Theoretical and Applied Fracture Mechanics 95 (2018) 28–41

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Theoretical and Applied Fracture Mechanics

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Plane stress fracture toughness of cryorolled 6082 Al alloy T

a,⁎ a b a,c
N. Kumar , G.M. Owolabi , R. Jayaganthan , O.O. Ajide
a
Department of Mechanical Engineering, Howard University, Washington, D.C. 20059, USA
b
Department of Engineering Design, Indian Institute of Technology Madras, Chennai 600036, India
c
Department of Mechanical Engineering, University of Ibadan, Ibadan, Nigeria

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

Keywords: In this paper, the plane stress fracture toughness of 6082 Al alloy produced by cryorolling is reported for the
Cryorolling first time. The rolling was performed to achieve a 75% reduction in the sample thickness at two different
Room temperature rolling temperatures, namely, liquid nitrogen temperature (−196 °C), and room temperature (25 °C). The plane stress
Ultrafine grains fracture toughness was evaluated for cryorolled (CR), room temperature rolled (RTR), cryorolled and annealed
Critical plane stress fracture toughness
(CR + AN), and room temperature and annealed (RTR + AN) samples using ASTM E1820-13 standard and
compact tension specimens. Two methods, i.e., the Load point displacement (LPD)-load and the J-Integral-
resistance (J-R) curves, were used to calculate the plane stress fracture toughness. The results showed that the
fracture toughness calculated using the J-R curve is more accurate since it accounts for all the constraints for
evaluating the critical plane stress fracture toughness of the alloy for all the processing routes. The values of
the critical plane stress fracture toughness (JIC) obtained via the J-R curve were 49 kJ/m2 for CR, 31 kJ/m2 for
RTR, 69 kJ/m2 for CR + AN and 39 kJ/m2 for RTR + AN samples. Microstructural features obtained through
scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD) were also correlated with
the fracture toughness. It is found from the SEM results that Mg-Si phases evolved at the crack tip/path during
crack propagation in all the investigated samples. The EBSD results showed that CR + AN sample exhibits high
kernel average missorentation and crack branches due to the evolution of small sized Mg-Si (Si-rich) pre-
cipitates during the fatigue testing. The presence of mixed grains (coarse and fine), fractographic features such
as shallow ridges, transgranular facets, flat circular and elongated dimples, small sized Si-rich precipitates and
high kernel average missorentation support the high plane stress fracture toughness observed for the CR + AN
sample.

1. Introduction
Ultrafine grained (UFG) materials are potential candidate for a wide
range of structural and functional applications due to their outstanding
mechanical and physical properties in terms of monotonic strength,
high cycle fatigue (HCF) strength and improved corrosion strength
[1,2]. In recent years, UFG and nanostructure materials with superior
strength, ductility, toughness, and corrosion resistance when compared
to their bulk alloys have been developed using several severe plastic
deformation routes (SPD) [3]. It has been reported that the combination
of UFG and coarser materials could improve the wear resistance, fatigue
crack initiation resistance and corrosion resistance of materials [4,5].
Different SPD techniques such as equal channel angular pressing
(ECAP) [6,7], equal channel angular rolling (ECAR) [8], high pressure
torsion (HPT) [9,10], extrusion compression (CEC) [11], constrained
groove pressing (CGP) [12], multi-axial forging (MAF) [13], cyclic and
accumulative roll bonding (ARB) [14], and cryorolling (CR) have been
used for the production of UFG and nanostructures in various metallic
materials [15,16]. The dimension of the sample remains the same as
that of the initial sample even after processing in most of the SPD
techniques [17], except CR [15]. Among the several SPD techniques, CR
has a unique advantage since it requires low true strain for the pro-
duction of the UFG material, easy operation, high production rate, and
convenient set up [15,16,18]. Cryorolling has been used in various
metals for the production of bulk UFG metals such as CuZr alloy [19],
Fe-25Cr-20Ni steel [20], 6082 Al alloy [21], 2014 Al alloy [22],
AA2219-T87 Al alloy [23], Cu-Cr-Zr-alloy [24], 6016 Al alloy [25],
6061 Al alloy [26], Zircaloy-2 [27], Ni-alloys [28], and Fe-36% Ni alloy
[29]. Xiong et al., reported that the yield strength and the ultimate
tensile strength of Fe-25Cr-20Ni steel processed by CR were 2.3 and 1.5
times of the original un-deformed sample, and the toughness increased
by 27% [20]. The yield strength of 6082 Al alloy after CR has increased
to 353 MPa (17.7% increase), 424 MPa (41.3%) and 488 MPa (62.7%)
for 40%, 70% and 90% thickness reductions, respectively [20]. Joshi

⁎
Corresponding author.
E-mail address: Nikhil.kumar@howard.edu (N. Kumar).

https://doi.org/10.1016/j.tafmec.2018.02.011
Received 2 November 2017; Received in revised form 13 February 2018; Accepted 13 February 2018
Available online 15 February 2018
0167-8442/ © 2018 Published by Elsevier Ltd.
N. Kumar et al.
et al., reported that cryorolled sample shows improved HCF strength
when compared to solution treated alloy due to the formation of ul-
trafined grains [22]. Babu et al., reported that after CR, the yield
strength, the hardness, and the impact strength of the alloy have im-
proved up to 14% in AA2219-T87 Al alloy [23]. Zhang et al., reported
that the ultimate tensile strength of the cryorolled and aged Cu-Cr-Zr
alloy was 690.13 MPa, which shows an increase of 23.4% and 44.3%
when compared with the CR and RTR samples [24]. Shoar et al., re-
ported that the yield strength of the alloy after solution treatment has
increased from 61 MPa to 268 MPa and the ultimate tensile strength
from 133.7 MPa to 297 MPa after CR of 6061 Al alloy [26]. Trivedi
et al., reported that the tensile strength of zircaloy-2 has increased from
as received (592 MPa) to CR + AN (400 °C) (842 MPa) and CR + AN
(450 °C) (726 MPa), respectively [27]. The cryorolled Fe-36% Ni alloy
has also shown high ultimate tensile strength of 1110 MPa, whereas
RTR sample showed low UTS value of 810 MPa [29].
Unfortunately, UFG materials processed by CR has not been widely
used in engineering structures since their fracture strength is not well
studied. Only very limited literature is available on relating the fracture
toughness of metals with their UFG structure. Moreover, the available
literature on the fracture strength of UFG materials contradicts one
another. For example, UFG tungsten alloy exhibits higher fracture
toughness (29 MPa·m1/2) when compared to the initial condition
(9 MPa·m1/2) [30]. The fracture toughness of UFG pure copper pro-
duced by CGP and Al 7075 alloy processed by ECAP have also shown
higher fracture toughness when compared with the initial conditions
[31,32]. However, Sabirov et al., reported that UFG nickel processed by
HPT and commercially pure titanium alloy processed by ECAP show
lower fracture toughness when compared with the initial conditions
[33]. Hohenwarter et al., reported that UFG iron shows lower fracture
toughness when compared to the bulk sample [34]. Ultrafined grained
Ti processed by ECAP and UFG Ni processed by HPT also have lower
fracture toughness when compared with the initial samples [33,35].
To the best of our knowledge, only the plane strain fracture
toughness (KI) of UFG metals have been published to some extent in
open literature. Studies conducted to relate the plane stress fracture
toughness (JI) of UFG metals processed by CR to their microstructure
are very rare. In the present work, the plane stress fracture toughness of
6082 Al alloy produced by cryorolling is reported for the first time. The
rolling was performed at two different temperatures: (i) liquid nitrogen
temperature (≈−196 °C), and (ii) room temperature (≈25 °C), to in-
vestigate the influence of deformation temperature on the secondary
phase particles and grain refinement and correlate it with the plane
stress fracture toughness of the 6082 Al alloy. To correlate the mor-
phology of precipitates with the fracture toughness, annealing was also
performed after processing at 200 °C. Samples with similar conditions
along with similar features of grain refinements, secondary phase par-
ticles and precipitation from EBSD and TEM studies obtained in our
earlier study [36] were adopted for the present study. It is important to
note that to calculate the plane strain fracture toughness, the thickness
of the sample should be large. However, in the case of plane stress
fracture toughness test, small thickness of the sample is sufficient. In the
present work, the JIC is also used to calculate the critical plane stress
fracture toughness (KJIC) of the UFG 6082 Al alloy, keeping the thick-
ness constrains in mind. By using this approach, the constraint of high
thickness needed to maintain plane strain condition for calculating the
plane strain fracture toughness can be avoided.
2. Experimental study
2.1. Materials
In the present work, 6082-T6 Al alloy with a chemical composition
of (wt%) Al: 96.31, Si: 1.35, Mg: 0.67, Mn: 0.72, Fe: 0.248, Zn: 0.12,
Cu: 0.062, Cr: 0.0698, Ti: 0.045 and the remaining impurity was used.
The alloy was procured from Hindalco Industries Ltd. Mumbai, India
29
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
in the form of 50 mm thick plate. Samples of dimension
100 mm × 60 mm × 25 mm were cut from the plate for further pro-
cessing.
2.2. Heat treatments
Solution treatment of 6082-T6 Al alloy was performed to dissolve
the precipitates into the α-Al-matrix and to form equi-axed grains. For
the solution treatment, the samples were kept in muffle furnace at
540 °C for 24 h and immediately followed by water quenching at room
temperature [37]. Short annealing of the 75% cryorolled (CR + AN)
and the 75% room temperature rolled (RTR + AN) samples at 200 °C
for 1 h in muffle furnace was also carried out followed by water
quenching at room temperature.
2.3. Cryorolling (CR) and room temperature rolling (RTR)
The CR and RTR of the 6082 Al alloy were carried out up to 75%
thickness reductions at a true strain of 1.38. Prior to each CR pass, the
samples were dipped in liquid nitrogen for 15 min to ensure a tem-
perature of −196 °C was maintained. During CR, liquid nitrogen tem-
perature was maintained by pouring liquid nitrogen unto the samples
during processing and the samples were also dipped in liquid nitrogen
container immediately after each pass. In RTR, the same procedure was
adopted as in case of CR, but instead of liquid nitrogen, tap water was
used. The CR and RTR were performed by applying a thickness re-
duction of 0.4 mm in each pass to obtain the final thickness of 6.25 mm.
The initial thickness (25 mm) was chosen due to constraint of the la-
boratory rolling machine and the thickness after processing, 6.25 mm
was chosen to ensure the formation of ultrafined grains in the 6082 Al
alloy [36] and to follow the thickness criteria according to ASTM
E1820-13.
2.4. Mechanical characterization
The effects of CR, RTR, CR + AN, RTR + AN were studied in terms
of the critical plane stress fracture toughness (JIc). The plane stress
fracture toughness test was performed on Instron 8802 machine.
Compact tension (CT) samples (shown in Fig. 1) were machined parallel
to the rolling direction according to the ASTM E1820-13 for evaluating
plane stress fracture toughness test. For each test condition, at least 4
samples were tested for reproducibility of the results. The parameter
used during the plane stress fracture toughness (J1) tests were as fol-
lows: (i) Bedding in cycle number: 10, (ii) Bedding in frequency (Hz): 1,
(iii) Bedding in Amplitude: 1200 N, (iv) Load point displacement (LPD)
start point for load/unload: 0.2 mm, (v) LPD increment for load/un-
load: 0.02 mm, (vi) Unload percent from peak: 20%, (vii) Number of
load/unload sequences: 200, (viii) Number of data points in unload
segment: 100, and (ix) Break detect percent: 50%.
Fig. 1. The Compact tension (CT) sample was prepared according to ASTM E1820-13.
N. Kumar et al. Theoretical and Applied Fracture Mechanics 95 (2018) 28–41

Fig. 2. The Load point displacement (LPD) Vs Load curve for: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.

2.5. Metallurgical characterization
The metallurgical characterizations of the CR, RTR, CR + AN and
RTR + AN samples were carried out using SEM and EBSD in FE-SEM
Quanta 200 machine operated at 10 kV and 25 kV, respectively. To
study the minute surface microstructural features in the broken CT
sample after testing, detailed investigation using SEM was done. To
ensure conductivity during the fractography study, silver paste and
copper tape were used. To study the influence of crack growth on strain
accumulation inside the grains, an EBSD study was carried out. For the
EBSD, the surface of the sample was polished like mirror before the
mechanical testing, and after the testing, electro-polishing was per-
formed using the parameters that are available in the literature [15,36].
The step size used during the EBSD scanning was 0.05 µm. The kernel
average missorentation (KAM) maps/KAM-bar charts (for average KAM
value) were obtained by first performing grain dilation at the following
conditions: (i) Grain tolerance angle, 5°and (ii) Minimum grain size,
100 nm. Then, again by providing the following conditions, (i) Nearest
neighbor-1st, (ii) Maximum orientation, 5-degree, (iii) perimeter only
and finally, the KAM maps/KAM-bar chart (for average KAM value)
were obtained.
fracture toughness (KI)-test, specimen thickness should be high. The in-
valid KI-test was highlighted due to the failure to meet the sample
thickness criteria in UFG material. Therefore, a conditional fracture
toughness (KQ) was evaluated and reported in the literature [38–40]. The
J-Integral was evaluated to account for the elastic-plastic behavior of the
materials. A small thickness specimen is required for the plane stress
fracture toughness (JI)-test with a large size of plastic zone at the vicinity
of the crack tip. Begley and Landes developed an experimental technique
based on J-Integral [41]. They used CT specimens with different initial
crack length, and the load-displacement relation for each specimen was
obtained on a tensile test machine. To investigate the J-integrals in the
present work, two approaches were used (i) Load point displacement
(LPD)-Load curve, and (ii) J integral-Resistance curve (J-R Curve).
3.1.1. Load point displacement (LPD)-load curve
The plane stress fracture toughness was calculated on the basis of LPD-
Load curve theory given by the following equation (ASTM E1820-13).
K 2 (1−v 2)
J= + Jpl
E (1)
where

3. Results and discussion

K=
P ⎢
⎡
{ (2 + a
w w
a 2
) ⎡⎣0.886 + 4.64 ( )−13.32 ( )
a
w
+ 14.72 ( ) −5.6 ( ) ⎤⎦ } ⎤⎥
a 3
w
a 4
w

BN W ⎢ a 3/2 ⎥
3.1. Plane stress fracture toughness (JIC) ⎢
⎣
(1− )
w
⎥
⎦

The UFG materials produced by SPD techniques have a small thick- (2)
ness. However, to meet the plane strain condition during plane strain and

30
N. Kumar et al.
ηpl Apl
Jpl =
BN b (3)
In Eqs. (1)–(3), Apl is the area under the LPD-Load curve from the
origin up to the maximum load as shown in Fig. 2, BN is the net spe-
cimen thickness (BN = B, the thickness of the sample, if no side grooves
are present), W is the width of the sample, K is the stress intensity
factor, v is the Poisson ratio, E is the Young modulus of rigidity, a is the
crack length, and b is the uncrack ligament given by:
b = (W −a), (4)
and
b as evident from Fig. 3.
ηpl = 2 + 0.522
W (5)
In the case of the Al alloys: E = 70 GPa, v = 0.33. For CR + AN
sample, the value of ηpl (from Eq. (5)) is 2.273 and the value of Apl is
found to be 6370 N-mm (from Fig. 2(c)). Thus, using Eq. (3), the value
of Jpl is found to be 88.44 kJ/m2 and using Eq. (2), the value of K is
calculated as 266.624 N/mm2. By substituting these values of K and Jpl
in Eq. (1), the plane stress fracture toughness of the CR + AN sample is
found to be 89.34 kJ/m2. Similarly, the value of the plane stress frac-
ture toughness for CR, RTR, and RTR + AN samples are found to be
86.5 kJ/m2, 28 kJ/m2 and 36 kJ/m2, respectively.
In order to validate whether the calculated fracture toughness ob-
tained through LPD-Load curve theory is the critical fracture toughness
(JIC), the following constraints required on the specimen must be met
[42]:
25JIC
b⩾
σf (6)
25JIc
B⩾
σf (7)
where B is the thickness of the sample, σf is the yield strength and JIC is
the critical plane stress fracture toughness. To validate the critical plane
stress fracture toughness, the values of the plane stress fracture
toughness (89.34 kJ/m2) and the yield strength (290 MPa) [36] of the
CR + AN sample are substituted in Eqs. (6) and (7). Based on Eqs. (6)
and (7), the minimum unbroken ligament (b) and the minimum thick-
ness (B) required to validate the critical plane stress fracture toughness
is 8.93 mm. Similarly, the required minimum unbroken ligament and
minimum thickness calculated for CR, RTR and RTR + AN sample is
7.45 mm, 2.98 mm and 3.32 mm, respectively.
In the present work, the thickness of the sample was 6.25 mm and
the unbroken ligament was 26.2 mm. Therefore it can be inferred that
the value of “B” obtained for the CR and CR + AN samples did not
satisfy the criterion in Eq. (7). However, the values of both “b” and “B”
obtained for the RTR and the RTN + AN met the criteria in both Eqs.
(6) and (7). It is can be inferred therefore that due to failure to meet
both of the thickness criteria, the calculated plane stress fracture
toughness is a conditional fracture toughness (JQ) for CR and CR + AN
sample, whereas for RTR and RTR + AN samples, the calculated frac-
ture toughness for each sample is the critical fracture toughness (JIC).
3.1.2. J-Integral-Resistance curve (J-R Curve)
To validate the improvement in the plane stress fracture toughness
evaluation in the investigated samples, the J-integral values and the
corresponding crack extension values (J-R curve) are plotted as shown
in Fig. 3. To find the conditional plane stress fracture toughness (JQ),
the following procedures are adopted as per ASTM E1820-13: (i)
Δa = 0.01 W = 0.5 mm, (ii) Determine a construction line in ac-
cordance with the equation given as J = 2σY Δa ; the σY (yield strength)
is obtained from our earlier work [36], (iii) Draw an exclusion line
parallel to the construction line intersecting the abscissa at 0.15 mm,
(iv) Draw a second exclusion line parallel to the construction the line
b σ
intersecting the abscissa at 1.5 mm, (v) Find, Jlimit = 07.5Y , (v) Plot all J-
31
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
Δa points that fail inside the area enclosed by these two parallel lines
and capped by Jlimit, (vi) Plot a line parallel to the construction and
exclusion lines at an offset value of 0.2 mm, (vii) From the intersection
point of 0.15 mm exclusion line and J-R curve, a line was drawn on
abscissa to find Δamin, (viii) From the intersection point of 1.5 mm ex-
clusion line and J-R curve, a line was drawn on the abscissa to find
Δalimit, (ix) At least five data points must remain between Δamin, Δalimit,
and Jlimit to validate plane stress fracture toughness. By adopting the
stated procedures, the J-R curve is constructed for CR, RTR, CR + AN
and RTR + AN samples, as shown in Fig. 3. The conditional plane stress
fracture toughness (JQ) is found to be CR (49 kJ/m2), RTR (31 kJ/m2),
CR + AN, (69 kJ/m2) and RTR + AN (39 kJ/m2) samples, respectively,
The following criteria must be satisfied in order to consider whether
the conditional plane stress fracture toughness obtained through the J-R
curve theory above is the critical plane stress fracture toughness (ASTM
E1820-13):
10JQ
Thickness, B >
σY (8)
10JQ
Unbroken ligament, b >
σY (9)
Using Eqs. (8) and (9), the minimum thickness and the minimum
unbroken ligament required for validating the critical fracture plane
stress fracture toughness are 1.96 mm for CR, 1.319 mm for RTR,
2.379 mm for CR + AN and 1.444 mm RTR + AN samples, respectively.
In the present work, the sample thickness (6.25 mm) and unbroken li-
gament (26.2 mm) were used, which were far higher than the minimum
requirements obtained for the different processed conditions. There-
fore, it can be inferred that the values of these parameters obtained via
the J-R curve for all the processing conditions satisfied both criteria in
Eqs. (8) and (9). Thus, based on the J-R curve, the values of the critical
plane stress fracture toughness (JIC) are 49 kJ/m2 for CR, 31 kJ/m2 for
RTR, 69 kJ/m2 for CR + AN, and 39 kJ/m2 for RTR + AN samples.
3.1.3. Comparison between the LPD-Load curve and J-R curve
The values of the plane stress fracture toughness for RTR and
RTR + AN samples calculated using the LPD-Load curve are nearly the
same as those calculated using the J-R curve theory. These values also
satisfy the required constraints in Eqs. (6)–(9). However, for CR and
CR + AN samples, the values of the critical plane stress fracture
toughness calculated via the LPD-Load curve did not satisfy the re-
quired constraint in Eq. (7). The J-R curve predicts lower critical plane
stress fracture toughness for these samples and satisfies the required
constraints in Eqs. (8) and (9). The findings from this study have shown
that the plane stress fracture toughness calculated from J-R curve is
more accurate when compared to that obtained using the LPD-Load
curve. Thus, the values of the critical plane strain fracture toughness
(JIC) for CR (49 kJ/m2), RTR (31 kJ/m2), CR + AN (69 kJ/m2) and
RTR + AN (39 kJ/m2) samples, respectively were obtained based on
the J-R curve theory.
3.1.4. JI-assisted critical plane strain fracture toughness (KJIc )
The critical plane strain fracture toughness (KJIc ) was calculated
from the critical plane stress fracture toughness using the following
equation obtained from the ASTM E1820-13:
E ∗JIc
KJIc = √
1−v 2 (10)
where is the critical plane stress fracture toughness, E is the Young’s
modulus of elasticity (for Al, it is 70 GPa) and is Poisson ratio (for Al it
is 0.33). A critical plane fracture toughness KJIc of 106.537 MPa √m was
obtained for CR + AN sample by substituting the (69 kJ/m2) value
calculated from the J-R curve, E (70 GPa) and v (0.33) in Eq. (10). The
same procedure is adopted to obtain the KJIc of CR (89.78 MPa √m),
N. Kumar et al.
Fig. 3. The J-R curve for: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
RTR (71.40 MPa √m) and RTR + AN (80.10 MPa √m) samples, respec-
tively. Obtaining higher thickness sample in most of the SPD techniques
is a challenge to the best of our knowledge. By using the present ap-
proach, the constraint of high thickness required for maintaining plane
strain condition for calculating the plane strain fracture toughness can
be avoided.
3.2. Microstructural study before fatigue testing
3.2.1. Electron Back Scattered Diffraction (EBSD) study
The EBSD maps of the initial state, that is, before fatigue testing of
CR, RTR, CR + AN (200 °C) and RTR + AN (200 °C) samples have been
reported in our earlier work [36]. Based on the earlier work, no sec-
ondary phase precipitation was found in the CR, RTR, CR + AN and
RTR + AN from the EBSD maps. The reason for this observation can be
explained as follows. For the CR sample, secondary phase precipitation
was not found from the EBSD map as the precipitates remained dis-
solved in the Al-matrix. However, for the RTR, CR + AN (200 °C) and
RTR + AN (200 °C) samples, secondary phase precipitation was not
found due to its very small size (nm). For the EBSD scanning, a step size
of 0.05 µm was used. This step size was more than the precipitates size
in the case of RTR and CR + AN sample, whereas, in the case of
RTR + AN sample, the step size (50 nm) was close to the average pre-
cipitate size (70 nm, obtained from TEM study). Therefore, observing
precipitates during the EBSD scanning is difficult (instrumentation
limitation) due to their small size. Thus, a TEM study was done in our
earlier work to investigate the precipitates size [36]. The TEM results
(see Section 3.2.2 for additional details) show that after CR, the
32
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
precipitates remained dissolved into the Al-matrix, whereas, after RTR
only cluster formation (atomic size) occurs. After CR + AN (200 °C) and
RTR + AN (200 °C) precipitates of average size 20 nm and 70 nm were
formed [36].
3.2.2. Transmission Electron Microscope (TEM) study
The details of the grain size distribution and the dislocation den-
sities after CR, RTR, CR + AN and RTR + AN, obtained from a TEM
study, have been reported in our earlier work [36]. After CR and RTR,
the 6082 Al alloy was heavily deformed and showed ill-defined grain
boundaries. The CR sample exhibited heavy dislocations tangles and
more deformed area, due to the suppression of recovery at cryogenic
temperature. However, in the RTR sample, recovery occurs due to high
working temperature, which led to low dislocation sites and less de-
formed area. After annealing of the CR sample at 200 °C, precipitates
(needle shape, β″) came out from the Al matrix with an average size of
20 nm in length and 1 nm in width. Whereas in RTR sample, after an-
nealing at 200 °C, precipitates (rod shape, β′) came out from the Al
matrix with an average size of 70 nm in length and 3 nm in width.
After annealing at 200 °C, in CR sample, sub grains of 100–500 nm
were formed, whereas, in RTR sample sub grain of 400–700 nm were
formed. From the EBSD image of CR, RTR, CR + AN and RTR + AN
sample [36], it is clear that two regions are formed: (i) deformed-region
ii) sub grain-region, after annealing. The presence of sub grains-region
are more in RTR and RTR + AN samples when compared to CR and
CR + AN samples due to low dislocation densities in RTR and
RTR + AN samples. Furthermore, needle shaped precipitates produce
more pinning effect in CR + AN sample when compared to rod shape
N. Kumar et al.
precipitates in RTR + AN sample, resulting in higher dislocation den-
sity (deformed areas) and smaller size sub grain formation in CR + AN
sample when compared to RTR + AN sample.
3.3. Strengthening mechanism in annealed samples
The strengthening mechanisms of precipitates is mostly by shearing
and by-passing depending upon the critical diameter (dc ) of the pre-
cipitates that can be calculated from the following equation [43].
4πGm b
dc =
GP
where Gm & GP are shear modulus of matrix and precipitates respec-
tively. If the precipitates size <dc , strengthening by shearing occurs and
if the precipitates size >dc , strengthening by by-passing occurs. The
shearing of precipitates provides maximum strengthening by pinning
the grain boundaries and dislocations when compared to by-passing
mechanism. During by-passing mechanism, however, a large number of
dislocations are accumulated at the crack tip and promotes stress con-
centration sites [44]. The fatigue crack initiates from these stress con-
centration sites and enhance fatigue crack growth.
In our previous work [36], precipitates (Mg2Si) of average size
((20 nm (length) & 1 nm (width), needle shape)) and (70 nm (length) &
3 nm (width), rod shape)) were observed in CR + AN and RTR + AN
sample, respectively. The shear modulus and the Burgers vector (b) of
the Al alloy is 26 GPa and 0.286 nm, respectively [37]. The shear
modulus of Mg2Si (i.e., 49.2 GPa) was cited from Ref. [45]. By sub-
stituting all these values in Eq. (11), the critical diameter is found to be
1.89 nm. Based on this calculation, it is expected in the present work
that in CR + AN sample, only when dislocations and grain boundaries
interact at the face (front) of Mg2Si precipitates, strengthening by
shearing could predominate since the width of the precipitate (1 nm) is
less than the critical diameter (1.89 nm). However, for the other in-
teractions, by-pass mechanism occurs since the length (20 nm) of the
precipitate is greater than the critical diameter. This shows that in
CR + AN sample, a mixed mode of strengthening (shearing as well as
by-pass) occurs. In RTR + AN sample, only by-pass mechanism occurs
since both the width (3 nm) and the length (70 nm) of the precipitates
Fig. 4. The Mg-Si phase evolution at crack tip during crack growth for: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
are more than the critical diameter (1.89 nm).
3.4. Microstructural study after fatigue testing
3.4.1. Scanning Electron Microscopy (SEM) study
The SEM-images of CR, RTR, CR + AN and RTR + AN sample, near
the crack tip/crack growth region are shown in Fig. 4. In the CR sample,
a large fraction of Mg-Si phase comes out from the Al matrix at the
crack tip as shown in Fig. 4(a), whereas, in RTR sample, a small fraction
of Mg-Si phase comes out from the Al matrix at the crack tip as shown in
Fig. 4(b). In CR + AN sample, small size of Mg-Si phase (Si-rich)
(11)
emerged from the Al matrix in the crack propagation region, as shown
in Fig. 4(c), whereas, in RTR + AN sample, Mg-Si phase (Mg-rich)
emerged out from the Al matrix at the crack propagation region as
shown in Fig. 4(d). He et al. [46] reported the dissolution of Mg2Si-
particles after three solution treatment temperature with soaking time.
They reported that Mg2Si-particles dissolved more with increasing so-
lution treatment temperature (530 °C, 550 °C, and 570 °C) and the dis-
solution of Mg2Si-particles is more affected by solution treatment
temperature instead of soaking time (15 s, 30 s, and 1 min) in AA6014
alloy. Vlach et al. [47] observed that Mg-particles dissolved in Al matrix
after heat treatment. The main alloying elements in 6xxx-Al alloy are
Mg and Si; these elments combine to form the main strengthening
phase, Mg2Si [48]. This phase remains dissolved after solution treat-
ment and quenching stage [46], but comes out from the Al matrix as a
partial precipitate in form of intermetallic compound phases during
ageing stage [49]. These Mg-Si phases caused intergranular cracking
during fatigue testing in Al-Mg-Si alloy, but after dissolution of Mg-Si
phases into the Al-matrix, intergranular cracking is converted to flat
planes cracking [50]. It is evident from our earlier work that after CR,
Mg-Si phases remained dissolved in the α Al-matrix, whereas after RTR,
Mg-Si phases emerged out from the Al-matrix due to heating during
processing [15,36].
While performing the plane stress fracture toughness JI-test, max-
imum heat was generated at the crack tip due to plastic blunting of the
crack tip. This heat helps in the evolution of Mg-Si phase at the crack tip
from the Al matrix in the present work. The presence of Mg-Si phase at
only the crack path in the whole micrograph also supports the evolution
33
N. Kumar et al.
of these phases due to crack tip blunting as evident from Fig. 4. In the
CR sample, prior to testing, all Mg-Si phases remain dissolved in the Al
matrix due to the liquid nitrogen temperature. However, during the J1-
testing of the CR sample, a large fraction of Mg-Si phases evolved from
the Al matrix, due to plastic blunting of the crack tip, as shown in
Fig. 4(a), whereas a small fraction of Mg-Si phases emerged from the Al-
matrix in RTR sample (Fig. 4(b)). The large fraction of evolution of Mg-
Si phases in CR sample signifies that during processing, these phases are
fully dissolved in the Al-matrix. The small fraction of Mg-Si phase
evolution in RTR sample signifies the evolution of small fraction of
these phases during processing itself as shown in Fig. 4(b). In CR + AN
sample, a small size of Mg-Si phases (Si-rich) emerged out from the Al-
matrix as shown in Fig. 4(c). In CR + AN sample, due to annealing at
200 °C, a major fraction of Mg-Si-phases emerged from the Al matrix
during the JI-testing. This led to the evolution of the remaining small
fraction of the dissolved Mg-Si phases from the Al-matrix as shown in
Fig. 4(c). After annealing at 200 °C in RTR sample, Mg-Si phases (Mg-
rich) come out from the Al matrix due to crack tip blunting as shown in
Fig. 4(d). In RTR sample, during processing itself, a major fraction of
Mg-Si phases evolved from the Al matrix and after annealing at 200 °C,
the remaining Mg-Si phases come out from the Al matrix. This led to
evolution of the remaining dissolved Mg-Si phases from the Al-matrix
during the JI-testing in RTR + AN sample.
The fracture toughness study as reported in the previous section
shows that CR + AN sample has the highest plane stress fracture
toughness in comparison to all other samples investigated in the present
work. In CR + AN sample, a major fraction of Mg-Si phases evolved
from the Al- matrix and a small fraction of Mg-Si phases remain dis-
solved into the Al-matrix [15,36], which comes out from the Al-matrix
during the JI-test. The evolution of small sized Mg-Si phases during the
JI-testing caused crack branches and slowed down the crack propaga-
tion. Whereas in CR and RTR samples, large size Mg-Si phases evolved
out from the Al matrix, in which crack is easily passed underneath the
particles layers due to their large sizes as shown in Fig. 4(a) and (b). In
RTR + AN sample, large sized Mg-rich particles evolved out from the
Al-matrix, in these particles, crack is easily passed underneath of them,
due to their large sizes as shown in Fig. 4(d)). It can be concluded based
on the present section that partial dissolution and partial evolution of
Mg-Si phases are ideal for improving the plane stress fracture toughness
of the UFG material.
Fig. 5. The (a) image quality (IQ) map and (b) kernel average missorentation (KAM) map of solution treated (ST) 6082 Al alloy.
34
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
3.4.2. Electron Back Scattered Diffraction (EBSD) study
The EBSD map of the initial condition of the material (i.e., after
solution treatment (ST)) is shown in Fig. 5. It can be seen from the
image quality map and KAM map for the ST sample that the crack
moved along the grain boundaries (Fig. 5(a) and (b)) and no secondary
phase precipitation is found. The KAM maps and the image quality
maps of CR, RTR and annealed samples in the crack propagation region
at the crack tip are shown in Fig. 6. It can be observed from these maps
that after fatigue testing, secondary phase precipitations of micron size
occurs at the crack tip. These results are in accordance with the SEM
micrograph (Fig. 4) in which precipitates were found only in the crack
path/crack tip. It has been reported in literature that after deformation,
the stresses can be enhanced at grain boundaries due to the formation
of dislocation pile-ups [51–53]. In this case, the relation between the
flow stress and the average grain boundary spacing DB is given as
[51–53]:
σf = σ0 + k2 DB−1/2 (12)
where σf is the flow stress, DB is the average boundary spacing, σ0 is
a friction stress and k2 is a constant. In the present work, due to frag-
mentation of grains, the grains size is reduced (space between grain
boundaries is reduced) and dislocations were piled up at the grain
boundaries in CR, RTR, CR + AN and RTR + AN samples. These two
reasons might be strengthening the grain boundaries area as compared
to parent Al-matrix. However, due to heterogeneous deformation
during CR and RTR, the Al-matrix is stronger in some portion than the
grain boundary areas. In the present work, it is proposed that in the ST
sample, due to weak grain boundaries area, crack moves along the grain
boundaries (intergranular crack movement), whereas, in the case of CR,
RTR, CR + AN and RTR + AN samples, heterogeneous crack propaga-
tions (intergranular and transgranular crack movement) occur due to
heterogeneous deformation. It is well known that precipitates remained
dissolved and evolved into the Al-matrix and in the grain, respectively.
Therefore, in the ST sample, due to the crack movement along the grain
boundary, no secondary phase precipitation is observed (Fig. 5).
Whereas, in the case of CR, RTR, CR + AN and RTR + AN samples,
when crack moves in transgranular form, due to heat generation of
plastic blunting of the crack tip, precipitates evolved from the Al-matrix
and interact with the crack path (Fig. 6). Thus, it can be inferred that
secondary phase precipitation occurs during transgranular failure only
N. Kumar et al.
Fig. 6. The image quality (IQ) maps and kernel average missorentation (KAM) maps of: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
as evident from the present study.
The EBSD micrographs have lots of non-indexed point due to three
reasons: (i) cracks, (ii) precipitates, and (iii) strain accumulation. The
high KAM and crack branches can be seen only in the CR + AN sample
when compared to CR, RTR and RTR + AN sample (Fig. 6(c)). The high
KAM and crack branches are observed in CR + AN sample, due to
precipitation of small size Mg-Si (Si-rich) precipitates during testing
(Fig. 6(c)), which is also confirmed by the SEM study. The CR sample
(Fig. 6(a)) has higher KAM when compared to RTR or RTR + AN
sample. The reason for the high KAM in CR sample is due to the pre-
cipitation of large sized Mg-Si phase from α Al- matrix during testing
and highly deformed microstructure after CR. The size of Mg-Si phase
that evolved is larger in CR sample relative to RTR sample, as observed
from the results of the SEM study.
The stored energy per unit volume in the material can be obtained
by using the KAM given by [37].
1 αθGb
E= αρGb2 ≈
2 2d
where ‘α ’ is the dislocation geometric constant, ρ is the dislocation
density per unit area, G is the shear modulus, ‘b’ is the Burgers vectors,
‘G’ is the shear modulus, ‘θ ’ is the KAM and ‘D’ is the step size which is
0.05 µm in the present work. It is obvious from Eq. (13) that high KAM
value corresponds to high stored energy. The KAM-bar charts were
analyzed to calculate the average KAM as shown in Fig. 7. The average
KAM value for the ST, CR, RTR, CR + AN (200 °C) and RTR + AN
(200 °C) are 0.69-degree, 1.45-degree, 1.20-degree 1.58-degree, and
1.07-degree, respectively. It is evident from the present section that
CR + AN sample shows high KAM, indicating higher amount of energy
stored in the CR + AN sample. The energy stored during crack growth
is the energy required for creating two new surfaces according to
Griffith criteria. It can be inferred from the present work that the high
KAM (stored energy) in CR + AN sample, denotes the high load re-
quired during crack growth. According to the Griffith criteria, CR + AN
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
sample shows the highest plane stress fracture toughness among the
investigated samples.
3.4.3. Fractography study
As reported in Ref. [54], cracks are initiated at surface/near-sub
surface, secondary phase particles/precipitates and grow along high
shear stress planes. The crack propagation region is identified as a re-
gion of slip bands initiation at high shear stress planes, leaving behind
ripples. These ripples are formed due to plastic blunting and re-shar-
pening of the crack tip. Final rupture region contained ductile dimples,
transgranular facets, intergranular failure, mixed mode of failure and
many more features depending on the conditions and type of materials.
3.4.3.1. Globular view. The globular views of fractured samples for the
CR, RTR, CR + AN and RTR + AN samples are shown in Fig. 8. The
fractography area is divided into three region: (i) crack initiation (ii)
(13)
crack propagation (iii) final rupture. The boundary line between the
three regions are approximate boundary line. This is because Fig. 8
images were first taken at higher magnification to identify the regions,
then taking to low magnification to draw the boundaries between three
different regions. While drawing boundary lines, some regions were
over lapped, so these regions/boundary lines are approximate. It can be
seen from Fig. 8 that an area of ductile fracture is found in CR, RTR and
RTR + AN samples as shown by dotted circles in the final rupture
regions. Whereas in CR + AN sample, ductile fractures region is absent
and transgranular facets are found even in the final rupture region
(Fig. 11(c), discussed further in rupture region section). The CR + AN
sample reveals the sub grains of around 100–500 nm size and most of
the areas remain deformed [36]. These small size hard precipitates,
small size sub grain and deformed areas promote strengthening by
shearing, are responsible for the appearance of transgranular facets
even in the rupture region.
35
N. Kumar et al. Theoretical and Applied Fracture Mechanics 95 (2018) 28–41

Fig. 7. The kernel average misorentation bar chart of: (a) ST, (b) CR, (c) RTR, (d), CR + AN and (e) RTR + AN sample, of 6082 Al alloy.

Fig. 8. Globular view of fractures samples of: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.

36
N. Kumar et al.
Fig. 9. Crack initiation region of: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
3.4.3.2. Crack initiation region. Results: The fractograph of the crack
initiation region for the CR, RTR, CR + AN and RTR + AN samples are
shown in Fig. 9. In the CR sample (Fig. 9(a)), the secondary phase
particles were small in size, whereas, in RTR sample, secondary phase
particles of large size were found all over the region (Fig. 9(b)). In CR
sample (Fig. 9a), sub surface crack initiation sites were found, whereas,
in RTR sample near-surface crack initiation sites were formed
(Fig. 9(b)). In CR + AN sample, shallow ridges and micro-voids are
found as shown in Fig. 9(c), whereas in RTR + AN sample, lesser
shallow ridges, and micro crack are found as shown in Fig. 9(d). These
shallow ridges are parallel fatigue patches and might have fine fatigue
striations.
Discussion: In CR sample, due to the liquid nitrogen temperature,
secondary phase particles are fragmented to smaller value, whereas in
RTR sample, large size secondary phase particles are found [15,36].
This may be the reason for the secondary phase particles that are all
over the region in RTR sample (Fig. 9(b)). The crack initiation life has
increased in CR sample due to the following: (i) large residual com-
pressive stresses are produced due to the the liquid nitrogen tempera-
ture in CR sample. This might be a reason for the change of the crack
initiation site from near surface to sub surface in CR sample, (ii) The
fatigue crack initiation sites became flat due to the fragmentation of
secondary phase particles in CR sample. In RTR sample, due to large
size of secondary phase particles, large stress is accumulated on parti-
cles during testing and further crack is initiated as saturation limit
reached, as shown in Fig. 9(b).
It was reported that voids initiated at and grew along dislocation
cell and cell block boundaries created by plastic deformation [55]. In
general, a high density of deformation-induced boundaries was ob-
served near the voids [55]. The Wilsdorf's 1983 seminal review [56]
37
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
established that in the absence of particles and grain boundaries, void
initiation occurs at deformation-induced dislocation boundaries. Re-
lieving of the stored strain energy associated with the deformation-in-
duced boundaries is the primary mechanism for void initiation [55]. In
CR + AN sample, due to the rearrangement of dislocations, sub grains
of 100–500 nm size were formed [36]. After annealing at 200 °C in CR
samples, very small size sub grains are formed due to the pinning effects
produced by β″-precipitates [36]. These small size sub grains were
surrounded by deformation-induced boundaries or dislocations [36].
When the crack front interacts with the grain boundary of sub grain
(surrounded by heavy dislocations), the energy is relieved and as a
result, micro void formation occurs in the CR + AN sample. Micro-
crack is formed in RTR + AN sample due to de-bonding of secondary
phase particles/β′-precipitates from the Al-matrix [15,36]. Overall, the
CR sample has a high crack initiation life due to the presence of small
size secondary phase particles. In CR + AN sample, due to presence of
β″-precipitates, crack initiation life increases even after annealing.
3.4.3.3. Crack propagation region. Results: The fractographs of the crack
propagation region for CR, RTR, CR + AN and RTR + AN samples are
shown in Fig. 10. Fig. 10(a) indicates mixed mode of failure (i.e.,
intergranular failure as well as cleavage transgranular failure) in the CR
sample. In the RTR sample, intergranular failure is found as shown in
Fig. 10(b). The fraction of secondary phase particles are more in RTR
sample when compared to CR sample (Fig. 10(a) and (b)). In CR + AN
sample, transgranular facets, micro-void and few micro-cracks are
found as shown in Fig. 10(c), whereas in RTR + AN sample, less
transgranular facets, micro-void and micro-cracks are observed as
shown in Fig. 10(d). It is evident from Fig. 10(c) and (d) that the
orientation of fatigue striation is different from patch to patch. This
N. Kumar et al.
Fig. 10. Crack propagation region of: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
signifies that crack path and crack front direction are changing during
the crack propagation (crack path is tortuous instead of linear). The
fraction of tortuous crack path is more in CR + AN sample (Fig. 10(c)).
Discussion: It was reported that intergranular failure and cleavage
transgranular failure are influenced by the Mg-Si phases and hard in-
termetallic particles, respectively [50]. In CR sample, cleavage trans-
granular failure is due to heavy deformation during processing and
intergranular failure is due to secondary phase particles. As reported in
our earlier work, after solution treatment, the average grain size of the
6082 Al alloy was 85.7 µm [37]. After CR some grains of 6082 Al alloy
were severely deformed, which showed high dislocation densities [36].
When the crack interacts with these heavily deformed grain, the whole
grain is ruptured; leaving behind high energy features like transgra-
nular facets. This is the mechanism responsible for the formation of
transgranular facets in CR sample of several micrometers (Fig. 10(a)).
During testing, more strains are accumulated at the secondary phase
particles and the binding strength of grain boundaries are weakened by
secondary phase particles. This further contributed to intergranular
cracking in CR sample. In RTR sample, due to high fraction of sec-
ondary phase particles, the binding strength of grain boundaries are
further weakened leading to intergranular cracking all over the region.
In CR + AN sample, hardenable β″-precipitates (Si-rich) and in
RTR + AN sample, semi-hardenable β′-precipitates (Mg-rich) come out
from the Al matrix [15,36]. These precipitates are absent in CR and RTR
sample [15,36]. The transgranular facets may be formed due to β″ (Si-
rich) and β′(Mg-rich) precipitates. The fraction of transgranular facets
in CR + AN sample is more due to more crack path hindrance produced
by β″ (Si-rich) precipitates when compared to β′ (Mg-rich) precipitates
in RTR sample. The more tortuous crack path in CR + AN sample re-
lative to RTR + AN sample, might be due to β″ (Si-rich) precipitates
38
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
and βˈ(Mg-rich) precipitates, respectively. The micro-void formed in the
CR + AN sample is due to interaction of crack path with the grain
boundary of sub grain (surrounding by heavy dislocations). Similar
results were obtained by Carvalho et al. [44]. In RTR + AN sample,
secondary phase particle is found inside micro-void as evident from
Fig. 10(d). This feature indicates that micro-void formed in RTR + AN
sample was due to de-cohesion of secondary phase particles from Al
matrix during crack propagation. The micro-cracks are absent in the CR
and the RTR samples, which were formed due to β″ (Si-rich) pre-
cipitates and β′ (Mg-rich) precipitates. The fraction of micro cracks in
RTR + AN sample are more due to large size of β′ (Mg-rich) pre-
cipitates. These coarser precipitates served as stress raiser sites and
when stresses were saturated at precipitates, micro-cracks are formed.
In CR sample shearing mechanism dominates due to small size of β″ (Si-
rich) precipitates, and therefore less stress is accumulated at pre-
cipitates, which led to small fraction of micro-cracks.
3.4.3.4. Rupture region. Results: The fractography of the rupture region
in the CR, RTR, CR + AN and RTR + AN samples are shown in Fig. 11.
In CR sample, flat dimples, transgranular facets, and elongated dimples
are found as shown in Fig. 11(a). In RTR sample, elongated dimples and
ductile rupture dimples are found as shown in Fig. 11(b). In CR + AN
sample, transgranular facets, flat circular dimples and in-depth
elongated dimples are found as shown in Fig. 11(c). In RTR + AN
sample, elongated dimples with containing secondary phase particles
are found all over the region as shown in Fig. 11(d).
Discussion: It can be seen from Fig. 11(a) that secondary phase
particles are present in the elongated dimples. The interface between
the secondary phase particles and the Al-matrix is weak. The elongated
dimples might be formed due to de-bonding of the secondary phase
N. Kumar et al.
Fig. 11. Final rupture region of: (a) CR, (b) RTR, (c), CR + AN and (d) RTR + AN sample, of 6082 Al alloy.
particles from the Al matrix. The flat dimples and transgranular facets
are the features of heavy deformation during processing. The fraction
and depth of sheared dimples in the RTR sample are more when com-
pared to the CR sample, due to larger size of secondary phase particles.
The ductile fine dimples are formed due to two reasons: (i) stress-re-
lieving during RTR, and (ii) formation of recovered grains. Transgra-
nular facets and flat circular dimples are absent in CR sample, these
features that appeared in the CR + AN sample may be due to β″ (Si-
rich) precipitates interaction with the crack path. In-depth elongated
dimples are formed due to coarsening of secondary phase particles as a
result of the annealing of CR sample. In RTR + AN sample, inter-
granular fracture predominates all over the region and only a small area
related to transgranular facets. The grain boundaries failed to impede
crack path when coarser secondary phase particles are present at the
grain boundaries [57]. The binding strength of the grain boundaries is
weakened by the coarse secondary phase particles [57]. As a result of
these factors, intergranular fractures predominate in RTR + AN sample.
The small fraction of transgranular facets is observed due to βˈ (Mg-
rich) precipitates in RTR + AN sample.
4. Conclusions
In the present work, 6082 Al alloy subjected to CR, RTR and an-
nealing was investigated for plane stress fracture toughness. The
amount of energy stored during crack propagation in the processed
6082 Al alloys was evaluated in terms of KAM and various features that
evolved on the surface of the fractured samples obtained through EBSD
and SEM studies. The following conclusions are made based on present
investigation:
39
Theoretical and Applied Fracture Mechanics 95 (2018) 28–41
(1) The plane stress fracture toughness calculated from the J-R curve
fulfilled all the constraints required for critical fracture toughness
for all the processing routes, while the fracture toughness calculated
from LPD-Load curve failed to fulfil the critical fracture toughness
constraints for the CR and CR + AN samples. Based on the present
work results, The J-R curve gives more accurate plane stress frac-
ture toughness correlated to LPD-Load curve. The values of the
critical plane stress fracture toughness (JIC) obtained are: CR
(49 kJ/m2), RTR (31 kJ/m2), CR + AN (69 kJ/m2) and RTR + AN
(39 kJ/m2) samples, respectively from the J-R curve.
(2) The Mg-Si phases evolved at the crack tip during crack propagation
as evident from SEM study. The large sized Mg-Si phase evolution
from the Al-matrix also verified the complete dissolution of Mg-Si
phase in the α-Al-matrix during CR, while in other samples, small
size Mg-Si phase represents the evolution of precipitates before
testing.
(3) The highest KAM and crack branches were found in CR + AN
sample due to the precipitation of Si-rich precipitates, when com-
pared to CR, RTR and RTR + AN samples.
(4) Large fraction of shallow ridges, micro-void formation due to crack
interaction with grain boundaries, random fatigue patches, trans-
granular facets and flat circular dimples were found on fracture
surface of CR + AN samples. These features were the symbols of
mixed mode of failure and are responsible for its high plane stress
fracture toughness.
(5) To maintain the plane strain condition while measuring the plane
strain fracture toughness, large thickness samples is essential. In most
of the SPD study, the thickness of samples is small after processing.
The thickness of samples is a major constraint in UFG metals to
maintain the plane strain conditions. By using the critical plane stress
N. Kumar et al.
fracture toughness, the thickness of samples required to maintain the
plane stress condition is small, and the following plane strain fracture
toughness (KJIC) are calculated for CR (89.78 MPa √m), RTR
(71.40 MPa √m), CR + AN (106.537 MPa √m) and RTR + AN
(80.10 MPa √m) samples, respectively, in the present work.
Acknowledgement
The authors would like to acknowledge the financial support from
the Department of Defense (contract #: W911NF-15-1-0457) under the
direct supervision of Patricia Huff (HBCU/MI Program Manager, Army
Research Office).
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