Electrochemical quartz crystal microbalance, X-ray photoelectron spectroscopy, and Raman spectroscopy analysis of SiCl4 reduction in ionic liquids

Yasuhiro Tsuyuki; Tram Anh Pham Huynh; Jason Komadina; Yasuhiro Fukunaka; Takayuki Homma

doi:10.1016/j.electacta.2015.04.167

Electrochemical quartz crystal microbalance, X-ray photoelectron spectroscopy, and Raman spectroscopy analysis of SiCl₄ reduction in ionic liquids

Yasuhiro Tsuyuki^*, Tram Anh Pham Huynh, Jason Komadina, Yasuhiro Fukunaka, Takayuki Homma

^*Corresponding author for this work

School of Advanced Science and Engineering

Research output: Contribution to journal › Article › peer-review

8 Citations (Scopus)

Abstract

The reaction mechanism of Si electrodeposition in the ionic liquid trimethyl-n-hexylammonium bis(trifluoromethylsulfonyl) imide (TMHATFSI) with SiCl₄ was investigated using an electrochemical quartz crystal microbalance (EQCM) and X-ray photoelectron spectroscopy (XPS). The deposited films were further characterized by Raman spectroscopy. The EQCM method measured the frequency change in situ during electrodeposition, whereas XPS provided the Si mass concentration in the electrodeposited films. By combining these results, the mass change due to SiCl₄ reduction was estimated. Then, the current efficiency for Si electrodeposition at various potentials was evaluated. The calculated current efficiency was almost 100% when it was assumed that SiCl₄ reduction progressed by four-electron electroreduction. The XPS and Raman results showed that the deposited films were composed primarily of amorphous Si with Si-Si bonds. Crystalline Si thin films were obtained after annealing in an Ar gas stream.

Original language	English
Pages (from-to)	49-55
Number of pages	7
Journal	Electrochimica Acta
Volume	183
DOIs	https://doi.org/10.1016/j.electacta.2015.04.167
Publication status	Published - 2015 Nov 20

Keywords

EQCM
Si electrodeposition
XPS
annealing
ionic liquids

ASJC Scopus subject areas

Chemical Engineering(all)
Electrochemistry

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10.1016/j.electacta.2015.04.167

Cite this

@article{41f73f7f0abb41cdb1b6213d77eb4273,

title = "Electrochemical quartz crystal microbalance, X-ray photoelectron spectroscopy, and Raman spectroscopy analysis of SiCl4 reduction in ionic liquids",

abstract = "The reaction mechanism of Si electrodeposition in the ionic liquid trimethyl-n-hexylammonium bis(trifluoromethylsulfonyl) imide (TMHATFSI) with SiCl4 was investigated using an electrochemical quartz crystal microbalance (EQCM) and X-ray photoelectron spectroscopy (XPS). The deposited films were further characterized by Raman spectroscopy. The EQCM method measured the frequency change in situ during electrodeposition, whereas XPS provided the Si mass concentration in the electrodeposited films. By combining these results, the mass change due to SiCl4 reduction was estimated. Then, the current efficiency for Si electrodeposition at various potentials was evaluated. The calculated current efficiency was almost 100% when it was assumed that SiCl4 reduction progressed by four-electron electroreduction. The XPS and Raman results showed that the deposited films were composed primarily of amorphous Si with Si-Si bonds. Crystalline Si thin films were obtained after annealing in an Ar gas stream.",

keywords = "EQCM, Si electrodeposition, XPS, annealing, ionic liquids",

author = "Yasuhiro Tsuyuki and {Pham Huynh}, {Tram Anh} and Jason Komadina and Yasuhiro Fukunaka and Takayuki Homma",

note = "Funding Information: The authors thank Mr. T. Nishida for his helpful cooperation and acknowledge the Leading Graduate Program in Science and Engineering, Waseda University, from MEXT, Japan . This study was financially supported in part by the Japan Science and Technology Agency (JST) CREST program . Publisher Copyright: {\textcopyright} 2015 Elsevier Ltd. All rights reserved.",

year = "2015",

month = nov,

day = "20",

doi = "10.1016/j.electacta.2015.04.167",

language = "English",

volume = "183",

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journal = "Electrochimica Acta",

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T1 - Electrochemical quartz crystal microbalance, X-ray photoelectron spectroscopy, and Raman spectroscopy analysis of SiCl4 reduction in ionic liquids

AU - Tsuyuki, Yasuhiro

AU - Pham Huynh, Tram Anh

AU - Komadina, Jason

AU - Fukunaka, Yasuhiro

AU - Homma, Takayuki

N1 - Funding Information: The authors thank Mr. T. Nishida for his helpful cooperation and acknowledge the Leading Graduate Program in Science and Engineering, Waseda University, from MEXT, Japan . This study was financially supported in part by the Japan Science and Technology Agency (JST) CREST program . Publisher Copyright: © 2015 Elsevier Ltd. All rights reserved.

PY - 2015/11/20

Y1 - 2015/11/20

N2 - The reaction mechanism of Si electrodeposition in the ionic liquid trimethyl-n-hexylammonium bis(trifluoromethylsulfonyl) imide (TMHATFSI) with SiCl4 was investigated using an electrochemical quartz crystal microbalance (EQCM) and X-ray photoelectron spectroscopy (XPS). The deposited films were further characterized by Raman spectroscopy. The EQCM method measured the frequency change in situ during electrodeposition, whereas XPS provided the Si mass concentration in the electrodeposited films. By combining these results, the mass change due to SiCl4 reduction was estimated. Then, the current efficiency for Si electrodeposition at various potentials was evaluated. The calculated current efficiency was almost 100% when it was assumed that SiCl4 reduction progressed by four-electron electroreduction. The XPS and Raman results showed that the deposited films were composed primarily of amorphous Si with Si-Si bonds. Crystalline Si thin films were obtained after annealing in an Ar gas stream.

AB - The reaction mechanism of Si electrodeposition in the ionic liquid trimethyl-n-hexylammonium bis(trifluoromethylsulfonyl) imide (TMHATFSI) with SiCl4 was investigated using an electrochemical quartz crystal microbalance (EQCM) and X-ray photoelectron spectroscopy (XPS). The deposited films were further characterized by Raman spectroscopy. The EQCM method measured the frequency change in situ during electrodeposition, whereas XPS provided the Si mass concentration in the electrodeposited films. By combining these results, the mass change due to SiCl4 reduction was estimated. Then, the current efficiency for Si electrodeposition at various potentials was evaluated. The calculated current efficiency was almost 100% when it was assumed that SiCl4 reduction progressed by four-electron electroreduction. The XPS and Raman results showed that the deposited films were composed primarily of amorphous Si with Si-Si bonds. Crystalline Si thin films were obtained after annealing in an Ar gas stream.

KW - EQCM

KW - Si electrodeposition

KW - XPS

KW - annealing

KW - ionic liquids

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