Abstract
We demonstrate the application of a new method of analytical transmission electron microscopy for measuring very accurately small amounts of solute atoms within a well-defined planar defect such as a stacking fault, grain boundary or an interface. The method is based on acquiring several spectra with different electron beam diameters from the same position centred on the defect. It can be applied to energy-dispersive X-ray microanalysis (EDXS) or electron energy-loss spectroscopy (EELS) and does not necessitate a scanning unit. The accuracy has been tested numerically under different conditions using simulations for a specific geometry and has been found to be substantially better than that of any other current standard technique. Our calculations suggest an extremely high accuracy theoretically achievable in the determination of e.g. the Gibbsian solute excess or the doping level of a grain boundary down to about ±1% of an effective monolayer, i.e. ±0.1 atoms/nm2 under typical experimental conditions. The method has been applied to zinc oxide, which forms inversion domain boundaries (IDBs) when doped with different transition metal oxides such as SnO2 or Sb2O3. We obtained an experimental precision of ±0.4 atoms/nm2, which has allowed us to solve the atomic structure of the IDBs.
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References
E.D. Hondros and M.P. Seah, Scripta Metall. 6(10), 1007 (1972).
C.J. McMahon Jr. and L. Marchut, J. Vac. Sci. Tecnol. 15(2), 450 (1978).
M.P. Seah and E.D. Hondros, Proc. Royal Soc. London A 335(1601), 191 (1973).
H. Müllejans and J. Bruley, Ultramicroscopy 53(4), 351 (1994).
L.E. Rehn, P.R. Okamoto, D.I. Potter, and H. Wiedersich, J. Nucl. Mater. 74(2), 242 (1978).
A. Recnik, M. Ceh, and D. Kolar, J. Eur. Ceram. Soc. 21(10/11), 2117 (2001).
A. Recnik, N. Daneu, T. Walther, and W. Mader, J. Am. Ceram. Soc. 84(11), 2657 (2001).
J. Bruley, U. Bremer, and V. Krasevec, J. Am. Ceram. Soc. 75(11), 3127 (1992).
J. Bruley, T. Höche, H.J. Kleebe, and M. Rühle, J. Am. Ceram. Soc. 77(9), 2273 (1994).
V.J. Keast and D.B. Williams, J. Microsc. 199(1), 45 (2000).
U. Alber, H. Müllejans, and M. Rühle, Ultramicroscopy 69(2), 105 (1997).
J. Bruley, J. Cho, H.M. Chan, M.P. Harmer, and J.M. Rickman, J. Am. Ceram Soc. 82(10), 2865 (1999).
V.J. Keast and D.B. Williams, Acta Mater. 47(15/16), 3999 (1999).
J. Bruley, Philos. Mag. Lett. 66(1), 47 (1992).
H. Gu, R.M. Cannon, and M. Rühle, J. Mater. Res. 13(2), 376 (1998).
D.A. Shashkov and D.N. Seidman, Mater. Science Forum 207(1), 429 (1996).
D.A. Shashkov, D.A. Muller, and D.N. Seidman, Acta Mater. 47(15/16), 3953 (1999).
D. Isheim, O.C. Hellman, D.N. Seidman, F. Danoix, A. Bostel, and D. Blavette, Microsc. Microanal. 7(5), 424 (2001).
J.J. Hren, J.I. Goldstein, and D.C. Joy (Eds.), in Introduc-tion to Analytical Electron Microscopy (Plenum, New York, 1979).
S.A. Collett, L.M. Brown, and M.H. Jacobs, in Proc.Quant.Mi-croanal.with High Spatial Resolution, Manchester (The Metals Society, London, 1981), p. 159.
T. Walther and C.J. Humphreys, J. Cryst. Growth 197(1/2), 113 (1999).
V.J. Keast and D.B. Williams, in Proc.EMAG 97, Cambridge, edited by J.M. Rodenburg, Inst. Phys. Conf. Ser. (IoP, Bristol, 1997), Vol. 153, p. 299.
R.D. Carter, D.L. Damcott, M. Atzmon, G.S. Was, S.M. Bruemmer, and E.A. Kenik, J. Nucl. Mater. 211(1), 70 (1994).
D.B. Williams, A.J. Papworth, and M. Watanabe, J. Electr. Microsc. 51(S), 113 (2002).
G. Drazic and M. Komac, in Proc.13th Int.Cong.Electron Microsc., edited by B. Jouffrey and C. Colliex (les editions de physique, Les Ulis, Paris, 1994), Vol. 1, p. 685.
J.I. Goldstein, J.L. Costley, G.W. Lorimer, and S.J.B. Reed, in Proc.Anal.Electr.Microsc., Scanning Electron Microsc. (IIT Res. Inst., Chicago, 1977), Vol. 1, p. 315.
S.J.B. Reed, Ultramicroscopy 7(4), 405 (1982).
T. Walther, A. Recnik, and N. Daneu, in Proc.15th Int.Cong.Electron Microsc., edited by J. Engelbrecht, M. Witcomb, and R. Cross (Microsc. Soc. South Africa, Onderstepoort, Durban, 2002), Vol. 1, p. 535.
N. Daneu, A. Recnik, S. Bernik, and D. Kolar, J. Am. Ceram Soc. 83(12), 3165 (2000).
N. Daneu, T. Walther, and A. Recnik, in Proc.15th Int.Cong.Electron Microsc., edited by J. Engelbrecht, T. Sewell, M. Witcomb, and R. Cross (Microsc. Soc. South Africa, Onderstepoort, Durban, 2002), Vol. 3, p. 63.
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Walther, T., Daneu, N. & Recnik, A. A New Method to Measure Small Amounts of Solute Atoms on Planar Defects and Application to Inversion Domain Boundaries in Doped Zinc Oxide. Interface Science 12, 267–275 (2004). https://doi.org/10.1023/B:INTS.0000028656.12913.8a
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DOI: https://doi.org/10.1023/B:INTS.0000028656.12913.8a