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Prepn process of oxygen place doped lithium ferric phosphate powder

A lithium iron phosphate, doped technology, used in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as insignificant effects, and achieve the effects of improving the basic capacity of the parent body, improving the cycle electrical performance, and widening sources.

Inactive Publication Date: 2006-05-17
TSINGHUA UNIV
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Problems solved by technology

[0004] In other cathode materials, such as spinel lithium manganese oxide LiMn 2 o 4 , usually doping with low-valent metal ions to replace the manganese site can improve the tetravalent manganese Mn 4+ The proportion in the compound, so as to stabilize the crystal structure and limit the occurrence of the Jahn-Teller effect, is a relatively effective method in improving the cycle performance at room temperature, but under high temperature (>55°C) operating conditions, the effect of this method is less not obvious

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  • Prepn process of oxygen place doped lithium ferric phosphate powder
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  • Prepn process of oxygen place doped lithium ferric phosphate powder

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preparation example Construction

[0028] The specific method for preparing the oxygen site-doped lithium iron phosphate powder is as follows:

[0029] 1) One-time mixing method of adulterant and parent material

[0030] According to the molar ratio of lithium salt, ferrous salt and phosphate to Li:Fe:P = 1:1:1, the parent material is mixed at a time at the molar ratio of parent: dopant = 1:0.001-2 Then add at least one of deionized water, industrial alcohol and anhydrous ethanol as a mixing medium. The mixing time is 6-12 hours and dried at 40-70℃. After drying, the powder is in nitrogen and argon. At least one of the mixed gas of nitrogen and hydrogen is heated under an inert atmosphere or a reducing atmosphere at 400-550°C and kept for 2-10 hours for pre-calcination; the precursor pre-calcined material is ball-milled for 6-12 hours at a temperature of 40-70 Drying at ℃, and then calcination at 550~850℃ under at least one of nitrogen, argon, and nitrogen-hydrogen mixed gas in an inert or reducing atmosphere to ob...

Embodiment 1

[0045] Mix 0.05 mol of lithium carbonate, 0.1 mol of ferrous oxalate and 0.1 mol of ammonium dihydrogen phosphate, add to a polyester tank, add 25 ml of anhydrous alcohol, seal and mix on a planetary ball mill for 10 hours, under 0.3 liters / min of nitrogen In the atmosphere, increase to 400°C at a heating rate of 5°C / min, keep at this temperature for 8 hours, then cool to room temperature along with the furnace, take out 0.1 mole of precursor pre-calcined material, add 0.04 mole of thiourea to the polyester tank, and add appropriate amount of alcohol , After sealing, ball mill for 6 hours, then in a nitrogen atmosphere of 0.3 liters / min, the temperature is increased to 700 ℃ at a heating rate of 4 ℃ / min, kept at this temperature for 8 hours, and then cooled to room temperature with the furnace. The resulting cathode material is LiFePS 0.4 O 3.6 , Marked as sample A. figure 1 Middle A is the resulting LiFePO 4 XRD pattern, the addition of dopants did not change LiFePO 4 The crysta...

Embodiment 2

[0048] Mix 0.05 lithium carbonate with 0.1 moles of ferrous oxalate, 0.1 moles of ammonium dihydrogen phosphate and 0.062 moles of elemental sublimed sulfur, add them to a polyester tank, add 30ml of anhydrous alcohol, seal and mix on a planetary ball mill for 6 hours. Under a nitrogen atmosphere of 1 liter / min, the temperature is increased to 430 ℃ at a heating rate of 5 ℃ / min, and kept at this temperature for 7.5 hours. After cooling to room temperature with the furnace, take out 0.1 mol of the precursor pre-burned material and add it to the polyester tank, and add an appropriate amount Alcohol, sealed and ball milled for 10 hours, then in a 0.3L / min nitrogen-hydrogen mixed atmosphere (nitrogen:hydrogen=9:1, volume ratio), the heating rate is 4℃ / min to 720℃, and the temperature is kept at this temperature After 7 hours, cool down to room temperature with the furnace. The resulting cathode material is LiFePS 0.62 O 3.38 , Marked as sample B. figure 1 Middle B is the resulting Li...

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Abstract

The present invention belongs to the field of electrochemical power source material preparing technology, and is especially preparation process of oxygen place doped lithium ferric phosphate powder. The oxygen place doped lithium ferric phosphate as positive pole material in lithium ion cell has the molecular expression LiFeP(MxO4-x), and is prepared through mixing the dopant and the mother body material and sintering the mixture, or through solid phase reaction of the dopant and the mother body material. The preparation process has effective doping in the oxygen place of mother body material and the prepared material can raise the capacity and the circular discharge performance of the cell effectively and thus can find its wide application as positive pole material in secondary lithium ion cell and power cell.

Description

Technical field [0001] The invention belongs to the technical field of electrochemical power supply material preparation. In particular, it relates to a method for preparing an oxygen-site doped lithium iron phosphate powder as a commonly used 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, low 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 in various countries around the world. The cathode material is an important part of...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 张中太罗绍华唐子龙卢俊彪闫俊萍
Owner TSINGHUA UNIV
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