See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/257707482

Achieving High Strength and High Ductility in Friction Stir-Processed Cast

Magnesium Alloy

Article in Metallurgical and Materials Transactions A · August 2013

DOI: 10.1007/s11661-013-1744-5

CITATIONS READS

43 506

3 authors:

Wei Yuan Sushanta Panigrahi

Hitachi America Ltd. Indian Institute of Technology Madras
41 PUBLICATIONS 1,742 CITATIONS 102 PUBLICATIONS 3,986 CITATIONS

SEE PROFILE SEE PROFILE

Rajiv S. Mishra
University of North Texas
524 PUBLICATIONS 30,889 CITATIONS

SEE PROFILE

All content following this page was uploaded by Sushanta Panigrahi on 09 May 2015.

The user has requested enhancement of the downloaded file.

Achieving High Strength and High Ductility in Friction
Stir-Processed Cast Magnesium Alloy
WEI YUAN, SUSHANTA K. PANIGRAHI, and RAJIV S. MISHRA

Friction stir processing (FSP) is emerging as an effective tool for microstructural modification
and property enhancement. As-cast AZ91 magnesium alloy was friction stir processed with
one-pass and two-pass to examine the influence of processing conditions on microstructural
evolution and corresponding mechanical properties. Grain refinement accompanied with
development of strong basal texture was observed for both processing conditions. Ultrafine-
grained (UFG) AZ91 was achieved under two-pass FSP with fine precipitates distributed on the
grain boundary. The processed UFG AZ91 exhibited a high tensile strength of ~435 MPa
(117 pct improvement) and tensile fracture elongation of ~23 pct. The promising combination of
strength and ductility is attributed to the elimination of casting porosity, and high density of fine
precipitates in an UFG structure with quite low dislocation density. The effects of grain size,
precipitate, and texture on deformation behavior have been discussed.

DOI: 10.1007/s11661-013-1744-5
 The Minerals, Metals & Materials Society and ASM International 2013

I. INTRODUCTION reduction in ductility, especially when the grain size is

MAGNESIUM alloys are attracting great interest
from transportation industries for structural applica-
tions because of their high strength-to-weight ratio.[1,2]
However, low ductility and room temperature formabil-
ity limit the processing and application.[3] As a result,
the main fabrication route of magnesium alloys remains
casting.[1,2] Casting defects such as microscopic shrink-
age porosity and inclusions adversely affect the strength
and ductility of magnesium alloy. It is expected that the
application will be expanded if the strength and ductility
of magnesium alloys can be enhanced.
Grain refinement has been a good option for enhanc-
ing the strength of magnesium alloys. Several severe
plastic deformation (SPD) tools, such as equal channel
angular extrusion/pressing,[4,5] high-pressure torsion,[6,7]
accumulated roll bonding,[8] alternate biaxial reverse
corrugated pressing,[9] differential speed rolling,[10,11]
and friction stir processing (FSP)[12–14] have demon-
strated capability in refining grain structure of magne-
sium alloys. However, grain refinement-induced
strength enhancement is generally accompanied by the
WEI YUAN, Researcher, is with the Department of Materials
Science & Engineering, Missouri University of Science and Technol-
ogy, Rolla, MO 65409, and also with the Research & Development
Division, Hitachi America Ltd., 34500 Grand River Avenue, Farm-
ington Hills, MI 48335. SUSHANTA K. PANIGRAHI, Assistant
Professor, is with the Department of Materials Science & Engineering,
Missouri University of Science and Technology, and also with the
Indian Institute of Technology Madras, Chennai 600036, India.
RAJIV S. MISHRA, Professor, is with the Department of Materials
Science & Engineering, Missouri University of Science and Technol-
ogy, and also with the Center for Friction Stir Processing, Department
of Materials Science and Engineering, University of North Texas,
Denton, TX 76203. Contact e-mail: Rajiv.Mishra@unt.edu
Manuscript submitted September 9, 2012.
Article published online April 20, 2013
refined to an ultrafine regime, mainly because of the
reduced work hardening.[15–17]
Texture, which is always observed in magnesium
alloys during intense shear deformation, plays an
important role on room-temperature deformation
behavior in addition to grain size as a result of limited
independent slip systems available. Texture modification
of wrought AZ magnesium alloys by SPD has shown
promising room-temperature ductility because of the
formation of a strong basal texture, which orientated the
easy basal slip plane to the preferred orientation;
however, the tensile yield strength was very low.[18–25]
The special basal texture generation during SPD also led
to the anisotropy in mechanical properties, especially in
yield strength, which is directly related to the activation
of deformation slip or twinning systems.[14,20,26]
It is desirable to enhance strength as well as ductility
in magnesium alloys. Recently, the FSP of cast alloys
has shown effective elimination of cast porosity, exten-
sive grain refinement, dissolution, and breakup of coarse
second phase.[12,27–32] Precipitation has been shown to
be an effective additive strengthening mechanism for
magnesium alloys in addition to the grain refinement-
related strengthening. Feng and Ma[28] reported a high
tensile strength of 337 MPa in AZ91 magnesium alloy
via FSP with average grain size refined to ~15 lm and
fine precipitates decorating the grain boundaries. By
introducing nanosized precipitates in a fine-grained rare
earth magnesium alloy EV31A through FSP, Freeney
and Mishra[30] obtained significant enhancement in
tensile strength and ductility. Xiao et al.[32] presented
similar findings on a FSP fine-grained Mg-Gd-Y-Zr
alloy with even higher tensile strength of 439 MPa, but a
noticeable loss of elongation to 3.4 pct. Our previous
study has achieved highly textured ultrafine-grained
(UFG) AZ31 using FSP, which exhibited high tensile
strength and ductility because of restricted basal slip.[26]

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 44A, AUGUST 2013—3675

The current study aims to (a) achieve high strength and
high ductility in commercial grade cast magnesium alloy
through microstructural modification, (b) verify whether
strong texture and strength anisotropy exist in FSP of
high aluminum content precipitation strengthened mag-
nesium alloy, and (c) explore the influence of grain size,
precipitates, and texture on deformation behavior of
processed magnesium alloy.
II. EXPERIMENTAL PROCEDURE
A high-pressure die-casting AZ91 magnesium alloy
having a thickness of 4.2 mm was used. The nominal
composition of this alloy was 9 wt pct aluminum and
1 wt pct zinc. To make friction stir passes, a tool with
12-mm diameter concave shoulder and 2.1-mm-stepped
spiral pin was employed. Two types of FSP runs were
made on the as-cast AZ91 with one-pass and two-pass
runs. A tool rotation rate of 600 revolutions per minute
(rpm) and a tool traverse speed of 1.7 mm/s were applied
to the one-pass run. Two-pass FSP was carried out with
300 rpm and 1.7 mm/s overlapping the first pass. A tool
tilt of 2.5 deg was adopted for all the FSP passes.
Microstructures of the friction stir-processed samples,
with cross section being perpendicular to the processing
direction (PD), were examined using optical microscopy
(OM), scanning electron microscope (SEM), and elec-
tron back-scattered diffraction (EBSD). For OM and
SEM observations, samples were mechanically polished
to 1 lm with alcohol-based diamond polishing com-
pounds and etched using an acetic picral solution (4.5 g
picric acid, 10 ml acetic acid, 10 ml water, and 70 ml
ethanol). The specimens for EBSD characterization
were further fine polished with 0.02 lm colloidal silica
solution. The EBSD characterization was performed at
the center of the processed AZ91 in a cross section
perpendicular to the PD. The linear intercept method
was used to obtain an average grain size. Transmission
electron microscope (TEM) samples were prepared by
focused ion milling in Helio Nano Lab 600 FIB/
FESEM. A TECNAI F20 TEM was used to examine
Fig. 1—Optical micrograph and SEM image of as-cast AZ91.
3676—VOLUME 44A, AUGUST 2013
grain structure and morphology and distribution of
precipitates under an operating voltage of 200 kV.
Tensile property characterization in the current study
was conducted using a computer-controlled, screw-driven
tensile testing machine at a constant crosshead velocity.
Tensile specimens have a gage length of 1.3 mm, a width
of 1.0 mm (to eliminate the effect of texture variation)
and a thickness of 0.6 mm. Specimens were machined
along the PD and transverse direction (TD) from the
center of the processed region and were polished with
1-lm finish and tested at room temperature at an initial
strain rate of 1 9 103 s1. Aging treatment at 441 K
(168 C) for 16 h was applied to two-pass AZ91 to
characterize the effect of post aging on tensile property.
At least three specimens for each condition were tested to
evaluate the average property values.
III. RESULTS
Figure 1 shows optical and SEM micrographs of
AZ91 alloy in the as-cast condition. The low magnifi-
cation of optical micrograph exhibits typical casting
features with dendritic pattern of a-Mg matrix in white
and second phase in gray.[29] The casting porosities in
black were visible in certain locations with an area
fraction of ~4.2 pct after averaging six randomly
selected locations with same magnification using ImageJ
software. The as-cast AZ91 varies in grain size with
small grains of about 10 lm and large dendrites of
about 120 lm. The secondary electron imaging at low
magnification shows high density of coarse second-
phase network distributed at grain boundaries. This
second phase was identified as b-Mg17Al12 phase
through energy dispersive X-ray (EDX) analysis. One
such b-Mg17Al12 phase is shown in Figure 2 with a size
of about 10 lm. The fraction of b-Mg17Al12 phase in as-
cast AZ91 was ~18.6 pct.
The friction stir-processed AZ91 was sectioned in the
TD for evaluation of the microstructure evolution.
Figure 3 presents the typical cross sections of friction
stir-processed AZ91 in one-pass and two-pass conditions.
METALLURGICAL AND MATERIALS TRANSACTIONS A
In the current study, different material flow behavior
can be observed for material processed with one-pass
and two-pass. The material processed with two-pass
shows a uniform macrostructure. However, a nonuni-
form structure can be observed for one-pass run, which
separates the processed region into top and bottom
parts.
Figure 4 presents the microstructures of one-pass
friction stir-processed AZ91 at top and bottom regions.
Figure 4(a) is a low-magnification view of the top region
and shows layer structure with alternate white and black
contrast. A high-magnification examination indicates
b-phase particle-rich layers, with some horizontally
elongated, incompletely dissolved coarse b-phase being
distributed alternately with a-Mg matrix. The cast
dendritic structure was completely eliminated and
substituted by much finer equiaxed grain structure.
Furthermore, examination of the processed region
showed complete elimination of cast porosity. A com-
parison between the top and bottom regions
(Figures 4(b) and (c)) indicates similar grain size with
an average grain size of about 2.8 ± 1.2 lm but distinct
precipitate distribution. As shown in Figure 4(d), the
initial coarse network type of Mg17Al12 phase were
dissolved or broken into much smaller and almost
equiaxed ones at the bottom region with majority of
them distributed at the grain boundaries.
Grain structure and precipitate morphology and
distribution of two-pass friction stir-processed AZ91
were examined using TEM. Figures 5(a) and (b) show a
bright-field image and scanning transmission electron
Fig. 2—Presence of b-Mg17Al12 phase and a-magnesium matrix in
the as-cast AZ91.
Fig. 3—Cross-sectional macrographs of friction stir-processed AZ91 with (a) single pass at 600 rpm/1.7 mm/s and (b) two-pass with 600 rpm/
1.7 mm/s for the first pass and 300 rpm/1.7 mm/s for the second pass.
METALLURGICAL AND MATERIALS TRANSACTIONS A
microscope (STEM) image at the same location. The
two-pass FSP caused a significant grain refinement
compared with the one-pass run with much finer and
more equiaxed grain structure. As shown in Figure 6(a),
the average grain size of two-pass friction stir-processed
AZ91 was 0.54 ± 0.20 lm computed based on STEM
images at six different locations. The grain boundaries
under bright field imaging are not distinct, which might
be related to the low misorienation angle nature of
boundaries. The round-edged b-Mg17Al12 phase parti-
cles were mainly observed on the grain boundaries and
grain triple junctions. Few round shaped finer precip-
itates were noticed in the grain interiors. The relatively
large precipitates have ellipse shape; however, the fine
precipitates retain a round shape. The size of precipi-
tates was computed in terms of equivalent circular
diameter (square root of the product of lengths in major
and minor axes of the ellipse) assuming ellipse shape of
precipitates. The size distribution of precipitates in two-
pass FSP is shown in Figure 6(b) with a phase fraction
of 12.8 pct. The average size of precipitates was
113 ± 98 nm. Few dislocations can be detected in the
processed region. Table I lists the EDX analysis of
contents at various locations, the grain interior con-
tained ~3.8 wt pct Al, and Zn was mainly concentrated
on precipitates or adjacent locations.
Figure 7 shows the {0002} and {10-10} pole figures of
friction stir-processed AZ91 in as-cast and friction stir-
processed conditions. The location for friction stir-
processed specimens was at the centerline of the pro-
cessed region at a depth of 1.0 mm. Pole figures of
{0002} and {10-10} of as-cast AZ91 indicate a relatively
random texture with maximum intensity of about 3.
This random texture of cast AZ91 was modified to a
strong basal fiber texture with alignment of the c-axes of
the grains tilting about 25 to 30 deg away from the ND
after FSP. The difference in degree of tilt between one-
pass and two-pass was negligible. The observation of
texture evolution in AZ91 is similar to that has been
reported in FSP of rolled AZ31 with a completely
different starting textures.[26]
Figure 8 presents the representative tensile engineer-
ing stress–strain curves of AZ91 in as-cast and friction
stir-processed conditions tested at room temperature
with an initial strain rate of 1 9 103 s1. At least three
(six for as-cast AZ91) specimens for each condition were
tested. The statistical value of mechanical properties,
including tensile yield strength (YS), ultimate tensile
strength (UTS), uniform elongation and total elonga-
tion to failure, are summarized in Table II. The as-
received AZ91 shows low tensile strength and poor
VOLUME 44A, AUGUST 2013—3677
room-temperature ductility of less than 3 pct total processed AZ91 tested in TD, after one-pass, the tensile
elongation to failure for average. Majority of the as-cast YS and total elongation increased from ~160 MPa to
AZ91 specimens failed abruptly. For friction stir- 302 MPa and ~3 pct to 19 pct, respectively. The tensile

Fig. 4—Micrographs show the grain structure and precipitate in one-pass friction stir-processed AZ91, (a, b) top region, and (c, d) bottom region.

Fig. 5—Grain structure and precipitates of two-pass friction stir-processed AZ91 in (a) TEM bright field image and (b) STEM image, location
‘A’ was marked in both images.

3678—VOLUME 44A, AUGUST 2013 METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 6—Frequency distribution plots of (a) grain size and (b) precipitate size in two-pass friction stir-processed AZ91.
Table I. Results of EDX Analysis of Fig. 5 (Weight Percent)
Location Al
A 3.8
B 39.6
C 3.6
D 19.4
Fig. 7—{0002} and {10-10} pole figures of AZ91 in (a) as-cast,
(b) one-pass FSP and (c) two-pass FSP.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Zn Mg
— 96.2
3.5 56.9
0.2 96.2
3.3 77.3
Fig. 8—Stress–strain curves of as-received and friction stir-processed
AZ91.
strength was further enhanced after two-pass FSP, with
average tensile YS of ~390 MPa and UTS of ~435 MPa.
The total elongation to failure for two-pass friction stir-
processed AZ91 was also improved to ~23 pct. Com-
parison of one-pass specimen with two-pass specimen
shows a decrease in uniform elongation from 13.6 pct to
8.8 pct, but an increase in total elongation as grain size
becomes finer. This observation is consistent with
previous findings on friction stir-processed AZ31.[23]
A significant anisotropy was also observed for friction
stir-processed AZ91 in PD and TD. For processed AZ91
tested in PD, all stress–strain curves exhibit a common
feature similar to that of the as-cast AZ91 specimens
that fractured without developing a macroscopic neck-
ing, i.e., there is no pronounced post-uniform elonga-
tion. However, unlike as-cast AZ91, the tensile strength
and total elongation were improved significantly after
FSP with more than 10 pct total elongation. Contrary to
the previous results on fine-grained and UFG AZ31,[23]
the ductility in PD for AZ91 increased as the grain grew
VOLUME 44A, AUGUST 2013—3679
 Table II. A Summary of Tensile Properties in Different Conditions
Condition YS (MPa) UTS (MPa)
As-Cast 162 ± 12 201
One-pass_TD 302 ± 3 379
One-pass_PD 203 ± 10 285
Two-pass_TD 390 ± 5 435
Two-pass_PD 258 ± 6 351
Two-pass+ aging_TD 381 ± 4 422
Two-pass + aging_PD 234 ± 8 329
finer. The discrepancy is likely to be due to the better
microstructural homogenization in two-pass AZ91 com-
pared with the one-pass. The observation that TD has
higher tensile strength as well as higher ductility than
those of PD for the current fine-grained and UFG AZ91
is similar to the findings of friction stir-processed
AZ31.[23] Aging of two-pass FSP did not enhance the
strength in either PD or TD, on the contrary, reduced
the ductility, especially in PD.
IV. DISCUSSION
A. Microstructural and Texture Evolution
The as-cast structure was modified by FSP with the
complete elimination of coarse dendritic grains and
casting porosity. Accompanying the grain refinement,
the coarse network type of precipitates was dissolved
and refined into much finer scale. However, distinct
difference in processed region was observed between
one-pass and two-pass FSP of as-cast AZ91, with
heterogeneous layer structure for one-pass and more
uniform structure for two-pass. Similar observation of
b-phase particles rich bands has been reported during
the FSPs of cast AZ91 and AZ80 magnesium alloys,
which was attributed to the lower strain rate/strain and
temperature conditions.[27,31] A high tool rotation rate
was suggested to dissolve b-phase and in turn achieve
uniform microstructure.[27] Processing parameters have
shown direct influence on the thickness of heterogeneous
layer during the FSP of cast AZ91. Previous observation
indicated that the top layer was thinner as the tool
rotation rate increased for a constant tool traverse speed
(images not shown).
Another factor causing the difference in the macro-
structures between one-pass and two-pass FSPs was the
characteristic of starting microstructure for processing.
During the FSP, material in front of the tool is driven
upward. The upward-moving material on the leading
side then sweeps around the pin in the rotation
direction;[33–35] however, on the trailing side, the layer
rotating with the tool is decelerated and is deposited in
the void in the wake of the pin with the assistance of tool
shoulder.[34] The heterogeneous layer structure is likely
related to the sweeping action of the shoulder as it
comes into contact with the as-cast material first and
transports it toward the trailing edge around the
rotating pin. Because of the significant difference
3680—VOLUME 44A, AUGUST 2013
Uniform Elongation (pct) Total Elongation (pct)
± 15 1.9 ± 1.4 2.7 ± 1.1
± 4 13.6 ± 0.8 19.1 ± 1.4
± 8 10.5 ± 1.3 10.5 ± 1.3
± 1 8.8 ± 0.3 23.4 ± 0.2
± 6 15.4 ± 0.4 15.6 ± 0.5
± 7 7.5 ± 0.4 21.2 ± 0.2
± 6 8.1 ± 0.5 8.1 ± 0.5
between the as-cast and the recrystallized microstruc-
tures, the transported cast material from the front of the
pin tool might not undergo full dissolution of precipi-
tates and exhibited the difference between top and
bottom regions. For the two-pass FSP, the starting
microstructure for the second pass is recrystallized grain
structure with remaining b-phase particles, which elim-
inated the variation in structure in the processed region
of the two-pass run. Pre-solution treatment of cast
magnesium alloy to homogenize the microstructure has
been proven to result in uniform microstructure in single
pass FSP.[29,31]
As shown in Figures 4 and 5, FSP eliminated cast
porosity, network type of coarse b-phase, and signifi-
cantly refined the grain structure as a result of dynamic
recrystallization.[12,27,36–39] Average grain sizes of
~2.8 and 0.5 lm were achieved in one-pass and two-
pass runs, respectively. UFG structure has been
reported by FSP of various metals and alloys, which
generally requires low frictional heat input, high strain
(rate) and extra cooling to recrystallize the grain
structure and suppress grain growth during post-
FSP.[13,40,41] The very low dislocation density in
two-pass friction stir-processed AZ91 might indicate
discontinuous dynamic recrystallization which sweeps
off dislocation during grain boundary migration, result-
ing in very low dislocation density in the recrystallized
grains. The current UFG structure via two-pass FSP
was mainly attributed to low heat input and homoge-
neous distribution of fine b-phase precipitates, which pin
grain boundary migration and inhibit grain growth.
The as-cast AZ91 had a random texture as expected
(Figure 7(a)). However, a strong basal texture devel-
oped during one-pass and two-pass FSPs. Similar to the
previous results in FSP of AZ31, a basal fiber texture for
both one-pass and two-pass runs shows a tilt of c-axis
toward the PD by about 25 through 30 deg at the
centerline of the processed region.[23,42] The formation
of basal texture has been well documented as a result of
shear deformation during FSP, which aligns the easy
basal slip planes roughly parallel to pin column sur-
face.[24–26,43] It has been suggested that rare earth
elements can weaken the deformation texture[44,45]
through particle-stimulated nucleation of recrystalliza-
tion.[46] However, from the current results, it can be
concluded that the b-phase particles have limited effect
on texture weakening with the evidence of much similar
strong basal texture between AZ91 and AZ31 both
obtained with FSP.
METALLURGICAL AND MATERIALS TRANSACTIONS A
B. Strengthening in Friction Stir-Processed AZ91
Magnesium Alloy
The strength of high aluminum content magnesium
alloy is influenced by the effect of alloy content on solid
solution strengthening, the size and volume fraction of
b-phase particles, as well as the grain size and existing
microstructural defects. The as-cast AZ91 exhibited
quite low tensile strength, poor elongation and large
variation in these properties. These are attributed to the
presence of cast porosities and network type coarse
Mg17Al12 phase at the grain boundaries that tend to
nucleate cracks or undergo debonding from the matrix
during deformation.[28]
FSP resulted in a significant improvement in both
tensile strength and ductility. This is mainly because of
porosity elimination, grain refinement, and significant
breakup and dissolution of the coarse Mg17Al12
phase.[28,30,31] Different from those reported by Feng
et al.[31] on AZ80 that one-pass FSP led to even less
ductility of ~3 pct (in PD) than that of as-cast, the
current one-pass FSP enhanced not only the tensile
strengths but also the ductility, although heterogeneous
microstructure was observed in both cases. The discrep-
ancy results from different thermal cycles which resulted
in different grain sizes and fractions of remaining
undissolved precipitates. The finer grain size and lower
amount of remaining coarse precipitates observed in the
one-pass specimens of the current study contributed to
the better tensile properties. The two-pass FSP in PD
further increased the tensile strength and ductility
compared with the one-pass FSP (as shown in Figure 8
and Table II) because of the further refinement of
grains, precipitates, and elimination of heterogeneous
microstructure as evidenced in Figures 4 and 5.
The TD testing exhibited much higher tensile strength
than that in PD for both one-pass and two-pass FSPs,
with extremely high tensile YS of ~390 MPa and UTS of
~435 MPa in two-pass FSP. The strength anisotropy
was attributed to the strong basal texture generated
during the FSP, which tilted the c-axis toward PD, and
in turn promoted easy basal slip in PD and difficult
nonbasal slip in TD.[26] High-strength AZ91 has also
been reported during high ratio differential speed
rolling, which appears difficult to interpret from
strengthening mechanisms point of view because of the
extremely fine grains of 280 nm and distribution of fine
b-phase particles (88 nm) on the grain boundaries.[47]
For the currently obtained high-strength AZ91, EDX
analysis (Table I) of grain interior of two-pass AZ91
showed low aluminum supersaturating with a content of
~3.8 wt pct, which was slightly higher than the content
in AZ31 magnesium alloy. Considering the much similar
c-axis tilts in friction stir-processed AZ91 and AZ31,
and the fact that the variation in basal c-axis tilt was
about 5 to 10 deg, it might be rational to compute the
tensile YS of the current friction stir-processed AZ91 by
adopting the empirical grain boundary strengthening
formula previously developed for friction stir-processed
AZ31 with additional strengthening from b-phase par-
ticles,[42] since the dislocation density was low for both
friction stir-processed AZ31 and AZ91 during dynamic
METALLURGICAL AND MATERIALS TRANSACTIONS A
recrystallization. The Hall–Petch parameters (friction
stress r0 and stress concentration factor ky) for grain-
boundary strengthening of friction stir-processed AZ31
with grain size between 0.7 and 10.2 lm is presented in
Table III.
The theoretically computed tensile YS values without
considering particle strengthening for two-pass friction
stir-processed UFG AZ91 were 163 MPa and 367 MPa
in PD and TD, respectively. The strengthening contri-
bution from interaction of b-phase particles with basal
dislocation through Orowan looping was developed by
Nie[48] and can be expressed as:
 
Gb d
DsOrowan ¼ pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi  ln p ; ½1
b
2p ð1  mÞ 0:953 p ffi  1 dp
f
where G is the shear modulus (17 GPa for magnesium),
b is the Burgers vector (3.2 9 1010 m), v is the
Poisson’s ratio (0.35),[49] f is the phase fraction (0.128)
of b-phase, dp is the mean planar diameter of the point
obstacles (1.13 9 107 m). The computed contribution
from particle strengthening to resolved shear stress is
34 MPa. A Taylor factor of 2.3 for basal slip dominated
deformation in PD was achieved from EBSD data by
assuming Sachs polycrystal deformation model (inter-
granular stress equilibrium). Therefore, the increase in
tensile YS due to b-phase particles was ~78 MPa. The
overall computed tensile YS in PD was 241 MPa,
slightly less than the experimentally determined value
of 258 MPa. Assuming similar particle–dislocation
interaction applies to nonbasal dislocation dominated
deformation in TD, by simply replacing the Taylor
factor to 2.2 for nonbasal slip according to EBSD data
analysis, an increase in tensile YS due to b-phase
particles was found to be ~75 MPa. This overestimates
the tensile YS to 442 MPa. These results indirectly
indicate that b-phase particles in two-pass friction stir-
processed UFG AZ91 have more effect on inhibiting
basal dislocation slip than nonbasal dislocation slip, at
least in the current study with this distribution of
precipitates. The slight variation in tensile YS and
significant reduction in ductility in PD, but hardly any
change in TD after aging might support this hypothesis.
The negligible effect of aging on property in current
UFG AZ91 compared with the significant strengthening
reported in fine-grained AZ91 by Feng et al.[28] was due
to the difference in Al contents in matrix, about 3.8 pct
for current study and 7.5 pct in Reference 28. It may be
speculated that grain boundary strengthening, solid
solution strengthening (initially embedded in Hall–Petch
formula for friction stir-processed AZ31) and particle
strengthening contributed to the overall strength at
Table III. Hall–Petch Parameters Developed for Friction
Stir-Processed AZ31[42]
Loading r0 (MPa) ky (MPa lm1/2)
PD 39 88
TD 145 157
VOLUME 44A, AUGUST 2013—3681
yielding in PD, and mainly grain boundary strengthen-
ing and solid solution strengthening in TD.
C. Effects of Grain Size and Precipitate on Work
Hardening and Ductility
The ductilities were significantly improved after FSPs
in both PD and TD compared with the as-cast condition
as shown in Figure 8 and Table II. The lower ductility
in the as-cast AZ91 was due to the presence of cast
porosity and network type of coarse b-phase, which
could be the stress concentration sites during loading: as
a consequence, crack nucleation, void coalescence, or
debonding between a-Mg matrix and b-phase led to
premature fracture. FSP eliminated casting defects and
coarse b-phase, and thus enhanced the tensile ductility.
The increase in ductility from one-pass to two-pass was
related to the particle refinement and microstructure
homogenization. Grain refinement to ultrafine scale
generally leads to reduction in ductility as a result of
reduced work hardening in finer grain size. It is also
reported that tensile ductility could be enhanced in the
UFG materials with lower dislocation density, which
can provide more room for dislocation storage.[50] The
current two-pass UFG AZ91 shows extremely high
tensile strength as well as high ductility, with a relatively
low uniform elongation but high post-uniform elonga-
tion in TD. The high post-uniform elongation was likely
related to the enhanced strain rate sensitivity as grain
size becomes finer.[51,52]
Although the uniform elongation in two-pass friction
stir-processed UFG AZ91 in TD was relatively low
compared with the PD or one-pass FSP, it is much
higher than that generally reported in UFG magnesium
alloy,[15,23] especially with such a high tensile strength.
This observation suggests that plastic instability was
delayed in current UFG AZ91 through either enhanced
work hardening ability or reduced rate of dislocation
recovery. Figure 9 plots the work hardening rate h
(=dr/de) derived from true stress verses true strain as a
function of true stress/net flow stress for friction
Fig. 9—Work hardening rate as a function of true stress and net flow stress for friction stir-processed AZ91 in PD and TD, work hardening
behavior of UFG AZ31 was also included.[23]
3682—VOLUME 44A, AUGUST 2013
stir-processed AZ91 in both PD and TD, as well as
friction stir-processed UFG AZ31(having ~2 pct uni-
form elongation in TD and ~10 pct uniform elongation
in PD).[23] After a short period of elastoplastic transi-
tion, the work hardening rate decreases linearly and
steadily for all testing conditions because of the balance
between dislocation storage and annihilation, which is
the stage III hardening range.[53] Stage III can be
expressed using Voce equation, which is given as
dr @Gbk1 k2 r
¼  ½2
de 2 2
where k1 is a constant and k2 is twice of the slope of the
strain hardening rate versus true stress plot and is an
indication of the rate of recovery. The first term on the
right-hand side is associated with the dislocation storage
discussed above and the second term is associated with
annihilation of dislocations. The stage III is different for
one-pass and two-pass FSP in PD and TD, evidenced
from the various slopes of stage III. The two-pass FSP
in TD shows the largest slope, followed by one-pass in
PD and one-pass in TD. The two-pass FSP in PD
exhibits lowest slope, i.e., the lowest rate of dislocation
recovery. As shown in Figure 9(b), the degree of work
hardening was smallest for two-pass in TD, and largest
for one-pass in TD and two-pass in PD, with one-pass in
PD in between. The largest degree of work hardening
and the lowest rate of dislocation recovery in PD for
two-pass AZ91 contribute to the highest uniform
elongation. On the contrary, the lowest in TD for two-
pass AZ91.
Comparing the UFG AZ91 with UFG AZ31, we find
that both have submicron grain sizes (0.5 lm for AZ91
and 0.8 lm for AZ31), similar inclined c-axis tilts of
about 25 through 30 deg, and low dislocation densities,
but completely different work hardening behaviors. The
initial work hardening rate was much higher for UFG
AZ31, but it quickly dropped below that of UFG AZ91
in a short net flow stress region. The recovery rate
determined by linear fit in stage III was much higher for
METALLURGICAL AND MATERIALS TRANSACTIONS A
UFG AZ31 than that for UFG AZ91 in both PD and
TD. It is quite possible that the fine b-phase precipitates
enhanced effective dislocation storage, which retarded
the drop of work hardening rate and resulted in the
improved uniform elongation in AZ91, although the
grain size was smaller than that of AZ31.
V. CONCLUSIONS
The as-cast AZ91 magnesium alloy was friction stir
processed with one-pass and two-pass runs. FSP elim-
inated porosity and significantly refined the average
grain sizes to 2.8 and 0.5 lm for one-pass and two-pass
runs, respectively, but also introduced strong basal fiber
texture. The network type of coarse precipitates was
dissolved and broken into fine particles mainly distrib-
uted at the grain boundaries. As the grain size reduced
during second FSP pass, the precipitates also became
finer. FSP remarkably enhanced the tensile property of
the as-cast AZ91. Two-pass FSP improved the tensile
YS to ~390 MPa, UTS to ~435 MPa (117 pct improve-
ment) in TD; and YS to ~258 MPa, and UTS to
~340 MPa (62 pct improvement) in PD. The tensile
failure elongations were also enhanced from 3.5 pct to
23 pct and to 16 pct in TD and PD, respectively. The
promising combination of strength and ductility was
attributed to the elimination of porosity in UFG
structure with low dislocation density and fine precip-
itates. Precipitates appear to influence basal dislocations
more than nonbasal dislocations in current UFG AZ91.
ACKNOWLEDGMENTS
The authors gratefully acknowledge the support
provided by the National Science Foundation through
grants NSF-EEC-0531019 and NSF-IIP-1157754.
REFERENCES
1. B.L. Mordike and T. Ebert: Mater. Sci. Eng. A, 2001, vol. 302,
pp. 37–45.
2. B.B. Clow: Adv. Mater. Process., 1996, vol. 150, p. 33.
3. S.R. Agnew, J.W. Senn, and J.A. Horton: JOM, 2006, vol. 58,
pp. 62–69.
4. M. Mabuchi, H. Iwasaki, K. Yanase, and K. Higashi: Scripta
Mater., 1997, vol. 36, pp. 681–86.
5. A. Yamashita, Z. Horita, and T.G. Langdon: Mater. Sci. Eng. A,
2001, vol. 300, pp. 142–47.
6. A. Galiyev and R. Kaibyshev: Mater. Trans., 2001, vol. 42,
pp. 1190–99.
7. M. Kai, Z. Horita, and T.G. Langdon: Mater. Sci. Eng. A, 2008,
vol. 488, pp. 117–24.
8. M.T. Pérez-Prado, J.A. Del Valle, and O.A. Ruano: Scripta
Mater., 2004, vol. 51, pp. 1093–97.
9. Q. Yang and A.K. Ghosh: Acta Mater., 2006, vol. 54, pp. 5147–58.
10. H. Watanabe, T. Mukai, and K. Ishikawa: J. Mater. Sci., 2004,
vol. 39, pp. 1477–80.
11. W.J. Kim, J.D. Park, J.Y. Wang, and W.S. Yoon: Scripta Mater.,
2007, vol. 57, pp. 755–58.
METALLURGICAL AND MATERIALS TRANSACTIONS A
12. R.S. Mishra and Z.Y. Ma: Mater. Sci. Eng. R, 2005, vol. 50, pp. 1–78.
13. C.I. Chang, X.H. Du, and J.C. Huang: Scripta Mater., 2007,
vol. 57, pp. 209–212.
14. G. Bhargava, W. Yuan, S.S. Webb, and R.S. Mishra: Metall.
Mater. Trans. A, 2010, vol. 41A, pp. 13–17.
15. S.X. Ding, W.T. Lee, C.P. Chang, L.W. Chang, and P.W. Kao:
Scripta Mater., 2008, vol. 59, pp. 1006–09.
16. W.J. Kim and Y.G. Lee: Mater. Sci. Eng. A, 2011, vol. 528,
pp. 2062–66.
17. W.J. Kim, Y.G. Lee, M.J. Lee, J.Y. Wang, and Y.B. Park: Scripta
Mater., 2011, vol. 65, pp. 1105–08.
18. T. Mukai, M. Yamanoi, H. Watanabe, and K. Higashi: Scripta
Mater., 2001, vol. 45, pp. 89–94.
19. J. Koike, T. Kobayashi, T. Mukai, H. Watanabe, M. Suzuki, K.
Maruyama, and K. Higashi: Acta Mater., 2003, vol. 51, pp. 2055–65.
20. S.R. Agnew, J.A. Horton, T.M. Lillo, and D.W. Brown: Scripta
Mater., 2004, vol. 50, pp. 377–81.
21. W.J. Kim, C.W. An, Y.S. Kim, and S.I. Hong: Scripta Mater.,
2002, vol. 47, pp. 39–44.
22. H.W. Lee, T.S. Lui, and L.H. Chen: J. Alloys Compd., 2009,
vol. 475, pp. 139–44.
23. W. Yuan and R.S. Mishra: Mater. Sci. Eng. A, 2012, vol. 558,
pp. 716–24.
24. Y.N. Wang, C.I. Chang, C.J. Lee, H.K. Lin, and J.C. Huang:
Scripta Mater., 2006, vol. 55, pp. 637–40.
25. W. Woo, H. Choo, D.W. Brown, P.K. Liaw, and Z. Feng: Scripta
Mater., 2006, vol. 54, pp. 1859–64.
26. W. Yuan, R.S. Mishra, B. Carlson, R.K. Mishra, R. Verma, and
R. Kubic: Scripta Mater., 2011, vol. 64, pp. 580–83.
27. Z.Y. Ma, A.L. Pilchak, M.C. Juhas, and J.C. Williams: Scripta
Mater., 2008, vol. 58, pp. 361–66.
28. A.H. Feng and Z.Y. Ma: Scripta Mater., 2007, vol. 56, pp. 397–
400.
29. P. Cavaliere and P.P. De Marco: J. Mater. Process. Technol., 2007,
vol. 184, pp. 77–83.
30. T.A. Freeney and R.S. Mishra: Metall. Mater. Trans. A, 2009,
vol. 41A, pp. 73–84.
31. A.H. Feng, B.L. Xiao, Z.Y. Ma, and R.S. Chen: Metall. Mater.
Trans. A, 2009, vol. 40A, pp. 2447–56.
32. B.L. Xiao, Q. Yang, J. Yang, W.G. Wang, G.M. Xie, and Z.Y.
Ma: J. Alloys Compd., 2011, vol. 509, pp. 2879–84.
33. H.N.B. Schmidt, T.L. Dickerson, and J.H. Hattel: Acta Mater.,
2006, vol. 54, pp. 1199–1209.
34. K. Colligan: Welding J., 1999, vol. 78, pp. 229–37s.
35. T.U. Seidel and A.P. Reynolds: Metall. Mater. Trans. A, 2001,
vol. 32A, pp. 2879–84.
36. J.A. Esparza, W.C. Davis, E.A. Trillo, and L.E. Murr: J. Mater.
Sci. Lett., 2002, vol. 21, pp. 917–20.
37. S.H.C. Park, Y.S. Sato, and H. Kokawa: J. Mater. Sci., 2003,
vol. 38, pp. 4379–83.
38. W.B. Lee, Y.M. Yeon, and S.B. Jung: J. Mater. Sci. Technol.,
2003, vol. 19, pp. 785–90.
39. U.F.H.R. Suhuddin, S. Mironov, Y.S. Sato, H. Kokawa, and
C.W. Lee: Acta Mater., 2009, vol. 57, pp. 5406–18.
40. C.I. Chang, X.H. Du, and J.C. Huang: Scripta Mater., 2008,
vol. 59, pp. 356–59.
41. J.Q. Su, T.W. Nelson, and C.J. Sterling: Scripta Mater., 2005,
vol. 52, pp. 135–40.
42. W. Yuan, S.K. Panigrahi, J.Q. Su, and R.S. Mishra: Scripta
Mater., 2011, vol. 65, pp. 994–97.
43. S.H.C. Park, Y.S. Sato and H. Kokawa: Metall. Mater. Trans. A,
2003, vol. 34A, pp. 987–94.
44. M.R. Barnett, M.D. Nave, and C.J. Bettles: Mater. Sci. Eng. A,
2004, vol. 386, pp. 205–11.
45. J. Bohlen, M.R. Nürnberg, J.W. Senn, D. Letzig, and S.R. Agnew:
Acta Mater., 2007, vol. 55, pp. 2101–12.
46. E.A. Ball and P.B. Prangnell: Scripta Metall., 1994, vol. 31,
pp. 111–16.
47. W.J. Kim, H.G. Jeong, and H.T. Jeong: Scripta Mater., 2009,
vol. 61, pp. 1040–43.
48. J.F. Nie: Scripta Mater., 2003, vol. 48, pp. 1009–15.
49. H.J. Frost and M.F. Ashby: Deformation-Mechanism Maps,
Pergamon Press, Oxford, 1982, p. 44.
VOLUME 44A, AUGUST 2013—3683
50. Y.H. Zhao, J.F. Bingert, Y.T. Zhu, X.Z. Liao, R.Z. Valiev, Z. 52. W.J. Kim, H.W. Lee, S.J. Yoo, and Y.B. Park: Mater. Sci. Eng. A,
Horita, T.G. Langdon, Y.Z. Zhou, and E.J. Lavernia: Appl. Phys. 2011, vol. 528, pp. 874–79.
Lett., 2008, vol. 92, p. 081903. 53. U.F. Kocks and H. Mecking: Prog. Mater Sci., 2003, vol. 48,
51. Q. Yang and A.K. Ghosh: Acta Mater., 2006, vol. 54, pp. 5159–70. pp. 171–273.

3684—VOLUME 44A, AUGUST 2013 METALLURGICAL AND MATERIALS TRANSACTIONS A

View publication stats