Synthesis of GaSe nanoparticles is carried out by the reaction of GaMe with trioctylphosphine selenium (TOPSe) in a high temperature solution of trioctylphosphine (TOP) and trioctylphosphine oxide (TOPO).
:GaMe + P[(CH)CH]Se → GaSe
A solution of 15 g TOPO and 5 mL TOP is heated to 150 °C overnight under nitrogen, removing any water that may be present in the original TOP solution. This initial TOP solution is vacuum distilled at 0.75 torr, taking the fraction from 204 °C to 235 °C. A TOPSe solution (12.5 mL TOP with 1.579 g TOPSe) is then added and the TOPO/TOP/TOPSe reaction mixture is heated to 278 °C. GaMe (0.8 mL) dissolved in 7.5 mL distilled TOP is then injected. After injection, the temperature drops to 254 °C before stabilizing in the range of 266–268 °C after 10 minutes. GaSe nanoparticles then begin to form, and may be detected by a shoulder in the optical absorption spectrum in the 400–450 nm range. After this shoulder is observed, the reaction mixture is left to cool to room temperature to prevent further reaction. After synthesis and cooling, the reaction vessel is opened and extraction of the GaSe nanoparticle solution is accomplished by addition of methanol. The distribution of nanoparticles between the polar (methanol) and non-polar (TOP) phases depends on experimental conditions. If the mixture is very dry, nanoparticles partition into the methanol phase. If the nanoparticles are exposed to air or water, however, the particles become uncharged and become partitioned into the non-polar TOP phase.