Assessment of Metallographic Preparation Techniques for Bi ...
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Assessment of Metallographic Preparation Techniques for
Bi2Sr2CaCu2O8+x (Bi-2212) Superconducting WiresSarah Sortedahl, James McFarlane, Mahira Araujo, Joseph Christian, Gavriel DePrenger-Gottfried,
Dr. Amir Kajbafvala, and Dr. Matthew JewellMaterials Science Center ���� University of Wisconsin – Eau Claire
Celebration of Excellence in Research and Creative Activity (CERCA) April 29 – 30, 2015
The authors thank our fellow UWEC students for the printing of this poster via differential tuition (Blugold Commitment).
Experimental Procedure
AcknowledgementsThis project is funded by the U.S. Department of Energy, Office of High Energy Physics grant no.
DE-FG02-13ER42036 and the National Science Foundation MRI award DMR-1428875. The authors
would like to thank the University of Wisconsin-Eau Claire, Material Science Center for the use of
experimental facilities and staff support.
Confocal Microscope
Summary
Introduction Results
Cutting
#1 #2 #3
Mounting
�Bi-2212 composite wires were cut, mounted, ground, and polished.
�We have developed a novel attack polish technique that yields a scratch-free
sample surface.
�To study details of Bi-2212 filament structures, we used a deep etching method
along with SEM and confocal microscope imaging.
�The combination of these sample preparations techniques allow us to assess
the effects of mechanical strain on the Bi-2212 filaments structure
Polishing
Automatic polisherManual polisher
� Bi2Sr2CaCu2O8+x (Bi-2212) is a high-temperature superconductor that can be formed into a round wire
for high field magnets applications.
� A good polishing technique is critical for further microstructural analysis of Bi-2212.
� The brittle Bi-2212 filaments are embedded in a soft Ag matrix. The extreme differences in the hardness
of these two materials makes creating a well-polished specimen difficult.
� Having a smooth sample surface is necessary for visual analysis and to observe various phases, voids,
and cracks inside the material.
� Here, we have developed an effective sample preparation technique to reveal the complex microstructure
of Bi-2212 wire and to efficiently correlate the electrical and mechanical behavior of the material.
Grinding and Polishing
Grinding using SiC Paper�Machines: manual, automatic
�Lubricants: water, dry, ethanol based lubricant
Polishing
�Machines: manual, automatic, vibratory
polisher
�Diamond Suspensions: 9, 6, 3 micron diamond
suspensions; water and ethanol based
�Alumina Suspensions: 1, 0.3, 0.05 micron
alumina suspensions; water and ethanol based
600 grit
SiC papers
800 grit 1200 grit
Bright field
Bright field Dark field
Dark field
Attack Polish
1200 grit800 grit600 grit
Grinding
Manual method using SiC papers
For the grinding steps, it was found that manually grinding, with no lubricant,
and with a paper towel cushion yielded the cleanest, most evenly polished
sample surface.
Alumina Polishing
SEM images showing the Bi-2212 wire surface after polishing with
1 µm alumina suspension in ethanol for 15 minutes
SEM images of a Bi-2212 wire low magnification (left) and high
magnification (right) with almost all of the Ag matrix etched away to reveal
the delicate Bi-2212 filaments.
An attack polish composed of a silver etchant and polishing suspension was
utilized. The silver etchant consisted of H2O2 and NH4OH. This silver etchant
was added to a 0.05 micron alumina 15 weight percent ethanol based
suspension. The ratio of the H2O2: NH4OH: 0.05 micron alumina suspension
was 1:1:50.
The scanning laser confocal microscope is used to assess the 3D morphology of the
composite Bi-2212 filamentary structure and identify the microstructural origin of electric
current-degrading fracture events.
Here, a quantitative height map
is used to evaluate matrix
etching, which is used to reveal
sub-surface crack initiation sites
in the Bi-2212 superconducting
filaments.
Image Analysis
SEM Micrographs of Deep Etched Samples
Vibratory polisher
Optical images showing the polishing quality for an attacked polished
sample in bright field (left) and dark field (right)
SEM images showing a final attack polished sample