in water High Pressure; stoich. amt. of salts were dissolved in the solvent, thioglycolic acid was added dropwise under stirring, 2 equiv. of thiourea was added, stirring for 30 min, teflon-lined autoclave, 160 °C for 20 h; cooling to room temp., ppt. was filtered off, washed with H2O and abs. EtOH several times, dried in vac. at 60 °C for 4 h;
in gas other Radiation; by radio frequency reactive sputtering process; H2S injected to Ar plasma, Cu/In (1:1) used as target, RF power was 100-500 W, substrate temp. changed from room to 400 °C, sputter time 5-30 min; detd. by XRD;
in neat (no solvent) mortaring of Cu(3-x)As, S and CuS, flushing of quartz ampoules with Ar, filling with this mixt., sealing, heating up to 750°C with a rateof 10 K/min, quenching; identification by X-ray diffraction;
in neat (no solvent) mortaring of Cu(3-x)As, S8 and Cu, flushing of quartz ampoules with Ar, filling with this mixt., sealing, heating up to 750°C with a rateof 10 K/min, quenching; further intermediates (As, Cu(2-x)S, β-As4 S4); identification by X-ray diffraction;
