Cryo-SEM photos and EDS data were obtained using a high-resolution scanning electron microscope with X-Ray Microanalysis and Cryo-SEM experimental facilities, namely a JSM 6301F microscope (JEOL, Ltd., Akishima, Tokyo, Japan), an INCA Energy 350 EDS spectrometer (Oxford Instruments plc, Abington, Oxfordshire, UK) and an ALTO 2500 cryo transfer system (Gantan, Pleasanton, CA, USA).
Aliquots from the reaction medium were taken at various stages of the MICROSCAFS® synthesis and rapidly cooled (by inserting them into sub-cooled nitrogen), then transferred under vacuum to the cold stage of the preparation chamber. The samples were subsequently broken and coated with Au/Pd by sputtering for 45 s before being placed into the SEM chamber and analyzed at a temperature of −150 °C.
Aliquots from the reaction medium were taken at various stages of the MICROSCAFS® synthesis and rapidly cooled (by inserting them into sub-cooled nitrogen), then transferred under vacuum to the cold stage of the preparation chamber. The samples were subsequently broken and coated with Au/Pd by sputtering for 45 s before being placed into the SEM chamber and analyzed at a temperature of −150 °C.