Hostname: page-component-78c5997874-m6dg7 Total loading time: 0 Render date: 2024-11-05T17:16:48.926Z Has data issue: false hasContentIssue false

Morphology Observation of Latex Particles with Scanning Transmission Electron Microscopy by a Hydroxyethyl Cellulose Embedding Combined with RuO4 Staining Method

Published online by Cambridge University Press:  26 February 2013

Xiang Geng*
Affiliation:
Analytical Sciences, Dow Chemical (China) Co. Ltd, 936 Zhangheng Road, Pudong District, Shanghai 201203, China
Myra Xuemei Zhai
Affiliation:
Analytical Sciences, Dow Chemical (China) Co. Ltd, 936 Zhangheng Road, Pudong District, Shanghai 201203, China
Tong Sun
Affiliation:
Analytical Sciences, Dow Chemical (China) Co. Ltd, 936 Zhangheng Road, Pudong District, Shanghai 201203, China
Greg Meyers
Affiliation:
Analytical Sciences, Building 1897, The Dow Chemical Company, Midland, MI 48667, USA
*
*Corresponding author. E-mail: [email protected]
Get access

Abstract

Imaging of latex particles, especially those with low glass transition temperature (Tg) has been a challenging issue. Different sample preparation methods for characterization of the morphology of a poly(n-butyl acrylate)/polystyrene two-phase latex are discussed and compared in this study. A method via hydroxyethyl cellulose embedding combined with ruthenium tetraoxide (RuO4) staining for scanning transmission electron microscope (STEM) observation is developed. By using this method, the spherical shape of latex particles can be maintained without deformation. The degree of incorporation of RuO4 into latex particles and cellulose matrix is different, which makes latex particles readily identifiable from cellulose matrix under STEM. A series of latexes with different structures such as copolymer latex and organic-inorganic hybrid latex were also successfully investigated by this method. The results indicate this specimen preparation method can be applied to study the morphology of a wide range of latex systems.

Type
Materials Applications
Copyright
Copyright © Microscopy Society of America 2013

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Barkay, Z., Rivkin, I. & Margalit, R. (2009). Three-dimensional characterization of drug-encapsulating particles using STEM detector in FEG-SEM. Micron 40, 480485.CrossRefGoogle ScholarPubMed
Blackson, J., Garcia-Meitin, E.I. & Darus, M.E. (2007). High resolution scanning electron microscopy examination of polymer morphology. Microsc Microanal 13, 10621063.CrossRefGoogle Scholar
Bogner, A., Jouneau, P.H., Thollet, G., Basset, D. & Gauthier, C. (2007). A history of scanning electron microscopy developments: Towards “wet-STEM” imaging. Micron 38, 390401.CrossRefGoogle ScholarPubMed
Crassous, J.J. & Ballauff, M. (2006). Imaging the volume transition in thermosensitive core-shell particles by cryo-transmission electron microscopy. Langmuir 22, 24032406.CrossRefGoogle ScholarPubMed
Disanayaka, B., Zhao, C.L., Winnik, M.A., Shivers, R. & Croucher, M.D. (1990). Polymer colloid morphology studied by freeze-fracture electron microscopy. Langmuir 6, 162168.CrossRefGoogle Scholar
Echlin, P. (2009). Handbook of Sample Preparation for Scanning Electron Microscope and X-Ray Microanalysis. New York: Springer.CrossRefGoogle Scholar
Erdem, B., Sudol, E.D., Dimonie, V.L. & El-Aasser, M.S.J. (2000). Encapsulation of inorganic particles via miniemulsion polymerization. I. Dispersion of titanium dioxide particles in organic media using OLOA 370 as stabilizer. J Polym Sci A 38, 44194430.3.0.CO;2-X>CrossRefGoogle Scholar
Gaillard, C., Fuchs, G., Plummer, C.J.G. & Stadelmann, P.A. (2007). The morphology of submicronsized core–shell latex particles: An electron microscopy study. Micron 38, 522535.CrossRefGoogle ScholarPubMed
Garcia-Meitin, E.I., Bar, G., Blackson, J. & Reuschle, D. (2008). High resolution polymer imaging using scanning transmission electron microscopy. Microsc Microanal 14(Suppl 2), 13801381.CrossRefGoogle Scholar
Guise, O., Strom, C. & Preschilla, N. (2011). STEM-in-SEM method for morphology analysis of polymer systems. Polymer 52, 12781285.CrossRefGoogle Scholar
Harris, J.R. & Horne, R.W. (1994). Negative staining: A brief assessment of current technical benefits, limitations and future possibilities. Micron 25, 513.CrossRefGoogle Scholar
Harris, J.R., Roos, C., Djalali, R., Rheingans, O., Maskos, M. & Schmidt, M. (1999). Application of the negative staining technique to both aqueous and organic solvent solutions of polymer particles. Micron 30, 289298.CrossRefGoogle Scholar
Kirsch, S., Landfester, K., Shaffer, O. & El-Aasser, M.S. (1999). Particle morphology of carboxylated poly-(n-butyl acrylate)/poly(methyl methacrylate) composite latex particles investigated by TEM and NMR. Acta Polym 50, 347362.3.0.CO;2-C>CrossRefGoogle Scholar
Lee, D.I. (2006). Nanostructured latexes made by a sequential multistage emulsion polymerization. J Polym Sci A 44, 28262836.CrossRefGoogle Scholar
Luna-Xavier, J.L., Guyot, A. & Bourgeat-Lami, E. (2002). Synthesis and characterization of silica/poly (methyl methacrylate) nanocomposite latex particles through emulsion polymerization using a cationic azo initiator. J Colloid Interface Sci 25, 8292.CrossRefGoogle Scholar
Luo, H., Scriven, L.E. & Francis, L.F. (2007). Cryo-SEM studies of latex/ceramic nanoparticle coating microstructure development. J Colloid Interface Sci 316, 500509.CrossRefGoogle ScholarPubMed
Maraloiu, V.A., Hamoudeh, M., Fessi, H. & Blanchin, M.G. (2010). Study of magnetic nanovectors by Wet-STEM, a new ESEM mode in transmission. J Colloid Interface Sci 352, 386392.CrossRefGoogle ScholarPubMed
Pei, M., Wu, Y., Kim, W., Hyung, W. & Soh, Y. (2004). Effect of the monomer ratio on the properties of poly(methyl methacrylate butyl acrylate) latex-modified mortars. J Appl Polym Sci 93, 24032409.CrossRefGoogle Scholar
Segall, I., Dimonie, V.L., El-Aasser, M.S., Soskey, P.R. & Mylonakis, S.G. (1995). Core-shell structured latex particles. II. Synthesis and characterization of poly(n-butyl acrylate)/Poly(benzyl methacrylatestyrene) structured latex particles. J Appl Polym Sci 58, 401417.CrossRefGoogle Scholar
Sherman, R.L. & Ford, W.T. (2005). Semiconductor nanoparticle/polystyrene latex composite materials. Langmuir 21, 52185222.CrossRefGoogle ScholarPubMed