利用報告書 / User's Report

【公開日：2023.08.01】【最終更新日：2023.05.12】

課題データ / Project Data

課題番号 / Project Issue Number

22KU1009

利用課題名 / Title

合成した光触媒複合体のXPS測定

利用した実施機関 / Support Institute

九州大学

機関外・機関内の利用 / External or Internal Use

内部利用（ARIM事業参画者以外）/Internal Use (by non ARIM members)

技術領域 / Technology Area

【横断技術領域 / Cross-Technology Area】（主 / Main）物質・材料合成プロセス/Molecule & Material Synthesis（副 / Sub）計測・分析/Advanced Characterization

【重要技術領域 / Important Technology Area】（主 / Main）革新的なエネルギー変換を可能とするマテリアル/Materials enabling innovative energy conversion（副 / Sub）次世代ナノスケールマテリアル/Next-generation nanoscale materials

キーワード / Keywords

電子顕微鏡/Electron microscopy,走査プローブ顕微鏡/Scanning probe microscopy,赤外・可視・紫外分光/Infrared and UV and visible light spectroscopy,X線回折/X-ray diffraction,電子分光,放射光/Synchrotron radiation,ワイドギャップ半導体,ナノ粒子,ナノ多孔体,ナノシート


利用者と利用形態 / User and Support Type

利用者名（課題申請者）/ User Name (Project Applicant)

Keiko Sasaki

所属名 / Affiliation

九州大学大学院工学研究院地球資源システム工学部門

共同利用者氏名 / Names of Collaborators in Other Institutes Than Hub and Spoke Institutes

Chitiphon Chuaicham

ARIM実施機関支援担当者 / Names of Collaborators in The Hub and Spoke Institutes

Chitiphon Chuaicham

利用形態 / Support Type

（主 / Main）機器利用/Equipment Utilization（副 / Sub）-


利用した主な設備 / Equipment Used in This Project

KU-501：電子状態測定システム


報告書データ / Report

概要（目的・用途・実施内容）/ Abstract (Aim, Use Applications and Contents)

In this work, photocatalyst and its composites such as iron-doped hydroxyapatite, iron-doped montmorillonite, graphitic carbon nitride/ZnTi-mixed metal oxide composites were prepared for photocatalytic degradation of ciprofloxacin (CIP), which is an antibiotic model pollutant and reduction of hexavalent chromium (Cr(VI)). To elucidate the chemical properties and band positions of each component in the composite, X-ray photoelectron spectroscopy (XPS) was utilized. For the XPS results, the chemical state of the backbone structure of single phase and composite was confirmed. Also, the valence band position of the pure phase photocatalyst was estimated to predict the direction of the electron transfer in the composite. Thus, the XPS results can support the explanation of the electron transfer mechanism of the photocatalyst composite, related to the photocatalytic activity. In this work, photocatalyst and its composites such as iron-doped hydroxyapatite, iron-doped montmorillonite, graphitic carbon nitride/ZnTi-mixed metal oxide composites were prepared for photocatalytic degradation of ciprofloxacin (CIP), which is an antibiotic model pollutant and reduction of hexavalent chromium (Cr(VI)). To elucidate the chemical properties and band positions of each component in the composite, X-ray photoelectron spectroscopy (XPS) was utilized. For the XPS results, the chemical state of the backbone structure of single phase and composite was confirmed. Also, the valence band position of the pure phase photocatalyst was estimated to predict the direction of the electron transfer in the composite. Thus, the XPS results can support the explanation of the electron transfer mechanism of the photocatalyst composite, related to the photocatalytic activity. 

実験 / Experimental

Using XPS, the chemical states of each element in photocatalyst and its composite and their valence band (VB) locations were studied. For XPS analysis, a dry powder sample was prepared by spreading it on the carbon tap. The blower was used to remove the unattached sample from the carbon tap.  After measurement, the results were calibrated using the contaminated carbon peak at 284.6 eV using the CasaXPS program.  

結果と考察 / Results and Discussion

In graphitic carbon nitride-based composite, C 1s orbitals can be separated into four peaks, contaminated carbon, sp3 (C–C) bond, (C)3–N, and N–C=N bonding in the CN structure's backbone. The N 1 s spectra show three peaks, corresponding to the CN structure. The dominant peak at EB[Zn 3p3/2] in the composite for the Zn 2p orbital is Zn2+ at 1021.2 eV. Moreover, the chemical state of the Ti in ZnTi-mixed metal oxide was +4, as shown by EB[Ti 3p3/2] = 458.3 eV. Also, in O 1s spectra, this composite has a distinct peak of metal oxide structure and adsorbed water. In iron-doped hydroxyapatite and iron-doped montmorillonite, the oxidation state of Fe was confirmed as +3, suggesting no reduction happen during the synthesis. Importantly, valence band (VB) locations were also examined by XPS examination of the valence area. The obtained VB results can be used to predict the position of the conduction band bottom by combining them with energy band gap results from UV-Vis diffuse reflectance spectroscopy. Also, the transfer of electrons and holes in the photocatalyst composite can be proposed. Thus, XPS analysis is a useful technique to provide the chemical and optical properties of photocatalyst composites. 

図・表・数式 / Figures, Tables and Equations
その他・特記事項（参考文献・謝辞等） / Remarks(References and Acknowledgements)

The work was supported by the Japan Society for the Promotion of Science (JSPS) KAKENHI (A) [No. JP19F19393].


成果発表・成果利用 / Publication and Patents

論文・プロシーディング（DOIのあるもの） / DOI (Publication and Proceedings)
  1. Chitiphon Chuaicham, Fabrication of graphitic carbon nitride/ZnTi-mixed metal oxide heterostructure: Robust photocatalytic decomposition of ciprofloxacin, Journal of Alloys and Compounds, 906, 164294(2022).
    DOI: https://doi.org/10.1016/j.jallcom.2022.164294
  2. Chitiphon Chuaicham, Efficient photocatalytic degradation of emerging ciprofloxacin under visible light irradiation using BiOBr/carbon quantum dot/saponite composite, Environmental Research, 212, 113635(2022).
    DOI: https://doi.org/10.1016/j.envres.2022.113635
  3. Jirawat Trakulmututa, Effect of transformation temperature toward optical properties of derived CuO/ZnO composite from Cu–Zn hydroxide nitrate for photocatalytic ciprofloxacin degradation, Optical Materials, 133, 112941(2022).
    DOI: https://doi.org/10.1016/j.optmat.2022.112941
  4. Sulakshana Shenoy, Simple tactic polycondensation synthesis of Z-scheme quasi-polymeric g-C3N4/CaFe2O4 composite for enhanced photocatalytic water depollution via p-n heterojunction, Chemical Engineering Journal, 453, 139758(2023).
    DOI: https://doi.org/10.1016/j.cej.2022.139758
  5. Chitiphon Chuaicham, Simultaneous Photocatalytic Sugar Conversion and Hydrogen Production Using Pd Nanoparticles Decorated on Iron-Doped Hydroxyapatite, Catalysts, 13, 675(2023).
    DOI: https://doi.org/10.3390/catal13040675
  6. Takumi Inoue, Z-scheme heterojunction of graphitic carbon nitride and calcium ferrite in converter slag for the photocatalytic imidacloprid degradation and hydrogen evolution, Journal of Photochemistry and Photobiology A: Chemistry, 440, 114644(2023).
    DOI: https://doi.org/10.1016/j.jphotochem.2023.114644
  7. Intan Nurul Rizki, Fabrication of Reduced Ag Nanoparticle Using Crude Extract of Cinnamon Decorated on ZnO as a Photocatalyst for Hexavalent Chromium Reduction, Catalysts, 13, 265(2023).
    DOI: https://doi.org/10.3390/catal13020265
  8. Chitiphon Chuaicham, Fabrication of visible-light-active ZnCr mixed metal oxide/fly ash for photocatalytic activity toward pharmaceutical waste ciprofloxacin, Journal of Industrial and Engineering Chemistry, 108, 263-273(2022).
    DOI: https://doi.org/10.1016/j.jiec.2022.01.006
  9. Li Zhang, Determination of the roles of FeIII in the interface between titanium dioxide and montmorillonite in FeIII-doped montmorillonite/titanium dioxide composites as photocatalysts, Applied Clay Science, 227, 106577(2022).
    DOI: https://doi.org/10.1016/j.clay.2022.106577
  10. Li Zhang, Effect of ionic Fe(III) doping on montmorillonite for photocatalytic reduction of Cr(VI) in wastewater, Journal of Photochemistry and Photobiology A: Chemistry, 429, 113909(2022).
    DOI: https://doi.org/10.1016/j.jphotochem.2022.113909
口頭発表、ポスター発表および、その他の論文 / Oral Presentations etc.
特許 / Patents

特許出願件数 / Number of Patent Applications：0件
特許登録件数 / Number of Registered Patents：0件

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