SAMPLE PREPARATION OF XPS

1) Eliminating volatile material

For the first step of the sample preparation for XPS, we begin the process by removing
the volatile material from the sample. Volatile substance can be described as a substance that
evaporates readily at normal temperatures and a substance that has a measurable vapor pressure.
Volatile materials are one of the main sources of photochemical reaction in the atmosphere
leading to various environmental hazards. In certain cases, when the volatile material gives
benefit for the sample, it is not being removed. Instead, the sample may be cooled before the
experiment.

The cooling process is carried out in a relatively low temperature to ensure that the
volatile material does not go through evaporation by any heat load that may be transmitted by
the analysis conditions. The unused volatile material were usually removed by washing it with
a fitting solvent or by using long-term pumping in a different vacuum system. If we choose to
remove it by using solvent, the most suitable solvent that can be used is ethanol and freshly
distilled solvent. This is because freshly distilled solvent can be used to prevent contamination
by high boiling point pollutant within the solvent. The solvent choices are very crucial and
must be chosen properly. The surface of sample might be altered by hexane or any other light
hydrocarbon solvents. Soxhlett extractor also can be used to wash the samples by using suitable
type of solvent.

Figure Diagram of Soxhlet extractor

2) Eliminating non-volatile organic contaminants

Relatively, if an organic contaminant is in interest or undistinguished underlying material that

is of interest, the contaminant may be detached with proper organic solvents. For the cases with
volatile materials, the solvent must be chosen carefully as it may be critical.

3) Surface etching

Etching is defined as the process of using strong acid or mordant to cut into the
unprotected parts of a metal surface to create a design in incised in the metal. In modern
manufacturing, other chemicals may be used on other types of material. Surface contaminants
on the samples can be removed by ion sputter-etching and other erosion techniques such as
using oxygen plasma on organic materials.

Figure 1 Etching process by ion sputtering

 Figure 2 Weak selectivity in ion beam etching

Figure 3 Plasma sputtering

Argon ion etching is usually used to acquire important information about the
composition as a function of the outlook time to ion etching.

4) Abrasion

Abrasion is a process of erosion and it occurs when specific material which are being
transported wears away at a surface over time. It is a frictional process that was caused by
scuffing, scratching, wearing down, marring, and rubbing away materials. Abrasion of a
surface can be done without remarkable contamination by using laboratory equipment such as
wipe, a cork, a file, or a knife blade. Due to this, local heating and reaction with environmental
gases might occur (example : oxidation in air and formation of nitrides in nitrogen). In order to
avoid oxidation of more active materials, abrasion should be performed in an inert atmosphere
such as a glove box. After that, the abraded material should be transferred to the ultra-high
vacuum, or better know as UHV chamber, in a secured vessel to protect the clean surface.

The rate of abrasion were determined by several factors such as size of the particle, the
pressure of abrasive agent, and the speed at which the abrasive particle moves across the surface.
For the size of particle, large particles will resulted in deeper scratches and will work harder.
Course abrasive are usually used on highly rough surface and followed by finer course surface.
For the second factor which is pressure of abrasive agent, a greater pressure will resulted in
deeper scratches and faster work. It also reduces control over abrasion process. For the speed
at which the abrasive particle moves across the surface that is being abraded, the higher the
speed, the higher rate of abrasion will be.

Figure 4 Illustration of abrasive wear

5) Fracturing and scraping

Generally, we know that there are variety of materials that can be fractured or scraped
within the test chamber under UHV conditions using suitable equipment. This process prevents
contamination by reaction with atmospheric gases. But, unexpected results might occur.
Fracturing might take place along the grain boundaries which may not be representing the bulk
material. Meanwhile, scraping process can be used to cover hard material with soft material
when the sample is multiphase.
6) Grinding to powder

Samples may be grounded to a powder in a mortar if spectra characteristic of bulk

composition are required. The clean surfaces of the sample must be protected from the
atmosphere. Localized high temperatures can be produced during the grinding process, so that
the grinding process should be done slowly in order to reduce the heat-induced chemical
changes at the freshly produced surfaces. Before carrying out the process, the mortar must be
cleaned thoroughly before reusing it again.

7) Mounting powder for analysis

In most cases, there is several methods that can be applied to mount powders for
analysis. Alternatively, methods for mounting powders include by pressing the powder into
indium or other soft foils, assisting the powder on a metallic mesh, pressing the powder into
pellets or simply depositing the powder by gravity. The most openly used method is by dusting
the powder into polymer-based adhesive tape with a camel-hair brush. The powder used must
be dusted across the surface attentively and lightly, with no wiping strokes. Some researchers
used organic tape for UHV condition, but there is some of them too who successfully applied
certain types of tape in the 10-10 Torr range.

By using the foil method, the powder was pressed in between two pieces of pure foil.
After that, the two pieces were detached and one of them is used for the analysis. There is
various results to this experiment. Among the possibilities is that the bare foil remains exposed
and if the sample is in separate insulator, parts of the powder can charge differently. Different
charging can lead to a problem when a metallic mesh is used to support the powder. If a press
is used to form the powder into a pellet of feasible dimensions, a press with hard and
exceptionally clean working surfaces should be applied. Some materials can be hold in place
by gravity attraction, specifically if a shallow well or depression is cut in the surface of the
sample mount. Another effective way that can be used to produce a uniform layer is by allowing
a liquid suspension of the powder to dry on the specimen holder. But, if this method is used,
some detailed precaution must be taken such as to ensure that gas advancement does not disturb
the sample.