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Ultramicrotomy for Materials Science

Published online by Cambridge University Press:  16 February 2011

T. F. Malis  and
D. Steele
T. F. Malis
Affiliation:
Metals Technology Laboratories, CANMET, 568 Booth St, Ottawa, Canada K1A OG1
D. Steele
Affiliation:
Alcan International Ltd, Kingston R & D Center Box, 8400 Kingston, Ontario K71 4Z4
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Abstract

Diamond knife sectioning, or ultramicrotomy, is being used increasingly as an attractive alternative or complimentary means of producing quality TEM specimens. This paper represents a first attempt to provide a basic methodology for this technique for materials scientists, point out its drawbacks, provide a comprehensive listing of more than three decades of widely-scattered and ingeneous applications, and illustrate the diversity of these applications with clear examples. Suggestions will be made for further improvements in ultramicrotomy so that it can be applied in a more routine fashion to modern advanced materials or TEM applications involving demanding chemical microanalysis.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 199: Symposium W – Specimen Preparation for Transmission Electron Microscopy of Materials II , 1990 , 3
Copyright
Copyright © Materials Research Society 1990

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References

REFERENCES

1. Goodhew, P.J., Thin Foil Preparation for Electron Microscopy, Practical Methods in Electron Microscopy, vol 11, Glauert, A.M., ed (Elsevier, Amsterdam, 1985).Google Scholar
2. Malis, T., EMAG-87 & Analytical Electron Microscopy (Inst. of Metals, London, 1988) pp. 127–134.Google Scholar
3. Goodhew, P.J., Soecimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp.51–62.Google Scholar
4. Malis, T.F., Microbeam Analysis 1989 (San Francisco Press, San Francisco, 1989) pp. 487–494.Google Scholar
5. Specimen Preoaration for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) 292 pp.Google Scholar
6. Rice, S. B. and Treacy, M.M.J., Specimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 15–27.Google Scholar
7. Sawyer, L.C. and Grubb, D.T., Polymer Microscopy (Chapman and Hall, London, 1987) pp 85–95.Google Scholar
8. Reimer, L., Metallkunde, Z., 5, 37–41 (a), 604–610 (b),(1959) (in German).Google Scholar
9. Phillips, V.A., Direct Observations of Imperfections in Crystals, Newkirk, J. and Wernick, J., eds (Wiley, New York, 1962) pp 179–203.Google Scholar
10. Phillips, V. A., Praktische Metallographie, 4, 637 (1967).Google Scholar
11. Tice, W.K. and Lasko, W.R., Anal. Chem., 35,1553–1554 (1963)Google Scholar
12. Dawson, I.M. and Follett, E.A.C., Proc. Roy. Soc., 253, 390–402 (1959)Google Scholar
13. Granzer, F., Haase, G. and Zorgiebel, F., J. App. Phys., 37, 457 (1966).Google Scholar
14. Dorsey, G.A. Jr., J. Electrochem. Soc., 116., 466–471 (1969).Google Scholar
15. Yada, K., Acta Crystallographica, 23, 704–707 (1967).Google Scholar
16. Thomas, G., Transmission Electron Microscopy of Metals (Wiley, New York, 1962) p. 182.Google Scholar
17. Hayat, M.A., Principles and Techniques of Electron Microscopy, Biological Applications, Vol.1 (Van Nostrand Reinhold, 1970).Google Scholar
18. Meek, G.A., Practical Electron Microscopy for Biologists (Second Edition, Wiley, New York, 1975).Google Scholar
19. Dawes, C.J., Biological Techniques for Transmission and Scanning Electron Microscopy (Ladd Research Industries, 1979).Google Scholar
20. Reid, N., Ultramicrotomy, Practical Methods in Electron Microscopy, vol 3, Glauert, A.M., ed (Elsevier, Amsterdam, 1974).Google Scholar
21. Sitte, H. and Neumann, K., Methods of Electron Microscopy, Schimmel, G. and Vogell, W., eds (Wiss. Veriag GmbH, Stuttgart, 1983).Google Scholar
22. Seveus, L. and Tarras-Wahlberg, C., The Science of Biological Specimen Preparation for Microscopy and Microanalysis, Proc. Fourth Pfefferkorn Conf. 1985 (Scanning Microscopy, Inc., AMF O'Hare, Chicago, 1986) pp 129–134.Google Scholar
23. Robinson, D.G., Ehlers, U., Herken, R., Herrmann, B., Mayer, F. and Schurmann, F.-W., Methods of Preparation for Electron Microscopy, An Introduction for the Biomedical Sciences (Springer-Verlag, New York, 1987) pp 43–76.Google Scholar
24. Fernandez-Moran, H., The Beginninos of Electron Microscoov (Academic Press, New York, 1985) pp. 167–224.Google Scholar
25. Warner, R.R., J. Micros., 13, 203–207 (1984).Google Scholar
26. Murphy, J.A. and Price, R.L., Proc. 41st Annual Meeting EMSA, 624–625 (1983).Google Scholar
27. Fosch, D., Westphal, C. and Bachhuber, K., Ultramicroscopy, 17., 141–46 (1985).Google Scholar
28. Acetarin, J.-D., Carlemalm, E., Kellenberger, E. and Villiger, W., J. of EM Techniques, 6, 63–79 (1987).Google Scholar
29. Fernandez-Moran, H., Ultramicroscopy, 20, 317–328 (1986).Google Scholar
30. Mollenhauer, H. and Bradfute, O.E., J. of EM Techniques, 6, 173–174 (1987).Google Scholar
31. Lauer, R., Ade, G. and Lickfeld, K.-G., Deutscher Verband fur Materialprufung 345–350 (1988) (in German).Google Scholar
32. Hodgson, C.P. and Cunningham, W.P., J. Micros., 146, 103–107 (1987).Google Scholar
33. Jesior, J.-C., J. Ultrastr. and Mol. Str. Res., 95, 210–217 (1986).Google Scholar
34. Jesior, J.-C., Scanning Microscopy Supplement, 3, 147–153 (1989).Google Scholar
35. Davidson, E.A. and Rieder, C.L., J. of EM Techniques, 2, 395–396 (1985).Google Scholar
36. Mollenhauer, H.H., J. EM. Techniques, 4,173–174 (1986).Google Scholar
37. Bradley, S.A., Dietz, N.L. and Karakek, K.R., Specimen Preparation for Transmission Electron Microscopy of Materials- Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh) 1988, pp 115–117.Google Scholar
38. Lee, S.Y., Jackson, M.L. and Brown, J.L., Clays and Clay Minerals, 23, 125–129 (1975).Google Scholar
39. Katz, W., Evans, C.A. Jr., Eaton, D.R. and Faulkner, L.R., J. Vac. Sci. Tech., 15, 1561–1564 (1978)Google Scholar
40. Marshall, A.F. and Dobbertin, D.C., Ultramicroscopy, 19, 69–74 (1986).Google Scholar
41. Csencits, R., Schooley, C. and Gronsky, R., J. EM. Techniques, 2, 643–644 (1985). See also R. Csencits and R. Gronsky, Specimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 103–108.Google Scholar
42. Heuer, J.P. and Howitt, D.G., J. EM. Techniques, 14, 79–82 (1990).Google Scholar
43. McMahon, G., Carpenter, G.J.C. and Malis, T.F., J. Mat. Sci., submitted.Google Scholar
44. McCune, R.C. and Plummer, H.K., Surace and Interface Analysis, 4, 257–260 (1982).Google Scholar
45. Stevens, D.W. and Gillmeister, R.N., Microstructural Science, vol 5, Proc. 9th Ann. Meeting Int. Metallogr. Soc. (Elsevier, New York, 1977) pp 277–285.Google Scholar
46. Swab, P. and Klinger, R.E., Specimen Preparation for Transmission Electron Microscoov of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 229–234.Google Scholar
47. Ekmejian, E.M. and Bulko, J.B., Specimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 87–92.Google Scholar
48. Stobbs, W.M., Kallend, J.S. and Williams, J.A., Acta Met., 24, 1083–1093 (1976).Google Scholar
49. Sawruk, S., Rohrman, A.C. Jr., and Kokotailo, G.T., J. Cataly., 40, 379–382 (1975).Google Scholar
50. Hall, J.B., Proc. 42nd Annual Meeting EMSA, 650–651 (1984).Google Scholar
51. Ho, H.-M., Thomas, G., Schooley, C. and Gau, J.-S., Specimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 149–154.Google Scholar
52. Maniette, Y., J. Mat. Sci., 9, 48–50 (1990).Google Scholar
53. Malis, T., Steele, D. and Ball, M.D., AEM Workshop. (San Francisco Press,1984) pp. 189–192.Google Scholar
54. Bethune, B., Furneaux, R.C. and Wood, G.C., J. Mat. Sci., L 2, 1764 (1977).Google Scholar
55. Kobayashi, K., Shimuzu, K. and Tsuda, Y., J. Japan Inst. Light Metals, 39, 457–459 (1989).Google Scholar
56. Zorgiebel, F., Zeindl, H.P. and Haase, G., Ultramicroscopy, 16, 115–118 (1985).Google Scholar
57. Alderson, R.H., Design of the Electron Microscope Laboratory, Practical Methods in Electron Microscopy, vol 4, Glauert, A.M., ed (Elsevier, Amsterdam, 1975) pp 92–94.Google Scholar
58. Fraser, T.W., J. Micros., 106, 97–99 (1976).Google Scholar
59. Krivanek, O.L. and Kundmann, M.K., Inst. Phys. Conf. Series 98, EMAG-MICRO 89 (Inst. Physics, London, 1990) pp. 33–40.Google Scholar
60. Egerton, R.F., Electron Energy Loss Spectroscopy in the TEM (Plenum, New York, 1986).Google Scholar
61. Malis, T., Rajan, K., Titchmarsh, J.M. and Weatherly, G.C., Intermediate Voltage Microscopy and Its Apolication to Materials Science (Philips, Mahwah, N. J., 1986) pp.78–86.Google Scholar
62. Goldstein, J.l., Williams, D.B. and Cliff, G., Princioles of Analytical Electron Microscopy (Plenum, New York, 1986).Google Scholar
63. Auerhammer, J., Rez, P. and Hofer, F., Ultramicroscopy, 30, 365–370 (1989).Google Scholar
64. Malis, T.F., Cheng, S.C. and Egerton, R.F., J. of EM Techniques, 8, 193–200 (1988).Google Scholar
65. Malis, T., Third Int. AI-Li Conf. (Inst. of Metals, London, 1986) pp.347–354.Google Scholar
66. Malis, T.F., Proc. Micros. Soc. of Canada, 16, 50–51 (1989).Google Scholar
67. Sitte, H., The Science of Biological Specimen Preparation for Microscopy and Microanalysis. Proc. Second Pfefferkorn Conf., 1983 (Scanning Microscopy, Inc., AMF O'Hare, Chicago,, 1984) pp. 97–104.Google Scholar
68. Ahlers, M. and Vasamillet, L.F., J. App. Phys., 39, 3592–3596 (1968).Google Scholar
69. Ramalingen, S. and Black, J.T., Met. Trans., 4, 1103–1112 (1973).Google Scholar
70. Williams, G. and Malis, T., unpublished work.Google Scholar
71. Kim, H.S., Thompson, G.E., Wood, G.C., Wright, I.G. and Maringer, R.E., Proc. 9th Int. Conf. Metallic Corrosion, Toronto, 1984 (National Research Council, Ottawa) vol.2, pp 659–666.Google Scholar
72. Thompson, G.E., Furneaux, R.C. and Wood, G.C., Trans. Inst. Metal Finishing, 5, 117–128 (1977).Google Scholar
73. Ogura, I., J. Elec. Micros.(Japan), 30, 171–176 (1981).Google Scholar
74. Thompson, G.E. and Wood, G.C., J. Microsc. Spectrosc. Electronique, 12, 391–402 (1987).Google Scholar
75. Karimzadeh, H., Thompson, G.E., Jeong, Y.S., Namgoong, E., Jones, S.N. and Wood, G.C., Inst. Phys. Conf. Series 90, EMAG-87 (Inst. of Phys., London, 1987), pp 27–30.Google Scholar
76. Omler, R.E. and Lloyd, P.F., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco,1989) pp 710–711.Google Scholar
77. Gupta, D. and Kim, K.K., J. App. Phys., 51, 2066–2069 (1980).Google Scholar
78. Merk, N. and Tanner, L.E., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco,1989) pp 678–679.Google Scholar
79. Legresy, J.M., Sainfort, P., Audier, M., Simon, J.P. and Guyot, P., J. Phys. Colloq. (France), 46, C8, 579–583 (1985).Google Scholar
80. Hanchet, V.E. and Geiss, R.H., IBM J. Res. & Dev., 27, 348–355 (1983).Google Scholar
81. Gebizlioglu, O.S., Argon, A.S. and Chen, R.E., Specimen Preparation for Transmission Electron Microscopy of Materials, Mat. Res. Soc. Symp. Proc., vol 115 (Materials Research Society, Pittsburgh, 1988) pp 137–142.Google Scholar
82. Wood, B.A., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco,1989) pp 352–353.Google Scholar
83. Kunz, M. and Moller, M., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 356–357.Google Scholar
84. Cieslinski, R.C., Dineen, M.T., Marshall, J.G., Blackson, J.H., Mizer, D. and Garrett, H.L., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 700–701.Google Scholar
85. Watts, E.J., Metallography, 9, 43–49 (1976).Google Scholar
86. Matsui, Y., Nat. Inst. for Res. in Inorganic Materials, Ibaraki, Japan, unpublished work, (ultramicrotomy follow-up to improve images in Matsui et al, Jap. J. App. Phys., 28, 602–605 (1989)).Google Scholar
87. Kerch, H.M., Gerhardt, R.A. and Grazul, J.L., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 436–437.Also Kerch and Gerhardt, pp 438–439.Google Scholar
88. Takahashi, H., Nagayama, M., Akahori, H. and Kitahara, A., J. of Elec. Micros. (Japan), 22, 149–157 (1973).Google Scholar
89. Furneaux, R.C., Thompson, G.E. and Wood, G.C., Corrosion Sci., 18, 853–881 (1978).Google Scholar
90. Cavalcanti, E., Thompson, G.E., Wood, G.C. and Dawson, J.L., Proc. 9th Int. Conf. Metallic Corrosion, Toronto, 1984 (National Research Council, Ottawa, 1984) vol 3, pp.36–43.Google Scholar
91. Shimuzu, K., Thompson, G.E., Wood, G.C., Kurima, Y. and Kobayashi, K., Thin Solid Films, 173, 263–268 (1989).Google Scholar
92. Kobayashi, K., Shimuzu, K. and Tsuda, Y., J. Japan Inst. Light Metals, 39, 457–459 (1989).Google Scholar
93. Kawai, S. and Ueda, R., J. Electrochem. Soc., 122, 32–36 (1975).Google Scholar
94. Dartyge, J.M. and Ferrieres, C., Wear, 63, 339–346 (1980).Google Scholar
95. Timsit, R.S., Hutchison, J.L. and Thornton, M.C., Ultramicroscopy, 15, 371 (1984).Google Scholar
96. Narayan, P.B., Proc. 43rd Ann. Meeting EMSA, (San Francisco Press, San Francisco, 1985) pp 212–213.Google Scholar
97. Steele, D. and Rosenfeld, A., EMAG-87 & Analytical Electron Microscopy (Inst. of Metals, London, 1988) pp.187–190.Google Scholar
98. Gaffet, E., Deluze, G., Martin, G. and Pelletier, J.M., J. Phys. Colloq. (France), 48, C7, 131–134 (1987).Google Scholar
99. Gaffet, E., Deluze, G., Martin, G., Pelletier, J.M. and Pergue, D., Mat. Sci. and Eng., 98, 291–294 (1988).Google Scholar
100. Crompton, J.S., J. Mat. Sci., 24, 1575–1581 (1989).Google Scholar
101. Bartella, J. and 26 coauthors, Applied Optics, 24, 2625–2646 (1985).Google Scholar
102. Yahalom, J., Tessier, D.F., Timsit, R.S., Rosenfeld, A.M., Mitchell, D.F. and Robinson, P.G., J. Mat. Res., 4, 755–758 (1989).Google Scholar
103. Hall, J.B. and Hruskoci, P.P., Proc. 41st Annual Meeting EMSA, 342–343 (1983).Google Scholar
104. White, D., Ramdas, S. and Millward, G.R., Inst. Phys. Conf. Series 78, EMAG-85 (Inst. of Physic, London, 1985) pp 501–504.Google Scholar
105. Chan, I.Y., J. Elec. Micros. Techniques, 2, 525–532 (1985).Google Scholar
106. Legrouri, A., Baird, T. and Fryer, J.R., Inst. Phys. Conf. Series 90, EMAG-87 (Inst. of Physic, London, 1987) pp 31–34.Google Scholar
107. Szymanski, R. and Lynch, J., Inst. Phys. Conf. Series 93, Eurem-88 (Inst. of Physic, London, 1988) vol 2, pp 295–296.Google Scholar
108. Ulan, J. and Gronsky, R., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 268–269 (a). See also these Proceedings (b).Google Scholar
109. Plummer, H.K. Jr, and Otto, K., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 270–271.Google Scholar
110. Van Dyck, D., Van Landuyt, J., Jellinek, F. and Amelinckx, S., Ultramicroscopy, 4, 467–471 (1979).Google Scholar
111. Matson, L.E. and Omlor, R.E., Rapid Solidification Processing, Principles and Technologies, 135–140 (1980).Google Scholar
112. Garland, C.M. and Johnson, R. W., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 718–719.Google Scholar
113. Tucker, D.S., Jenkins, E.J. and Hren, J.J., J. EM. Techniques., 2, 29–33 (1985).Google Scholar
114. Pickles, P.G. and Lilly, E., J. Amer. Ceramic Soc., 68, C–222 (1985).Google Scholar
115. Dufner, D.C., Ram, R.A.Mohan and Clearfield, A., Proc. 47th Annual Meeting EMSA, 1989 (San Francisco Press, San Francisco, 1989) pp 192–193.Google Scholar
116. Serin, V., Guigon, M., Fourmeaux, R., Kihn, Y. and Sevely, J., Inst. Phys. Conf. Series 98, EMAG-MICRO 89 (Inst. Phys., London, 1990) pp 79–82.Google Scholar
117. Steele, D. and Otto, A., Inst. Phys. Conf. Series 90, EMAG-87 (Inst. of Physic, London, 1987) pp 27–30.Google Scholar
118. Ball, M.D. and Furneaux, R.C., Inst. Phys. Conf. Series 61, EMAG-81 (Inst. of Physic, London, 1982) pp 179–180.Google Scholar
119. Xu, Y., Thompson, G.E. and Wood, G.C., J. Electrochem. Soc., 130, 2395 (1983).Google Scholar
120. Oster, C.F., Proc. 26 th Annual Meeting EMSA, 332–333 (1968).Google Scholar
121. Russell, R.R., Proc. Ninth Int. Congress on Elec. Micros., vol.1, 488–489 (1978).Google Scholar
122. Shimizu, K., Thompson, G.E. and Wood, G.C., Thin Solid Films, 77, 313–318 and 85, 53–59 (1981).Google Scholar
123. Furneaux, R.C., Trans. Inst. Metal Finishing, 61 (1983).Google Scholar
124. Blake, D.F., Bunch, T.E., Philpott, D.E. and Zeiger, R., J. Elec. Micros. Techniques, 6, 305–306 (1987).Google Scholar
125. Takahashi, H. and Nagayama, M., Electrochemica Acta, 23, 279–286 (1978).Google Scholar