JP6585063B2 - 電極材料およびそれを用いた電極層、電池並びにエレクトロクロミック素子 - Google Patents
電極材料およびそれを用いた電極層、電池並びにエレクトロクロミック素子 Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims description 85
- 239000000843 powder Substances 0.000 claims description 118
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 59
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 59
- 239000002245 particle Substances 0.000 claims description 28
- 230000004913 activation Effects 0.000 claims description 24
- 150000002736 metal compounds Chemical class 0.000 claims description 19
- 206010021143 Hypoxia Diseases 0.000 claims description 16
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 7
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000010410 layer Substances 0.000 description 52
- 230000000052 comparative effect Effects 0.000 description 40
- 230000007547 defect Effects 0.000 description 33
- 239000003990 capacitor Substances 0.000 description 32
- 238000005259 measurement Methods 0.000 description 32
- 238000010438 heat treatment Methods 0.000 description 26
- 208000028659 discharge Diseases 0.000 description 25
- 239000012298 atmosphere Substances 0.000 description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 24
- 239000001301 oxygen Substances 0.000 description 24
- 229910052760 oxygen Inorganic materials 0.000 description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 21
- 238000000034 method Methods 0.000 description 19
- 229910044991 metal oxide Inorganic materials 0.000 description 16
- 150000004706 metal oxides Chemical class 0.000 description 16
- 239000013078 crystal Substances 0.000 description 14
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 11
- 238000005092 sublimation method Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 230000005611 electricity Effects 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 230000007812 deficiency Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 239000006230 acetylene black Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 230000009191 jumping Effects 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000002905 metal composite material Substances 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 4
- 238000009832 plasma treatment Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 4
- 238000001075 voltammogram Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005315 distribution function Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000002772 conduction electron Substances 0.000 description 1
- 239000002482 conductive additive Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000013532 laser treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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Description
(1)酸化タングステン:WO3−x、0≦x≦1。
(2)酸化モリブデン:MoO3−x、0≦x≦1。
(3)酸化チタン:TiO2−x、0≦x≦1。
(4)MoxWyOz、0<x≦1、0<y≦1、x+y=1としたとき2≦z≦3。
(5)WxTiyOz、0<x≦1、0<y≦1、x+y=1としたとき2≦z≦3。
(6)MoxTiyOz、0<x≦1、0<y≦1、x+y=1としたとき2≦z≦3。
(7)MoxWyOzTiα、0<x≦1、0<y≦1、0<α≦1、x+y+α=1としたとき2≦z≦3。
(8)タングステン酸リチウム:LixWyO3−z、0<x≦1、0<y≦1、0≦z≦1。
(9)モリブデン酸リチウム:LixMoyO3−z、0<x≦1、0<y≦1、0≦z≦1。
(10)チタン酸リチウム:LixTiyO3−z、0<x≦1、0<y≦1、0≦z≦1。
(11)硫化モリブデン:MoS2−x、0<x≦1。
(実施例1〜3および比較例1〜2)
原料粉末として平均粒径が1.5μmの酸化タングステン粉末を用意した。この原料粉末を、空気をキャリアガスとして誘導結合プラズマ炎に平均流速が1.5m/sとなるように噴霧し、原料粉末を昇華させながら酸化反応を行う昇華工程により酸化タングステン(WO3)粉末を得た。得られた酸化タングステン(WO3)粉末の平均粒径は8.2nm(0.008μm)であった。
原料粉末として平均粒径が2.0μmの酸化タングステン粉末を用意した。この原料粉末を、空気をキャリアガスとして誘導結合プラズマ炎に平均流速1.2m/sとなるように噴霧し、原料粉末を昇華させながら酸化反応を行う昇華工程により酸化タングステン(WO3)粉末を得た。得られた酸化タングステン(WO3)粉末の平均粒径は12.1nm(0.0012μm)であった。
実施例1〜3および比較例1〜2に係る酸化タングステン粉末を使用してキャパシタを作製した。キャパシタの構成は図8に示す。図8中、符号20はキャパシタであり、21は負極側電極層であり、22は負極層であり、23はセパレータ層であり、24は正極層であり、25は正極側電極層である。負極側電極層21および正極側電極層25は厚さ15μmのアルミ箔から成る。
平均粒径が1 μmである酸化モリブデン(MoO3)粉末を用意した。この酸化モリブデン粉末に対し、大気中で60分間の熱処理を実施した。
電極材料を実施例5〜6および比較例3に代えた以外は実施例1と同様に処理して実施例5A〜6Aおよび比較例3Aに係るキャパシタを作製した。各キャパシタについて、実施例1Aと同様の方法で初期の電気容量、サイクル試験後の容量維持率、内部抵抗値を測定した。その測定結果を下記表10に示す。
実施例2の酸化タングステン粉末の窒素中での熱処理条件を、窒素と水素との混合ガスに変えたものを実施例7とした。なお、窒素と水素の混合ガスは水素を3vol%、残部が窒素からなるものである。また、熱処理条件は700℃×5分とした。
実施例2Aのキャパシタの電極材料を実施例7の酸化タングステン粉末に代えたキャパシタを作成し実施例7Aとした。実施例2Aと同様の測定方法で、初期の電気容量およびサイクル試験後の容量維持率を測定した。その測定結果を下記表13に示す。
2 …測定用試料
3 …n−Si層
4 …SiO2層
5 …実施例(または比較例)の酸化タングステン粉末からなる電極層
6 …金属電極
20…キャパシタ
21…負極側電極層
22…負極層
23…セパレータ層
24…正極層
25…正極側電極層
Claims (10)
- 酸化タングステン、酸化モリブデン、MoxWyOz(0<x≦1、0<y≦1、x+y=1、2≦z≦3)から選択される少なくとも1種の金属化合物粉末から成る電極材料であり、上記金属化合物粉末の平均粒径が50μm以下であり、上記金属化合物粉末の酸素欠損量が1×10 18 cm −3 以上であり、活性化エネルギーEαが0.05eV以下であり、キャリア密度が1×1018cm−3以上であることを特徴とする電極材料。
- 前記金属化合物粉末が常温(25℃)でホッピング伝導特性を有することを特徴とする請求項1記載の電極材料。
- 測定温度をT(°K)とした場合に、1000/T値が2.8〜4.0の範囲で前記金属化合物粉末がホッピング伝導特性を有することを特徴とする請求項1ないし請求項2のいずれか1項に記載の電極材料。
- 前記金属化合物粉末の常温(25℃)での抵抗率が10Ωcm以下であることを特徴とする請求項1ないし請求項3のいずれか1項に記載の電極材料。
- 前記金属化合物粉末の平均粒径が10μm以下であることを特徴とする請求項1ないし請求項4いずれか1項に記載の電極材料。
- 前記金属化合物粉末の平均粒径が5μm以下であることを特徴とする請求項5に記載の電極材料。
- 請求項1ないし請求項6のいずれか1項に記載の電極材料を50質量%以上100質量%以下含有することを特徴とする電極層。
- 請求項7記載の電極層を具備したことを特徴とする電池。
- 請求項7記載の電極層を負極として具備したことを特徴とする請求項8記載の電池。
- 請求項1ないし請求項6のいずれか1項に記載の電極材料を具備したことを特徴とするエレクトロクロミック素子。
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