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Electrochemical behavior of Zn–Co–Fe alloy electrodeposited from a sulfate bath on various substrate materials
⁎Corresponding author. agshammri@imamu.edu.sa (A.G. Alshammari)
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Received: ,
Accepted: ,
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.
Peer review under responsibility of King Saud University.
Abstract
Electrodeposition of ternary Zn–Co–Fe alloy, on copper (high purity 99.9%), AISI 4340 steel, 9021I steel rod (iron 99.98%) and 304-stainless steel substrates, from a sulfate bath was studied. The electrodeposition of Zn–Co–Fe alloy on the various substrate materials was investigated by using cyclic voltammetric (CV) technique, to understand the reduction and oxidation processes occurring at the different electrodes surfaces, and galvanostatic technique to detect the formation of the initial deposits. Also potentiodynamic polarization method was used to assess the corrosion performance of the coating on each substrate material. The results were confirmed using EDXF and SEM analysis which show that the substrate material type influences the electrodeposition process and morphology of the deposits. The obtained results using galvanostatic technique showed that the substrate type affects the deposition potential. The cyclic voltammograms for steel substrate have different behavior than the other used substrate materials; also a clear reduction was shown in the associated charge for copper substrate. The corrosion resistance for Zn–Co–Fe alloy deposited on stainless steel substrate was better corrosion resistant than for a steel rod, steel and copper substrates.
Keywords
Electrodeposition
Corrosion resistance
Ternary Zn–Co–Fe alloy
1 Introduction
The interest in zinc alloys electrodeposits; including Zn–Co and Zn–Fe alloys that have drawn a lot of attention because these alloys exhibit considerably higher corrosion resistance than pure Zn (Fratesi et al., 1994; Zhang et al., 2001; Ortiz-Aparicio et al., 2007; Gharahcheshmeh and Sohi, 2009) and as a substitute for toxic and high price cadmium coatings (Tomachuk et al., 1999; Abou-krisha and Abushoffa, 2007). It is known that from the metallurgical point of view a resulting microstructure morphology strongly affects the material’s properties [e.g. mechanical, electrical and corrosion resistance] (Osorio et al., 2011a,b). Besides, the microstructure array is also intimately associated with the anode/cathode area ratio, and as a direct consequence, with the electrochemical corrosion behavior, as previously reported (Osorio et al., 2011a,b). Furthermore, other properties such as weldability, hardness and ductility of zinc also were enhanced. There is a growing interest on the electrodeposited Zn–Co–Fe alloys because of their superior protective properties (Lodhi et al., 2007a,b). The electrodeposition of these Zn alloys is considered as codeposition of the anomalous type, according to Brenner (1963) who defined the electrochemical deposition process as the less noble metal is deposited preferentially compared to the more noble metal. Although this phenomenon has been known since 1907, the codeposition mechanisms of zinc and metal are not well understood (Growcock and Jasinski, 1989). Several theories have been developed to explain this anomalous behavior (Peter et al., 2010; Chung and Chang, 2009; Koza et al., 2008; Higashi et al., 1981; Lodhi et al., 2008; Chen and Sun, 2001; Matlosz, 1993; Zech et al., 1999).
The aim of the present work was to make a clear influence varying the substrate type on the electrodeposition of Zn–Co–Fe alloy from a sulfate bath by using cyclic voltammetry and galvanostatic measurements and also to investigate the suitable substrate material, which can make the best corrosion resistance and morphology.
2 Experimental
The compositions of the electrolyte used for Zn–Co–Fe alloy electrodeposition consist of ZnSO4 (0.2 mol L−1), CoSO4 (0.2 mol L−1), FeSO4 (0.2 mol L−1), Na2SO4 (0.2 mol L−1), H3BO3 (0.2 mol L−1) and H2SO4 (0.01 mol L−1). All reagents were of analytical grade. Use of the acid sulfate bath is increasing due to its relatively low cost, safety features and pollution control characteristics (Loto, 2012). The pH of electrolyte was 2.50 ± 0.02, and deposition was carried out at 25.0 °C.
The coatings were deposited on various sheets: copper (high purity 99.9%), AISI 4340 low alloy steel (0.41% C, 0.73% Mn, 0.8% Cr, 1.74% Ni, 0.25% Mo and 0.005% Si (wt%)) and 304-stainless steel (Fe, <0.08% C, 17.5–20% Cr, 8–11% Ni, <2% Mn, <1% Si, <0.045% P, <0.03% S) with area 2 cm2, and also 9021I-steel rod (iron 99.98%) with a geometrical area of 0.196 cm2 was used. Before each experiment the surface of steel and stainless steel sheets were etched in 30% HCl for 2 min and 20% HNO3 for copper sheet to activate the surface. Steel rod was handed polish with emery paper (up to 1500 mesh) then immersed in anhydrous ethyl alcohol. Finally, the substrate materials were rinsed with doubly distilled water and then dried. After surface preparations the sheets were immediately placed in the plating bath to prevent formation of an oxide layer on their surfaces. The electrolytic cell was used in the present work as detailed in Abou-Krisha (2005). Before each run, the cell was cleaned with chromic/sulfuric mixture, washed with singly and doubly distilled water and filled with 50 cm3 of the electroplating solution of temperature 25.0 °C. During the experiment the cell was placed in an air thermostat cabinet to make sure adjustment steady temperature of 25.0 °C.
Electrochemical experiments were carried out in a three electrode cell using an EG&G potentiostat/galvanostat model 273A, controlled by a PC using corrosion analysis software model 352. Platinum electrode and saturated calomel electrode (SCE) were used as counter and reference electrodes, respectively. Steel rod that had been placed in a Teflon mounting material and copper, steel and stainless steel sheets were also used as a working electrode. The electrodeposition was done using the galvanostatic method and the potential-time dependence for the deposition of Zn–Co–Fe alloy obtained on different substrates at constant current density 10 mA cm−2 for 10 min at 25.0 °C.
The potential scan was started from 0.0 mV and reversed to −1300 mV in the opposite direction, while potential scan rate was at 5 mV s−1. The potentiodynamic polarization resistance measurements were performed in 0.05 mol L−1 HCl solution. In an environment with the presence of chloride ions, localized corrosion such as pitting and crevice corrosion is still a serious problem for the steel. For this reason, the research study of the passive film of steels and their stability, particularly in chloride solutions has a technological importance.
The surface morphology of the coatings was characterized by Scanning Electron Microscope (SEM) model JSM-5500 LV (JEOL, Japan). The qualitative and semiquantitative chemical analysis of the Zn–Co–Fe alloy was determined via Energy Dispersive X-ray Fluorescence (EDXRF) model JEOL JSX 3222 (JEOL, Japan). The chemical composition of each deposit has been determined by Atomic Absorption Spectrophotometer AA-6701F (SHIMADZU). For this analysis, the deposits were dissolved in 50 cm3 of 30% HCl then diluted with doubly distilled water up to 100 cm3, and analyzed to get the Zn, Co, and Fe contents in the deposits.
The film thickness (Abou-Krisha, 2005) of the deposited alloy layer is valued from the mass of the deposit, the densities of Zn (dZn = 7.14 g cm−3), Co (dCo = 8.90 g cm−3) and Fe (dFe = 7.87 g cm−3) and the surface area (2 cm2). Using the following equation, the thickness can be calculated as the height of the film (h), where mt = total mass of the deposit, sa = surface area, and da = alloy density = [dZn (mZn/mt) + dCo (mCo/mt) + dFe (mFe/mt)], where mZn = Zn amount in the deposit, mCo = Co amount in the deposit and mFe = Fe amount in the deposit. The cathode current efficiency was calculated using the following equation for n as an example of
The values of the electrochemical corrosion measurements of the coatings, the corrosion potential (Ecorr.), the polarization resistance (Rp) and the corrosion current (icorr.) were obtained using the software model 352 and are given in Table 1. The crystalline constituents of the coatings were analyzed by XRD model Bruker Axs-D8 Advance with Cu Kα radiation (λ = 1.5406 Å and 40 mA).
| Parameter | Zn–Co–Fe alloy deposit | ||
|---|---|---|---|
| Copper sheet | Steel sheet | Stainless steel sheet | |
| Zn amount in the deposit (10−5 g) | 46.9 | 49 | 46.5 |
| Co amount in the deposit (10−5 g) | 6.2 | 10 | 18.5 |
| Fe amount in the deposit (10−5 g) | 17.9 | 17 | 22 |
| Total mass of the deposit (10−5 g) | 71 | 76 | 87 |
| Zn content (%) | 66.05 | 64.47 | 53.44 |
| Co content (%) | 8.73 | 13.15 | 21.26 |
| Fe content (%) | 25.21 | 22.36 | 25.28 |
| Zn–Co–Fe deposit current efficiency (eZn–Co–Fe) (%) | 36.76 | 39.35 | 45.64 |
| Thickness of the deposit (μm) | 0.47 | 0.50 | 0.56 |
| Rp (Ohms) | 67.8 | 74 | 91 |
| icorr. (A cm−2 × 10−4) | 9.25 | 6.72 | 5.77 |
| (Ecorr.) Corrosion potential (mV) | −962 | −943 | −924 |
All experiments have been carried out in duplicate; the measurements have shown good reproducibility. For a standard bath deposition, a series of experiments on electrodeposition on steel sheet, as an example, at different times were carried out and the relative standard deviation (RSD%) was found to be 3.5%, 5.2% and 4.3% for the Zn, Fe and Ni contents in the deposit, respectively, and 1.1%, 0.8% and 0.9% for the electrochemical measurements (Ecorr.), (Rp) and (icorr.) respectively.
3 Results and discussion
3.1 Cyclic voltammograms
Fig. 1a shows the cyclic voltammogram curves for Zn–Co–Fe alloy electrodeposited on various substrate materials: Cu, S, S rod and SS with scan rate 5 mV s−1 and at 25.0 °C. The cathodic scan shows two reduction peaks: the first reduction peak (C1), which appears with a small current density (faint peak) with SS, S and S rod substrates, but does not appear with copper substrate, and relates to the codeposition of sulfur from reduction of sulfate group (Abou-Krisha et al., 2008). In Fig. 1b, the cathodic part C1 of (a) is shown in (b), which reveals that there is a reduction peak C1 for copper that is attributed to sulfur, but smaller than for others substrates. The second reduction peak relates to the massive deposition of Zn–Co–Fe alloy which occurs simultaneously with the hydrogen evolution reaction (HER). HER appears as a further increase in the cathodic current density at more negative potentials. The use of SS, S rod, S and Cu substrates affects the deposition potential. The potential necessary to begin the alloy deposition shifted to more negative values for SS, S rod, S and Cu substrates.
(a and b) i–E curves (cyclic voltammograms) for Zn–Co–Fe alloy deposited from Zn–Co–Fe bath obtained on various substrate materials between Ei = 0.0 mV and Ef = −1300 mV and at a scan rate of 5 mV s−1. The cathodic part of (a) is shown in (b).
Several oxidation peaks appeared in the positive scan and their relative size depend on the amount of the deposits (Lodhi et al., 2007a,b) and the type of substrate. These anodic peaks are assigned as follows: shoulder A′ and peak A1 correspond to zinc oxidation to Zn2+, peak A2 to oxidation of iron from FeCo phases and peak A3 to cobalt matrix oxidation of these phases. During the anodic scan, the cyclic voltammogram for Zn–Co–Fe alloy obtained on Cu substrate has very low current density, which means that content of the deposit is low in comparison with SS, S rod and S substrates.
The anodic peak A1 which is attributed to the dissolution of zinc shifts to more positive direction only with S substrate; otherwise, the anodic peak A1 of SS, S rod and Cu substrates does not change. Also, the height of the anodic peak A1 for SS, S rod, S and Cu, shows that the type of substrate has a clear effect on the amount of the deposits formed on the substrate surface. The anodic peak A2 which is ascribed to dissolution of Fe from FeCo phase shifts to more positive direction for either SS or S otherwise S rod and Cu substrates. Also, the height of the anodic peak A2 for SS, S rod, S and Cu, shows that the amount of the deposits changes by changing the substrate. The anodic peak A3 which is ascribed to dissolution of Co from FeCo phase shifts to more positive direction for either SS or S rod but shifts to more negative direction with Cu substrate. An interesting behavior has occurred on S substrate, in the negative direction, the onset of the cathodic process; cyclic voltammogram starts with high anodic current density. Also, from the positive scan; in the last of the anodic process, a sharp increase in the current density occurs. The low alloy steel nature, due to its chemical composition, may be responsible for the positive potential of the anodic dissolution peaks in the cyclic voltammograms. This behavior appears in the presence or absence of metallic ions (Zn, Co and Fe), as can be seen in Fig. 2.
i–E curves (cyclic voltammograms) for steel substrate in solely sulfate bath containing; 0.01 mol L−1 H2SO4, 0.20 mol L−1 Na2SO4 and 0.20 mol L−1 H3BO3 at 25.0 °C, Ei = 0.0 mV and Ef = −1300 mV and at a scan rate of 5 mV s−1.
The cyclic voltammetry measurement in aqueous solution containing solely the bath composition obtained on steel substrate is presented in Fig. 2. As can be seen in the cathodic scan, an anodic peak is observed with high current density 46.5 mA cm−2 which could be attributed to the dissolution of iron with bath. At more negative potential a deposition peak is observed at −760 mV which may be due to the deposition of sulfur from the sulfate group (Abou-Krisha et al., 2008). In the following reverse scan, the cyclic voltammogram does not show well-defined dissolution peaks due to decrease in the current density of corresponding cathodic peak (C1). A sharp increase in the current density takes place starting from −502 mV which may be due to oxygen evolution reaction.
3.2 Galvanostatic technique
The use of the galvanostatic deposition is most useful in detecting the formation of the initial deposits (Gomez et al., 2001). The potential-time dependence for the deposition of Zn–Co–Fe alloy obtained on SS, S rod, S and Cu substrates at constant current density 10 mA cm−2 for 10 min at 25.0 °C is represented in Fig. 3. It could be seen that the deposition potential greatly depends on the substrate type. Low overpotential is needed to create the initial nucleus during the deposition of Zn–Co–Fe alloy on SS substrate. Deposition potential is −1215 mV which takes place at 40 s. On the other hand, high overpotential is needed to create the initial nucleus on copper substrate and grows at high cathodic potential −1260 mV at time about 2 min. Deposition potential for Zn–Co–Fe alloy on S rod and S substrates lies between SS and Cu substrates −1233 mV and −1253 mV, respectively and a moderate overpotential needed to create the initial nucleus. Also deposition of Co and Fe increases by using SS, S rod, S and Cu, respectively in comparison with the deposition of zinc (Table 1).
Galvanostatic deposition and the chronopotentiometric curves for Zn–Fe–Co electrodeposits in the deposition bath obtained on various substrate materials at 10 mA cm−2 for 10 min at 25.0 °C.
3.3 XRD and EDXF measurements
X-ray diffraction measurements are carried out on Zn–Co–Fe electrodeposits which deposited galvanostatically from a sulfate bath, on SS, S and Cu substrates and are presented in Fig. 4a–c. The deposits are composed mainly of Zn and Fe/FeCo phase. Overlay of pure Fe and FeCo phase is observed on XRD analysis (Bai et al., 2003; Zhang and Douglas, 2007). Some researchers have shown that the X-ray analysis is not always able to identify the deposited phases because Zn–Co–Fe alloy is poorly crystallized in a wide range of composition (Alfantazi et al., 1996; Li et al., 2005). Previously (Alfantazi et al., 1997) the effect of S and Cu substrates on electrodeposited Zn–Ni alloy, was found do not have a significant effect on the deposit characteristics.
XRD patterns for Zn–Co–Fe alloy, electrodeposited galvanostatically on (a) copper, (b) steel and (c) stainless steel substrate materials from Zn–Co–Fe bath at 10 mA cm−2 for 10 min at 25.0 °C.
The grain size of the deposited Zn–Co–Fe alloy was calculated using Scherrer’s equation (1) (Sartale and Lokhande, 2001):
The surface chemical composition was obtained by EDX. The EDX spectrums of deposited Zn–Co–Fe alloy obtained on SS, S and Cu substrates are shown in Fig. 5. The presence and the amount of deposited metal depend on the used substrate material. SS substrate has the highest amount of the more noble components cobalt and iron. Cu substrate has the highest amount of the more negative component zinc, so deposition of Zn–Co–Fe alloy is preferable on SS substrate.
EDXF peaks for Zn–Co–Fe alloy, electrodeposited galvanostatically on (a) copper, (b) steel and (c) stainless steel substrate materials from Zn–Co–Fe bath at 10 mA cm−2 for 10 min at 25.0 °C.
3.4 Potentiodynamic measurements
The potentiodynamic polarization curves for Zn–Co–Fe deposits in 0.05 mol L−1 HCl solution at i = 10 mA cm−2 that deposited galvanostatically on SS, S rod, S and Cu substrates from a sulfate bath are shown in Fig. 6a and b. The corrosion potentials (Ecorr.) measured from Fig. 6a for Zn–Co–Fe deposit on SS, S rod, S and Cu substrates are −924, −930, −943 and −962 mV, respectively. Fig. 6b indicates that there is a difference between Tafel’s slopes for different substrates. These differences in Ecorr. may be attributed to the nature of each substrate surface or to the changes in the electrode potentials of each substrate. SS substrate exhibits enhanced corrosion performance, with the noblest (less negative) corrosion potential. The improvement was achieved in the corrosion resistance of deposits due to the use of various substrate materials, which may be responsible for increasing the content of the nobler elements in the coating and increasing the thickness of the deposit. Also, the corrosion resistance of the deposits on SS substrate increases may be attributed to the noble nature of SS which resulted in a little interaction with its surface and the alloy components.
(a) Log i–E and (b) i–E curves for Zn–Co–Fe alloy, electrodeposited galvanostatically on a – copper, b – steel, c – steel (rod) and (d) – stainless steel substrate materials from Zn–Co–Fe bath at 10 mA cm−2 for 10 min at 25.0 °C, in 0.05 mol L−1 HCl solution at a scan rate of 5 mV s−1 at 25.0 °C.
3.5 Surface morphology
Fig. 7 shows the SEM images for Zn–Co–Fe alloy deposits from the plating bath, and the morphology of the deposit indicates a clear difference in each substrate material. The deposit of the alloy on S substrate is clusters and on Cu substrate is not compact and without any homogeneity. The surface morphology of SS substrate represents the compact and homogeneous deposits.
SEM photograph for Zn–Co–Fe alloy, electrodeposited galvanostatically on copper, steel and stainless steel substrate from Zn–Co–Fe bath at 10 mA cm−2 for 10 min at 25.0 °C. (a) Electrodeposited Zn–Co–Fe on copper sheet. (b) Electrodeposited Zn–Co–Fe on steel sheet. (c) Electrodeposited Zn–Co–Fe on stainless steel substrate.
The SEM pictures of the deposit corresponding to SS, S and Cu show that the morphology of the final deposits varies significantly with the use of different substrates and illustrate that SS minimizes the dendrite formation and leads to more homogeneous deposits.
3.6 The chemical composition of Zn–Co–Fe deposit
Influence of Cu, S and SS substrate materials on the chemical composition of Zn–Co–Fe alloy deposit is shown in Table 1. SS substrate has the lowest zinc percentage in the deposit (53.44%), and the highest cobalt and iron contents in the deposit (21.26% and 25.28%, respectively) otherwise with Cu and S substrates, the zinc percentage of the deposit (66.05% and 64.47%, respectively), iron percentage (8.73% and 13.15%, respectively) and cobalt percentage (25.21% and 22.36%, respectively). This decrease in zinc content and the increase in cobalt and iron contents on SS substrate lead to an increase in the alloy current efficiency 45.64% and increase in the thickness of the deposit 0.56 μm, and according to these results Zn–Co–Fe alloy deposits on SS substrate produce higher corrosion resistance in comparison with Cu and S substrates.
4 Conclusions
The main conclusions of this research investigation are the following:
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The type of substrate influences both the electrodeposition process and the alloy morphology.
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The cyclic voltammograms of steel substrate have different behavior than the other substrate materials, at which the onset of the cathodic process takes place in the anodic scan at the more positive potential and the final of the anodic process increases the current density violently. The low alloy steel nature, due to its chemical composition, may be responsible for these manners. This behavior appears in the presence or absence of metallic ions (Zn, Co and Fe).
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SEM micrographs demonstrated that stainless steel exhibited more preferred surface morphology and high quality deposits.
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XRD analysis showed that the deposits are composed mainly of Zn and Fe/FeCo phase.
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EDXF patterns and AAS analysis indicated that the stainless steel substrate has higher amount of Fe and Co than steel and copper substrates but copper substrate has the highest amount of Zn. This is may be due to that SS enhanced the normal codeposition.
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The corrosion resistance of the deposited Zn–Co–Fe alloy on stainless steel substrate was better corrosion resistant than for a steel rod, steel and copper substrates. The high corrosion resistance of SS substrate is attributed to that can help in the defect areas of the electrodeposit in addition to the morphology and chemical composition of the electrodeposit on SS.
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