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Divalent alkaline-earth metal and tantalum co-doped Li7La3Zr2O12 solid electrolyte material and preparation method

A technology of solid electrolyte and divalent alkali, which is applied in the field of new materials and electrochemistry, can solve problems such as low conductivity, greenhouse effect, and difficulty in densification, so as to improve conductivity, promote phase formation and sintering densification, and reduce migration and activation Can effect

Inactive Publication Date: 2018-06-12
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

Fossil fuels are currently the most widely used energy sources. However, the large-scale use of fossil fuels has brought about major problems: on the one hand, they take tens of millions of years to form in the earth's crust, while their reserves are depleted very quickly On the other hand, the use of fossil fuels will inevitably bring about problems such as environmental pollution and the greenhouse effect
First, the conductivity of traditional liquid electrolytes at room temperature is 10 -2 On the order of S / cm, the conductivity of the currently reported garnet-type solid electrolyte at room temperature is much lower
Second, the heat treatment temperature in the pure-phase preparation process of garnet-type solid electrolyte is high, the cost is high, and the preparation process is complicated
Third, in its practical application, high-temperature sintering and compaction are required, and lithium is easy to volatilize in the form of lithium oxide at high temperatures, so it is difficult to densify under the premise of maintaining a pure phase

Method used

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  • Divalent alkaline-earth metal and tantalum co-doped Li7La3Zr2O12 solid electrolyte material and preparation method
  • Divalent alkaline-earth metal and tantalum co-doped Li7La3Zr2O12 solid electrolyte material and preparation method
  • Divalent alkaline-earth metal and tantalum co-doped Li7La3Zr2O12 solid electrolyte material and preparation method

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specific Embodiment approach

[0026] The embodiment of the present invention provides a divalent alkaline earth metal and tantalum co-doped Li 7 La 3 Zr 2 o 12 Solid electrolyte material, the specific implementation method is as follows:

[0027] (1) Raw material mixing

[0028] The lithium source compound, the lanthanum source compound, the divalent alkaline earth metal compound, the zirconium source compound and the tantalum source compound are uniformly mixed according to the molar ratio of each element being 7-y+x:3-x:x:2-y:y. Wherein, 0<y<2, 0<x<y, in order to make up for the volatilization loss of the lithium source during the sintering process, the lithium source is in excess of 5% to 20%, preferably 10%. The mixing method is ball milling, and the ball milling medium can be organic solvents such as ethanol and isopropanol, among which isopropanol is preferred, and the spheres can be agate balls, zirconium balls, etc., among which zirconium balls are preferred. After ball milling, it was taken o...

Embodiment 1

[0036] Embodiment 1: prepare Li 6.5 La 2.9 Sr 0.1 Zr 1.4 Ta 0.6 o 12 Co-doped solid electrolyte materials

[0037] Weigh 1.321 grams of lithium carbonate, 2.362 grams of lanthanum oxide, 0.074 grams of strontium carbonate, 0.863 grams of zirconium oxide, and 0.663 grams of tantalum oxide according to the molar ratio of Li, La, Sr, Zr, and Ta of 6.5:2.9:0.1:1.4:0.6 , wherein the excess of lithium carbonate is 10%. Then ball mill in isopropanol medium for 12 hours, the speed of ball milling is 300 rpm, and dry treatment is carried out after the end. After heat treatment at 850°C for 12h, it was compressed into a tablet under a pressure of 300MPa, and then treated at 1100°C for 3h to obtain the Li 6.5 La 2.9 Sr 0.1 Zr 1.4 Ta 0.6 o 12 Co-doped solid electrolyte materials. The material has a lithium ion migration activation energy of 0.456eV, a total resistance of 139.8Ω at 25°C, a radius of 0.6175cm, a thickness of 0.05cm, and a conductivity of 2.99×10 -4 S / cm, the t...

Embodiment 2

[0038] Embodiment 2: prepare Li 6.6 La 2.6 Sr 0.4 Zr 1.2 Ta 0.8 o 12 Co-doped solid electrolyte materials

[0039] Weigh 1.341 grams of lithium carbonate, 2.118 grams of lanthanum oxide, 0.295 grams of strontium carbonate, 0.739 grams of zirconium oxide, and 0.884 grams of tantalum oxide according to the molar ratio of Li, La, Sr, Zr, and Ta of 6.6:2.6:0.4:1.2:0.8 , wherein the excess of lithium carbonate is 10%. Then ball mill in isopropanol medium for 12 hours, the speed of ball milling is 300 rpm, and dry treatment is carried out after the end. After heat treatment at 850°C for 12h, it was compressed into a tablet under a pressure of 300MPa, and then treated at 1100°C for 3h to obtain the Li 6.6 La 2.6 Sr 0.4 Zr 1.2 Ta 0.8 o 12 Co-doped solid electrolyte materials. The material has a lithium ion migration activation energy of 0.379eV, a total resistance of 155.3Ω at 25°C, a radius of 0.6165cm, a thickness of 0.06cm, and a conductivity of 3.21×10 -4 S / cm, indic...

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Abstract

The invention relates to a divalent alkaline-earth metal and tantalum co-doped Li7La3Zr2O12 electrolyte material and a preparation method, which belong to the field of electrolyte materials. A stoichiometric equation is Li7-y+xLa3-xAxZr2-yTayO12, wherein A is one of doping elements Sr and Ba, y is greater than 0 and less than 2, and x is greater than 0 and less than y. The purpose of doping Ta ona Zr site is to stabilize a cubic phase of the material, so that the ion electric conductivity of the material can be increased; and a purpose of doping a divalent alkaline-earth metal on an La site is to increase a carrier concentration. A crystal structure is adjusted by utilizing the difference of an element radius and bond valence, a transport channel which is more suitable for transferring lithium ions is formed, the migration activation energy of the lithium ions can be reduced, the ion electric conductivity is increased, the phase forming temperature is reduced, the sintering is promoted, and the compactness of the material is increased. By virtue of co-doping, the Li7La3Zr2o12 solid electrolyte material with a stable cubic phase structure is obtained, and the material also has goodsintering performance, low lithium ion migration activation energy, high ion electric conductivity, and important application value.

Description

technical field [0001] The invention belongs to the field of new materials and electrochemistry, in particular to a lithium ion conducting Li 7 La 3 Zr 2 o 12 Solid electrolyte material and preparation method thereof. technical background [0002] The current human energy system is mainly composed of fossil fuels, nuclear energy and renewable energy. Fossil fuels are currently the most widely used energy sources. However, the large-scale use of fossil fuels has brought about major problems: on the one hand, they take tens of millions of years to form in the earth's crust, while their reserves are depleted very quickly ; On the other hand, the use of fossil fuels will inevitably bring about problems such as environmental pollution and the greenhouse effect. Water energy, wind energy, solar energy, geothermal energy, and tidal energy are the fastest-growing green and environmentally friendly renewable energy sources since the 21st century. However, the instability and int...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/052
CPCH01M10/052H01M10/0562H01M2300/0071Y02E60/10
Inventor 赵海雷徐涛张赛赛
Owner UNIV OF SCI & TECH BEIJING
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