Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound

Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound

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Materials Today: Proceedings xxx (xxxx) xxx

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Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound Olusoji O. Ayodele a,⇑, Mary A. Awotunde a, Adewale O. Adegbenjo a, Mxolisi B. Shongwe b, Babatunde A. Obadele a, Peter A. Olubambi a a b

Centre for Nanoengineering and Tribocorrosion, School of Mining, Metallurgy and Chemical Engineering, University of Johannesburg, Johannesburg 2092, South Africa Institute for Nanoengineering Research, Department of Chemical, Metallurgy and Materials Engineering, Tshwane University of Technology, Pretoria 0001, South Africa

a r t i c l e

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Article history: Received 18 September 2019 Received in revised form 14 October 2019 Accepted 26 December 2019 Available online xxxx Keywords: Heating rate Vickers microhardness Nickel aluminide Mechanical properties Densification

a b s t r a c t This present study revealed the synthesis and heating rate effect on the mechanical attributes of spark plasma sintered NiAl intermetallic compound. The milled specimen was consolidated by field assisted sintering technique (SPS), morphology of the specimens was determined using the scanning electron microscope. The microstructures of the sintered NiAl that was carried out between the heating rates of 50 to 150 °C/min showed the presence of micro pores. The hardness value (Vickers microhardness) of the specimens was found to increase while the heating rate increases. Furthermore, highest hardness value of 555.4 HV0.1 was recorded for the sintered pellet possessing the heating and cooling rate of 150 °C/min. In addition, the densification of the sintered specimen (150 °C/min heating rate) was measured as 96.2%. Ó 2020 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the scientific committee of the 2nd International Conference on Recent Advances in Materials & Manufacturing Technologies.

1. Introduction Remarkable attributes of intermetallic compounds have made them functional and desirable in the industries. On account of their astonishing properties such as high thermal conductivity, good corrosion resistance, high strength and excellent melting point [1,2]. Intermetallic compounds have been widely used in various industries, for instance as turbine blades in the aerospace because they possess relevant thermo-mechanical attributes [3]. However, the use of this material has been restricted, attributable to poor fracture toughness and ductility at ambient temperature [4]. Investigation on how to enhance the attributes of the intermetallic compound have been reported and some of these method includes second phase strengthening, grain refinement and alloying [5]. Recently, powder metallurgy routes have been utilized to synthesis nickel aluminide (intermetallic compound) because of their flexibility, economical and near-net shapes production [6]. This method entails the combination of metal powders (mixing or milling) in order to manufacture several components. Amongst the powder metallurgy techniques are traditional methods (hot ⇑ Corresponding author. E-mail address: [email protected] (O.O. Ayodele).

pressing and isostatic pressing, etc.), microwave sintering and spark plasma sintering [7]. Fast assisted sintering technique or spark plasma sintering is being regarded as a novel consolidating approach due to their rapid heating rate and densification. The sintering technique entails the utilization of pulsed electric current and pressure for effective consolidation of metal powders [8]. SPS has recently been reported to be an effective technique for fabricating a variety of titanium based alloys. Owing to the extremely fast heating and cooling rates during spark plasma sintering, the desired phases and grains are easily controlled, even when sintering materials with different compositions. However, this research work investigated the synthesis and heating rate effect on the mechanical characteristics of spark plasma sintered NiAl intermetallic compound. 2. Experimental Pure nickel powders with the purity of 99.5% and average particle size of 3.0 µm, provided by WearTech Limited. Also as received aluminum powder with average particle size of 25 µm (99.8% purity) delivered by TLS Technik GmbH (Germany) were used as the starting powders. Nickel and aluminum powders were weighed with equal stoichiometric ratio of 50 wt% in a dry

https://doi.org/10.1016/j.matpr.2019.12.298 2214-7853/Ó 2020 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the scientific committee of the 2nd International Conference on Recent Advances in Materials & Manufacturing Technologies.

Please cite this article as: O. O. Ayodele, M. A. Awotunde, A. O. Adegbenjo et al., Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2019.12.298

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environment. The powders were placed into a 250 ml stainless steel vials with inner diameter of 100 mm. Two ball sizes (3 mm and 7 mm) were used as grinding media. Dissimilar ball sizes were employed in order to avert cold welding of the particles as a result of overheating and to accelerate the contact energy attainable by the powder particles [9]. Low energy ball milling (LEBM, Retsch PM 100, Germany) was employed for milling of the powders. This was carried out in the manner that would allow the machine (LEBM) begins and stop at every 10 min, in order to avoid overheating. The powders were milled for 6 h with BPR of 10: 1. Morphology of the samples was characterized through field emission scanning electron microscopy (FESEM) furnished with energy dispersive X-ray spectrometry (EDX). The analysis of crystalline

phases and structural identification of the sintered samples were carried out using X-ray diffractometer (Rigaku, XRD) by employing Cu-Ka radiation (ƛ = 0.154). This was done at the speed of 0.500 deg/min over the angular range of 10–90°. The milled powder was weighed in a dry environment and fabricated using SPS, in a graphite die. The milled powder was consolidated in vacuum using the optimized parameter: sintering temperature of 1000 °C, pressure of 50 MPa and heating rate between 50 °C/min and 150 °C/min. The sintered bulk composite discs retrieved from the SPS were sandblasted, ground and polished to remove the graphite from the composites and to prevent surface contamination. The density of the sintered composites was determined in accordance with Archimedes concept and relative density of the samples was

Fig. 1. SEM images of the starting and admixed powders: (a) Al, (b) Ni, and (c) NiAl.

Fig. 2. SEM images of the sintered samples at different heating rate: (a) 50 °C/min, (b) 100 °C/min, and (c) 150 °C/min.

Please cite this article as: O. O. Ayodele, M. A. Awotunde, A. O. Adegbenjo et al., Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2019.12.298

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calculated with respect to the theoretical density. Vickers microhardness test was achieved using an InnovaTest Falcon 500, at ambient temperature on a polished specimen, using 100 gf as the load for the period of 10 s. In addition, average value of the indentations was recorded after five indentations were taken across the specimen surface.

3. Results and discussion The SEM micrograph of Al powder was represented in Fig. 1(a). It has spherical and non-porous particles, showing some clustered satellites. Fig. 1(b) illustrates the SEM image of Ni particles consisting of a sticky and irregular shape. The SEM image of the

Fig. 3. XRD pattern of the sintered NiAl at different heating rates: (a) Sample A at 150 °C/min, (b) Sample B at 100 °C/min, and (c) Sample C at 150 °C/min.

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NiAl powder obtained through the mixture of Ni and Al powders was represented in Fig. 1(c). The EDX spectrum of the admixed NiAl was represented in Fig. 1(d). It consists of Al and Ni particles. Fig. 2 depicts the microstructures of the sintered NiAl at heating rate between 50 and 150 °C/min. Fig. 2(a) shows the sintered NiAl at 50 °C/min revealing the presence of micro pores. This suggests the reason for its relative density at 94.9%. Fig. 2(b) shows the sintered NiAl at 100 °C/min, showing micro pores in its microstructures. The pores are much bigger as compared to the microstructres of the sintered NiAl at 50 °C/min. The sinter density of this sample was found to be 90.8%. However, the microstructures of the sintered NiAl at the heating rate of 150 °C/min (Fig. 2(c)) also revealed the presence of micro pores. This also indicates the reason for its high relative density at 96.2%. We noticed that the increase from 50 °C/min to 100 °C/min (heating rate) could have caused more porosity in the sintered sample, and further increase in the heating at 150 °C/min improved the microstructures. The XRD analysis of the sintered NiAl with the heating between 50 and 150 °C/min was shown in Fig. 3. It was observed that heating rate increased while the peak intensity decreased. NiAl peaks were observed to be the dominant peaks in the sintered NiAl pattern. NiAl can be noticed at 2h = 30.6, 44.1, 54.76, 64.2, and 81.5 which matches the planes (1 0 0), (1 1 0), (1 1 1), (2 0 0), and (2 1 1). Fig. 4 represents the densification and the Vickers hardness values of the consolidated NiAl at different heating rates. The densfication of the consolidated NiAl between 50 °C/min and 150 °C/min heating rate were measured as 94.9%, 90.7% and 96.2%. This indicates that the densification decreased as the heating rate was increased for the consolidated sample between 50 °C/min and 100 °C/min. This is could be due to adequate time for neck formation and particle bonding at lower heating rate [10]. Furthermore, we noticed a slight increase in densification, supposedly due to the increase in heating rate (150 °C/min). Nevertheless, this a bit contrary to what has been reported in the literature. According to Lavish et al [11], higher heating causes the formation of large thermal gradients which allow the sinterability of the outer region of the sample before the inner region, thereby resulting into porosity.

Fig. 4. Plot of the microhardness and relative density against the heating rates of the sintered samples.

Please cite this article as: O. O. Ayodele, M. A. Awotunde, A. O. Adegbenjo et al., Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2019.12.298

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As stated, higher heating rate may cause insufficient particle re-arrangement during early phase of sintering which causes higher porosity in the samples [12]. The microhardness of the sintered NiAl at different heating rates 50 °C/min, 100 °C/min, and 150 °C/min were measured as 537.2 HV0.1, 538.7 HV0.1, and 555.4 HV0.1. This revealed that the microhardness increases with increasing heating rate. There is an anamalous behaviour in the micohardness and the heating rate relation because the influence of heating rates is not so dominant as sintering temperature [11].

Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Acknowledgements The authors would like to appreciate National Research Foundation (NRF), South Africa for funding this work.

4. Conclusions References In this investigation: 1. The microstructures of the sintered NiAl revealed the presence of micro pores at 50 °C/min and 150 °C/min heating rate. Bigger pores were observed for the sintered NiAl at 100 °C/min (heating rate) 2. XRD pattern of the sintered NiAl indicates the presence of NiAl peaks as the dominant peak but the degrees of the peaks was minimal after the heating was increase. 3. Densification of the fabricated NiAl decreases as heating rate increased from 50 °C/min to 100 °C/min due to adequate power input and time for neck formation and particle bonding at lower heating rate. Further increase was noticed at 150 °C/min. In addition, the microhardness increases with increasing heating rate. Sineterd NiAl at the heating rate of 150 °C/min showed an improved mechanical properties.

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Please cite this article as: O. O. Ayodele, M. A. Awotunde, A. O. Adegbenjo et al., Synthesis and heating rate effect on the mechanical properties of NiAl intermetallic compound, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2019.12.298