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K.N. Braszczynska-Malik
Czestochowa University of Technology, Institute of Materials Engineering, Al. Armii Krajowej 19, 42-200 Czestochowa, Poland
a r t i c l e
i n f o
Article history:
Received 5 May 2009
Received in revised form 15 July 2009
Accepted 17 July 2009
Available online 25 July 2009
Keywords:
Magnesium alloy
Precipitation
Microstructure
Equal-channel angular pressing
a b s t r a c t
The microstructure investigations of the AZ91 alloy after equal-channel angular pressing (ECAP) were
presented. Solution annealed billets were processed at a 0.16 mm s1 pressing rate and temperatures of
623 and 553 K. The average grain size was reduced from 150 m initially to a nal value of 10 m. The
microstructure analyses revealed -Mg17 Al12 precipitates with a spherical morphology located particularly inside the equiaxal grains of an -solid solution. Additionally, different shapes of precipitates,
plate-like or rod-like (typical for heat treatment processes) were not observed. The spherical shape of
precipitates was obtained due to correlate magnesium matrix alloy deformation during pressing with
precipitation process.
2009 Elsevier B.V. All rights reserved.
1. Introduction
The AZ91 (MgAlZn) alloy is the most widely used magnesium
alloy exhibiting a good combination of high strength at room temperature, good castability and excellent corrosion resistance [14].
The microstructure of as-cast AZ91 alloy is generally characterized
by a solid solution of aluminium in magnesium (an -Mg phase
with a hexagonal closely-packed, hcp structure) and an + eutectic. In MgAl type alloys, the phase (called also phase [59])
is an intermetallic compound with a stoichiometric composition
of Mg17 Al12 (at 43.95 wt.% Al) and an -Mn-type cubic unit cell.
The zinc that is present in the AZ91 alloy does not create new
phases but substitutes aluminium in the -Mg17 Al12 phase, forming
a ternary intermetallic compound Mg17 Al11.5 Zn0.5 or Mg17 (Al,Zn)12
type [9,10].
Magnesiumaluminium alloys are susceptible to heat treatment
due to the variable solubility of aluminium in a solid state from
12.9 wt.% Al at an eutectic temperature of 710 K to about 2.9 wt.%
Al at 473 K. During conventional heat treatment of the AZ91 alloy,
involving solution annealing at about 690 K for a minimum of 24 h
(Fig. 1a), followed by ageing at about 430 K for 16 h (T6 conditions),
the discontinuous precipitates of the phase appear [4,10]. On the
other hand, during the ageing of a supersaturated solid solution at
a higher temperature, continuous precipitates of the phase can
also occur simultaneously [4,10]. Fig. 1b and c presents a discontinuous and continuous precipitates of the phase after ageing
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ECAP deformation carried out at 498 (four passes) and 453 K (two
passes) at a pressing speed of 25.2 mm/min and via route BC (before
ECAP samples were hot-rolled). Mthis et al. [32] observed rod-like
precipitates in AZ91 alloy pressed four times at 543 K using route
C with a pressing rate of 5 mm/min. They also concluded that long
rod-like precipitates were broken into smaller parts during ECAP
carried out in up to eight passes. Miyahara et al. [26] presented
small phase particles lying preferentially on the grain boundary
in the AZ61 alloy after pressing in four passes at 473 and 523 K via
route BC .
In the present work, ECAP processing was applied to obtain
a new shape of phase precipitates in AZ91 alloy thanks to
correlate plastic deformation behaviour during pressing with a precipitation process. Investigations of the individual microstructure
development were conducted using light, scanning and transmission electron microscopy.
2. Experimental procedures
Fig. 1. Microstructure of AZ91 alloy after: (a) solution annealing at 693 K for 24 h,
supersaturated solid solution; light microscopy, (b) ageing at 423 K for 16 h, discontinuous precipitates of phase, (c) ageing at 623 K for 8 h, continuous precipitates
of phase; SEM.
The commercial as-cast AZ91 magnesium alloy with a nominal chemical composition of 9 wt.% Al, 1 wt.% Zn, 0.5 wt.% Mn was used in this study. The investigated
AZ91 alloy was cut into rods of 50 mm in length and 11.8 mm in diameter. Before
the ECAP process, the samples were heat treated in order to obtain a homogeneous
microstructure. Solution annealing was carried out at 693 K for 26 h in a protective
argon atmosphere followed by water quenching (at approximately 287 K) for all the
samples. The microstructure obtained after this heat treatment was characterized
by large grains of supersaturated solid solution with an average grain size of about
150 m (Fig. 1a).
The ECAP die used in this investigation was designed to obtain a maximum shear
strain of about 1.15 during each pass. It contained an inner contact angle equal
to 90 and corner angle of 0 . The billets were processed at a pressing rate of
0.16 mm s1 using a plunger attached to a hydraulic press on an Instron machine. All
the pressings were conducted using route BC . This procedure was adopted because it
is evident from many experiments [16,17,2330] that the BC route leads most effectively to an array of equiaxed, ne grains separated by high-angle grain boundaries.
For each separate pressing, the samples were coated with molybdenum disulphide
(MoS2 ) as a lubricant. The temperature of the process was controlled using a thermocouple in a die. The process was conducted at 623 and 553 K, i.e. below the solvus
curve (in the range of ageing temperatures).
The samples were subjected up to four pressings and then sectioned for
microstructure examination. All microstructure analyses were carried out from both
transverse and longitudinal sections of the as-pressed billets using light and scanning electron microscopy (SEM) techniques. A standard metallographic technique
was applied for sample preparation including wet prepolishing and polishing with
different diamond pastes without contact with water. To reveal the microstructure, samples were etched in a 1% solution of HNO3 in C2 H5 OH for about 60 s. An
XL30ESEM FEG (Philips, Eindhoven, The Netherlands) scanning electron microscope
was used. The microstructure of the deformed samples was also studied using transmission electron microscopy (TEM) on a Philips CM20 instrument equipped with
an energy dispersive X-ray (EDX) spectrometer operating at 200 kV (Philips, Eindhoven, The Netherlands). For TEM analyses, the thin foils for transmission electron
microscopy study were polished electrolytically. The slices of material from both
the transverse and longitudinal sections of the as-pressed billets were mechanically thinned down, followed by punching of 3-mm diameter discs. Finally, the discs
were thinned to perforation using a Fischione double-jet electropolisher (Fischione,
Export, PA) with a solution of 33% nitric acid and 67% methyl alcohol at a temperature
of 245 K and a voltage of 20 V. The brighteld technique was used for microstructure
observations and selected area electron diffraction (SAED) patterns were employed
to dene structural constituents.
3. Results
Fig. 2 shows a representative microstructure of the AZ91 alloy
observed after four passes of the ECAP process conducted at 623 K.
The initial average grain size for the annealed condition was about
150 m as shown in Fig. 1a. The grain structure shown in Fig. 2
was recorded after four passes via route BC using the die with
contact angle equal to 90 (which allowed attainment of a maximum shear strain of about 1.15 during each pass). The average grain
size was reduced to a nal value of about 10 m. This result conrms that ECAP is a powerful technique to obtain a fast decrease of
grain size in the AZ91 magnesium alloy. Additionally, it can also be
seen that the microstructure was characterized by the presence of
K.N. Braszczy
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265
Fig. 2. Microstructure of AZ91 alloy after four ECAP passes at 623 K (a) transverse
section (b) longitudinal section; light microscopy.
Fig. 3. Microstructure of AZ91 alloy after two ECAP passes at 553 K (a and b) transverse section (c) longitudinal section; light microscopy.
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Fig. 6. TEM image of AZ91 alloy after two ECAP passes at 623 K; longitudinal section
(a) and result of EDX analysis obtained from precipitate marked as X (b).
Fig. 4. Microstructure of AZ91 alloy after four ECAP passes at 623 K (a) longitudinal
section (b) transverse section; SEM.
Fig. 5. TEM image of AZ91 alloy after two ECAP passes at 623 K; longitudinal section.
K.N. Braszczy
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267
Fig. 7. TEM images of AZ91 alloy after two (a) and four (b) ECAP passes at 623 K; longitudinal sections (SAED patterns obtained from the spherical precipitates marked
as Y and Z).
268
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