Highly-dispersed 1-nm SnO2 particles on GNSs are synthesized using SCCO2 process.
Tuning SCCO2 temperature affects SnO2 size, distribution, and performance.
Synchrotron ex situ XAS and XRD are used to examine electrode reaction mechanism.
Reversible conversion reaction and sluggish Sn–Na alloying reaction are observed.
First-cycle efficiency loss is mainly attributed to trapping of Na in SEI layer.