Title : Microscopy of thallium thiostibate in some organic solvents
Abstract:
0.25 g sample of sodium thiostibiat crystalline hydrate (Na3SbS4*9H2O) is dissovled in a 1:1 mixture of ethylene glycol and polyethylene glycol as the organic medium. Thallium n itrate, which is suitable for the reaction, is also dissovled in the same mixture. Both solutions are combined in a test tube and stirred with a magnetic stirrer at 343 K for 30-40 min. The mixture is then transferred to a Teflon cuvette, tightly closeed, and placed in a microwave oven. The sample is heated at 423 K for 12h. The reaction equation for the process in written as follows.
Na3SbS4 +3TlNO3 ——> Tl3SbS4 +3NaNO3
In this work, Tl3SbS4-nanocrystals were synthesized by solvotermal method in various organic solvents (ethylene glycol+polyetylene glycol). Optimal conditions for obtaining nanoparticles were determined (molar rations of the amount of components, volume ratio of the solvent, temperature, time, etc.) The crystal structere, morphology, nano-size and the obtained thallium thiostibitate nanocompound were studied usung a scanning electron micricsope (SEM). During the experinments, potassium antimonyl tartrate was used as the antimony material, and a solution of sulfur in ethylenediamine was used as the sulfide material. The synthesis of Tl3SbS4 nanoparticles was carried out by adjusting the moolare ratio of sulfur to thalliuym and controlling the volume ratios of the solvent and the organic medium (ethylene glycol+polyetylene glycol and polyvinylpyrrolidonne triethanolamine+dimethylformamide). The process was carried out at a tempereature of 383-393K for 12 hours, and thallium-thiostibate nanoparticles were synthesized with a viled of 89%. The results of scanning electron microscopy analysis showed that the synthesized thalliuym thiostibitate nanoparticles had various shapes (wine-line, oval, quadrangular, triangular, spherial shapes etc.) and their sizes ranged from 180 to 400nm. The size of Tl3SbS4 nanoparticles obtained in ethylene glycol+polyethylene glycol medium was 250-700 nm, the size Tl3SbS4 nanopartciles obtained in polyvinylpyrrolidone medium was180-350nm.
SEM analysis results showed that the synthesized Tl3SbS4 nanoparticles exhibited a variety of shapes, including oval and spherial shapes, with diameters ranging from 250-700 nm and lenghtrs up to several micrometers
In a separate experiment, dimethylformamide (DMF) and triethanolamine (TEA) were used as solvents. A new organic mixture was created by combining one part triethanolamine and two parts dimethylformamide (1:2). SEM analysis of the Tl3SbSv compound synthesized in this mixture recvealed that most of rthe particles were spherical and covered the entire surface. The particle sizes ranged from 200 to 560 nm.
Result: Tl3SbS4 nanocrystals were synthesized by solvotermal method with TlNO3 Na3SbS4 in ethylene glycol+polyetylene gylcol, polyvinypyrrolidon medium, triethanolamine+dimethylformamide medium.
