A kind of preparation method of 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 obvious electrochemical performance, improve environmental and electrical conductivity, and simple preparation method

Active Publication Date: 2021-03-02
郑州中科新兴产业技术研究院 +1
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  • 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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  • A kind of preparation method of metal oxide conductive powder composite lithium titanate material
  • A kind of preparation method of metal oxide conductive powder composite lithium titanate material

Examples

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Comparison scheme
Effect test

Embodiment 1

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

[0030] (1) According to Li 4 Ti 5 O 12 Lithium hydroxide (D50=65nm, excess lithium 3%) and titanium dioxide (D50=80nm) were weighed in stoichiometric ratio, poured into a ball mill jar, and dry mixed in a 360-degree three-dimensional rotation (20r / min in the vertical direction, 300r / min in the horizontal direction). min) 3h, put the mixed precursor in a muffle furnace and raise the temperature to 800°C at a heating rate of 2°C / min, keep for 8 h, cool naturally, and then vibrate and sieve (400 mesh) after grinding to obtain D50 = 0.3 μm 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 balls to material is 5:1), prepare the solid content to reach 40%, put it on the ball mil...

Embodiment 2

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

[0035] (1) According to Li 4 Ti 5 O 12 Lithium carbonate (D50=2.5μm, excess lithium 7%) and titanium dioxide (D50=1.3μm) were weighed in a stoichiometric ratio, poured into a ball mill jar, and dry mixed in a 360-degree three-dimensional rotation (20r / min in the vertical direction and 200r in the horizontal direction). / min) for 12h, put the mixed precursor in a muffle furnace and raise the temperature to 800°C at a heating rate of 5°C / min, keep for 16 h, cool down naturally, and then vibrate and sieve (400 mesh) after grinding to obtain 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), prepare the solid content to reach 55%, put it on the...

Embodiment 3

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

[0040] (1) According to Li 4 Ti 5 O 12 Lithium hydroxide (D50=0.65μm, excess lithium 5%) and titanium dioxide (D50=1.2μm) were weighed in the stoichiometric ratio, poured into a ball mill jar, and dry mixed in a 360-degree three-dimensional rotation (20r / min in the vertical direction and 20 r / min in the horizontal direction). 200r / min) for 10h, put the mixed precursor in a muffle furnace and raise the temperature to 800°C at a heating rate of 5°C / min, keep it for 10 h, cool it naturally, and then 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 balls to material is 5:1), prepare the solid content to 5...

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Abstract

The invention discloses a preparation method of a metal oxide conductive powder composite lithium titanate material, which comprises the following steps: (1) taking lithium salt and titanium dioxide according to the ratio of stoichiometric lithium excess of 3% to 7% to prepare pure phase titanium Lithium acid material Li 4 Ti 5 o 12 ; (2) Prepare metal oxide conductive powder (antimony-doped tin oxide) according to the ratio of n(Sb):n(Sn)=1.1%~2.1%; (3) Mix the above metal oxide conductive powder with lithium titanate Material Li 4 Ti 5 o 12 ; Prepare the compound by mixing and crushing after high-temperature roasting to obtain a high-performance lithium titanate composite material. The particle size of the lithium titanate composite material prepared by the invention is uniform, and the intergranular conductors improve the electron diffusion ability between the particles, and at the same time increase the conductivity of the lithium titanate material. In addition, the preparation method of the material is simple, convenient for scale-up preparation, and realizes 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] As a kind of clean energy, lithium-ion batteries have been widely used since the early 1990s due to their small size, high energy density, safety and environmental protection, and the negative electrode materials as their main components have also made great progress. . [0003] Lithium titanate batteries have the advantages of excellent low-temperature performance, high-power charge-discharge characteristics, high safety, and low life-cycle costs, and are especially suitable for green energy storage technologies that require long life, high safety, and low cost. Although lithium titanate battery has the above advantages, at the same time lithium titanate (Li 4 Ti 5 O 12 ) materials have low electronic and ionic c...

Claims

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Application Information

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Patent Type & Authority Patents(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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