TY - JOUR
T1 - Amphoteric SnO2 nanoparticles via pH-controlled continuous flow solvothermal synthesis
AU - Mamakhel, Aref
AU - Kløve, Magnus
AU - Bondesgaard, Martin
AU - Christiansen, Troels L.
AU - Pedersen, Steen Uttrup
AU - Skibsted, Jørgen
AU - Iversen, Bo Brummerstedt
PY - 2024/10
Y1 - 2024/10
N2 - Amphoteric oxides can be challenging to produce in phase pure form due to their sensitivity to the pH of the reaction mixture. The high-pressure, high-temperature reaction conditions of hydrothermal processes make the pH difficult to control. Here we report a simple approach to obtain nanoparticles of amphoteric oxides, where cheap metal nitrate precursors are reacted in alcohol (2-propanol) water mixtures (25 vol%:75 vol%) to maintain a neutral pH under solvothermal conditions. Phase pure SnO2 nanoparticles were synthesized in a continuous flow solvothermal reactor at 250 °C, 300 °C, 350 °C and 400 °C with sizes ranging from 3 nm to 7 nm. The nanoparticles were characterized using powder X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectroscopy, Raman spectroscopy, 119Sn MAS NMR spectroscopy, Brunauer-Emmett-Teller nitrogen adsorption, UV–VIS, and as anode material in CR2032 Li-ion battery cells. To demonstrate generality, amphoteric oxides ZnO, Bi2O3, Cr2O3 and γ-AlOOH were also synthesized.
AB - Amphoteric oxides can be challenging to produce in phase pure form due to their sensitivity to the pH of the reaction mixture. The high-pressure, high-temperature reaction conditions of hydrothermal processes make the pH difficult to control. Here we report a simple approach to obtain nanoparticles of amphoteric oxides, where cheap metal nitrate precursors are reacted in alcohol (2-propanol) water mixtures (25 vol%:75 vol%) to maintain a neutral pH under solvothermal conditions. Phase pure SnO2 nanoparticles were synthesized in a continuous flow solvothermal reactor at 250 °C, 300 °C, 350 °C and 400 °C with sizes ranging from 3 nm to 7 nm. The nanoparticles were characterized using powder X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectroscopy, Raman spectroscopy, 119Sn MAS NMR spectroscopy, Brunauer-Emmett-Teller nitrogen adsorption, UV–VIS, and as anode material in CR2032 Li-ion battery cells. To demonstrate generality, amphoteric oxides ZnO, Bi2O3, Cr2O3 and γ-AlOOH were also synthesized.
KW - Amphoteric oxides
KW - Continuous flow
KW - SnO
KW - Solvothermal synthesis
UR - http://www.scopus.com/inward/record.url?scp=85197548283&partnerID=8YFLogxK
U2 - 10.1016/j.supflu.2024.106341
DO - 10.1016/j.supflu.2024.106341
M3 - Journal article
AN - SCOPUS:85197548283
SN - 0896-8446
VL - 212
JO - Journal of Supercritical Fluids
JF - Journal of Supercritical Fluids
M1 - 106341
ER -