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Method for preparing metal oxide conductive powder composite lithium titanate material

A technology for oxide conduction and composite lithium titanate, applied in circuits, electrical components, battery electrodes, etc., can solve problems such as increasing the contact area between electrode materials and electrolyte, aggravating the flatulence of lithium titanate batteries, and large specific surface areas of materials , to achieve the effect of improving the surface environment and electrical conductivity, the electrochemical performance is obvious, and the preparation method is simple

Active Publication Date: 2019-05-03
郑州中科新兴产业技术研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this modification method has the problems of harsh synthesis conditions and high preparation costs, and the nanoscale material has a large specific surface area, which increases the contact area between the electrode material and the electrolyte, and will aggravate the flatulence of the lithium titanate battery.
Another example is that the patent application publication number is CN104538610B, and the title of the invention is "an improved preparation method of alkali metal ion-doped lithium titanate". The sol-gel method is used to prepare lithium titanate materials doped with Na, K and other elements. The obtained samples The particle size distribution is uniform, the high-rate discharge is stable, and the electrochemical performance is excellent. However, the cost of the sol-gel method is too high, and a large amount of organic solvents are introduced, and the environmental protection problem is prominent.

Method used

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  • Method for preparing metal oxide conductive powder composite lithium titanate material
  • Method for preparing metal oxide conductive powder composite lithium titanate material
  • Method for preparing metal oxide conductive powder composite lithium titanate material

Examples

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Embodiment 1

[0029] The preparation method of metal oxide conductive powder composite lithium titanate material in this embodiment comprises the following steps:

[0030] (1) According to Li 4 Ti 5 o 12 Stoichiometric ratio Lithium hydroxide (D50=65nm, lithium excess 3%) and titanium dioxide (D50=80nm) were weighed respectively, poured into a ball mill jar, 360-degree three-dimensional rotation dry mixing (vertical direction 20r / min, horizontal direction 300r / min) min) for 3 hours, put the mixed precursor in a muffle furnace and raise the temperature to 800°C at a rate of 2°C / min, keep it warm for 8 hours, cool naturally, vibrate and sieve (400 mesh) after grinding to obtain D50 = 0.3μm Lithium titanate material;

[0031] (2) Weigh Sb according to the ratio of n(Sb):n(Sn) = 1.1% 2 o 3 and SnO 2 , pour it into the agate ball mill jar, add deionized water and agate balls (the ratio of ball to material is 5:1), adjust the solid content to 40%, put it on the ball mill and mix and grind a...

Embodiment 2

[0034] The preparation method of metal oxide conductive powder composite lithium titanate material in this embodiment comprises the following steps:

[0035] (1) According to Li 4 Ti 5 o 12 Stoichiometric ratio Lithium carbonate (D50=2.5μm, lithium excess 7%) and titanium dioxide (D50=1.3μm) were weighed respectively, poured into a ball mill jar, 360-degree three-dimensional rotation dry mixing (vertical direction 20r / min, horizontal direction 200r / min) for 12h, put the mixed precursor in the muffle furnace and raise the temperature to 800°C at a rate of 5°C / min, keep it warm for 16h, cool naturally, vibrate and sieve (400 mesh) after grinding to get D50 = 2.2 μm lithium titanate material;

[0036] (2) Weigh Sb according to the ratio of n(Sb):n(Sn) = 2.1% 2 o3 and H 3 SnO 3 , pour it into the agate ball mill jar, add ethanol and agate balls (the ratio of ball to material is 4:1), adjust the solid content to 55%, put it on the ball mill and mix and grind for 6 hours at a...

Embodiment 3

[0039] The preparation method of metal oxide conductive powder composite lithium titanate material in this embodiment comprises the following steps:

[0040] (1) According to Li 4 Ti 5 o 12 Stoichiometric ratio Lithium hydroxide (D50=0.65μm, lithium excess 5%) and titanium dioxide (D50=1.2μm) were weighed respectively, poured into a ball mill jar, 360-degree three-dimensional rotation dry mixing (vertical direction 20r / min, horizontal direction 200r / min) for 10h, put the mixed precursor in the muffle furnace and raise the temperature to 800°C at a rate of 5°C / min, keep it warm for 10h, cool naturally, vibrate and sieve (400 mesh) after grinding to obtain D50 = 0.53μm lithium titanate material;

[0041] (2) Weigh Sb according to the ratio of n(Sb):n(Sn) = 2% 2 o 3 and Sn(NO 3 ) 2 , pour it into the agate ball mill jar, add ethylene glycol and agate balls (the ratio of ball to material is 5:1), adjust the solid content to 50%, put it on the ball mill and mix and grind for...

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Abstract

The invention discloses a method for preparing a metal oxide conductive powder composite lithium titanate material, which comprises the following steps: (1) preparing a pure phase lithium titanate material Li4Ti5O12 by weighing lithium salt and titanium dioxide according to a stoichiometric ratio that the lithium has an excess of 3% to 7%; (2) preparing a metal oxide conductive powder (doped withantimony tin oxide) according to a ratio of n(Sb):n(Sn)=1.1% to 2.1%; and (3) mixing the metal oxide conductive powder and the pure phase lithium titanate material Li4Ti5O12 to obtain high-performancelithium titanate composite material by high-temperature calcinations and pulverization. The lithium titanate composite material prepared by the method has a uniform particle size, the inter-particleconductive material improves the diffusion ability of the electrons between the particles, and improves the electrical conductivity of the lithium titanate material. The preparation method of the material is simple, and is convenient for amplification preparation and industrial production.

Description

technical field [0001] The invention relates to the technical field of lithium ion negative electrode materials, in particular to a metal oxide conductive powder composite lithium titanate material and a preparation method thereof. Background technique [0002] Lithium-ion batteries, as a clean energy source, have been widely used since the early 1990s due to their small size, high energy density, safety and environmental protection, and the anode materials as their main components have also made great progress. . [0003] Lithium titanate batteries have the advantages of excellent low-temperature performance, high-power charging and discharging characteristics, high safety, and low life-cycle cost, and are especially suitable for green energy storage technologies that require long life, high safety, and low cost. Although the lithium titanate battery has the above advantages, but at the same time lithium titanate (Li 4 Ti 5 o 12 ) The electronic and ionic conductivity o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/62H01M10/0525
CPCY02E60/10
Inventor 刘艳侠张锁江柴丰涛张鹏飞刘福园李晶晶
Owner 郑州中科新兴产业技术研究院
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