Abstract
Doped skeletal copper catalysts, created by selective dissolution of aluminium from a copper-aluminium alloy by caustic in the presence of an additive, has been imaged at very high magnification using a TEM. The location of the additive species has been determined by elemental mapping using an attached EDS detector. Zinc resides primarily inside the copper ligaments while chromium resides on the outside of the ligaments. Since skeletal copper is highly porous and extremely sensitive, conventional TEM preparation techniques could not be used. The preparation of the TEM samples was carried out using a focussed ion beam (FIB) miller. Several methods are outlined, along with the reasons some of them were unsuccessful for this particular material. The successful result indicates this technique may be used to analyse similar skeletal materials, such as nickel, cobalt, etc., which are otherwise difficult to prepare. It may also provide a basis for high resolution imaging or elemental analysis of other porous and/or highly sensitive materials.
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References
L. Faucounau, Bull. Soc. Chim. 4(5) (1937) 58 (Chem. Abs. 31:32171).
A. D. Tomsett, M. S. Wainwright, and D. J. Young, Appl. Catal. 12 (1984) 43.
M. S. Wainwright, in “Handbook of Heterogeneous Catalysis,” edited by G. Ertl, H. Knözinger and J. Weitkamp (1998) p. 64.
M. Raney, Ind. Eng. Chem. 32(9) (1940) 1199.
B. V. Aller, J. Appl. Chem. 7 (1957) 130.
M. Raney, US Patent no. 1, 563, 587 (Dec. 1, 1925).
Idem., US Patent no. 1, 628, 190 (May 10, 1927).
L. M. Kefeli and S. L. Lel'chuk, Doklady Akad. Nauk S.S.S.R. 84 (1952) 285 (Chem. Abs. 46:10822c).
idem rentgen. metody issledovan. i primenenie v khim. prom. goskhimizdat (sbornik) (1953) 78 (chem. abs. 50:3862d).
M. M. Kalina, A. B. Fasman and V. N. Ermolaev, Deposited Doc. VINITI 1022–80 (1980) 15 (Chem. Abs. 95:66291p).
U. Birkenstock, R. Holm, B. Reinfandt and S. Storp, J. Catal. 93 (1985) 55.
J. Szot, D. J. Young, A. Bourdillon and K. E. Easterling, Phil. Mag. Lett. 55(3) (1987) 109.
A. J. Smith, T. Tran and M. S. Wainwright, J. Appl. Electrochem. 29(9) (1999) 1085.
L. Ma, D. L. Trimm and M. S. Wainwright, in “Advances of Alcohol Fuels in the World” (Beijing, China, 1998) p. 1.
Idem., Topics in Catalysis 8 (1999) 271.
A. J. Smith, L. Ma, T. Tran and M. S. Wainwright, J. Appl. Electrochem. 30 (2000) 1097.
A. J. Smith, T. Tran and M. S. Wainwright, ibid. 30 (2000) 1103.
H. E. Curry-hyde, M. S. Wainwright and D. J. Young, Appl. Catal.77 (1991) 75.
L. Ma, A. J. Smith, T. Tran and M. S. Wainwright, Chem. Eng. Process. 40 (2001) 59.
R. Anderson and S. J. Klepeis, in Specimen Preparation for Transmission Electron Microscopy of Materials IV, San Francisco, California, U.S.A., 1997 (Materials Research Society) Vol. 480, p. 187.
D. H.-I. Su, H. T. Shishido, F. Tsai, L. Liang and F. C. Mercado, in Specimen Preparation for Transmission Electron Microscopy of Materials IV, San Francisco, California, U.S.A., 1997 (Materials Research Society) Vol. 480, p. 105.
M. W. Phaneuf, N. Rowlands, G. J. C. Carpenter and G. Sundaram, in Specimen Preparation for Transmission Electron Microscopy of Materials IV, San Francisco, California, U.S.A., 1997 (Materials Research Society) Vol. 480, p. 39.
J. L. Murray, Intern. Metals Rev. 30(5) (1985) 211.
M. M. Kalina, A. B. Fasman and V. N. Ermolaev, Kinet. Katal. 21(3) (1980) 813 (Chem. Abs. 93:81065v).
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Smith, A.J., Munroe, P.R., Tran, T. et al. FIB preparation of a sensitive porous catalyst for TEM elemental mapping at high magnifications. Journal of Materials Science 36, 3519–3524 (2001). https://doi.org/10.1023/A:1017984618032
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DOI: https://doi.org/10.1023/A:1017984618032