Tga 4000 thermogravimetric analyser

Nanoparticles were fabricated according to methods in the literature [48 (link)]: 0.20 g of bis(N-diisopropyl-N-octyldithiocarbamato) Pb(II) complex was dissolved in 4 mL oleic acid (OA) and injected into 3 g of hot hexadecylamine (HDA) at 360 °C. An initial temperature of 20–30 °C was attained for the mixture. The reaction was stabilized at 360 °C, and the process lasted for 1 h. The process was allowed to drop to 70 °C, signifying the completion of the process, and about 50 mL of methanol was used to remove excess OA and HDA. Centrifugation was used to separate the flocculent precipitate, which was redispersed with toluene. Low air pressure was used to remove solvent, giving rise to metal sulfides of OCT-PbS/HDA nanoparticles. Synthesis of OCT-PbS nanocrystals was obtained according to the study by a co-worker [49 (link)], using (PerkinElmer TGA 4000 thermogravimetric Analyser, San Jose, CA, USA ). A portion of 25 mg of the complex was loaded into an alumina pan and weight changes were recorded as a function of temperature for a 10 °C min⁻¹ temperature gradient between 30–900 °C. A purge gas of flowing nitrogen at a rate of 20 mL min⁻¹ was used. At temperatures between 360 and 900 °C, the complex end-product was converted into the residue of OCT-PbS nanoparticles from the TGA.

Experiments were performed using a TGA 4000 Thermogravimetric Analyser from PerkinElmer. Around 2–10 mg of sample were placed in a cylindrical 146 μL ceramic crucible (ID 7.18 mm, depth 4.79 mm). The TGA furnace was constantly purged with 20 mL min⁻¹ of N₂ gas. Samples were heated from 30 °C to 950 °C at a heating rate of 10  °C min⁻¹ in a stream of N₂ “reactive gas” provided directly above the sample with a flow rate of 20 mL min⁻¹. A baseline, obtained under the same conditions with empty ceramic crucibles, was subtracted from the measured thermograms.

Synthesis of SnS nanocrystals was obtained through high-temperature thermal decomposition of bis (N-1,4-Phenyl-N-Morhpo-dithiocarbamato) tin(II) complex using Perkin Elmer TGA 4000 ThermoGravimetric Analyser (TGA) (San Jose, CA, USA). About 25 mg of the complex was loaded into an alumina pan and weight changes were recorded as a function of temperature for a 10 °C min⁻¹ temperature gradient between 30–900 °C. A purge gas of flowing nitrogen at a rate of 20 mL min⁻¹ was used. At temperatures between 360 and 900 °C, the complex end product was converted into residue, which was expected for the formation of SnS nanocrystals from the residue obtained from the TGA.