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Laboratoire d'Etudes des Matriaux en Milieux Agressifs, EA3167, Universit de La Rochelle, Av. Michel Crpeau, F-17042 La Rochelle,
France
b
Fdration 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, France
c
Institut Pprime, UPR 3346 CNRS, Universit de Poitiers, SP2MI, Boulevard Marie et Pierre Curie, BP 30179, 86962 Chasseneuil,
Futuroscope Cedex, France
d
INSA Toulouse, Dpartement de Physique, 135 avenue de Rangueil, 31077 Toulouse Cedex 4, France
AR TIC LE D ATA
ABSTR ACT
Article history:
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
25 October 2010
decreases, grain refinement and texture modifications are observed which are linked with
the grain boundary character (disorientation angle and Coincidence Site Lattice). Moreover,
Keywords:
Electrodeposited nickel
Grain refinement
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.
Grain boundaries
EBSD
Chemical composition
1.
Introduction
M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
2.
j
mA/cm2
(SEM)
m
d (EBSD)
m
d (TEM)
m
CD1
CD5
CD10
CD20
CD50
1
5
10
20
50
0.37
0.74
1.4
3.9
4.3
0.25
0.35
1.02
0.120
0.180
165
3.
Results
166
MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
3.1.
SEM cannot be directly assigned to grains and other characterization tools will be used below to clarify this point.
3.2.
Fig. 1 SEM top views showing the 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)).
M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
3.3.
167
3.4.
168
MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
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.
3.5.
Composition Analysis
M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
169
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.
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 drastically 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. Concentration profiles and cartographies were obtained for each
atomic element, showing that the impurities were homoge-
4.
Discussion
170
MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
CD5
CD50
93
91
42
58
42
58
57
43
57
43
CSL denotes coincidence site lattice (CSL) with low sigma (LCSL,
< 29) or high sigma (HCSL, > 29).
M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
171
Fig. 6 TEM observations (CD50) and stereographic projections showing the orientation of different grains in a random
oriented region. The table gives the grain population in terms of angle between the coating normal surface and the (hkl) plane.
CD50
CD5
CD1
Cl
Fe
Co
Cu
Mo
1
70
130
5
100
400
25
400
1000
<1
6
25
<1
230
1000
4
15
7
32
100
155
25
150
600
<40
<40
<40
172
MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
and higher contamination. Both light elements and substitution impurities are incorporated when grain size
decreases, which can affect mechanical properties and
corrosion resistance. So, chemical contamination of electrodeposited 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.
REFERENCES
5.
Conclusion
Although extensive experimental works have been published concerning characterization of nickel electrodeposited coatings, a study combining composition analyses and
multi-scale microstructural characterization is missing. In
sulphamate bath without additive, microstructure modifications 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 <100>
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 different 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
M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 1 6 4 1 7 3
173