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ScienceDirect 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:
[email protected] 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. © Published by Elsevier B.V.B.V. This is an open access article under the CC BY-NC-ND license © 2016 2016The TheAuthors. Authors. Published by Elsevier (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
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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 Keller’s 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
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Vickers Hardness (Hv)
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
80.0
Annealed A5052
75.0 70.0
Cryorolled raw A5052
65.0 60.0 10
20
30
60
90
120
Cryorolled 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.
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(a) 340
Tensile strength (MPa)
330
320
Annealed A5052
310 300
Cryorolled raw A5052
290 280
Cryorolled annealed A5052
270 260 10 20 30 40 50 60 70 80 90 100 110 120 Immersion duration in liquid nitrogen (min)
280
(b)
Yield strength (MPa)
270 Annealed Al 5052
260 250 240
Cryorolled raw Al 5052
230 220
Cryorolled annealed Al 5052
210 200 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.
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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)
(c)
(b)
(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.
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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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