Surface and Electronic Structure Study of Substrate-dependent Pyrite Thin Films

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1 Surface and Electronic Structure Study of Substrate-dependent Pyrite Thin Films Talk Outline Stoichiometry and sodium study of pyrite thin films: Quick Review Surface structure of pyrite thin films Electronic structure of pyrite thin films Ming H. Cheng, Alexandria Margarella, Yu Liu Department of Chemistry, University of California, Irvine Department of Physics and Astronomy, University of California, Irvine John C. Hemminger group August 25,

2 Pyrite Thin Films Grown by MOCVD Substrates: Si, Glass Ar Carrier Gas or Ar/H 2 Mixtures Temperature: 300~350 C Precursors: Why Glass works?! Annealing in Elemental Sulfur above 450 C Law Research Group 2

3 Sodium on the Surface of Pyrite on Glass Na only exists on the surface (Na is removed by Ar Sputtering) Sulfur preferential sputtering (shown by the broadening of Fe-2p and S-2p peaks) Where does Na come from? 3

4 Water Effect of Pyrite on Glass Water remove Na from the surface of pyrite on glass Na-1s fitting 4

5 Stoichiometry of Pyrite Thin Films Single crystal Sample Area(%) Fe-2p S-2p S/Fe stoichio metry Fresh HF single crystal (From Moriz samples) pyrite on Si Pyrite on Si Atomic Sensitivity Factor: 4.17 (Lab XPS, Irvine) Polished pyrite single crystal with HF cleaning or HF:AA:HNO3 (1:1:2) cleaning Raw Data Moritz, Law Research Group 5

6 Pyrite on Glass with and w/o Annealing Pyrite on Glass- Before and After Annealing Band Gap Pyrite: 0.95 ev indirect transition Pyrite: 1.03 ev for direct transition Marcasite 0.34eV Marcasite XRD+XPS High quality pyrite thin films 6 Law Research Group

7 Surface Study of Pyrite Thin Films with Different Chemical Treatments Talk Outline Stoichiometry and sodium study of pyrite thin films Surface structure of pyrite thin films Electronic structure of pyrite thin films Photoelectric Current Reducing Impurities?! Defects?! Distortion Effect?! Crystal Phase?! Synchrotron Light Source: continuous tunable Substrate-Dependent Pyrite Thin Films o o o Pyrite on Si with Elemental Sulfur Annealing Pyrite on Glass without Annealing Pyrite on Glass with Elemental Sulfur Annealing Synchrotron Light (various hν) Lab XPS: 2~10 nm ALS: 0.5~1 nm Detector e - Z e - 7

8 Relative Count Surface Structure of Pyrite Thin Films S-2p of Pyrite on Si (KE=125eV) Raw Data Fitting Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur S-2p(Lab XPS) Collected Kinetic Energy (ev) 125 (~5Å) Bindng Energy (ev) S 2p BE (ev) Area(%) Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur Binding Energy Calibrated by Au 4f 159 M. Bronold et al. Surf. Sci. Lett. 314 (1994), pp. L931 L936 Note FeS 2 (FCC) Edge, loss one S S 2-8

9 Relative Count KE=800eV KE=300eV Depth Profile of Pyrite on Silicon S-2p of Pyrite on Si 800eV-Raw Data 800eV-Fitting 800eV-Bulk Sulfide 800eV-Surface Sulfide 800eV-Monosulfide 800eV-Elemental Sulfur Collected Kinetic Energy (ev) 800 (~14Å) 300 (~7Å) 125 (~5Å) S 2p BE (ev) Area(%) Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur Binding Energy Calibrated by Au 4f Electron Inelastic Mean Free Path KE=125eV Lab XPS: 2 nm ALS: 0.5~1.4 nm Bindng Energy (ev) 9

10 Depth Profile of Pyrite on Silicon Concentration (%, normalized to total area) Bulk Sulfide Surface Sulfide Monosulfide Elemental Sulfur Depth Profile of Sulfur of Pyrite on Si Collected Kinetic Energy (ev) Bulk Sulfide Concentration (%) Surface Monosul Sulfide fide Element al Sulfur Collected Kinetic Energy (ev) KE=125eV ~ 5Å KE=300eV ~ 7Å KE=800eV ~ 14Å Elemental Sulfur Monosulfide Surface Sulfide Bulk Sulfide Si 10

11 Relative Count KE=800eV KE=300eV KE=125eV Depth Profile of Pyrite on Glass S-2p of Pyrite on Glass 800eV-Raw Data 800eV-Fitting 800eV-Bulk Sulfide 800eV-Surface Sulfide 800eV-Monosulfide 800eV-Residual Sulfur S 2p BE (ev) Area(%) Bulk Sulfide Surface Sulfide Monosulfide Residual Sulfur Bulk Sulfide Surface Sulfide Monosulfide Residual Sulfur Bulk Sulfide Surface Sulfide Monosulfide Residual Sulfur Binding Energy Calibrated by Au 4f Collected Kinetic Energy (ev) Higher Binding Energy Species: Residual Sulfur?! Elemental Sulfur?! Bindng Energy (ev) 11

12 C-1s Spectra of Pyrite on Si and Glass C-1s of Pyrite Thin Films (KE=200eV) C-1s of Pyrite on Si (KE=200eV) C-1s of pyrite on Glass C-1s of pyrite on Si Relative Count Raw Data Adventitious carbon Abs. Count BeinfingEnergy (ev) C-1s of Pyrite on Glass (KE=200eV) 280 Adventitious: Residual: Raw Data Fitting Relative Count Adventitious carbon Residual Sulfur Bindng Energy (ev) Bindng Energy (ev)

13 Depth Profile of Pyrite on Glass Depth Profile of Sulfur of Pyrite on Glass Concentration (%, normalized to total area) Bulk Sulfide Surface Sulfide Monosulfide Residual Sulfur Collected Kinetic Energy (ev) Bulk Sulfide Concentration (%) Surface Monosul Sulfide fide Residual Sulfur Collected Kinetic Energy (ev) KE=125eV ~ 5Å KE=300eV ~ 7Å KE=800eV ~ 14Å Residual Sulfur Monosulfide Surface Sulfide Bulk Sulfide Si 13

14 Relative Count Depth Profile of Pyrite on Glass w/ Annealing S-2p of Pyrite on on Glass with Annealing 800eV-Raw Data 800eV-Fitting 800eV-Bulk Sulfide 800eV-Surface Sulfide 800eV-Sodium Sulfide 800eV-Elemental Sulfur KE=800eV KE=300eV S 2p BE (ev) Area(%) Bulk Sulfide Surface Sulfide Sodium Sulfide Elemental Sulfur Bulk Sulfide Surface Sulfide Sodium Sulfide Elemental Sulfur Bulk Sulfide Surface Sulfide Sodium Sulfide Elemental Sulfur Binding Energy Calibrated by Au 4f Collected Kinetic Energy (ev) KE=125eV Lower Binding Energy Species: Sodium Sulfide eV?! Monosulfide eV?! Bindng Energy 159 (ev) Lab XPS: 2 nm ALS: 0.5~1.4 nm 14

15 0.2 Depth Profile of Pyrite on Glass w/ Annealing Depth Profile of Na of Pyrite on Glass (with and without aneealing) Concentration (10XNa/S) Aglass-1 Aglass-2 Glass Collected Kinetic Energy (ev) Collected Kinetic Energy (ev) Concentration (Na 2s/ S 2p) AGlass-1 (X10) AGlass-2 (X10) Glass (X10)

16 Depth Profile of Pyrite on Glass w/ Annealing Depth Profile of Sulfur of Pyrite on Glass with Annealing Concentration (%, normalized to total area) Collected Kinetic Energy (ev) Bulk Sulfide Surface Sulfide Sodium Sulfide Elemental Sulfur Collected Kinetic Energy (ev) Bulk Sulfide Concentration (%) Surface Sodium Sulfide Sulfide Element al Sulfur

17 Surface Study of Pyrite Thin Films with Different Chemical Treatments Talk Outline Stoichiometry and sodium study of pyrite thin films Surface structure of pyrite thin films Electronic structure of pyrite thin films Lab XPS: 2~10 nm ALS: 0.5~1 nm Short Summary Surface chemical composition and stoichiometry (Lab XPS) Sulfur defects and the elemental composition depth profiles (ALS) 17

18 Electronic Structure Study of Pyrite Thin Films Talk Outline Stoichiometry and sodium study of pyrite thin films Surface structure of pyrite thin films Electronic structure of pyrite thin films Photoelectric Current Reducing Impurities?! Defects?! Distortion Effect?! Crystal Phase?! M. Bronold et al. Surf. Sci. Lett. 314 (1994), pp. L931 L936 CB tail: 0.4 ev above the VB edge Bulk Surface MIT group, Physical Review B 83, (2011) Yanning Zhang, Ruqian 18Wu

19 Band Gap Estimation of Pyrite on Thin Films 2568 Chem. Mater., Vol. 21, No. 13, 2009 VB only XAS + XES (S L-edge Spectrum only) M. Bronold et al. Surf. Sci. Lett. 314 (1994), pp. L931 L936 VB only XAS with XPS + VB (both Fe and S L-edge Spectra) 19

20 Relative Count Density of State of Valence Band VB of Pyrite-Glass (BL9) KE=200eV KE=400eV KE=600eV KE=700eV KE=800eV Binding Energy (ev) Bulk Band Gap 0.95 ev indirect transition 1.03 ev for direct transition Surface Band Gap 0.3~0.5 ev Slope (1/eV) Collected Kinetic Energy (ev) Pyrite-AGlass Photon Energy (ev) Slope (1/eV) AGlass-AVG Silicon Glass Substrates: Si, Glass, Glass with annealing

21 Density of State of Conduction Band Relative Count S L-edge of Pyrite on Different Substrates Si AGlass Glass Photon Energy (ev) Yanning Zhang, Ruqian Wu 21

22 Band Gap Estimation of Pyrite on Thin Films Relative Count Relative Count S L-edge of Pyrite on Si S L_edge VB 200KE Relative Energy (ev) 1 S L-edge of Pyrite on Glass with Annealing Band Gap Estimations half-half S-Ledge+VB VB only Pyrite Thin Films Silicon AGlass Glass Relative Count S L_edge VB 200KE Relative Energy (ev) S L-edge of Pyrite on Glass S L-edge VB 200KE Photon Energy (ev) 2568 Chem. Mater., Vol. 21, No. 13,

23 Band Gap Estimation of Pyrite on Thin Films DOS of Pyrite on Si (with error bar) Fe L_edge VB 200KE Band Gap Estimations Pyrite Thin Films Silicon AGlass Glass Relative Count 0.5 half-half S-Ledge+VB Relative Energy (ev) DOS of Pyrite on Si 1 VB only zero-zero Fe L-edge+VB Relative Count Fe L_edge 0.40 VB 200KE Relative Energy (ev) MIT group, Physical Review B 83, (2011) 23

24 Summary Surface and Electronic structures of substrate-dependent pyrite thin films grown by MOCVD Surface chemical composition and stoichiometry Sulfur defects and the elemental composition depth profiles Density of state of valence and conduction bands Band gap estimations 1. Surface Structure and Depth Profile Study of Pyrite Thin Films Grown by MOCVD 2. Depth Profile of Valence Photoemission and X-ray Absorption Study of Substrate-Dependent Pyrite Thin Films 24

25 Acknowledgements Hemminger Group, UC Irvine Ming H. Cheng Allie Margarella Kathryn A. Perrine Prof. Matt Law, Prof. Ruqian Wu, Dr. Yanning Zhang, Nicholas Berry, Moritz Limpinsel, Beamline Scientist: Hendrik Bluhm (BL11), Zhi Liu (BL9) 25

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