JP4532128B2 - 固体電解質、その製造方法及びそれを採用した電池 - Google Patents
固体電解質、その製造方法及びそれを採用した電池 Download PDFInfo
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- JP4532128B2 JP4532128B2 JP2004024681A JP2004024681A JP4532128B2 JP 4532128 B2 JP4532128 B2 JP 4532128B2 JP 2004024681 A JP2004024681 A JP 2004024681A JP 2004024681 A JP2004024681 A JP 2004024681A JP 4532128 B2 JP4532128 B2 JP 4532128B2
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- 239000007784 solid electrolyte Substances 0.000 title claims description 74
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000010409 thin film Substances 0.000 claims description 33
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 31
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 27
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 22
- 239000000155 melt Substances 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 18
- 229910052744 lithium Inorganic materials 0.000 claims description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 description 39
- 150000002500 ions Chemical class 0.000 description 21
- 229910001416 lithium ion Inorganic materials 0.000 description 14
- 229910003002 lithium salt Inorganic materials 0.000 description 12
- 159000000002 lithium salts Chemical class 0.000 description 12
- 239000012071 phase Substances 0.000 description 12
- 239000003607 modifier Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- 230000001965 increasing effect Effects 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910012305 LiPON Inorganic materials 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000006183 anode active material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005191 phase separation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- -1 SO 4 Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 150000001450 anions Chemical group 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000006182 cathode active material Substances 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000001989 lithium alloy Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 239000002227 LISICON Substances 0.000 description 1
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 229910008572 Li2O—B2O3-SiO2 Inorganic materials 0.000 description 1
- 229910008585 Li2O—B2O3—SiO2 Inorganic materials 0.000 description 1
- 229910012050 Li4SiO4-Li3PO4 Inorganic materials 0.000 description 1
- 229910012069 Li4SiO4—Li3PO4 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- CJYZTOPVWURGAI-UHFFFAOYSA-N lithium;manganese;manganese(3+);oxygen(2-) Chemical compound [Li+].[O-2].[O-2].[O-2].[O-2].[Mn].[Mn+3] CJYZTOPVWURGAI-UHFFFAOYSA-N 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/04—Construction or manufacture in general
- H01M10/0436—Small-sized flat cells or batteries for portable equipment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Secondary Cells (AREA)
- Conductive Materials (AREA)
- Glass Compositions (AREA)
Description
Li2Oの前駆体として常温で安定したLi2CO3とB2O3及びTiO2を下記の表1のガラス組成によって称量した後、エタノールを使用して20時間ボールミリングした。その後、加熱板で攪拌しながら乾燥した。
原料物質としてTiO2の代りにV2O5を使用したことを除いては実施例1と同じ方法でガラス質固体電解質を製造した。この時の組成によるガラス質固体電解質のイオン伝導度変化を表2に示した。
原料物質としてTiO2の代りにWO3を使用したことを除いては実施例1と同じ方法でガラス質固体電解質を製造した。この時の組成によるガラス質固体電解質のイオン伝導度変化を表3に示した。
固体電解質のイオン伝導度をさらに向上させるために実施例3、実施例7及び実施例9の組成にリチウム塩としてLi2SO4を追加で添加した。すなわち、Li2O/B2O3/TiO2(50/47/3)、Li2O/B2O3/V2O5(47/50/3)及びLi2O/B2O3/WO3(47/50/3)それぞれの組成物100モル%に対してリチウム塩であるLi2SO4を5モル%及び15モル%添加して実施例1と同じ方法でガラス質固体電解質を製造した。Li2SO4添加によるイオン伝導度の変化を図3Aないし図3Cに示した。図3AはLi2O/B2O3/TiO2(50/47/3)、図3BはLi2O/B2O3/V2O5(47/50B2/3)及び図3CはLi2O/B2O3/WO3(47/50/3)に対するLi2SO4追加量によるイオン伝導度の変化を示したものである。
12 カソード、
13 アノード、
14 固体電解質、
15 保護層。
Claims (9)
- aは0.45ないし0.52であり、bは0.45ないし0.52であり、cは0.03ないし0.04であり、dは0.001ないし0.15であることを特徴とする請求項1に記載の固体電解質。
- (a)Li2O前駆体化合物;B2O3;並びにTiO2 、WO3及びTa2O5よりなる群から選択されたいずれか1つ以上の化合物を混合し、ミリングする段階と、
(b)前記Li2O前駆体化合物がLi2Oに熱分解されるように前記生成された粉末混合物を加熱する段階と、
(c)均一な状態の溶融物を形成できるように前記生成された混合物を加熱する段階と、
(d)前記溶融物を急冷させてガラス質固体電解質を得る段階と、を含む下記化学式1の固体電解質の製造方法:
0.4<a<0.55、0.4<b<0.55、0.02<c<0.05、a+b+c=1であり、0≦d<0.2である。 - 前記(a)段階の混合物にLiCl及びLi2SO4よりなる群から選択された1つ以上の化合物をさらに添加することを特徴とする請求項3に記載の固体電解質の製造方法。
- 前記(b)段階でLiO2は600ないし800℃の温度でLiO2前駆体化合物から分解されることを特徴とする請求項3に記載の固体電解質の製造方法。
- 前記(c)段階で前記溶融物は900ないし1500℃の温度で得られることを特徴とする請求項3に記載の固体電解質の製造方法。
- 前記(d)段階で前記溶融物は0ないし25℃の温度で急冷されることを特徴とする請求項3に記載の固体電解質の製造方法。
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2003-0006288A KR100513726B1 (ko) | 2003-01-30 | 2003-01-30 | 고체 전해질, 이를 채용한 전지 및 그 고체 전해질의 제조방법 |
Publications (2)
Publication Number | Publication Date |
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JP2004235155A JP2004235155A (ja) | 2004-08-19 |
JP4532128B2 true JP4532128B2 (ja) | 2010-08-25 |
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Application Number | Title | Priority Date | Filing Date |
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JP2004024681A Expired - Lifetime JP4532128B2 (ja) | 2003-01-30 | 2004-01-30 | 固体電解質、その製造方法及びそれを採用した電池 |
Country Status (4)
Country | Link |
---|---|
US (1) | US7273682B2 (ja) |
EP (1) | EP1443582A1 (ja) |
JP (1) | JP4532128B2 (ja) |
KR (1) | KR100513726B1 (ja) |
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US5338625A (en) | 1992-07-29 | 1994-08-16 | Martin Marietta Energy Systems, Inc. | Thin film battery and method for making same |
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