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As research progresses towards nanoscale materials, there has become a need for a more efficient and effective way to obtain ultra-thin samples for imaging under transmission electron microscope (TEM) for atomic resolution analysis. There are various methods used to obtain thin samples (<50 nm in thickness). However, most of the resultant TEM images of soft materials, such as CNT/epoxy composites, are of poor quality due to the sample cutting difficulties. Such poor quality samples are characterized by uneven sample thicknesses, objective overlapping, overall darkness due to large thickness, and defects such as cutting scratches. This research is a continuous effort to study and improve the ultra-microtome cutting technique to provide an effective and reliable approach of obtaining an ultra-thin (25-50 nm) cross section of a CNT/polymer composite for high resolution TEM analysis. Improvements were achieved by studying the relationships between the chosen cutting parameters, sample characteristics and TEM image quality. From this information, a cutting protocol was established so that ultra-thin sample slices can be achieved by different microtome operators for high resolution TEM analysis. In addition, a custom tool was created to aid in the sample collection process. In this research, three composite samples were studied for both microtome cutting and TEM analysis: 1) Unidirectional (UD) IM7/BMI composite; 2) Single-layer CNT buckypaper (BP)/ epoxy nanocomposite; 3) 3-layer CNT BP/BMI nanocomposite. The resultant TEM images revealed a clear microstructure consisting of amorphous resin and graphite crystalline packing. UD IM7/BMI composite TEM results did not reveal an interfacial region resulting in a need for even thinner sliced cross sections. TEM results for the single-layer CNT BP/epoxy nanocomposite revealed the alignment direction of the nanotubes and numerous stacks of CNT bundles. In addition, there was visible flattening of CNT packing into dumbbell shapes similar to results obtain by Alan Windle. TEM results for the 3-layer CNT BP/BMI nanocomposite revealed uniformly cut resin. However, when the diamond knife reached graphite crystalline regions, the nanotube either became deformed into a cone-like structure, was cut at a thicker thickness than the resin, or folded over onto itself. This is most likely a result of the nanotubes high mechanical properties in response to the stress of cutting.
Carbon Nanotube, Nanocomposites, TEM, Ultra Microtome
Date of Defense
April 11, 2014.
A Thesis submitted to the Material Science and Engineering Program in partial fulfillment of the requirements for the degree of Master of Science.
Includes bibliographical references.
Richard Liang, Professor Directing Thesis; Okenwa Okoli, Committee Member; Mei Zhang, Committee Member.
Florida State University
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