研究目的
To study the photocatalysis and increase of antimicrobial properties of Fe3+ and Pb2+ co-doped ZnO nanoparticles obtained by microwave-assisted hydrothermal method.
研究成果
The microwave-assisted hydrothermal method effectively produced Fe3+ and Pb2+ co-doped ZnO nanoparticles without secondary phases. Doping introduced defects, reduced crystallite size, and altered morphology. While photocatalytic activity decreased, antimicrobial activity increased against E. coli and S. aureus, making the materials promising for antimicrobial applications despite limitations in photocatalysis.
研究不足
The co-doping reduces photocatalytic activity, which may limit applications in photocatalysis. The use of toxic Pb requires careful handling and stability checks to prevent environmental release. The method may not be scalable for industrial applications, and further optimization is needed for enhanced properties.
1:Experimental Design and Method Selection:
The study used a microwave-assisted hydrothermal method to synthesize ZnO nanoparticles co-doped with Fe3+ and Pb2+ at varying concentrations (0, 1, 3, 7 mol%). The rationale was to develop new materials for treating organic effluents and combating microbial resistance. Theoretical models included Rietveld refinement for structural analysis and Kubelka-Munk function for optical properties.
2:Sample Selection and Data Sources:
Samples were prepared using precursor materials: Zn(NO3)2·6H2O, Fe(NO3)3·9H2O, Pb(NO3)2, NaOH, and deionized water. Specific samples included pure ZnO and co-doped variants (e.g., Z1F, Z1F1P).
3:List of Experimental Equipment and Materials:
Equipment included Shimadzu diffractometer (XRD-6000), Supra 35 SEM microscope (Zeiss), Belsorp II BET equipment (Bel Japan, INC), Shimadzu IRTracer-100 FTIR, Shimadzu UV-2550 DRS-UV, Shimadzu EDX-720 XRF, Shimadzu UV-2600 spectrophotometer, TOC analyzer Shimadzu 500, UVC lamps (Philips TUV 15W), and autoclave for hydrothermal synthesis. Materials were sourced from Sigma-Aldrich and Synth.
4:Experimental Procedures and Operational Workflow:
Synthesis involved dissolving precursors, adjusting pH to 13 with NaOH, heating in a Teflon autoclave at 140°C for 30 min under microwave radiation (2.45 GHz, 800 W max power, 3 atm pressure), followed by centrifugation, washing, and drying. Characterization involved XRD, SEM, BET, FTIR, DRS-UV, XRF. Photocatalytic tests used methylene blue dye degradation under UV radiation; antimicrobial tests used agar diffusion method against E. coli and S. aureus.
5:45 GHz, 800 W max power, 3 atm pressure), followed by centrifugation, washing, and drying. Characterization involved XRD, SEM, BET, FTIR, DRS-UV, XRF. Photocatalytic tests used methylene blue dye degradation under UV radiation; antimicrobial tests used agar diffusion method against E. coli and S. aureus. Data Analysis Methods:
5. Data Analysis Methods: Data were analyzed using Rietveld refinement with GSAS and EXPGUI for structural parameters, Kubelka-Munk and Wood-Tauc equations for band gap estimation, statistical analysis of inhibition halo diameters, and TOC measurements for mineralization.
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X-ray diffractometer
XRD-6000
Shimadzu
Used for X-ray diffraction analysis to characterize the crystalline phases of the samples.
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Field emission scanning electron microscope
Supra 35
Zeiss
Used to observe the morphology and size of the nanoparticles.
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FTIR equipment
IRTracer-100
Shimadzu
Used for Fourier transform infrared spectroscopy to determine functional groups.
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UV-vis spectrophotometer
UV-2550
Shimadzu
Used for ultraviolet diffuse reflectance spectroscopy to estimate band gap.
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XRF spectrometer
EDX-720
Shimadzu
Used for elemental X-ray fluorescence analysis to check chemical stability.
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Spectrophotometer
UV-2600
Shimadzu
Used to monitor the absorption band of methylene blue during photocatalytic tests.
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TOC analyzer
500
Shimadzu
Used to estimate mineralization degrees by measuring total organic carbon.
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BET equipment
Belsorp II
Bel Japan, INC
Used to calculate specific surface areas from adsorption isotherms.
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UVC lamp
TUV
Philips
Used as a UV light source for photocatalytic tests.
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Autoclave
Used for hydrothermal synthesis under controlled temperature and pressure.
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