Combustion synthesis of Ni doped SnO2 nanoparticles for applications in Zn-composite coating on mild steel

Among Zn-Ni doped SnO 2 com- posite coatings, the Zn-1.5 g/L Ni doped SnO 2 composite coating posses less E corr via 1.121 V, indicating the less response of a Zn- composite coated stee[r]

Original Article

in Zn-composite coating on mild steel

Department of Studies in Chemistry, School of Chemical Sciences, Kuvempu University, Shankaraghatta, 577451, Shimoga, Karnataka, India

a r t i c l e i n f o

Article history:

Received 3 June 2018

Received in revised form

14 November 2018

Accepted 18 November 2018

Available online 24 November 2018

Keywords:

Ni doped SnO 2 nanoparticles

Zn-composite coating

Corrosion behavior

Tafel polarization

EIS

a b s t r a c t

Zinc (Zn)-composite coatings are still in demand as good corrosion barrier coatings to protect steel substrates from corrosion environment In this article, the Ni doped SnO2nanoparticles were synthesized and used as a composite additive for Zn-coating The synthesis was carried out by the combustion method using citric acid as a fuel The Zn-Ni doped SnO2composite coating was produced on mild steel

by an electroplating technique The surface characterization and elemental analysis of the coated samples were examined by X-ray diffraction spectroscopy (XRD), scanning electron microscopic images (SEM) followed by energy dispersive spectroscopy (EDAX) The surface morphology of Zn-Ni doped SnO2

composite before and after corrosion showed a more compact surface structure with respect to the pure Zn-coat The corrosion resistance property of the Zn-Ni doped SnO2composite coating was studied by Tafel polarization and electrochemical impedance spectroscopy

© 2018 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)

1 Introduction

The steel materials have diverse applications throughout the

world in variousfields because of the ease of production, availability,

low-price and better mechanical strength The main drawback of

these materials is‘corrosion’ in their applications which leads to

economic problems The diversity in applications of steel made it so

important to protect from corrosion process[1e3] The study on the

protection of steel substrates from corrosion phenomena was an

interesting research topic since many years Considering the

corro-sion problem of steel metals, investigations were focused on the

development of protective layers on the surface of a steel substrate

by an electrochemical process [4,5] The electroplating technique

has been widely applied to the surface treatment of steel substrates

to achieve better corrosion resistance properties of steel[6,7] The

deposition of metallic layers on steel substrates involved the

elec-trolysis of certain metals like Zn, Ni, Cu, Sn etc., provided a good

corrosion protection under aggressive atmosphere[8e10] Indeed,

the chrome coating provided an excellent corrosion passivation for

the steel surface from the surrounding environment thereby

corrosion resistance of the steel metal was sacrificial The chrome

passivation, however, has been prohibited due to the toxicity

towards the environment Thus, it is of essential to develop non-toxic and longer life spanned surface coating for steel surface pro-tection[11,12] Among various coatings, zinc coating found much importance because of its broad range of applications in the auto-mobile industry, construction platforms and also marine applica-tions thanks to cost friendly and good mechanical property The presence of the salinity in the marine environment causes the deterioration of Zn-coated steel substrates which affects the service life of the Zn-coating[13] In recent years, efforts have been moved

on to Zn-composite coatings due to their better corrosion resistance property compared to pure Zn-coating The extensive research on composite materials for Zn-composite coating was focused on the utilization of metal oxides[14], carbides[15], nitrides[16], polymers

[17] These coatings improved the corrosion resistance properties of Zn-coating with respect to the pure Zn-coating in the presence of a corrosive atmosphere Amongst, the metal oxide nanoparticles received more attention due to their availability and low cost of preparation[18,19]

Nowadays, doped metal oxides and mixed metal oxides exhibit remarkable physical and chemical properties Practically, Zn-1% Mn-doped TiO2composite coating on the steel substrate has been studied by Kumar et al [20] They obtained a better corrosion resistance property in comparison to the Zn-composite coating The corrosion resistance property and tribological properties of

Zn-Al2O3-CrO3-SiO2 have been reported by Malatji et al [21] The observed results signified the enhanced anticorrosive property of

* Corresponding author Fax: þ91 08282 256255.

E-mail address: drtvvenkatesha@yahoo.co.uk (T.V Venkatesha).

Peer review under responsibility of Vietnam National University, Hanoi.

Contents lists available atScienceDirect Journal of Science: Advanced Materials and Devices

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 s a m d

https://doi.org/10.1016/j.jsamd.2018.11.005

2468-2179/© 2018 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license

Journal of Science: Advanced Materials and Devices 3 (2018) 412e418

Zn-mixed metal oxides composite coating A good improvement

was reported for Zn-TiO2-WO3composite coating[22]

The present effort focused on increasing the service life of

Zn-coating with the reinforcement of Ni doped SnO2nanoparticles as

a composite additive in the Zn-matrix The tin metal and its oxides

have many applications in various fields because of its better

thermal stability and good mechanical property SnO2is a n-type

semiconductor metal oxide having a bandgap of 3.6 eV[23,24] The

research on SnO2metal oxide nanoparticles as a composite material

in zinc coating has been investigated by Fayomi et al.[25] They

found that the anticorrosive and tribological properties of

Zn-Al-SnO2composite coating were satisfactorily good compared with

that of Zn-Al alloy coating To our best knowledge, no work has

been found regarding incorporation of Ni doped SnO2nanoparticles

as a composite additive in Zn-coating for corrosion protection of

steel

2 Experimental

2.1 Materials and synthesis methods

Nickel (II) chloride heptahydrate (NiCl2$7H2O) was supplied

from Himedia Laboratories Pvt Ltd Mumbai Tin (II) chloride

dihydrate (SnCl2$2H2O) was received from Merck Life Science Pvt

Ltd Mumbai Citric acid anhydrous was arrived from Merck

Spe-cialties Pvt Ltd Mumbai and Millipore water In a typical synthesis

of Ni doped SnO2 nanoparticles, salt precursors of SnCl2$2H2O,

NiCl2$7H2O and citric acid as a fuel were taken as 1:1 ratio and

completely dissolved in a dilute HNO3solution to get a combustion

mixture Afterward, the solution mixture was heated on a hotplate

with constant stirring until a solution mixture converted into a gel

form[26e28] The gel was transferred into a quartz crucible and

kept into a preheated furnace maintained at 400C Within a few

seconds, precursor gel gets boiled and ignited Then the crucible

was taken out and kept for cooling for few minutes at atmospheric

temperature The product wasfinely grounded in an agate mortar

and calcined for 2 h at 500C Scheme 1illustrated the

experi-mental steps involved during the synthesis of Ni doped SnO2

nanoparticles

The crystallite size of Ni doped SnO2 was determined by

Powder x-ray diffraction analysis (PANalytical X'pert pro powder

diffractometer, lKaCu ¼ 1.5418 Å) The surface morphology and

percentage composition of the prepared products were studied by

scanning electron microscopic photographs (FESEM-Carl ZEISS,

Supra 40 VP) followed by energy dispersive spectroscopy

2.2 Fabrication of Zn and Zn-Ni doped SnO2composite coatings

The electroplating bath composition and parameters were listed

inTable 1 Steel substrates with dimensions of 4 4  0.1 cm3were

used as cathode substrates and zinc sheets of the same dimension

were used as anode materials Before electroplating experiment,

the surface cleaning of steel plates was carried out using emery

papers and acetone Finally, plates were rinsed with distilled water and used The zinc sheets were plunged in 5% HCl to activate the surface of the anode material each time[29] The bath solution prepared for Zn-Ni doped SnO2composite coating has been stirred for 10 h to prevent the agglomeration of nanoparticles.Scheme 2

demonstrates the experimental setup carried out for generation

of the Zn-Ni doped SnO2composite coating

The fabricated Zn and Zn-Ni doped SnO2 coatings were sub-jected to electrochemical corrosion studies of Tafel and electro-chemical impedance spectroscopy (EIS) using potentiostat CHI660C electrochemical workstation The EIS studies were executed at the open circuit potential (OCP) with frequency ranging from 0.1 Hz to

10 kHz and amplitude of 5 mV The morphology and composition of the deposits were scrutinized by XRD, scanning electron micro-scopic images and energy dispersive spectral investigation

3 Results and discussion 3.1 XRD analysis

Fig 1depicts the XRD patterns of as-prepared Ni doped SnO2 nanoparticles The characteristic peaks corresponding to Miller indices at (110), (101), (200), (111), (210), (211), (220), (002), (310), (112), (301), (202) and (321) confirmed that the prepared product is

a tetragonal structured SnO2 [30e32] No impurity peaks were appeared indicating the formation of a single phase tetragonal shaped Ni doped SnO2 The DebyeeScherer equation was applied to calculate the crystallite size of the particles:

D¼ Kl

where D is the diameter of the crystallite size,lis the wavelength of the radiation source, K is the shape factor (0.9),qis the Bragg's angle and b is the angular peak width at half maximum intensity (FWHM) The calculated average crystallite size was found to be 27.70 nm

3.2 SEM with EDAX studies The surface morphology and elemental analysis of the prepared nanoparticles were displayed inFig 2 As can be seen that the par-ticles appeared like agglomerated spherical shaped flakes like morphology of Ni doped SnO2nanoparticles The elemental compo-sition showed that the presence of Ni, Sn and O with the percentage

of constituents and there was no foreign elements were observed 3.3 Characterization of the coatings

The XRD patterns of the Zn and Zn-Ni doped SnO2coatings are represented inFig 3 The crystallite size was calculated using Debye Scherer equation and the obtained size for zinc coating was 33.88 nm and for Zn-composite coating it was 28.48 nm The characteristic

K Deepa, T.V Venkatesha / Journal of Science: Advanced Materials and Devices 3 (2018) 412e418 413

peaks at (102) and (103) planes showed the highest intensity in case

of pure Zn-coating and they are decreased for Zn-Ni doped SnO2

composite coating This finding indicated that the presence of Ni

doped SnO2 nanoparticles inhibited the crystal growth thereby

reduced the grain size[33,34] The reduction in grain size on the zinc

surface leads to a compact structured surface and less number of surface pores

SEM photographs of pure Zn coatings and Zn-Ni doped SnO2 composite coatings were represented inFig 4 The pure zinc deposit was accompanied with some gaps and micro holes on its surface as displayed inFig 4(a) These micro-holes were greatly reduced and nearly absent in the Zn-Ni doped SnO2 composite deposit, which exhibitedfine compact structured surface morphology as shown in

Fig 4(b)[35,36] It can be seen that the reduced grain size leads to the formation of tiny Znfibers like compact surface morphology in the case of Zn-Ni doped SnO2composite coated steel surface compare to pure Zn deposit The energy dispersive spectrum demonstrated in

Fig 5indicates the presence of Ni doped SnO2nanoparticles in the Zn-composite matrix

3.4 Electrochemical corrosion studies 3.4.1 Tafel

The Tafel plots were recorded for the study of the corrosion resistance property in terms of the polarization resistance behavior

of the electrodeposited samples in 3.65% NaCl solution as corrosion media In order to measure the corrosion resistance property of the deposits, the electrolytic cell was used, in which the platinum wire

is served as an auxiliary electrode, calomel electrode as a reference electrode and coated specimens as the working electrodes Initially, the coated samples were dipped in the corrosive electrolyte solu-tion to attain the OCP The potential varies with respect to the time

Table 1

Bath composition and operating parameters.

Cathode: mild steel plate Current density: 3 A/dm 2

Plating time: 10 min Stirring speed: 300 rpm pH: 3 Temperature: 303 K

Na 2 SO 4 -40 g/L

H 3 BO 3 -12 g/L SLS-0.5 g/L

1(a)þ Ni doped SnO 2 1.5 g/L Z III

Scheme 2 Electroplating setup for the Zn-Ni doped SnO 2 composite coating.

Fig 1 XRD patterns of Ni doped SnO 2 nanoparticles.

K Deepa, T.V Venkatesha / Journal of Science: Advanced Materials and Devices 3 (2018) 412e418 414

and attained a steady state potential (referred to as OCP)[37,38] The electrode potential of the working electrode was polarized in the range ofþ200 mV anodically and 200mv cathodically with respect to their OCP The Tafel plots are depicted in Fig 6 The electrochemical parameters such as Ecorr(corrosion potential), Icorr (corrosion current), Rp(polarization resistance) were recorded and Fig 2 SEM image with EDAX analysis of Ni doped SnO 2 nanoparticles.

Fig 3 XRD patterns of Zn and Zn-Ni doped SnO 2 deposits Fig 5 Energy dispersive spectrum of Zn and Zn-Ni doped SnO 2 composite deposits.

K Deepa, T.V Venkatesha / Journal of Science: Advanced Materials and Devices 3 (2018) 412e418 415

results were tabulated inTable 2 It can be observed that the Ecorr

value of Zn-coating was1.138 V and it was slowly reduced with

the addition of Ni doped SnO2nanoparticles in Zn-coat

(concen-tration varying from 0.5 to 2 g/L) Among Zn-Ni doped SnO2

com-posite coatings, the Zn-1.5 g/L Ni doped SnO2 composite coating

posses less Ecorrvia1.121 V, indicating the less response of a

Zn-composite coated steel metal surface towards corrosion

atmo-sphere Similarly, the corrosion current (Icorr) was higher for pure

Zn deposit and it gradually reduced for Zn-composite deposits The

optimum composite coating has been achieved at 1.5 g/L

nano-particles concentration The corrosion rate (CR) of the respective

coatings was calculated by the following equation

CRðmpyÞ ¼0:13 IcorrðEq:wtÞ

The Zn-coating at Zn-1.5 g/L of Ni doped SnO2 nanoparticles

concentration yields a good corrosion resistance property

compared to the all other concentrations The increased amount of

nanoparticles caused the reduced polarization resistance behavior

This is due to the fact that the agglomeration of nanoparticles at

higher concentration leads to the poor adhesion on the surface and

slows down the deposition process [39,40] Hence the further

addition of nanoparticles in Zn-coating was stopped after the Zn-2

g/L Ni doped SnO2deposition

3.4.2 Electrochemical impedance spectroscopy

The corrosion resistance property of the prepared coated

sam-ples was examined by EIS test carried out in 3.65% NaCl solution at

OCP value of the respective coated sample EIS measurements were

recorded as Nyquist and bode plots at the frequency range of

0.1 Hze10 kHz with amplitude of 5 mV as shown inFigs 7 and 9

Noted that the measured Nyquist plots shown in Fig 7 was

matched with the suitable equivalent circuit model using Z-simp

win 3.21 software given inFig 8 The obtained experimental data

are tabulated inTable 3 The circuit was composed of the coating resistance (Rcoat), the coating capacitance (Qcoat), the double layer capacitance (Qdl) and the charge transfer resistance (Rct) The capacitance was replaced by a constant phase element to achieve good results of thefitted circuit with experimental EIS plots The constant phase element (CPE) implies the departure from the ideal capacitance behavior of the working electrode thanks to the surface inhomogeneity and micro-roughness[41,42] The impedance ob-tained by CPE was given by

where Y0is CPE constant, i2¼ 1, an imaginary number,uis the angular frequency and n represents the component of CPE which provides the details regarding the degree of the inhomogeneity of the metal surface, micro-roughness and porosity[43]

The Qdl and Qcoat values of a pure Zn-coating was higher compared to that of the Zn-Ni doped SnO2composite coating The presence of Ni doped SnO2nanoparticles in the Zn-composite pro-vided a more stability for coated surface and formed a strong corrosion barrier under corrosive atmosphere The lower Rctvalue

Fig 6 Tafel plots of Zn and Zn-composite coatings.

Table 2

Tafel parameters.

Samples E corr (V vs SCE) I corr  10 5 (A/cm 2 ) ebc (V1dec) ba (V1dec) LP (Ucm 2 ) Corrosion rate  10 5 (g/h)

Fig 7 Nyquist plots of Zn and Zn-Ni doped SnO 2 composite coatings.

Fig 8 Equivalent circuit model matched with Nyquist plots.

K Deepa, T.V Venkatesha / Journal of Science: Advanced Materials and Devices 3 (2018) 412e418 416

for Zn-Ni doped SnO2 composite coating compared to pure Zn-coating indicated a reduced number of surface active pores which are the cause of corrosion reactions The incorporation of Ni doped SnO2nanoparticles in Zn-coating accumulates the surface pores and thereby slows down the corrosion reactions at the interface of the metal surface and electrolyte in aggressive media [36,44] The corrosion resistance property was satisfactory at the Zn-1.5 g/L Ni doped SnO2 composite coating Further increase of the Ni doped SnO2 concentration in the zinc matrix results in a decreased impedance of the deposit Hence, the 1.5 g/L concentration of the Ni doped SnO2composite additive has been considered as an optimum concentration for the good Zn-composite coating The polarization resistance (RP) was given by the sum of the resistances of Rcoatand

Rct The Zn-Ni doped SnO2composite coating has higher RPvalue in view of more corrosion resistance property compared to pure zinc coating Similar results have been observed in bode plot and bode phase angle plot as displayed inFig 9a,b in which higher modulus impedance was observed for the Zn-1.5 g/L Ni doped SnO2 com-posite coating and it was lesser for pure Zn-coating Also, a maximum phase angle was attained for the Zn-Ni doped SnO2 composite coating due to the more homogeneous surface with good corrosion resistance property of Zn- Ni doped SnO2 composite coating

3.4.3 Corrosion morphology The SEM images depicted inFig 10 shows that the corroded surface morphology captured after corrosion studies in 3.65% NaCl solution The surface of pure Zn coated specimen was highly deteriorated and some cracks were also observed in Fig 10(a) This indicates the poor corrosion resistance property under cor-rosive environment The Zn-1.5 g/L Ni doped SnO2 composite coated surface exhibited a little effect on the corrosion reactions

as shown inFig 10(b) Here, less deterioration and no cracks were appeared on the surface The presence of Ni doped SnO2 nano-particles in Zn-matrix provided a strong corrosion barrier in corrosion media

Fig 9 Bode magnitude plot (a) and Bode phase angle plot (b) of Zn and Zn-Ni doped

SnO 2 composite coatings.

Table 3

EIS parameters.

Samples Q coat (S nU1 cm2) n Q dl (S nU1 cm2) n C dl (F/cm 2 ) RP¼(R coat þ R ct ) (Ucm 2 )

K Deepa, T.V Venkatesha / Journal of Science: Advanced Materials and Devices 3 (2018) 412e418 417

4 Conclusion

The Ni doped SnO2nanoparticles were prepared by combustion

method The Zn-Ni doped SnO2composite coating was fabricated

by an electroplating technique X-ray-diffraction study revealed the

nano size of the Ni doped SnO2particles Surface morphology of Ni

doped SnO2showed the spherical nanoflakes structure The EDAX

analysis confirmed the percentage composition of the prepared

nanoparticles The Zn-Ni doped SnO2composite coating exhibited

an improved surface texture The incorporation of the Ni doped

SnO2particles in the Zn-composite coating was confirmed by the

EDAX analysis The Tafel and electrochemical impedance studies

proved that the presence of the Ni doped SnO2 in Zn-coating

increased the corrosion resistance property of Zn-deposit as

compared to pure Zn-deposit

Acknowledgments

The authors gratefully acknowledge the Department of

Chem-istry, Kuvempu University, Jnana Sahyadri, Karnataka, India for lab

facilities to complete the present work and also UGC-New Delhi,

Government of India for providing UGC-BSR Fellowship (Order No

F, 25-1/2013-14(BSR) 7-229/2009)

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