High-conductivity solid electrolyte prepared by sol-gel method

A solid electrolyte, sol-gel technology, applied in the field of high-conductivity solid electrolytes, can solve the problems of large grain boundary resistance of solid electrolytes, difficult recycling of impurities, heat treatment temperature sensitivity, etc., and achieves low heat treatment temperature sensitivity, high density, The effect of low grain boundary resistance

Inactive Publication Date: 2020-03-17
GUIZHOU MEILING POWER SUPPLY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, oxide solid electrolytes are mainly prepared by co-precipitation method, sol-gel method, solvent method, microwave synthesis method, electrospinning method, high-temperature solid-phase method, etc., such as patent No. CN201810697845.9 discloses a A novel lithium ion conductive oxide solid electrolyte and a preparation method thereof, specifically weighing raw materials according to a designed stoichiometric ratio and performing wet ball milling and mixing; calcining the mixed raw materials step by step to obtain a solid electrolyte powder; The electrolyte powder is kept under a suitable pressure for 30-60 minutes, and then the green body is buried in the powder of the same composition, and the temperature is raised to 1100-1200°C at 1°C/min-2°C/min, and kept for 12h-24h , to prepare the required solid electrolyte, but the calcination temperature is too high, the energy consumption is high, and the impurities are difficult to recycle due to direct calcination; CN201710962086.X discloses a lithium halide-doped oxide solid electrolyte and its low-temperature sintering method , specifically a perovskite-type, NASICON-type, garnet-type electrolyte as a matrix, using a lithium halide solution

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  • High-conductivity solid electrolyte prepared by sol-gel method
  • High-conductivity solid electrolyte prepared by sol-gel method
  • High-conductivity solid electrolyte prepared by sol-gel method

Examples

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Example Embodiment

[0041] Example 1

[0042] A high-conductivity solid electrolyte prepared by the sol-gel method, using lithium nitrate as the dopant and lithium aluminum titanium phosphate (LATP) as the main material. The dopant is embedded in the lithium aluminum titanium phosphate (LATP) by the sol-gel method. ) In the skeleton, a NASICON structure is formed;

[0043] The preparation method of the high-conductivity solid electrolyte includes the following steps:

[0044] S1 preparation solution A: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 The stoichiometric ratio of tetrabutyl titanate was weighed, and ammonia was added and washed with suction for several times. Then tetrabutyl titanate was slowly added to 0.4mol / L citric acid aqueous solution, heated and magnetically stirred for 6 hours to form a clear liquid, namely Get solution A;

[0045] S2 preparation solution B: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 Weigh lithium acetate, ammonium dihydrogen phosphate, and citric acid according to th...

Example Embodiment

[0051] Example 2

[0052] A high-conductivity solid electrolyte with germanium oxide as the dopant and lithium titanium aluminum phosphate (LATP) as the main material. The dopant is embedded in the lithium aluminum titanium phosphate (LATP) framework by the sol-gel method to form NASICON Structure; structural formula after doping is Li 1.3 Al 0.3 Ti 1.6 Ge 0.1 (PO 4 ) 3 ;

[0053] The preparation method of the high-conductivity solid electrolyte includes the following steps:

[0054] S1 preparation solution A: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 The stoichiometric ratio of tetrabutyl titanate was weighed, and ammonia was added and washed with suction for several times. Then tetrabutyl titanate was slowly added to 0.4mol / L citric acid aqueous solution, heated and magnetically stirred for 6 hours to form a clear liquid, namely Get solution A;

[0055] S2 preparation solution B: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 Weigh lithium nitrate, ammonium dihydrogen phosphate, and...

Example Embodiment

[0061] Example 3

[0062] A high-conductivity solid electrolyte prepared by the sol-gel method, using tetraethyl orthosilicate as the dopant and lithium aluminum titanium phosphate (LATP) as the main material. The dopant is embedded in the titanium aluminum phosphate by the sol-gel method In the lithium (LATP) framework, a NASICON structure is formed; the structural formula after doping is Li 1.3 Al 0.3 Ti 1.6 Si 0.1 (PO 4 ) 3 ;

[0063] The preparation method of the high-conductivity solid electrolyte includes the following steps:

[0064] S1 preparation solution A: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 The stoichiometric ratio of tetrabutyl titanate was weighed, and ammonia was added and washed with suction for several times. Then tetrabutyl titanate was slowly added to 0.4mol / L citric acid aqueous solution, heated and magnetically stirred for 6 hours to form a clear liquid, namely Get solution A;

[0065] S2 preparation solution B: according to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3...

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Abstract

The invention relates to the technical field of solid electrolyte, and in particular, relates to a high-conductivity solid electrolyte prepared by a sol-gel method. Any one or a composition of more oflithium nitrate, germanium oxide and tetraethoxysilane is used as a doping agent, lithium titanium aluminum phosphate is used as a main material, the doping agent is embedded into the lithium titanium aluminum phosphate framework by the sol-gel method, and an NASICON structure is formed; the solid electrolyte disclosed by the invention is small in grain boundary impedance, high in ionic conductivity, low in sensitivity to heat treatment temperature and suitable for industrial production, and integrates the characteristics of low synthesis temperature, low energy consumption, high product purity, small particle size and high density of traditional sol-gel; citric acid and ethylene glycol are adopted as auxiliary agents, environmental pollution is prevented, the temperature and the stirringrate are reasonably controlled, and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of solid electrolytes, in particular to a high-conductivity solid electrolyte prepared by a sol-gel method. Background technique [0002] With the development of industrial society, the increase in energy consumption and the depletion of non-renewable resources, people's demand for new energy is becoming more and more urgent, and the requirements for energy storage technology are becoming more and more stringent. Lithium-ion batteries are considered to have very broad development prospects in energy storage due to their high energy density and long service life. [0003] At present, commercial lithium-ion batteries use organic electrolytes. Because they are flammable and easy to leak, there are great safety hazards in large-scale use. In addition, the existence of electrolytes makes the battery structure complicated, making it difficult to miniaturize the battery. develop. Solid-state batteries have high t...

Claims

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Application Information

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IPC IPC(8): C04B35/447C04B35/624C04B35/622
CPCC04B35/447C04B35/622C04B35/624C04B2235/3203C04B2235/3217C04B2235/3232C04B2235/3287C04B2235/3418C04B2235/6562
Inventor 杨程响石斌王庆杰陈晓涛陈铤王振吴宁宁张红梅张亮吴启兵
Owner GUIZHOU MEILING POWER SUPPLY CO LTD
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