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Chloride solid electrolyte with stable conductivity and preparation method thereof

A solid electrolyte and chloride technology, applied in the field of lithium-ion batteries, can solve the problems of reduced conductivity, sensitivity, and inability to accurately control the ratio of raw materials to achieve the effect of low sensitivity

Inactive Publication Date: 2021-06-08
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the current chloride solid-state electrolytes have strict requirements on the proportion of raw materials, and inaccurate control of the proportion of raw materials will lead to a significant decrease in conductivity, such as Li 3 ScCl 6 The conductivity of this system is very sensitive to the ratio of raw materials. When the ratio of raw materials deviates greatly, the conductivity will even decrease by an order of magnitude (J.Am.Chem.Soc.2020,142,15,7012– 7022.), so for the reported chloride solid electrolytes, precise control of the ratio of raw materials is crucial to ensure their high conductivity
However, large-scale production in the industry usually cannot guarantee precise control of the ratio of raw materials, so it is difficult for different batches of solid electrolytes to maintain good consistency in performance.

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  • Chloride solid electrolyte with stable conductivity and preparation method thereof
  • Chloride solid electrolyte with stable conductivity and preparation method thereof
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preparation example Construction

[0031] The present invention also provides a method for preparing the above-mentioned chloride solid electrolyte with stable conductivity, comprising: S1) mixing lithium chloride and yttrium chloride according to the molar ratio x:(6-x) / 3 for ball milling, A mixed powder is obtained; wherein, 2<x<3; S2) annealing the mixed powder in a protective atmosphere to obtain a chloride solid electrolyte.

[0032] Among them, the present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0033] Lithium chloride and yttrium chloride are mixed and carried out ball milling according to the ratio of molar ratio x:(6-x) / 3, obtain mixed powder; Said x is the same as above, no longer go into details here; The method of described mixing is preferably Grinding; the grinding is preferably carried out in an agate mortar; the mixing time is preferably 5 to 20 minutes, more preferably 10 to 15 minutes; in the examples provided by the prese...

Embodiment 1

[0039] According to the chemical formula Li 2.9 Y 1.03 Cl 6 Weigh a certain amount of lithium chloride and yttrium chloride powder in an argon atmosphere glove box, then transfer to an agate mortar and grind and mix for 10 minutes, then weigh the corresponding mass according to the ball-to-material ratio of 25:1 Put the tungsten carbide balls into the tungsten carbide ball milling tank, then put the uniformly mixed reaction raw materials into the ball milling tank with tungsten carbide balls of corresponding quality, seal and transfer to the high-energy ball mill, at a speed of 500 rpm Ball milled for 40 hours to obtain Li 2.9 Y 1.03 Cl 6 Electrolyte powder. The obtained electrolyte powder was packaged in a quartz tube filled with an argon atmosphere, then transferred to a muffle furnace, heated to 450 °C at a heating rate of 5 °C / min, and annealed at a temperature of 5 hours to obtain the final chloride solid electrolyte Li 2.9 Y 1.03 Cl 6 .

[0040] Under 500MPa, th...

Embodiment 2

[0045] According to the chemical formula Li 2.8 Y 1.07 Cl 6 Weigh a certain amount of lithium chloride and yttrium chloride powder in an argon atmosphere glove box, then transfer to an agate mortar and grind and mix for 10 minutes, then weigh the corresponding mass according to the ball-to-material ratio of 25:1 Put the tungsten carbide balls into the tungsten carbide ball milling tank, then put the uniformly mixed reaction raw materials into the ball milling tank with tungsten carbide balls of corresponding quality, seal and transfer to the high-energy ball mill, at a speed of 500 rpm Ball milled for 40 hours to obtain Li 2.8 Y 1.07 Cl 6 Electrolyte powder. The obtained electrolyte powder was packaged in a quartz tube filled with an argon atmosphere, then transferred to a muffle furnace, heated to 450 °C at a heating rate of 5 °C / min, and annealed at a temperature of 5 hours to obtain the final chloride solid electrolyte Li 2.8 Y 1.07 Cl 6 .

[0046] Under 500MPa, th...

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Abstract

The invention provides a chloride solid electrolyte with stable conductivity. The molecular formula of the chloride solid electrolyte is LixY(6-x) / 3Cl6, wherein, x is greater than 2 and less than 3. Compared with the prior art, the ionic conductivity of the chloride solid electrolyte provided by the invention in the interval that x is greater than 2 and less than 3 can be stabilized at the order of magnitude of 10<-4>S.cm<-1>, which indicates that the conductivity has high tolerance to the raw material ratio deviation, and the requirements of industrial large-scale production scenes can be met.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a chloride solid electrolyte with stable conductivity and a preparation method thereof. Background technique [0002] By replacing the flammable and leaky organic liquid electrolyte with a non-flammable solid electrolyte, the all-solid-state lithium battery can not only greatly alleviate the safety problem of lithium-ion batteries, but also is expected to further increase the energy density. [0003] In solid electrolytes, Li 3 YCl 6 Chloride solid-state electrolytes such as (Adv. Mater. 2018, 30, 1803075) have recently received extensive attention. Most chloride solid-state electrolytes simultaneously possess high Li-ion conductivity, good deformability, and a wide electrochemical stability window, properties that cannot be simultaneously possessed by existing oxide and sulfide electrolytes. Moreover, the cations in most chloride solid electrolytes are in the hi...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525C01F17/36
CPCH01M10/0562H01M10/0525C01F17/36H01M2300/008C01P2002/72C01P2006/40Y02E60/10
Inventor 马骋段超民
Owner UNIV OF SCI & TECH OF CHINA