TY - JOUR
T1 - Molten-salt synthesis of manganese-doped intermetallic TiFexMn(1−x) nanoparticles from oxide precursors
AU - Kobayashi, Yasukazu
AU - Yamaoka, Shohei
AU - Nakagawa, Shinichiro
AU - Hanada, Nobuko
N1 - Funding Information:
We acknowledge the Advanced Characterization Nanotechnology Platform of the University of Tokyo. The authors thank Prof. Suguru Noda at Waseda University for his support in SEM-EDS measurement. This study was supported by JSPS KAKENHI Grant Number 21K14465. The authors thank Mr. Takahiro Gotoh at the Materials Characterization Central Laboratory at Waseda University for TEM observation under the MEXT Project for promoting public utilization of advanced research infrastructure (Program for supporting construction of core facilities, Grant Number JPMXS0440500021). The authors thank Sumire Miyakoshi, Waseda University for TEM observation. The authors thank Ryota Zukeran at Waseda University for the measurement of hydrogen storage properties. The authors thank Masanao Narita at Renewable Energy Research Centre, National Institute of Advanced Industrial Science and Technology for some SEM observations.
Funding Information:
We acknowledge the Advanced Characterization Nanotechnology Platform of the University of Tokyo. The authors thank Prof. Suguru Noda at Waseda University for his support in SEM-EDS measurement. This study was supported by JSPS KAKENHI Grant Number 21K14465 . The authors thank Mr. Takahiro Gotoh at the Materials Characterization Central Laboratory at Waseda University for TEM observation under the MEXT Project for promoting public utilization of advanced research infrastructure (Program for supporting construction of core facilities, Grant Number JPMXS0440500021 ). The authors thank Sumire Miyakoshi, Waseda University for TEM observation. The authors thank Ryota Zukeran at Waseda University for the measurement of hydrogen storage properties. The authors thank Masanao Narita at Renewable Energy Research Centre, National Institute of Advanced Industrial Science and Technology for some SEM observations.
Publisher Copyright:
© 2023 Elsevier B.V.
PY - 2023/4/25
Y1 - 2023/4/25
N2 - Manganese-doped intermetallic TiFexMn(1−x) nanoparticles (NPs) were synthesized by a molten-salt synthesis method using TiO2, FeSO4•7H2O, and Mn(NO3)2•6H2O as the raw materials. The Ti–Fe–Mn oxide precursors prepared from the raw materials were efficiently reduced at temperatures as low as 600 °C in molten LiCl in the presence of CaH2 as the reducing agent. This resulted in the formation of TiFexMn(1−x) NPs exhibiting few impurities (e.g., TiFe2 or/and TiFe39). Increase in the Mn content led to peak shifts in the X-ray diffraction (XRD) patterns, indicating good incorporation of Mn into the cubic CsCl-type structure of intermetallic TiFe to form a solid solution. Nano-sized particles of< 100 nm were clearly observed in the obtained powders by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Moreover, homogeneous distribution of the constituent elements (i.e., Ti, Fe, and Mn) was confirmed by energy dispersive X-ray (EDX) spectroscopy. Finally, the hydrogen absorption properties of the prepared TiFe0.7Mn0.3 NPs were analyzed. Notably, with the exception of micron-sized TiFe0.7Mn0.3 prepared by common arc melting, the generated NPs exhibited almost no hydrogen absorption. The results obtained herein demonstrated the importance of particle size in activating TiFe-based hydrogen absorption materials.
AB - Manganese-doped intermetallic TiFexMn(1−x) nanoparticles (NPs) were synthesized by a molten-salt synthesis method using TiO2, FeSO4•7H2O, and Mn(NO3)2•6H2O as the raw materials. The Ti–Fe–Mn oxide precursors prepared from the raw materials were efficiently reduced at temperatures as low as 600 °C in molten LiCl in the presence of CaH2 as the reducing agent. This resulted in the formation of TiFexMn(1−x) NPs exhibiting few impurities (e.g., TiFe2 or/and TiFe39). Increase in the Mn content led to peak shifts in the X-ray diffraction (XRD) patterns, indicating good incorporation of Mn into the cubic CsCl-type structure of intermetallic TiFe to form a solid solution. Nano-sized particles of< 100 nm were clearly observed in the obtained powders by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Moreover, homogeneous distribution of the constituent elements (i.e., Ti, Fe, and Mn) was confirmed by energy dispersive X-ray (EDX) spectroscopy. Finally, the hydrogen absorption properties of the prepared TiFe0.7Mn0.3 NPs were analyzed. Notably, with the exception of micron-sized TiFe0.7Mn0.3 prepared by common arc melting, the generated NPs exhibited almost no hydrogen absorption. The results obtained herein demonstrated the importance of particle size in activating TiFe-based hydrogen absorption materials.
KW - Chemical synthesis
KW - Hydrogen absorption
KW - Intermetallic TiFeMn
KW - Nanoparticles
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U2 - 10.1016/j.jallcom.2023.168996
DO - 10.1016/j.jallcom.2023.168996
M3 - Article
AN - SCOPUS:85146844741
SN - 0925-8388
VL - 941
JO - Journal of the Less-Common Metals
JF - Journal of the Less-Common Metals
M1 - 168996
ER -