La superficie di film e cristalli di SrTiO 3
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1 U. Scotti di Uccio La superficie di film e cristalli di SrTiO 3 Coherentia-CNR-INFM Napoli, Italy Prof. R. Vaglio F. Miletto Granozio, N. Lampis, P. Perna, M. Radovic, A. Sambri M. Salluzzo, G. De Luca, R. Di Capua
2 Research activity on SrTiO 3 In Napoli: Applications 1. Substrate 2. SuFET, OFET 3. Dielectric properties, Breakdown field, etc. This presentation: Focus on fundamental physics 1. properties of SrTiO 3 surface at conditions of typical UHV deposition environments (LEED, STM, XPS, XRD) treatments up to 900 C - NO ion cleaning procedure 2. growth mode of thin films
3 Outline The MODA lab Surface properties #1 - First experiments and results Surface properties #2 - Comparison with literature Experimental support to basic ideas Surface properties #3 - Electronic and optical properties
4 Coherentia Labs. Napoli UHV base P < mbar Modular system for Oxide Deposition and Analyses PLD chamber AFM STM SPA-LEED XPS RHEED
5 PLD chamber Base pressure P = 5 x 10-9 mbar Radiative heater T max = 1000 C in air Quadrupole Residual gas determination High pressure RHEED Fast photography setup for analysis of the plume expansion
6 XPS chamber source detector Sample holder
7 Instrumental Setup SPA LEED Spot Profile Analysis LEED
8 Variable temperature STM/AFM
9 Surface properties #1 - Experimental First experiments and results
10 Surface properties #1 - Experimental Surface preparation Single crystal (100) SrTiO 3 with TiO 2 termination plane
11 Surface properties #1 - Experimental Surface preparation Low temperature annealing NO ion etching Single crystal (100) SrTiO 3 with TiO 2 termination plane Selective ethcing procedure Un. Twente, APL 73, 2920 (1998)
12 Surface properties #1 - Experimental 350 C O 2 C UHV 250x250 nm 2
13 Surface properties #1 - Experimental nm 250x250 nm 2
14 Surface properties #1 Experimental LEED patterns Simple perovskitic structure of SrTiO 3 SrTiO 3 single crystal (100)
15 Surface properties #1 - Experimental (100) SrTiO 3 - TiO 2 termination $! %$ %! (01) 2h UHV P < 10-9 Torr T = 910 C (-10) (10) (0-1) E = 22 C 1 1 lattice No reconstruction
16 Surface properties #1 - Experimental (100) SrTiO 3 - TiO 2 termination $! %$ %! (01) 2h UHV P < 10-9 Torr T = 800 C (-10) (10) Cps (0 0) (1 /2 0) (1 0) K // / K B Spot Analysis Profile LEED (0-1) E = C 2 1 lattice double domain
17 Surface properties #1 - Experimental (100) SrTiO 3 - TiO 2 termination 2 1 reconstruction double domain
18 Surface properties #1 - Experimental PLD homoepitaxial (100) STO film FILM DEPOSITION CONDITIONS: Eccimer laser KrF - λ = 248 nm Target substrate 41 mm P(O 2 ) = 0.1 mbar Effective Fluence: 80 mj /2.6 mm 2 Repetition rate: 2 Hz Deposition temperature: 890 C
19 Surface properties #1 - Experimental PLD homoepitaxial (100) STO film room temperature STM 2D island growth mode 10 pa 2 V Typical 10 pa 2 V T d = 890 C 1 µm 1 µm 1 µm 1 µm (100) Single crystal STO 1h UHV 900 C 20 nm thick (100) STO film 1h UHV 800 C
20 Surface properties #1 - Experimental PLD homoepitaxial (100) STO film $! %$ %! (01) c (2 2) reconstruction (-10) (10) (0-1) Reconstructions of films are different from crystals
21 Surface properties #1 - Experimental PLD homoepitaxial (100) STO film C(2 x 2) reconstruction
22 Stop and wonder Is SrTiO 3 a simple material? Is it interesting? Papers on SrTiO 3 surface (in my laptop that is, non-comprehensive) 25 papers on STO surface Science Nature PRL APL Surf. Sc. PRB M. R. Castell, Oxford Univ. J. Zegenaghen, Max Planck Inst. K. Szot, Julich M. Lippmaa, Tokio Univ.
23 Surface properties #2 Comparison with literature Experimental support to basic ideas
24 Surface properties #2 - Literature A critical review High temperature annealing NO Chemical etching Hypothesis: Ti-O termination - Ordered O Vacancies Q.D. Jiang, J. Zegenhagen Surface Science 425 (1999)
25 Surface properties #2 - Literature A critical review High temperature annealing Ion etching STM Ar Ion sputtering + UHV annealing Hypothesis: Ti-O termination - Ordered Sr Adatoms
26 Surface properties #2 - Literature Single crystal (100) SrTiO 3 2 x 1 C(6 x 4) Karen Johnston, Martin R. Castell, et al., PRB 70, (2004) Q.D. Jiang, J. Zegenhagen, Surf. Sc. 425, 343 (1999) Ti O V(O) Ti O V(O) C(2 x 2)
27 Surface properties #2 - Literature A critical review Evidence: Sr adatoms segregate at SrTiO 3 surface T. Ohnishi, K. Shibuya, and M. Lippmaa, APL 85, 272 (2004)
28 Surface properties #2 - Literature A critical review High temperature annealing NO Ion etching Hypothesis: Ti-O termination - Ordered Sr Adatoms % Sr coverage x2 C(4x4) 2x2 C(4x4) 4x T ( C) T. Kubo, H. Nozoye Surface Science 542 (2003)
29 Surface properties #2 - Literature A critical review O vacancy n type doping Typical values µ ~ 10 4 cm 2 V s 4.2 K, cm -3 K. Szot, et al., PRL 88, (2002) Short annealings high mobility Prolonged annealings disorder
30 Surface properties #2 - Experimental XPS data - Sr evolution at the surface 0.8 Sr increases up to ~500 C Sr 3d / Ti 2p Sr decreases above ~500 C T ( C)
31 Surface properties #2 - Experimental ID32 ESRF Grenoble Surface structure of SrTiO3 single crystal having nominal TiO 2 and SrO termination studied by Grazing Incidence X-Ray Diffraction (GXID) A. Fragneto, M. Salluzzo, U. Scotti di Uccio, R.Vaglio COHERENTIA CNR-INFM and Dipartimento di Scienze Fisiche, Università di Napoli Federico II X. Torrelles, Institut de Ciencia de Materials de Barcelona (C.S.I.C.) Campus de la U.A.B., Bellaterra, Barcelona, Spain C. Damen TSST, Twente Solid State Technology, Twente (Netherland)
32 Surface properties #2 - Experimental Measurements performed on several samples TiO 2 terminated Different nominal termination Different treatments Data analysis still incomplete Indications of 10% coverage of Sr-O on nominal Ti-O 2 surfaces (as-received samples) SrO terminated
33 Surface properties #2 - Experimental (110) STO SrO precipitates 400 x 400 nm C 500 x 500 nm C 500 x 500 nm C UHV annealing 550 C STM shows increasing disorder Log ( I / I o ) 20 C SPA LEED Scans along [ 110 ] k x (a. u.)
34 Surface properties #2 - Experimental (110) STO SrO precipitates 400 x 400 nm C 500 x 500 nm C 500 x 500 nm C UHV annealing STM shows increasing disorder LEED pattern is preserved! Log ( I / I o ) 550 C 20 C SPA LEED Scans along [ 110 ] k x (a. u.)
35 Surface properties #2 - Experimental (110) STO C UHV annealing Structure and electronic states on reduced SrTiO3 (110) H. Bando, et al. J. Vac. Sci. Technol. B 13, 1150, (1995) ( ) (6 x 4) reconstruction
36 Surface properties #2 - Experimental (110) STO C UHV annealing 200 x 200 nm 2 ( ) (6 x 4) reconstruction
37 Surface properties #2 - Experimental Single crystal (100) SrTiO 3 Is O responsible for the observed reconstructions on the (100) orientation of SrTiO 3? Surface BULK emission to the vacuum: high activation energy diffusion from the bulk: low activation energy O vacancies start at step edges and move through colunar defects SrTiO 3 (001) (2 1) reconstructions: First-principles calculations K. Johnston, M. R. Castell, A. T. Paxton, and M. W. Finnis PRB 70, (2004) Switching the electrical resistance K. Szot, et al., Nature Materials 5, 312 (2006)
38 Surface properties #2 - Experimental Single crystal (100) SrTiO 3 Is O responsible for the observed reconstructions on the (100) orientation of SrTiO 3? Surface 800 C annealing in UHV BULK Room temperature C annealings in UHV
39 Surface properties #2 - Experimental Single crystal (100) SrTiO 3 SrTiO 3 (100)K4 0 (010) a, E=148.9eV α α = 4 Γ = nm k = 7.02 % Γ = nm
40 Surface properties #2 - Experimental Single crystal (100) SrTiO 3 $! %$ %!$ (100) SrTiO 3 K 4 (010) Two domains One domain No reconstr. T = 23 C T = 255 C T = 280 C Line of O vacancies Reconstruction domain O diffusion from the bulk is filling vacancies
41 Surface properties #2 Tentative conclusions Sr at the surface is a desordered phase
42 Surface properties #2 Tentative conclusions Sr at the surface is a desordered phase Reconstructions are likely due to ordered oxygen vacancies
43 Surface properties #2 Issues supercell area x4 C(4x4) C(4x4) 1x2 2x T ( C) The observed 900 C is probably a inhomogeneous phase The explanation of the increasing order at increasing T is counterintuitive
44 Surface properties #3 Electronic and optical properties
45 Surface properties #3 Theory Electronic DOS Chemical scheme Sr ione 2+ O ione 2- Ti ione 4+ Sr [Kr] 5s 2 Sr 2+ [Kr] O [He] 2s 2 2p 4 O 2- [Ne] Ti [Ar] 3d 2 4s 2 Ti 4+ [Ar] empty full Sr 4p Ti 2p VB O 2p CB Ti 3d Sr 4d Ti 3d O 2p O 2s E- E F (ev)
46 Surface properties #3 Theory Electronic DOS 0.2 σ o e g pπ 0.1 π* σ π o π pσ t 2g 0.0 σ Ti 3d BE (ev) O 2p (O 2pπ + Ti t 2g ) pdπ π, π, π o (O 2pσ+ Ti e 2g ) pdσ σ, σ *, σ o
47 Surface properties #3 Experimental XPS Failing of the rigid band filling model 1.0 Preparation 500 C O 2 Counts (a. u.) O 2p Sr 4p + O 2s Ti 3p 800 C UHV Heating in UHV 100 C UHV 200 C UHV 300 C UHV BE (ev) XPS
48 Surface properties #3 Experimental XPS ev σ O 2p 5.4 ev π O 2p untreated sample ev O Vacancies 5.2 ev σ O 2p 7.4 ev π O 2p 200 C UHV annealing I (a.u.) 0.5 I (a.u.) BE (ev) BE (ev) O vacancies states F centres
49 Surface properties #3 Experimental XPS ev σ O 2p 5.4 ev π O 2p untreated sample ev O Vacancies 5.2 ev σ O 2p 7.4 ev π O 2p 200 C UHV annealing I (a.u.) 0.5 I (a.u.) BE (ev) BE (ev) O vacancies states F centres Ti 3d localized states
50 Surface properties #3 Experimental XPS ev σ O 2p 5.4 ev π O 2p untreated sample ev O Vacancies 5.2 ev σ O 2p 7.4 ev π O 2p 200 C UHV annealing I (a.u.) 0.5 I (a.u.) BE (ev) BE (ev) O vacancies states F centres Ti 3d localized states Correlation effects on Ti 3d t2 g
51 Surface properties #3 Experimental STM 2h 130 C (1 1) LEED pattern STM topography 120x120 nm 2
52 Surface properties #3 Experimental Electronic DOS 2h 130 C Counts (a. u.) E F 1 h 600 C in O h 130 C UHV normal emission Transparent sample Conducting surface 0.0 VB = 3.15 ev BE (ev) VB position = 3.15 ev Standard extrapolation High quality surface ' Shallow angle surface states Excess DOS at the surface
53 Surface properties #3 Experimental Electronic DOS 29 SEPTEMBER 2006 VOL 313 SCIENCE
54 Surface properties #3 Experimental STM 120x120 nm 2 2h 200 C STM Tunneling Spectroscopy I = 0.3 na, V bias = 1.5 V Volt - unoccupied SrTiO 3 states 50x25 nm Volt - occupied SrTiO 3 states
55 Surface properties #3 - Literature K. Szot, et al., Nature Materials 5, 312 (2006)
56 Surface properties #3 - Literature Recent breakthrow: blue photoluminescence Nature Materials 4, 816 (2005) Green UV Blue
57 Surface properties #3 Literature UPS 2.4 ev a 0.1 ev b 0.8 ev VB 3.2 ev T. Higuchi, et al., PRB 61, (2000) b VB 2.4 ev
58 Surface properties #3 Experimental Optical properties SrTiO 3 TIME-RESOLVED PHOTOLUMINESCENCE 355 nm 3rd harm Nd:YAG 1 intensity (a.u.) 0 STO wavelength nm monochromator photonmultiplier oscilloscope NonLinear Optical Spectroscopy Lab D. Paparo, L. Marrucci, A. Rubano
59 Surface properties #3 Experimental Optical properties TIME-RESOLVED PHOTOLUMINESCENCE voltage (mv) time (ns) 355 nm 3rd harm Nd:YAG Fast photodiode oscilloscope NonLinear Optical Spectroscopy Lab D. Paparo, L. Marrucci, A. Rubano
60 Surface properties #3 Experimental Optical properties XPS x ev 2.8 ev 2.4 ev VB
61 Surface properties #3 Conclusions STM, XPS, Fotoluminescence measurements give complementary information A consistent picture of SrTiO 3 electronic DOS is emerging
62 General conclusions SrTiO 3 is a complex, fascinating material
63 General conclusions SrTiO 3 is a complex, fascinating material There are several recent breakthroughs that open new perspectives for research and applications
64 General conclusions SrTiO 3 is a complex, fascinating material There are several recent breakthroughs that open new perspectives for research and applications There are controversial issues regarding surface properties (i.e. reconstructions) and DOS of doped samples Our research will continue Aknowledgements Special thanks to: The whole staff operating on MODA The whole staff of the NonLinear Optical Spectroscopy Lab A. Cassinese, A. Fragneto
65 General conclusions SrTiO 3 is a complex, fascinating material There are several recent breakthroughs that open new perspectives for research and applications There are controversial issues regarding surface properties (i.e. reconstructions) and DOS of doped samples Our research will continue Aknowledgements Special thanks to: The whole staff operating on MODA The whole staff of the NonLinear Optical Spectroscopy Lab A. Cassinese, A. Fragneto
66 References Selective ethcing procedure Stability of SrTiO 3 reconstructions Diffusion of oxygen in bulk SrTiO 3 Role of Sr adatoms TiO SrTiO 3 reconstructions Un. Twente, APL 73, 2920 (1998) K. Johnston, M. R. Castell, A. T. Paxton, and M. W. Finnis PRB 70, (2004) K. Szot, et al., Nature Materials 5, 312 (2006) T. Kubo, et al., Surf. Sci. 542 (2003) Q. Jiang, ej. Zegenhagen, Surf. Sci. Lett. 367, L42 (1996) U. Diebold, Surf. Sci. Rep. 48, 53 (2003) Yong Liang, et al., PRB 63, (2001) H. Bando, et al. J. Vac. Sci. Technol. B 13, 1150, (1995)
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