研究目的
To synthesize ceria nanoparticles using a modified polymer complex method and evaluate their structural and optical properties for potential applications in environmental remediation, biomedicine, gas sensing, and optoelectronics.
研究成果
The modified polymer complex method successfully synthesized CeO2 nanoparticles with controlled size and high purity. The nanoparticles exhibited a cubic fluorite structure, with energy gaps of 3.8 eV and 3.4 eV due to band transitions and defect states. High concentrations of Ce3+ ions and oxygen vacancies were confirmed, leading to promising optical properties for applications in biomedicine, gas sensing, and optoelectronics. Future work should explore other synthesis methods to achieve similar characteristics.
研究不足
The study may have limitations in controlling particle agglomeration, as high agglomeration was observed in TEM and SEM images. The synthesis parameters (pH and heat treatment) were varied, but other factors like solvent type or surfactant effects were not extensively explored. The optical properties are influenced by defects, which might vary with synthesis conditions not fully optimized.
1:Experimental Design and Method Selection:
The study used a modified polymer complex method for synthesis, involving citric acid and ethylene glycol with cerium nitrate precursor, heated and stirred, followed by pH adjustment and heat treatments. Characterization techniques included XRD, SEM, TEM, Raman, UV-Vis absorption, diffuse reflectance, photoluminescence, and XPS spectroscopies to analyze structural and optical properties.
2:Sample Selection and Data Sources:
Samples were synthesized at different pH values (e.g., pH ~1, 2, 9.1) and subjected to heat treatments at 550°C for 3 hours. A total of 17 samples were analyzed.
3:1) and subjected to heat treatments at 550°C for 3 hours. A total of 17 samples were analyzed. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included X-ray diffractometer (Pro PANalytical X’Pert X-ray), TEM (Jeol JEM-1200EX), SEM (EVO MA10, Carl Zeiss), Raman spectrometer (Thermo Scientific DXR SmartRaman), UV-Vis spectrophotometer (Thermo Scientific Genesys 6 and Jasco V-670), photoluminescence setup with Ar+ and Xenon lasers, and XPS system (SPECS with Phoibos 150 analyzer). Materials included cerium nitrate (Ce(NO3)3·6H2O, Alfa Aesar), citric acid (Merck), ethylene glycol (Mallinckrodt), ammonium hydroxide (Merck), and distilled water.
4:Experimental Procedures and Operational Workflow:
Synthesis involved mixing precursors, heating at 100°C, adjusting pH with NH4OH, high-shear treatment (Ultraturrax T50), heating to form resin, pre-calcination at 350°C, and final calcination at 550°C. Characterization steps included sample preparation (e.g., dispersion for TEM), data collection using specified instruments, and data analysis with software like Fityk, MAUD, and CasaXPS.
5:Data Analysis Methods:
Data were analyzed using Scherrer equation for crystal size, Kubelka-Munk transform for band gap, deconvolution of spectra with Gaussian functions, and XPS peak fitting for oxidation states.
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X-ray diffractometer
Pro PANalytical X’Pert X-ray
PANalytical
Used for X-ray diffraction analysis to determine crystalline phases and lattice parameters.
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Transmission electron microscope
Jeol JEM-1200EX
Jeol
Used for imaging to determine particle size and morphology.
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Scanning electron microscope
EVO MA10
Carl Zeiss
Used for imaging to determine particle size and morphology.
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Raman spectrometer
Thermo Scientific DXR SmartRaman
Thermo Scientific
Used for Raman spectroscopy to investigate disordered structures and crystal defects.
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UV-Vis spectrophotometer
Thermo Scientific Genesys 6
Thermo Scientific
Used for UV-Vis absorption spectroscopy.
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UV-Vis-NIR spectrophotometer
Jasco V-670
Jasco
Used for diffuse reflectance spectroscopy.
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Dispenser
Metrohm Dosimat 685
Metrohm
Used for adding ammonium hydroxide to the solution.
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Photoluminescence spectrometer
Horiba FluoroMax 4
Horiba
Used for photoluminescence spectroscopy.
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XPS system
SPECS with Phoibos 150 2D-DLD
SPECS
Used for X-ray photoelectron spectroscopy to analyze chemical and electronic structure.
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High-shear equipment
Ultraturrax T50
Ultraturrax
Used to remove agglomerates in the mixture.
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Oven
Haceb HL40
Haceb
Used for heat treatment of samples.
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Ar+ laser
Used as excitation source for photoluminescence spectroscopy.
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Xenon laser
Used as excitation source for photoluminescence spectroscopy.
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Flood Gun
FG 15/40-PS FG500
Used for surface charge compensation in XPS measurements.
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