Abstract

In this study, a mixture of magnesium oxide and titanium dioxide was mechanically activated in order to investigate the possibility of mechanochemical synthesis of magnesium titanate. Mechanical activation was performed for 1000 min in a high-energy vibro mill (type MH954/3, KHD Humboldt Wedag AG, Germany). The mill is equipped with housing having a horizontally placed shutter. The cylindrical stainless steel working vessel, with inner dimensions of 40 mm in height and 170 mm in diameter, has working elements consisting of two free concentric stainless steel rings with a total weight of 3 kg. The engine power is 0.8 kW. Respecting the optimal amount of powder to be activated of 50-150 g and the stoichiometric ratio of the reactants in the equation presenting the chemical reaction of magnesium titanate synthesis, the starting amounts were 20.2 g (0.5 mol) of MgO and 39.9 g (0.5 mol) TiO2. During the experiments, X-ray diffraction analysis of the samples taken from the reaction system after 60, 180, 330, and 1000 min of mechanical activation was performed. Atomic absorption spectrophotometry was used for chemical composition analysis of samples taken at different activation times. Based on the X-ray diffraction analysis results, it can be concluded that the greatest changes in the system took place at the very beginning of the mechanical activation due to the disturbance of the crystal structure of the initial components. X-ray diffraction analysis of the sample after 1000 min of activation showed complete amorphization of the mixture, but diffraction maxima characteristic for magnesium titanate were not identified. Therefore, the mechanical activation experiments were stopped. Evidently, the energy input was not sufficient to overcome the energy barrier to form a new chemical compound - magnesium titanate. The failure to synthesize magnesium titanate is explained by the low negative Gibbs energy value of -25.8 kJ/mol (despite the theoretical possibility that the reaction will happen), as well as by the amount of mechanical energy entered into the system during activation which was insufficient to obtain the reaction product. Although the synthesis of MgTiO3 was not achieved, significant results were obtained which identify models for further investigations of the possibility of mechanochemical reactions of alkaline earth metals and titanium dioxide.

Highlights

  • Hemijska analiza reaktanata i uzoraka iz reakcionog sistema tokom mehaničke reakcije vršena je metodom atomske apsorpcione spektrofotometrije na atomskom adsorpcionom spektrofotometru (AAS) Analyst 300

  • Rendgenostrukturna analiza reaktanata i uzoraka iz reakcionog sistema tokom mehaničke aktivacije vršena je na PHILIPS PW-1700 automatizovanom difraktometru sa bakarnom cevi koji radi na 40 kV

  • Imajući u vidu prikazane vrednosti slobodne Gibsove energije, prema kojima je sintezu titanata ostalih zemnoalkalnih metala lakše ostvariti u odnosu na magnezijum titanat, dalja istraživanja će se izvršiti u vibro mlinu sa većom snagom motora i istim parametrima težine prstenova, kao i u planetarnom mlinu, a u funkciji odnosa mase kuglica i mase unetog materijala (MgO i TiO2) u vidu smeše prahova, kako bi mehanička energija koju sistemu predaje primenjeni tip mlina bila dovoljna za prevazilaženje energetske barijere i za dobijanje magnezijum titanata

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Summary

EKSPERIMENTALNI DEO

Za eksperimentalna ispitivanja u ovom radu upotrebljen je magnezijum oksid, MgO, kao bazni reaktant i titanijum dioksid, TiO2, kao kiseli reaktant. Hemijska analiza reaktanata i uzoraka iz reakcionog sistema tokom mehaničke reakcije vršena je metodom atomske apsorpcione spektrofotometrije na atomskom adsorpcionom spektrofotometru (AAS) Analyst 300 (proizvođač ”Perkin Elmer”- SAD). Pri čemu je kao rastvarač korišćen 10 % rastvor sirćetne kiseline (99,5 % glacijalna sirćetna kiselina, Zorka Pharma, Hemija – DOO, Srbija). Rendgenostrukturna analiza reaktanata i uzoraka iz reakcionog sistema tokom mehaničke aktivacije vršena je na PHILIPS PW-1700 automatizovanom difraktometru (proizvođač ”Philips”, Holandija) sa bakarnom cevi koji radi na 40 kV i 35 mA. Mehanohemijska aktivacija je u okviru eksperimentalne procedure obavljena jedanput, dok su uzorci za hemijsku analizu uzimana po 2 uzorka za analizu na atomskom adsorpcionom spektrofotometru (AAS) Analyst 300 (proizvođač ”Perkin Elmer”- SAD) pri čemu je kao rastvarač korišćen 10 % rastvor sirćetne kiseline (99,5 % glacijalna sirćetna kiselina, Zorka Pharma, Hemija – DOO., Srbija)

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