Abstract
In the past few decades, various surface analysis techniques find wide applications in studies of interfacial phenomena ranging from fundamental surface science, catalysis, environmental science and energy materials. With the help of bright synchrotron sources, many of these techniques have been further advanced into novel in-situ/operando tools at synchrotron user facilities, providing molecular level understanding of chemical/electrochemical processes in-situ at gas–solid and liquid–solid interfaces. Designing a proper endstation for a dedicated beamline is one of the challenges in utilizing these techniques efficiently for a variety of user’s requests. Many factors, including pressure differential, geometry and energy of the photon source, sample and analyzer, need to be optimized for the system of interest. In this paper, we discuss the design and performance of a new endstation at beamline 02B at the Shanghai Synchrotron Radiation Facility for ambient pressure X-ray photoelectron spectroscopy studies. This system, equipped with the newly developed high-transmission HiPP-3 analyzer, is demonstrated to be capable of efficiently collecting photoelectrons up to 1500 eV from ultrahigh vacuum to ambient pressure of 20 mbar. The spectromicroscopy mode of HiPP-3 analyzer also enables detection of photoelectron spatial distribution with resolution of 2.8 ± 0.3 µm in one dimension. In addition, the designing strategies of systems that allow investigations in phenomena at gas–solid interface and liquid–solid interface will be highlighted through our discussion.
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References
G.A. Somorjai, Y. Li, Introduction to Surface Chemistry and Catalysis (Wiley, Hoboken, 2010)
S. Hüfner, Photoelectron spectroscopy: principles and applications (Springer, Berlin, 2013)
M. Salmeron, R. Schlögl, Ambient pressure photoelectron spectroscopy: a new tool for surface science and nanotechnology. Surf. Sci. Rep. 63(4), 169–199 (2008). https://doi.org/10.1016/j.surfrep.2008.01.001
D. Starr, Z. Liu, M. Hävecker et al., Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy. Chem. Soc. Rev. 42(13), 5833–5857 (2013). https://doi.org/10.1039/C3CS60057B
H.-J. Freund, H. Kuhlenbeck, J. Libuda et al., Bridging the pressure and materials gaps between catalysis and surface science: clean and modified oxide surfaces. Top. Catal. 15(2–4), 201–209 (2001). https://doi.org/10.1023/A:1016686322301
P. Stoltze, J. Nørskov, Bridging the “Pressure Gap” between ultrahigh-vacuum surface physics and high-pressure catalysis. Phys. Rev. Lett. 55(22), 2502–2505 (1985). https://doi.org/10.1103/PhysRevLett.55.2502
K. Siegbahn, C. Nordling, G. Johansson et al., ESCA Applied to Free Molecules (North-Holland Publishing Co., Amsterdam, 1969)
R.W. Joyner, M.W. Roberts, K. Yates, A “high-pressure” electron spectrometer for surface studies. Surf. Sci. 87(2), 501–509 (1979). https://doi.org/10.1016/0039-6028(79)90544-2
H. Siegbahn, S. Svensson, M. Lundholm, A new method for ESCA studies of liquid-phase samples. J. Electron Spectrosc. Relat. Phenom. 24(2), 205–213 (1981). https://doi.org/10.1016/0368-2048(81)80007-2
H. Ruppender, M. Grunze, C. Kong et al., In situ X-ray photoelectron spectroscopy of surfaces at pressures up to 1 mbar. Surf. Interface Anal. 15(4), 245–253 (1990). https://doi.org/10.1002/sia.740150403
D.F. Ogletree, H. Bluhm, G. Lebedev et al., A differentially pumped electrostatic lens system for photoemission studies in the millibar range. Rev. Sci. Instrum. 73(11), 3872–3877 (2002). https://doi.org/10.1063/1.1512336
D.F. Ogletree, H. Bluhm, E.D. Hebenstreit et al., Photoelectron spectroscopy under ambient pressure and temperature conditions. Nucl. Instrum. Methods A 601(1), 151–160 (2009). https://doi.org/10.1016/j.nima.2008.12.155
H. Bluhm, M. Hävecker, A. Knop-Gericke et al., Methanol oxidation on a copper catalyst investigated using in situ X-ray photoelectron spectroscopy. J. Phys. Chem. B 108(38), 14340–14347 (2004). https://doi.org/10.1021/jp040080j
M.E. Grass, P.G. Karlsson, F. Aksoy et al., New ambient pressure photoemission endstation at Advanced Light Source beamline 9.3.2. Rev. Sci. Instrum. 81(5), 053106 (2010). https://doi.org/10.1063/1.3427218
J. Schnadt, J. Knudsen, J.N. Andersen et al., The new ambient-pressure X-ray photoelectron spectroscopy instrument at MAX-lab. J. Synchrotron. Radiat. 19(5), 701–704 (2012). https://doi.org/10.1107/S0909049512032700
R. Toyoshima, M. Yoshida, Y. Monya et al., In situ ambient pressure XPS study of CO oxidation reaction on Pd(111) surfaces. J. Phys. Chem. C 116(35), 18691–18697 (2012). https://doi.org/10.1021/jp301636u
S. Kaya, H. Ogasawara, L.-Å. Näslund et al., Ambient-pressure photoelectron spectroscopy for heterogeneous catalysis and electrochemistry. Catal. Today 205, 101–105 (2013). https://doi.org/10.1016/j.cattod.2012.08.005
C. Zhang, M.E. Grass, A.H. McDaniel et al., Measuring fundamental properties in operating solid oxide electrochemical cells by using in situ X-ray photoelectron spectroscopy. Nat. Mater. 9(11), 944–949 (2010). https://doi.org/10.1038/nmat2851
F. Tao, M.E. Grass, Y. Zhang et al., Reaction-driven restructuring of Rh-Pd and Pt-Pd core-shell nanoparticles. Science 322(5903), 932–934 (2008). https://doi.org/10.1126/science.1164170
G.A. Somorjai, H. Frei, J.Y. Park, Advancing the frontiers in nanocatalysis, biointerfaces, and renewable energy conversion by innovations of surface techniques. J. Am. Chem. Soc. 131(46), 16589–16605 (2009). https://doi.org/10.1021/ja9061954
M. Favaro, B. Jeong, P.N. Ross et al., Unravelling the electrochemical double layer by direct probing of the solid/liquid interface. Nat. Commun. 7, 12695 (2016). https://doi.org/10.1038/ncomms12695
N.J. Divins, A. Inma, E. Carlos et al., Influence of the support on surface rearrangements of bimetallic nanoparticles in real catalysts. Science 346(6209), 620–623 (2014). https://doi.org/10.1126/science.1258106
S. Axnanda, E.J. Crumlin, B. Mao et al., Using “Tender” X-ray ambient pressure X-ray photoelectron spectroscopy as a direct probe of solid-liquid interface. Sci. Rep. 5, 9788 (2015). https://doi.org/10.1038/srep09788
S.K. Eriksson, M. Hahlin, J.M. Kahk et al., A versatile photoelectron spectrometer for pressures up to 30 mbar. Rev. Sci. Instrum. 85(7), 075119 (2014). https://doi.org/10.1063/1.4890665
D. Teschner, A. Pestryakov, E. Kleimenov et al., High-pressure X-ray photoelectron spectroscopy of palladium model hydrogenation catalysts: part 1: effect of gas ambient and temperature. J. Catal. 230(1), 186–194 (2005). https://doi.org/10.1016/j.jcat.2004.11.036
S. Nemšák, E. Strelcov, H. Guo et al., In aqua electrochemistry probed by XPEEM: Experimental setup, examples, and challenges. Top. Catal. 61(20), 2195–2206 (2018). https://doi.org/10.1007/s11244-018-1065-4
N. Mårtensson, P. Baltzer, P.A. Brühwiler et al., A very high resolution electron spectrometer. J. Electron Spectrosc. Relat. Phenom. 70(2), 117–128 (1994). https://doi.org/10.1016/0368-2048(94)02224-N
F. Tao, S. Dag, L.-W. Wang et al., Break-up of stepped platinum catalyst surfaces by high CO coverage. Science 327(5967), 850–853 (2010). https://doi.org/10.1126/science.1182122
P. Gao, S. Li, X. Bu et al., Direct conversion of CO2 into liquid fuels with high selectivity over a bifunctional catalyst. Nat. Chem. 9(1), 1019–1024 (2017). https://doi.org/10.1038/nchem.2794
C. Zhang, M.E. Grass, Y. Yu et al., Multielement activity mapping and potential mapping in solid oxide electrochemical cells through the use of operando XPS. ACS Catal. 2(11), 2297–2304 (2012). https://doi.org/10.1021/cs3004243
C. Zhang, Y. Yu, M.E. Grass et al., Mechanistic studies of water electrolysis and hydrogen electro-oxidation on high temperature ceria-based solid oxide electrochemical cells. J. Am. Chem. Soc. 135(31), 11572–11579 (2013). https://doi.org/10.1021/ja402604u
M.O.M. Edwards, P.G. Karlsson, S.K. Eriksson et al., Increased photoelectron transmission in High-pressure photoelectron spectrometers using “swift acceleration”. Nucl. Instrum. Methods A 785, 191–196 (2015). https://doi.org/10.1016/j.nima.2015.02.047
Y. Han, S. Axnanda, E.J. Crumlin et al., Observing the electrochemical oxidation of Co metal at the solid/liquid interface using ambient pressure X-ray photoelectron spectroscopy. J. Phys. Chem. B. (2017). https://doi.org/10.1021/acs.jpcb.7b05982
M.F. Lichterman, S. Hu, M.H. Richter et al., Direct observation of the energetics at a semiconductor/liquid junction by operando X-ray photoelectron spectroscopy. Energy Environ. Sci. 8(8), 2409–2416 (2015). https://doi.org/10.1039/C5EE01014D
P. Baltzer, L. Karlsson, M. Lundqvist et al., Resolution and signal-to-background enhancement in gas-phase electron spectroscopy. Rev. Sci. Instrum. 64(8), 2179–2189 (1993). https://doi.org/10.1063/1.1143957
J.L. Campbell, T. Papp, Widths of the atomic K-N7 levels. Atomic Data Nucl. Data Tables 77(1), 1–56 (2001). https://doi.org/10.1006/adnd.2000.0848
H. Fellner-Feldegg, Ph.D. dissertation, Uppsala University, 1974
S. Mähl, M. Neumann, S. Dieckhoff et al., Characterisation of the VG ESCALAB instrumental broadening functions by XPS measurements at the Fermi edge of silver. J. Electron Spectrosc. Relat. Phenom. 85(3), 197–203 (1997). https://doi.org/10.1016/S0368-2048(97)00074-1
J.J. Olivero, R.L. Longbothum, Empirical fits to the Voigt line width: a brief review. J. Quant. Spectrosc. Radiat. Transf. 17(2), 233–236 (1977). https://doi.org/10.1016/0022-4073(77)90161-3
Y. Ning, Q. Fu, Y. Li et al., A near ambient pressure photoemission electron microscope (NAP-PEEM). Ultramicroscopy 200, 105–110 (2019). https://doi.org/10.1016/j.ultramic.2019.02.028
R. Follath, M. Hävecker, G. Reichardt, K. Lips, J. Bahrdt, F. Schäfers and P. Schmid, presented at the Journal of Physics: Conference Series, 2013 (unpublished)
G. Materlik, T. Rayment, D.I. Stuart, Diamond light source: status and perspectives. Philos. Trans. A Math. Phys. Eng. Sci 373(2036), 20130161 (2015). https://doi.org/10.1098/rsta.2013.0161
X. Liu, W. Yang, Z. Liu, Recent progress on synchrotron-based in-situ soft X-ray spectroscopy for energy materials. Adv. Mater. 26(46), 7710–7729 (2014). https://doi.org/10.1002/adma.201304676
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This work was supported by the National Natural Science Foundation of China (No. 11227902) as part of NSFC ME2 beamline project and Science and Technology Commission of Shanghai Municipality (No. 14520722100). Y.H., Y.Y., and B.M. are supported by National Natural Science Foundation of China (Nos. 21802096, 21832004, and 11805255).
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Cai, J., Dong, Q., Han, Y. et al. An APXPS endstation for gas–solid and liquid–solid interface studies at SSRF. NUCL SCI TECH 30, 81 (2019). https://doi.org/10.1007/s41365-019-0608-0
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DOI: https://doi.org/10.1007/s41365-019-0608-0