Abstract
In the last several decades, a variety of surface analysis techniques which can probe the geometric/electronic/molecular structures of the interfaces, as well as the elemental composition, have been developed and applied for the investigation of electrochemical processes taking place at solid–liquid interfaces. Designing spectroelectrochemical cells is one of the big challenges for utilization of those techniques to a variety of electrochemical interfaces because the thickness of solution layers, materials used as a window, geometry of the photon source, sample, and spectrometer/analyzer/detector need to be optimal for the electrochemical reaction of interest and photons used in the individual techniques. To date, various unique spectroelectrochemical cells have been used for in situ electrochemical studies on interfacial processes even by using the techniques which intrinsically require vacuum. In this paper, recent progress on in situ spectroelectrochemical cells, especially used for X-ray photoelectron spectroscopy, is reviewed.
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References
Masuda T, Uosaki K (2017) Chap. 6. Novel In Situ Techniques. In: Uosaki K (ed) Electrochemical Science for a Sustainable Society A Tribute to J. O’M Bockris. Springer International Publishing, Switzerland, pp 147–174
Uosaki K (2015) In situ real-time monitoring of geometric, electronic, and molecular structures at solid/liquid interfaces. Jpn J Appl Phys 54:030102
Abruña HD, Interfaces E (1991) Modern Techniques for In-situ Interface Characterization. VCH Publishers, New York-Weinheim-Cambridge
Lipkowski J, Ross PN (1992) Adsorption of Molecules at Metal Electrodes. Frontiers of Electrochemistry. VCH Publishers, New York-Weinheim-Cambridge
Lipkowski J, Ross PN (1993) Structure of Electrified Interfaces. Frontiers of Electrochemistry. VCH Publishers, New York-Weinheim-Cambridge
Wieckowski A (1999) Interfacial Electrochemistry: Experimental, Theory and Applications. Marcel Dekker, New York
Itkis DM, Velasco-Velez JJ, Knop-Gericke A, Vyalikh A, Avdeev MV, Yashina LV (2015) Probing Operating Electrochemical Interfaces by Photons Neutrons Chemelectrochem 2:1427–1445
Masuda T, Kondo T, Uosaki K (2016) Chap. 31. Solid–liquid Interfaces. In: Iwasawa Y, Asakura K, Tada M (eds) XAFS Techniques for Catalysts, Nanomaterials, and Surfaces. Springer International Publishing, Switzerland, pp 505–525
Kondo T, Masuda T, Uosaki K (2016) Chap. 7. In: Situ SXS and XAFS Measurements of Electrochemical Interface. In: Kumar CSSR (eds) X-ray and Neutron Techniques for Nanomaterials Characterization. Springer-Verlag, Berlin Heidelberg, pp 367–449
Lovelock KRJ, Villar-Garcia IJ, Maier F, Steinruck HP, Licence P (2010) Photoelectron Spectroscopy of Ionic Liquid-Based Interfaces. Chem Rev 110:5158–5190
Starr DE, Liu Z, Havecker M, Knop-Gericke A, Bluhm H (2013) Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy. Chem Soc Rev 42:5833–5857
Crumlin EJ, Liu Z, Bluhm H, Yang WL, Guo JH, Hussain Z (2015) X-ray spectroscopy of energy materials under in situ/operando conditions. J Electron Spectrosc Relat Phenom 200:264–273
Stoerzinger KA, Hong WT, Crumlin EJ, Bluhm H, Shao-Horn Y (2015) Insights into Electrochemical Reactions from Ambient Pressure Photoelectron Spectroscopy. Acc Chem Res 48:2976–2983
Trotochaud L, Head AR, Karslioglu O, Kyhl L, Bluhm H (2017) Ambient pressure photoelectron spectroscopy: practical considerations and experimental frontiers. J Phys Condens Matter 29:053002
Wu CH, Weatherup RS, Salmeron MB (2015) Probing electrode/electrolyte interfaces in situ by X-ray spectroscopies: old methods, new tricks. Phys Chem Chem Phys 17:30229–30239
Kolmakov A, Gregoratti L, Kiskinova M, Gunther S (2016) Recent Approaches for Bridging the Pressure Gap in Photoelectron Microspectroscopy. Top Catal 59:448–468
Liu XH, Liu Y, Kushima A, Zhang SL, Zhu T, Li J, Huang JY (2012) In Situ TEM Experiments of Electrochemical Lithiation and Delithiation of Individual Nanostructures. Adv Energy Mater 2:722–741
Huang JY, Zhong L, Wang CM, Sullivan JP, Xu W, Zhang LQ, Mao SX, Hudak NS, Liu XH, Subramanian A, Fan HY, Qi LA, Kushima A, Li J (2010) In Situ Observation of the Electrochemical Lithiation of a Single SnO2 Nanowire Electrode. Science 330:1515–1520
Holtz ME, Yu YC, Gunceler D, Gao J, Sundararaman R, Schwarz KA, Arias TA, Abruña HD, Muller DA (2014) Nanoscale Imaging of Lithium Ion Distribution During In Situ Operation of Battery Electrode and Electrolyte. Nano Lett 14:1453–1459
Zeng ZY, Liang WI, Liao HG, Xin HLL, Chu YH, Zheng HM (2014) Visualization of electrode-electrolyte interfaces in LiPF6/EC/DEC electrolyte for lithium ion batteries via in situ TEM. Nano Lett 14:1745–1750
Gu M, Parent LR, Mehdi BL, Unocic RR, McDowell MT, Sacci RL, Xu W, Connell JG, Xu PH, Abellan P, Chen XL, Zhang YH, Perea DE, Evans JE, Lauhon LJ, Zhang JG, Liu J, Browning ND, Cui Y, Arslan I, Wang CM (2013) Demonstration of an Electrochemical Liquid Cell for Operando Transmission Electron Microscopy Observation of the Lithiation/Delithiation Behavior of Si Nanowire Battery Anodes. Nano Lett 13:6106–6112
Wu F, Yao N (2015) Advances in sealed liquid cells for in-situ TEM electrochemical investigation of lithium-ion battery. Nano Energy 11:196–210
Bewick A, Kunimatsu K, Pons BS, Russell JW (1984) Electrochemically Modulated Infrared-Spectroscopy (EMIRS) - Experimental Details. J Electroanal Chem 160:47–61
Ataka K, Yotsuyanagi T, Osawa M (1996) Potential-dependent reorientation of water molecules at an electrode/electrolyte interface studied by surface-enhanced infrared absorption spectroscopy. J Phys Chem 100:10664–10672
Iwasawa Y (1996) X-ray Absorption Fine Structure for Catalyst and Surfaces. World Scientific, Singapore
Masuda T, Uosaki K (2017) In situ determination of electronic structure at solid/liquid interfaces. J Electron Spectrosc Relat Phenom 221:88–98
Gorlin Y, Lassalle-Kaiser B, Benck JD, Gul S, Webb SM, Yachandra VK, Yano J, Jaramillo TF (2013) In Situ X-ray Absorption Spectroscopy Investigation of a Bifunctional Manganese Oxide Catalyst with High Activity for Electrochemical Water Oxidation and Oxygen Reduction. J Am Chem Soc 135:8525–8534
Velasco-Velez JJ, Wu CH, Wang BY, Sun Y, Zhang Y, Guo JH, Salmeron M (2014) Polarized X-ray Absorption Spectroscopy Observation of Electronic and Structural Changes of Chemical Vapor Deposition Graphene in Contact with Water. J Phys Chem C 118:25456–25459
Velasco-Velez JJ, Wu CH, Pascal TA, Wan LWF, Guo JH, Prendergast D, Salmeron M (2014) The structure of interfacial water on gold electrodes studied by X-ray absorption spectroscopy. Science 346:831–834
Seidel R, Pohl MN, Ali H, Winter B, Aziz EF (2017) Advances in liquid phase soft-X-ray photoemission spectroscopy: a new experimental setup at BESSY II. Rev Sci Instrum 88:073107
Tokushima T, Horikawa Y, Harada Y, Takahashi O, Hiraya A, Shin S (2009) Selective observation of the two oxygen atoms at different sites in the carboxyl group (-COOH) of liquid acetic acid. Phys Chem Chem Phys 11:1679–1682
Niwa H, Kiuchi H, Miyawaki J, Harada Y, Oshima M, Nabae Y, Aoki T (2013) Operando soft X-ray emission spectroscopy of iron phthalocyanine-based oxygen reduction catalysts. Electrochem Commun 35:57–60
Harada Y, Tokushima T, Horikawa Y, Takahashi O, Niwa H, Kobayashi M, Oshima M, Senba Y, Ohashi H, Wikfeldt KT, Nilsson A, Pettersson LGM, Shin S (2013) Selective probing of the OH or OD stretch vibration in liquid water using resonant inelastic soft-X-ray scattering. Phys Rev Lett 111:193001
Asakura D, Nanba Y, Okubo M, Mizuno Y, Niwa H, Oshima M, Zhou HS, Okada K, Harada Y (2014) Distinguishing between High- and Low-Spin States for Divalent Mn in Mn-Based Prussian Blue Analogue by High-Resolution Soft X-ray Emission Spectroscopy. J Phys Chem Lett 5:4008–4013
Nagasaka M, Yuzawa H, Horigome T, Hitchcock AP, Kosugi N (2013) Electrochemical Reaction of Aqueous Iron Sulfate Solutions Studied by Fe L-Edge Soft X-ray Absorption Spectroscopy. J Phys Chem C 117:16343–16348
Nagasaka M, Yuzawa H, Horigome T, Kosugi N (2014) In operando observation system for electrochemical reaction by soft X-ray absorption spectroscopy with potential modulation method. Rev Sci Instrum 85:104105
Kotz R (1990) Photoelectron Spectroscopy of Practical Electrode Material. In: Gerischer H, Tobias CW (eds) Advances in Electrochemical Science and Engineering, vol 1. VCH Publishers Inc., New York, pp 76–123
Vericat C, Wakisaka M, Haasch R, Bagus PS, Wieckowski A (2004) Binding energy of ruthenium submonolayers deposited on a Pt(111) electrode. J Solid State Electrochem 8:794–803
Mayer T, Lebedev M, Hunger R, Jaegermann W (2005) Elementary processes at semiconductor/electrolyte interfaces: Perspectives and limits of electron spectroscopy. Appl Surf Sci 252:31–42
Wakisaka M, Mitsui S, Hirose Y, Kawashima K, Uchida H, Watanabe M (2006) Electronic structures of Pt-Co and Pt-Ru alloys for Co-tolerant anode catalysts in polymer electrolyte fuel cells studied by EC-XPS. J Phys Chem B 110:23489–23496
Wakisaka M, Udagawa Y, Suzuki H, Uchida H, Watanabe M (2011) Structural effects on the surface oxidation processes at Pt single-crystal electrodes studied by X-ray photoelectron spectroscopy. Energy Environ Sci 4:1662–1666
Lebedev MV, Calvet W, Kaiser B, Jaegermann W (2017) Synchrotron Photoemission Spectroscopy Study of p-GaInP2(100) Electrodes Emersed from Aqueous HCI Solution under Cathodic Conditions. J Phys Chem C 121:8889–8901
Ogletree DF, Bluhm H, Lebedev G, Fadley CS, Hussain Z, Salmeron M (2002) A differentially pumped electrostatic lens system for photoemission studies in the millibar range. Rev Sci Instrum 73:3872–3877
Salmeron M, Schlogl R (2008) Ambient pressure photoelectron spectroscopy: A new tool for surface science and nanotechnology. Surf Sci Rep 63:169–199
Ketteler G, Ogletree DF, Bluhm H, Liu HJ, Hebenstreit ELD, Salmeron M (2005) In situ spectroscopic study of the oxidation and reduction of Pd(111). J Am Chem Soc 127:18269–18273
Yamamoto S, Andersson K, Bluhm H, Ketteler G, Starr DE, Schiros T, Ogasawara H, Pettersson LGM, Salmeron M, Nilsson A (2007) Hydroxyl-induced wetting of metals by water at near-ambient conditions. J Phys Chem C 111:7848–7850
Porsgaard S, Jiang P, Borondics F, Wendt S, Liu Z, Bluhm H, Besenbacher F, Salmeron M (2011) Charge State of Gold Nanoparticles Supported on Titania under Oxygen Pressure. Angew Chem Int Ed 50:2266–2269
Shimada T, Mun BS, Nakai IF, Banno A, Abe H, Iwasawa Y, Ohta T, Kondoh H (2010) Irreversible Change in the NO Adsorption State on Pt(111) under High Pressure Studied by AP-XPS, NEXAFS, and STM. J Phys Chem C 114:17030–17035
Zhang CJ, Grass ME, McDaniel AH, DeCaluwe SC, El Gabaly F, Liu Z, McCarty KF, Farrow RL, Linne MA, Hussain Z, Jackson GS, Bluhm H, Eichhorn BW (2010) Measuring fundamental properties in operating solid oxide electrochemical cells by using in situ X-ray photoelectron spectroscopy. Nat Mater 9:944–949
Lu YC, Crumlin EJ, Veith GM, Harding JR, Mutoro E, Baggetto L, Dudney NJ, Liu Z, Shao-Horn Y (2012) In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions. Sci Rep 2:715
Toyoshima R, Yoshida M, Monya Y, Kousa Y, Suzuki K, Abe H, Mun BS, Mase K, Amemiya K, Kondoh H (2012) In Situ Ambient Pressure XPS Study of CO Oxidation Reaction on Pd(111) Surfaces. J Phys Chem C 116:18691–18697
Nemsak S, Shavorskiy A, Karslioglu O, Zegkinoglou I, Rattanachata A, Conlon CS, Keqi A, Greene PK, Burks EC, Salmassi F, Gullikson EM, Yang SH, Liu K, Bluhm H, Fadley CS (2014) Concentration and chemical-state profiles at heterogeneous interfaces with sub-nm accuracy from standing-wave ambient-pressure photoemission. Nat Commun 5:5441
Trotochaud L, Tsyshevsky R, Holdren S, Fears K, Head AR, Yu Y, Karshoglu O, Pletincx S, Eichhorn B, Owrutsky J, Long J, Zachariah M, Kuklja MM, Bluhm H (2017) Spectroscopic and computational investigation of room-temperature decomposition of a chemical warfare agent simulant on polycrystalline cupric oxide. Chem Mater 29:7483–7496
Karslioglu O, Nemsak S, Zegkinoglou I, Shavorskiy A, Hartl M, Salmassi F, Gullikson EM, Ng ML, Rameshan C, Rude B, Bianculli D, Cordones AA, Axnanda S, Crumlin EJ, Ross PN, Schneider CM, Hussain Z, Liu Z, Fadley CS, Bluhm H (2015) Aqueous solution/metal interfaces investigated in operando by photoelectron spectroscopy. Faraday Discuss 180:35–53
Axnanda S, Crumlin EJ, Mao BH, Rani S, Chang R, Karlsson PG, Edwards MOM, Lundqvist M, Moberg R, Ross P, Hussain Z, Liu Z (2015) Using “Tender” X-ray Ambient Pressure X-Ray Photoelectron Spectroscopy as A Direct Probe of Solid–liquid Interface. Sci Rep 5:9788
Favaro M, Jeong B, Ross PN, Yano J, Hussain Z, Liu Z, Crumlin EJ (2016) Unravelling the electrochemical double layer by direct probing of the solid/liquid interface. Nat Commun 7:12695
Lichterman MF, Hu S, Richter MH, Crumlin EJ, Axnanda S, Favaro M, Drisdell W, Hussain Z, Mayer T, Brunschwig BS, Lewis NS, Liu Z, Lewerenz HJ (2015) Direct observation of the energetics at a semiconductor/liquid junction by operando X-ray photoelectron spectroscopy. Energy Environ Sci 8:2409–2416
Lichterman MF, Richter MH, Hu S, Crumlin EJ, Axnanda S, Favaro M, Drisdell W, Hussain Z, Brunschwig BS, Lewis NS, Liu Z, Lewerenz HJ (2016) An Electrochemical, Microtopographical and Ambient Pressure X-Ray Photoelectron Spectroscopic Investigation of Si/TiO2/Ni/Electrolyte Interfaces. J Electrochem Soc 163:H139–H146
Casalongue HS, Kaya S, Viswanathan V, Miller DJ, Friebel D, Hansen HA, Nørskov JK, Nilsson A, Ogasawara H (2013) Direct observation of the oxygenated species during oxygen reduction on a platinum fuel cell cathode. Nat Commun 4:2817
Arrigo R, Hävecker M, Schuster ME, Ranjan C, Stotz E, Knop-Gericke A, Schlögl R (2013) In Situ Study of the Gas-Phase Electrolysis of Water on Platinum by NAP-XPS. Angew. Chem Int Ed 52:11660–11664
Takagi Y, Wang H, Uemura Y, Ikenaga E, Sekizawa O, Uruga T, Ohashi H, Senba Y, Yumoto H, Yamazaki H, Goto S, Tada M, Iwasawa Y, Yokoyama T (2014) In situ study of an oxidation reaction on a Pt/C electrode by ambient pressure hard X-ray photoelectron spectroscopy. Appl Phys Lett 105:131602
Takagi Y, Wang H, Uemura Y, Nakamura T, Yu LW, Sekizawa O, Uruga T, Tada M, Samjeske G, Iwasawa Y, Yokoyama T (2017) In situ study of oxidation states of platinum nanoparticles on a polymer electrolyte fuel cell electrode by near ambient pressure hard X-ray photoelectron spectroscopy. Phys Chem Chem Phys 19:6013–6021
Takagi Y, Nakamura T, Yu LW, Chaveanghong S, Sekizawa O, Sakata T, Uruga T, Tada M, Iwasawa Y, Yokoyama T (2017) X-ray photoelectron spectroscopy under real ambient pressure conditions. Appl Phys Express 10:076603
Doh WH, Gregoratti L, Amati M, Zafeiratos S, Law YT, Neophytides SG, Orfanidi A, Kiskinova M, Savinova ER (2014) Scanning Photoelectron Microscopy Study of the Pt/Phosphoric-Acid-Imbibed Membrane Interface under Polarization. Chemelectrochem 1:180–186
Law YT, Zafeiratos S, Neophytides SG, Orfanidi A, Costa D, Dintzer T, Arrigo R, Knop-Gericke A, Schlogld R, Savinova ER (2015) In situ investigation of dissociation and migration phenomena at the Pt/electrolyte interface of an electrochemical cell. Chem Sci 6:5635–5642
Saveleva VA, Papaefthimiou V, Daletou MK, Doh WH, Ulhaq-Bouillet C, Diebold M, Zafeiratos S, Savinova ER (2016) Operando Near Ambient Pressure XPS (NAP-XPS) Study of the Pt Electrochemical Oxidation in H2O and H2O/O-2 Ambients. J Phys Chem C 120:15930–15940
Johnston M, Lee JJ, Chottiner GS, Miller B, Tsuda T, Hussey CL, Scherson DA (2005) Electrochemistry in ultrahigh vacuum: Underpotential deposition of Al on polycrystalline W and Au from room temperature AlCl3/1-ethyl-3-methylimidazolium chloride melts. J Phys Chem B 109:11296–11300
Kuwabata S, Tsuda T, Torimoto T (2010) Room-Temperature Ionic Liquid. A New Medium for Material Production and Analyses under Vacuum Conditions. J Phys Chem Lett 1:3177–3188
Smith EF, Villar Garcia IJ, Briggs D, Licence P (2005) Ionic liquids in vacuo; solution-phase X-ray photoelectron spectroscopy. Chem Commun 5633–5635
Smith EF, Rutten FJM, Villar-Garcia IJ, Briggs D, Licence P (2006) Ionic liquids in vacuo: Analysis of liquid surfaces using ultra-high-vacuum techniques. Langmuir 22:9386–9392
Taylor AW, Qiu FL, Villar-Garcia IJ, Licence P (2009) Spectroelectrochemistry at ultrahigh vacuum: in situ monitoring of electrochemically generated species by X-ray photoelectron spectroscopy. Chem Commun 5817–5819
Qiu FL, Taylor AW, Men S, Villar-Garcia IJ, Licence P (2010) An ultra high vacuum-spectroelectrochemical study of the dissolution of copper in the ionic liquid (N-methylacetate)-4-picolinium bis(trifluoromethylsulfonyl)imide. Phys Chem Chem Phys 12:1982–1990
Wibowo R, Aldous L, Jacobs RMJ, Manan NSA, Compton RG (2011) In situ electrochemical-X-ray Photoelectron Spectroscopy: Rubidium metal deposition from an ionic liquid in competition with solvent breakdown. Chem Phys Lett 517:103–107
Kolmakov A, Dikin DA, Cote LJ, Huang JX, Abyaneh MK, Amati M, Gregoratti L, Gunther S, Kiskinova M (2011) Graphene oxide windows for in situ environmental cell photoelectron spectroscopy. Nat Nanotechnol 6:651–657
Masuda T, Yoshikawa H, Noguchi H, Kawasaki T, Kobata M, Kobayashi K, Uosaki K (2013) In situ X-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents. Appl Phys Lett 103:111605
Kraus J, Reichelt R, Gunther S, Gregoratti L, Amati M, Kiskinova M, Yulaev A, Vlassiouk I, Kolmakov A (2014) Photoelectron spectroscopy of wet and gaseous samples through graphene membranes. Nanoscale 6:14394–14403
Velasco-Velez JJ, Pfeifer V, Havecker M, Weatherup RS, Arrigo R, Chuang CH, Stotz E, Weinberg G, Salmeron M, Schlogl R, Knop-Gericke A (2015) Photoelectron Spectroscopy at the Graphene-Liquid Interface Reveals the Electronic Structure of an Electrodeposited Cobalt/Graphene Electrocatalyst. Angew Chem Int Ed 54:14554–14558
Nemšák S, Strelcov E, Duchoň T, Guo H, Hackl J, Yulaev A, Vlassiouk I, Mueller DN, Schneider CM, Kolmakov A (2017) Interfacial electrochemistry in liquids probed with photoemission electron microscopy. J Am Chem Soc 139:18138–18141
Guo HX, Strelcov E, Yulaev A, Wang J, Appathurai N, Urquhart S, Vinson J, Sahu S, Zwolak M, Kolmakov A (2017) Enabling Photoemission Electron Microscopy in Liquids via Graphene-Capped Microchannel Arrays. Nano Lett 17:1034–1041
Kobayashi K, Kobata M, Iwai H (2013) Development of a laboratory system hard X-ray photoelectron spectroscopy and its applications. J Electron Spectrosc Relat Phenom 190:210–221
Tsunemi E, Watanabe Y, Oji H, Cui YT, Son JY, Nakajima A (2015) Hard X-ray photoelectron spectroscopy using an environmental cell with silicon nitride membrane windows. J Appl Phys 117:234902
Velasco-Velez JJ, Pfeifer V, Havecker M, Wang R, Centeno A, Zurutuza A, Algara-Siller G, Stotz E, Skorupska K, Teschner D, Kube P, Braeuninger-Weimer P, Hofmann S, Schlogl R, Knop-Gericke A (2016) Atmospheric pressure X-ray photoelectron spectroscopy apparatus: bridging the pressure gap. Rev Sci Instrum 87:053121
Weatherup RS, Eren B, Hao YB, Bluhm H, Salmeron MB (2016) Graphene Membranes for Atmospheric Pressure Photoelectron Spectroscopy. J Phys Chem Lett 7:1622–1627
Ma T, Miyazaki K, Ariga H, Takakusagi S, Asakura K (2015) Investigation of the Cleanliness of Transferred Graphene: The First Step toward Its Application as a Window Material for Electron Microscopy and Spectroscopy. Bull Chem Soc Jpn 88:1029–1035
Acknowledgements
The present work was partially supported by the Development of Environmental Technology using Nanotechnology from the Ministry of Education, Culture, Sports, Science and Technology (MEXT), Japan. T.M. acknowledges the Japan Science and Technology Agency, PRESTO, for financial support. Synchrotron radiation experiments were performed as projects approved by the Japan Synchrotron Radiation Research Institute (JASRI) (Proposal Nos. 2011B4609, 2012A4611, 2012B4605, 2013B3601, and 2013B4601).
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Masuda, T. Various spectroelectrochemical cells for in situ observation of electrochemical processes at solid–liquid interfaces. Top Catal 61, 2103–2113 (2018). https://doi.org/10.1007/s11244-018-1067-2
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DOI: https://doi.org/10.1007/s11244-018-1067-2