Download presentation
Presentation is loading. Please wait.
Published byHolly Owen Modified over 9 years ago
1
Scanning tunneling microscopy (STM) Atomic force microscopy (AFM) Scanning electrochemical microscopy (SECM) UV & visible spectroscopy Transmission experiments Specular reflectance & ellipsometry Internal reflection spectroelectrochemistry Second harmonic spectroscopy Vibrational spectroscopy: IR spectroscopy, Raman spectroscopy Electron & ion spectroscopy XPS, AES, LEED, HREELS, mass spectroscopy Magnetic resonance methods: ESR, NMR Quartz crystal microbalance X-ray methods: XAS, XRD B Spectroelectrochemistry (ch. 17)
2
Vibration spectroscopy Infrared spectroscopy Infrared spectroelectrochemistry (IR-SEC)
3
Cell for IR-SEC
4
EMIRS (electrochemically modulated infrared reflectance spectrosocpy) Potential is modulated between one where the species of interest is absent & one where it is electrochemically generated
5
SNIFTIRS (subtractively normalized interfacial Fourier transform IRS) or PDIRS (potential difference IRS) or SPAIRS (single potential alteration) Spectra obtained separately at two potentials → subtraction
6
IRRAS (IR reflection absorption spectroscopy) IR absorption at fixed potential
7
SEIRA (surface enhanced IR absorption) IR to study adsorbed species (reactants, intermediates, products) → orientation & potential dependence of the adsorbed species SNIFTIRS
8
Attenuated Total Reflectance Spectroscopy (ATR) Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFT) IR incidence sample ZnSe or KRS-5 crystal *Transmission measurement *Reflection-Aborption infrared Spectroscopy (RAS) *Photoacoustic Spectroscopy (PAS) *Surface Electromagnetic Wave spectroscopy (SEW) In-situ FT-IR spectroscopy
9
In-situ FT-IR In situ FT- IR cell
10
In situ FT-IR CO/Pt
11
Raman spectroscopy
12
Raman spectroscopy: molecular vibrational information complementing IR spec. Raman in electrochemical system: signal enhancement - Resonance Raman spectroscopy (RRS) - Surface enhanced Raman spec. (SERS): molecules adsorbed on certain surfaces (Ag or Au)
13
RRS of TCNQ & electrochemically generated TCNQ -
14
Transients in Raman intensity
15
SERS for Os compound on Ag electrode as ftn of potential
16
SER spectra for benzene on Pd
17
In-situ Raman Spectroscopy
18
In-situ Raman microscopy ( 탄소재 음극과 LiCoO 2 양극재 분석 ) LiCoO 2 graphite acetylene black Fresh anode Brodd (2003) 25 o C 60 o C
19
Electron and ion spectrometry Ultra high vacuum (UHV) Excitation Detection X-ray photoelectron spectroscopy (XPS) Photons(X-ray) Electrons UV photoelectron spectroscopy (UPS) Photons (UV) Electrons Auger electron spectroscopy (AES) Electrons Electrons Low-energy electron diffraction (LEED) Electrons Electrons High resolution e - E loss spec. (HREELS) Electrons Electrons Rutherford backscattering (RBS) H+ or He+ H+ or He+ Secondary ion mass spec. (SIMS) Ions Ions Laser desorption mass spec. (LDMS) Photons Ions
20
Detection limits, sampling depth, spot size (spatial resolution)
21
UHV-electrochemistry
22
X-ray photoelectron spectroscopy (XPS, or ESCA)
23
Schematic diagram of XPS
24
XPS for Pt 4f levels:
25
XPS for gassy carbon electrodes
26
XPS for copper electrodeposition (a) Bulk Cu (b) Cu UPD
27
Electrochemical X-ray Photoelectron Spectroscopy Univ. of Illinois
28
Ex-situ Analysis without Contamination Glove BoxUHV-XPS Electrochemical XPS
29
Auger electron spectroscopy
30
Ni oxide on Au
31
AES Depth profiles for GaAs
32
AES depth profiles for MgPc
33
Electrochemical Auger Electron Spectroscopy
34
Low-energy electron diffraction
35
High resolution electron energy loss spectroscopy SCN - on Ag(111) (a)-0.3 V (b)+0.14 V
36
Mass spectrometry Differential electrochemical mass spectrometry (DEMS)
37
DEMS: fuel cell catalysts for methanol(solid) & formic acid(dotted) oxidation
38
Magnetic resonance methods Electron spin resonance & NMR
39
Electrochemical ESR
40
Quartz crystal microbalance
41
QCM: PVF on Au
42
X-ray methods Synchrotron X-ray absorption spectroscopy Absorption edge (energy that is just needed to eject a particular core electron, e.g., 1s e - (K edge), 2p 3/2 e - (L 3 edge) Fe & Fe oxides K-edge: 7.112 keV Within 10-40 eV: X-ray absorption near-edge structure (XANES) (or near-edge absorption fine structure (NEXAFS)) → oxidation state & ligand envirionment About 50 keV: extended X-ray absorption Fine structure (EXAFS) → distance & arrangement of atoms
43
X-ray diffraction techniques
44
In-situ XRD In-situ XRD patterns of Li x FeSnO 4 during initial lithium intercalation and deintercalation.
Similar presentations
© 2024 SlidePlayer.com. Inc.
All rights reserved.