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Melt-Conditioned, High-Pressure Die Casting of Mg–Zn–Y Alloy

MINGXU XIA, SUBHAJIT MITRA, BRIJ DHINDAW, GUOJUN LIU,


and ZHONGYUN FAN

The liquid Mg–Zn–Y alloy was conditioned by an application of high-intensive shearing with a
pair of intermesh twin screws prior to high-pressure die casting (HPDC). Melt conditioning
produces a uniform microstructure with fine grain size and high integrity. The microstructure
was analyzed thoroughly, and the solidification characteristics of the melt-conditioned HPDC
(MC-HPDC) structure were discussed. The enhancement in I-phase precipitation and the
improvement in mechanical properties of MC-HPDC Mg–Zn–Y alloy can be achieved through
cyclic annealing.

DOI: 10.1007/s11663-009-9312-5
 The Minerals, Metals & Materials Society and ASM International 2009

I. INTRODUCTION nuclei in the subsequent solidification process.[5] More


importantly, the final MC-HPDC products have close-
BECAUSE they are the lightest structural material, to-zero porosity owing to bulk solidification and,
magnesium alloys have been used increasingly for therefore, can be heat treated in downstream processes.
structural components for several decades, particularly It also has been shown that a wider composition range
in the automobile industry. However, magnesium alloys of Mg alloys with limited castability can be processed by
exhibit moderate strength with limited ductility at room MC-HPDC, which opens up new opportunities for die-
temperature because of their hexagonal close-packed cast Mg alloys in high-performance applications.
(HCP) structure. Thus, magnesium alloys mostly are In various Mg alloys, Mg–Zn alloys have shown
fabricated through casting, especially, die casting.[1] improved mechanical properties compared with other
Although high-pressure die casting (HPDC) is a well- Mg alloys through the addition of rare earth elements
established process with high efficiency and low cost, the like yttrium (Y), which form quasicrytalline precipitates
application of this procedure is limited to only certain named the I-phase.[6–9] Most quasicrystal phases in
Mg alloys, such as AZ91D and AM60, because most Mg Mg–Zn–Y alloys is a stable three-dimensional phase
alloys have poor castability. HPDC components also that looks like an icosahedron platonic solid in normal
contain a substantial amount of porosity because of gas casting conditions.[8,9] However, only limited public
entrapment during filling of the die cavity and hot literature is available for HPDC Mg–Zn–Y alloys. In
tearing during solidification.[2] Such porosity not only this article, we investigate the microstructural develop-
adversely affects mechanical properties but also prevents ment and mechanical properties of a dilute Mg–Zn–Y
property enhancement with a subsequent heat treatment. alloy produced by the MC-HPDC process and apply the
One of the promising technologies capable of pro- annealing technique to improve the mechanical proper-
ducing high-integrity components is the melt- ties of the diluted Mg–Zn–Y alloy.
conditioned HPDC (MC-HPDC) process,[3] which
offers advantages such as extremely low porosity, fine
and uniform microstructure, as well as enhanced II. EXPERIMENTAL PROCEDURE
mechanical properties.[4] In this process, the liquid melt
undergoes high-intensive shearing and turbulence, A ternary Mg95.99–Zn3.45–Y0.56 alloy with a liquidus
which are generated by specially designed twin profile temperature of 613 C was prepared in an electric
screws in a heated barrel with precise temperature resistance furnace from pure Mg, Zn, and Mg–Y master
control. The application of intensive shearing to the alloy with 78 wt pct Y, in an protective atmosphere with
liquid melt has shown an increase in the effective a mixture of (N2 + 0.5 vol pct SF6). The alloy was
nucleation rate by maintaining a homogeneous chemical melted at 720 C and then held at 680 C for 30 minutes
composition and temperature distribution in the liquid to homogenize the chemical composition. The melt was
melt, which gives survival opportunity to numerous processed with HPDC and MC-HPDC under identical
conditions for comparison study. For the MC-HPDC
process, the liquid metal was fed into the melt condi-
MINGXU XIA and GUOJUN LIU, Research Fellows, and
ZHONGYUN FAN, Director, are with BCAST, Brunel University,
tioner and sheared at 611 C (semisolid), 614 C
Uxbridge, Middlesex UB8 3PH, United Kingdom. SUBHAJIT (around liquidus), and 623 C (above liquidus) for
MITRA, Researcher/Manager, is with Tata Steel, Jamshedpur, India. 45 seconds at a shearing speed of 800 rpm to find the
BRIJ DHINDAW, Dean of Academic & Research, is with the Indian microstructural differences among the shearing temper-
Institute of Technology, IIT Ropar, Rupnagar, India. Contact e-mail: atures. The barrel was heated and held the temperature
dhindaw@gmail.com
Manuscript submitted April 2, 2009. with multiple sets of heaters equipped with separated
Article published online October 29, 2009. precise temperature controllers. The temperature

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 41B, FEBRUARY 2010—209


deviation of each controller was under ±1 C. Typical microscope, Zeiss Axioskop2 (Zeiss Gmbh, Gottingen,
MC-HPDC setup is shown in Figure 1. For conven- Germany), equipped with quantitative analysis software
tional HPDC, the liquid metal was poured directly into Axiovision 4.3 was used for the OM observations and
the shoot sleeve at 660 C without melt conditioning. A grain size measurement under the ASTM E112-96
280-ton cold chamber HPDC machine was used to standard. The experimental error in this experiment
produce standard tensile test samples. The dimensions was ±5 lm. Transmission Electron Microscopy (TEM)
of the tensile test samples were 6.4 mm and 25 mm in foil was prepared using Ion-miller from a 3 mm diameter
gauge diameter and length, respectively. Die tempera- discs with a thinness of 80–90 lm. High resolution TEM
ture was kept constant at 220 C. (HRTEM) analysis was carried out using JEOL
Several heating and cooling cycles were carried out JEM2100 microscope (JEOL Ltd., Tokyo, Japan)
for the cyclic annealing between 360 C and 420 C for equipped with EDS, operated at an accelerating voltage
different times, whereas for the conventional annealing of 200 kV. Phase identification also was performed with
process, the samples were held at a specific temperature a Philips PW1710 (Philip, Eindhoven, The Netherlands)
between 360 C and 420 C for 3 hours and air cooled X-ray diffractometer using monochromatic Cu K-radi-
after the heat treatment. The heating and cooling rates ation. Tensile testing was performed at a strain rate of
used in annealing were 20 C/min. The schematic 1 9 10 3 s 1 at room temperature using an Instron
illustration of the difference between conventional and 5500 Universal Electromechanical Testing Systems
cyclic annealing is shown in Figure 2. (Norwood, MA) equipped with a Bluehill software
The specimens for optical microscopy (OM) were and a ±50 kN load cell, and the hardness was measured
prepared through the standard technique of grinding by a Vickers microhardness tester, Buehler Micromet II
them with SiC abrasive papers, polishing them with an (Buehler Ltd., Lake Bluff, IL).
Al2O3 suspension, and then etching them in a solution
of 75 vol pct ethylene glycol, 24 vol pct acetic acid,
and 1 vol pct concentrated HNO3. A Zeiss optical
III. RESULTS AND DISCUSSION
A. As-Cast Microstructure of MC-HPDC
Mg95.99–Zn3.45–Y0.56 Alloy
High Pressure Die Casting Machine Figure 3 illustrates the microstructures of the con-
ventional HPDC and MC-HPDC Mg95.99–Zn3.45–Y0.56
alloy. The typical microstructure of HPDC shows highly
developed dendrites with an extremely nonuniform
microstructure. Some dendrites have much coarser arms
Melt Conditioner
than others. Porosity was observed in the grain bound-
aries of the HPDC sample in Figure 3(a). In contrast,
MC-HPDC shows a more uniform microstructure
than conventional HPDC as shown in Figure 3(b)
through (d). The presence of porosity and shrinkage
cavity hardly was observed in the MC-HPDC samples
even under high magnification (Figure 4). The micro-
Fig. 1—MC-HPDC setup (combination of a melt conditioner and structure of the MC-HPDC samples mostly consists of
conventional high-pressure die-casting machine).
equiaxed primary a phase instead of dendrites in
conventional HPDC. The average grain size of the
primary phase was 28 ± 2 lm for the sample sheared
at 611 C (Figure 2(a)), 21 ± 5 lm at 614 C, and
30 ± 3 lm at 623 C. Obvious primary a-Mg rosettes
were observed in the samples with shearing temperature
of 614 C and 623 C. X-Ray Diffraction (XRD)
Temperature
Interval

patterns of MC-HPDC samples suggest the presence


of a-Mg, I-phase and weak Mg7Zn3 peaks that are
illustrated by the spectrum in Figure 5. The presence of
Temperature

I-phase in the as-cast alloys with similar composition


has been reported in Reference 10.
It is well known that a liquid Mg alloy has potential
Cyclic Annealing nucleation sites for subsequent solidification. The appli-
cation of high-intensive shearing and turbulence to the
Conventional Annealing liquid metal will disperse nucleation sites uniformly and
maintain a uniform composition and temperature dis-
tribution throughout the liquid metal.[5] If the shearing
Time hr temperature is lower than the liquidus temperature, then
primary a-Mg will nucleate homogeneously and form
Fig. 2—Schematic illustration of cyclic and conventional annealing. semisolid slurry inside the twin screw barrel. After the

210—VOLUME 41B, FEBRUARY 2010 METALLURGICAL AND MATERIALS TRANSACTIONS B


Fig. 3—Optical microstructure of (a) conventional die-casted sample and MC-HPDC sample sheared at 800 rpm for 45 seconds at (b) 611 C (c)
614 C, and (d) 623 C.

Fig. 4—High magnification OM view of MC-HPDC (sheared at


611 C for 45 seconds at 800 rpm) (scale bar 20 lm). Fig. 5—XRD pattern of as-cast MC-HPDC Mg–Zn–Y alloy reveal-
ing I-phase containing.

semisolid slurry is delivered into shoot sleeves, more shearing temperatures were varied, then solidification
solidification occurs on the presolidified a-Mg. Only a microstructures would be different as shown in
few of the survived nuclei can develop independently to Figures 3(b) through (d). Samples sheared at a higher
the rosette a-Mg phase as shown in Figure 3(b). If the temperature show more primary a-Mg rosettes than

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 41B, FEBRUARY 2010—211


Fig. 6—OM view of MC-HPDC sample (a) conventional annealed for 24 hours at 380 C and (b) cyclic annealed for 1.5 hours between 380 C
and 400 C (scale bar 20 lm).

Fig. 7—XRD pattern of annealed MC-HPDC Mg–Zn–Y alloy


showing W-phase and I-phase containing.
Fig. 8—High resolution TEM (HRTEM) image of cyclic annealed
those samples sheared at a lower temperature. It is MC-HPDC Mg–Zn–Y alloy (sheared at 611 C for 45 seconds at
interesting to see that finally solidified secondary a 800 rpm) showing needle-like shape I-phase precipitate.
phases continues to reveal equiaxed grains in the
MC-HPDC samples, as shown in Figure 4.
Table I. Hardness Value of As-Cast MC-HPDC
Mg95.99–Zn3.45–Y0.56 Alloy Continuously Annealed
B. Annealed Microstructure of MC-HPDC for 3 Hours
Mg95.99–Zn3.45–Y0.56 Alloy
Temperature, C Hardness (Hv)
The microstructure of cyclic annealed MC-HPDC is
shown in Figure 6 comparing with the conventional As-cast 68.5
annealed sample. Discontinuous precipitates along the 360 61.2
380 59.2
grain boundaries and across the original a phase were 400 60.3
observed in conventional annealed samples. However, in 420 55.5
the cyclic annealed samples, the primary a phase
retained the similar grain size as the as-cast sample,
and the precipitates only formed within the grain precipitates comprise mostly a phase, I-phase, minor
boundaries (Figure 6(b)). No obvious coarsening could w-phase, and Mg7Zn3. Detailed characteristics of the
be found in either primary or secondary a phase. The particles precipitated in the grain boundaries were
XRD results presented in Figure 7 suggest that those studied using TEM techniques for the cyclic annealed

212—VOLUME 41B, FEBRUARY 2010 METALLURGICAL AND MATERIALS TRANSACTIONS B


Table II. Hardness Value of Cyclic Annealed MC-HPDC for the samples all were measured by the Instron testing
Mg95.99–Zn3.45–Y0.56 Alloy machine, and the results are listed in Table III. An
increase in the elongation to the point of failure along
Annealing Process Hardness (Hv) with an improvement in tensile strength were observed
360 C ~ 400 C, 1.5 h 62.2 after cyclic annealing between 360 C and 400 C across
360 C ~ 380 C, 3 h 59.1 1.5 hours for the MC-HPDC sample with YS, UTS, and
380 C ~ 420 C, 3 h 59.2 elongation to failure measurements of 148 MPa,
217 MPa, and 4.5 pct, respectively.
Because of the high-intensive shearing effect, the
MC-HPDC Mg–Zn–Y products achieved a fine uniform
Table III. Mechanical Properties of HPDC and MC-HPDC microstructure with dispersed tiny I-phase after cyclic
Mg95.99–Zn3.45–Y0.56 annealing. The yield strength of the Mg alloy depended
YS, UTS, Elongation, greatly on grain size,[11] whereas UTS was determined
Process MPa MPa pct by the amount of the defects. For the MC-HPDC
process, the samples had fine equiaxed grains, less
HPDC 111 161 2.9 porosity/hot cracks, and microstructural nonuniformity
As-cast MC-HPDC 132 179 2.8 under optimized conditions, thus showing the improve-
MC-HPDC + Conventional 131 200 3.8 ment in mechanical property compared with the HPDC
annealing at 380 C for 3 h
MC-HPDC + Cyclic annealing 148 217 4.5
process. However, because of the Y enrichment after the
between 360 C and heat treatment, many precipitated particles, including
400 C for 1.5 h I-phase, occurred in the grain boundaries (as shown in
Figure 6). Moreover, because of the close-to-zero poros-
ity, cyclic annealing can be applied to the MC-HPDC
MC-HPDC sample. The results are shown in Figure 8. samples so that I-phase can precipitate more dispersively
A selected area diffraction pattern shows 3-fold symme- in an ultra-fine size to help increase the strength of the
try in the black needlelike precipitates. It also suggests samples.
that the precipitates in the cyclic heat-treated sample
contain I-phase.
IV. CONCLUSIONS
C. Mechanical Properties of MC-HPDC Application of high-intensive shearing to the liquid
Mg95.99–Zn3.45–Y0.56 Alloy Mg–Zn–Y melt produces a uniformly fine microstruc-
Variations of hardness values for the samples sub- ture with no noticeable porosity or cavities and shows
jected to conventional and cyclic annealing are tabulated improvement in tensile properties. Application of cyclic
in Tables I and II, respectively. A fluctuation in hard- annealing is identified as a unique technique to improve
ness was observed in the conventional annealed samples, the tensile properties of the MC-HPDC Mg–Zn–Y alloy
which can be linked to the formation and dissolution of because it allows I-phase to be precipitated without
precipitates in annealed Mg–Zn–Y alloys. Table I shows coarsening the primary a-Mg with cyclic annealing.
that the hardness of the alloy decreased from 68.5 Hv at
room temperature to 59.2 Hv at 380 C annealing for
3 hours. This result reveals that solid solution occurred
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