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Surface Techniques: Woodruff, T.A. Delchar, Cambridge Solid State Science Series)

1. Several techniques are used to study surface structure, composition, and electronic properties at the atomic level, including LEED, HEED, STM/AFM, AES, XPS, UPS, SIMS, IR, EELS, and TPD. 2. Key techniques like LEED use low energy electron diffraction to determine surface atom arrangement, while AES, XPS, and SIMS provide information about surface composition through detection of ejected core electrons or ions. 3. Other surface characterization methods such as STM/AFM, IR, EELS, and TPD probe surface electronic structure, bonding configurations, and reaction pathways through measurement of currents, vibrational energies

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111 views7 pages

Surface Techniques: Woodruff, T.A. Delchar, Cambridge Solid State Science Series)

1. Several techniques are used to study surface structure, composition, and electronic properties at the atomic level, including LEED, HEED, STM/AFM, AES, XPS, UPS, SIMS, IR, EELS, and TPD. 2. Key techniques like LEED use low energy electron diffraction to determine surface atom arrangement, while AES, XPS, and SIMS provide information about surface composition through detection of ejected core electrons or ions. 3. Other surface characterization methods such as STM/AFM, IR, EELS, and TPD probe surface electronic structure, bonding configurations, and reaction pathways through measurement of currents, vibrational energies

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SURFACE TECHNIQUES

Therefore, for surface experiments you need UHV in order of 10-10Torr or better. This is the worst case, non-reactive
surfaces could be studied in lower vacuum.
How do you obtain a clean surface in UHV?
By under vacuum ( to maintain clean surface)
- Cleavage
- Heating
- Ion bombardment
- Chemical processing (dry etching)
Experiment techniques for surface characterization:(Further reading – Modern techniques of surface Science, D.P.
Woodruff, T.A. Delchar, Cambridge Solid State Science Series)
Study of surfaces involves three types of measurements:
- Geometrical structure – atom arrangement
- Composition
- Electronic structure – determines reactivity of the surface
Table 1 lists some of the techniques used to study surfaces:
LEED:
Probing with electron ~ 10-100eV energy. A schematic of LEED apparatus is shown in figure 3. Low energy of
electrons ensures that diffraction pattern is obtained only from surface atoms. Arrangement of atoms on the surface is
obtained by analyzing the diffraction pattern. (There are 5 two dimensional Bravais lattices, and 17 unique two
dimensional space groups.)

Detailed analysis of the intensity of each of the spots as a function of the voltage of the incident beam (i.e. LEED I-V
curves) gives information about the position of all of the atoms on the surface.
HEED or REED:
This is similar to LEED, except electron energies are in 10-30 KeV range and one uses a glancing angle.

STM/AFM:
In STM and AFM, one scans a small tip over a surface as shown in figure 5. One then uses a current to adjust the
height of the tip so that it keeps either the current to the surface or the force between the tip and the surface constant. The
current and force are a function of the distance between the tip and the surface.
AES:
It is used to measure the surface composition. In AES, a beam of electrons or X-rays is used to knock out a core
electron from an atom either in the surface or in an adsorbed layer.
A schematic of an AES experiment is shown in figure 6.

Typically, one observes a series of peaks corresponding to each of the elements in the surface and adsorbed overlayer. The
intensity of the peaks is related to the concentration of the atoms on the surface.
AES is sensitive to sub-monolayer levels of impurities, but quantitative analysis is difficult because some of the
secondary electrons are lost due to impacts with other atoms. Other Auger electrons do not travel in the right direction to
reach the detector. Further, the probability that an Auger electron is formed on a given atom varies somewhat with the
composition of the surrounding atoms.

XPS:
In XPS one directs a beam of X-rays at a solid surface and measured the energy distribution of the electrons
which leave the surface with an electron analyzer.

Figure 7

During the XPS process, the X-rays knock electrons out of the core levels in the surface atoms. Each element has
its own characteristic core levels. As a result, an XPS spectrum shows a series of peaks corresponding to each individual
element in the surface.
XPS can also be used to examine the electronic structure and the bonding of molecules on surfaces. In XPS one is
measuring the energy distribution of the electrons which leave the surface. That distribution of electrons in the surface
(i.e. the surface electronic structure).
XPS also provides information about the bonding of molecules in the surface. The core levels of the atoms in a
surface shift according to the chemical environment around the surface atoms. For example, an oxygen atom bound to the
carbon in adsorbed CO has a slightly different core levels than an oxygen bound to a metal surface.

UPS:
UPS is similar to XPS, except that probing beam is made of ultraviolet photons. Ultraviolet photons excite the
valence electrons in molecules or the conduction electrons in surfaces. Generally, UPS is used to probe the electronic
structure of surfaces, and the changes in the electronic levels due to the presence of adsorbates.

SIMS:
SIMS is also used to measure surface composition. Figure-8 shows a schematic of the SIMS experiment. Ion
Beam energy is 1000 ev. Sufficient to knock of surface atoms and molecules.

Figure 8

In SIMS, one directs a beam of ions at a solid surface and measures the mass distribution of the ions which are
produced when the incident ions collide with the surface. One limitation of SIMS is that it cannot detect neutrals that are
produced in the collision. Hence, quantitative analysis is difficult.

IR and EELS:
IR and EELS are much better probes of the structure and bonding of molecules at surfaces. Figure-9 shows a
diagram of a typical refraction infrared apparatus. In IR one directs a beam of infrared photons at a solid surface, and
measures the fraction of frequency. One then compares the observed IR spectrum to ones from a series of reference
compounds to learn about the bonding of molecules to surfaces.
In EELS (Figure-10), one directs a mono-energetic beam of electrons at a solid surface, and measures the energy
distribution of the electrons which scatter from the surface. Generally, one can observe distinct peaks for each of the
vibrational losses. As a result, we get information similar to IR.

TPD, TPR and TDS:


These are all very similar. One adsorbs gas onto a surface, and then heats the surface in a controlled way. A mass
spectrometer is then used to measure the rate at which products desorb from the surface (Figure-11).

Figure 11

Using TPD, one can tell what reactions occur when the sample is heated. One can also see how strongly
molecules are bound to the surface. Once also learn about reaction pathways.

(See attached pages from Woodruff &Delchar on generation of Auger electrons.)

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