Atomic Layer Deposition-Assisted Surface-Selective Isotopic Labeling for the <sup>17</sup>O Solid-State NMR Studies of Metal Oxide Surfaces
<sup>17</sup>O solid-state NMR spectroscopy is widely used to investigate metal oxide surfaces and is increasingly recognized for the unique insights into surface structures. Given the low natural abundance of the <sup>17</sup>O nucleus (0.037%), <sup>17</sup>O surface-selective isotopic labeling is commonly employed in relevant studies. Conventional thermal treatment (CTT)-labeling methods rely on rapid <sup>17</sup>O/<sup>16</sup>O exchange may yield insufficient labeling on less reactive surfaces. Our approach uses atomic layer deposition (ALD) epitaxial growth to directly deposit <sup>17</sup>O onto metal oxide surfaces regardless of surface reactivity. This method minimizes the formation of excessive surface hydroxyl groups, reducing overlapping NMR signals and enabling better <sup>17</sup>O NMR identification of hydroxyl groups, as observed in Al<sub>2</sub>O<sub>3</sub>. Moreover, heteronuclear <sup>27</sup>Al{<sup>17</sup>O} <i>J</i>-HMQC NMR analysis reveals that the CTT method creates more correlations between penta-coordinated Al sites and hydroxyl groups in Al<sub>2</sub>O<sub>3</sub> compared to ALD, indicating that the labeling techniques vary in their effectiveness at different surface sites.
Authors
- Kuizhi Chen (ORCID: https://orcid.org/0000-0002-9853-7070)
- Jia‐Huan Du (ORCID: https://orcid.org/0000-0003-2408-0060)
- Jennifer S. Gómez (ORCID: https://orcid.org/0000-0003-2101-9889)
- Luming Peng (ORCID: https://orcid.org/0000-0003-1935-1620)
- Xiaoli Xia
- Yujie Wen (ORCID: https://orcid.org/0000-0002-7105-0465)
- Ivan Hung (ORCID: https://orcid.org/0000-0001-8916-739X)
- Zhehong Gan (ORCID: https://orcid.org/0000-0002-9855-5113)
- Fang Wang (ORCID: https://orcid.org/0000-0003-2280-3923)
- Yang Wang (ORCID: https://orcid.org/0000-0002-5861-6081)
- Rong Chen (ORCID: https://orcid.org/0000-0001-7371-1338)
- Xiao Liu (ORCID: https://orcid.org/0000-0003-4178-5775)
- Junchao Chen (ORCID: https://orcid.org/0000-0002-7601-5458)
- Li Shen (ORCID: https://orcid.org/0000-0002-1454-3896)
- Weiping Tang
Institutions
- Nanjing Tech University (CN)
- Radboud University Nijmegen (NL)
- Dalian Institute of Chemical Physics (CN)
- Shanghai Jiao Tong University (CN)
- Chinese Academy of Sciences (CN)
- National High Magnetic Field Laboratory (US)
- Dalian National Laboratory for Clean Energy (CN)
- State Key Laboratory of Vehicle NVH and Safety Technology (CN)
- Collaborative Innovation Center of Chemistry for Energy Materials (CN)
- State Key Laboratory of Materials-Oriented Chemical Engineering
- Huazhong University of Science and Technology (CN)
- Yangzhou University (CN)
- Nanjing University (CN)
Publication Details
- Journal
- The Journal of Physical Chemistry Letters
- Published
- 2025-06-28
- DOI
- https://doi.org/10.1021/acs.jpclett.5c01138
- Citations
- 1
- Primary Topic
- Advanced NMR Techniques and Applications
- Type
- article
- Field-Weighted Citation Impact
- 0.76
Funders
- National Science Foundation
- Newton Fund
- National High Magnetic Field Laboratory
- Royal Society
- National Natural Science Foundation of China
- Radboud Universiteit
- Nanjing University
- Priority Academic Program Development of Jiangsu Higher Education Institutions
- National Key Research and Development Program of China
- Division of Materials Research
- High Magnetic Field Laboratory, Chinese Academy of Sciences