10. Characterization of Electrodeposited Nickel Coatings From Sulphamate Electrolyte Without Additive

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Characterization of electrodeposited nickel coatings from

sulphamate electrolyte without additive

A. Godona, J. Creusa, X. Feaugasa, E. Confortob, L. Pichonc, C. Armandd, C. Savalla,

aLaboratoire d'Etudes des Matriaux en Milieux Agressifs, EA3167, Universit de La Rochelle, Av. Michel Crpeau, F-17042 La Rochelle,

FrancebFdration de Recherche en Environnement pour le Dveloppement Durable (FR-EDD), FR CNRS 3097, Centre Commun Analyses,

Universit de La Rochelle, 5 Alle de l'Ocan, F-17042 La Rochelle Cedex 9, FrancecInstitut Pprime, UPR 3346 CNRS, Universit de Poitiers, SP2MI, Boulevard Marie et Pierre Curie, BP 30179, 86962 Chasseneuil,

Futuroscope Cedex, FrancedINSA Toulouse, Dpartement de Physique, 135 avenue de Rangueil, 31077 Toulouse Cedex 4, France

A R T I C L E D A T A A B S T R A C T

Article history:

Received 28 June 2010

Received in revised form

25 October 2010

Accepted 18 November 2010

In this paper, the influence of deposition current density on microstructure and purity of

nickel coatings was studied. Complementary characterization methods (SEM, TEM, XRD,

EBSD, GDOES and SIMS) were used to investigate different scales of the microstructure and

to understand the metallurgical states of the coatings. As deposition current density

decreases, grain refinement and texture modifications are observed which are linked with

the grain boundary character (disorientation angle and Coincidence Site Lattice). Moreover,

in sulphamate bath without additive, the contamination by light elements and metallic

impurities strongly depends on deposition parameters and must be taken into account to

discuss the microstructure changes.

2010 Elsevier Inc. All rights reserved.

Keywords:Electrodeposited nickel

Grain refinement

Grain boundaries

EBSD

Chemical composition

1. Introduction

Nanocrystalline materials have been the subject of intensive

research because of their unique properties [13]. For example,

concerning the corrosion resistance of pure metals, severalworks report that the susceptibility to localized corrosion is

lower in nanocrystalline materials[46], but the mechanisms

responsible for this superior corrosion resistance are not

clearly established [5,7]. As corrosion resistance can be

affected by several metallurgical parameters (defects, grain

size, grain boundary, purity, crystallographic texture, rough-

ness, etc.), a careful control of microstructure is necessary.

Nanocrystalline nickel with a grain size below 100 nm was

obtained by electrodeposition but deposition parameters

largely vary from one study to another. For example, in

additive-free Watts bath[8] ultra-fine-grained nickel electro-

deposits (grain size down to 100 nm) were obtained by pulseplating at very high pulse-current. By using organic additives

(especially saccharin in the case of nickel), several studies

show that it was possible to produce nanocrystalline nickel

coatings in different baths with grain sizes in the range of 6

100 nm[6,8,9]. It was shown that the use of organic additives

leads to an increase of the contamination of coatings[10,11],

which can affect both mechanical properties and corrosion

M A T E R I A L S C H A R A C T E R I Z A T I O N 6 2 ( 2 0 1 1 ) 1 6 4 1 7 3

Corresponding author.Tel.: +33 5 46 45 72 93; fax: +33 5 46 45 72 72.E-mail address:[email protected](C. Savall).

1044-5803/$ see front matter 2010 Elsevier Inc. All rights reserved.doi:10.1016/j.matchar.2010.11.011

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resistance. Few studies have tried to explain the influence of

deposition parameters by a careful analysis of the microstruc-

ture [8,12]. In most cases, only one parameter is studied,

mainly grain size which is evaluated by analyzing the

broadening of the diffraction peaks [3,9,13] or by scanning

electron microscopy[14,15]. However, it was shown that for

the same electrodeposited nickel sample, the size of structural

elements can largely vary depending on the observation tool,and thus the microstructure needs to be evaluated at different

scales[11].

Among the different baths, sulphamate based bath is of

particular interest as it leads to ductile deposits with low

internal stress [17,18], even without sulphur (S) containing

additive[16].

In this paper, an additive-free sulphamate bath is used in

order to limit the incorporation of impurities and especially S

because of its dramatic effect on corrosion resistance. The

influence of current density on the microstructure and on

contamination of nickel coatings is studied by using different

characterization methods. The correlation between structural

observations at different scales and chemical analysis allows

understanding the metallurgical states of the coatings.

2. Material and Methods

Nickel coatings were prepared by direct-current galvanostatic

deposition in a three-electrode cell by using a VSPpotentiostat

from Biologic. A conventional sulphamate bath (V=400 mL)

without additive was used, and composed of 300 g/L Ni(NH2SO3)2.4H2O, 15 g/L NiCl2.6H2O, and 30 g/L H3BO3. Solutions

were prepared by dissolving pure salts in ultrapure water

(18.2 M cm) and pH was then adjusted to 4.2 by adding nickel

carbonate. Special attention was devoted to avoid contami-

nation of the bath. A thermostated glass reactor was used to

fix the temperature at 50 C and the solution was mechani-

cally stirred during the deposition. The anode was of pure

nickel (99.99%) and embedded in a polypropylene anode bag.

Nickel substrates (S= 2 cm2) were polished with silicon carbide

(particle size 5 m), sonicated for 2 min, rinsed with ultrapure

water and dried before electrodeposition. Deposition current

density wasvaried between 1 and50 mA/cm2. In thefollowing,

the nomenclature of samples (Table 1) refersto this deposition

parameter (for example CD 1 refers to a deposition current

density of 1 mA/cm2). Cathodic efficiency was estimated by

weighting the samples before and after deposition. Deposition

time was adjusted to obtain thicknesses of 50 m.

Thesurfacemorphology was observedby scanningelectron

microscopy (SEM) with a FEIQuanta 200ESEM-FEG operatingat

20 kV as acceleration voltage. Electron backscatter diffraction

(EBSD) was used to obtain grain size and to characterize

microtexture and grain boundaries. For top-view EBSD analy-

ses, samples of 75 m thickness were electrodeposited and

then electropolished in a H2SO4/CH3OH mixture [19] in order to

remove 25 m. After electropolishing, samples were very flat,with a roughness below 2 nm (estimated by Atomic Force

Microscopy experiments). For cross-section EBSD analyses,

samples were cut with a wire saw and cross-sections were

mechanically polished. A final polishing was performed with

OPSpreparation fromStruers. EBSDmaps wereacquired at half

of the coating thickness using an acceleration voltage of 25 kV

on SEMand theTSL OIMData collection 5 Software, with a step

size of 30 nm or 70 nm, dependingon thegrainsize. A clean-up

was performed on maps in order to remove points which were

not indexed or to index according to the first neighbours those

which were originally incorrectly indexed. Grain size and

orientation pictures were then calculated using TSL OIM

Analysis 5 software.

Complementary transmission electronic microscopy (TEM)

observations were carried out with a JEOL JEM 2011 electron

microscope operating at 200 kV. Foils for TEM were thinned in

double twin-jet electro-polisher using an electrolyte of 25%

nitric acid and 75% methanol at a temperature of 30 C and a

current of 150 mA. To understand the microstructure observed

at high current density, TEM observations were also per-

formed on the cross-sections of sample CD50. For this

specimen, stereographic analyses (stereographic projection)

were established for each observed grain in order to evaluate

the orientation of each grain. Special care was taken in the

marking of TEM specimens. So, the direction of the normal of

the electrodeposited surface was identified on the stereo-

graphic map of each studied grain.

X-ray diffraction analyses in 2 mode were performed on

a Brucker apparatus (AXS D8-Advanced) with the Cu-K

radiation (=0.15405 nm). Spectra were acquired between 40

and 100, with a step width of 0.02 and the K2 peak and

background were removed. Composition analyses were

obtained by Glow Discharge Optical Emission Spectrometry

(GD Profiler from Horiba Jobin Yvon). Secondary Ion Mass

Spectrometry (IMS 4FE6 from CAMECA) was also used with

two ionic sources Cs+ (at 14.5 keV) and O2+ (at 5.5 keV) to obtain

the best sensitivity. Concentration profiles were acquired after

a pulverization of 5 to 10m in order to avoid surface

contamination effects. All atomic elements were analyzed

except nitrogen. For both methods, the detection limit for this

element was too high. Calibration with bulk nickel samples of

known composition was performed for quantitative analysis.

Several profiles were obtained for each sample, leading to

reliable results. However, due to the small volumes which are

analyzed by these techniques, concentration values cannot be

given with a high accuracy.

3. Results

Theaim of this work is tousecomplementary analyses toobtain

an overview of the metallurgical state of electrodeposited

Table 1 Mean sizes deduced from SEM, EBSD and TEMfor coatings elaborated at different current densities.

Name jmA/cm2

(SEM)m

d (EBSD)m

d (TEM)m

CD1 1 0.37 0.25 0.120

CD5 5 0.74 0.35 0.180

CD10 10 1.4

CD20 20 3.9

CD50 50 4.3 1.02

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coatings.Section 3.1describes surface morphologies in relation

with SEM observations.Section 3.2outlines the interest to use

X-ray diffraction analyses to study the macroscopic texture and

to extract dimensional data. The followingSections 3.3 and 3.4

deal with the opportunity to obtain spatial information using

EBSD maps and TEM analyses. Finally, chemical composition

was analyzed in connection with structural results.

3.1. Scanning Electron Microscopy

SEM views presented inFig. 1show the surface morphology of

coatings prepared at different current densities. At high

current densities, largecrystallites with a truncated pyramidal

shape are observed leading to bright deposits in good

agreement with previous results in sulphamate bath [12,15].

A strong hydrogen evolution leads to the formation of bubbles

and edge effects at current densities above 50 mA/cm2. As the

current density decreases, this pyramidal morphology is

replaced by a nodular morphology. The mean size of the

nodules deduced from SEM was estimated by statistical

analyses of images obtained at different magnifications

(Table 1). The values suggest a refinement at low current

density. However, the morphological features observed by

SEM cannot be directly assigned to grains and other charac-

terization tools will be used below to clarify this point.

3.2. X-ray Diffraction Analysis

The diffraction patterns for different deposition current

densities are plotted onFig. 2. At high current density (above

30 mA/cm2), a strong crystallographic texture along the direction is observed, which is replaced by a preferred

orientation at currentdensities below 20 mA/cm2. At 1 mA/cm2,

no preferred orientation is observed but the (220) line is

slightly high and the (200) one is slightly low respectively to a

non texture nickel sample (JCPDS data no. 00-004-0850).

Complementary texture analysis by using inverse pole figures

obtained by EBSD will be presented inSection 3.3, confirming

the above results. For coating CD1, a broadening of the

diffraction peaks can be noticed, suggesting a grain refinement

effect. Assuming a Cauchy-shaped profile, the full width at

half maximum (FWHM) was evaluated for each diffraction

peak, after correction by the experimental broadening esti-

mated by using the LaB6 standard sample. The Scherrer

equation obviously led to a strong underestimation of

the grain sizes of these coatings. So, an approach based on

Fig. 1 SEM top viewsshowingthe surface morphology of the coatings deposited at different current densities. (a: CD1 (1 mA/cm2),

b: CD5 (5 mA/cm2), c: CD10 (10 mA/cm2), and d: CD50 (50 mA/cm2)).

166 M A T E R I A L S C H A R A C T E R I Z A T I O N 6 2 ( 2 0 1 1 ) 1 6 4 1 7 3
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WilliamsonHall diagrams was used in order to estimate

crystallite sizes and internal stresses. The approach developed

by Reimann[20] and used by Thiele [11] in electrodeposited

nickel was followed, which takes into account the elastic

anisotropy of nickel.

The WilliamsonHall plots obtained for coatings deposited

at 1 mA/cm2 (CD1) led to a mean internal stress (1/2)

of 300 MPa. This value is in the range of those previously

reported in electrodeposited nickel [11] which showed an

increase of mean internal stress as the grain size decreases.

The mean size of coherent scattering regions for sample CD1

deduced from this analysis is around 130 nm. For coatings

deposited at higher current densities, the broadening of the

diffraction peaks is smaller. Moreover, for these coatings, the

presence of a crystallographic texture does not allow this

approach.

3.3. Electron Backscatter Diffraction

Top-view orientation maps for coatings elaborated at different

current densities are presented onFig. 3. Inverse pole figures

were calculated from these orientation maps, showing the

orientation densities for the different crystallographic direc-

tions parallel to the sample normal direction. The preferred

orientation along the direction suggested by 2XRD

scans for coatings prepared at 50 mA/cm2 (CD50) is confirmed.

Comparison with SEM views shows that the large truncated

pyramidalstructures are mainly oriented with their axis

perpendicular to the substrate surface. Between these pyra-

midal grains, much smaller grains are found, with different

crystallographic orientations. Even if a preferred orientation

along the direction is found for the coating prepared at

5 mA/cm2 (CD5), the texture is less marked (as the proportion

of pixels which crystal direction is disoriented versus the

sample normal direction is higher). For the coating deposited

at the lowest current density (CD1), the crystallographic

texture along the direction is very weak, in accordance

with 2 XRD scans. Grain boundary position is super-

imposed as grey lines to the orientation maps of Fig. 3.

Neighbouring pixels in the map with disorientation smaller

than 5 are associated with the same grain. According to this

disorientation angle, the grain size distribution can be

measured and a mean grain size (dEBSD) can be evaluated.

For each sample, the analyzed area was large enough to take

into account more than 5000 grains. The results are given in

Table 1, and in accordance with SEM observations, the grain

size decreases and the grain distribution becomes narrower

when the deposition current density is reduced.

EBSD orientation maps obtained on cross-sections ofdifferent deposits are given on Fig. 4. The growth direction

which is perpendicular to the surface of the substrate is also

shown on this figure. For the CD50 sample, fibers (whose axis

is perpendicular to the substrate surface) characterized by a

dominant colour are observed. These fibers are formed by

grains slightly disoriented with regard to the neighbouring

grains, but with the (100) direction mainly parallel to the

growth direction. Between these fibers, some less oriented

regions are found. The thickness of these fibers (around 5 m)

is quite similar to the size of large crystallites with a truncated

pyramidal shape, which are observed on the surface (4.3 m,

Table 1). As the deposition current density decreases, these

fibers are no longer observed and the mean size of the grains

decreases. It can be noticed that the grains do not show any

elongation along the growth direction whatever the deposi-

tion current density.

Two parameters are mainly used to describe the nature of

grain boundaries: the disorientation angle and the factor,

which denotes the fraction of atoms in the grain boundary

plane which are coincident to both lattices. These parameters

were evaluated by using EBSD[21]and are given in Table 2

andFig. 5. An increase of the fraction of high angle grain

boundaries (HAGB) is observed as the grain size decreases and

as the marked texture along the direction is replaced by

a weak texture along the direction(Table 2). The amount

of coincidence site lattice (CSL) is also strongly modified,

showing a decrease of the abundance of1 boundaries and an

increase of the number of3 and 9 boundaries when the

grain size decreases (Fig. 5).

3.4. Transmission Electronic Microscopy

Grain size was evaluated using TEM observation on a

population around 150 grains and the mean values are given

for CD1 and CD5 inTable 1. These values are lower than the

ones obtained by EBSD, but for the CD1 sample, the value is in

agreement with XRD analysis (130 nm). As a strong heteroge-

neity of grain sizes was observed for CD50, the mean value is

not relevant for this sample. TEM observations were also

performed on cross sections for this sample to evaluate the

crystallographic orientation of different grains. These analy-

ses are time consuming, thus only a semi-statistical study

on 56 grains at different locations inside the sample was

performed. However, 56 grains seemed to be sufficient to

reflect theheterogeneity of the sample, as the results were not

significantly modified when this number was increased.

Different populations of grains were identified, characterized

by three angles(100), (111) and(110) (Fig. 6).(hkl) relates

the angle between (hkl) plane and the normal to the coating

surface. The first one (V1) corresponds to the largest grains

(>700 nm) andexhibitsan angle(100) near 0. This means that

this crystallographic population mainly contributes to the

Fig. 2 2scans of coatings elaborated at different current

densities.



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macroscopic texture observed by XRD. In a randomzone (cf.

EBSD analyses), three other kinds of crystallographic popula-

tions were identified (Fig. 6), which do not correspond to

macroscopic texture obtained by XRD. The size of these grains

is generally lower (130 to 250 nm) than the grain with V1

variant. The correlations of these observations with SEM and

EBSD results show that two kinds of regions can be distin-

guished in the CD50 coating: the first one corresponds to large

grains with a preferred orientation and the second one

is associated with randomregions, with a much lower grain

size and weaker texture.

3.5. Composition Analysis

Table 3 lists the different elements detected in the coatings

and their contents in weight ppm obtained by SIMS and

Fig. 3 Left: Top view orientation maps obtained by EBSD for coatings elaborated at different current densities: CD1 (a), CD5 (b),

and CD50 (c). Right: Inverse pole figures of the normal direction for the three coatings.



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GDOES. For the coating CD50, impurity amounts are very low,

leading to a purity around 99.99%. However, for the coatings

prepared at lower current density the contamination drasti-

cally increases especially for light elements (H, O, C, etc.) and

for Cl and Cu. For these coatings, some impurity contents are

given with a large inaccuracy, and the purity of the coating

could not be evaluated. In these cases and especially for

chloride for which the concentration in ppm was not given,

the quantification was not reliable as the reference samples

contained much lower amounts of these elements. Concen-

tration profiles and cartographies were obtained for each

atomic element, showing that the impurities were homoge-

neously distributed laterally and through the thickness of the

coatings.

4. Discussion

Electrodeposited layers often exhibit a fiber texture, i.e.

preferred crystallographic orientation of their crystallites

along the growth direction, which is the case for deposits

CD5 and CD50. Our results are in good agreement with

published results for sulphamate bath which report a strong

crystallographic texture along the axis associated

Fig. 4 Cross-section orientation maps obtained by EBSD for coatings elaborated at different current densities: CD1 (a), CD5 (b),

and CD50 (c). The substrate surface normal is given by an arrow.



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with large grains for deposition currents between 30 and

200 mA/cm2 [12,13]. Based on cross-section observations by

optical microscopy or SEM after chemical etching, the

texture has been associated with the formation of long

columnar grains, some of them extending across the wholethickness of the coatings (10 to 50 m)[15,18]. Cross-section

observations of the CD50 coating by optical microscopy after

acidic etching show kinds of columns, parallel to the growth

direction, with a width of few micrometers (Fig. 7a). EBSD

and TEM observations on cross sections allow to distinguish

unambiguously the grains and to evaluate their orientations.

Theresults obtained by EBSD clearly show that these columns

are formed by grains weakly disoriented with regard to their

neighbouring, with the direction perpendicular to the

substrate surface. This microstructure, associated with a quite

high amount of low angle grain boundaries and particularly of

1 boundaries explains the large disagreement between the

structure size elements deduced by EBSD and SEM observationsin these coating (Table 1). Results obtained by TEM confirm that

the largest grains (and the more numerous) are oriented with

one direction parallel to the growth direction. However, a

significant amount of grains, much smaller (


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coatings deposited at 1 mA/cm2). Voltammograms obtained in

the plating bath with the same stirring conditions allowed us

to estimate the dioxygen reduction current density around

0.1 mA/cm2 and thus the contribution of this reaction could

explain the decrease of deposition efficiency. At low current

densities, and thus low deposition rates, this reaction could

hinderthe growthof crystallites, contributing to the refinement

effect. Moregenerally,the adsorptionof different foreign species

(including O, H, C, and Cl) at the cathode surface probably

prevents grain growth by avoiding surface diffusion of adatoms

and significant amounts of these species are incorporated into

the coatings. EBSD analyses show that, in coatings deposited at

low current density,grainboundariesare moredefective (higher

disorientation angle and factor) with probably an increased

concentration of vacancies. Thus, the results are consistent

with a decrease of grain size when current density decreases,

associated with the incorporation of impurities at grain

boundaries.

Fig. 6 TEM observations (CD50) and stereographic projections showing the orientation of different grains in a random

oriented region. The table gives the grainpopulation in terms of angle between the coatingnormal surface and the (hkl) plane.

Table 3 Impurity content in weight ppm for coatingsdeposited at different current densities. For the values initalics, the quantification was not possible as thereference samples contained a much lower amount ofthese impurities.

H C O S Cl Fe Co Cu Mo

CD50 1 5 25


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5. Conclusion

Although extensive experimental works have been pub-

lished concerning characterization of nickel electrodepos-

ited coatings, a study combining composition analyses and

multi-scale microstructural characterization is missing. In

sulphamate bath without additive, microstructure modifica-

tions are linked with the incorporation of impurities and

particularly light atomic elements whose content largely

depends on electrodeposition conditions. Deposits obtained

at current densities above 20 mA/cm2 show a strong

texture along the growth direction but are characterized by

different structural heterogeneities which can be evidenced

by using complementary observation tools. TEM and EBSD

observations offer the opportunity to distinguish the differ-

ent microstructural scales and to better understand the

microstructure of coatings. As the current density decreases,

grain refinement and texture modifications are observed

which are associated with more defective grain boundaries

and higher contamination. Both light elements and substi-

tution impurities are incorporated when grain size

decreases, which can affect mechanical properties and

corrosion resistance. So, chemical contamination of electro-

deposited coatings must be carefully evaluated before

discussing the influence of their microstructure on

properties.

Acknowledgement

Thanks are due to the Agence Nationale de la Recherche (GIP

ANR Program no. ANR-06JCJC-0023-01) for the financial

support.

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Fig. 7 a) Cross-section view of the coating CD50 obtained by

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etching.



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10. Characterization of Electrodeposited Nickel Coatings From Sulphamate Electrolyte Without Additive