研究目的
The synthesis of zirconia nanoparticles through a modified facile sol–gel route and the analysis of their structural phase transition with annealing temperatures.
研究成果
The study successfully synthesized zirconia nanoparticles through a modified sol–gel route, observing a phase transition from tetragonal to monoclinic with increasing annealing temperatures. The optical energy gap was found to decrease with increasing temperature. The findings contribute to the understanding of zirconia nanoparticles' structural and optical properties.
研究不足
The study did not detect the cubic phase within the annealing temperature range. The particle size calculated from XRD was smaller than that observed in TEM images, indicating agglomeration.
1:Experimental Design and Method Selection:
The synthesis of zirconia nanoparticles was initiated by dissolving zirconyl nitrate hydrate in double distilled water at 60°C under vigorous stirring until a clear solution was obtained. Ammonia solution was added dropwise to form a gel, which was then washed, filtered, and dried. The dried gel was annealed at various temperatures for 2 h.
2:Sample Selection and Data Sources:
The as-prepared gel and annealed powders at different temperatures were used for analysis.
3:List of Experimental Equipment and Materials:
Zirconyl nitrate hydrate, ammonia solution, double distilled water, acetone, ultrasonic cleaner, muffle furnace, X-ray diffractometer, thermal analyzer, FTIR spectrometer, HR-TEM, scanning electron microscope with EDAX unit, UV-Visible spectrophotometer.
4:Experimental Procedures and Operational Workflow:
The gel was formed, washed, dried, and annealed at specified temperatures. The annealed powders were then characterized using various techniques to study their structural, thermal, and optical properties.
5:Data Analysis Methods:
XRD patterns were analyzed for phase identification, TGA/DTA for thermal behavior, FTIR for vibrational bands, HR-TEM for morphology, and UV-Vis for optical properties.
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transmission electron microscope
JEOL JEM-2100
JEOL
Morphology analysis of nanoparticles
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UV-Visible Spectrophotometer
Thermo Evolution 300
Thermo
Optical absorbance measurements
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zirconyl nitrate hydrate
LOBA Chemie
Starting material for the synthesis of zirconia nanoparticles
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ammonia solution
R.P.NORMAPUR
Used in the gelation process
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X-ray diffractometer
Philips PW 1710
Philips
Phase analysis of the annealed powders
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thermal analyzer
Netzsch, STA 449C
Netzsch
Thermogravimetric and differential temperature analysis
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FTIR spectrometer
NICOLET FTIR 6700
NICOLET
Analysis of vibrational bands
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scanning electron microscope
QUANTA FEG 250
QUANTA
Elemental analysis with EDAX unit
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