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Optimal Sample Preparation to Characterize Corrosion in Historical Photographs with Analytical TEM

Published online by Cambridge University Press:  26 September 2014

Eva Grieten ,
Joost Caen  and
Dominique Schryvers
Eva Grieten*
Affiliation:
EMAT, Department of Physics, University of Antwerp, Groeneborgerlaan 171, 2020 Antwerp, Belgium Research Group Heritage & Sustainability, Faculty of Design Sciences, Conservation Studies, University of Antwerp, Blindestraat 9, 2000 Antwerp, Belgium
Joost Caen
Affiliation:
Research Group Heritage & Sustainability, Faculty of Design Sciences, Conservation Studies, University of Antwerp, Blindestraat 9, 2000 Antwerp, Belgium
Dominique Schryvers
Affiliation:
EMAT, Department of Physics, University of Antwerp, Groeneborgerlaan 171, 2020 Antwerp, Belgium
*
*Corresponding author. eva.grieten@uantwerpen.be
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Abstract

An alternative focused ion beam preparation method is used for sampling historical photographs containing metallic nanoparticles in a polymer matrix. We use the preparation steps of classical ultra-microtomy with an alternative final sectioning with a focused ion beam. Transmission electron microscopy techniques show that the lamella has a uniform thickness, which is an important factor for analytical transmission electron microscopy. Furthermore, the method maintains the spatial distribution of nanoparticles in the soft matrix. The results are compared with traditional preparation techniques such as ultra-microtomy and classical focused ion beam milling.

Keywords

sample preparationfocused ion beamultra-microtomyconservation of cultural heritagecomposite materialsnanoparticles
Type
Instrumentation and Techniques Development
Information
Microscopy and Microanalysis , Volume 20 , Issue 5 , October 2014 , pp. 1585 - 1590
Copyright
© Microscopy Society of America 2014 

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References

Aronova, M.A., Kim, Y.C., Zhang, G. & Leapman, R.D. (2007). Quantification and thickness correction of EFTEM phosphorus maps. Ultramicroscopy 107, 232–244.CrossRefGoogle ScholarPubMed
Bals, S., Tirry, W., Geurts, R., Yang, Z.Q. & Schryvers, D. (2007). High-quality sample preparation by low kV FIB thinning for analytical TEM measurements. Microsc Microanal 13, 80–86.CrossRefGoogle ScholarPubMed
Bassim, N.D., De Gregorio, B.T., Kilcoyne, A.L.D., Scott, K., Chou, T., Wirick, S., Cody, G. & Stroud, R.M. (2012). Minimizing damage during FIB sample preparation of soft materials. J Microsc 245, 288–301.CrossRefGoogle Scholar
Casadio, F., Xie, S., Rukes, S.C., Myers, B., Gray, K.A., Warta, R. & Fiedler, I. (2011). Electron energy loss spectroscopy elucidates the elusive darkening of zinc potassium chromate in Georges Seurat’s A Sunday on La Grande Jatte–1884. Anal Bioanal Chem 399, 2909–2920.CrossRefGoogle Scholar
Di Pietro, G. & Ligterink, F. (2002). Silver-mirroring edge patterns: Diffusion-reaction models for the formation of silver mirroring on silver gelatin glass plates. J Am Inst Conserv 41, 111–126.Google Scholar
Edwards, H.K., Fay, M.W., Anderson, S.I., Scotchford, C.A., Grant, D.M. & Brown, P.D. (2009). An appraisal of ultramicrotomy, FIBSEM and cryogenic FIBSEM techniques for the sectioning of biological cells on titanium substrates for TEM investigation. J Microsc-Oxford 234, 16–25.CrossRefGoogle ScholarPubMed
Fraga, A.N. & Williams, R.J.J. (1985). Thermal-properties of gelatin films. Polymer 26, 113–118.CrossRefGoogle Scholar
Giachi, G., Bugani, S., Lucejko, J.J., Modugno, F. & Tatti, F. (2009). Different techniques (SR-µCT, SEM, SEM/FIB) for the evaluation of the deposition of impregnation substances into waterlogged archaeological wood. In International Conference on Wooden Cultural Heritage: Evaluation of Deterioration and Management of Change, COST IE0601, pp.1–8. Hamburg: Institute of Wood Technology and Wood Biology (HTB), Johann Heinrich von Thünen-Institute (vTI)/Federal Research Institute for Rural Areas, Forestry and Fisheries.Google Scholar
Grandfield, K. & Engqvist, H. (2012). Focused ion beam in the study of biomaterials and biological matter. Adv Mater Sci Eng 2012, Article ID 841961, 6pp.CrossRefGoogle Scholar
Hayat, M.A. (1989). Principles and Techniques of Electron Microscopy – Biological Applications. London: The Macmillan Press Ltd.CrossRefGoogle Scholar
Kejser, U. (1995). Examination of photographs with TEM-sample preparation and interpretation of the image. In Research Techniques in Photographic Conservation, American Institute for Conservation, pp. 41–45. Copenhagen: Royal Danish Academy of Fine Arts, School of Conservation.Google Scholar
Kim, S., Park, M.J., Balsara, N.P., Liu, G. & Minor, A.M. (2011). Minimization of focused ion beam damage in nanostructured polymer thin films. Ultramicroscopy 111, 191–199.CrossRefGoogle ScholarPubMed
Knott, G., Marchman, H., Wall, D. & Lich, B. (2008). Serial section scanning electron microscopy of adult brain tissue using focused ion beam milling. J Neurosci 28, 2959–2964.CrossRefGoogle ScholarPubMed
Lubelli, B., de Winter, D.A.M., Post, J.A., van Hees, R.P.J. & Drury, M.R. (2013). Cryo-FIB-SEM and MIP study of porosity and pore size distribution of bentonite and kaolin at different moisture contents. Appl Clay Sci 80–81, 358–365.CrossRefGoogle Scholar
Monico, L., Van der Snickt, G., Janssens, K., De Nolf, W., Miliani, C., Verbeeck, J., Tian, H., Tan, H., Dik, J., Radepont, M. & Cotte, M. (2011). Degradation process of lead chromate in paintings by Vincent van Gogh studied by means of synchrotron X-ray spectromicroscopy and related methods. 1. Artificially aged model samples. Anal Chem 83, 1214–1223.CrossRefGoogle Scholar
Schaffer, M., Schaffer, B. & Ramasse, Q. (2012). Sample preparation for atomic-resolution STEM at low voltages by FIB. Ultramicroscopy 114, 62–71.CrossRefGoogle ScholarPubMed