Room-temperature synthesis of tungsten silicide powders using various initial systems

Didem Ovalı; Duygu Ağaoğulları; M. Lütfi Öveçoğlu

doi:10.1016/j.ijrmhm.2019.03.028

Room-temperature synthesis of tungsten silicide powders using various initial systems

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

7 Citations (Scopus)

Abstract

The present study investigated the synthesis of tungsten silicide powders using ternary (WO ₃ -Si-Mg and W-SiO ₂ -Mg) and binary (W-Si) initial systems at room temperature via mechanochemical synthesis (MCS) and mechanical alloying (MA) processes. Milling time was used as a process parameter. Subsequently, undesired Mg-based phases were leached out using aqueous HCl solution. Compositional analyses of powders were conducted by using an X-ray diffractometer (XRD) and Fourier transform infrared spectrometer (FTIR). Microstructural observations of powders were performed by utilizing particle size analyzer (PSA), scanning (SEM) and transmission electron microscopes (TEM). Also, differential scanning calorimetry (DSC) analyses were carried out for the synthesized powders. While the reaction for tungsten silicide formation took place by MCS in WO ₃ -Si-Mg system after 1 min and by MA in W-Si system after 15 h, it did not occur in W-SiO ₂ -Mg system even after 15 h milling. WSi ₂ , W ₅ Si ₃ and W phases were found in WO ₃ -Si-Mg system whereas only WSi ₂ formed in W-Si system. The ternary WO ₃ -Si-Mg system resulted in SiO ₂ coated nanoparticles owning a mean size of 203 nm. WSi ₂ submicron particles with an average size of 688 nm were obtained in binary W-Si system. The experimental results showed a good consistency with the reaction mechanisms predicted by FactSage™ thermodynamic calculations.

Original language	English
Pages (from-to)	58-68
Number of pages	11
Journal	International Journal of Refractory Metals and Hard Materials
Volume	82
DOIs	https://doi.org/10.1016/j.ijrmhm.2019.03.028
Publication status	Published - Aug 2019

Bibliographical note

Publisher Copyright:
© 2019 Elsevier Ltd

Funding

The authors acknowledge the Scientific and Technological Research Council of Turkey (TÜBİTAK, Project No: 216M070 ) for supporting this research. The authors would like to thank Assoc. Prof. Dr. Bora Derin for Factsage™ thermodynamic calculations and Selçuk University Advanced Technology Research & Application Center (İLTEK) for TEM investigations.

Funders	Funder number
TÜBİTAK	216M070
Türkiye Bilimsel ve Teknolojik Araştirma Kurumu

Keywords

Electron microscopy
Mechanical alloying
Mechanochemical synthesis
Metal oxides
Silicides

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10.1016/j.ijrmhm.2019.03.028

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title = "Room-temperature synthesis of tungsten silicide powders using various initial systems",

abstract = " The present study investigated the synthesis of tungsten silicide powders using ternary (WO 3 -Si-Mg and W-SiO 2 -Mg) and binary (W-Si) initial systems at room temperature via mechanochemical synthesis (MCS) and mechanical alloying (MA) processes. Milling time was used as a process parameter. Subsequently, undesired Mg-based phases were leached out using aqueous HCl solution. Compositional analyses of powders were conducted by using an X-ray diffractometer (XRD) and Fourier transform infrared spectrometer (FTIR). Microstructural observations of powders were performed by utilizing particle size analyzer (PSA), scanning (SEM) and transmission electron microscopes (TEM). Also, differential scanning calorimetry (DSC) analyses were carried out for the synthesized powders. While the reaction for tungsten silicide formation took place by MCS in WO 3 -Si-Mg system after 1 min and by MA in W-Si system after 15 h, it did not occur in W-SiO 2 -Mg system even after 15 h milling. WSi 2 , W 5 Si 3 and W phases were found in WO 3 -Si-Mg system whereas only WSi 2 formed in W-Si system. The ternary WO 3 -Si-Mg system resulted in SiO 2 coated nanoparticles owning a mean size of 203 nm. WSi 2 submicron particles with an average size of 688 nm were obtained in binary W-Si system. The experimental results showed a good consistency with the reaction mechanisms predicted by FactSage{\texttrademark} thermodynamic calculations.",

keywords = "Electron microscopy, Mechanical alloying, Mechanochemical synthesis, Metal oxides, Silicides",

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

note = "Publisher Copyright: {\textcopyright} 2019 Elsevier Ltd",

year = "2019",

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doi = "10.1016/j.ijrmhm.2019.03.028",

language = "English",

volume = "82",

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AU - Ovalı, Didem

AU - Ağaoğulları, Duygu

AU - Öveçoğlu, M. Lütfi

PY - 2019/8

Y1 - 2019/8

N2 - The present study investigated the synthesis of tungsten silicide powders using ternary (WO 3 -Si-Mg and W-SiO 2 -Mg) and binary (W-Si) initial systems at room temperature via mechanochemical synthesis (MCS) and mechanical alloying (MA) processes. Milling time was used as a process parameter. Subsequently, undesired Mg-based phases were leached out using aqueous HCl solution. Compositional analyses of powders were conducted by using an X-ray diffractometer (XRD) and Fourier transform infrared spectrometer (FTIR). Microstructural observations of powders were performed by utilizing particle size analyzer (PSA), scanning (SEM) and transmission electron microscopes (TEM). Also, differential scanning calorimetry (DSC) analyses were carried out for the synthesized powders. While the reaction for tungsten silicide formation took place by MCS in WO 3 -Si-Mg system after 1 min and by MA in W-Si system after 15 h, it did not occur in W-SiO 2 -Mg system even after 15 h milling. WSi 2 , W 5 Si 3 and W phases were found in WO 3 -Si-Mg system whereas only WSi 2 formed in W-Si system. The ternary WO 3 -Si-Mg system resulted in SiO 2 coated nanoparticles owning a mean size of 203 nm. WSi 2 submicron particles with an average size of 688 nm were obtained in binary W-Si system. The experimental results showed a good consistency with the reaction mechanisms predicted by FactSage™ thermodynamic calculations.

AB - The present study investigated the synthesis of tungsten silicide powders using ternary (WO 3 -Si-Mg and W-SiO 2 -Mg) and binary (W-Si) initial systems at room temperature via mechanochemical synthesis (MCS) and mechanical alloying (MA) processes. Milling time was used as a process parameter. Subsequently, undesired Mg-based phases were leached out using aqueous HCl solution. Compositional analyses of powders were conducted by using an X-ray diffractometer (XRD) and Fourier transform infrared spectrometer (FTIR). Microstructural observations of powders were performed by utilizing particle size analyzer (PSA), scanning (SEM) and transmission electron microscopes (TEM). Also, differential scanning calorimetry (DSC) analyses were carried out for the synthesized powders. While the reaction for tungsten silicide formation took place by MCS in WO 3 -Si-Mg system after 1 min and by MA in W-Si system after 15 h, it did not occur in W-SiO 2 -Mg system even after 15 h milling. WSi 2 , W 5 Si 3 and W phases were found in WO 3 -Si-Mg system whereas only WSi 2 formed in W-Si system. The ternary WO 3 -Si-Mg system resulted in SiO 2 coated nanoparticles owning a mean size of 203 nm. WSi 2 submicron particles with an average size of 688 nm were obtained in binary W-Si system. The experimental results showed a good consistency with the reaction mechanisms predicted by FactSage™ thermodynamic calculations.

KW - Electron microscopy

KW - Mechanical alloying

KW - Mechanochemical synthesis

KW - Metal oxides

KW - Silicides

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VL - 82

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JO - International Journal of Refractory Metals and Hard Materials

JF - International Journal of Refractory Metals and Hard Materials

ER -

Room-temperature synthesis of tungsten silicide powders using various initial systems

Abstract

Bibliographical note

Funding

Keywords

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