Mechanochemical synthesis and characterisation of niobium silicide nanoparticles

Didem Ovalı; Duygu Ağaoğulları; M. Lütfi Öveçoğlu

doi:10.1016/j.ceramint.2019.02.135

Mechanochemical synthesis and characterisation of niobium silicide nanoparticles

Didem Ovalı^*, Duygu Ağaoğulları, M. Lütfi Öveçoğlu

^*Corresponding author for this work

Department of Metallurgical and Materials Engineering

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

9 Citations (Scopus)

Abstract

Mechanochemical synthesis (MCS) investigations of niobium silicide powders in Nb ₂ O ₅ –]SiO ₂ –]Mg powder mixtures were conducted via high-energy ball milling and leaching by means of process parameters such as the milling duration, initial Nb ₂ O ₅ crystal structure, and excess Mg amount. The compositional, thermal, and microstructural properties of the products were characterised using X-ray diffractometry (XRD), Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), particle size analysis (PSA), stereomicroscopy (SM), scanning electron microscopy (SEM), and transmission electron microscopy/energy-dispersive spectrometry (TEM/EDS). After the 5 h milling of the stoichiometric mixtures, an instantaneous ignition occurred and NbSi ₂ , Nb ₅ Si ₃ , Nb, and MgO phases formed with some residual Mg. In addition, the use of excess Mg inhibited the formation of Nb ₅ Si ₃ . Afterwards, leaching treatments (in a 4 M HCl solution) completely removed the Mg-based phases from the synthesised products. The XRD calculations revealed that the resultant product consisted of 97 wt% NbSi ₂ and 3 wt% Nb ₅ Si ₃ phases. The TEM analyses indicated that each Nb silicide nanoparticle was coated with a SiO ₂ layer. According to random measurements, the average particle size of the Nb silicide cores and average thickness of the SiO ₂ layer were approximately 61 and 7.5 nm, respectively.

Original language	English
Pages (from-to)	10654-10663
Number of pages	10
Journal	Ceramics International
Volume	45
Issue number	8
DOIs	https://doi.org/10.1016/j.ceramint.2019.02.135
Publication status	Published - 1 Jun 2019

Bibliographical note

Publisher Copyright:
© 2019 Elsevier Ltd and Techna Group S.r.l.

Funding

This study was financed by The Scientific and Technological Research Council of Turkey (project # 216M070 ). The authors would like to thank the Advanced Technology Research & Application Center at Selçuk University (İLTEK) for the TEM analyses. This study was financed by The Scientific and Technological Research Council of Turkey (project # 216M070). The authors would like to thank the Advanced Technology Research & Application Center at Sel?uk University (?LTEK) for the TEM analyses.

Funders	Funder number
Sel?uk University
Türkiye Bilimsel ve Teknolojik Araştirma Kurumu	216M070

Keywords

Electron microscopy
Powders: solid state reaction
Silicides
Transition metal oxides

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10.1016/j.ceramint.2019.02.135

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title = "Mechanochemical synthesis and characterisation of niobium silicide nanoparticles",

abstract = " Mechanochemical synthesis (MCS) investigations of niobium silicide powders in Nb 2 O 5 –]SiO 2 –]Mg powder mixtures were conducted via high-energy ball milling and leaching by means of process parameters such as the milling duration, initial Nb 2 O 5 crystal structure, and excess Mg amount. The compositional, thermal, and microstructural properties of the products were characterised using X-ray diffractometry (XRD), Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), particle size analysis (PSA), stereomicroscopy (SM), scanning electron microscopy (SEM), and transmission electron microscopy/energy-dispersive spectrometry (TEM/EDS). After the 5 h milling of the stoichiometric mixtures, an instantaneous ignition occurred and NbSi 2 , Nb 5 Si 3 , Nb, and MgO phases formed with some residual Mg. In addition, the use of excess Mg inhibited the formation of Nb 5 Si 3 . Afterwards, leaching treatments (in a 4 M HCl solution) completely removed the Mg-based phases from the synthesised products. The XRD calculations revealed that the resultant product consisted of 97 wt\% NbSi 2 and 3 wt\% Nb 5 Si 3 phases. The TEM analyses indicated that each Nb silicide nanoparticle was coated with a SiO 2 layer. According to random measurements, the average particle size of the Nb silicide cores and average thickness of the SiO 2 layer were approximately 61 and 7.5 nm, respectively.",

keywords = "Electron microscopy, Powders: solid state reaction, Silicides, Transition metal oxides",

author = "Didem Ovalı and Duygu Ağaoğulları and {\"O}ve{\c c}oğlu, \{M. L{\"u}tfi\}",

note = "Publisher Copyright: {\textcopyright} 2019 Elsevier Ltd and Techna Group S.r.l.",

year = "2019",

month = jun,

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doi = "10.1016/j.ceramint.2019.02.135",

language = "English",

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T1 - Mechanochemical synthesis and characterisation of niobium silicide nanoparticles

AU - Ovalı, Didem

AU - Ağaoğulları, Duygu

AU - Öveçoğlu, M. Lütfi

PY - 2019/6/1

Y1 - 2019/6/1

N2 - Mechanochemical synthesis (MCS) investigations of niobium silicide powders in Nb 2 O 5 –]SiO 2 –]Mg powder mixtures were conducted via high-energy ball milling and leaching by means of process parameters such as the milling duration, initial Nb 2 O 5 crystal structure, and excess Mg amount. The compositional, thermal, and microstructural properties of the products were characterised using X-ray diffractometry (XRD), Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), particle size analysis (PSA), stereomicroscopy (SM), scanning electron microscopy (SEM), and transmission electron microscopy/energy-dispersive spectrometry (TEM/EDS). After the 5 h milling of the stoichiometric mixtures, an instantaneous ignition occurred and NbSi 2 , Nb 5 Si 3 , Nb, and MgO phases formed with some residual Mg. In addition, the use of excess Mg inhibited the formation of Nb 5 Si 3 . Afterwards, leaching treatments (in a 4 M HCl solution) completely removed the Mg-based phases from the synthesised products. The XRD calculations revealed that the resultant product consisted of 97 wt% NbSi 2 and 3 wt% Nb 5 Si 3 phases. The TEM analyses indicated that each Nb silicide nanoparticle was coated with a SiO 2 layer. According to random measurements, the average particle size of the Nb silicide cores and average thickness of the SiO 2 layer were approximately 61 and 7.5 nm, respectively.

AB - Mechanochemical synthesis (MCS) investigations of niobium silicide powders in Nb 2 O 5 –]SiO 2 –]Mg powder mixtures were conducted via high-energy ball milling and leaching by means of process parameters such as the milling duration, initial Nb 2 O 5 crystal structure, and excess Mg amount. The compositional, thermal, and microstructural properties of the products were characterised using X-ray diffractometry (XRD), Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), particle size analysis (PSA), stereomicroscopy (SM), scanning electron microscopy (SEM), and transmission electron microscopy/energy-dispersive spectrometry (TEM/EDS). After the 5 h milling of the stoichiometric mixtures, an instantaneous ignition occurred and NbSi 2 , Nb 5 Si 3 , Nb, and MgO phases formed with some residual Mg. In addition, the use of excess Mg inhibited the formation of Nb 5 Si 3 . Afterwards, leaching treatments (in a 4 M HCl solution) completely removed the Mg-based phases from the synthesised products. The XRD calculations revealed that the resultant product consisted of 97 wt% NbSi 2 and 3 wt% Nb 5 Si 3 phases. The TEM analyses indicated that each Nb silicide nanoparticle was coated with a SiO 2 layer. According to random measurements, the average particle size of the Nb silicide cores and average thickness of the SiO 2 layer were approximately 61 and 7.5 nm, respectively.

KW - Electron microscopy

KW - Powders: solid state reaction

KW - Silicides

KW - Transition metal oxides

UR - https://www.scopus.com/pages/publications/85061922268

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DO - 10.1016/j.ceramint.2019.02.135

M3 - Article

AN - SCOPUS:85061922268

SN - 0272-8842

VL - 45

SP - 10654

EP - 10663

JO - Ceramics International

JF - Ceramics International

IS - 8

ER -

Mechanochemical synthesis and characterisation of niobium silicide nanoparticles

Abstract

Bibliographical note

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Keywords

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