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Lecture 3-5Instrumentation
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Requirements1. Vacuum
Mean Free PathContaminationSticking probability
UHVMaterialsStrengthStabilityPermeation
Design considerationsPumping speedVirtual leaksLeakingde-greasing
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Vacuum pumps
DiffusionIon pumpsTurbo molecular pumpsSublimation pumpsCryo pumps
2. Sample handlingPreparationTreatment in vacuumManipulation
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Instrument : Light source, analyser, detector
Resolution, SensitivityWidth of radiationWidth of the level Analyser resolution
FW HM
Analysers
Dispersive Retarding potential
I(Photoelectrons V, Inr, AS, D Analyser solid angleat detector)
Cross section Area of the slit
Photon Intensity
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Transmission Fraction of electrons reaching the detector from an isotropic point source
= Useful instrument solid angle . Transmission factor
Integral of point source transmission over slit area luminority
Integral of solid angle over slit area étendue
Line width of radiation pressure broadening (Stark, van der Waals, resonance)
Doppler broadeningRecoil of atoms
Life time
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I(T) = 1 + E/2 [3/2 (sin2 T ) – 1] for unpolarised photonsE- asymmetry parameter
Surface Sensitivity
e-Angle
hQe-
AdsorbateI
Bulk
T
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Other techniquesPhoto detachment EXAFS, SEXAPS, synchrotron radiation
EPMA or Electron probe x-ray micro analysis
Ion beam techniques
SIMSdynamic
staticINS (ion neutralization spectroscopy)
SNMS (sputtered neutral mass spectrometry)PIXE (particle induced x-ray emission
ISSRBSFABMS
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History
Photoelectric effect 1887 HertzRutherford E ray spectroscopy Before WWI
Basic XPS equation, EK = hQ - EB Originally stated by Rutherford 1914
Moseley After WWIRawlinsonRobinson E ray spectrum of elements
Anomalous lines corresponding to electron ejection due to fluorescence excitation.
Anger spectroscopy 1925
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Steinhardt 1951
“An x-ray photoelectron spectrometer for chemical analysis”
Kai Seigbahn – Uppsala 1940’s 1967 “ESCA: Atomic, Molecular and solid state structure studied by means of Electron spectroscopy”
Acronym ESCA is due to Seigbahn
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Early Hertz Experiment
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U vs. Z for a number of metals
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Simple UPS
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Heart of the instrument
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What is inside
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X-Ray Source
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X-Ray emissionspectrum
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Detail of the spectrum
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X-ray source with dual filament and anode faces
Water Inlet Tube
Focusing Shields
Filament 2Filament 1
Anode Face 1 Anode Face 2
WindowX-rays
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UV Source
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Synchrotron
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ResolutionAbsolute resolution, FWHM 'EBase width 'EB = 2 'E
Relative resolution R = 'E/E0
Represented normally, in percentage, 'E/E0 x 100
Resolving power U = 1/R = E0/'E
XPS line widths 0.7eV Mg KD, 0.85 eV Al KD, Ffr an absolute resolution of 0.2 eV, the relative resolution is 10-4 or a resolving power of 10,000.
To keep the analyser size to an optimum value, the KEs have to be retarded - pass energy.
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For an absolute resolution of 0.2 eV, the relative resolution is only 10-3. High absolute resolution can be achieved by retardation.
Not always advantageous.
Requirement in UPS
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EDC around EF in an UPS spectrum of Ag. Solid line is
the Fermi function at RT
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Electronic structure of solids
s
p
s band
p band
Band gap
Half full
Full
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Energy
Zero
Fermi level
Occupied
Unoccupied
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In a piece of metal, there are 1023 electrons.We have high quantum states for most electrons.
Probability that a given quantum state is occupied is given by the Fermi factor,
f(E) = 1/[e(E-µ)/kT + 1]
Plot of this is given here which gives a definition of Femi level.
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µ is chemical potential, is the energy of the level for which f(E) = ½
EF
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How the given energy states are occupied at a given temperature is given by Fermi-Dirac distribution.
N(E)dE = f(E)S(E)dE= S(E)dE/e(E-µ)/kT + 1]
N(E) = number of electrons per unit volume, having energy between E and E + dES(E) = number of available quantum states in this energy range.
This distribution obeys Pauli exclusion principle.Number of electrons N(E) can never be larger than the number of available statesS(E) as the denominator is always greater than one.
For states with energies well above µ, 1 in the denominator can be neglected. N(E)dE § e-(E-µ)/kT This resembles Bolzmann distribution
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UPS EDC at EF of Ag (15 K). Resolution, 'E is obtained by convoluting a Fermi
function with a Gaussian function
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AnalysersAnalysers
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Electron beam
Sample
Retarding Field Analyser
Scan
Detector
Amplifier
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Intensity
Retarding Voltage
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Eo/eV = k/ln(r2/r1) mv2/r = eV
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ElectronGun
ElectronMultiplier
First Stage SecondState
Sample
X-Ray Source
Inner and OuterMagnetic Shields
OuterCylinder Inner
CylinderRotary Motion
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eǻV = E(R2/R1 – R1/R2)
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1. Single-Channel DetectorChannel electron multiplier:A continuousdynode surface. High count rate of 106
counts per second.
2. Multi-Channel DetectorA set of parallel detector chains or positionsensitive detectors kept at the analyserexit slit plain.
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Semi Conducting Surface
Lead doped glass
HVe-
film
glass
106electron
Channel electron multiplier
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Hemispherical sector electron energy analyser and control
electronics.
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Spectrometer with X-ray monocromatisation
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Modern instrument for UPS, XPS, AES and EELS
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An electron gun for beams up to 10 ke V
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Ion gun using a Penning discharge.
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A liquid-metal field emission ion source
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A simple method of XPS imaging using a conventional HAS instrument
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Data analysis