JP6336470B2 - 多孔化された構造のチタン酸化物と炭素系物質が結合されたスーパーキャパシター電極材料およびその製造方法 - Google Patents
多孔化された構造のチタン酸化物と炭素系物質が結合されたスーパーキャパシター電極材料およびその製造方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 89
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 85
- 239000007772 electrode material Substances 0.000 title claims description 32
- 239000003575 carbonaceous material Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000000034 method Methods 0.000 title description 8
- 239000003990 capacitor Substances 0.000 claims description 30
- 239000010410 layer Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 18
- 239000002041 carbon nanotube Substances 0.000 claims description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 9
- 239000011229 interlayer Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- -1 hydrogen ions Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 15
- 239000002253 acid Substances 0.000 description 11
- 238000004146 energy storage Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 229910000314 transition metal oxide Inorganic materials 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052792 caesium Inorganic materials 0.000 description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 2
- 229910000024 caesium carbonate Inorganic materials 0.000 description 2
- WMRRGFKAQUKRPY-UHFFFAOYSA-N cesium oxygen(2-) titanium(4+) Chemical compound [O-2].[Ti+4].[Cs+] WMRRGFKAQUKRPY-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910006913 SnSb Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
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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
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Description
1)多孔化された構造のチタン酸化物の製造
Cs2CO3(炭酸セシウム)とTiO2(二酸化チタン)は、化学式Cs0.67Ti1.83□0.17O4(ここで、□は電極材料層において負電荷の原因となるベイカンシー(vacancy)を意味する)で表される層状Cs−チタネート(セシウムチタン酸化物)を製造するために化学量論的に混合して800℃で20時間熱処理を行った。次に、前記で合成された物質を1MのHCl溶液に浸るほど混合して放置しておくことで3日間反応させた。この時、酸溶液は1日1回新しい酸溶液に交替した。
前記過程から得られたチタン酸化物と炭素ナノチューブを質量比8:1で準備し、乳鉢を利用して物理的に混合し、NMP(N−Methyl pyrrolidone)を溶媒として3mL投入した後に攪拌した。そして110℃以上のオーブンで乾燥してスーパーキャパシター電極材料を製造した。
一般的に商用化されたチタン酸化物(TiO2、Sigma Aladrich)と炭素ナノチューブを質量比8:1で準備し、乳鉢を利用して物理的に混合し、NMP(N−Methyl pyrrolidone)を溶媒として3mL投入した後に攪拌した。そして110℃以上のオーブンで乾燥してスーパーキャパシター電極材料を製造した。
実施例および比較例で製造されたスーパーキャパシター電極材料、バインダーであるPVDF(Polyvinylidene fluoride)および導電材を質量比8:1:1で投入して攪拌した。得られた溶液を集電体であるアルミニウム箔上に薄くコーティングして作業電極を製造し、対電極および基準電極としてステンレススチールホイル(foil)を用いた。その次に、CV(サイクリック・ボルタンメトリー(Cyclic voltammetry))を用いて100mV/s スキャンレート(scan rate)で0Vから2.8Vの範囲で容量を測定した。
Claims (10)
- 多孔化された構造のチタン酸化物と炭素系物質とを含み、
前記多孔化された構造のチタン酸化物は、層状チタン酸化物層間に球状チタン酸化物が位置している形態であることを特徴とするスーパーキャパシター電極材料。 - 前記炭素系物質は、多孔化された構造のチタン酸化物100重量部に対して10〜800重量部の範囲で含まれることを特徴とする、請求項1に記載のスーパーキャパシター電極材料。
- 前記多孔化された構造のチタン酸化物において、球状チタン酸化物は層状チタン酸化物100重量部に対して10〜100重量部の範囲で含まれることを特徴とする、請求項1に記載のスーパーキャパシター電極材料。
- 前記球状チタン酸化物の粒径は1〜10nmの範囲であることを特徴とする、請求項1に記載のスーパーキャパシター電極材料。
- 前記炭素系物質は、炭素ナノチューブであることを特徴とする、請求項1に記載のスーパーキャパシター電極材料。
- 層状チタン酸化物の層間に巨大有機物を挿入して層間力を弱化させるステップ、
層状チタン酸化物層間に球状チタン酸化物を挿入するステップ、
熱処理して多孔化された構造のチタン酸化物を得るステップ、および
前記多孔化された構造のチタン酸化物と炭素系物質とを結合するステップを含むことを特徴とするスーパーキャパシター電極材料の製造方法。 - 前記層状チタン酸化物の層間力を弱化させるために、層状チタン酸化物に含まれた水素イオンと同一モル数の巨大有機物を層状チタン酸化物と共に蒸留水に投入して混合することを特徴とする、請求項6に記載のスーパーキャパシター電極材料の製造方法。
- 前記層状チタン酸化物層間に球状チタン酸化物を挿入するために、層状チタン酸化物100重量部に対して10〜100重量部の範囲の球状チタン酸化物を混合することを特徴とする、請求項6に記載のスーパーキャパシター電極材料の製造方法。
- 前記熱処理は、200〜600℃の温度範囲で1〜3時間行うことを特徴とする、請求項6に記載のスーパーキャパシター電極材料の製造方法。
- 前記多孔化された構造のチタン酸化物と炭素系物質を結合するために、チタン酸化物100重量部に対して10〜800重量部の範囲の炭素系物質を混合することを特徴とする、請求項6に記載のスーパーキャパシター電極材料の製造方法。
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KR10-2012-0144745 | 2012-12-12 | ||
KR1020120144745A KR101973050B1 (ko) | 2012-12-12 | 2012-12-12 | 다공화된 구조의 티타늄 산화물과 탄소계 물질이 병합된 슈퍼 캐패시터 전극재료 및 그 제조방법 |
PCT/KR2013/008739 WO2014092313A1 (ko) | 2012-12-12 | 2013-09-30 | 다공화된 구조의 티타늄 산화물과 탄소계 물질이 병합된 슈퍼 캐패시터 전극재료 및 그 제조방법 |
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JP6336470B2 true JP6336470B2 (ja) | 2018-06-06 |
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US (1) | US9972448B2 (ja) |
EP (1) | EP2933809B1 (ja) |
JP (1) | JP6336470B2 (ja) |
KR (1) | KR101973050B1 (ja) |
WO (1) | WO2014092313A1 (ja) |
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WO2016161587A1 (en) * | 2015-04-09 | 2016-10-13 | Kechuang Lin | Electrode material and energy storage apparatus |
WO2017139952A1 (zh) * | 2016-02-18 | 2017-08-24 | 华为技术有限公司 | 一种波长控制方法和装置 |
WO2022174264A1 (en) * | 2021-02-11 | 2022-08-18 | Drexel University | Bottom-up, scalable synthesis of oxide-based sub-nano and nanofilaments and nanofilament-based two-dimensional flakes and mesoporous powders |
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US5665625A (en) * | 1995-05-19 | 1997-09-09 | Micron Technology, Inc. | Method of forming capacitors having an amorphous electrically conductive layer |
JP2002158140A (ja) | 2000-11-20 | 2002-05-31 | Hitachi Maxell Ltd | 電気化学キャパシタ |
JP2004221531A (ja) * | 2002-12-26 | 2004-08-05 | Toin Gakuen | 光充電可能な積層型電気二重層キャパシタ |
KR100569188B1 (ko) * | 2004-01-16 | 2006-04-10 | 한국과학기술연구원 | 탄소-다공성 지지체 복합 전극 및 그 제조방법 |
JP4995428B2 (ja) * | 2004-03-10 | 2012-08-08 | 東海旅客鉄道株式会社 | 酸化チタン塗膜形成方法 |
WO2007015710A2 (en) * | 2004-11-09 | 2007-02-08 | Board Of Regents, The University Of Texas System | The fabrication and application of nanofiber ribbons and sheets and twisted and non-twisted nanofiber yarns |
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EP2118948A1 (en) | 2007-03-05 | 2009-11-18 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | A material, in particular for use in electrochemical cells or supercapacitors and a method of making such a material |
JP5612857B2 (ja) | 2007-08-30 | 2014-10-22 | 石原産業株式会社 | チタン酸化合物及びその製造方法並びに該チタン酸化合物を含む電極活物質、電極活物質を用いてなる蓄電デバイス |
JP4558085B2 (ja) * | 2008-06-20 | 2010-10-06 | 大阪瓦斯株式会社 | 多孔質酸化チタン被覆炭素材料組成物 |
US8629076B2 (en) * | 2010-01-27 | 2014-01-14 | Lawrence Livermore National Security, Llc | High surface area silicon carbide-coated carbon aerogel |
KR20110115659A (ko) * | 2010-04-16 | 2011-10-24 | 한국생명공학연구원 | 다공성 금속산화물 나노구조체로 코팅된 탄소나노튜브 복합체 및 그 용도 |
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JP5284400B2 (ja) | 2011-03-18 | 2013-09-11 | 株式会社田中化学研究所 | カーボン複合チタン酸リチウム、その製造方法、非水電解質電池用活物質、及び非水電解質電池 |
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