研究目的
The controlled fabrication of ZnO nanosystems and their functionalization with TiO2 or WO3 for use as photoanodes in photoelectrochemical water splitting, with a focus on investigating their surface composition and chemical interplay using XPS and Auger electron spectroscopy.
研究成果
The XPS analyses confirm the successful fabrication of pure ZnO and ZnO-based composites with TiO2 and WO3, where each component's identity is preserved. An electronic interplay between ZnO and WO3 phases is identified, which could enhance functional properties for applications such as photoanodes. The results provide foundational insights for further development of nanostructured oxide materials.
研究不足
The study is limited to surface analysis via XPS and does not cover other characterization techniques or performance testing in applications like photoelectrochemical water splitting. The functionalization may not fully optimize the composite properties, and the electronic interplay is only observed in ZnO-WO3, not ZnO-TiO2.
1：Experimental Design and Method Selection:
A combined chemical vapor deposition (CVD) and radio frequency (RF)-sputtering route was used to fabricate ZnO-based nanocomposites on FTO-coated glass substrates, followed by thermal treatments in air. X-ray photoelectron spectroscopy (XPS) and x-ray excited Auger electron spectroscopy were employed for detailed surface analysis.
2：Sample Selection and Data Sources:
Samples included pure ZnO, ZnO-TiO2, and ZnO-WO3 composites. FTO-coated glass slides (Aldrich, ≈7 Ω sq?1) were used as substrates, precleaned according to established procedures.
3：List of Experimental Equipment and Materials:
Equipment includes a home-made hot-wall CVD apparatus with a Carbolite HST 12/200 furnace, a custom-built RF-sputtering apparatus with an RF generator (ν = 13.56 MHz), a Perkin-Elmer Physical Electronics, Inc. 5600ci XPS instrument, a Bruker D8 Advance diffractometer for XRD, and a Zeiss SUPRA 40VP FE-SEM instrument. Materials include Zn(hfa)2 ? TMEDA precursor, Ti target (Alfa Aesar, purity=99.95%), WO3 target (Neyco, purity=99.99%), and gases like N2 and Ar.
4：56 MHz), a Perkin-Elmer Physical Electronics, Inc. 5600ci XPS instrument, a Bruker D8 Advance diffractometer for XRD, and a Zeiss SUPRA 40VP FE-SEM instrument. Materials include Zn(hfa)2 ? TMEDA precursor, Ti target (Alfa Aesar, purity=95%), WO3 target (Neyco, purity=99%), and gases like N2 and Ar.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: ZnO was deposited via CVD at 450°C for 2 hours, followed by functionalization with TiO2 or WO3 via RF-sputtering (e.g., 4 hours for TiO2, 3 hours for WO3), and annealing in air (e.g., 550°C for ZnO, 350°C for composites). Samples were mounted for XPS analysis without in situ preparation, and spectra were acquired under specific conditions (e.g., Mg Kα source, 200 W, analyzer pass energy 58.7 eV).
5：7 eV).
Data Analysis Methods:
5. Data Analysis Methods: Binding energy values were corrected using the C 1s peak of adventitious carbon at 284.8 eV. Peak fitting used Shirley background subtraction and Gaussian/Lorentzian functions. Atomic concentrations were calculated using sensitivity factors from PHI V5.4A software.
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