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ScienceDirect Materials Today: Proceedings 2 (2015) 3042 – 3048
4th International Conference on Materials Processing and Characterization
Electro deposition of Nickel-Alumina Composite Coating. Arshali Sasi1, Manoj Mondal2, Saurabh Dayal3, Sasi Kumar 1c 1
Department of Material Science & Metallurgical Engineering, MANIT, Bhopal, M.P, India
Abstract Nickel-alumina composite coatings were synthesized by electrodeposition technique. The co-deposition of alumina was accomplished by using magnetic stirring, variation of current density and temperature. The xrd analysis confirmed the formation of Ni-Al2O3 composites and the SEM studies revealed uniform dispersion of alumina into nickel matrix. The morphology of the alumina particles found significantly affected by the current density and temperature. The incorporation of alumina showed increased hardness and wear resistance of the coatings. © 2014Elsevier The Authors. Ltd. All rights reserved. © 2015 Ltd. AllElsevier rights reserved. Selection andpeer-review peer-review under responsibility of the conference of the 4thconference International conference on Selection and under responsibility of the conference committeecommittee members ofmembers the 4th International on Materials Materials and Characterization. Processing Processing and Characterization. Keywords: Electrodeposition, Ni-Al2O3 composite, co-deposition, composite coatings
1. Introduction. Here introduce the paper, and put a nomenclature if necessary, in a box with the same font size as the rest of the paper. The paragraphs continue from here and are only separated by headings, subheadings, images and formulae. The section headings are arranged by numbers, bold and 10 pt. Here follows further instructions for authors. Electro deposition is widely used to improve the corrosion resistance, hardness, wear resistance of materials and to impart special functional properties. However, there is growing interest among the researchers to modify the properties of the coatings by co-deposition of different metals, oxides and inter metallic compounds. Composite coatings normally contain second phase particles of oxides, carbides, boride and nitride particles such as Al2O3, TiO2, SiO2, ThO2, Y2O3, SiC, WC, B4C, BN, TiN etc. [1]. Many research works are been carried by researchers using diamond particles or solid lubricants such as PTFE, Graphite into a metallic phase. Fe oxides are doped into the coatings to impart magnetic or electronic properties [2]. However, the major challenge is co-deposition of electrically inert particles into the metallic matrix phase. * Corresponding author. Tel.: +0-000-000-0000 ; fax: +0-000-000-0000 .
2214-7853 © 2015 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing and Characterization. doi:10.1016/j.matpr.2015.07.292
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[email protected] Nickel electroplating is a commercially important and versatile surface-finishing process. A survey reports that the amount of nickel in the form of metal and salts consumed 100,000 metric ton worldwide annually for electroplating as reported by Dibari and Watson [3]. In the current work, electro deposition of nickel composite coatings is achieved by co-deposition of alumina particles besides electroplating of nickel from watt’s solution. 2. Experimental 2.1 Electrodeposition Ni-Al2O3 composite coatings were prepared in an electrolytic cell using a potentiostat (Gamry, model reference 600) with three electrode system. For Ni depositon a Watt’s bath solution was prepared using nickel sulphate (NiSO4), nickel chloride (NiCl2) and boric acid. A highly pure and fine alumina powders (Al2O3) were dispersed in the solution. About 50 g/L of alumina powders were used in all the experiments and the solution was subjected to stirring using a magnetic bead to assist co-deposition of alumina and to avoid settling of these dense particles. The speed of strring was varied in the range of 200 to 350 rpm. A stationary nickel plate was used as an anode stainless steel sheet as a cathode and Ag/AgCl used as a reference electrode. The pH of the solution was maintained at 4.0 and the experiments were carried out using a potentiostatic mode. The current density was varied between 5 to 40 mA/cm2 to study its effet on co-deposition. Few experiments were repeated at different temperatures between 200 C to 500 C. 2.2 Characterization The surface morphology and hard alumina particle distribution in nickel matrix was investigated using a scanning electron microscopy (JEOL, JSM 6490A). A PANalytical Empyrean x-ray diffractometer is used to confirm the incorporation of alumina into nickel matrix and to study their particle size. The hardness of coatings were studied by using a Microviker’s hardness tester. The wear resistance of the coatings were investigated using a Pin-on disc wear tester (Magnum). 3. Results and Discussion 3.1. XRD Analysis of Ni-Al2O3 Composites coatings The x-ray diffractograms of the electrodeposited samples without and with alumina co-dposition are delineated in fig. 1. The samples before addition of alumina revealed the formation of nickel coating on stainless steel substrate. However the samples co-deposited with alumina particles had confirmed the presence of Al2O3 in nickel matrix phase. Gheorghies et al., [4] had also showed similar results in Ni-alumina nano-composites. It is found that the relative intensity of (111) plane is high while alumina is absent, however the intensity of (200) plane had increased after alumina additions. This may be attributed to the preferential growth of Ni grains in presence of alumina.
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Fig. 1 x-ray diffractograms of Nickel composite coating without and with alumina co-deposition on stainless steel
3.2 SEM Analysis The nickel-alumina composite coatings were developed at different stirring speed and temperatures. The typical SEM images of nickel composite coatings prepared at different stirring speed and temperatures are shown in fig.2 a-d respectively. The strirring speed as well as deposition temperature influences the morphology of alumina particles significantly. At low speed and temperatures the particles found to be agglomerated/grouped as a spherical particles. The typical size of these agglomerates were found to be about 10 μm. However the increase in stirring speed and deposition temperature had reduced the size of agglomerates evidently. At 400C and above 250 rpm the agglomerates were completely disappeared and the alumina particles found uniformly distributed into nickel matrix.
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Fig. 2 SEM images Nickel-Alumina composite coatings deposited at different temperature and stirring speeds. (a) 300C and 200 rpm (b) 350C and 230 rpm (c) 400C and 260 rpm (d) 400C and 300 rpm.
3.3 Effect of electrodeposition parameters on Ni-Al2O3 Coating Characteristics The coating thickness and hardness of the Ni-Al2O3 composites films were significantly afftected by current density, temperature and stirring speed. The effect of the above mentioned parameters are demonstrated in fig.3-5 respectively.
3.3.1 Effect of current density
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750
16
Hardness
Coat thickness
700 Hardness (Hv)
Coat thickness (μm)
14
12
10
8
650
600
1.5
2.0
2.5
3.0
3.5
4.0
2
1.5
Current density (A/dm )
2.0
2.5
3.0
3.5
4.0
2
Current density (A/dm )
Fig. 3 Effect of current density of on coating thickness and hardness
20 18
800
Coat thickness Hardness
14
700 Hardness (Hv)
Coat thickness (μm)
16
12 10 8 6
600
4 2 0
500
30
35
40 0
Temperture ( C)
45
28
30
32
34
36
38
40 0
Temperature( C)
Fig. 4 The role of deposition temperature on temperature on coating thickness and hardness
42
44
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800
Coat thickness 16
Hardness
700
12
Hardness (Hv)
Coat thickness (μm)
14
10 8 6
600
4 2
500
0 200
220
240
260
Agitation speed (rpm)
280
300
200
250
300
Agitation speed (rpm)
Fig.5 The strirring speed/agiation of electrolytic bath illustrates increased coating thickness and hardness
As shown in fig.3 the thickness and hardness of electrodeposited nickel-alumina composite coatings increased exponentially with current density. It was observed that that the coating thickness increased from 12 to 16 m while the current density varied from 1 to 4A/dm2. The maximum hardness of the composites were found to be about 750 HV0.1 at 4A/dm2. Besides increasing the throwing power of alumina particles the grain size is also refined at higher current density. Thus the hardness foun increasing with current density. The effect of temperature on coating parameters are illustrated in fig.4. The coating thickness increased exponentially with temperature, however the hardness found decreasing linealy with temperature. Results showed that when the temperature was increased from . This is attributed to the effect of room temperature to 45Ԩ, the coat thickness increased from 8 to 16 temperature in accelerating the reaction kinetics which in turn results in fast dissolution and migration of Ni2+ ions and consequently faster deposition rates. The agitation of the electrolyte solution is essential to keep the inert dispersion suspended and improve the transport process of particles to the cathode surface. Agitation also has a role in removing evolved hydrogen at the cathode surface [3] and helps to homogenize the concentration of Ni ions in the electrolyte solution. The decrease in hardness may be attributed to the increase in grain size at higher deposition temperature. The effect of stirring speed is shown in fig.5. Upon examining the coat thickness for samples deposited from electrolyte having an agitation speed of 200, 230 ,260 and 290 rpm had demostatred a thickness of 8.06, 12.8, 14.6 and 15.7 μm respectively. The incorporation of alumina particles into nickel coating was found more at higher stirring speed and the particles were uniformly distributed into the coating. Thus the hardness of composite films increased with stirring speed. 4. Conclusion In summary, electrodeposited Nickel and Ni-Al2O3 composite coatings were successfully processed with varying
concentration of Al2O3 in the bath. The xrd analysis showed alumina peaks in the composite coatings and the growth in (200) plane. Microstructural analysis of the films revealed that the alumina particles found agglomerated as globular particles at low speeds and uniformly distributed at high temperature and stirring speed. The current density and stirring speed increased the hardness of the films significantly. A maximum of 750 HV0.1 was achieved at 300 rpm. Hower the temperature showed inverse relationship with hardness because of grain growth at higher deposition temperatures.
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Acknowledgement The authors are thankful to HOD (MSME) and Director, MANIT Bhopal, India for their support in pursuing this research work. The authors also acknowledge IISRER (Bhopal), India for their assistance in XRD analysis. References [1] S. T. Aruna, V.K. William Grips, K.S. Rajam Ni-based electrodeposited composite coating exhibiting improved microhardness, corrosion and wear resistance properties: Journal of Alloys and Compounds 468 (2009) 546-552. [2] M.S. Ali Eltoum, A.M. Baraka, M. Saber M. And ELfaith A. Hassan International Journal of Multidisciplinary Science and Engineering, Vol.2,No.4 July 2011. [3]M. Stroumbouli, P. Gyftou, E.A. Pavlatou, N. Spyrellis, surface and coating technology 195 (2005)325-332. [4] C. Gheorghies, G. Carac, I. V. Stasi, Preparation and structural characterization of Nickel/ Alumina nano-particles composite coatings, Journal Of Optoelectronics And Advanced Materials Vol. 8, No. 3, June 2006, P. 1234 – 1237 [5] Meenu Srivastava, V. Ezhil Selvi, V.K. William Grips, K.S. Rajam Corrosion resistance And microstructure of electrodeposited nickel-cobalt alloy coatings Surface & Coatings Technology 201 (2006) 3051-3060. [6]Q.Wang , P. Zang, X. Wang, D.Ren , D.Lang, Y. Zhang, J .of Metastables and Nanocrystalline materials, Vol. 23 (2005) pp.191-194. [7]S.C. Wang and W.C.J. Wei, J. Mater. Res., Vol 18, No. 7, Jul 2003. [8]N. Sombatsompop, K. Sukeemith, T. Markpin and N.Tareelap, Mat. Sci. and Eng A 381 (2004) 175-188. [9]N. Guglielmi, Journal of Electrchemical Society 119(1972) 1009 [10] P. Debye, E. Huckel, Physik. Z., 25, 204(1924) [11] M. von Smoluchowski, Bull. Int. Acad. Sci. Cracovie, 184 (1903) [12]E. C. Lee, and J.W. Choi, J. Surface and Coating Technology.148(2001) 234-240 [13]C.S. Lin, P.C. Hsu, L. Chang and C.H. Chen, J. Appl. Electrochem. 31(2001) 925 [14] Sheng Lung Kuo, Yann Cheng Chen, Ming Der Ger, Wen Hwa Hwu, Materials Chemistry and Physics, 86 (2004)5-10. [15]Saraby- Reintjes, M. Fleischmann, Electrchim, Acta 29(1984) 557 [16]E. Chassaing, M. Joussellin and R. Wiart, J. Electronal. Chem. 157(1983) 75 [17] Bhargavi Rebba And N.Ramanaiah Studies on Mechanical Properties of 2024 Al – B4c Composites: Advanced Materials Manufacturing & Characterization Vol 4 Issue 1 (2014).