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Preparation method of transition element doped iron lithium phosphate powder

A technology of lithium iron phosphate and transition elements, which is applied in the field of preparation of electrochemical power materials, can solve the problems that have not been mentioned, the research on doping modification has not been reported, and the ideas and examples have not been mentioned, so as to achieve wide application prospects, Improved capacity and capacity cycle performance, good crystallization performance

Inactive Publication Date: 2006-06-14
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composition of the compound mentioned in US2004005265 is A x (M' 1-a M" a ) y (XD 4 ) z , whose M" is a doping element, 0.0001<a≤0.1, including IIA~VIIIA, IB~VIB elements, but does not mention VIIB and Group VIII as doping elements; although it is mentioned that M' involves the first The transition metal elements of the transition system, but they are the status of the main element rather than the dopant element
On the other hand, whether the crystal structure formed by these doping forms has the properties of lithium insertion-storage, there is no example in this patent as a verification and support of feasibility
Moreover, in this patent, there is no mention of ideas and examples about doping transition elements at the A site
In summary, so far, the effects of transition elements (excluding Fe) on lithium iron phosphate LiFePO 4 The research on the doping modification at the lithium site has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 0.0997 moles of lithium hydroxide LiOH·H 2 O, 0.1 mole ferrous oxalate Fe(C 2 o 4 )·2H 2 O and 0.1 mole ammonium dihydrogen phosphate NH 4 h 2 PO 4 and 0.0003 mol cobalt oxalate tetrahydrate Co(C 2 o 4 )·4H 2 O mixed, put into a polyester tank, add 70ml of absolute alcohol, seal and mix on a planetary ball mill for 10 hours. To 400°C, keep warm for 8 hours, cool down to room temperature with the furnace, get pre-burned material, use denatured 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 a temperature of 8 hours, and then cooled to room temperature with the furnace, and the obtained positive electrode material Li 0.997 co 0.003 FePO 4 .

[0029] Weigh 0.9g of positive electrode powder, add 0.19g of carbon black, 0.096g of polyvinylidene fluoride, use absolute ethanol as a dispersant, mix with ultras...

Embodiment 2

[0031] 0.0495 moles of lithium carbonate Li 2 CO 3 , 0.1 mol of ferrous acetate Fe(CH 3 COO) 2 2H 2 O and 0.1 mole ammonium phosphate (NH 4 ) 3 PO 4 Mix it with 0.001 mole of cobalt oxide CoO, add it to a polyester tank, add 100ml of industrial alcohol, seal it and mix it on a planetary ball mill for 6 hours. The heating rate was raised to 430°C, kept for 7.5 hours, and cooled to room temperature with the furnace to obtain pre-fired material, which was ball milled with water for 10 hours, and dried in a nitrogen-hydrogen mixed atmosphere of 0.3 liters / minute (nitrogen: hydrogen) =9:1, volume ratio), the temperature was raised to 720°C at a rate of 4°C / min, kept for 7 hours, and cooled to room temperature with the furnace to obtain the positive electrode material Li 0.99 co 0.01 FePO 4 .

[0032] Weigh 1.125g of positive electrode powder, add 0.169g of carbon black, 0.12g of polyvinylidene fluoride, make electrode sheets and assemble batteries according to the method ...

Embodiment 3

[0034] 0.098 moles of lithium acetate Li(CH 3 COO, 0.1 mole ferrous chloride FeCl 2 and 0.1 mole diammonium hydrogen phosphate (NH 4 ) 2 HPO 4 and 0.002 mole cobalt chloride hexahydrate CoCl 2 ·6H 2 O mixed, put into a polyester tank, add 75ml of absolute alcohol, seal it and mix it on a planetary ball mill for 7 hours. to 450°C, keep it warm for 9 hours, cool down to room temperature with the furnace, and obtain pre-fired material, use industrial alcohol as the medium for ball milling for 10 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 increased to 700 °C, kept at this temperature for 8 hours, and cooled to room temperature with the furnace to obtain the positive electrode material Li 0.98 co 0.02 FePO 4 .

[0035] Weigh 1.02g of positive electrode powder, add 0.184g of carbon black, 0.096g of polyvinylidene fluoride, make electrode sheets and assemble batteries according to the...

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Abstract

The present invention discloses a preparation method of transition element Mn, Co and Ni doped iron lithium phosphate powder body, belonging to the field of electrochemical power supply material preparation technology. Its molecular formula is Li1-x TRxFePO4, and its preparation method includes the following steps: weighting lithium salt, ferrous salt, phosphate and adulterant according to mole ratio, mixing them, drying, low-temperature prebaking and high-temperature secondary calcining so as to obtain the invented product which can be used as positive electrode material of lithium ion cell.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrochemical power source materials. In particular, it relates to a preparation method of a transition element-doped lithium iron phosphate powder used 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 is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45
Inventor 唐子龙罗绍华张中太卢俊彪闫俊萍
Owner TSINGHUA UNIV
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