphere of 0.3 liters / minute (nitrogen: hydrogen = 9: 1, volume ratio), at 4 ° C / minute The heating rate rose to 720 °C, kept at this temperature for 7 hours, and cooled to room temperature with the furnace, and the obtained positive electrode material LiFe(P 0.7 B 0.3 o 4 ) is recorded as sample B. figure 1 In B is obtained LiFe(P 0.7 B 0.3 o 4 ) XRD pattern, the addition of boron did not change ...

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Abstract

The present invention discloses a preparation method of phosphorus position partial substituted type iron lithium phosphate powder body, belonging to the field of electrochemical power supply material preparation technology. The molecular formula of said positive electrode iron lithium phosphate of lithium ion cell is LiFeP1-yDyO4. Its preparation method includes the following steps: mixing lithium salt, ferrous salt, phosphate and substitution compound according to a certain mole ratio, drying, low-temperature prefiring and high-temperature secondary calcining so as to obtain the phosphorus position partial substituted type iron lithium phosphate powder body. Said invention uses the compound of boron, tungsten, sulfur and silicon or elementary substance as substitution compound.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrochemical power source materials. In particular, it relates to a method for preparing a phosphorous partially substituted lithium iron phosphate powder as a common secondary lithium ion battery or a modified lithium ion battery positive electrode material for power energy. technical background [0002] Lithium-ion battery is a new type of green high-energy rechargeable battery that appeared in the early 1990s. It has many advantages such as high voltage, high energy density, good cycle performance, small self-discharge, no memory effect, and wide operating temperature range. It is widely used in mobile Telephones, notebook computers, portable electric tools, electronic instruments, weapons and equipment, etc. also have good application prospects in electric vehicles, and have become the focus of research and development by countries all over the world. The positive electrode material...

Claims

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Application Information

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IPC IPC(8): C01G49/00C01B17/98C01B25/08C01B33/00C01D15/00C01G41/00
CPCY02E60/10
Inventor 唐子龙罗绍华张中太卢俊彪闫俊萍
Owner TSINGHUA UNIV
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