Solid State Phenomena Vol.

163 (2010) pp 13-18

Online available since 2010/Jun/07 at www.scientific.net
© (2010) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/SSP.163.13

Orientation mapping study on the inhomogeneous microstructure

evolution during annealing of 6013 aluminum alloy

M. Bieda1, a, K. Sztwiertnia1,b , A. Korneva1,c, T. Czeppe1,d , R. Orlicki2,e

1
Institute of Metallurgy and Materials Science, Polish Academy of Science, 25 Reymonta St.,
30-059 Krakow, Poland
2
Department of Materials Science, Medical University of Silesia, 1 Akademicki Sq.,
41-9002 Bytom, Poland
a b c
[email protected], [email protected], [email protected],
d
[email protected], [email protected]

Keywords: Transmission electron microscopy (TEM), Convergent beam electron diffraction

(CBED), Orientation imaging microscopy (OIM), Aluminum alloys.

Abstract. Orientation mapping in transmission electron microscope was successfully applied to

study microstructural changes at the initial stage of recrystallization in the aluminum alloy with a
bimodal second-phase particle distribution. The alloy samples were reversibly cold rolled resulting
in the formation of laminar structure with zones of localized strain around large second-phase
particles. Orientation mapping and in-situ investigations carry information about the processes
which are active in the deformation zones during annealing.

Introduction
The characterization of microstructures has advanced in great part to the development of new
generations of computer-controlled electron microscopes. New technologies have improved spatial
resolution and have increased the rate of collecting and processing of large quantities of data. The
Orientation Imaging Microscopy (OIM) is a well-established technique for studying and quantifying
microstructures and can determine crystallographic orientations and topography by using Electron
Back Scattered Diffraction (EBSD) in a Scanning Electron Microscope (SEM) e.g. [1]. The main
concept behind this technique is the automatic collection and indexing of many diffraction patterns
that are correlated with sample coordinates. Characteristics based on the sets of measured
orientations provide essential information about the grains, grain boundaries and about local
crystallographic lattice deformation. Systems created using EBSD in SEM are very common, and
that one’s commercially available are essentially fully automated e.g. [1, 2].
Nevertheless, the spatial resolution of SEM measurements is strongly dependent on the type
of electron gun and material being investigated. The resolution in special cases is as good as 30 nm;
however generally is about 100 nm. This limitation restricts the application of SEM in investigating
very fine-grained and deformed materials. In order to obtain better spatial and angular resolution,
similar systems were developed for a Transmission Electron Microscope (TEM) [2, 3, 4]. Despite
some restrictions, such as the unsolved problems with image analysis, difficulties in the
measurement automation and sample preparation, the OIM technique in TEM offers spatial
resolution less than 10 nm and can be used for quantitative analysis of the microstructure at the
nanoscale. Such a system was built in the Institute of Metallurgy and Materials Science and is
based on the general methods for indexing Kikuchi-type diffraction patterns that were introduced in
the literature [4, 5, 6]. Convergent Beam Electron Diffraction (CBED) patterns are mainly used for
creating orientations maps.
An example of the results obtained by applying this system to recrystallization in aluminum
alloy 6013 is presented in this paper. Aluminum alloy 6013 was chosen as a prototype material that
represents a group of commercial alloys with a bimodal second phase particle distribution. Such

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14 Applied Crystallography XXI

alloys can be interesting for considering the role of second phase particles in a recrystallization
process e.g. [7, 8, 9, 10]. There is a need for investigating the early stages of the recrystallization,
based on the analyzing changing orientation topography during annealing [11, 12].

Materials and methods

The testing material was supersaturated and aged. The heat treatment produced a relatively
uniform distribution of stable particles, both small (<< 1 µm) and large (> 1 µm). Aged samples
were then 75% and 90% reversibly cold-rolled.
Specimens were prepared mainly from longitudinal sections (i.e. section perpendicular to the
transverse direction). Bright field images and crystallographic orientations maps of particular sites
of the deformed state, as well as the partly recrystallized state, were obtained by gathering and
indexing the CBEDs in the TEM. Two type of investigations were carried out in parallel. In-situ
studies provided information about the temporal relationships between changes that occurred at the
onset of recrystallization. In order to check up on the reliability of the in-situ results, combined
calorimetric-microscopic studies of the bulk samples were also performed.
During the first investigation, a thin foil was annealed inside the TEM with the help of a
heating holder. After annealing, the identical sites as in the deformed state were analyzed and the
orientation of the nuclei and the new grains were determined.

Results and discussion

TEM observations showed that the deformed structure was comprised of wavy layers of
microbands, lying roughly parallel to the rolling plane. Small and large particles were dispersed in
this lamellar structure. The large particles broke up the lamellar structure and created deformation
zones (DZ) in the adjacent areas.
Because of insufficient spatial resolution of the EBSD method, investigating the orientation
of the deformed alloy using an SEM with FEG (Field Emission Gun) was not feasible, even in the
matrix areas. Furthermore, the high degree of deformation, especially in the 90 % cold-rolled
material, resulted in low quality diffraction patterns in the TEM. Kikuchi lines were diffuse and
blurred. However, it was still possible to measure orientation maps of DZs in TEM for both 75%
and 90% cold-rolled materials. In the zones, small grains and distorted fragments of microbands
were identified. The small grains were about 50-200 nm in size. The strong orientation changes,
more than 15°, either identify high angle grain boundaries (HAGB) lying at distances lower than
200 nm or they are an effect of strong grain bending (Fig. 1b). In order to precisely distinguish
between these two phenomena, small-step orientation maps were measured [13]. Strongly diffused
orientation distributions in the zones, which tended to group in the areas of deformation
components, rotated transverse (TD) to and/or normal (ND) to the sheet plane e.g. [11]. This
suggests that at least a part of the strong orientation changes can result from grain bending. In the
matrix, outside of the DZs, the HAGBs lie roughly parallel to the sheet plane at distances 0.5 - 1 µm
along the ND, as shown in previous work [12].
 Solid State Phenomena Vol. 163 15

Fig. 1. Microstructure of 6013 aluminum alloy cold rolled up to 90%, the deformation zone
surrounding large particle (a), longitudinal section, TEM. Orientation topographies and pole figures
in areas of the deformation zone before (b) and after (c) heating in-situ in TEM; particles of the
second phase - black, white regions – not indexed; thick lines – high angle grain boundaries, thin
lines – low angle grain boundaries. Areas with similar orientation (blue, red, yellow) were imaged
before and after annealing (d, e).

After annealing the sample in the microscope, the same areas were investigated using OIM.
Fig. 1c shows an example of a DZ orientation map after annealing. Nuclei or new grains are
observed in regions within the zone. For each orientation of new grains, it was easy to see similar
orientations in the deformed state that appeared in the same region of the DZ (Fig. 1 d, e). This
observation suggests that the orientation of nuclei approximately reproduce (with accuracy better
than 10°) the orientation of the deformed matrix fragments. At the onset of recrystallization, the
growth of the nuclei is associated with the migration of HAGBs in the vicinity of the large particles.
Misorientation distribution functions were calculated between the grains in the deformed state and
the new grains that appear in the same place (Fig. 2). Both for 75% and 90 % deformation, there
were no relationships describing favored growth. It seems at this very early stage of recrystallization
that all HAGBs in DZs are moved with the similar mobility. In the areas of matrix outside the
zones, migration of HAGBs was not observed.
16 Applied Crystallography XXI

Fig. 2. Misorientation distribution functions between the orientations of the crystallites in the
deformation zones (before annealing) and the new grains appearing in the same position after
annealing (a) 75% cold-rolled 6013 aluminum alloy, (b) 90% cold-rolled 6013 aluminum alloy;
Rodrigues’ representation r1, r2, r3, cross-section r3=const., asymmetric domain (O, O).

In order to confirm the in-situ results, combined microscopic-calorimetric investigations

were performed. Thin foils were prepared from the sample that was annealed in the calorimeter at a
temperature corresponding to the peak which was recognized as the peak of early recrystallization
stages [11]. Orientation maps were then measured in the DZ (Fig. 3). The new grains in the DZs are
observed, just as they were during the TEM in-situ studies.
 Solid State Phenomena Vol. 163 17

Fig. 3. Microstructure of 6013 aluminum alloy cold rolled up to 90% after heating to 275 oC,
longitudinal section, TEM. Bright field image (a) and orientation map in the vicinity of the
deformation zone (b) after annealing in the calorimeter (c).

Conclusions
In summary, the OIM technique in TEM is a very useful tool for quantitative and qualitative
characterizing of fine crystalline and deformed microstructures in polycrystalline materials. It is
possible to obtain information about grain distribution, misorientation between grains, material
phases, the local orientation distribution function, and the misorientation distribution function.
Transitioning between SEM measurements to TEM measurements improves the resolution
capability down to a few square nanometers. Both methods can be used for complementary analysis
of crystalline materials at the ”micro” and “nano” scale. Together with in-situ studies, orientation
mapping in TEM can provide additional information about material behavior during annealing,
particularly in the deformation zones.
It was shown on the example material (aluminum alloy 6013) that the first recrystallization stage
starts in the highly deformed zones in the vicinity of large particles; the particle stimulated
nucleation PSN e.g. [7, 8, 9]. It consists of nucleation and the growth of the nuclei. The growth is,
however, limited to the areas within the zones - at this stage of recrystallization, the migration of
HAGBs was observed in the DZ only [11]. The orientation of the nuclei (and new grains) roughly
reproduces the orientation of deformation.

Acknowledgements
Financial support from the State Committee for Scientific Research (N507 047 31/1152) is
gratefully acknowledged.
18 Applied Crystallography XXI

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Applied Crystallography XXI
doi:10.4028/www.scientific.net/SSP.163

Orientation Mapping Study on the Inhomogeneous Microstructure Evolution during

Annealing of 6013 Aluminum Alloy
doi:10.4028/www.scientific.net/SSP.163.13