Materials Characterization 175 (2021) 111065

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Materials Characterization
journal homepage: www.elsevier.com/locate/matchar

The measurement of the dislocation density using TEM

Yang Meng a, *, Xinhua Ju a, b, Xiaopeng Yang c
a
Shougang Group Company Limited Research, Institute of Technology, Beijing 100043, China
b
Beijing Engineering Research Center of Energy Steel, Beijing 100043, China
c
Oxford Instruments Technology (Shanghai) Co. Ltd, Beijing 100085, China

A R T I C L E I N F O A B S T R A C T

Keywords: The line intercept method is well developed for estimating the dislocation density in metals, but its application is
Dislocation density limited by the intersection counting, which is deeply depending on the TEM image quality. Manual interscetion
Invisibility criterion counting is quite time and labor consuming. If most of the dislocations has good contrast and homogenous
Two-beam condition
background in an image, it is possible to perform automatic counting by the computer program. In this work a
Zone axis STEM image
series of imaging conditions were investigated on a slightly deformed IF steel thin foil. Though the invisibility
criterion remains applicable for both the conventional transmission electron microscopy (CTEM) and the scan­
ning transmission electron microscopy (STEM), the STEM images revealed more dislocations and had more
homogenous background than the CTEM images. The STEM bright field (BF), annular dark field (ADF) and
annular bright field (ABF) images at a low index zone axis contained the most dislocations visible and were
suitable for automatic intersection counting of dislocations.

1. Introduction
The line intercept method is widely applied in the estimation of the
dislocation density [1–4]. By measuring the foil thickness and the
intersection count between a given grid and the dislocations on a TEM
image, the dislocation density ρ in the current grain can be achieved by
Eq. (1).
2n
ρ=
lt
where n is the intersection count, l is the total length of the grid, and t is
the thickness of the foil on this TEM image. This method is effective
when the dislocation density in the metal is less than 1014 cm− 2. The
thickness t can be accurately measured by the trace analysis [5], and
Kossel-Möllenstedt patterns in convergent beam electron diffraction
(CBED) method [6]. The difficulty is the measurement of the intersec­
tion counting.
In the conventional transmission electron microscopy (CTEM) mode,
the electron beam is parallelly illuminating on the sample, and good
contrast of the defects can be achieved at two-beam conditions. Since the
extinction of the dislocation is inevitable, a series of images at the same
position with different two-beam conditions must be acquired in order
to get more dislocations visible. The superposition of the images at all
the two-beam conditions is likely to reveal all the dislocations. However,
the number of two-beam conditions is limited by the sample tilting an­
gels and image distortion. Moreover, the uniformity of the image
background is ruined by the bend contours and the second phase
contrast in CTEM. Therefore, the intersection counting on the CTEM
images can only be conducted manually. It is quite time and labor
consuming, and its accuracy is closely dependent on the imaging
condition.
(1) In the scanning transmission electron microscopy (STEM) mode, due
to the convergent illumination of the electron beam on the sample, a
STEM image is equivalent to an averaged image of a series of CTEM
images acquired with the sample tilted in a range of directions. The
dislocation contrast is enhanced and the elastic strain contrast in the
background is reduced by the averaging the intensities from all the di­
rections. As a result, the dislocations are much easier to distinguish in
STEM images [7–10] than in CTEM images. Therefore, it is possible to
perform the automatic counting of the intersection on the STEM images,
which will greatly enhance the much wider application of measuring the
dislocation density through TEM. Besides, the convergent beam has
higher brightness and can be applied on thicker foil, which is benefit to
the thickness measurement by CBED method [6].
However, in literatures very little work has been found on STEM
application in measuring the dislocation density. In present work, a

* Corresponding author.
E-mail address: mengyang@shougang.com.cn (Y. Meng).

https://doi.org/10.1016/j.matchar.2021.111065
Received 10 November 2020; Received in revised form 24 March 2021; Accepted 25 March 2021
Available online 26 March 2021
1044-5803/© 2021 Elsevier Inc. All rights reserved.
Y. Meng et al. Materials Characterization 175 (2021) 111065

Fig. 1. The full image of the grain: (a) CTEM BF image and (b) STEM BF image with camera length of 40 cm.

sample of a slightly deformed interstitial free (IF) steel was imaged by a

series of imaging conditions of CTEM and STEM modes. A detailed
comparison was made to select the optimized conditions for further
automatic intersection counting by using self-designed program. Finally,
the dislocation density in the observed field was determined.

2. Experiment

The continuous-annealed IF steel with 3.3% tensile deformation was

observed in JEOL 2100 FEG-TEM in this study. The TEM samples were
taken parallel to the steel sheet surface, and then prepared by me­
chanical grinding and electropolishing. Since the steel sheet had a strong
γ texture, the normal directions of the grains observed were close to
〈111〉 zone axis.
A specified grain with diameter about 12 μm was chosen for the
estimation of dislocation density. The full image of the grain was
montaged from CTEM and STEM bright field (BF) images respectively,
as shown in Fig. 1. The full image from STEM had more uniform back­
ground contrast than from CTEM. The left part of the grain was thicker
than the right in general. The region of interest in white box on the
upper-left corner was subsequently further examined in detail.
3. Results and discussion
In CTEM mode good contrast of dislocationcould be obtained when
the sample was near to a two-beam condition where the deviation
parameter of the reflector was small and positive. When it was at a zone
axis, the contrast of dislocations was weak. Therefore, only two-beam
sample condition was used in CTEM mode. While in STEM mode the
contrast of dislocation could be strong due to the averaging of the in­
tensities over the range of incident illumination angles. Phillips et al. [9]
indicated that the contribution of reflectors from multiple directions,
made the contrast of defects in crystal clearer under appropriate con­
ditions, including the zone axis index, the convergent angle, the
collection angle, etc. So, both zone axes and two-beamconditions were
used in STEM mode. In this work, the images were acquired with a series
of imaging conditions, and the number of dislocations and image quality
were systematically compared to select the suitable ones for automatic
intersection counting.
3.1. CTEM and STEM dislocation BF images under two-beam conditions
Since the continuously annealed IF steel had strong γ texture, the
Fig. 2. SAD pattern at zone [111]bcc.
observed grain in Fig. 1 reached low index zone [111]bcc after a small
tilting about 6.5◦ , and the selected area diffraction (SAD) pattern was
shown in Fig. 2. The sample was then tilted from zone [111]bcc to reach a
series of two-beam conditions, in which the reflectors, g1 = (011), g2 =
(101) and g3 = (110), reached Bragg condition, respectively. The cor­
responding diffraction patterns and the central BF images of CTEM were
shown in Fig. 3(a–b), 3(c–d) and 3(e–f) respectively. At each two-beam
condition, there were some dislocations invisible. By overlapping the
three BF images, Fig. 4 was obtained, which contained all the visible
dislocations in CTEM BF images nearby zone [111]bcc. Compared with
Fig. 4, the invisible dislocations in each CTEM BF image were marked by
white arrows with black border as shown in Fig. 5(a), (c), and (e).
The STEM image could be enhanced by the multiple reflectors and
the dislocation contrastwas formed by the interference of the strong
reflections from the high strain region around the dislocation core. So,
the key point of good dislocation contrast was which part of reflectors
would be collected for imaging, and it deeply depended on the imaging
conditions, including the convergent angle and collection angle. In this
work, the 3rd convergent lens (CL) aperture was selected, and the half
convergent angle was fixed to be 12.5 mrad. The annular detector had
inner diameter of 3 mm and outer diameter of 8 mm. The collection
angles of the annular detector for dark field (DF) images varied with the
camera length, and their lower limits were measured in experiment

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Y. Meng et al. Materials Characterization 175 (2021) 111065

Fig. 3. CTEM observation at two-beam conditions: SAD pattern (a) and BF image (b) with the strongest reflector g1 = (011); SAD pattern (c) and bBF image (d) with
the strongest reflector is g2 = (110); SAD pattern (e) and BFB image (f) with the strongest reflector g3 = (101).

(exp.) and the upper limits were calculated (cal.) from the inner and
outer diameters, and all of them were listed in Table 1. The collection
angle of the bright field detector was just a little smaller than the lower
limits of collection angle of the annular detector.
The STEM BF images were also acquired at the same two-beam
conditions with the cameral length of 40 cm and the range of the
collection angle of the BF detector was less than 17.5 mrad according to
Table 1. For the ferrite, 2θ110 = 12.4 mrad, so the transmission disk and
strong reflector {110} disk were collected. There are more dislocations
in each STEM BF image than in each CTEM BF image at the same two-
beam condition, but no more than in Fig. 4. By comparison with the
CTEM BF image at the same two-beam condition, the dislocations were
marked by white arrows with black border if they were still invisible and
marked by white arrow without border if they were visible, as shown in
Fig. 5(b), (d) and (f). No more extinction was found in any STEM BF
image.
The dislocation contrast was determined by the invisibility criterion
g⋅b = 0 in the CTEM mode with parallel beam condition. No more
extinction in STEM BF image than in CTEM BF image indicated that the
invisibility criterion in the CTEM mode remained applicable in the STEM

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Y. Meng et al. Materials Characterization 175 (2021) 111065

transmission disk and all the {110} diffraction disks when the camera
length was 40 cm, as the white circle indicated on the CBED pattern at
[111]bcc zone axis in Fig. 6(a), and the STEM BF image was shown in
Fig. 6(b). The STEM annular dark field (ADF) image in Fig. 6(c) was
acquired with the camera length of 20 cm, where the range of the
collection angle was 35–93.3 mrad, and the diffraction disks with index
higher than {123} can be collected (2θ123 = 32.8 mrad). The ADF image
had an inverted contrast to the STEM BF image (Fig. 6(b)). The STEM
annular brigth field (ABF) image in Fig. 6(d) was acquired with the
camera length of 150 cm, where the range of the collection angle was
4.7–12.4 mrad and the outer part of the transmission disk and half of
{110} diffraction disks were collected. The STEM ABF image had a
consistent contrast with the STEM BF image (Fig. 6(b)).
According to the diffraction mechanism, at a two-beam conditon,
Fig. 4. The superposition of the three two-beam conditions: g1 = (011), g2 =
(110) and g3 = (101). Table 1
Collection angle of the annular detector.
mode. Due to the convergent beam condition in STEM mode, the Camera length (cm) Range of the collection angle (mrad)
contrast of the extinction dislocations was enhanced, therefore, only a
8 87.5(exp.) ~ 233.3(cal.)
part of the extinctions still kept invisible, and the others had a fuzzy but 10 70.0(exp.) ~ 186.7(cal.)
recognizable contrast. 12 58.3(exp.) ~ 155.6(cal.)
20 35.0(exp.) ~ 93.3(cal.)
40 17.5(exp.) ~ 46.7(cal.)
3.2. STEM dislocation images at [111]bcc zone axis 80 8.8(exp.) ~ 23.3(cal.)
120 5.8(exp.) ~ 15.6(cal.)
150 4.7(exp.) ~ 12.4(cal.)
In order to get good dislocation contrast at [111]bcc zone axis, the
strong reflectors should be selected. The BF detector can cover the

Fig. 5. Comparison of the dislocation images at two-beam conditions: CTEM (a) STEM (b) BF images with the strongest reflector of g1 = (011); CTEM (c) STEM (d) BF
images with the strongest reflector of g2 = (110); CTEM (e) STEM (f) BF images with the strongest reflector of g3 = (101). By the comparison with Fig. 4 the white
arrows with black border indicated the invisible extinctions and the white arrows without border indicated the extinctions with weak contras in STEM images.

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Y. Meng et al.
there was only one strong reflection, and the dislocations satisfied the
invisibility criteria g⋅b = 0 and were invisible without auxiliary contrast.
Whereas at a zone axis there were multiple reflectors, and the invisibility
criterion could not be simultaneously satisfied, only if the Burgers vector
of the dislocation was parallel to the zone axis, i.e. [111]bcc for the
present grain. For most dislocations, whose Burger vectors were not
parallel to the zone axis, the auxiliary were not zero and they should be
visible. In the STEM mode, the image at the zone axis, no matter the BF
or DF, was the average contrast of all the reflectors, and was equal to
overlap the images at all the two-beam conditions around the zone. So
the comparison between the STEM BF image at zone [111]bcc (Fig. 6(b))
and Fig. 4 proved that all of the visible dislocations in CTEM BF images
under 3 two-beam conditions could be found in the single STEM BF
Fig. 6. The CBED pattern and STEM images at zone [111]bcc, (a) the CBED pattern, the white circle indicates the edge of the bright field detector, (b) the BF image,
(c) the ADF image and (d) the ABF image.
Fig. 7. Comparison of dislocations in the same area within the white frame, (a)the overlapped CTEM image of 3 two-beam conditions around [111]bcc zone axis and
(b) the STEM bright field image at [111]bcc zone axis.
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Materials Characterization 175 (2021) 111065
image as shown in Fig. 7.
3.3. STEM dislocation images at high index zone axes
High index zone axes, [331]bcc, [231]bcc, and a zone between
[355]bcc and [122]bcc, were achieved by tilting 17.5◦ , 12.2◦ and 16.2◦
from [111]bcc, respectively. The corresponding diffraction patterns were
shown in Fig. 8(a), (c) and (e), and the dislocation images from the same
area were shown in Fig. 8(b), (d) and (f). Since the magnetic sample was
tilted by large angles, the TEM alignment was seriously disturbed, which
made it hard to eliminate the strong astigmatism of the object lens and
the quality of STEM BF and ABF images were poor. But it was still
possible to distinguish some dislocations. All the STEM images at high
Y. Meng et al.
Fig. 8. STEM images at high index zone axes: SAD pattern (a) and ABF image
(b) at [331]bcc; SAD pattern (c) and BF image (d) at [231]bcc; (e) SAD pattern
and ABF image (f) between [355]bcc and [122]bcc; STEM BF image (g) at
[111]bcc. The arrows with letter a indicated the dislocations invisible in Fig. 8
(b), the arrows with letter b indicated the dislocations invisible in Fig. 8(d), and
the arrows with letter c indicated the dislocations invisible in Fig. 8(f).
index axes were compared to the STEM BF image at [111]bcc zone axis in
Fig. 8(g), and all the invisible dislocations were marked by arrows, and
no more dislocation was found. Therefore, the number of visible dislo­
cations at [111]bcc zone was larger than that at high index zone axes.
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Materials Characterization 175 (2021) 111065
3.4. CTEM and STEM dislocation DF images under two-beam condition
The CTEM central DF image (Fig. 9(a)) and weak beam dark field
(WBDF) image (Fig. 9(b)) were obtained at the 1st two-beam condition
with the reflector of g1 = (011). As marked in Fig. 5(a) there were 7
extinction dislocations in the CTEM BF image. All of them were invisible
in the central DF image and 5 out of them were still invisible and the
other 2 were recognizable in the WBDF image, and no more extinction
was found. The invisible ones were marked by the white arrow with
black border and the recognizable ones were marked by white arrows
without border in Fig. 9(a) and (b). The dislocation contrast in the CTEM
DF images was weaker than that in the BF image and uniformity of the
background was worse.
In the STEM mode, the ADF images and the central DF images were
acquired at the 1st two-beam condition with the reflector of g1 = (011).
The ADF images (Fig. 10(a) and 10(b)) were acquired by the annular
detector with camera length of 40 cm and 20 cm, respectively. The
corresponding collection angle were 17.5–46.7mrad and 35–93.3 mrad
according to Table 1. The central DF images were acquired by the BF
detector with shifting the strong diffraction disk g(011) (Fig. 10(c)) and
the weak diffraction disk g(011) (Fig. 10(d)) to the center, respectively.
Fig. 10(c) had nearly consistent contrast with the STEM BF image in
Fig. 5(b): the contrast of the dislocations was darker than the back­
ground. It was because the transmission disk was inevitably overlapped
with the disk g(011) and the BF detector collected the whole disk g(011)
and part of the transmission disk. The 7 extinction dislocations in Fig. 5
(a) were examined in every image: only the 6th dislocation was recog­
nizable in Fig. 10(a), and 4 out of them were recognizable in Fig. 10(b);
and all of them were invisible in Fig. 10(c), and only the 5th dislocation
was invisible in Fig. 10(d). No more extinction was found. The contrast
of the 7 dislocations in all the images at the 1st two-beam condition was
listed in detail in Table 2.
All the images at the 1st two-beam condition, including Fig. 5(a) and
(b), Fig. 9 and Fig. 10, were compared with the images at the low index
zone axis in Fig. 6. Though the contrast of dislocations varied with the
imaging condition, no more dislocations were found and the images at
low index zone axis showed the most dislocations.
3.5. Measurement of the dislocation density
According to the above comparison, both the STEM ADF and ABF
images had uniform background and could be used to count in­
tersections by digital image processing technology. And the images at
low index zone axis [111]bcc had the most recognizable were suitable for
the measurement of dislocation density. A program had been developed
to automatically count the intersection. In the program, the digital im­
ages of ADF and ABF (Fig. 6(c) and (d)) were processed to be black-white
(BW) images and masked by a 20 × 20 grid as shown in Fig. 11. The
intersections between the grid and the dislocations were then counted
automatically. The total counts in each image were 442 and 449,
respectively. The average counts were 445. In order to verify the validity
of the automatic counting by program, the manual countingon the ABF
image was also conducted and the result was 454, which is in good
consistency with the automatic counting result. The nl value was 3.89/
μm. The foil thickness was determined to be 201 μm according to the
CBED pattern at a two-beam condition [6] in current grain in Fig. 12.
The dislocation density in this grain was estimated to be 3.9 × 1012
cm− 2.
Y. Meng et al. Materials Characterization 175 (2021) 111065

Fig. 9. The CTEM DF images at the g1 = (011)two-beam condition, (a)the central DF image and (b) the WBDF image.

Fig. 10. The DF images at the two-beam condition with the reflector of g1 = (011): (a) the ADF image with the collection angle 17.5– 46.7 mrad; (b) the ADF image
with the collection angle 35– 93.3 mrad; (c) the central DF image with strong disk g(011) in the center; (d) the central DF image with weak disk g(011)in the center.

Table 2
The contrast of the 7 extinct dislocations at the two-beam conditions with reflector of g1 = (011).
CTEM STEM

BF DF WBDF BF ADF (17.5–46.7mrad) ADF (35–93.3 mrad) DF,strong g(011) DF, weak g(011)

1 × × × × × o × o
2 × × × o × o × o
3 × × o o × o × o
4 × × × o × o × o
5 × × × × × × × ×
6 × × o o o o × o
7 × × × × × × × o

×: Invisible.
o: Recognizable.

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Y. Meng et al. Materials Characterization 175 (2021) 111065

Fig. 11. The automatic intersection counting on the STEM images: (a) the BW image of Fig. 6(c); (b) the contrast enhanced image with a 20 × 20 grid on Fig. 6(c); (c)
the BW image of Fig. 6(d); (d) the contrast enhanced image with a 20 × 20 grid on Fig. 6(d).

Declaration of Competing Interest

None.

Acknowledgements

The authors thank Professor Delu Liu of University of Science &

Technology Beijing for discussion and advices on the TEM imaging
methods.

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Fig. 12. CBED pattern at a two-beam condition for thickness determination.
4. Conclusions
The different sample conditions and imaging methods for the dislo­
cation density estimation were investigated in present work on a slightly
deformed IF steel thin foil. A software was developed to automatically
count the intersection in the TEM dislocation images. The following can
be concluded.
1. The STEM images revealed more dislocations than the CTEM images
and they contained most dislocations visible at a low index zone axis.
The background of the STEM images was more homogenous than
that of the CTEM images.
2. The STEM BF, ADF and ABF images at a low index zone axis were
suitable for automatic intersection counting of dislocations.
3. The self-designed program could perform the automatic intersection
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