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Procedia Chemistry 19 (2016) 241 246

5th International Conference on Recent Advances in Materials, Minerals and Environment

(RAMM) & 2nd International Postgraduate Conference on Materials, Mineral and Polymer
(MAMIP), 4-6 August 2015

Effect of immersion duration in liquid nitrogen for cryorolled

A5052 aluminium sheet alloy
N. M. Anas, W. L. Quah, H. Zuhailawati, A. S. Anasyida
School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang,
Malaysia.
*Corresponding author. E-mail address: anasyida@usm.my Tel.: +604 599 5216

Abstract

In this paper the effect of immersion duration on mechanical properties of cyrolled and non-cryorolled A5052 aluminium sheet
alloy were studied. The sheets with and without annealing were rolled up to 30 % reduction at liquid nitrogen temperature. The
mechanical behaviour of the sample were evaluated through hardness and tensile tests performed at room temperature. The
evolution of microstructure was investigated using optical microscopy (OM). The optimum immersion duration of A5052 Al sheet
alloy was 60 minutes as the hardness, tensile and yield strength were the highest for annealed sample with and without directly
cryorolled. All the cryorolled samples showed elongated grain.

2016
2016TheTheAuthors. Published
Authors. by Elsevier
Published B.V.B.V.
by Elsevier This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia.
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia
Keywords: Cryorolling; 5052 Aluminium alloy; annealing

1. Introduction

Aluminum alloys are broadly utilized for manufacturing high strength and light weight structures in automotive
and aerospace applications. The non-heat treatable wrought Al-Mg alloys (5xxx) are utilized for components that
require greater design efficiency, better welding attributes, great superplasticity, high resistance to corrosion, and
relatively high strength-to-weight ratio coupled with minimum cost1.
In order to obtain sheets of ultrafine-grained Al alloys in large amount for structural applications, the conventional
rolling may be a viable choice. However, it is hard to create UFG structure particularly for aluminium through
conventional rolling process, because of its high stacking fault energy and the decreased driving force available for

1876-6196 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia
doi:10.1016/j.proche.2016.03.100
242 N.M. Anas et al. / Procedia Chemistry 19 (2016) 241 246

recrystallization2. Cryorolling has been identified as one of the potential routes to produce ultrafine-grained materials
from its bulk metals and alloys in order to hinder these difficulties.
Cryorolling is a simple low-temperature rolling process in which the low temperature is maintained by liquid
nitrogen3. It is a unique mechanical deformation process at cryogenic temperatures by which high strength and
ductility combinations can be achieved. In cryorolling process, the material cools, its molecular structure contracts
and hence there is entanglement of dislocations near the grain boundaries4. The suppression of dynamic recovery in
the materials due to rolling at the cryogenic temperature causes density of accumulated dislocations to reach a higher
steady state level, which in turn acts as a driving force for the formation of sub-microcrystalline or ultrafine grain
structures (UFG) during subsequent annealing treatment 5.
The immersion duration of A5052 Al sheet alloy in the liquid nitrogen affects the amount of contraction of
aluminium matrix and hence contributed to the improvement of hardness and strength value. Therefore, selection of
suitable immersion duration is essential to obtain better mechanical properties of A5052 sheet alloy. In this study, the
immersion duration was studied in order to determine optimum duration for dipping A5052 Al sheet alloy in the liquid
nitrogen.

2. Experimental

A commercial A5052 Al sheet alloy used for structural applications was chosen for the present work. The
chemical compositions of Al alloy are 1.83 wt% Mg, 0.37 wt% Si, 0.33 wt% Fe, 0.14 wt% Cr, 0.01 wt% Ga, 0.007
wt% Ni, 0.004 wt% Zn and Al balance. The A5052 Al sheet alloy plates were machined into the dimensions of 1.2
mm x 20 mm x 50 mm. The materials with different condition were investigated to study the effect of annealed,
cryorolled and combination of annealed and cryorolled at various immersion duration in liquid nitrogen.
The A5052 Al sheet alloy was annealed at 300 C for 2 h. The specimens of raw A5052 Al sheet alloy and in
annealed condition were cryorolled up to 30% thickness reduction.
Initially, the samples were dipped in liquid nitrogen at different immersion duration such as 10 min, 20 min, 30
min, 60 min, 90 min and 120 min. To investigate the effect of immersion duration on the mechanical properties of
A5052 Al sheet alloy, microhardness and tensile tests were carried out on the cryorolled and non-cryorolled samples
dipped in liquid nitrogen for the different immersion duration times. Vickers hardness testing was performed at room
temperature using 100 gf load and a dwell time of 10 seconds. To obtain Vickers hardness, minimum of five readings
were taken on the well-polished surface parallel to the rolling direction. For tensile tests, the specimens were machined
into the ASTM subsize specimen of 25 mm gauge length. Uniaxial tensile tests were conducted with the initial strain
rate of 1 mm/min on Instron Universal Testing Machine operating at a constant crosshead speed. .
Microstructural characterization of the A5052 Al sheet alloy samples before and after rolled at cryogenic
temperatures were subjected to microscopic studies. The microstructures of the sample were revealed by chemical
etching with Kellers reagent and were examined using the optical microscope.

3. Result and discussion

3.1. Hardness properties

Fig. 1 shows the hardness properties of raw, annealed, cryorolled raw, and cryorolled annealed of A5052 sheet
alloy samples at different sample immersion durations in liquid nitrogen temperature prior to each cryorolling pass.
When the samples (raw material, annealed, cryorolled) immersion duration in liquid nitrogen prior cryorolling process
was increased from 10 minute to 30 minute, significant improvement in the hardness for all the samples were observed.
The improvement in hardness is due to prolong immersion duration in liquid nitrogen which increase the volume
contraction of aluminium matrix causing the shrink of the microporosities and voids inside the sample 6. The hardness
of the samples (annealed and cryorolled annealed) achieved the highest hardness at immersion duration of 60 minutes
and the hardness dropped as the immersion duration increase to 120 minute. For the high hardness value obtained at
60 minute immersion duration, it is considered the suitable immersion duration because all the microporosities and
 N.M. Anas et al. / Procedia Chemistry 19 (2016) 241 246 243

voids inside the sample having enough shrinkage and thus, decreasing the volume of the material and restored the
energy. However, a contradicted result was obtained for raw sample and sample directly cryorolled without subjected
to annealing process which achieved the highest hardness of 72.7 Hv and 82.9 Hv respectively at 120 minute
immersion duration. This might be due to higher times required for the microporosities and void of direct cryorolled
samples to shrink to obtain highest hardness as compared with the annealed sample. In annealed sample, during
annealing process the atom in the sample rearranged themselves, thus less void was left behind and shorter time is
required for material to achieve volume contraction.

85.0 Raw A5052

Vickers Hardness (Hv)

80.0

75.0 Annealed
A5052
70.0
Cryorolled raw
65.0 A5052

60.0 Cryorolled
10 20 30 60 90 120 annealed A5052
Immersion duration in liquid nitrogen (min)

Fig. 1. Variation in Vickers hardness of A5052 alloy samples at various sample immersion duration.

3.2. Tensile properties

The tensile and yield properties of annealed, cryorolled (CR) and cryorolled annealed A5052 Al alloy samples at
different sample immersion durations in liquid nitrogen prior to cryorolling pass are shown in Fig. 2. As the sample
immersion duration in liquid nitrogen during cryorolling increases from 10 min to 30 min, tensile and yield strength
of annealed, cryorolled raw A5052, and cryorolled annealed A5052 increases significantly follow the hardness trend.
There are also studied have reported that 6063 Al sheet alloy7 and A7075 Al sheet alloy8 showed improved in
hardness, yield strength and ultimate tensile strength. The improvement of tensile and yield strength is due to increase
amount of contraction of Al matrix. As the immersion duration in liquid nitrogen increase to 60 min, all the samples
have the highest tensile and yield strength. The tensile and yield strength of the samples decreased as the immersion
duration increase up to 120 min. Thus, the sample immersion duration for A5052 Al sheet alloy prior to each
cryorolling pass was set at 1 hour due to the highest hardness and tensile achieved for all the samples.
244 N.M. Anas et al. / Procedia Chemistry 19 (2016) 241 246

(a) 340
330

Tensile strength (MPa) 320

Annealed A5052
310

300
Cryorolled raw
290 A5052

280
Cryorolled
270 annealed A5052

260
10 20 30 40 50 60 70 80 90 100 110 120
Immersion duration in liquid nitrogen (min)

(b) 280

270

260 Annealed Al
Yield strength (MPa)

5052
250

240 Cryorolled
raw Al 5052
230

220 Cryorolled
annealed Al
210
5052
200
10 20 30 40 50 60 70 80 90 100 110 120
Immersion duration in liquid nitrogen (min)

Fig. 2 Variation in tensile strength and yield strength values of A5052 alloy samples at various sample dipping durations.

3.3. Microstructure

The samples with 60 minutes immersion duration in liquid nitrogen were chosen due to highest hardness value.
The optical micrograph of the raw sample and annealed sample with immersion duration of 1 hour in liquid nitrogen
before cryorolling is shown in Fig.3 (a) and (b) respectively. The microstructure showed the presence of equiaxed
grains. As shown in Fig. (b), the microstructure of A5052 Al sheet alloy shows coarse grains because the sample
underwent annealing process at 300 C for 2 hours.
 N.M. Anas et al. / Procedia Chemistry 19 (2016) 241 246 245

Fig. 3 (c) and (d) show the optical microstructure of the cryorolled raw and cryorolled annealed sample after
cryorolling process up to 30% reduction. The cryorolled samples exhibited severely deformed grains which are
elongated along the rolling direction. This deformation causes the increase of dislocation density with plastic
deformation and reduces the grain size. The average distance between dislocations decreased and dislocations start
blocking the motion of each other. Thus, the hardness, tensile and yield strength increasing as the result of strain
hardening.

(a) (b)

(c) (d)

Fig. 3 The optical microscope of (a) raw A5052 Al sheet alloy (b) annealed A5052 Al sheet alloy (c) cryorolled raw A5052 Al sheet
alloy and (d) cryorolled annealed A5052 Al sheet alloy.

4. Conclusion

Cryorolling is a simple low temperature processing route and requires a relatively lower load to induce severe
strain for producing the ultrafine structural features in the materials. The hardness, tensile and yield strength values of
all the samples shows improvements when the immersion duration is increased up to 60 minutes. The cryorolled
sample of A5052 Al sheet alloy produce elongated grains due to grain deformation and expected to produce subgrains.
Therefore, the suitable immersion duration is 60 minutes due to excellent mechanical properties.
246 N.M. Anas et al. / Procedia Chemistry 19 (2016) 241 246

Acknowledgements

The authors gratefully thank Universiti Sains Malaysia for providing the fund for this study under RU grant
(1001/PBahan/814197).

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