ME1302 Structure and Properties: Part Characterization; Exercises

1. A fracture surface of a metal matrix composite (nickel with silicon carbide

fibres) is investigated with a Scanning Electron Microscope (SEM).
Questions:
a. Which signals can you use to make an image of the sample?
b. Which signal do you prefer to observe the fracture surface?
c. How can you discriminate between the matrix and the fibres?
d. How can you increase the magnification to observe a detail with the
SEM?
2. A corrosion resistant zinc coating is applied to steel sheets. When coating
the steel sheet some aluminium is added to the zinc to improve the
coating properties. The thickness of the zinc coating is 1 m. The
composition of the zinc coating will be determined with X-ray
microanalysis.
Questions:
a. What is the maximum energy of the primary electron beam if the
electrons may only penetrate the zinc coating?
b. The aluminium content will be determined from the intensity of the AlK radiation generated with an electron beam of 15 KeV. What is then
the analysis depth?
c. Also the zinc content of the coating is determined with an 15 keV
electron beam. Both Zn-K and Zn-L radiation can be observed.
Calculate the energy of the mean components of the Zn-K and Zn-L
radiation using the binding energies of the electron involved in the Xray emission process?
d. Which radiation (Zn-K of Zn-L) would you observe to determine the
zinc content of the coating?
3. A wear resistant titanium nitride layer is analysed with X-ray Photoelectron
Spectroscopy (XPS) using Mg K straling ( = 1253.6 eV ). The
workfuction of the spectrometer is 1.6 eV. The Ti 2p3/2 electron line is
observed at a binding energy of 457 eV and the Ti 3p electron line at 37
eV. The chemical bonding between
Ti and N has no effect on the binding
energy of the N electrons.
Questions:
a. What is the chemical shift of the Ti 2p3/2 electron line.
b. At which (apparent) binding energy is the Ti L3M2,3M2,3 Auger line
expected?
c. How much is the separation between the N KL2,3L2,3 and the Ti
L3M2,3M2,3 Auger lines in the spectrum.
d. Is an other X-ray source a solution to make a better discrimination
between the N KL2,3L2,3 and the Ti L3M2,3M2,3 Auger lines?

W.G. Sloof

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ME1302 Structure and Properties: Part Characterization; Exercises

4. The growth of a thin copper film on a titanium substrate is observed with

X-ray photoelectron spectroscopy (XPS) using Mg-K radiation
( = 1253.6 eV ).The workfuction of the spectrometer is 1.6 eV.
The inelastic mean free path (IMFP) of the electrons depends on their
kinetic energy E (in eV) according to = E /100 (nm) for E > 50 eV.
The Ti 2p3/2 photoelectrons are observed at a take-off angle of 45 with
respect to the surface. The copper film was grown with a constant rate of
0.1 nm per minute during 30 minutes.

Questions:
a. Calculate the inelastic mean free path of the Ti 2p3/2 photoelectrons.
b. How does the intensity of the Ti 2p3/2 line change as a function of the
copper film growth time?
c. When island growth occurs, how can this be investigated with XPS?
Note: The photoelectron intensity of the substrate is given by:
Is = Iso exp [-d/( cos )], where Iso is the intensity of the uncovered
substrate and d the thickness of the overlayer.
5. An oxidized silicon surface is analysed with Auger Electron Spectroscopy
(AES) using a 3 keV primary electron beam. In the electron emission
spectrum two main line of silicon are observed: Si KL3L3 @ 1625 eV and Si
L3VV @ 80 eV.
The inelastic mean free path (IMFP) of the electrons depends on their
kinetic energy E (in eV) according to =

E /100 (nm) for E > 50 eV.

Questions:
a. What is the shift of both Auger lines due to chemical bonding between

silicon and oxygen?

b. At which value of the energy will the O KLL line be observed if the
binding energies of the oxygen electrons are not effected by the
chemical bonding with silicon?
c. In the electron emission spectrum only the Si KL3L3 line of the
substrate can be observed. Estimate the thickness of the silicon oxide
layer.
6. Boron is added to a nickel base alloy to improve the creep resistance. To
this end, Ni3B must be formed at the grain boundaries. A fracture surface
is studied with AES and SIMS.
Questions:
a. Discuss which technique is most sensitive to locate the boron?
b. How is the local composition quantified from an AES and a SIMS
spectrum?

W.G. Sloof

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ME1302 Structure and Properties: Part Characterization; Exercises

7. Silver (Ag) has been implanted into an optical lens made of quartz (SiO2)
to absorb UV radiation. This lens is analysed with Rutherford
Backscattering Spectroscopy (RBS). The RBS analysis was performed with
a 4He+ ion beam directed perpendicular to the lens surface. The kinetic
energy E0 of the ion beam is 2.0 MeV. The scattered ions were detected at
an angle of = 170 with respect to the incident beam. A peak at 1650
keV in the RBS spectrum was observed which correspond to the implanted
silver. The peak height of the implanted Ag is one hundredth of the silicon
signal,
HAg / HSi = 10-2. The density of SiO2 is 2.3x1022 molecules
thus:
3
SiO2/cm and the atomic masses are: MO = 16 amu, MSi = 28 amu en MAg
= 108 amu.
Questions:
a. Draw the RBS spectrum with the appropriate intensity ratios for the O,
Si en Ag signals. Indicate the energies of the O, Si en Ag signals.
b. Determine the implantation depth of silver (projected range).
c. Estimate the atomic fraction silver at the implantation depth.
8. An aluminium (MAl = 27 amu) foil is covered with a monolayer of gold
(MAU = 197 amu) at both sides. This material is analysed with Rutherford
Backscattering Spectroscopy (RBS). The RBS analysis is executed with a 3
MeV 4He+ ion beam. The scattered ions are detected at an angle = 170 .
The separation between the two gold peaks is 200 keV.
Questions:

a. Give the RBS spectrum of the material and specify the appropriate
energy values at the horizontal axes and give the relative intensities of
the Au and Al signals at the vertical axes.
b. Determine the thickness of the Al foil.
9. Auger Electron Spectroscopy is employed to investigate a joint between
copper and silver. After sputter cleaning the surface with argon ions a
spectrum is recorded at different locations using an electron beam with
energy of 5 keV.
Questions:
a. Why is the Auger electron spectrum usually differentiated?
b. At which kinetic energy do you expect the Ag M5VV line?
c. What is the advantage to use AES instead of X-ray microanalysis?

W.G. Sloof

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ME1302 Structure and Properties: Part Characterization; Exercises

10. A steel surface has been analysed with SIMS and SNMS in order to
determine segregation of alloying element. Both analyses have been
executed with the same ion beam.
Questions:
a. Is the sputter yield for SIMS the same as for SNMS?
b. Explain possible differences between the secondary ion intensities of
the analysis with SIMS and SNMS.
11. A steel surface is coated with a thin layer of zinc. A composition depth
profile has been recorded using ion sputtering. The sublimation heat U0 of
Zn is equal to 0.1x10-15 eVcm2 and of Fe 0.3x10-15 eVcm2. The stopping
cross section Sn of Zn is equal to 200x10-15 eVcm2 and of Fe 150x10-15
eVcm2.
Questions:
a. Calculate the Zn/Fe sputter yield ratio. What does this ratio mean for
the acquired composition depth profile?
b. Which sputtering effects must be considered, when analysing the zinc
coating / steel interface?
c. Which analytical techniques may be used in combination with ion
sputtering?

W.G. Sloof

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