American Journal of Oil and Chemical Technologies: Volume 4. Issue 1. Januart 2016

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American Journal of Oil and Chemical Technologies

Journal Website: http://www.petrotex.us/2013/02/17/317/

Improvement the surface structure of Nickel-Aluminum Bronze (NAB) alloy using Al2o3 nanoparticles and FSP method

Keshavarz, S1 *, Abbasi Khazayi, B2 1 M.A student of material engineering, Department of Mechanical Engineering, Technical Faculty, Kermanshah Razi University 2 Assistant professor in Department of Mechanical Engineering, Technical Faculty,Kermanshah Razi University

Abstract:

Nickel-Aluminum bronze (NAB) alloy is an alloy of copper base that is used extensively for marine applications such as propellers, because it exhibits excellent corrosion resistance and mechanical properties. For surface hardening and elimination of defects caused by the casting alloy, FSP is applied on NAB. In recent years, this process has been used as an acceptable way to create composite surface layers. In this paper, alumina oxide (Al2O3) nanoparticles are used in order to create a composite layer on the NAB alloy by FSP. Then the hardness and microstructure in three states of casting, FSP, FSP with alumina oxide nanoparticles on the surface are studied and compared. Based on the results, surface composite layer created by FSP has the highest hardness and along with alloy proceeded under FSP process without the presence of nanoparticles in surface has a structure which is fine and free of cast defects.

Keyword: NAB alloy, FSP, surface nano composite

1. Introduction The nickel- aluminum bronze alloy (NAB) is used for many applications such as screw propeller because it is good resistant against to corrosion and also has acceptable mechanical properties. It is seemed that Accorded problems are available along to manufacture process. In this manufacture process of some important industrial and marine pieces such as screw propeller, most macro pieces are achieved to ambient temperature in along to a weak in casting process and cooled gently. Therefore, this state causes to be macro granule and decrease effects of mechanical properties. However, thin pieces are cooled by more rate and parting is developed because of more changes in rate of cooling in different pieces and in the result, it lead to porous damages. Given problems lead to decreasing hardness, strength and resistance in alloy [1, 2]. The surface hardening of nickel- aluminum bronze alloy (NAB) by FSP achieved from FSW welding increases age of the pieces produced by NAB [1]. FSP is known as surface engineering technology in last years, that it can be used for many metals such as aluminum, magnesium, iron, titanium, and nickel-based alloy. In the result of processing FSP, casting damages as porous surfaces are deleted, microstructure are cured and mechanical properties are improved [3]. In this article, nickel- aluminum bronze alloy (NAB) has casted and cured by FSP and for first time, Alumina nanoparticles (Al2O3 nanoparticles) was used in surface alloy that was formed by FSP of surface Nano composite layer. Then every three molten samples namely molten sample, sample processed by FSP and produced by FSP in presence of Alumina nanoparticles were studied and compared in view of mechanical properties, microstructure.

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1. Materials and Methods

1.1. casting

For casting, at first primal materials involved of commercial copper, aluminum, nickel of purity 99.9% and solid iron and other ingredient as manganese, magnesium, zinc and tin were placed in graphite furnace, then melted in ground furnace. Obtained molten was casted in sandy cast Y in 1200℃ . Chemical compound sample is shown in table 1. After casting, three samples of nickel- aluminum bronze alloy in size of 98*32*10 mm were cut and their surfaces were finished. After then, three samples were studied. Sample 1 is molten sample. Sample2 is processed by friction-stir process (FSP). Sample3 was considered in production of surface Nano composite by using FSP and nanoparticles of Al2O3 in size of 20 nanometer.

Table1: Chemical compound of nickel aluminum bronze alloy

Alloy Cu% Al% Fe% Ni% Other elements%

C95500 78.00

Min

10.00-

11.00

3.00-

5.00

3.00-

5.00

1.00-

1.5

1.2. friction-stir process (FSP)

Simulation of friction-stir process is shown in figure1 [15]. In this simulation, a tool was used that involved of shoulder and pin of super alloy kind with based-nickel (Inconel 738) (figure2). Diameter of shoulder and its length are 25 and 35 mm, respectively and Diameter and length of pin were selected in sizes of 6 and 3 mm, respectively. In this process, rotational speed of tool was 1200 rpm and its move speed was 50 mm/min. slope angle of machine was selected 30. In sample 3, groove in size of 98*32*3 mm was set for nanoparticles of alumina oxide on surface of alloy and nanoparticles were poured in groove. Scale of nanoparticles was 10% of alloy volume in surface. After considering given parameters, friction-stir process (FSP) was performed on molten samples 2 and 3.

figure1: Simulation of friction-stir process[15].

figure2: friction-stir tool.

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1.3. observation of microstructure For the observation of microstructure, samples were cut in sizes of 10*30*10 mm and processed by preparation operation and metallography. Preparation operation was involved of grinding samples that in this stage, it had numbers 100 to 300 and then final operation was polishing. Solution etch 5gr Fecl3 + 2ml Hcl + 95ml C2H5oH was used for etching samples. The spectrum microscope of Olympus was used to study microstructure. The sweep-electron microscope (SEM) with model VEGA\\TESCAN-LMU and field-electron microscope (FESEM) with model Mira3-XMU equipped to EDS to identify and distribute particles and phases. 1.4. hardness test For testing hardness, three samples were cut in sizes of 10*30*10mm (molten samples, samples processed by FSP, and samples processed by FSP in presence of Alumina particles in surface) and grinding and polishing operations were used to test hardness. In this research, hardness-meter Vickers was used and hardness test was performed for each three samples and then their median of each samples was recorded. 2. results and discussion 2.1. EDS analysis Figure 3 shows the chemical composition of casted nickel- aluminum bronze that contained four main ingredients cupper (based metal), aluminum, iron and nickel. In according to this analysis, chemical combination of casted alloy was compared to standard limit shown in table 1, and this comparison shows that content of cupper is less than minimum standard limit and also, content of iron and nickel were considered to be 4%. Its reason was loss of melt.

Elt Line Int Error K Kr W% A% ZAF Al Ka 185.3 12.3443 0.0447 0.0415 9.29 18.73 0.4473 Fe Ka 43.1 0.8746 0.0516 0.0480 4.06 3.96 1.1804 Ni Ka 20.0 0.8746 0.0373 0.0347 3.27 3.03 1.0600 Cu Ka 354.7 0.8746 0.8605 0.7993 82.25 70.43 0.9718

1.0000 0.9289 100.00 100.00 Figure 3: EDS analysis of molten nickel- aluminum bronze.

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2.2. microstructure 2.2.1. As cast alloy Microstructure of molten nickel- aluminum bronze alloy contains phase α of gross widman eshtaton, phase β of gross martensit and Precipitates of phase K that are described at following.

- Phase α

Phase α is the final solid solution combination of nickel- aluminum bronze. Structure of this phase is FCC in room temperature and has parameter of lattice 0.364 nm. Composition of Phase α is various during chilling process. This phase is formed by wideman eshtaton morphology of phase β in 10300c. This phase is solid soluble enriched of cupper that sometimes it as perlite forms eutectoid with phase Kiii and other times, it forms a mixture with Kiv. In finally, it can said that based phase is available in nickel- aluminum bronze alloy that is observed in microstructure by bright color. It may been considered that phase α in microstructure plays the main role on the mechanical properties and corrosion resistance of alloy [1, 6]. In this research, obtained images of spectrum microscope from molten nickel- aluminum bronze alloy show phase α clearly (figures 4, 5).

- phase β and remained β

Phase β is solid soluble in high temperature of nickel- aluminum bronze alloy. This phase is formed by friction stir process in temperature over than 1000 ℃ during hot-work. This phase has structure BCC in high temperature that has parameters of lattice 0.3568nm. This phase is unstable in ambient temperature and is inverted to different phases when cooling process. When cooling process, some part of this phase remains in structure without changeable state that martensitic structure and is named as β´. In nickel- aluminum bronze alloy, transmutation is performed from molten to solid Phase β. In following cooling process, Phase α is grown in intergranular β and forms wideman eshtain, s structure in in long to cristalin surfaces. Phase β is harder than Phase α. However, strength of alloy is increased by its addition in microscopic structure and the relative longitude is decreased. But totally, this phase has less corrosion resistance than based phase (α) and Phase β or eutectoid structure in aluminum bronze can be attacked in circumstance [1,6,27]. Microscopic images of sample 1 (As cast sample) shows this phase in black color in various zoom (figures 4, 5).

- Precipitates of micro phase K

Four phase K are severally formed during cooling process that is described on details later sections.

Phase Ki may be formed in fusion zone and generally is surrounded by α in microstructure. Precipitates Ki have enriched- iron and surround particles enriched-small cupper and seen as combinations of FeAl and Fe3Al. Crystalline lattice of this phase is variable between B2, DO3 and BCC. If content of iron is more than 5%, this phase is seen in microstructure. Phase Ki is seen as great rose in dimension of 10 to 50 micron and after etching in micrograph, it is visible as grey color. In light of performed studies, this phase has been hardly reported in different research [1, 6, and 27]. In this research, according to iron content in alloy, this phase was no shown by spectrum microscope, but it was visible in structure of nickel- aluminum bronze by stir electron microscope (SEM) partly that its results have been showed in figure 6.

Phase Kii is enriched of iron and has crystalline latticeDO3 by combination Fe3Al. These particles nucleates in Phase β in close to common area between α/ β. These particles are spherical and their germination occur in temperature limit of 9300c. Also, these particles have diameters of 5 to 10 micrometers. Particles of Phase Kii have tendency to form Phase α of widman eshtain in same temperature [1, 6, and 27]. In this research, Phase Kii were seen from sample1 (As cast sample) by microscopic images and its results was represented in figure 5.

Phase Kiii is only enriched of nickel in As cast nickel- aluminum bronze alloy that has combination of NiAl. This phase is formed by analyzing remained phase β and eutectic reaction in about 8000c and has layer morphology. This phase contained of structure of lattice B2 and is more visible in molten nickel- aluminum bronze alloy that has high percent of nickel [1, 6, and 27]. In this research, Phase Kiii were seen from sample1 (molten sample) by microscopic images and its results was represented in figure 5.

Precipitates Phase Kiv micro - sediments are formed in 8600c and contained of combination Fe3Al. Phase Kiv has interatomic distance and same structure with Phase Kii (crystalline lattice DO3). These particles are distributed in across of granular α [1, 6, and 27]. In this research, microscopic images of molten sample demonstrate availability of this Phase and its results are represented in figure 5.

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Figure 4: microstructure of molten nickel- aluminum bronze alloy.

Figure 5: microstructure of molten nickel- aluminum bronze alloy.

Figure 6: image SEM of phase Ki in microstructure of molten alloy.

2.2.2. alloy processed by FSP process Now we study and explain the obtained results of microstructure of alloy in sample 2 (processed by friction-stir process (FSP)). In this stage, by friction-stir process (FSP) molten damages and partings are deleted by friction-stir process (FSP) and granules are fragmented and microstructure is cured. Therefor these operations are led to improve mechanical properties in surface specially. Figure 7 shows border between based metal and area processed by FSP and shows that this area has very micro structure. As figure 7 are shown, friction-stir process causes to develop four zones in side and center of stirred zone that are following as:

- Stirred zone (SZ) that involved of recrystallized and uniaxial granules. - Zone effected by thermodynamic operations (TMAZ) that in this zone, granules are lengthened by mechanical

work and this case is recognized by structure that has been deformed severely. - Zone effected by hot (HAZ) that has been effected by thermal cycles only and no changing structure occurs on it. - Fourth zone that is same based metal.

Figures 8 and 9 show microstructure of stirred zone in various zooms.

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Figure 7: microstructure of stirred zone for alloy processed by FSP and created regions.

Figure 8: microstructure of alloy processed by FSP.

Figure 9: microstructure of alloy processed by FSP.

In according to microscopic observations and aforesaid results, it can be said that Stirred zone (SZ) has smaller granules because of stirred center and in this zone, less amount of phase α and relative phase K are inverted to granules β during friction-stir process. Also, phase α is inverted to same and small granules because of dynamic recrystallization and sever deformation of plastic. It can be considered that no change occurs in transmutation of phase and chemical combination during friction-stir process and only we will see curing surface microstructure such as fragmenting granules and deleting constructional damages and parting. Therefore, in friction-stir process, phases α, Kii, Kiii, Kiv are indissoluble and only sever deformation with high heat is developed during this process [1]. Small granules α is dominant structure in microstructure of nickel- aluminum bronze alloy that processed by friction-stir process. In upon images of microstructure of nickel- aluminum bronze alloy processed by FSP, bright and black regions and blue granules with red lines ( in figure 9) show phase α, phase β, sediments of phases Kiii, respectively. In friction-stir process, recrystallization is developed because of sever deformations and high temperature is led to globing Precipitates of phases Kiii as layer remainder on surface α [1, 17]. 2.2.3. alloy processed by FSP process in presence of Alumina nanoparticles in surface In there, we study the obtained results of microscopic observations in sample 3 (surface Nano composite). In sample 3, nanoparticles (Al2O3) has been used to form surface Nano composite by friction-stir process. Four zones in similar to sample 2, were developed by friction-stir process that shown in figure 10.

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Figure 10: microstructure of stirred zone for alloy processed by FSP and created regions.

As upon image, stirred zone (SZ) has smaller and homogenous granules but in zones of thermodynamic operation (TMAZ) and areas affected by high hot situations (HAZ), there are larger granules than stirred zone. In figures 11 and 12, obtained results of microscopic observations of sample 3 are given.

Figure 11: microstructure of alloy processed by FSP in presence of nanoparticles of Alumina on surface.

Figure 12: microstructure of alloy processed by FSP in presence of nanoparticles of Alumina on surface.

In according to given images, it can be said that changes of microstructure in sample3 obvious than sample 2 that only was processed by friction-stir process. The effect of nanoparticles of Alumina (Al2O3) in microstructure of sample3 shows that according to given results in upon images, microstructure has self-dominant phases as phase α and remained phase β. Nonetheless, particles of phase α and phase β have special direction/orientation. In according to given images, it can be said that amount of phase β has been increased appreciably and phase α has been clustered but it cannot talked about globing phase α. Considerable amounts of Precipitates of phases Kiii are observed in microstructure but these particles are almost observed in phase β as distributed state in comprised to sample 2 (figure 9), but in sample 2, these particles are adhesive to particles of α. In figure 9, particles of phase α and β have been distributed uniformly but in sample 3 (figure 12) that contained of nanoparticles of Alumina on surface, there is deploying state between phase α and β and particles of every phase have been connected together that it can be said strictly that created changes in microstructure of this sample are because of the presence of nanoparticles of Alumina on surface and formation of surface Nano composite. It can be said that orientation of particles of phase β is because of martensitic nature of self-

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phase β in addition to presence and effects of Nano particles. In according to microstructural changes in alloys contained of Nano particles on surface, it can be expected that there is modification state in corrosion and mechanical properties in comparison to two previous samples. In following, obtained results of test FESEM from sample 3 have been represented to demonstrate the presence of Nano particles on surface and their effects on microstructure of nickel- aluminum bronze alloy in figure 13. The presence of nanoparticles of Alumina on surface is obvious in according to the image obtained of test FESEM. This figure 13 shows the special orientation of nanoparticles on surface and their effect on the orientation and deploying particles of phase α and β.

Figure 13: image FESEM for determining nanoparticles of alumina.

2.3. hardness Hardness test was performed for three samples (As cast sample, sample protected with FSP and sample protected with FSP in presence of Alumina nanoparticles in surface that their results have been shown in figure 14. One of the important surface properties for nickel- aluminum bronze alloy is hardness testing. Because of application of this alloy in marine industries and sensible sections, surface of alloy must have high hardness. Therefore, inn molten state, mechanical properties especially hardness are decreased because of available damages, porous surface and parting. Hardness of self-alloy of 203 Vickers was obtained in molten conditions. Hardness of self-alloy was increased by friction-stir process and reached to 203 Vickers. It reason was infusion of granules, deletion of damages and porous surfaces and reaching to perfect and homogenous structure. But most amount of hardness is related to sample 3 that in there, surface Nano composites are formed by friction-stir process. As it was pointed in microstructural section, Alumina nanoparticles (Al2O3) causes to change microstructure of alloy that we can point to orientation and special clustering of phase α and β, distributing particles of phase Kiii in inside of phase β and special directing Alumina Oxide nanoparticles on surface (results of testing FESEM). Also it was said that all changes of microstructure led to changes of mechanical properties that this problem was proved by hardness test and alloy had higher hardness (235 Vickers) in between two molten samples and FSP because of formation of surface Nano composites.

Figure 14: graph of Vickers hardness test

203

223

235

180

190

200

210

220

230

240

Ascast FSP Al2O3

Hardne

ss

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3. conclusion

- In accord to microstructure of nickel- aluminum bronze alloy, phases α as based-phase and β with morphology withman eshtain and macro-martensit, respectively play important role on phase development of this alloy.

- Friction-stir process is acceptable process for improving surface structure and producing surface Nano composite in nickel- aluminum bronze alloy.

- In between four zones developed by Friction-stir process, stirred zone (SZ) has smaller structure and harder zone. - By applying Friction-stir process, surface microstructure is improved, molten damages and partings are deleted

and mechanical properties are decreased. - By applying Friction-stir process, morphology of sediments of phase K is changed in addition to being smaller

phases α and β. - By applying Friction-stir process and Alumina nanoparticles on surface, layer of surface Nano composite in

nickel- aluminum bronze alloy. - In respect to hardness and comparison of hardness results in between three alloys, it can be said that As cast

nickel- aluminum bronze alloy has less hardness and alloy contained of layer of surface Nano composite has more hardness, and nickel- aluminum bronze alloy processed by FSP has medial hardness namely its hardness is higher than molten alloy and lower than alloy contained of layer of surface Nano composite.

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