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Production method of TiN-S and TiO2-S composite material with hollow nanosphere structure

A technology of hollow nano and composite materials, which is applied in the direction of structural parts, electrical components, battery electrodes, etc., can solve the problems of capacity attenuation, limit the initial capacity value of the battery, and poor conductivity, so as to increase the initial specific capacity, inhibit dissolution, and improve The effect of conductivity

Inactive Publication Date: 2020-04-14
XIJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The research on lithium-sulfur batteries has been going on for decades, but there are few reports on practical applications, mainly due to the fact that the sulfur element and its reduction products (Li 2 S 2 , Li 2 S) poor conductivity, which limits the initial capacity of the battery; polysulfides formed during charging and discharging are easily soluble in the organic electrolyte and diffuse to the surface of the negative electrode (lithium metal), reacting to produce a shuttle effect, resulting in the discharge and charging process. Severe attenuation

Method used

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  • Production method of TiN-S and TiO2-S composite material with hollow nanosphere structure
  • Production method of TiN-S and TiO2-S composite material with hollow nanosphere structure
  • Production method of TiN-S and TiO2-S composite material with hollow nanosphere structure

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Effect test

Embodiment 1

[0029] Embodiment 1, the preparation method of the TiN-S composite material of hollow nanosphere structure, comprises the following steps:

[0030] (1) Dissolve 2g of HDA in 100ml of KCl solution (0.1m / L) and stir for 20min, then add 7-10ml of titanium isopropyl (TIP) dropwise under electromagnetic stirring;

[0031] (2) Then add 0.7ml of ammonia to the mixture prepared in step (1), and incubate at 160° C. for 20 to 30 hours, and wash the precipitated product with ethanol;

[0032] (3) Transfer the precipitated product washed in step (2) to a muffle furnace and keep it at 580°C for 3 hours to obtain TiO 2 hollow nanospheres;

[0033] (4) in NH 3 Under the atmosphere, the TiO prepared in step (3) 2 Hollow nanospheres were further incubated at 900°C for 2 hours to prepare TiN composites;

[0034] (5) Mix the TiN composite material prepared in step (4) with sulfur at a mass ratio of 1:3, then transfer it to a tube furnace, and heat the mixture to 155 °C for 12 h under a nitro...

Embodiment 2

[0035] Embodiment 2, the preparation method of the TiN-S composite material of hollow nanosphere structure, comprises the following steps:

[0036] (1) Dissolve 3g of HDA in 100ml of KCl solution (0.3m / L) and stir for 40min, then add 10ml of titanium isopropyl (TIP) dropwise under electromagnetic stirring;

[0037] (2) Then add 0.9ml of ammonia to the mixture prepared in step (1), and incubate at 160°C for 30h, and wash the precipitated product with ethanol;

[0038] (3) Transfer the precipitated product washed in step (2) to a muffle furnace and keep it at 580°C for 5 hours to obtain TiO 2 hollow nanospheres;

[0039] (4) in NH 3 Under the atmosphere, the TiO prepared in step (3) 2 Hollow nanospheres were further incubated at 900°C for 4 hours to prepare TiN composites;

[0040] (5) Mix the TiN composite material prepared in step (4) with sulfur at a mass ratio of 1:4, then transfer it to a tube furnace, heat the mixture to 155°C for 14h under a nitrogen atmosphere, and p...

Embodiment 3

[0041] Embodiment 3, the preparation method of the TiN-S composite material of hollow nanosphere structure, comprises the following steps:

[0042] (1) Dissolve 3g of HDA in 100ml of KCl solution (0.2m / L) and stir for 30min, then add 8ml of titanium isopropyl (TIP) dropwise under electromagnetic stirring;

[0043] (2) Then add 0.8ml of ammonia to the mixture prepared in step (1), and incubate at 160°C for 15h, and wash the precipitated product with ethanol;

[0044] (3) Transfer the precipitated product washed in step (2) to a muffle furnace and keep it at 580°C for 4 hours to obtain TiO 2 hollow nanospheres;

[0045] (4) in NH 3 Under the atmosphere, the TiO prepared in step (3) 2 Hollow nanospheres were further incubated at 900°C for 3 hours to prepare TiN composites;

[0046] (5) Mix the TiN composite material prepared in step (4) with sulfur at a mass ratio of 1:3, then transfer it to a tube furnace, and heat the mixture to 155 °C for 13 h under a nitrogen atmosphere t...

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Abstract

The invention discloses a preparation method of a TiN-S and TiO2-S composite material with a hollow nanosphere structure. The production method comprises the following steps: dissolving HDA in a KCl solution, stirring the materials, dropwise adding isopropyl titanium under the action of electromagnetic stirring, adding ammonia, carrying out heat preservation at 160 DEG C for 20-30 hours, washing aprecipitate product with ethanol, transferring the precipitate product into a muffle furnace, and carrying out heat preservation at 580 DEG C for 3-5 hours to obtain TiO2 hollow nanospheres; under the NH3 atmosphere, carrying out heat preservation on the TiO2 hollow nanospheres for 2-4 hours at the temperature of 900 DEG C, and producing a TiN composite material; mixing a TiN composite material or TiO2 hollow nanospheres with sulfur; transferring the material into a tubular furnace, heating the mixture to 155 DEG C in a nitrogen atmosphere, and keeping the temperature for 12-14 hours to produce the TiN-S composite material or the TiO2-S composite material. The TiN-S composite material or the TiO2-S composite materialinhibits the dissolution of polysulfide while improving the conductivityof the electrolyte.

Description

technical field [0001] The invention belongs to the technical field of lithium-sulfur batteries, in particular to TiN-S and TiO with hollow nanosphere structures 2 -S Composite material preparation method. Background technique [0002] In recent years, lithium-ion batteries, including lithium-sulfur batteries, lithium-air batteries, and sodium metal batteries, have been widely used in electric vehicles and mobile electronic devices due to their excellent electrochemical performance. Among these energy storage systems, lithium-sulfur batteries have become a research hotspot around the world due to their high specific capacity (1675mAh / g) and high energy density (2600wh / kg), and the active material sulfur is non-polluting to the environment and low in cost. [0003] The research on lithium-sulfur batteries has been going on for decades, but there are few reports on practical applications, mainly due to the fact that the sulfur element and its reduction products (Li 2 S 2 , ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/052
CPCH01M4/362H01M4/38H01M4/626H01M10/052Y02E60/10
Inventor 刘守法罗杰乔勋
Owner XIJING UNIV
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