M A TE RI A L S CH A RACT ER IZ A TI O N 59 ( 20 0 8 ) 3 8 5 3 8 9

Effect of chip size on mechanical property and microstructure

of AZ91D magnesium alloy prepared by solid state recycling

Maoliang Hu, Zesheng Ji, Xiaoyu Chen, Zhenkao Zhang

College of Materials Science and Engineering, Harbin University of Science and Technology, Harbin 150040, China

AR TIC LE D ATA ABSTR ACT

Article history: In this study, different kinds of AZ91D magnesium alloy chips were prepared by solid state
Received 3 September 2006 recycling. Mechanical properties and microstructures of the recycled specimens were
Received in revised form investigated. Various microstructural analyses were performed using the techniques of
8 February 2007 optical microscopy, scanning electron microscopy and oxygen-nitrogen analysis.
Accepted 19 February 2007 Microstructural observations revealed that all the recycled specimens consisted of fine
grains due to dynamic recrystallization. The oxide precipitate content is closely related to
Keywords: the recycled chip size. Accumulated oxygen concentration linearly increases with the total
AZ91D magnesium alloy surface area of the machined chips in the recycled specimens. Ambient oxide in the recycled
Solid state recycling specimen contributes to a higher ultimate tensile strength and a higher elongation to
Chip size failure; however, excessive oxide in the recycled specimen may adversely affect the
Mechanical property elongation to failure.
Microstructure 2007 Elsevier Inc. All rights reserved.

1. Introduction energy required for more efficient recovery. Expenditures

Magnesium alloys are the lightest alloys used as structural
metals, combining many advantages such as high specific
stiffness, high specific strength, good dimensional stability
and machinability. For these reasons, the demand for magne-
sium alloys is increasing rapidly. A large amount of waste in
the form of chips and discards is produced in the machining
process of products made by die casting and rolling. An
important requirement to sustain the development of magne-
sium alloys is to recycle the chips and discarded or recycled
parts. At present, many factories manufacturing magnesium
alloys pay significant attention to these matters [15].
Using the common recycling methods, magnesium alloy
chips and scrap are remelted, whereby some of the alloy is
recovered and reutilized in the production process. During the
melting/recycling of the chips and scraps, a lot of magnesium
alloy is lost as a result of oxidation and the costs of labor and
associated with environmental protection further increase the
general costs. A solid recycling process is proposed as a new
method of recycling magnesium alloys. In the solid recycling
process, chips and scraps are recycled by consolidation using
plastic deformation processes such as cold or hot pressing
followed by hot extrusion [69]. Furthermore, solid recycled
magnesium alloys show high strength due to grain refinement
and homogeneous dispersion of oxide precipitates.
It has been reported that oxide precipitates in the recycled
specimen leads to a compromise of the ductility, especially at
elevated temperature [10,11]. Oxide precipitation is closely
related with recycled magnesium alloy chip size. Oxidization
increases with an increase in surface area. In previous studies,
no quantitative evaluations were made of the effects of chip size
on the mechanical properties and microstructure of the recycled
specimens. It is judged important to investigate this relation-
ship. Hence, in this paper, different kinds of magnesium alloy

Corresponding author. Tel.: +86 451 86392557; fax: +86 451 86674840.
E-mail address: humaoliang309@yahoo.com.cn (M. Hu).

1044-5803/$ see front matter 2007 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2007.02.002
386 MA TE RI A L S CH A R A CT ER IZ A TI O N 59 ( 20 0 8 ) 3 8 53 8 9

Fig. 1 Chips and compact billet: (a) recycled chips 1; (b) recycled chips 2; (c) recycled chips 3; (d) compact billets.

chips were recycled and the mechanical properties and micro- testing was done in a WDW-10 electron universal strength
structures of these specimens were investigated. tester. Microstructures of the specimens were observed by
OLYMPUS-GX71-6230A optical microscope (OM). The speci-
mens were polished with a Cr2O3 polishing medium and
2. Materials and Experimental Procedures etched in a 4% aqueous nitric acid solution. Fractures were
characterized on a FEI-SIRION scanning electron microscope
The AZ91D magnesium alloy is widely used. Machined chips (SEM). The oxygen content of the recycled AZ91D chips was
of this alloy were prepared by machining an ingot in a lathe, determined using an EMGA-620W oxygen-nitrogen analyzer.
Fig. 1. Machined chips were kept clean in the turning process.
They were loaded into a 40-mm diameter cylindrical container
and cold-pressed. The pressure and the holding time were 3. Results and Discussion
300310 MPa and 35 s, respectively. Following the cold-press
process, the container with the formed billet was heated at 3.1. Recycled AZ91D Magnesium Alloy
673 K for 20 min. Finally, hot extrusion was carried out at an
extrusion ratio of 25:1 to produce an 8-mm diameter bar. For The virgin industrial AZ91D magnesium alloy microstructure
comparison, extrusions were processed from as-received consists of (Mg) solid solution and phase (Mg17Al12), shown
AZ91D magnesium alloy ingot under the same conditions as in Fig. 2. The phase is distributed discontinuously along the
the extrusions from three kinds of machined chips. Recycled
chips with the sizes of (46) (3.54.5) (1.451.55) mm, (10
16) (1.82.2) (0.480.52) mm and (58) (1.82.2) (0.18
0.22) mm are called recycled specimen 1, recycled specimen
2 and recycled specimen 3, respectively, Table 1.
Standard tensile specimens oriented plane perpendicular
to the extrusion direction were prepared to determine the
tensile strength and elongation at room temperature. The

Table 1 Size of recycled chip specimens

Recycled Length/ Width/ Thickness/
specimen mm mm mm

1 46 3. 54.5 1.451.55
2 1016 1.82.2 0.480.52
Fig. 2 Microstructure of the as-cast AZ91D magnesium alloy
3 58 1.82.2 0.180.22
specimen.
 M A TE RI A L S CH A RACT ER IZ A TI O N 59 ( 20 0 8 ) 3 8 5 3 8 9
Fig. 3 Microstructure of recycled AZ91D magnesium alloy
chip 1.
grain boundaries. The mean grain size is very coarse (about
200 m) [12]. It is well known that a high dislocation density
results from the machining process [13], Fig. 3. Severe plastic
strain and high dislocation density promote recrystallization.
As described above, the machined chips were pressed to
form a compact 40-mm diameter billet. The densities of the
three kinds of billets after cold-pressing were 1.56 g/cm3,
1.51 g/cm3 and 1.49 g/cm3 for recycled specimens 1, 2 and 3,
respectively. The surface of the chips exhibited some breaking
and bonding. Large numbers of voids and cracks could be seen
and relative densities of 87%, 84% and 83%, respectively, were
measured. These values can be contrasted with a density of
the fully condensed solid of 1.79 g/cm3. However, the fact that
variability is seen for the different chips means that metal-
lurgical bonding of the chips is not yet complete, indicating
the need for an additional consolidation process. Hot extru-
sion, involving high compressive and shear forces at high
temperature, was thus used for producing more complete
consolidation of the recycled chips.
3.2. Mechanical Properties
Fig. 4 shows ultimate tensile strength and elongation to
failure at room temperature for an as-cast specimen, the
Fig. 4 Ultimate tensile strength and elongation to failure of
AZ91D magnesium alloy at room temperature. Data are
presented for an as-cast specimen, an as-extruded specimen
and the three recycled specimens.
387
reference as-extruded specimen and the three recycled
specimens. Recycled specimen 1 shows a good combination
of higher ultimate tensile strength of 340 MPa and elongation
to failure (10.5%), compared to those of the as-cast specimen.
These values are nearly the same as those of the as-extruded
specimen. The ultimate tensile strengths of recycled speci-
mens 2 and 3 are slightly lower; however, their elongations to
failure are significantly lower than those of recycled speci-
men 1. The three recycled specimens are distinguished by
chip size. Therefore, in view of the ready oxidation of the
magnesium alloys in the machining process, the oxygen
content is different and may be responsible for the differ-
ences observed.
Oxide precipitation was primarily introduced from the
machined chip surface. The chip surface area is expected to be
closely related to the chip size. The relationship between the
accumulated oxides and the total surface area of the
machined chips in the recycled specimen can be estimated.
If it is assumed that the shape of the machined chips is cubic,
the relationship can be calculated by using Eq. (1).
2ab bc ac
S 1
abc
where S is the total surface area per unit volume, a is the chip
length, b is the chip width and c is the chip thickness. Fig. 5
shows the relationship between the accumulated oxygen
concentration determined for the recycled specimens and
the total surface area of the chips in the recycled specimens
per unit volume. The accumulated oxygen concentration
increases linearly with the total surface area. This tendency
agrees well with that measured for repeatedly re-extruded
magnesium alloy specimens [14].
3.3. Microstructure
Microstructures of three kinds of recycled specimens and the
reference specimen are shown in Fig. 6. All micrographs are for
the plane perpendicular to the extrusion direction. Individual
machined chips were not clearly observed and none of the
specimens exhibited cracks or voids. The equiaxed grains
formed high angle boundaries; features of the deformation
processing are clearly seen. Few grains did not happen to
recrystallize but exhibited an elongated fiber-like structure.
Fig. 5 Relationship between oxygen concentration and total
surface area volume for a reference specimen and the three
recycled specimens.
388 MA TE RI A L S CH A R A CT ER IZ A TI O N 59 ( 20 0 8 ) 3 8 53 8 9

Fig. 6 Microstructure of AZ91D magnesium alloy specimen (a) recycled specimen 1; (b) recycled specimen 2; (c) recycled
specimen 3; (d) reference specimen.

Because the 673 K extrusion temperature was higher than work-softening occurred simultaneously. Moreover, the stack-
0.5Tm (Melting temperature), the magnesium alloy was in a ing fault energy of magnesium alloy is low (about 78 mJm 2)
condition of high plasticity such that work-hardening and [15], allowing. dynamic recrystallization and easy grain

Fig. 7 Fractographs of AZ91D magnesium alloy specimens (a) recycled specimen 1; (b) recycled specimen 2; (c) recycled
specimen 3; (d) reference specimen.
 M A TE RI A L S CH A RACT ER IZ A TI O N 59 ( 20 0 8 ) 3 8 5 3 8 9
refinement. The grain sizes of recycled specimens 1, 2 and 3,
and the reference specimen were 11 m, 22 m, 25 m and
11 m, respectively.
The strength of recycled specimen 1 was higher than that
of the reference specimen, Fig. 4, and the grain size was almost
equal to that of the reference specimen, Fig. 6a and d.
However, these specimens differed in oxygen content, thus
the higher strength for the recycled specimen. When the
oxygen content continued to increase, such as in recycled
specimens 2 and 3, the elongation to failure decreased
significantly. One reason for this was the increased grain
size; another contributor was the increased oxide precipita-
tion. During tensile testing, the matrix adjacent to the oxide
precipitates might be prone to form micro-voids, which can
coalesce into large cracks and result in lower elongation.
Fractographs of the three kinds of recycled specimens and
the reference specimen are shown in Fig. 7. All of the samples
had a similar fracture mechanism. In the process of tensile
testing, the specimens exhibited no tendency to neck and
fractured by brittle rupture. Short, crooked tearing edges were
observed between fracture planes, while concavities and
micro-cracks could be seen on the fracture surfaces. Overall,
the fractures exhibited the characteristics of quasi-cleavage. A
large number of micro-cracks could be seen in the fracture
surface of the three recycled specimens but the fracture
surface of the reference specimen exhibited no micro-
cracking.
4. Conclusions
Recycled specimen 1 prepared with chip dimensions of (4
6) (3. 54.5) (1.451.55) mm showed a good combination of
higher ultimate tensile strength (340 MPa) and higher elonga-
tion to failure (10.5%), compared to those of an as-cast
specimen. These values were almost the same as those of
the as-cast and extruded specimen. In general, it was observed
that oxides in the recycled specimen contributes to higher
tensile strength and elongation to failure, whereas excessive
oxide can adversely affect the elongation to failure. A small
amount of oxide precipitation appears to result in dispersion
strengthening but excessive oxide may be prone to cause the
early development of micro-voids and contribute to lower
elongation.
It is worth noting that the AZ91D chips in this study were
used directly to prepare the rods without melting. The
experimental materials exhibited a good combination of
strength and plasticity, implying that solid-state recycling is
an efficient method for the recycling of magnesium alloy
chips.
Acknowledgement
This research was funded by a broad scholar scientific research
program of Heilongjiang educational office (1151hz002) and
the National Natural Science Foundation of China (50674038).
389
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