Growth and electronic properties of Rh and Au nanoclusters supported on CuO/Cu(110)

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李易暽(Yi-Lin Li) 查詢紙本館藏

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物理學系

論文名稱

(Growth and electronic properties of Rh and Au nanoclusters supported on CuO/Cu(110))

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摘要(中)

本研究透過掃描穿隧電子顯微術(STM)、高能電子繞射儀(RHEED)及位於新竹同步輻射中心的X光光源與能譜儀研究銠及金在氧化銅/銅(110)上的生長形貌及電子特性。STM顯示銠在室溫下在氧化銅/銅(110)上便透過自組裝形成三維結構，即便是在很小的鍍量下(0.09 ML)。此三維結構也被RHEED監測到，呼應STM的結果。銠奈米團簇的平均直徑隨著鍍量上升，並在達到0.62 ML以上時，達到1.50奈米左右並趨於飽和。然而平均高度並未隨著鍍量上升，並保持在0.22奈米左右。銠奈米團簇於表面的密度在鍍量達到0.62 ML以上時也達到飽和。綜合團簇密度及粒徑大小的不變性來看，下層的銠奈米團簇可能已經結合形成薄膜。銠奈米團簇的電子特性透過XPS量測。在小鍍量時(0.02到0.12 ML)，銠〖3d〗_(5/2) 軌域的束縛能坐落在306.3 eV，比塊材銠小0.7 eV。隨著鍍量上升，銠〖3d〗_(5/2) 軌域的束縛能逐漸往高束縛能移動且接近塊材值。並在達到1.44 ML時，坐落於306.8 eV。銠3d雙峰的束縛能在小鍍量時比塊材值還小許多，此結果與一般認知及其他研究的實驗結果不同，可能與電荷從基板或擔體轉移至銠奈米粒子有關。
金在鍍量小於1 ML時以二維團簇的形式存在於表面，並由STM鑑定。當鍍量增加超過1 ML時，金薄膜便成形，被STM及RHEED所確認。金團簇與薄膜的電子結構也由XPS所鑑定，在小鍍量時(≤ 0.23 ML)，金〖4f〗_(7/2) 軌域的束縛能坐落於84.1 eV，高於塊材0.1 eV。隨著鍍量上升後增加至84.2 eV。金4f雙峰隨鍍量上升的移動方向與一般認知不同，代表金表面的化學環境有所改變，可能與底層氧原子浮出至表面有關。

摘要(英)

By utilizing the reflection high energy diffraction (RHEED), scanning tunneling microscopy (STM), and X-ray photoelectron spectroscopy (XPS), we have investigated the growth and electronic properties of Rh and Au nanoclusters grown on CuO/Cu(110).
Rh atoms that are deposited on CuO/Cu(110) at 300 K self-assemble into nanoclusters in a 3D (three-dimensional) fashion even at small coverage (0.09 ML), indicated by STM. RHEED patterns also reflect the 3D structure of Rh nanoclusters, and are consistent with STM results. The averaged diameter of these nanoclusters increases with Rh coverage, and saturates at around 1.50 nm when above 0.62 ML. However, the averaged height does not increase with coverage but maintains at around 0.22 nm. The cluster density also saturates when above 0.62 ML, together with the unchanged size of Rh nanoclusters, the clusters at the lower position may merge into a Rh film. Electronic structure of Rh nanoclusters evolves with coverage. At small coverages (0.02 to 0.12 ML), Rh 〖3d〗_(5/2) centers at 306.3 eV which is 0.7 eV smaller than the bulk value (307.0 eV). On increasing the Rh coverage, Rh 〖3d〗_(5/2) shifts toward it bulk value, and finally locates at 306.8 eV when at 1.44 ML. This unusual shift of Rh 3d doublet may indicate a charge transfer from substrate or support to Rh nanoclusters.
The Au nanoclusters grow in a 2D fashion at sub-monolayer level, indicated by STM. Au films form on the surface when increasing the coverage, identified by the STM images and RHEED patterns. The electronic structure of Au nanoclusters also evolves with coverage. At the low coverages (≤ 0.23 ML), Au 〖4f〗_(7/2) centers at 84.1 eV which is 0.1 eV higher than its bulk value (84.0 eV), and increases to 84.2 eV at higher coverage. The abnormal shift of the Au 4f doublet may indicate that the chemical enviroment on the Au surface is modified by an extra element, such as the oxygen atoms floating to the CuO surface.

關鍵字(中)

★ 銠
★ 金
★ 氧化銅
★ 高能電子繞射儀
★ 掃描穿隧式顯微鏡
★ X光光電子能譜儀

關鍵字(英)

★ Rh
★ Au
★ CuO
★ RHEED
★ STM
★ XPS

論文目次

摘要 i
Abstract ii
誌謝 iii
Contents v
List of Figures viii
List of Tables xviii
Chapter 1 Introduction 1
Chapter 1 References 3
Chapter 2 Literature Survey 4
2.1 Oxygen-induced Cu(110)-(2×1)O reconstruction on
Cu(110) 4
2.2 Oxygen-induced Cu(110)-c(6×2)O reconstruction on
Cu(110) 7
2.3 Phase transitions between Cu(110)-(2×1)O and Cu(110)-
c(6×2)O & Escape of oxygen atoms from Cu(110)-(2×1)O
reconstruction after deposition of Ni 8
2.3.1 Phase transition from Cu(110)-(2×1)O to Cu(110)-c(6×2)O 8
2.3.2 Phase transition from Cu(110)-c(6×2)O to Cu(110)-(2×1)O 11
2.3.3 Escape of oxygen atoms from Cu(110)-(2×1)O reconstruction after deposition of Ni 12
2.4 Supported Rh nanoclusters 14
2.4.1 Rh nanoclusters supported on the 〖Al〗_2 O_3/NiAl(100) 14
2.4.2 Rh nanoclusters supported on the graphene/Ir(111) 17
2.5 Supported Au single atoms, nanoclusters and thin film(s) ..........................................................20
2.5.1 Au single atoms supported on Cu(110)-(2×1)O/Cu(110) 20
2.5.2 Au nanoclusters supported on the 〖Al〗_2 O_3/NiAl(100) 22
2.5.3 Monolayer and bilayer Au supported on Mo(112)-(8×2)-TiO_x 24
Chapter 2 References 27
Chapter 3 Experimental Apparatus & Procedure 31
3.1 Vacuum system 31
3.1.1 Introduction of vacuum 31
3.1.2 Ultrahigh vacuum system 32
3.2 Scanning tunneling microscopy (STM) 34
3.2.1 An example of barrier penetration (tunneling) through a one-dimensional square barrier 34
3.2.2 Operation and working principles of STM 35
3.2.3 RHK-UHV 300 STM system with beetle type scan head 37
3.2.4 Preparation of STM Tips 39
3.3 Reflection high energy electron diffraction (RHEED) 41
3.3.1 Theory of diffraction and diffraction condition 41
3.3.2 Operation principle of RHEED 42
3.4 X-ray Photoelectron spectroscopy (XPS) 43
3.4.1 Basic theory of XPS : Photoelectron effect 43
3.4.2 The synchrotron radiation produced by TLS beamline at NSRRC 44
3.4.3 The XPS system at TLS 09A2 endstation 45
3.5 Experimental procedure 45
3.5.1 Sample cleaning 45
3.5.2 Growth of thin-film CuO on Cu(110) 46
3.5.3 Deposition of Rh or Au on CuO/Cu(110) 46
3.6 Estimation of Rh and Au coverage 50
Chapter 3 References 51
Chapter 4 Results 52
4.1 Cu(110) surface 52
4.2 Cu(110)-(2×1)O reconstruction surface 53
4.3 The coexistence surface of Cu(110)-(2×1)O and Cu(110)-
c(6×2)O 61
4.4 Rh nanoclusters supported on CuO/Cu(110) 70
4.4.1 RHEED studies of Rh nanoclusters 70
4.4.2 RHEED studies of annealing effect on Rh nanoclusters..............................................74
4.4.3 STM studies of Rh nanoclusters 76
4.4.4 XPS studies of Rh nanoclusters 84
4.5 Au nanoclusters supported on CuO/Cu(110) 87
4.5.1 RHEED studies of Au nanoclusters 88
4.5.2 RHEED studies of annealing effect on Au nanoclusters ..........................................................91
4.5.3 STM studies of Au nanoclusters 92
4.5.4 STM studies of annealing effect on Au nanoclusters 96
4.5.5 XPS studies of Au nanoclusters 98
Chapter 4 References 101
Chapter 5 Conclusion 104

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[14] K. Moritani, M. Okada, Y. Teraoka, A. Yoshigoe, and T. Kasai, Kinetics of oxygen adsorption and initial oxidation on Cu(110) by hyperthermal oxygen molecular beams. The Journal of Physical Chemistry A. 113(52): p. 15217-15222, 2009.
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[17] L. Li, Q. Liu, J. Li, W. A. Saidi, and G. Zhou, Kinetic barriers of the phase transition in the oxygen chemisorbed Cu(110)-(2×1)-O as a function of oxygen coverage. The Journal of Physical Chemistry C. 118(36): p. 20858-20866, 2014.
[18] Y. Li, H. Chen, W. Wang, W. Huang, Y. Ning, Q. Liu, Y. Cui, Y. Han, Z. Liu, and F. Yang, and X. Bao, Crystal-plane-dependent redox reaction on Cu surfaces. Nano Research. 13: p. 1677-1685, 2020.
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[26] A. Cavallin, M. Pozzo, C. Africh, A. Baraldi, E. Vesselli, C. Dri, G. Comelli, R. Larciprete, P. Lacovig, S. Lizzit, and D. Alfè, Local electronic structure and density of edge and facet atoms at Rh nanoclusters self-assembled on a graphene template. ACS nano. 6(4): p. 3034-3043, 2012.
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Chapter 3 References

[1] 蘇青森等編著，真空技術與應用，行政院國家科學委員會精密儀器發展中心，台灣新竹市，2001。
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[10] J. Chastain and R. C. King Jr, Handbook of X-ray photoelectron spectroscopy., Perkin-Elmer Corporation., 40: p. 221, 1992.
[11] 國家同步輻射研究中心中心簡介，取自https://www.nsrrc.org.tw/chinese/img/pdf/info.pdf。

Chapter 4 References

[1] W. Moritz and D. Wolf, Structure determination of the reconstructed Au (110) surface. Surface Science. 88(2-3): p. L29-L34, 1979.
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[4] L. D. Sun, M. Hohage, R. Denk, and P. Zeppenfeld, Oxygen adsorption on Cu(110) at low temperature. Physical Review B. 76(24): p. 245412, 2007.
[5] D. J. Coulman, J. Wintterlin, R. Behm, and G. Ertl, Novel mechanism for the formation of chemisorption phases: The (2×1)O-Cu(110) ‘‘added row’’ reconstruction. Physical review letters. 64(15): p. 1761, 1990.
[6] J. F. Wendelken, The chemisorption of oxygen on Cu(110) studied by EELS and LEED. Surface Science. 108(3): p. 605-616, 1981.
[7] K. Kern, H. Niehus, A. Schatz, P. Zeppenfeld, J. Goerge, and G. Comsa, Long-range spatial self-organization in the adsorbate-induced restructuring of surfaces: Cu{100}-(2×1)O. Physical review letters. 67(7): p. 855, 1991.
[8] F. M. Chua, Y. Kuk, and P. J. Silverman, Oxygen chemisorption on Cu(110): An atomic view by scanning tunneling microscopy. Physical review letters. 63(4): p. 386, 1989.
[9] L. D. Sun, M. Hohage, and P. Zeppenfeld, Oxygen-induced reconstructions of Cu(110) studied by reflectance difference spectroscopy. Physical Review B. 69(4): p. 045407, 2004.
[10] R. Feidenhans’l and I. Stensgaard, Oxygen-adsorption induced reconstruction of Cu(110) studied by high energy ion scattering. Surface science. 133(2-3): p. 453-468, 1983.
[11] F. Jensen, F. Besenbacher, E. Lægsgaard, and I. Stensgaard, Surface reconstruction of Cu(110) induced by oxygen chemisorption. Physical Review B. 41(14): p. 10233, 1990.
[12] Q. Liu, L. Li, N. Cai, W. A. Saidi, and G. Zhou, Oxygen chemisorption-induced surface phase transitions on Cu(110). Surface science. 627: p. 75-84, 2014.
[13] S. Kishimoto, M. Kageshima, Y. Naitoh, Y. J. Li, and Y. Sugawara, Study of oxidized Cu(110) surface using noncontact atomic force microscopy. Surface science. 602(13): p. 2175-2182, 2008.
[14] A. P. Baddorf and J. F. Wendelken, High coverages of oxygen on Cu(110) investigated with XPS, LEED, and HREELS. Surface science. 256(3): p. 264-271, 1991.
[15] K. Moritani, M. Okada, Y. Teraoka, A. Yoshigoe, and T. Kasai, Kinetics of oxygen adsorption and initial oxidation on Cu(110) by hyperthermal oxygen molecular beams. The Journal of Physical Chemistry A. 113(52): p. 15217-15222, 2009.
[16] X. Duan, O. Warschkow, A. Soon, B. Delley, and C. Stampfl, Density functional study of oxygen on Cu(100) and Cu(110) surfaces. Physical Review B. 81(7): p. 075430, 2010.
[17] S. Y. Liem, G. Kresse, and J.H.R. Clarke, First principles calculation of oxygen adsorption and reconstruction of Cu(110) surface. Surface science. 415(1-2): p. 194-211, 1998.
[18] L. Li, Q. Liu, J. Li, W. A. Saidi, and G. Zhou, Kinetic barriers of the phase transition in the oxygen chemisorbed Cu(110)-(2×1)-O as a function of oxygen coverage. The Journal of Physical Chemistry C. 118(36): p. 20858-20866, 2014.
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指導教授

羅夢凡(Meng-Fan Luo)

審核日期

2023-7-10

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