Long-Range Order Parameter Determination by Convergent Beam Electron
Diffraction
K.L. Torres,* R.R. Vanfleet,** and G.B. Thompson*
* Department of Metallurgical and Materials Engineering, University of Alabama College of
Engineering, Tuscaloosa, AL 35487
** Department of Physics and Astronomy, Brigham Young University College of Physical and
Mathematical Science, Provo, UT 84602
The L1
0
phase of Fe-Pt has been identified as a leading candidate for ultrahigh-density magnetic
storage media because of its high magnetocrystalline anisotropy, K
u
[1]. The K
u
of this alloy has
been known to be strongly dependent on the long-range order parameter S, where K
u
decreases with
S [2]. S can be determined by a number of methods. The most readily available technique is x-ray
diffraction. Experimentally, S is determined by measuring the total integrated peak intensities of the
superlattice and fundamental reflections according to kinematical scattering theory [3]. However, the
amount of x-ray scattering from thin films can be very small and difficult to measure with laboratory
diffractometers. In contrast, electron scattering can be more amenable for diffraction studies of small
volumes, though the strong interaction of electrons with the thin film results in multiple scattering
events. As a result, the traditional methodology of taking the ratio of integrated intensities no longer
applies and S determination becomes more complex. In this study, the multislice simulation
approach was used to simulate electron transmission in crystalline thin films including dynamical
scattering [4] to determine S which was then compared to x-ray measurements of S on the same
films.
An 11.7 nm Fe
50
Pt
50
thin film was dc magnetron sputter-deposited from commercially pure Fe and
Pt targets onto an MgO <001> substrate heated to a temperature of 500 °C. Post-deposition, the film
was annealed at 600°C for 30 minutes in an Ar/4%H
2
atmosphere. The composition of the film was
determined by Rutherford backscattering spectrometry (RBS). Convergent-beam electron diffraction
(CBED) patterns were experimentally collected using scanning transmission electron microscopy
(STEM) in a FEI Tecnai F20 operated at 200 keV. A convergent beam of 4 mrad convergence semi-
angle was focused on the specimen to obtain the CBED patterns. This angle was chosen to give the
minimal overlap between the diffracted disks. In this experiment, CBED patterns with [001] beam
incidence were recorded using a 1k charge-coupled device (CCD) camera using an integration time
of 0.5 s.
To correctly account for multi-scattering events of the electrons, a multislice simulation needs to be
used to predict the CBED intensities for given order parameters and thicknesses. In this study, the
ratio of the (110) superlattice to the (220) fundamental reflection (I
110
/I
220
) was used. The input
parameters for the multislice simulations were matched to the experimental conditions (e.g.
convergence semi-angle of 4 mrad; spherical aberration coefficient C
s
of 1.35 mm; temperature of
94K; and specimen thickness). Fig. 1a is a simulated CBED pattern for [001] zone axis, order
parameter of 0.4, and a film thickness of 11.7 nm. Fig. 2 is the simulated results for the measured
film thickness and for thicknesses associated with the estimated error of the measurements.
250
doi:10.1017/S1431927610058113
Microsc. Microanal. 16 (Suppl 2), 2010
© Microscopy Society of America 2010
. https://doi.org/10.1017/S1431927610058113
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