Brass Sample Preparation for Scanning Electron Microscopy

APPLICATIONNOTE
Brass Sample Preparation
for Scanning Electron
Microscopy
Proper preparation of samples for ion milling increases milling process speed and improves the
quality of the resulting scanning electron microscope (SEM) images. In this application note,
a brass sample is mechanically polished and then milled using the Model 1060 SEM Mill in
preparation for SEM imaging.
Materials
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Hot plate
CrystalbondTM adhesive
Tripod-type holder
Aluminum SEM stub
Buehler grinder/polisher
Abrasive disks (1200 grit)
Diamond lapping films (3 and 1 µm)
Fischione Model 1060 SEM Mill
Mounting, Polishing, and Ion Milling
Mount a brass sample (12.5 mm x 12.5 mm)
on an aluminum SEM stub using a thermoset
adhesive (e.g., Crystalbond). Apply pressure
to the sample while the adhesive is hardening
to ensure a more level surface for grinding and
polishing (Figure 1).
maintaining orientation so that scratches are
consistent (Figure 2).
Figure 2. Grind the sample on a 1200-grit abrasive disk, then
polish the sample using 3 and 1 µm diamond lapping films.
Use a tripod-type holder (e.g., an Allied TEM
Wedge Polisher) to keep the sample steady
and parallel to the abrasive surface, if desired
(Figure 3). Use plenty of water to lubricate the
surfaces and remove debris during the grinding
and polishing process.
Figure 1. Mount a 12.5 mm x 12.5 mm brass sample on an
aluminum SEM stub using a thermoset adhesive.
Figure 3. Brass sample and aluminum stub mounted on a
handheld tool.
Using the stub post as a handle, grind the
sample on a rotating 1200-grit abrasive disk,
Use 3 µm and then 1 µm diamond lapping films
to reach a 1 µm finish; allow the sample to dry.
E.A. Fischione Instruments, Inc.
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Application Note
Brass Sample Preparation for Scanning Electron Microscopy
Load the sample and stub into the SEM Mill. Perform
the milling operation with the following parameters: a
single ion source set to 4 kV, 45% focus, and 4° beam
angle for 30 minutes with continuous sample rotation.
Imaging
field emission scanning electron microscope. The
overall quality near the center and edge of the sample
is compared for magnifications of 1000X and 5000X
(Figures 4-7). Some embedded grinding media remained
as a result of the initial mechanical preparation.
The ion-milled sample was imaged at 5 kV using the
upper secondary electron detector in an Hitachi S-4700
Selected areas at the center were imaged at 20,000X with
and without tilting to 45° (Figures 8-10).
Figure 4. 5 kV SEM images acquired near the edge of the ion-milled
brass sample (magnified 1000X).
Figure 5. 5 kV SEM images acquired near the center of the ion-milled
brass sample (magnified 1000X).
Figure 6. 5 kV SEM images acquired near the edge of the ion-milled
brass sample (magnified 5000X).
Figure 7. 5 kV SEM images acquired near the center of the ion-milled
brass sample (magnified 5000X).
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E.A. Fischione Instruments, Inc.
Application Note
Brass Sample Preparation for Scanning Electron Microscopy
Figure 8. 5 kV SEM images of selected areas of the ion-milled brass sample at 0° stage tilt (magnified 20,000X).
Figure 9. 5 kV SEM images of selected areas of the ion-milled brass sample at 0° stage tilt (magnified 20,000X).
E.A. Fischione Instruments, Inc.
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Application Note
Brass Sample Preparation for Scanning Electron Microscopy
Figure 10. 5 kV SEM images of selected areas of the ion-milled brass sample at 45° stage tilt (magnified 20,000X).
E.A. Fischione Instruments, Inc.
9003 Corporate Circle
Export, PA 15632 USA
Tel+1-724-325-5444
Fax+1-724-325-5443
info@fischione.com
www.fischione.com
©2013 E.A. Fischione Instruments, Inc. All rights reserved.
All trademarks are the property of their respective owners.
Document Number AN005 Revision 00 07/2013
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E.A. Fischione Instruments, Inc.