Preparation method of lithium ion battery cathode material carbon-coated columnar lithium vanadium phosphate

A lithium-ion battery, cathode material technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of difficult mass production, long production cycle, easy powder agglomeration, etc., to achieve uniform size and short calcination time , the effect of low calcination temperature

Inactive Publication Date: 2012-09-12
陕西精泰计量检测校准有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently used to synthesize carbon-coated Li 3 V 2 (PO 4 ) 3 Powder methods include solid-phase method and sol-gel method. Although the solid-phase method has a simple process, the calcination temperature is relatively high, and the obtained powder is easy to agglomerate; the sol-gel method can effectively improve the purity and crystallinity of the product , the calcination temperature is also low, but its production cycle is long and it is difficult to produce on a large scale

Method used

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  • Preparation method of lithium ion battery cathode material carbon-coated columnar lithium vanadium phosphate
  • Preparation method of lithium ion battery cathode material carbon-coated columnar lithium vanadium phosphate
  • Preparation method of lithium ion battery cathode material carbon-coated columnar lithium vanadium phosphate

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Experimental program
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Effect test

Embodiment 1

[0016] Step 1: By heating and stirring, the NH 4 VO 3 Dissolve in deionized water, the solution concentration is 0.06mol / L, add LiOH·H 2 O, citric acid and H 3 PO 4 , stir, and form a transparent yellow precursor solution after mixing evenly, in which LiOH·H 2 O, NH 4 VO 3 、H 3 PO 4 The molar ratio with citric acid is 3:2:3:2.

[0017] Step 2: Put the precursor solution in a hydrothermal kettle and react at 160°C for 1~2 hours. After the reaction is completed and the temperature drops to room temperature, open the reaction kettle and take out the blue gel-like product in the kettle.

[0018] Step 3: Put the blue gel-like product in an oven, dry at 90-100°C for 12-15 hours to obtain a xerogel, and then grind the xerogel into a powder with an agate mortar.

[0019] Step 4: Put dry gel powder in N 2 Calcined under protective conditions for 6 hours, the calcination temperature was 700 ° C, and after cooling down, carbon-coated columnar Li 3 V 2 (PO 4 ) 3 Powder.

Embodiment 2

[0021] Step 1: By heating and stirring, the NH 4 VO 3 Dissolve in deionized water, the solution concentration is 0.08mol / L, add LiOH·H 2 O, citric acid and H 3 PO 4 , stir, and form a transparent yellow precursor solution after mixing evenly, in which LiOH·H 2 O, NH 4 VO 3 、H 3 PO 4 The molar ratio with citric acid is 3:2:3:2.

[0022] Step 2: Put the precursor solution in a hydrothermal kettle and react at 160°C for 1~2 hours. After the reaction is completed and the temperature drops to room temperature, open the reaction kettle and take out the blue gel-like product in the kettle.

[0023] Step 3: Put the blue gel-like product in an oven, dry at 90-100°C for 12-15 hours to obtain a xerogel, and then grind the xerogel into a powder with an agate mortar.

[0024] Step 4: Put dry gel powder in N 2 Calcined under protective conditions for 6 hours, the calcination temperature was 700 ° C, and after cooling down, carbon-coated columnar Li 3 V 2 (PO 4 ) 3 Powder.

Embodiment 3

[0026] Step 1: By heating and stirring, the NH 4 VO 3 Dissolve in deionized water, the solution concentration is 0.10mol / L, add LiOH·H 2 O, citric acid and H 3 PO 4 , stir, and form a transparent yellow precursor solution after mixing evenly, in which LiOH·H 2O, NH 4 VO 3 、H 3 PO 4 The molar ratio with citric acid is 3:2:3:2.

[0027] Step 2: Put the precursor solution in a hydrothermal kettle and react at 160°C for 1~2 hours. After the reaction is completed and the temperature drops to room temperature, open the reaction kettle and take out the blue gel-like product in the kettle.

[0028] Step 3: Put the blue gel-like product in an oven, dry at 90-100°C for 12-15 hours to obtain a xerogel, and then grind the xerogel into a powder with an agate mortar.

[0029] Step 4: Put dry gel powder in N 2 Calcined under protective conditions for 6 hours, the calcination temperature was 700 ° C, and after cooling down, carbon-coated columnar Li 3 V 2 (PO 4 ) 3 Powder.

[0...

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Abstract

The invention provides a method for preparing a lithium ion battery cathode material carbon-coated columnar lithium vanadium phosphate, which comprises the following steps: preparing a NH4VO3 water solution of which the concentration is 0.06-0.10 mol / L, sequentially adding LiOH.H2O, citric acid and H3PO4 into the solution, and evenly mixing to form a precursor solution, wherein the LiOH.H2O-NH4VO3 -H3PO4-citric acid mol ratio is 3:2:3:2; putting the precursor solution into a hydrothermal kettle to react at 160 DEG C for 1-2 hours, so as to obtain a blue gel after the reaction finishes, drying the gel, and grinding the dried gel to obtain powder; and calcining the dry gel powder in an N2 furnace to obtain the carbon-coated columnar lithium vanadium phosphate composite material. By combining the hydrothermal method and the calcining technique, the technique provided by the invention is simpler and more efficient as compared with the traditional sol-gel method, and has the advantages of lower calcining temperature and shorter calcining time as compared with the traditional solid-phase method. Besides, the powder has the advantages of high purity and uniform dimension, and the crystal appearance appears columnar.

Description

technical field [0001] The invention belongs to the field of functional materials, and relates to a method for preparing carbon-coated columnar lithium vanadium phosphate, a cathode material of a lithium ion battery. Background technique [0002] As a new generation of lithium-ion battery cathode material, lithium vanadium phosphate (Li 3 V 2 (PO 4 ) 3 ) has the characteristics of good thermal stability, large charge and discharge voltage, high discharge specific capacity and excellent safety performance, and has gradually become a research hotspot for scholars. Li 3 V 2 (PO 4 ) 3 It has two crystal structures, one is monoclinic and the other is orthorhombic. Due to the monoclinic structure of Li 3 V 2 (PO 4 ) 3 The electrochemical performance is much better than that of orthorhombic Li 3 V 2 (PO 4 ) 3 , the current research on lithium vanadium phosphate mainly focuses on the monoclinic Li 3 V 2 (PO 4 ) 3 . Monoclinic Li 3 V 2 (PO 4 ) 3 Each unit cel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/10
Inventor 夏傲黄剑锋谈国强
Owner 陕西精泰计量检测校准有限责任公司
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