Influence of SiC Nanoparticles and Saccharin on the Structu

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Journal of Alloys and Compounds xxx (2009) xxx–xxx

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Journal of Alloys and Compounds

j o u r n a l h o m e p a g e : w w w . e l s e v i e r . c o m / l o c a t e / j a l l c o m

Influence of SiC nanoparticles and saccharin on the structure and properties of electrodeposited Ni–Fe/SiC nanocomposite coatings

Hamed Ataee-Esfahani a,b, M.R. Vaezi a,∗, Leila Nikzad a, Bahare Yazdani a, S.K. Sadrnezhaad a,b

a Materials and Energy Research Center, P.O. Box 14155-4777, Tehran, Iranb Department of Materials Science and Engineering, Sharif University of Technology, P.O. Box 11365-9466, Tehran, Iran

a r t i c l e i n f o

Article history:

Received 15 December 2008Received in revised form 28 April 2009Accepted 29 April 2009

Keywords:

ElectrodepositionNi–Fe/SiC nanocomposite coatingX-ray diffractionMicrohardnessCorrosion resistanceSaccharin

a b s t r a c t

In this study, Ni–Fe/SiC nanocomposite coatings with smooth and crack-free surface were successfullyprepared by means of the conventional electrodeposition in the presence of saccharin in electrolyte. Thegoal of this work was to investigate the effect of SiC nanoparticles and saccharin on the structure andproperties of permalloy nanocomposite coatings. The nanocomposite coatings were characterized usingoptical and scanning electron microscopy, energy dispersive X-ray (EDX) analysis and X-ray diffraction(XRD)technique. The significantvariationin the crystallographictextureof the coatings wasobserveddueto the addition of SiC nanoparticles and saccharin in the electrodeposition bath. Increasing the amountof saccharin in the electrolyte led to a change in the texture from a (2 0 0) fiber texture to mixed (31 1)and (2 0 0) textures. Our results indicated that inclusion of SiC nanoparticles suppressed the preferredgrowth direction of the Ni–Fe matrix, resulting in a decrease in the sharpness of the (2 0 0) fiber textureand formation of a more random texture. The presence of SiC nanoparticles in the metallic matrix alsoled to the production of compositefilms with bettercorrosion resistanceand higher microhardness thanthe Ni–Fe coating.

© 2009 Elsevier B.V. All rights reserved.

1. Introduction

In the last decade, a great deal of attention has been paid to thestudy of permalloy (80% Ni–20% Fe), because of the widespreaduse of this material in applications involving micro-electro-mechanical-systems (MEMS) and mesoscopic systems [1–4]. Ni–Fecoatings are easily produced using electrodeposition techniques.The deposited films have been shown to have low residual stress,low energy requirement, rapid deposition rate, low cost, capabilityto handle complex geometry and to control the film thickness, andsimple scale-up with easily maintained equipment. Permalloy isintroduced as a structural material for the LIGA (Lithographie, Gal-vanformung, Abformung, equivalent to lithography, electroplatingand molding) method which is used to fabricate discrete, free-

standing metallic parts and high-aspect ratio microstructures [2].Saccharin is a strong leveling and grain refinement agent, capableof decreasing internal stress in the permalloy coating [2,4]. Sac-charin, as a sulfur-bearing additive, increases the sulfur content inthe electrodeposited coating which is insoluble in permalloy. Sul-fur segregation to grain boundaries after the coating is exposuredto high temperatures,promotes grain boundary embrittlement andintergranular fracture [2].

∗ Corresponding author. Tel.: +98 261 6204131; fax: +98 261 6201888.E-mail address: [email protected] (M.R. Vaezi).

The codeposition of inertparticlesin metallic coatings improvesphysical and mechanical properties of these coatings and forms ananocrystalline metallicdeposit dueto themodified growth[5–11].Since the electrodeposited composite coatings combine the advan-tages of both the electrodeposited coatings and codeposition of hardparticles,Ni–Fenanocompositecoatingshavepropertiessupe-rior to the Ni–Fe alloy coatings [12,13]. Two articles related to thereinforcementofNi–Fealloyswithceramicparticleshavebeenpub-lished in the pastfive years. Li and Li [12] have studied the effect of Si3N4 nanoparticles content and annealing on the microhardnessof electrodeposited Ni–Fe/Si3N4 nanocomposites. More recently,Starosta and Zielinski [13] investigated the influence of coatingcomposition on corrosion and wear behavior of the Ni–Fe/Al 2O3

composite coatings. However, to our knowledge, the electrodepo-

sition of Ni–Fe/SiC nanocomposite coatings has not been studiedup to now.

Due to theeffect of microstructure on the physical and mechan-ical properties of nanocomposite coatings, it seems to be necessaryto examine the influence of some parameters such as embeddednanoparticles and organic additives, on the microstructure of theresulting nanocomposite coating. In this research, we reported theeffect of saccharin and SiC nanoparticles on the microstructure of the permalloy nanocomposites, special attention was paid to thedistribution of crystallographic orientations because texture canhave a great influence on physical and mechanical properties of coating due to the anisotropic properties. The relationship between

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SiC incorporationandfinal performancesuch as the corrosionresis-tance and microhardness for deposited Ni–Fe/SiC nanocompositewas also studied. Besides, in order to better understand the natureof theprocedureof electrodereactions,the role of SiCnanoparticlesin the electrodeposition of Ni–Fe/SiC nanocomposite was analyzed.

2. Experimental

In this study, the plating bath was composed of 112 g/l NiSiO4·6H2O and 5g/lFeSO4 asmetalsources,2g/lboricacidasabuffer,0.5g/lsodiumdodecylsulfate(SDS)as a surfactantand saccharinas a brightener andstress-reducer. Also,1 g/l L-ascorbicacidwas added to minimize Fe2+ oxidation. The concentration of saccharin was var-ied from 0 to 6 g/l to investigate the effect of saccharin addition on microstructureof the nanocomposite. Analytical reagents and distilled water were used to preparethe plating solution. With the aim to synthesis of Ni–Fe/SiC nanocomposite, the SiCnanoparticles of a meandiameter50 nm (Kaier,Hefei, China) with different concen-trations (i.e. 0, 5, 10, 15, 20, 25 g/l) were dispersed in the electrolyte prior to plating.During the experiments, the electrolyte was agitated by a mechanical stirrer, asshown in Fig.1. The pH of theelectrolyte was4, andtemperature waskept constantat 50 ◦C. Ni–Fe/SiC nanocomposite was deposited onto polished copper substrateusing a currentdensity of30 mA/cm2. A platinumplate of40mm×40mmwas usedas theanode.The distance betweenanode andcathodewas 4 cm.Beforeeach experi-ment, cathode was ultrasonically cleaned in ethanol, acetone and distilled water for10min, activated in 10% H2SO4 for 30 s, washed in distilled water, before imme-diately immersed in the plating bath, to allow the electrodeposition of the targetnanocomposite coatings. Deposits were ultrasonically cleaned in de-ionized water

for 15min in order to remove loosely adsorbed nanoparticles. The average thicknessof deposited layers was about 50m.

All electrochemical experiments wereperformed in a three-electrode cell usingan AUTOLAB PGSTAT 30 potentiostat/galvanostat device and an Ag/AgCl electrode(Argenthal, 3MKCl, 0.207V vs. SHE at 25 ◦C) was used as the reference electrode.The polarization curves of the electrolyte were recorded at a sweep rate of 1 mV/s.The Tafel curves were measured at a sweep rate of 1 mV/s in 0.5 M NaCl at roomtemperature.

Surface morphologies of nanocomposite coatings were examined by a PhilipsMV2300scanningelectronmicroscope(SEM) operatingat 25 kV.The chemicalcom-position of the deposits was determined using the Kevex model energy dispersiveX-ray spectroscopy (EDAX) system attached to the SEM. All chemical compositionvalues are expressed in weight percent and represent the average of at least fivemeasurements. X-ray diffraction (XRD) was used to determine the present phasesand the preferred orientation of the deposits. A Philips Xpert-ProX-raydiffractome-ter with a Cu K␣ radiation (= 1.5418Å) was employed to obtain XRD spectra usingstandard Â –2Â geometry. A computer-based search and match was used for phase

identification.Thehardness of thenanocompositecoatings wasmeasuredon a Vickers’ micro-hardness instrument at an applied load of 50 g for 5 s. Five measurements wereconducted on each sample and the results were averaged.

Fig. 1. Schematic diagram of the electrodeposition system.

Fig. 2. Cathodic potentiodynamic diagrams for co-deposited SiC nanoparticles withNi–Fe (20 g/l SiC in the electrolyte) and electrodeposited Ni–Fe at a sweep rate1mV/s.

3. Results and discussion

3.1. Effect of SiC nanoparticles on permalloy electrodeposition

Fig. 2 shows the potentiodynamic diagram plotted at variouscathodicpotentials withand withoutdispersednanoparticlesin thepermalloy plating bath. The addition of silicon carbide nanoparti-clesaffectedthereductioncurvebyincreasingthecurrentdensities.This behavior can be associated with two facts; on one hand, whenintroduced to the electrolyte, the SiC nanoparticles are surroundedby an adsorbed thin layer of metallic ions, resulting in a possibleincrease in ionic transport by nanoparticles. On the other hand,incorporation of nanoparticles increases the available nucleationsites for the metallic ions [14–17].

3.2. Effect of sachharin on the structure of Ni–Fe/SiC nanocomposite

The surface of electrodeposited nanocomposite coating in thesolution with 20g/l SiC nanoparticles (without saccharin in elec-trolyte)isshownin Fig.3a. Itiseasilyseenthatthesurfaceofcoatinghas a network of cracks. It is attributed to very high-generatedinternal stress during Ni–Fe/SiC electrodeposition, exceeding thefracture strength of the deposit [18–20]. In contrast, as seen inFig. 3b, the nanocomposite coating electrodeposited in the pres-ence of saccharinhas a smooth, shiny and crack-free surface, whichcanbe explainedby a decrease in internal stressdue tothe presenceof saccharin [21,22].

Ni–Fe/SiC composite coatings were electrodeposited with dif-ferent saccharin concentrations in electrolyte containing 20g/l SiCnanoparticles. Each electrodeposited film was investigated by XRDtechnique to determine the crystalline structure and phase forma-tion.The XRD patterns of the electrodepositedNi–Fe/SiCcompositecoatings for various saccharin concentrations are shown in Fig. 4.It can be seen that all the coatings exhibit single phase of Ni–Fematrix with FCC crystal structure. In order to describe thestructureand preferred orientation of the deposit in detail, the TC is used, asdefined in Eq. (1):

TC(hkl) =I (hkl)I 0(hkl)

1n

I (hkl)I 0(hkl)

−1

(1)

where I (hkl) is the measured intensity of the (hkl) reflection, I 0(hkl) is standard intensity of the standard powder pattern diffrac-

tiondata (JCPDS 47-1417), n is the number ofreflections used in the







H. Ataee-Esfahani et al. / Journal of Alloys and Compounds xxx (2009) xxx–xxx 3

Fig. 3. Electrodeposited Ni–Fe/SiC nanocomposite without sachharin (a) and with2 g/l saccharin (b) in electrolyte containing 20 g/l SiC.

Fig. 4. XRD patterns of Ni–Fe/SiCcompositecoatingswith saccharinconcentrations

of (a) 0, (b) 2, (c) 4, and (d) 6 g/L.

Fig. 5. TCs of the electrodeposited Ni–Fe/SiC composite coating as a function of saccharin concentration.

calculation. It is noteworthy that if TC is greater than 1, it indicatesthe existence of a preferred orientation [22,23].

Fig. 5 illustrates the relationship between the saccharin concen-tration in electrolyte and the TCs of composite coating. When thesaccharin concentration was less than 2g/l, the preferred orienta-

tion of the electrodeposited nanocomposite was the (2 0 0) fibertexture. However, by further increasing saccharin, the (20 0) fibertexture diminished and (3 1 1) fiber texture strongly developed. Inaddition, (2 2 0) fiber texture, which was negligible at low con-centration of saccharin starts to develop with increasing saccharinconcentration. So, it was observed that as the amount of saccha-rin increased, the crystal orientation progressively changed from a(2 0 0) fiber texture to mixed (3 1 1) and (20 0) textures. The calcu-lated TC of each diffraction line and total TCs of diffraction lines of each coating in Fig. 4 are listed in Table 1.

Theresults suggesting that microstructureof theNi–Fematrix issignificantly changed dueto theadditionof saccharinto theplatingbath are in agreement with earlier observations in other electrode-position systems [22,24,25].

3.3. Effect of SiC incorporation on the structure of Ni–Fe/SiC

nanocomposite

The SEM images (Fig. 6) show the nodular surface structure of the Ni–Fe/SiC nanocomposite coating. It is observed that the SiCnanoparticles are covered by a Ni–Fe layer. It can be due to thereductionoftheadsorbedlayerofmetallicionsonSiCnanoparticles[14,26]. Embedded particles are uniformly distributed in the Ni–Fematrix which is confirmed by EDX analysis. Agglomeration of theco-deposited SiC nanoparticles is also seen on the magnified imageof nanocomposite coating surface (See Fig.6b). It is attributed tothefact that nanoparticles strongly tend to agglomerate due to theiractivity. [27].

Fig. 7 shows the XRD patterns of Ni–Fe/SiC composite coatingswith different SiC contents. It is observed that incorporation of SiCnanoparticles has affected the XRD patterns and crystallographictexture. X-ray diffraction line broadening analysis was employedfor the determination of crystallite size. Pure Ni–Fe deposit exhib-

Table 1

Thecalculated TC of each diffractionline andthe totalTCs of diffractionlinesof eachcoating in Fig. 4.

Saccharinconcentration (g/l)

TC20 0 TC11 1 TC31 1 TC22 0 Total TCs of diffraction lines

0 1.57 0.92 0.51 0 32 1.44 0.94 0.62 0 34 1.41 0.94 1.47 0.18 46 1.30 0.96 1.53 0.21 4







4 H. Ataee-Esfahani et al. / Journal of Alloys and Compounds xxx (2009) xxx–xxx

Fig. 6. SEM image of surface morphology of Ni–Fe/2.5% SiC nanocomposite coating(a) and the magnified image (b).

ited a crystallite size of 22 nm (reference to (2 0 0) reflection). Thecodeposition of SiC nanoparticles (2.5 wt%) decreased the crys-tallite size of the deposit to 10 nm. During the electrodepositionprocess a competition occurred between the nucleation sites andcrystalline growth. When introduced to the electrolyte, the SiCnanoparticles provided more nucleation sites for the metallic ionsand perturbed the crystalline growth of Ni–Fe deposit. Subse-quently, a nanocrystalline structurewas facilitated byincorporationof SiC nanoparticles.

In order to study the effect of SiC content on microstructure of Ni–Fe/SiC coatings, the TC was calculated according to Eq. (1). It

Fig. 7. XRD patterns of Ni–Fe/SiC composite coatings (in the presence of 2 g/L sac-

charin) with different SiC contents: (a) 0, (b) 0.8, (c) 1.4, and (d) 2.5 wt%.

Fig. 8. TCs of the electrodeposited Ni–Fe/SiC composite coating as a function of SiCcontent in coatings.

is evident from Fig. 8 that all of the electrodeposited coatings have(200)preferredorientation.But,itshouldbementionedthat(200)fiber texture of theNi–Fe/SiC decreases with increasing SiC contentfrom0 to2.5wt%, inspiteofthefact that(11 1)and(31 1)fiber tex-tures are slowlydeveloped. The increasingof (11 1)and (31 1)fibertextures can be linked with the reinforcement of [21 1] crystallineorientation [28]. From the TC values, it can be concluded that theembeddingof silicon carbide nanoparticles results in more randomdistribution of crystallographic orientation and textural modifica-tionfrom[1 0 0] tothemixed [21 1]orientation.It can beattributedto the suppression of the preferred growth direction, due to thecodeposition of SiC nanoparticles during the electrodeposition pro-cess [28–30]. TheamountsofTCofeachdiffractionlineandtotaltheTCs of diffraction lines of each coating in Fig. 7 are listed in Table 2.

3.4. Effect of SiC incorporation on the corrosion and

microhardness of Ni–Fe/SiC nanocomposite

According to the literature, a uniform distribution of SiCnanoparticles yields in improved mechanical and corrosion resis-tance properties [5]. The effect of the SiC content in the coating onthe microhardnesss of the Ni–Fe/SiC composite coating layer wasinvestigated. It is evident from Fig. 9 that the microhardness of theNi–Fe/SiCincreased with increasing SiCcontent in thecoating,sim-ilar to what was reported on Ni–Fe/Si3N4 nanocomposite coatings[12]. The hardening effect can be associated with uniform disper-sion of SiCnanoparticles in theNi–Fematrix that yieldsin finegrainsize and dispersion strengthening [8,31–34].

The corrosion rate of Ni–Fe coatings containing SiC nanoparti-cles was also investigated. Fig. 10 shows the anodic polarizationcurves for Ni–Fe alloy and Ni–Fe/SiC nanocomposite coating in0.5M/l NaCl solutions. Thevalues of corrosion potential andcurrentdensity were estimated using Tafel slope method. The corrosionpotential and corrosioncurrent density of the nanocomposite werefound to be −254 mV and 5.1×10−5 A/cm2, respectively, and thosefor the Ni–Fe alloy coating were determined to be −314 mV and9×10−4 A/cm2. The obtained results reveal that the presence of

Table 2

ThecalculatedTC ofeachdiffractionlineand thetotal TCsof diffraction lines ofeachcoating in Fig. 7.

SiC content (wt%) TC11 1 TC20 0 TC31 1 Total of the TCs of diffraction lines

0 0.39 1.61 0 20.85 0.83 1.58 0.59 31.44 0.88 1.5 0.62 32.5 0.99 1.28 0.73 3







H. Ataee-Esfahani et al. / Journal of Alloys and Compounds xxx (2009) xxx–xxx 5

Fig.9. Effect of SiC contentin coatings on themicrohardnessof Ni–Fe/SiCcompositecoatings.

Fig. 10. Potentiodynamic polarization behavior of Ni–Fe and Ni–Fe/2.5% SiC com-posites in 0.5M NaCl solution using a scan rate of 1mV/s.

nanosized SiC particles in the deposit gives better corrosion resis-tance than a pure layer which is in agreement with our previousstudy for the electrodeposited Ni–SiC nanocomposite [5]. It is con-sideredthatwhenSiCnanosizedparticlesareembeddedinthealloymatrix, the defect size of nanocomposite coating can be reduced.These SiC nanoparticles also act as inert physical barriers to theinitiation and development of defect corrosion, hence improve thecorrosion resistance of the coating [5,32].

4. Conclusion

Ni–Fe/SiC nanocomposite coatings were successfully electrode-posited in the presence of saccharin. The presence of saccharin

was proved to be necessary for obtaining smooth and crack-freedeposits. Saccharin addition also affected the crystallographic tex-ture of the Ni–Fe matrix. It was indicated that as the concentrationof saccharin increased, fiber texture changed from a (200) fibertexture to mixed (3 1 1) and (2 0 0) textures. In this study, it wasestablished that incorporation of SiC nanoparticles suppressed thepreferredgrowthdirection of theNi–Fedeposit,and a morerandomtexture was produced as a result. The texture studies determined(2 0 0) fiber texture of the Ni–Fe/SiC decreased with increasing SiCcontent, in spite of the fact that (11 1) and (3 1 1) fiber texturesdeveloped.

According to the experimental findings, the microhardness andcorrosionresistanceof the nanocompositecoatings wereenhancedwith the increasing of SiC nanoparticles content. Enhanced micro-hardness was attributed to the smaller grain size and dispersionstrengthening effect of the embedded hard SiC nanoparticles.

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Influence of SiC Nanoparticles and Saccharin on the Structu