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Electrodeposition of bismuth, tellurium and bismuth telluride through sub-10 nm mesoporous silica thin films

Electrodeposition of bismuth, tellurium and bismuth telluride through sub-10 nm mesoporous silica thin films
Electrodeposition of bismuth, tellurium and bismuth telluride through sub-10 nm mesoporous silica thin films
Templated electrodeposition is an efficient technique for the bottom-up fabrication of nanostructures and can effectively control the size and shape of the electrodeposits. Here, mesoporous silica thin films with highly ordered mesopores and a regular three-dimensional mesostructure were synthesised as templates for electrodeposition. The mesoporous silica films have small mesopores (∼8 nm) and complex mesopore channels (Fmmm mesostructure with the [0 1 0] axis perpendicular to the substrate). Electrodeposition of bismuth, tellurium and bismuth-tellurium was investigated from electrolytes containing [NnBu4][BiCl4], [NnBu4]2[TeCl6] and [NnBu4]Cl dissolved in dry dichloromethane. Top-view SEM images showed Bi, Te and Bi doped-Te nanoparticles in the mesopores and cross-section SEM showed there were a few Te nanowires, in addition to the particle aggregations on the surface. This is a promising observation as it demonstrates the possibility of preparing sub-10 nm nanowires by templated electrodeposition even though the deposits are not uniformly electrodeposited in all the mesopores. EDX shows the deposited Bi-Te nanoparticles were tellurium-rich, XRD shows they were trigonal tellurium (ICSD 65692). A variety of parameters including the choice of pulsed electrodeposition conditions and [NnBu4][BiCl4] concentration (2.25 mM and 3 mM) were investigated in order to control the composition of the deposit. All samples prepared by pulsed electrodeposition showed very low Bi:Te ratio (Bi/Te<0.02), whereas samples deposited for 5 min at −0.6 V achieved high Bi content (Bi/Te=0.49).
0013-4686
Shao, Li
e273c42f-6065-40f8-8077-35a0b8a2505a
Zhelev, Nikolay
76a8a0dd-0c24-4483-a217-b17ee26bd79b
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Huang, Ruomeng
c6187811-ef2f-4437-8333-595c0d6ac978
Bartlett, Philip N.
d99446db-a59d-4f89-96eb-f64b5d8bb075
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Shao, Li
e273c42f-6065-40f8-8077-35a0b8a2505a
Zhelev, Nikolay
76a8a0dd-0c24-4483-a217-b17ee26bd79b
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Huang, Ruomeng
c6187811-ef2f-4437-8333-595c0d6ac978
Bartlett, Philip N.
d99446db-a59d-4f89-96eb-f64b5d8bb075
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5

Shao, Li, Zhelev, Nikolay, Zhang, Wenjian, Reid, Gillian, Huang, Ruomeng, Bartlett, Philip N. and Hector, Andrew L. (2024) Electrodeposition of bismuth, tellurium and bismuth telluride through sub-10 nm mesoporous silica thin films. Electrochimica Acta, 505, [144989]. (doi:10.1016/j.electacta.2024.144989).

Record type: Article

Abstract

Templated electrodeposition is an efficient technique for the bottom-up fabrication of nanostructures and can effectively control the size and shape of the electrodeposits. Here, mesoporous silica thin films with highly ordered mesopores and a regular three-dimensional mesostructure were synthesised as templates for electrodeposition. The mesoporous silica films have small mesopores (∼8 nm) and complex mesopore channels (Fmmm mesostructure with the [0 1 0] axis perpendicular to the substrate). Electrodeposition of bismuth, tellurium and bismuth-tellurium was investigated from electrolytes containing [NnBu4][BiCl4], [NnBu4]2[TeCl6] and [NnBu4]Cl dissolved in dry dichloromethane. Top-view SEM images showed Bi, Te and Bi doped-Te nanoparticles in the mesopores and cross-section SEM showed there were a few Te nanowires, in addition to the particle aggregations on the surface. This is a promising observation as it demonstrates the possibility of preparing sub-10 nm nanowires by templated electrodeposition even though the deposits are not uniformly electrodeposited in all the mesopores. EDX shows the deposited Bi-Te nanoparticles were tellurium-rich, XRD shows they were trigonal tellurium (ICSD 65692). A variety of parameters including the choice of pulsed electrodeposition conditions and [NnBu4][BiCl4] concentration (2.25 mM and 3 mM) were investigated in order to control the composition of the deposit. All samples prepared by pulsed electrodeposition showed very low Bi:Te ratio (Bi/Te<0.02), whereas samples deposited for 5 min at −0.6 V achieved high Bi content (Bi/Te=0.49).

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Accepted/In Press date: 28 August 2024
e-pub ahead of print date: 30 August 2024
Published date: 5 September 2024

Identifiers

Local EPrints ID: 493978
URI: http://eprints.soton.ac.uk/id/eprint/493978
ISSN: 0013-4686
PURE UUID: 1f4716f9-e156-45bf-8632-5fd3999dc7c7
ORCID for Li Shao: ORCID iD orcid.org/0000-0001-6029-5574
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468
ORCID for Ruomeng Huang: ORCID iD orcid.org/0000-0003-1185-635X
ORCID for Philip N. Bartlett: ORCID iD orcid.org/0000-0002-7300-6900
ORCID for Andrew L. Hector: ORCID iD orcid.org/0000-0002-9964-2163

Catalogue record

Date deposited: 18 Sep 2024 16:32
Last modified: 19 Sep 2024 02:02

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Contributors

Author: Li Shao ORCID iD
Author: Nikolay Zhelev
Author: Wenjian Zhang
Author: Gillian Reid ORCID iD
Author: Ruomeng Huang ORCID iD

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