US20160380304A1 - Solid electrolyte for all solid-state lithium-ion battery and manufacturing method therefor - Google Patents

Solid electrolyte for all solid-state lithium-ion battery and manufacturing method therefor Download PDF

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US20160380304A1
US20160380304A1 US14/902,488 US201414902488A US2016380304A1 US 20160380304 A1 US20160380304 A1 US 20160380304A1 US 201414902488 A US201414902488 A US 201414902488A US 2016380304 A1 US2016380304 A1 US 2016380304A1
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solid electrolyte
powder
heat treatment
hours
treatment temperature
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Ho Sung Kim
Tae Won Kim
Duck Rye Chang
Jong Ho Lee
Kyeong Wan Kim
Min Young Kim
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Korea Institute of Industrial Technology KITECH
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Definitions

  • a solid electrolyte for an all-solid-state lithium-ion battery is required to have an ion conductivity of about 10 ⁇ 3 S/cm at room temperature for practical use.
  • Solid electrolytes having ion conductivity in this level include sulfide solid electrolytes and oxide solid electrolytes, such as perovskite and NASICON.
  • oxide solid electrolytes such as perovskite and NASICON.
  • Studies on oxide solid electrolytes have been actively conducted since 2000. Initial ion conductivity of oxide solid electrolytes has been improved from 10 ⁇ 13 S/cm up to about 10 ⁇ 3 S/cm recently.
  • perovskite and NASICON oxide solid electrolytes are relatively excellent in ion conductivity and yield, but exhibit limited potential window characteristics, having limitations in application to next-generation medium and large-size all-solid-state lithium-ion batteries required to employ a high-energy-density anode material and a low-potential high-capacity cathode material.
  • powder of a solid electrolyte for a lithium-ion battery is formed through heat treatment to have a composition of Li x La y Zr z O 12 , where x is 6 to 9 moles, y is 2 to 4 moles, and z is 1 to 3 moles, and is manufactured using a characteristic that a predominating crystal structure is changed to a cubic structure or tetragonal structure depending on heat treatment temperature.
  • a garnet-structure oxide solid electrolyte (LixLayZrzO12) may be manufactured using co-precipitation.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a solid electrolyte according to the present invention.
  • FIG. 4 is a graph illustrating an XRD analysis result showing a cubic structure at 1200° C. according to Example 3.
  • FIG. 6 is a graph illustrating a result of measuring ion conductivity of a cubic structure at 1200° C.
  • FIG. 7 is a graph illustrating a result of measuring ion conductivity of a tetragonal structure at 900° C.
  • compositions of the solid electrolyte powders prepared by heat treatment temperature are identified through inductively coupled plasma (ICP) analysis, and structures and shapes of the synthesized materials are identified through thermal analysis with thermogravimetry analysis (TGA)/differential scanning calorimetry (DSC), X-ray diffraction (XRD) analysis and scanning electron microscope (SEM) analysis
  • ICP inductively coupled plasma
  • TGA thermogravimetry analysis
  • DSC differential scanning calorimetry
  • XRD X-ray diffraction
  • SEM scanning electron microscope
  • a crystal phase predominantly maintained was selected and subjected to XRD Rietveld analysis, thereby listing lattice constants and crystallite sizes of the synthesized powders by heat treatment temperature in Table 2.
  • a lattice constant of the cubic structure was maintained in a temperature range of 700 to 800° C.
  • lattice constant a tended to increase while lattice constant c tended to decrease, so that the crystal structure was finally changed drastically from the cubic structure to the tetragonal structure.
  • crystallite (monocrystal) size was increased by about 20 times from 266 ⁇ to 5625 ⁇ .
  • Example 3 illustrates a method of manufacturing a pellet molded product (sheet), in which 700° C. and 800° C. heat-treated powders exhibiting the cubic structure or tetragonal structure predominating depending on synthesis and heat treatment conditions for precursors were fully put into pellet molding molds, followed by molding into regular size and thickness and heat treatment at 1200° C. for 2 hours (sample #1), 5 hours (sample #2) and 10 hours (sample #3), thereby manufacturing calcinated pellet products. Also, 900° C. heat-treated powder exhibiting the tetragonal structure predominating was subjected to the same method to obtain molded pellets, followed by heat treatment at 900° C.

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US14/902,488 2013-07-04 2014-06-27 Solid electrolyte for all solid-state lithium-ion battery and manufacturing method therefor Abandoned US20160380304A1 (en)

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Cited By (7)

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US10818968B2 (en) * 2017-07-28 2020-10-27 Korea Institute Of Industrial Technology Method of preparing a gallium-doped LLZO solid electrolyte for an all-solid-state lithium secondary battery
US20210151793A1 (en) * 2018-08-03 2021-05-20 Kaneka Corporation Garnet-type composite metal oxide and method for producing same
US11094998B2 (en) * 2019-06-19 2021-08-17 GM Global Technology Operations LLC Ceramic-coated separators for lithium-containing electrochemical cells and methods of making the same
US11251463B2 (en) * 2016-11-18 2022-02-15 Korea Institute Of Industrial Technology Method for preparing a sintered solid electrolyte having high ionic conductivity for an all-solid-state battery
US11342581B2 (en) * 2019-07-19 2022-05-24 Daiichi Kigenso Kagaku Kogyo Co., Ltd. Ceramic powder material, method for producing ceramic powder material, and battery
US20230080488A1 (en) * 2021-09-02 2023-03-16 Xtc New Energy Materials(Xiamen) Co., Ltd. Ternary positive material of large monocrystal-like particles, method for preparing the same, and lithium-ion battery having the same
US12095026B2 (en) * 2017-11-09 2024-09-17 Research Institute Of Industrial Science & Technology All-solid-state battery, manufacturing method therefor, secondary battery comprising same and monolithic battery module comprising same

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JP6369281B2 (ja) * 2014-10-17 2018-08-08 東京電力ホールディングス株式会社 固体電解質材料の製造方法
KR101728434B1 (ko) 2015-09-18 2017-04-20 한국생산기술연구원 전고체 리튬이차전지용 고체전해질의 제조방법 및 그를 포함하는 전고체 리튬이차전지의 제조방법
KR101718880B1 (ko) * 2015-12-30 2017-03-23 주식회사 이아이지 리튬-란타늄-지르코늄계 고체 전해질의 제조 방법
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