研究目的
To determine the dominating synthesis parameters for producing Gd2O3 nanopowders with physiochemical properties suitable for applications in gas sensing devices, SOFCs, and MRI.
研究成果
Pure cubic phase Gd2O3 nanopowders were successfully synthesized with optimal conditions at 40 °C co-precipitation for 1 h and 650 °C calcination for 4 h, yielding small crystallite sizes (16.54 nm) and high surface area (9.16 m2/g). The method is feasible for industrial applications.
研究不足
The study is limited to specific synthesis conditions and may not cover all possible parameters. Agglomeration increases with higher temperatures and durations, which could affect material properties. Industrial scalability and long-term stability were not fully addressed.
1：Experimental Design and Method Selection:
A co-precipitation method followed by calcination was used to synthesize Gd2O3 nanopowders. Gadolinium nitrate hexahydrate and di-ammonium oxalate monohydrate were reacted in a distillate pack system with ethylene glycol, using a reverse-strike method at controlled temperatures and durations. The precipitate was centrifuged, washed, dried, and calcined in a tubular furnace.
2：Sample Selection and Data Sources:
Samples were prepared by varying co-precipitation temperatures (27-100 °C), durations (0.5-3 h), calcination temperatures (500-800 °C), and durations (2-8 h).
3：5-3 h), calcination temperatures (500-800 °C), and durations (2-8 h). List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment includes a magnetic hot plate stirrer, tubular furnace (MTI Corporation GSL-1100X), thermogravimetric analyser (TGA Q50, TA Instruments), FESEM (Hitachi SU8010), TEM (FEI Tecnai G220 S-Twin), FTIR spectrometer (Nicolet iS10), XRD (Bruker D8 Advance), Raman microscope (Reinshaw inVia), and BET analyser (Micrometrics ASAP2020). Materials include gadolinium nitrate hexahydrate, di-ammonium oxalate monohydrate, ethylene glycol, distilled water.
4：0). Materials include gadolinium nitrate hexahydrate, di-ammonium oxalate monohydrate, ethylene glycol, distilled water. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Reactants were dissolved, mixed in a flask submerged in an oil bath, dripped at 3 mL/min, reacted for specified times, centrifuged at 4000 rpm for 10 min, washed, dried at 60 °C, and calcined at 2 °C/min heating rate.
5：Data Analysis Methods:
Data were analyzed using Scherrer equation for crystallite size from XRD, BET for surface area, and various spectroscopic methods for phase and structural analysis.
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Field Emission Scanning Electron Microscope
SU8010
Hitachi
Analysis of microstructural morphology of as-synthesized nanopowders.
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Transmission Electron Microscope
Tecnai G220 S-Twin
FEI
High-resolution microscopy to understand morphology of Gd2O3 nanopowders.
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X-Ray Diffractometer
D8 Advance
Bruker
X-ray diffraction analysis to examine crystallinity and average crystallite size.
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Thermogravimetric Analyser
TGA Q50
TA Instruments
Used to determine the decomposition temperature of the dried co-precipitated Gd2(C2O4)3 precursor.
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Fourier Transform Infrared Spectrometer
iS10
Nicolet
Obtain IR spectra to reveal chemical structures and functional groups.
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Raman Microscope
inVia Confocal
Reinshaw
Obtain Raman spectra to affirm phase structure of specimen.
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BET Analyser
ASAP2020
Micrometrics
Pore size and specific surface area analyses.
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Tubular Furnace
GSL-1100X
MTI Corporation
Calcination of precursors to obtain Gd2O3 nanopowder.
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