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Materials Today: Proceedings 5 (2018) 4515–4522 www.materialstoday.com/proceedings

ICMPC 2017

Experimental studies on Friction stir processing of AZ31

Magnesium alloy
J.Babua*, M.Anjaiah b Anoop Mathewa.
a
Department of Mechanical Engineering, St. Joseph’s College of Engineering& Technology, Choondacherry,686575, Kerala,India.
b
Department of Mechanical Engineering, Gurunanak Institutions, Technical Campus, Ibrahimpatnam, ,501506 Telangana, India

Abstract

Friction stir processing is a solid-state technique for microstructural modification using the heat from friction and stirring. The
mechanical properties of friction stir processed AZ31 magnesium alloys can be improved due to the grain refinement of the
microstructure which makes them suitable for Superplastic forming.The parameters of friction stir processing for AZ31
magnesium alloys are studied at the three different travelling speeds: 20, 30 and 40 mm/min with two different rotation speeds
600 and 800 rpm in the present investigation.Results reveal that the smallest precipitate size is obtained at spindle speed and feed
rate combination of 800 rpm and 40mm/min. The corresponding Vickers hardness value is 63 which is around 50% higher than
that of the base metal.

© 2017 Elsevier Ltd. All rights reserved.

Selection and/or Peer-review under responsibility of 7th International Conference of Materials Processing and Characterization.

Keywords:Friction stir processing; Grain refinement; AZ31 magnesium Alloys; Hardness

1. Introduction

Magnesium alloys are replacing Aluminum alloys as, these are lightest among structural materials, for
applications in aerospace and automobile industries [1-3]. However, its lower elastic modulus and strength limits
are limitations in certain applications [ 4,5]. It is well established that a fine grain size is an essential pre-requisite
for enhancing mechanical and also for superplastic forming. An understanding of the basic metallurgical principles
underlying grain refinement and grain growth is therefore important to the development of superplasticity in
materials, which would not normally be superplastic. Several methods are available for grain refinement including
phase separation, phase transformation and mechanical working with recrystallization.

* Corresponding author.
E-mail address: jalumedi.babu@gmail.com

2214-7853© 2017 Elsevier Ltd. All rights reserved.

Selection and/or Peer-review under responsibility of 7th International Conference of Materials Processing and Characterization.
4516 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522

The imposition of mechanical working during any stage of the heat treatment makes it thermo- mechanical
process. Such methods produce the required grain size in a fewer number of processing steps. The different methods
to obtain fine grain size are: Multidirectional forging [6,7], High pressure torsion [8,9], Equal channel angular
pressing [10,11], and Friction stir processing [12-13].

Wang Zhongjun et al [14] presented the superplasticity of coarse grain AZ80 Magnesium alloy. The
temperatures and strain rates chosen were 350-4500 C, 1.31 X 10-4- 1.31 X 10-2 and obtained an elongation of 239%
at 4500 C, m value 0.49 and grain size was approximately 35 μm. The authors did not use any grain refinement
method prior to forming. Abdel- Wahab EI-Morsy et al [15] tried superplastic forming of AZ31 sheet in to
rectangular pan to evaluate superplastic behaviour by bi-axial multi dome test at different temperatures and obtained
maximum m value of 0.45 at 4000 C. Herain, Svoboda and Fedirico Vago [11] presented Superplastic behaviour of
AZ31 processed by ECAP with 4 passes and showed that the deformation to fracture improved with ECAP
processing reaching 250 % for 3500C and at strain rate of 10-4. Pan Wang et al [16] used two step superplastic
forging of semi-continuously cast AZ70 magnesium alloy with upsetting of the blanks and subsequent annealing.
Heat treated preforms were forged in to end products at the superplastic conditions. Kaifeng Zhang et al [17]
presented cavitation behaviour during superplastic deformation of hot rolled AZ31 magnesium alloy. They
examined superplastic behaviour at the temperature range of 250-4500 C. Maximum elongation obtained was 362%
for 4000 C at a strain rate of 0.7 X 10-3. Yu Xia et al [18] presented the effect of grain refinement on fracture
toughness and fracture mechanism in AZ31 magnesium alloy.

Chengqi Wang et al [19] presented an improvement in grain refinement efficiency of Mg-Zr master alloy
by friction stir processing. Tests on grain refinement revealed that the refining efficiency of Mg, 30%Zr alloy
significantly improved by FSP. This study provided a new method to develop a more efficient Mg-Zr refiner. Vit
Janik et al [20] presented the Superplastic forming ability of as-cast AZ91 Mg alloy prepared by twin roll casting.
Twin roll cast strips were tested in uniaxial tension at 325, 350 and 375 ºC, and at strain rates from 10-2 to 10-4 s-1. At
temperature 350 C and at medium strain rates the maximum elongation reached almost 200% in the direction
parallel to the strip casting.
Li Jang et al [21] presented superplastic behavior of Mg–7Y–4Gd–1Zn (wt%) alloy that was prepared by
hot extrusion technology. The alloy showed the maximum elongation of 700% at 470 °C and 1.7×10−4s−1. Kim and
Wang [22] presented Superplastic behavior of a fine-grained ZK60 magnesium alloy processed by high-ratio
differential speed rolling. They could reduce the grain size of the ZK60 alloy to 1∼2 μm through high-ratio
differential speed rolling (HRDSR) for a thickness reduction of 70% in a single pass. Low temperature
superplasticity was attained by them at 473–493K at low strain rates (5×10−4s−1) and high strain rate superplasticity
was attained at 523–553K at high strain rates (10−2s−1). The optimum superplastic temperature was found to be 553K
and tensile elongation of ∼1000% was obtained at 1×10−3s−1.

Ling-yun Wang et al presented [23] Superplastic instability of AZ31B magnesium alloy sheet and could
achieve maximum elongation of 216% and strain rate sensitivity of 0.36 at 723 K and a strain rate of 1 × 10−3s−1.
Panicker et al [24] investigated microstructural evolution and grain boundary sliding in a superplastic magnesium
AZ31 alloy. Tensile experiments on a fine-grained single-phase Mg–Zn–Al alloy (AZ31) at 673 K revealed
superplastic behavior with an elongation to failure of 475% at 1×10−4s−1 and non-superplastic behavior with an
elongation to failure of 160% at 1×10−2s−1; the corresponding strain rate sensitivities under these conditions were
reported as ∼0.5 and ∼0.2, respectively. CavaliereandDe Marco [25] investigated the room temperature and hot
tensile properties of AZ91 magnesium alloy produced by high pressure die casting after friction stir processing
(FSP). Superplastic behaviour was analysed by means of hot tensile tests in longitudinal direction. The ranges of
temperature and strain rate were 225–300°C and 10−2 to 10−4s−1, respectively.

Ramesh Babu et al [26] investigated the effect of friction stir processing on the superplastic forming of AZ31B
alloy. Strain rate sensitivity increased for friction stir processed specimens. Mohan et al [27] could achieve ultrafine
grained materials with average grain size of 0.8 μm and 0.5 μm in a rolled AZ31 alloy and a high pressure die cast
AZ91 alloy by friction stir processing. The best elongation of 1251% was achieved at a strain rate of 1×10−2s−1 and
temperature of 330 0C. Chegqi Wang et al [28] investigated the improvement in grain refinement efficiency of Mg-
Zr alloy by friction stir processing. Darras, Khraisheh et al [29] studied the friction stir processing of AZ31B-H24
 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522 4517

magnesium alloy sheets. Significant grainrefinement and homogenizationcould be achieved ina single FSPpass
leading toimproved formability. Present investigation aims to refine the microstructure of as rolled AZ31 magnesium
alloy by single pass friction stir processing. Present study also focuses on evaluation of improvement of hardness at
different processing conditions. introduce the paper, and put a nomenclature if necessary, in a box with the same font
size as the rest of the paper.

2. Experimental Procedure

2.1. Work piece Material.

AZ31 magnesium alloy of size 150 X150 X4 mm³ was used in the present study. The work piece material was
supplied by Nextgen suppliers, Mumbai in hot rolled condition. The chemical composition is shown in Table 1. The
figure 1 shows the SEM image of the rolled structure

Table.1. Chemical composition of AZ31.

Si% Mn% Fe% Ca% Cu% Ni% Ti% Al% Zn% Mg%
0.04 0.221 0.003 0.020 0.030 0.002 0.010 2.160 0.710 96.20

Fig. 1. SEM image of Hot rolled AZ31 Magnesium alloy.

2.2. Experimental details.

Experiments were conducted with High speed steel tool with tool depth of 1 mm, Tool shoulder diameter of 18
mm and Tool pin diameter of 6 mm on a vertical milling machine at Annamalai University at Chennai as shown in
Fig.2 The spindle speeds of 600 & 800 rpm and feed rates of 20, 30, 40 mm/min were chosen for the study as
tabulated in Table 2. Hardness of Friction stir samples were measured with Vickers hardness testing machine at St.
Joseph’s College of Engineering & Technology, Palai. Hardness tests were carried out with a load of 5kg with a
dwell period of 10 seconds.
4518 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522

Fig. 2. Experimental setup

Table 2. Input parameters
Expt. No Spindle speed Feed rate
(rpm) (mm/min)
1. 600 20
2. 600 30
3. 600 40
4. 800 20
5. 800 30
6. 800 40

3. Results and discussion

3.1. Microstructural studies.

In order to reveal the microstructural changes with the friction stir processing, SEM images of all the samples were
analysed
SEM images reveal the formation of fine precipitates of aluminium and magnesium at the grain boundaries. As
present study deals with the single pass friction stir processing, smallest size of the precipitates are noted for each
combination of spindle speed and feed rate are tabulated in Table.3. These precipitates accumulate at the grain
boundaries and pin them. Subsequent passes results in the formation of precipitates at the grain boundaries and
results in the formation of ultrafine grains as shown in Fig.3[30]. SEM images representing the formation of
precipitates and their sizes for these combinations are shown in Fig.4 (a) (b).
 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522 4519

Fig. 3. Schematic illustration of the evolution of ultrafine structure [30].

Table 3. Size of smallest precipitate obtained from friction stir processed AZ31

Experiment. Spindle speed Feed rate Smallest size of the

No (rpm) (mm/min) Precipitate(μm)
1 600 20 1.27

2 600 30 1.00

3 600 40 0.89

4 800 20 1.00

5 800 30 0.93

6 800 40 0.80

From the Table.3, it can be observed that high spindle speed and feed rate combination results in small size
of the precipitates. It is found that size of the precipitates decreases with increase in travel speed. This is due to the
high travel speed causing the distribution of precipitate particles more uniformly than at low travel speed [30].

It is also found that, the high rotation speed generates fine precipitates compared to low rotation speed
because increase in rotation speed causes higher temperatures resulting more heat input. But continued increase in
rotation speed may generate higher temperatures above the recrystallization temperature. This can result in grain
growth and cause reduction in mechanical properties. So, an appropriate rotation speed threshold is, necessary to
produce enough heat for plastic deformation which result in reduction of porosity and fine grain size in the friction
stir zone.
4520 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522

Higher temperatures leading to larger grain size can be minimised, by using additional cooling during
friction stir processing. Recent works of Arora et al [30] presented the cooling effect on the grain size evolution in
friction processing of Magnesium based AE42 alloy. Lower cooling temperatures (-10 ̊ C) could evolve finer grain
by restricting the time and energy available for the growth of recrystallized nuclei. They observed that the grain
structure became coarser with corresponding hardness value reduction in multi-pass FSP at a higher cooling
temperature of 300 C. It is believed that the presence of fine precipitate particles contributes to the evolution of fine
grain structure. But slower cooling rates provide more time for the growth of recrystallized fine nuclei which result
in comparatively coarser grain structure.

Fig. 4 SEM images representing smallest precipitation sizes obtained from friction stir processing of AZ31 Mg alloy processed
at different spindle speeds and feed rates (a) 600 rpm 20 m/min (b) 600 rpm 30 m/min (c) 600 rpm 40 m/min (d) 800 rpm
20m/min (e) 800 rpm 30m/min (f) 800 rpm 40m/min
Fig.4 (c) (d) (e) and (f) shows the fragmented precipitates produced in the nugget zone of FSP AZ31. The FSP
process parameters such as spindle speed and number of FSP passes significantly affect the size and distribution of
in-situ precipitate particles. It is observed that single pass FSP of AZ31 alloy resulted in generation of in-situ
precipitates with smallest size of the precipitate, 0.80 µm which can get further refined during double pass FSP and
also in subsequent passes. It is concluded that the presence of fine in-situ precipitates contributes to the evolution of
the ultra-fine grain structure through particle pinning of the fine nuclei.

The major part of the heat generation in the FSP process is the frictional heat by the FSP tool shoulder. Therefore,
FSP tool rpm is one of the key parameters which decide the amount of heat input into the FSP zone. Future studies
can be done on multi-pass friction stir processing with additional cooling to obtain finer grains.
 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522 4521

3.2. Hardness

The initial hardness of the base material obtained by Vickers hardness is 41. The hardness test is conducted with
5kg load and a dwell time of 10 seconds. Table 4 shows the average hardness of nugget zone of the FSP processed
AZ31 magnesium plate. Variation of hardness value with spindle speed and feed rates is shown in Fig.5.

Table 4. Average hardness obtained at nugget zone at different processing conditions

Expt. No Spindle speed (rpm) Feed rate Average hardness (Vickers)
(mm/min)
1 600 20 48.3

2 600 30 51

3 600 40 56.6

4 800 20 59.3

5 800 30 61

6 800 40 63

It is found that the average hardness value increases after the single pass FSP with high spindle speed and
feed rate combination. Higher hardness is a result of finer precipitates in the microstructure, which increases the
mechanical properties. The smallest precipitate size obtained is 0.80 µm at spindle speed and feed rate combination
of 800 rpm and 40 mm/min. The corresponding hardness value is 63. Hardness value increased by around 50% in
friction stir processing.

Fig.5. Comparison of hardness values at different regions and different combinations of spindle speed and feed rate.

4. Conclusions

Present study presents the friction stir processing of AZ31 magnesium alloy at different spindle speeds and
feed rates for the grain refinement and hardness. The process results in superior mechanical properties and facilitates
Superplastic forming. Following conclusion are drawn from the present study.
• It is found that fine precipitates are obtained with increase in travel speed.
• This is due to the high travel speed causing more distribution of precipitate particles than at low travel
speed.
• It is also found that, the high rotation speed produces smaller precipitates than the low rotation speed.
• This is due high rotational speed causing higher temperatures result in more heat input.
• It is observed that single pass FSP of AZ31 alloy results in generation of in-situ precipitates with smallest
particle size of the order of 0.8 µm which can get further refined during double pass FSP and also in
subsequent passes.
4522 J.Babu et al./ Materials Today: Proceedings 5 (2018) 4515–4522

• The smallest precipitate size is obtained at spindle speed and feed rate combination of 800 rpm and
40mm/min. The corresponding Vickers hardness value is 63 which is around 50% higher than that of the
base metal.

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