Li-ion conductive oxide ceramic material with garnet type crystal structure or crystal structure similar to garnet type

An oxide ceramic, garnet-type technology, applied in electrochemical generators, electrical components, circuits, etc., can solve the problem that all-solid-state lithium-ion secondary batteries are not practical.

Active Publication Date: 2016-09-28
TDK CORPARATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, high-capacity all-solid-state lithium-ion secondary batteries have not yet been put into practical use worldwide.

Method used

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  • Li-ion conductive oxide ceramic material with garnet type crystal structure or crystal structure similar to garnet type
  • Li-ion conductive oxide ceramic material with garnet type crystal structure or crystal structure similar to garnet type

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Experimental program
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Effect test

Embodiment 1～ Embodiment 10

[0087] In order to verify the effect of the present embodiment, as an example of a lithium ion conductive oxide ceramic material having a garnet type or a garnet-like crystal structure, proposed are respectively substituted Li 7.10 La 3.00 (Zr 1.90 A 0.10 )O 12 (A=Y, Nd, Gd, Ho, Yb) composition (Example 1-Example 5), further adding 1.0wt% Al to each composition 2 o 3 The composition of (embodiment 6-embodiment 10). Li was used in the starting material 2 CO 3 、La(OH) 3 , ZrO 2 , Y 2 o 3 、Nd 2 o 3 、Gd 2 o 3 、Ho 2 o 3 , Yb 2 o 3 and Al 2 o 3 . First, starting materials were weighed so as to have a stoichiometric ratio, and mixed and pulverized in ethanol with a ball mill (120 rpm / zirconia ball) for 16 hours. After the mixed powder of the starting material was separated from the balls and ethanol, it was calcined in an alumina crucible at 900° C. in the air atmosphere for 5 hours. Then, for mixing, the calcined powder was treated with a ball mill (120 rpm / zi...

Embodiment 11～ Embodiment 26

[0089] In addition, it is proposed to substitute Li for Zr with A, respectively 7.35 La 3.00 (Zr 1.65 A 0.35 )O 12 , (A=Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) composition (Example 11-18) and further added 1.0wt% Al to each composition 2 o 3 The composition of (embodiment 19-embodiment 26). The starting material used Li 2 CO 3 、La(OH) 3 , ZrO 2 、Gd 2 o 3 , Tb 2 o 3 、Dy 2 o 3 、Ho 2 o 3 、Er 2 o 3 、Tm 2 o 3 , Yb 2 o 3 、Lu 2 o 3 and Al 2 o 3. First, the starting materials were weighed until the stoichiometric ratio was reached, and mixed and pulverized in ethanol with a ball mill (120 rpm / zirconia ball) for 16 hours. After the mixed powder of the starting material was separated from the balls and ethanol, it was calcined in an alumina crucible at 900° C. in the air atmosphere for 5 hours. Then, for mixing, the calcined powder was treated with a ball mill (120 rpm / zirconia ball) in ethanol for 16 hours. After the pulverized powder was separated from the balls ...

Embodiment 27～ Embodiment 29

[0091] In addition, to Li 7.05 La 3.00 (Zr 1.95 Gd 0.05 )O 12 , Li 7.25 La 3.00 (Zr 1.75 Gd 0.25 )O 12 , Li 7.50 La 3.00 (Zr 1.50 Gd 0.50 )O 12 Add 1.0wt% Al respectively 2 o 3 . The initial raw material uses Li 2 CO 3 、La(OH) 3 , ZrO 2 、Gd 2 o 3 and Al 2 o 3 . First, the starting materials were weighed so that the stoichiometric ratio was obtained, and mixed and pulverized in ethanol with a ball mill (120 rpm / zirconia ball) for 16 hours. After the mixed powder of the starting material was separated from the balls and ethanol, it was calcined in an alumina crucible at 900° C. in an air atmosphere for 5 hours. Then, for mixing, the calcined powder was treated with a ball mill (120 rpm / zirconia ball) in ethanol for 16 hours. After the pulverized powder was separated from the balls and ethanol and dried, the powder before main sintering was obtained. Next, an organic binder is added to these pre-sintered powders to produce pellets. The pellets were mol...

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Abstract

The invention provides a Li-ion conductive oxide ceramic material with a garnet type crystal structure or a crystal structure similar to a garnet type, and internal resistance component in a crystalline grain has high contribution on ionic conductance. The Li-ion conductive oxide ceramic material with a garnet type crystal structure or a crystal structure similar to a garnet type contains Li, La, Zr, and O, and also contains more than one element selected from rare earth elements.

Description

technical field [0001] The present invention relates to a lithium ion conductive oxide ceramic material having a garnet-type or garnet-like crystal structure. Background technique [0002] Compared with lithium secondary batteries using non-aqueous electrolytes, all-solid-state lithium ion secondary batteries use ceramic materials in which electrolytes are sintered, and therefore have higher thermal stability. However, high-capacity all-solid-state lithium-ion secondary batteries have not yet been put into practical use worldwide. One of the reasons is the problem of the solid electrolyte itself. The main characteristics required of a solid electrolyte include three characteristics of high ion conductivity (conductivity), excellent chemical stability, and a large potential window. Among these properties, garnet-type oxide ceramic materials are excellent candidates for solid electrolytes due to their excellent chemical stability and large potential window (see, for example,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562C04B35/48C04B35/50H01M10/0525
CPCC04B35/48C04B35/50H01M10/0525H01M10/0562Y02E60/10
Inventor 塚田岳夫田中祯一角田宏郁益子泰辅
Owner TDK CORPARATION
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