Evolution of Anodic Product from Molybdenum Metal in Absolute Ethanol and Humidity Sensing under Ambient Conditions

Chengsheng Ni; Darragh Carolan; Jianing Hui; Conor Rocks; Dilli Babu Padmanaban; Jiupai Ni; Deti Xie; Zeguo Fang; John Irvine; P Maguire; Davide Mariotti

doi:10.1021/acs.cgd.9b00646

Evolution of Anodic Product from Molybdenum Metal in Absolute Ethanol and Humidity Sensing under Ambient Conditions

Chengsheng Ni, Darragh Carolan, Jianing Hui, Conor Rocks, Dilli Babu Padmanaban, Jiupai Ni, Deti Xie, Zeguo Fang, John Irvine, P Maguire, Davide Mariotti

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Abstract

Room-temperature nonaqueous synthetic routes turn out to be particularly competitive among all the available liquid-phase synthetic methods for nanometer-sized metal oxides for multiple applications. Microplasma-assisted anodization is employed to prepare soluble and crystalline Mo species in a water-deficient and extraneous ionic-salt-free ethanol electrolyte. The anodization of Mo in absolute ethanol is found to produce Mo oxyethoxide in the liquid ethanol phase, along with a small montage of mixed hexagonal and orthorhombic MoO ₃ crystals. The evolution of Mo species in solid and liquid phases is characterized to study the crystallization of MoO ₃ crystal and the formation of blue spherical Mo polyoxometalates (POMs) after extended aging. The addition of water in the suspension delayed the formation of molybdenum blue while hydrogen peroxide induced the precipitation of a dendritic framework of hexagonal MoO ₃. A thin MoO ₃ film was produced from the solution and can be used for humidity sensing by the facile conductivity measurement.

Original language	English
Pages (from-to)	5249-5257
Number of pages	9
Journal	Crystal Growth & Design
Volume	19
Issue number	9
Early online date	9 Aug 2019
DOIs	https://doi.org/10.1021/acs.cgd.9b00646
Publication status	Published (in print/issue) - 4 Sept 2019

Bibliographical note

Funding Information:
We would like to thank the support from National Natural Science Foundation of China (NSFC) (Nos. 51702264 and 41371275), Fundamental Research Funds for the Central Universities (No. XDJK2017B033), and Research Funding of Southwest University (No. SWU117019). The funding from the Engineering and Physical Sciences Research Council (EPSRC) (under Grant Nos. EP/K022237/1, EP/K036769/1, and EP/M024938/1) is also acknowledged. We also appreciate the funding from the EU COST Action (No. TD1208) for useful exchanges and discussions. We also thank Ms. Zhang Ziye (Southwest University) for the measurement of conductivity under different relative humidity values.

Publisher Copyright:
© 2019 American Chemical Society.

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acs.cgd.9b00646Final published version, 8.3 MBLicence: CC BY

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@article{e99214b9ddd94a359aabd88cd7ed5dc8,

title = "Evolution of Anodic Product from Molybdenum Metal in Absolute Ethanol and Humidity Sensing under Ambient Conditions",

abstract = "Room-temperature nonaqueous synthetic routes turn out to be particularly competitive among all the available liquid-phase synthetic methods for nanometer-sized metal oxides for multiple applications. Microplasma-assisted anodization is employed to prepare soluble and crystalline Mo species in a water-deficient and extraneous ionic-salt-free ethanol electrolyte. The anodization of Mo in absolute ethanol is found to produce Mo oxyethoxide in the liquid ethanol phase, along with a small montage of mixed hexagonal and orthorhombic MoO 3 crystals. The evolution of Mo species in solid and liquid phases is characterized to study the crystallization of MoO 3 crystal and the formation of blue spherical Mo polyoxometalates (POMs) after extended aging. The addition of water in the suspension delayed the formation of molybdenum blue while hydrogen peroxide induced the precipitation of a dendritic framework of hexagonal MoO 3. A thin MoO 3 film was produced from the solution and can be used for humidity sensing by the facile conductivity measurement. ",

author = "Chengsheng Ni and Darragh Carolan and Jianing Hui and Conor Rocks and Padmanaban, {Dilli Babu} and Jiupai Ni and Deti Xie and Zeguo Fang and John Irvine and P Maguire and Davide Mariotti",

note = "Funding Information: We would like to thank the support from National Natural Science Foundation of China (NSFC) (Nos. 51702264 and 41371275), Fundamental Research Funds for the Central Universities (No. XDJK2017B033), and Research Funding of Southwest University (No. SWU117019). The funding from the Engineering and Physical Sciences Research Council (EPSRC) (under Grant Nos. EP/K022237/1, EP/K036769/1, and EP/M024938/1) is also acknowledged. We also appreciate the funding from the EU COST Action (No. TD1208) for useful exchanges and discussions. We also thank Ms. Zhang Ziye (Southwest University) for the measurement of conductivity under different relative humidity values. Publisher Copyright: {\textcopyright} 2019 American Chemical Society.",

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AU - Ni, Chengsheng

AU - Carolan, Darragh

AU - Hui, Jianing

AU - Rocks, Conor

AU - Padmanaban, Dilli Babu

AU - Ni, Jiupai

AU - Xie, Deti

AU - Fang, Zeguo

AU - Irvine, John

AU - Maguire, P

AU - Mariotti, Davide

N1 - Funding Information: We would like to thank the support from National Natural Science Foundation of China (NSFC) (Nos. 51702264 and 41371275), Fundamental Research Funds for the Central Universities (No. XDJK2017B033), and Research Funding of Southwest University (No. SWU117019). The funding from the Engineering and Physical Sciences Research Council (EPSRC) (under Grant Nos. EP/K022237/1, EP/K036769/1, and EP/M024938/1) is also acknowledged. We also appreciate the funding from the EU COST Action (No. TD1208) for useful exchanges and discussions. We also thank Ms. Zhang Ziye (Southwest University) for the measurement of conductivity under different relative humidity values. Publisher Copyright: © 2019 American Chemical Society.

PY - 2019/9/4

Y1 - 2019/9/4

N2 - Room-temperature nonaqueous synthetic routes turn out to be particularly competitive among all the available liquid-phase synthetic methods for nanometer-sized metal oxides for multiple applications. Microplasma-assisted anodization is employed to prepare soluble and crystalline Mo species in a water-deficient and extraneous ionic-salt-free ethanol electrolyte. The anodization of Mo in absolute ethanol is found to produce Mo oxyethoxide in the liquid ethanol phase, along with a small montage of mixed hexagonal and orthorhombic MoO 3 crystals. The evolution of Mo species in solid and liquid phases is characterized to study the crystallization of MoO 3 crystal and the formation of blue spherical Mo polyoxometalates (POMs) after extended aging. The addition of water in the suspension delayed the formation of molybdenum blue while hydrogen peroxide induced the precipitation of a dendritic framework of hexagonal MoO 3. A thin MoO 3 film was produced from the solution and can be used for humidity sensing by the facile conductivity measurement.

AB - Room-temperature nonaqueous synthetic routes turn out to be particularly competitive among all the available liquid-phase synthetic methods for nanometer-sized metal oxides for multiple applications. Microplasma-assisted anodization is employed to prepare soluble and crystalline Mo species in a water-deficient and extraneous ionic-salt-free ethanol electrolyte. The anodization of Mo in absolute ethanol is found to produce Mo oxyethoxide in the liquid ethanol phase, along with a small montage of mixed hexagonal and orthorhombic MoO 3 crystals. The evolution of Mo species in solid and liquid phases is characterized to study the crystallization of MoO 3 crystal and the formation of blue spherical Mo polyoxometalates (POMs) after extended aging. The addition of water in the suspension delayed the formation of molybdenum blue while hydrogen peroxide induced the precipitation of a dendritic framework of hexagonal MoO 3. A thin MoO 3 film was produced from the solution and can be used for humidity sensing by the facile conductivity measurement.

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Evolution of Anodic Product from Molybdenum Metal in Absolute Ethanol and Humidity Sensing under Ambient Conditions

Abstract

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ACS-Crystal Growth & Design, Chengsheng-MOx synthesis

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Evolution of Anodic Product from Molybdenum Metal in Absolute Ethanol and Humidity Sensing under Ambient Conditions

Abstract

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ACS-Crystal Growth & Design, Chengsheng-MOx synthesis

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