click image to enlarge (36K)
Figure 2 |
This extraction replication technique is especially useful
when the surface is rough and soft at the same time. The collodion film
will separate the particles lightly held in crevices without removing
any of the substrate as follows:
Step 1. Two drops of the collodion
solution are picked up on a tungsten needle and spread over about
10-20 mm2 of the contaminated surface. More drops may
be used to cover a larger area. A third drop may be necessary to
obtain a final film thickness of about 20 µm. Thinner films are
fragile and harder to remove. The solvent should evaporate in 5-15
minutes at room temperature. The preparation can be dried faster
in an oven at about 60-80°C (see Figure 2). |
click image to enlarge (19K)
Figure 3 |
Step 2. The dry collodion film with
the particles is pulled off the substrate and placed, particle side
down, on a glass slide for analysis by polarized light microscopy. The
contamination particles may be hard to characterize if, for example,
the substrate was a roughly machined part. The replica of the machining
marks may interfere with the microscopical characterization (see
Figure 3). |
click image to enlarge (23K)
Figure 4 |
Step 3. A 3-5 nL drop of amyl acetate,
delivered from a micropipette, is brought in with a tungsten needle
and allowed to flow halfway under the collodion film. This area
of film is referred to as the “cleared replica.” The particles in
the cleared portion of the 20 µm film of collodion are clearly visible
with a polarized light microscope. The film acts like a refractive
index liquid with nD=1.51. The other half of the film
is used for comparison (see Figure 4). |
click image to enlarge (27K)
Figure 5 |
Analysis of the Contaminants by SEM/EDS
To obtain the elemental compositions of the contaminants,
cut out a square of the replica, measuring ~0.2 mm, transfer it
to a polished carbon or beryllium substrate, and dissolve the collodion
by quickly passing small drops of amyl acetate over the square. Allow
each drop to dry before passing another drop over the replica (see
Figure 5). |