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Inorganic nano particle filler for solid state electrolyte and preparation method of inorganic nano particle filler

An inorganic nanoparticle, solid electrolyte technology, applied in solid electrolyte, non-aqueous electrolyte, inorganic pigment treatment and other directions, can solve the problems of inability to meet large-scale industrial production, inability to uniformly disperse, harsh preparation process, etc., and achieve a simple and easy preparation process. performance, ensure conductivity, and improve flexibility

Active Publication Date: 2017-09-05
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Doping aluminum oxide nanoparticles in polyethylene oxide matrix is ​​the earliest report on composite electrolyte materials (Solid State Ionics, 1982, 7, 75-79), but unmodified nanoparticles will inevitably agglomerate, resulting in the inability to disperse evenly in the electrolyte system
Then, nanoparticles modified by ionic liquids (Adv. Mater., 2012, 24, 4430-4435) or sulfonic acid groups (Adv. Funct. Mater., 2013, 23, 1019-1027) were also used as fillers for Although the dispersion of nanoparticles is improved by constructing composite electrolyte materials, the raw materials used in the above methods are all expensive experimental grade reagents, and the preparation process is relatively harsh, which cannot meet the needs of large-scale industrial production.

Method used

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  • Inorganic nano particle filler for solid state electrolyte and preparation method of inorganic nano particle filler
  • Inorganic nano particle filler for solid state electrolyte and preparation method of inorganic nano particle filler

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preparation example Construction

[0032] The preparation method may specifically include the following steps:

[0033] (1) Place the inorganic nanoparticles in an alkaline aqueous solution (such as sodium hydroxide aqueous solution) for activation treatment at 60-90°C for 2-24 hours, the ratio of the inorganic nanoparticles to the alkaline aqueous solution is 1g / 100mL-1g / 2mL, Then cool to room temperature, wash repeatedly with deionized water, and dry to obtain inorganic nanoparticles grafted with hydroxyl groups on the surface; the pH value of the alkaline aqueous solution can be 9-12;

[0034] (2) Disperse the surface hydroxyl-rich inorganic nanoparticles obtained in step (1) in deionized water at a ratio of 1g / 10mL to 1g / 2mL. After ultrasonic dispersion at room temperature for 10 to 40 minutes, add dissolved The organic solution of mercaptopropyltrimethoxysilane (that is, mercaptopropyltrimethoxysilane coupling agent), the mass ratio of inorganic nanoparticles to silane coupling agent is 10 / 1~1 / 10, and the ...

Embodiment 1

[0044] The ionic bond modified inorganic nano particle filler is specifically the amino-terminated polyether ( M-600) obtained through sulfonic acid-amino ionic bonds, and the mass ratio of the two is 10 / 1.

[0045] The specific preparation method is:

[0046] Disperse 1 g of silica particles with an average particle size of 10 nm in 100 mL of aqueous sodium hydroxide solution with a concentration of 0.1 mol / L, oscillate ultrasonically for 30 min, then heat and reflux at 60°C for 2 h, filter with suction, wash with deionized water several times, and dry to obtain Surface activation of silica nanoparticles with a large number of hydroxyl groups. Disperse 50 g of silica nanoparticles modified with hydroxyl groups in 100 mL of deionized water, vibrate ultrasonically for 10 min, and then add dropwise 5 mL of acetone solution in which 5 g of mercaptopropyltrimethoxysilane is dissolved. Heat to reflux at 60°C for 12 hours, wash with acetone several times after suction filtration,...

Embodiment 2

[0049] Ionic bond modified inorganic nanoparticle filler, specifically the amino-terminated polyether ( M-1000) obtained through sulfonic acid-amino ionic bonds, the mass ratio of the two is 5 / 1.

[0050] The specific preparation method is:

[0051] Disperse 20g of silica particles with an average particle size of 100nm in 100mL of 2mol / L sodium hydroxide aqueous solution, oscillate ultrasonically for 30min, then heat and reflux at 80°C for 12h, wash with deionized water several times after suction filtration, and dry to obtain the surface Activates silica nanoparticles with a large number of hydroxyl groups. Disperse 20 g of silica nanoparticles modified with hydroxyl groups in 100 mL of deionized water, vibrate ultrasonically for 20 min, and then add dropwise 4 mL of methanol solution in which 4 g of mercaptopropyltrimethoxysilane is dissolved. Heat to reflux at 80°C for 24 hours, wash with methanol several times after suction filtration, and dry to obtain silica nanopart...

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Abstract

The invention discloses an inorganic nano particle filler for a solid state electrolyte and a preparation method of the inorganic nano particle filler. The inorganic nano particle filler for the solid state electrolyte is mainly formed by linking sulfonic acid group-modified inorganic nano particles and amino-terminated polyether by virtue of sulfonic acid-amino ionic bonds; and the mass ratio of the sulfonic acid group-modified inorganic nano particles to the amino-terminated polyether is 10 / 1-1 / 10. By adjusting the key components and shell components of the filler as well as the proportion between the key components and the shell components and improving the integrated process flow design and parameter conditions of each reaction step of the preparation method, the obtained inorganic nano particle filler for the solid state electrolyte has the advantages that on the one hand the surface of the filler is grafted with charges of the same polarity, and the mutual repulsion effect of the charges ensures the uniform dispersion of nano particles in the system; and on the other hand, the uniformly distributed filler can effectively inhibit the growth of polymer crystals so as to improve the ionic conductivity of the electrolyte.

Description

technical field [0001] The invention belongs to the field of lithium-ion battery electrolytes, and more specifically relates to an inorganic nanoparticle filler for solid electrolytes and a preparation method thereof. Background technique [0002] In recent years, especially in the autumn and winter seasons, the severe smog that has almost spread across the central and eastern regions of my country and Urumqi in Xinjiang has once again aroused people's attention to the current cruel environmental status, and the exhaust gas emitted by vehicles powered by traditional fossil energy is the cause of this One of the chief culprits of environmental problems, which makes it extremely urgent to develop electric vehicles powered by clean and efficient secondary batteries. Since secondary batteries will directly affect the performance of electric vehicles, lithium-ion batteries have attracted widespread attention due to their high energy density and long cycle life. However, because m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/056C09C1/30C09C1/36C09C1/40C09C3/00C09C3/08C09C3/10
CPCC09C1/309C09C1/3692C09C1/407C09C3/006C09C3/08C09C3/10H01M10/056H01M2300/0065Y02E60/10Y02P20/10
Inventor 薛志刚胡骥解孝林周兴平郭梦可黄路周波
Owner HUAZHONG UNIV OF SCI & TECH
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