Sample Preparation for Textile Nanofiber Composites

Garcia, R. D. M.; Fedorova, Nataliya; Knowlton, Valerie M.; Oldham, Christopher J.; Pourdeyhimi, Behnam

doi:10.1017/s1551929500051476

Cited by 2 publications

(4 citation statements)

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“…The use of freeze fracturing to produce cross sections can reduce effects resulting from disparate materials properties, but fracturing often occurs along paths that are dictated by materials properties (Severs & Hotton, 1995). Assuming that an embedding media having a suitable match with fiber properties can be found, microtomy can be used to produce useful fiber cross sections with minimal fiber distortion (Plummer, 1997; Garcia et al, 2005). However, even if successful, the embedding and microtomy process can be time-consuming and can sometimes require considerable trial and error to find the proper embedding medium to insure production of undistorted fiber cross sections.…”

Section: Discussionmentioning

confidence: 99%

“…Microtomed cross sections of microfibers and nanofibers have been examined by different microscopy techniques. For example, Garcia et al (2005) used oxygen plasma etching of microtomed I/S fibers to enhance the secondary electron imaging of the polymers in I/S fiber cross sections. Wang et al (2007) utilized atomic force microscopy tapping mode techniques to image and manipulate isotactic polypropylene nanofibers in a cellulose acetate butyrate matrix.…”

Section: Introductionmentioning

confidence: 99%

“…Various spunbonding process parameters govern the final I/S fiber structure and properties. Previous studies on revealing the cross-section morphology utilizing oxygen plasma [5][6] and scanning electron microscopy (SEM) can also provide structural information. However, the sample preparation and the necessary transfer between the different instrumentations during the examination process can be troublesome and there is no ability to perform site specific investigation as is provided by the FIB.…”

mentioning

confidence: 99%

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Focused Ion Beam Characterization of Bicomponent Polymer Fibers

et al. 2010

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Previous work has shown that focused ion beam (FIB) nanomachining can be effectively utilized for the cross-sectional analysis of polymers such as core-shell solid microspheres and hollow latex nanospheres. While these studies have clearly demonstrated the precise location selection and nanomachining control provided by the FIB technique, the samples studied consisted of only a single polymer. In this work, FIB is used to investigate bicomponent polymeric fiber systems by taking advantage of the component's differing sputter rates that result from their differing physical properties. An approach for cross sectioning and thus revealing the cross-sectional morphology of the polymeric components in a bicomponent polymeric fiber with the island-in-the-sea (I/S) structure is presented. The two I/S fibers investigated were fabricated using the melt spinning process and are composed of bicomponent combinations of linear low density polyethylene (LLDPE) and nylon 6 (PA6) or polylactic acid (PLA) and an EastONE proprietary polymer. Topographical contrast as a result of differential sputtering and the high surface specificity and high signal-to-noise obtained using FIB-induced secondary electron imaging is shown to provide a useful approach for the rapid characterization of the cross-sectional morphology of bicomponent polymeric fibers without the necessity of staining or other sample preparation.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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Focused Ion Beam Characterization of Bicomponent Polymer Fibers

et al. 2010

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“…Previous studies on revealing the cross-section morphology utilizing oxygen plasma [5][6] and scanning electron microscopy (SEM) can also provide structural information. However, the sample preparation and the necessary transfer between the different instrumentations during the examination…”

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confidence: 99%

Focused Ion Beam Characterization of Bicomponent Polymer Fibers

et al. 2009

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Previous work has shown that focused ion beam (FIB) can be effectively utilized for the cross-sectional analysis of polymers such as core-shell solid micro-spheres [1] and hollow latex nanospheres [2]. While these have clearly demonstrated the precise location selection and milling control provided by the FIB technique, the samples studied consisted of only a single polymer. In this work, FIB is used to investigate bicomponent polymeric fiber systems by taking advantage of the component's differing physical properties. An approach for cross sectioning and thus revealing the morphology with respect to the polymeric components in a bicomponent polymeric fiber crosssection with the island-in-the-sea (I/S) structure is presented. The I/S fibers investigated were fabricated using the spunbonding process and are composed of bicomponent combinations of polypropylene (PP), polylactic acid (PLA), polyethylene terephthalate (PET), or nylon 6 (PA6).Bicomponent I/S fibers [3] were coated with approximately 30 nm of palladium-gold using a Denton Desk II sputter coater. An FEI Quanta 200 3D Dual Beam system was used for crosssectioning and imaging. The fibers were cross-sectioned by using a 30keV Ga + ion beam for both the mass removal and cross-section polishing steps of the process. Initial mass removal was carried out using a water injection system to chemically enhance material removal [4]. The injection of the water vaper into the vacuum chamber resulted in an increase of chamber pressure of about 1 order of magnitude (from about 5E-6 Torr to 5E-5 Torr). Prior to the mass removal step, a platinum strip was deposited onto a selected area across the width of the fiber to protect the surface of the fiber by preventing unwanted etching of the fiber surface. An approximately 20x20 µm 2 area with a depth equals to the fiber diameter (~10µm) was removed in the mass removal step by using a 20nA beam and a rectangle raster pattern. Beam currents of 5nA, 1nA and 100pA were subsequently used for cross-section polishing using a cleaning cross-section milling pattern to provide line-by-line material removal. Finally, a 30pA beam with a dwell time of 55µs and a 1024x768 pixels scan resolution was directed perpendicular to the cross section surface to provide a secondary electron (SE) image. An example of an I/S fiber cross-section is presented in Figure 1. Differential sputtering of the respective polymers gave rise to the necessary topographical contrast since sputtering occurred over the cross-section surface during ion induced secondary electron imaging. This differential sputtering combined with the contrast generated by ion-induced secondary electron microscopy provided the ability to differentiate the structure of the bicomponent fiber.Various spunbonding process parameters govern the final I/S fiber structure and properties. Previous studies on revealing the cross-section morphology utilizing oxygen plasma [5][6] and scanning electron microscopy (SEM) can also provide structural information. However, the sample preparation and ...

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Sample Preparation for Textile Nanofiber Composites

Cited by 2 publications

References 4 publications

Focused Ion Beam Characterization of Bicomponent Polymer Fibers

Focused Ion Beam Characterization of Bicomponent Polymer Fibers

Focused Ion Beam Characterization of Bicomponent Polymer Fibers

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