Zadání diplomové práce
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3 Zadání diplomové práce Ústav: Ústav fyzikálního inženýrství Student: Bc. Zdeněk Jakub Studijní program: Aplikované vědy v inženýrství Studijní obor: Fyzikální inženýrství a nanotechnologie Vedoucí práce: Ing. Miroslav Bartošík, Ph.D. Akademický rok: 2015/16 Ředitel ústavu Vám v souladu se zákonem č.111/1998 o vysokých školách a se Studijním a zkušebním řádem VUT v Brně určuje následující téma diplomové práce: Příprava vzorků pro elektrochemické studium povrchů transport vzorku mezi UHV a elektrochemickým prostředím Stručná charakteristika problematiky úkolu: K dalšímu vývoji nízkoteplotních palivových článků je třeba nalézt vhodný katalyzátor pro redukci kyslíku. Hledaný katalyzátor by měl v ideálním případě být levný, stabilní a neškodný k životnímu prostředí. Nedávné publikace napovídají, že některé oxidy mohou mít katalytickou aktivitu pro redukci kyslíku srovnatelnou s platinou, dosud však není zcela jasné, proč tomu tak je. Mnoho oxidů relevantních pro katalýzu je již základně prozkoumáno pomocí ultravakuových metod, detailní výzkum stále probíhá (např. studium vlastností různých adatomů na magnetitu Fe3O4). Pro další výzkum v tomto směru je nutné porozumět vlastnostem vybraných povrchů i v elektrochemickém prostředí. Cíle diplomové práce: 1. Navrhnout a sestrojit systém pro transport vzorků z UHV komory do elektrochemického prostředí. Systém musí minimalizovat kontaminaci vzorků z atmosféry, měl by být snadný na obsluhu a měl by umožňovat transport vzorků různých velikostí a tvarů. 2. Otestovat sestrojený UHV-EC transfer systém měřením voltametrie známých standartních vzorků, např. Au(111) v kyselině sírové nebo Pt(111) v kyselině chloristé. 3. Vyvinout postup UHV přípravy vzorků pro in-situ elektrochemické STM. 4. Provádět další studium systémů kov/fe3o4. Seznam literatury: H. E. HOSTER, H. A. GASTEIGER. Ex-situ surface preparation and analysis: Transfer between UHV and electrochemical cell, Handbook of Fuel Cells Fundamentals, Technology and Applications, John Wiley & Sons, Ltd, 2003, ISBN: Fakulta strojního inženýrství, Vysoké učení technické v Brně / Technická 2896/2 / / Brno
4 M.H.M. AHMED, F.P. LYDIATT, D. CHEKULAEV, P.L. WINCOTT, D.J. VAUGHAN, J.H. JANG, S. BALDELLI, A.G. THOMAS, W.S. WALTERS, et al. Wet chemically prepared rutile TiO2(110) and TiO2(011): Substrate preparation for surface studies under non-uhv conditions. Surface Science. 2014, 630: DOI: /j.susc A. J. BARD, L. R. FAULKNER. Electrochemical methods: fundamentals and applications. New York: Wiley, 2001, 833 p. ISBN Termín odevzdání diplomové práce je stanoven časovým plánem akademického roku 2015/16 V Brně, dne L. S. prof. RNDr. Tomáš Šikola, CSc. ředitel ústavu doc. Ing. Jaroslav Katolický, Ph.D. děkan fakulty Fakulta strojního inženýrství, Vysoké učení technické v Brně / Technická 2896/2 / / Brno
5 3 4 α 2 3 ( 2 2)R α α ( 2 2)R ( 2 2)R45 α 2 3 α
6 3 4 α α 2 3
7
8
9
10
11 3 4 α 2 3
12 α
13 α α α 2 3 α α α 2 3
14 3 4 α 2 3
15 x x
16 tet oct oct 3+ oct 3 4 oct tet {111} {100} {111} {100} {110}
17 3 4 {111} tet oct 2 4 oct 2 4 ( 2 2) R p = ) int tet int oct int R p = 0.125
18 a) sufrace b) hydroxyls n w n w n w n w sufrace hydroxyls 1 nm oct int oct int oct int int
19 3 4 ( 2 2)
20 α
21 α α { }
22 3 4 α 3 3 α 2 3 (1 1) (2 1) (1 1) (2 1) (1 1) (2 1) 2+ (2 1)
23 α 2 3 (1 1) (2 1) (1 1) (2 1) (2 1) 2 (2 1) (1 1) (1 1) 2 (2 2) 2 (1 1) (2 1)
24
25 ψ( r,t) Ψ 2 i Ψ( r,t) t = Ψ( r,t) + V ( r,t)ψ( r,t), 2m h/2π V V ( r) t i Ψ(x,t) t = Ψ(x,t) + V (x)ψ(x,t), 2m Ψ(x,t) Ψ(x,t) = ψ(x)φ(t)
26 ψ(x) φ(t) 2m ψ(x) 1 + V (x) ψ(x) = E, i φ) 1 t φ(t) = E, V 0 > E L ψ(x) = A exp(ikx) + B exp( ikx), k k = 2m(V (x) E). V (x) = 0 k V (x) = V 0 > E A B P P = Ψ 3 Ψ 1 = A2 3 A 2 1 = exp( 2k2 L). V 0 L Ψ 1 Ψ 3 x
27
28 z z z
29 E kin = hν E b Φ spec, hν E b Φ spec sample spectrometer e - vacuum level Fermi level hν E k * Φ sample E k Φ spec inner shell E b E k = hν E b Φ spec
30 X-rays Al foil filament e - Mg anode Al anode water cooling 15
31 s Photoelectron excitation Auger electron excitation Fermi level L 2,3 L 1 hν K α
32 1 2 λ = h 2mE, ki k f = G, k i k f G g 1 g 2 g 1 = 2π a 1 n a 2 a 2, g 2 = 2π n a 1 a 1 a 2, a 1 a 2 n k z
33 k f G k i k z 10 2
34 E m E d E m E d E d E m i
35 E = E 0 + RT nf ln a ox, a red E E 0 R T K n F a ox a red 59/n n
36
37
38
39
40 φ p main = p LL =
41 D C LEED XYZ manipulator X-Ray source B STM Load-lock A
42
43 z manipulator CF flange connection microparticles generate in the bellows metal microparticles axis of magnetic transfer rod copper gasket sample loading Electrochemical cell
44
45 2
46 a) b)
47 glass capillary vetical transfer PEEK holder dropmaker KF flange Electrochemical cell
48 2
49
50 Side view Top view Ports: GL 18 for reference electrode GL 18 for counter electrode GL 18 + needle valve for gas in GL 18 + needle valve for gas bubbler 3x GL 14 for possible future needs 1x ball joint for gas out
51 Gas in (wall) Swagelok valves venting line overpressure valve Ar out syringe gate valve Load-lock dropmaker needle valves Ar out Gas bubbler electrolyte out 2
52 Scan 1 Scan WE current density [ua/cm 2 ] WE potential vs. RHE [V]
53 < < μ ± Ω 25 2
54 μ p O2 =
55 ( 2 2)R45 V sample = 1.2 I =
56 ( 2 2)R45 (1 1) ( 2 2)R ( 2 2)R45 ( 2 2)R45 2 ( 2 2)R45 ( 2 2)R45
57 Counts per second 4,5e+04 4e+04 3,5e+04 3e+04 2,5e+04 2e+04 1,5e+04 O1s venting through a separate line, rough pumping by cryo venting through the turbo pump, rough pumping by a rotary pump Counts per second C1s 1e Binding energy [ev] Binding energy [ev]
58 2 ( 2 2)R ( 2 2)R45 3 4
59 3 4 6e+04 O1s C1s 5e+04 Clean surface After H2O drop Counts per second 4e+04 3e+04 2e+04 Counts per second e Binding energy [ev] Binding energy [ev] 2 2 ( 2 2)R
60 7e+04 6e+04 Clean surface After H2O drop O1s C1s Counts per second 5e+04 4e+04 3e+04 2e+04 Counts per second e Binding energy [ev] Binding energy [ev]
61 ±
62 0.3 ± ( 2 2)R45 ( 2 2)R
63 α 2 3 α 2 3 (1 1) ± 50) p O2 = (1 1) (2 1) μ (2 1) (2 1) (3 1) (1 1) (1 1) μ 30
64 150 (1 1) 2 (2 1) (3 1) (1 1) (2 1)
65 α 2 3 (3 1) (2 1) (3 1) (3 1) (2 1) (1 1) 2 (20 40) 0.5 2e+04 1,5e+04 O Auger Fe 2p O1s Counts/s 1e Fe 2s Fe Auger O1s satellite Ta 4p Ta 4d Mo 3d Fe 4s Au 4f Fe 3p Ta 4f Binding energy [ev] ± ± 20) 2 2
66 ± 20) )
67 α ±1 1 1)
68 ) 1 1) 2 1) 1 1) 2 1) ( ) )
69 α ±60 2 1) 2 1) 2 1) 2 1)
70 V sample = 2 I = 0.10
71 α (2 1)
72 2 1
73 α )
74 =
75 α [121]
76 (2 1) (2 2) 2 (2 1) 2 2
77 α (
78
79 3 4 ( 2 2)R
80 3 4
81
82
83 α
84 α α 1 α
85
86
87
88
89
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