研究目的
To synthesize and characterize pure nanocrystalline BaSnO3 using two different milling activation processes (mechanical activation via planetary ball milling and mechanical mixing in agate mortar) followed by sintering, and to analyze phase formation, crystallite size, bond characteristics, optical properties, and morphology.
研究成果
Pure nanocrystalline BaSnO3 with a cubic perovskite structure and crystallite size around 50 nm was successfully synthesized using both milling methods. FTIR confirmed bond vibrations and minor BaCO3 presence, UV-VIS showed absorption in UV region with band gaps of 2-2.78 eV (indirect) and 2.78-3.14 eV (direct), and SEM revealed morphological differences with agglomerations. EDX confirmed elemental composition. Both methods are effective, with mechanochemical activation not significantly altering crystallite size compared to simple mixing.
研究不足
The study is limited to pure BaSnO3 without doping; potential contamination from atmospheric CO2 affecting FTIR results; differences in morphology due to milling methods but similar crystallite sizes; no comparison with other synthesis methods like sol-gel or hydrothermal processes.
1：Experimental Design and Method Selection:
Two physical routes were used: mechanical activation with high energy planetary ball milling and mechanical mixing in an agate mortar, both followed by sintering at 1350 °C for 2 hours in an oxidizing atmosphere.
2：Sample Selection and Data Sources:
Stoichiometric amounts of BaCO3 and SnO2 (from Merck India, Ltd.) were used as precursors.
3：List of Experimental Equipment and Materials:
High energy planetary ball mill (Fritsch Pulverisette 5), zirconia balls, toluene, agate mortar pestle, tubular furnace, X-ray diffractometer (Rigaku Ultima III), FTIR spectrometer (Shimadzu IR-21 Prestige), UV-VIS spectrophotometer (Perkin Elmer Lambda35), SEM with EDX (INCAX, Oxford Instruments), ultrasonicator, steel die, KBr, Pt-Rh sputtering coater (JEOL JFC-1600 Auto fine coater).
4：Experimental Procedures and Operational Workflow:
For mechanical activation, milling at 200 rpm for 8 hours with ball-to-powder ratio of 10:1, drying, and sintering. For mechanical mixing, hand mixing for 3 hours, decomposition of BaCO3 at 1250 °C for 1 hour to get BaO, mixing with SnO2, and sintering. XRD scans from 10-80° at 5°/min, FTIR scans from 5000-400 cm?1, UV-VIS scans from 150-750 nm, SEM imaging after Pt-Rh coating.
5：Data Analysis Methods:
Crystallite size calculated using Scherrer's formula from XRD data, band gap calculated using Tauc relation from UV-VIS data, elemental analysis via EDX.
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