InSituTEMPlasticDeformation Gartnerova

Microprocesses of plastic deformation
studied by In situ TEM in magnesium

prepared by equal channel angular pressing
at room temperature
V. Gärtnerová, J. Duchoň,
A. Jäger, P. Lejček
Institute of Physics of the Academy of Sciences
of the Czech Republic Prague, Czech Republic
Motivation
In situ straining in Transmission Electron Microscope was used to

investigate the microprocesses of plastic deformation, dislocation structure
and deformation modes in pure Mg after severe plastic deformation (SPD) at
room temperature. This can help to understand plasticity in SPD Mg.
Magnesium with hcp structure is classified as difficult-to-work

material due to a lack of active slip systems at ambient
temperatures.
Dominant deformation modes:

i) Basal slip with Burgers vector 1/3<1120> i.e. <a> slip.
ii) {10-12} twinning
This results in limited plasticity and to fulfill Von-Mises

criterion, <c+a> slip system is necessary to be activated.
Viera Gärtnerová, Institute of Physics ASCR, Prague, Czech Republic Plasticity 2013
Material used for experiments
Material Preparation procedure

• 99,9% pure Mg Bc route – 90° rotation around the
longitudinal axis applied after each pass
• ECAP with applied BP (back pressure), inner
channel angle of 90°, no outer curvature
ECAP die
• 4 passes by Bc route at Room Temperature
and 0.4mm/s
• BP was regulated to be ~200, ~300, ~400 and

~400MPa for 1st, 2nd, 3rd and 4th pass
respectively, to maintain an average plunger
load of ~1GPa
By applying BP an improvement in plasticity was achieved by

deformation under „high hydrostatic pressure“.
Initial microstructure analyses
Inverse Pole Figure map
Ellipse shows the region
on the measured (ID-ED)
plane from which the
presented analyses were
taken.
IPF map of pure Mg

after four passes by
ECAP-BP at RT
following processing
rout Bc
• Crack-free microstructure with average grain size determined by EBSD

on high angle grain boundaries (>15°) was 5mm.
• Microstructure was predominantly free of shear bands and fully free of
twins with reasonably equiaxed grains separated by high-angle grain
boundaries, such microstructure manifests dynamic recrystallisation
during ECAP-BP.
• The extend of recrystallisation seen was unexpected.
Initial microstructure analyses
X-ray measurement PAS measurements
2.0
The (0002) (left) and {10-10} Positron annnihilation Mean
(right) direct pole figures spectroscopy (PAS) shows 1.8 dislocation
show slight texture after that concentration of defects density
in material after 4th pass is
D (10 m )
4xBc route ECAP-BP with
-2
1.6
tendency to align the basal lower than for two preceding
14
planes parallel with the passes.
1.4
theoretical shear plane of
Concentration of defects
the ECAP die.
was calculated from the 1.2
intensities of the exponential
positron decay components. 1.0
0 1 2 3 4 5
number of passes
X-ray measurement TEM observation

The narrow profiles of TEM observation prior to
diffraction peaks, which are In situ TEM tensile
close to instrumental experiments confirmed:
broadening, combined with
Slight texture, twin free
the well-distinguished Ka1
structure and equiaxed
and Ka2 lines confirm a low
grains with a very rear
value of accumulated strain.
occurrence of shear bands
measured by EBSD and X-
ray analyses.
Relatively low dislocation
density measured by PAS
and X-ray analyses.
In situ straining
Transmission Electron Microscopy
• In situ tensile experiments in TEM were Home-made double tilt

performed on home-made double tilt straining straining holder
holder at Room Temperature (RT). X-tilt:±45°
Y-tilt:±12°
• Samples for in situ straining in TEM were Max. load: 20N

prepared from (ID-ED) plane with tensile axis
parallel to ED (see Fig.)
F 1st grain
F
Samples for in situ experiments Sample for In situ TEM experiments
were taken from (ID-ED) plane. 5.6x1.7x0.09mm³ 2nd grain
1st grain
F
In situ TEM 1 st grain

F
Table of b.g values calculation for perfect

Imaging condition for the 1st grain dislocations in hcp structure
zone Axis 2-1-10
during In situ tensile test Mode b.g 0002 01-10 0-11-1 01-1-1 01-11
<a> 1/3[11-20] 0 1 1 1 1
1/3[1-210] 0 1 1 1 1
1/3[-2110] 0 0 0 0 0
<c+a> 1/3[11-23] 2 1 2 0 2
1/3[1-213] 2 1 0 2 0
crack 1/3[-2113] 2 0 1 1 1
1/3[11-2-3] 2 1 0 2 0
1/3[1-21-3] 2 1 2 0 2
1/3[-211-3] 2 0 1 1 1
<c> [0001] 1 0 1 1 1
b Burgers vector
g operative reflection
B zone axis
From the table of b.g calculation,

it is seen that all types of
Zone axis dislocations, <a>, <c+a> and <c>
B=[2110] types, are potentially visible in
Bragg condition g=(01-11) diffraction condition.
Bright field images g=(0111)
1st grain
F

F
Tensile test 500 nm
Dislocations with line

directions parallel to the
trace of the (0002) basal Zone axis
planes and (0-11-1) first B=[2110]
order pyramidal planes Bragg condition
are visible. g=(0111)
Calculation of b.g values for perfect
dislocations in hcp structure
zone Axis 2-1-10
Mode b.g 0002 01-10 0-11-1 01-1-1 01-11

<a>
<c+a>
1/3[11-20]
1/3[1-210]
1/3[-2110]
1/3[11-23]
0
0
0
2
1
1
0
1
1
1
0
2
1
1
0
0
1
1
0
2
1/3[1-213] 2 1 0 2 0
1/3[-2113] 2 0 1 1 1
Zone axis 1/3[11-2-3] 2 1 0 2 0
1/3[1-21-3] 2 1 2 0 2
B=[2110]
1/3[-211-3] 2 0 1 1 1
Bright field images a=0 c=0
<c> [0001] 1 0 1 1 1
Weak beam images (shows fine images formed only by dislocation cores)
BF image taken with B=[2-1-10] with From the calculation of b.g values for BF images taken with B=[2-1-10] with
g=0002 shows straight dislocations with perfect dislocations in hcp structure, g=(01-1-1) and g=(0-11-1) show all
line directions parallel to the trace of the under two beam condition g=01-10, types of dislocations <a>, <c+a> and
basal planes. All dislocation are of <c> or 2/3 of <a> dislocations and 4/6 <c+a> <c> type. Straight lines dislocation are
<c+a> type while <a> type dislocations dislocations are visible and <c> type parallel to the (0002) plane traces.
should be invisible. dislocation should be invisible.
Calculation of b.g values for perfect
zone Axis 2-1-10
Mode b.g 0002 01-10 0-11-1 01-1-1 01-11

<a>
<c+a>
1/3[11-20]
1/3[1-210]
1/3[-2110]
1/3[11-23]
0
0
0
2
1
1
0
1
1
1
0
2
1
1
0
0
1
1
0
2
1/3[1-213] 2 1 0 2 0
1/3[-2113] 2 0 1 1 1
Zone axis 1/3[11-2-3] 2 1 0 2 0
1/3[1-21-3] 2 1 2 0 2
B=[2110]
1/3[-211-3] 2 0 1 1 1
Bright field images a=0 c=0
<c> [0001] 1 0 1 1 1
Weak beam images (shows fine images formed only by dislocation cores)
<a> <a>
<a> <c+a>
<c>
<a> <a>
BF image taken with B=[2-1-10] with From the calculation of b.g values for BF images taken with B=[2-1-10] with Burgers vector for <c+a> dislocation:
g=0002 shows straight dislocations with perfect dislocations in hcp structure, g=(01-1-1) and g=(0-11-1) show all 1/3[11-23]
line directions parallel to the trace of the under two beam condition g=01-10, types of dislocations <a>, <c+a> and 1/3[1-21-3]
basal planes. All dislocation are of <c> or 2/3 of <a> dislocations and 4/6 <c+a> <c> type. Straight lines dislocation are
Burgers vector for <a> dislocation:
<c+a> type while <a> type dislocations dislocations are visible and <c> type parallel to the (0002) plane traces.
1/3[11-20]
should be invisible. dislocation should be invisible.
1/3[1-210]
F
In situ TEM 2 nd grain F
2nd grain
Bright field images

Imaging condition for the 2nd grain
0112 during In situ tensile test
Table of b.g values calculation for perfect
Zone axis 01-11
Mode b.g 01-1-2 1-101 -1011
<a> 1/3[11-20] 1 0 1
1/3[1-210] 1 1 0
1/3[-2110] 0 1 1
<c+a> 1/3[11-23] 1 1 0
1/3[1-213] 3 2 1
1/3[-2113] 2 0 2
1/3[11-2-3] 3 1 2
1/3[1-21-3] 1 0 1
1/3[-211-3] 2 2 0
<c> [0001] 1 1 1
b Burgers vector
g operative reflection
B zone axis
crack
From the table of b.g calculation,
it is seen that all types of
Zone axis dislocations, <a>, <c+a> and <c>
B=[0111] types, are potentially visible in
Bragg condition g=(0-112) diffraction condition.
g=(0112)
F
In situ TEM 2 nd grain F
2nd grain
Tensile test
0112
Dislocations with line

directions parallel to the
trace of the (2-1-10)
prismatic planes and
(1-101) first order
pyramidal planes are
visible.
Zone axis
B=[0111]
(2-1-10) Bragg condition
g=(0112)
Zone axis 01-11
Mode b.g 01-1-2 1-101 -1011
<a> 1/3[11-20] 1 0 1
1/3[1-210] 1 1 0
In situ TEM 2 nd grain

1/3[-2110]
<c+a> 1/3[11-23]
1/3[1-213]
1/3[-2113]
0
1
3
2
1
1
2
0
1
0
1
2
1/3[11-2-3] 3 1 2
Zone axis 1/3[1-21-3] 1 0 1
B=[0111] 1/3[-211-3] 2 2 0
<c> [0001] 1 1 1
Bright field images
Dark field images
Zone axis 01-11
Mode b.g 01-1-2 1-101 -1011
<a> 1/3[11-20] 1 0 1
1/3[1-210] 1 1 0
In situ TEM 2 nd grain

1/3[-2110]
<c+a> 1/3[11-23]
1/3[1-213]
1/3[-2113]
0
1
3
2
1
1
2
0
1
0
1
2
1/3[11-2-3] 3 1 2
Zone axis
Plastic deformation at the crack-tip 1/3[1-21-3] 1 0 1
B=[0111] 1/3[-211-3] 2 2 0
has complex character <c> [0001] 1 1 1
Bright field images
Dark field images
Conclusions
In situ straining in TEM was performed on 99.9% Mg samples subjected to
4xBc ECAP BP at room temperature. The samples had homogenous and
twin-free microstructure with an average grain size of 5 mm.
During straining, the sample was observed close to crack propagation.
It was found:
• Plastic deformation at RT has complex character with an activity of different
slip systems (it differs from grain to grain).
• We observed <c+a> dislocations that are not easily activated due to high
CRSS (much higher than for preferred basal slip and {10-12} twinning).
• No twinning was observed during in situ straining (can be influenced by thin
TEM sample).
• New dislocations often originate at grain boundaries (and from abundant
loops in grain interior which nature remains to explain).

InSituTEMPlasticDeformation Gartnerova

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Microprocesses of plastic deformation

studied by In situ TEM in magnesium

In situ straining in Transmission Electron Microscope was used to

Magnesium with hcp structure is classified as difficult-to-work

Dominant deformation modes:

This results in limited plasticity and to fulfill Von-Mises

Material Preparation procedure

• BP was regulated to be ~200, ~300, ~400 and

By applying BP an improvement in plasticity was achieved by

IPF map of pure Mg

• Crack-free microstructure with average grain size determined by EBSD

X-ray measurement TEM observation

• In situ tensile experiments in TEM were Home-made double tilt

• Samples for in situ straining in TEM were Max. load: 20N

In situ TEM 1 st grain

Table of b.g values calculation for perfect

From the table of b.g calculation,

In situ TEM 1 st grain

Tensile test 500 nm

Dislocations with line

In situ TEM 1 st grain

In situ TEM 1 st grain

In situ TEM 2 nd grain F

Bright field images

In situ TEM 2 nd grain F

Dislocations with line

In situ TEM 2 nd grain

Dark field images

In situ TEM 2 nd grain

Dark field images

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