Solid-State NMR Studies on the Surface Structure and Properties of Oxide Nanomaterials

  • Xi-feng XIA ,
  • Wen-jing ZHANG ,
  • Zhi-ye LIN ,
  • Xiao-kang KE ,
  • Yu-jie WEN ,
  • Fang WANG ,
  • Jun-chao CHEN ,
  • Lu-ming PENG
Expand
  • 1. Analysis and Testing Center, Nanjing University of Science and Technology, Nanjing 210094, China
    2. Key Laboratory of Mesoscopic Chemistry of Ministry of Education and Collaborative Innovation Center of Chemistry for Life Sciences, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China

Received date: 2021-07-13

  Online published: 2021-08-18

Abstract

Many applications of oxide nanomaterials depend on their surface structure and properties. Solid-state nuclear magnetic resonance (NMR) spectroscopy has been used to obtain such key information in related studies. This paper summarizes two recently developed approaches based on solid-state NMR spectroscopy for determining the surface structure and properties of oxide nanomaterials, including surface-selective isotopic labeling 17O NMR and dynamic nuclear polarization surface enhanced NMR spectroscopy. The development trend for investigating oxide nanomaterials with solid-state NMR spectroscopy is also introduced.

Cite this article

Xi-feng XIA , Wen-jing ZHANG , Zhi-ye LIN , Xiao-kang KE , Yu-jie WEN , Fang WANG , Jun-chao CHEN , Lu-ming PENG . Solid-State NMR Studies on the Surface Structure and Properties of Oxide Nanomaterials[J]. Chinese Journal of Magnetic Resonance, 2021 , 38(4) : 533 -542 . DOI: 10.11938/cjmr20212936

References

1 YANG P D . Crystal cuts on the nanoscale[J]. Nature, 2012, 482, 41- 42.
2 LI Y , SHEN W J . Morphology-dependent nanocatalysts: rod-shaped oxides[J]. Chem Soc Rev, 2014, 43 (5): 1543- 1574.
3 XIE X W , LI Y , LIU Z Q , et al. Low-temperature oxidation of CO catalysed by Co3O4 nanorods[J]. Nature, 2009, 458 (7239): 746- 749.
4 ZHOU K B , LI Y D . Catalysis based on nanocrystals with well-defined facets[J]. Angew Chem Int Ed, 2012, 51 (3): 602- 613.
5 LI Y H , WU X P , JIANG N X , et al. Distinguishing faceted oxide nanocrystals with 17O solid-state NMR spectroscopy[J]. Nat Commun, 2017, 8, 581.
6 Chapter 7: Basics of X-ray diffraction[M]. Scintag, Inc, 1999.
7 DU J H , PENG L M . Recent progress in investigations of surface structure and properties of solid oxide materials with nuclear magnetic resonance spectroscopy[J]. Chin Chem Lett, 2018, 29 (6): 747- 751.
8 VOGT T, DAHMEN W, BINEV P. Modeling nanoscale imaging in electron microscopy[M]. Springer, 2012.
9 MARCHETTI A , CHEN J , PANG Z F , et al. Understanding surface and interfacial chemistry in functional nanomaterials via solid-state NMR[J]. Adv Mater, 2017, 29 (14): 1605895.
10 LEVITT M H. Spin dynamics: basics of nuclear magnetic resonance[M]. Second edition, John Wiley & Sons, Ltd, 2008.
11 PENG L M , LIU Y , KIM N , et al. Detection of Bronsted acid sites in zeolite HY with high-field 17O-MAS-NMR techniques[J]. Nat Mater, 2005, 4, 216- 219.
12 ZHENG A M , LI S H , LIU S B , et al. Acidic properties and structure-activity correlations of solid acid catalysts revealed by solid-state NMR spectroscopy[J]. Acc Chem Res, 2016, 49 (4): 655- 663.
13 ZHENG A M , LIU S B , DENG F . 31P NMR chemical shifts of phosphorus probes as reliable and practical acidity scales for solid and liquid catalysts[J]. Chem Rev, 2017, 117 (19): 12475- 12531.
14 MACKENZIE K J D, SMITH M E. Multinuclear solid-state NMR of inorganic materials[M]. Pergamon, 2002.
15 WANG M , WU X P , ZHENG S J , et al. Identification of different oxygen species in oxide nanostructures with 17O solid-state NMR spectroscopy[J]. Sci Adv, 2015, 1 (1): e1400133.
16 CHEN J C , WU X P , HOPE M A , et al. Polar surface structure of oxide nanocrystals revealed with solid-state NMR spectroscopy[J]. Nat Commun, 2019, 10, 5420.
17 CHEN J C , HOPE M A , LIN Z Y , et al. Interactions of oxide surfaces with water revealed with solid-state NMR spectroscopy[J]. J Am Chem Soc, 2020, 142 (25): 11173- 11182.
18 SHEN L , WANG Y , DU J H , et al. Probing interactions of γ-alumina with water via multinuclear solids-state NMR spectroscopy[J]. Chem Cat Chem, 2020, 12 (6): 1569- 1574.
19 CHAMPOURET Y , COPPEL Y , KAHN M L . Evidence for core oxygen dynamics and exchange in metal oxide nanocrystals from in situ 17O MAS NMR[J]. J Am Chem Soc, 2016, 138 (50): 16322- 16328.
20 XU M , CHEN J C , WEN Y J , et al. 17O solid-state NMR studies of Ta2O5 nanorods[J]. ACS Omega, 2020, 5 (14): 8355- 8361.
21 SHEN L , WU X P , WANG Y , et al. 17O solid-state NMR studies of ZrO2 nanoparticles[J]. J Phys Chem C, 2019, 123 (7): 4158- 4167.
22 LI Y H , WU X P , LIU C . NMR and EPR studies of partially reduced TiO2[J]. Acta Phys Chim Sin, 2020, 36 (4): 1905021.
23 WANG Q , LI W Z , HUNG I , et al. Mapping the oxygen structure of gamma-Al2O3 by high-field solid-state NMR spectroscopy[J]. Nat Commun, 2020, 11, 3620.
24 LIU L , CHEN X B . Titanium dioxide nanomaterials: Self-structural modifications[J]. Chem Rev, 2014, 114 (19): 9890- 9818.
25 CARVER T R , SLICHTER C P . Polarization of nuclear spins in metals[J]. Phys Rev, 1953, 92, 212- 213.
26 LESAGE A , LELLI M , GAJAN D , et al. Surface enhanced NMR spectroscopy by dynamic nuclear polarization[J]. J Am Chem Soc, 2010, 132 (44): 15459- 15461.
27 SONG C , HU K N , JOO C G , et al. TOTAPOL: A biradical polarizing agent for dynamic nuclear polarization experiments in aqueous media[J]. J Am Chem Soc, 2006, 128 (35): 11385- 11390.
28 REIF B , ASHBROOK S E , EMSLEY L , et al. Solid-state NMR spectroscopy[J]. Nat Rev Methods Primers, 2021, 1, 2.
29 LAFON O , THANKAMONY A S L , ROSAY M , et al. Indirect and direct 29Si dynamic nuclear polarization of dispersed nanoparticles[J]. Chem Commun, 2013, 49 (28): 2864- 2866.
30 BLANC F , SPERRIN L , JEFFERSON D A , et al. Dynamic nuclear polarization enhanced natural abundance 17O spectroscopy[J]. J Am Chem Soc, 2013, 135 (8): 2975- 2978.
31 PERRAS F A , KOBAYASHI T , PRUSKI M . Natural abundance 17O DNP two-dimensional and surface-enhanced NMR spectroscopy[J]. J Am Chem Soc, 2015, 137 (26): 8336- 8339.
32 ZHAO X , HOFFBAUER W , SCHMEDT AUF DER GUNNE J , et al. Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR[J]. Solid State Nucl Magn Reson, 2004, 26 (2): 57- 64.
33 HOPE M A , HALAT D M , MAGUSIN P C M M , et al. Surface-selective direct 17O DNP NMR of CeO2 nanoparticles[J]. Chem Commun, 2017, 53, 2142- 2145.
34 VITZTHUM V , MIEVILLE P , CARNEVALE D , et al. Dynamic nuclear polarization of quadrupolar nuclei using cross polarization from protons: surface-enhanced aluminium-27 NMR[J]. Chem Commun, 2012, 48, 1988- 1990.
35 LI W Z , WANG Q , XU J , et al. Probing the surface of γ-Al2O3 by oxygen-17 dynamic nuclear polarization enhanced solid-state NMR spectroscopy[J]. Phys Chem Chem Phys, 2018, 20 (25): 17218- 17225.
Outlines

/