JP7106188B2 - 板状二酸化マンガンナノ粒子の製造方法 - Google Patents
板状二酸化マンガンナノ粒子の製造方法 Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 16
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- 238000006243 chemical reaction Methods 0.000 claims description 14
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- 150000002696 manganese Chemical class 0.000 claims description 10
- 239000007800 oxidant agent Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 8
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- UFULAYFCSOUIOV-UHFFFAOYSA-N cysteamine Chemical compound NCCS UFULAYFCSOUIOV-UHFFFAOYSA-N 0.000 claims description 3
- 229960003151 mercaptamine Drugs 0.000 claims description 3
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- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 claims description 2
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
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- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 description 1
- 229950004394 ditiocarb Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
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- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
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- 235000014705 isoleucine Nutrition 0.000 description 1
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- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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- 239000000243 solution Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/42—Powders or particles, e.g. composition thereof
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
本出願は、2017年11月10日付韓国特許出願第10-2017-0149678号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれている。
本発明は、板状二酸化マンガンナノ粒子の製造方法に関する。
また、本発明は、前記製造方法で製造された板状二酸化マンガンナノ粒子を提供する。
また、本発明は、前記板状二酸化マンガンナノ粒子を含む酸化・還元キャパシタの陽極を提供する。
以下、各段階別に本発明を詳細に説明する。
前記段階1は、マンガン塩とアミン系カップリング剤を反応させることによって、最終的に製造しようとする二酸化マンガンが板状を有するようにする段階である。
好ましくは、前記アミン系カップリング剤は、下記化学式1で表される化合物である:
R1は天然アミノ酸の残基であり、
R2はCOOH、またはCH2SHである。
前記段階2は、前記段階1の生成物に酸化剤を添加して反応させることによって、最終的に板状の二酸化マンガンナノ粒子を製造する段階である。
前記酸化剤としては、K2S2O8、Na2S2O8、または(NH4)2S2O8を使用し得る。
また、本発明は上述した製造方法で製造される板状二酸化マンガンナノ粒子を提供する。前記板状二酸化マンガンナノ粒子は、表面積が広いため炭素系導電材料、例えばカーボンブラック、炭素ナノチューブのような材料とうまく混合され得、製造過程で炭素ナノチューブなどの1D材料がある場合に炭素表面に一部の二酸化マンガンが付着して炭素ナノチューブとの混合が自然に行われる。
(段階1)
反応容器に酢酸マンガン(Mn acetate)2mmolおよび水20mLを入れ、グリシン(glycine)4mmolを添加した。次いで、NaOH 5gおよび水50mLを添加して常温で30分間攪拌して反応させた。
(段階2)
前記段階1の生成物に、K2S2O8 1.6gおよび水50mLをさらに添加し、常温で12時間さらに反応させて板状の二酸化マンガンを製造した。
(段階1)
反応容器に炭素ナノチューブ(CNT)40mg、酢酸マンガン(Mn acetate)2mmolおよび水20mLを入れ、グリシン(glycine)4mmolを添加した。次いで、NaOH 5gおよび水50mLを添加して常温で30分間攪拌して反応させた。
(段階2)
前記段階1の生成物に、K2S2O8 1.6gおよび水50mLをさらに添加し、常温で12時間さらに反応させて板状の二酸化マンガンを製造した。
グリシンの代わりにシステアミン(cysteamine)を使用することを除いては、前記実施例2と同様の方法により板状の二酸化マンガンを製造した。
KMnO4 0.5mmol、ホルムアルデヒド0.2mL、および水35mLを混合した溶液を高圧反応器に入れ、120℃で10時間反応させた。次いで、空気中で280℃に加熱して二酸化マンガンを製造した。
KMnO4 3mmol、MnSO4 0.5mmol、水40mL、およびNaOH 500mgを混合した溶液を高圧反応器に入れ、160℃で12時間反応させて二酸化マンガンを製造した。
グリシンの代わりにナトリウムジエチルジチオカルバメート(sodium diethyldithiocarbamate)を使用することを除いては、前記実施例2と同様の方法により板状の二酸化マンガンを製造した。
前記実施例および比較例で製造した二酸化マンガンをSEMで観察し、その結果を図1~6に示した。
本発明の実施例の場合、板状形態が観察されることに対し、比較例1の場合、針状が観察され、比較例2の場合、蜂の巣状が観察された。
また、比較例3の場合、不明な形状の粒子が合成された。
前記実施例または比較例で製造した二酸化マンガン85重量%、カーボンブラック10重量%およびポリフッ化ビニリデン(Polyvinylidene Fluoride(PVDF))バインダー5重量%を混合した後、混合された粉末0.1gに対してNMP 3.9gを添加して溶液を作って小型ガラスバイアルに1mm直径のZrO2ビーズとともに入れた後、3次元混合器を用いて混合した。インクをガラス状炭素(glassy carbon)電極上に配置して真空で乾燥した後、1MのLi2SO4溶液で0~1.0V範囲または0~1.2V範囲でサイクリックボルタンメトリ(CV)により比静電容量を測定し、その結果を下記表1に示した。
Claims (5)
- マンガン塩を含む水溶液にアミン系カップリング剤を添加して反応させる段階(段階1);および
前記段階1の生成物に酸化剤を添加して反応させる段階(段階2)を含み、
前記マンガン塩は、Mn(CH3COO) 2 であり、
前記アミン系カップリング剤は、グリシンまたはシステアミンであり、
前記酸化剤は、K2S2O 8 である、
板状二酸化マンガンナノ粒子の製造方法。 - 前記マンガン塩とアミン系カップリング剤のモル比は、1:0.5~2である、請求項1に記載の製造方法。
- 前記段階1の反応時間は、5分~1時間である、請求項1または2に記載の製造方法。
- 前記段階1で使用したマンガン塩と酸化剤のモル比が1:2~10である、請求項1から3のいずれか一項に記載の製造方法。
- 前記段階2の反応時間は、2時間~12時間である、請求項1から4のいずれか一項に記載の製造方法。
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KR10-2017-0149678 | 2017-11-10 | ||
PCT/KR2018/010863 WO2019093648A2 (ko) | 2017-11-10 | 2018-09-14 | 판상형 이산화망간 나노 입자의 제조 방법 |
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WO2007006585A2 (de) | 2005-07-14 | 2007-01-18 | Elsper Ruediger | Synthese von porösen und/oder schichtstrukturierten manganoxiden |
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US3647835A (en) * | 1969-11-12 | 1972-03-07 | Mobil Oil Corp | Method of direct generation of manganese (iii) solution from manganese (ii) solution |
JP2815611B2 (ja) * | 1989-05-10 | 1998-10-27 | 正同化学工業株式会社 | 酸化マンガンの製造方法 |
KR100842295B1 (ko) * | 2007-04-03 | 2008-06-30 | 한국전자통신연구원 | 이산화망간 나노입자의 제조방법 |
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US20200207637A1 (en) | 2020-07-02 |
CN111094186A (zh) | 2020-05-01 |
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EP3659973A2 (en) | 2020-06-03 |
JP2020525387A (ja) | 2020-08-27 |
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