Sol-gel method for preparing zinc-ion-modified carbon-coated lithium vanadium phosphate used as anode material of lithium ion battery

A technology of carbon-coated lithium vanadium phosphate and sol-gel method, which is applied in the field of lithium vanadium phosphate materials and its preparation, can solve the problems of low electronic conductivity and poor cycle performance, and achieve excellent electrochemical performance of the material and optimize the electrochemical performance. Chemical performance and the effect of less reactants

Inactive Publication Date: 2013-12-04
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of low electronic conductivity and poor cycle performance of lithium-ion battery positive electrode materials, and prepare zinc ion-doped carbon-coated lithium vanadium phosphate positive electrode materials by using a sol-gel method with pH control

Method used

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  • Sol-gel method for preparing zinc-ion-modified carbon-coated lithium vanadium phosphate used as anode material of lithium ion battery
  • Sol-gel method for preparing zinc-ion-modified carbon-coated lithium vanadium phosphate used as anode material of lithium ion battery
  • Sol-gel method for preparing zinc-ion-modified carbon-coated lithium vanadium phosphate used as anode material of lithium ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0024]Dissolve 6.189g of citric acid in 20mL of deionized water, pour it into a beaker containing 2.679g of vanadium pentoxide, and stir on a magnetic heating stirrer at a constant temperature of 60°C for 30 minutes to form a dark blue solution. Dissolve 5.080 g of ammonium dihydrogen phosphate and 1.632 g of lithium carbonate in 20 mL of deionized water, respectively, and add them to the dark blue solution. At this time, the pH value of the solution was 7, and the mixed liquid was stirred at a constant temperature of 60° C. for 1.5 hours on a magnetic heating stirrer. Raise the temperature to 80°C, stir to evaporate the solvent to form a dark blue wet gel, put it in an oven at 80°C and let it stand for 1 day to form a dry gel. Grinding the xerogel with a mortar for 30 minutes turned into a green powder. Incubate at 350°C for 4 hours under a hydrogen-nitrogen mixture containing 5% (volume ratio) of hydrogen to remove gases such as ammonia and water vapor. Then heat up to 750...

Embodiment 2

[0027] Dissolve 5.156g of citric acid in 20mL of deionized water, pour it into a beaker containing 2.219 vanadium pentoxide, and stir on a magnetic heating stirrer at a constant temperature of 60°C for 30 minutes to form a dark blue solution. Dissolve 4.232g of ammonium dihydrogen phosphate, 1.360g of lithium carbonate and 0.011g of zinc oxide in 20mL of deionized water respectively, add to the dark blue solution, and stir for 30 minutes at a constant temperature of 60°C on a magnetic heating stirrer. The pH value was adjusted to 4 with acetic acid, and the mixed liquid was stirred at a constant temperature of 60° C. for 1 hour on a magnetic heating stirrer. Raise the temperature to 80°C, stir to evaporate the solvent to form a dark blue wet gel, put it in an oven at 80°C and let it stand for 1 day to form a dry gel. Grinding the xerogel with a mortar for 30 minutes turned into a green powder. Incubate at 350°C for 4 hours under a hydrogen-nitrogen mixture containing 5% (volu...

Embodiment 3

[0030] Dissolve 5.154g of citric acid in 20mL of deionized water, pour it into a beaker containing 2.208g of vanadium pentoxide, and stir on a magnetic heating stirrer at a constant temperature of 60°C for 30 minutes to form a dark blue solution. Dissolve 4.231g of ammonium dihydrogen phosphate, 1.360g of lithium carbonate and 0.021g of zinc oxide in 20mL of deionized water respectively, add to the dark blue solution, and stir for 30 minutes at a constant temperature of 60°C on a magnetic heating stirrer. The pH value was adjusted to 4 with acetic acid, and the mixed liquid was stirred at a constant temperature of 60° C. for 1 hour on a magnetic heating stirrer. Raise the temperature to 80°C, stir to evaporate the solvent to form a dark blue wet gel, put it in an oven at 80°C and let it stand for 1 day to form a dry gel. Grinding the xerogel with a mortar for 30 minutes turned into a green powder. Incubate at 350°C for 4 hours under a hydrogen-nitrogen mixture containing 5% (...

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Abstract

The invention discloses a sol-gel method for preparing zinc-ion-modified carbon-coated lithium vanadium phosphate used as an anode material of a lithium ion battery. The sol-gel method is characterized in that zinc doping is carried out in a reaction environment with the pH (potential of hydrogen) of 4. The sol-gel method includes adding vanadium pentoxide, zinc oxide, citric acid, ammonium dihydrogen phosphate and lithium carbonate into deionized water and uniformly mixing the vanadium pentoxide, the zinc oxide, the citric acid, the ammonium dihydrogen phosphate, the lithium carbonate and the deionized water with one another to obtain a mixture; regulating the mixture until a pH value of the mixture reaches 4-9, enabling the mixture to form wet gel at the temperature of 80 DEG C, and shifting the wet gel into a drying oven to form dry gel at the temperature of 80 DEG C; calcining the dry gel in hydrogen and nitrogen mixed gas (with a 5:95 volume ratio of hydrogen to nitrogen) at the temperature of 750 DEG C for 8 hours, naturally cooling the calcined dry gel and then grinding and sieving the cooled calcined dry gel to obtain zinc-doped carbon-coated lithium vanadium phosphate powder (with an x ranging from 0 to 0.1). A molar ratio of the vanadium pentoxide to the zinc oxide to the citric acid to the ammonium dihydrogen phosphate to the lithium carbonate is 2-x:x:4:6:3, and the x ranges from 0 to 0.1. The citric acid is simultaneously used as a complexing agent, a reducing agent and a carbon source. The sol-gel method has the advantages that the electronic conductivity and the discharge ratio capacity of the lithium vanadium phosphate anode material are improved, the circulation performance is optimized, a process is simple, the cycle is short, the cost is low, and the soil-gel method is suitable for industrial production.

Description

technical field [0001] The invention relates to lithium ion battery cathode materials, in particular to a Zn ion-modified carbon-coated lithium vanadium phosphate material and a preparation method thereof. Background technique [0002] Due to the advantages of high working voltage, small size, light weight, high specific energy, no memory effect, and no environmental pollution, lithium-ion batteries are increasingly becoming the main force in the market due to their long cycle life and good safety performance compared with lithium batteries. military. The specific capacity of the positive electrode material of lithium ion battery is much lower than that of the negative electrode material, so the final performance of the battery depends largely on the performance of the positive electrode material. The monoclinic structure polyanion positive electrode material lithium vanadium phosphate, as a potential lithium ion battery positive electrode material, has the following advant...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62
CPCY02E60/12Y02E60/10
Inventor 郭瑞松许雯雯刘丽王超
Owner TIANJIN UNIV
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