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Hot Corrosion of an Electrodeposited Ni-11 wt % Cr Nanocomposite under Molten

Na[sub 2]SO[sub 4]–K[sub 2]SO[sub 4]–NaCl

Article  in  Journal of The Electrochemical Society · January 2005

DOI: 10.1149/1.1952667

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 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲 B321
0013-4651/2005/152共9兲/B321/6/$7.00 © The Electrochemical Society, Inc.

Hot Corrosion of an Electrodeposited Ni-11 wt % Cr

Nanocomposite under Molten Na2SO4–K2SO4–NaCl
C. Zhang, X. Peng,z J. Zhao, and F. Wang
State Key Laboratory for Corrosion and Protection, Institute of Metal Research, Chinese Academy
of Sciences, Shenyang, 110016, China

A Ni–Cr nanocomposite with an average Cr concentration of 11 共wt %兲 was deposited onto nickel plate by simultaneous elec-
trodeposition of Ni and Cr nanoparticles from a nickel sulfate bath. The nanocomposite consisted of a nanocrystalline Ni matrix
and dispersed Cr nanoparticles with a mean size of 33 nm. For comparison, two Ni–Cr alloys, one with similar Cr content
共10 wt %兲 and the other with much higher Cr content 共20 wt %兲, were prepared using electro-arc melting. Hot corrosion testing
under molten Na2SO4–K2SO4–NaCl in air at 700°C showed that rapid formation of a continuous chromia-rich scale is essential
for hot corrosion protection. This was the case only for the nanocomposite. Internal sulfidation was observed for arc-melted alloys,
but not for the nanocomposite. The results demonstrate that it was not primarily the Cr content but the unique structure of the
nanocomposite that was responsible for its superior hot corrosion resistance. The protection mechanism lies in the fast formation
of a continuous chromia scale on the nanocomposite, due to the easy nucleation of chromia on both chromium nanoparticles and
abundant nickel grain boundaries, and then fast linking of the nuclei as a result of enhanced diffusion of Cr through those grain
boundaries.
© 2005 The Electrochemical Society. 关DOI: 10.1149/1.1952667兴 All rights reserved.

Manuscript submitted November 21, 2004; revised manuscript received March 21, 2005. Available electronically July 21, 2005.

A typical power plant burns one type of fuel 共usually coal兲 for that grain refinement could promote the formation of the protective
electricity generation. In the Vision 21 concept,1 a new high- oxide scale. This can be interpreted using Wagner’s model,22 that is,
efficiency energy production plant would be fuel flexible, i.e., ca- the critical content for the formation of protective oxide scale, for
pable of operating on a wide range of fuels including natural gas, example, the Cr content for external Cr2O3 scale formation, de-
kerosenes, diesel oils, residual oils, and gaseous fuels made from creases with the grain size of alloys. The effect of the grain refine-
coal, biomass, and waste, etc. The burning of fuels causes the pro- ment on selective oxidation is remarkable when the crystalline
duction of corrosive gases and salt contaminants such as deposits of grains of alloys are in the nanometer range.23-29 Recent calculation30
sulfates and chlorides.2-6 The sulfates in combination with chlorides indicates that the critical content will be reduced by 30% if the grain
could lead to the formation of low-melting salts, which would dis- size is reduced from 10 ␮m to less than 10 nm when the grain
solve the growing oxide scales and consequently result in aggra- boundary diffusivity of the scale-forming element is 100 times
vated degradation of the boiler components.7-11 This phenomenon is larger than its lattice diffusivity, and by 70% when the grain bound-
called hot corrosion. Hot corrosion, together with erosion from solid ary diffusivity is 1000 times larger. Nanocrystalline materials may
particles and gas flow, is one of the important factors leading to the therefore be very promising for corrosion-resistant coatings. How-
recession of steel boiler components. ever, more research is necessary to clarify the relationship between
One of the major technological requirements for supporting the the production process, the structure, and the corrosion performance
new high-efficiency energy production plant is to improve the per- of these materials before they can be used in advanced power pro-
formance of the materials used in these high-temperature aggressive duction systems.
environments. Chromium steels are currently employed in power The oxidation-resistant nanocoatings were usually deposited in a
plants for temperatures below 900°C. However, the steels have low high-vacuum chamber by magnetron sputtering.24-29 Recently, Peng
Cr contents 共normally below 20 wt %, because a higher Cr content et al.31 developed an oxidation-resistant Ni–Cr nanocomposite coat-
would increase the brittleness兲. The low Cr contents limit the ability ing by composite electrodeposition. Electrodeposition is a sophisti-
of the steels to form an external, protective Cr2O3-rich scale. As a cated technique with the merits of simple processing and ease of
result, developing protective coatings becomes a preferred choice fabrication, low expense, high productivity, and good compositional
and is also a cost-efficient approach. Coatings with high Cr contents control. This will allow us to find a way for the possible application
have been developed by different techniques. Diffusional chromized of the electrodeposited nanocomposites as corrosion-resistant coat-
coatings by pack cementation can enhance the high-temperature cor- ings. In the present work, an electrodeposited Ni–11Cr 共weight per-
rosion resistance of low-alloy steels, which has been known since centage兲 nanocomposite was produced, and its hot corrosion perfor-
the early 1950s.12 Unfortunately, the production of the chromized mance was studied under a molten salt mixture of sulfates and
coatings must be conducted at high temperatures, which would harm chlorides which simulated deposits formed in boilers burning sulfur-
the mechanical properties of boiler component of alloys. By a deto- and chlorine-containing fuels. For comparison, hot corrosion tests of
nation spray method, Yamada et al.13 produced a Ni–50Cr coating arc-melted Ni–10Cr and Ni–20Cr alloys were also conducted in the
which increased the hot corrosion resistance of boiler tubes. High- same condition. The objective of this study was to explore the dif-
velocity oxy-fuel 共HVOF兲 spraying is proposed to be a competitive ference in the hot corrosion behavior of the nanocomposite and that
technique for developing homogeneous and dense nickel-based of the traditional Ni–Cr alloys. The results will help develop new
coatings with high Cr contents to improve the corrosion resistance.14 deposited nanocomposite coatings with a variation of composition
However, the spray coatings always contain some oxides and pores and properties tailored to the requirements of practical applications.
at splat boundaries.15 Because the intrinsic porosity could provide
paths for the inward penetration of corrosive species, the corrosion
resistance of these spray coatings has been questioned.16,17 To seal
the porosity, some postspray treatments, such as annealing18 or laser
cladding,17,19 were proposed. Experimental
Another approach is to refine the grain structure of alloys, rather The Cr nanoparticles 共⬎99%兲 were manufactured using a direct-
than increasing the Cr content. Giggins et al.20 and Mertz21 found current plasma process and were passivated in an ionized Ar atmo-
sphere. Specimens with dimensions of 15 ⫻ 10 ⫻ 2 mm were cut
from a pure electrolytic nickel plate 共⬎99.9%兲. A ␾2 mm hole was
z
E-mail: xpeng@imr.ac.cn drilled in the upper center of the specimens so that they could be
B322 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲

Table I. The nickel-electrolyte compositions and parameters for uniformly distributed in the Ni matrix. The electrodeposited nano-
the electrodeposition of Ni–11Cr nanocomposite. composite was compact and no cracks between the nanoparticle and
nickel were seen.
Sodium Current
NiSO4·7H2O citrate NaCl H3BO3 density Temperature pH
Hot corrosion.— Figure 5 shows the mass-change vs time
curves for the as-deposited Ni–11Cr nanocomposite, and the arc-
100 g/L 120 g/L 12 g/L 25 g/L 3 A/dm2 30°C 7.0–7.2 melted Ni–10Cr and Ni–20Cr alloys in air at 700°C under the mol-
ten Na2SO4–K2SO4–NaCl mixture. The mass-change data were the
net result of the combination of mass gain by oxide scale formation
during exposure and mass loss due to scale exfoliation during cool-
hung for electroplating, and finally they were abraded to 800 grit
ing 共the mass loss as a result of salt evaporation was not considered
SiC paper. After ultrasonic cleaning in acetone, they were electrode-
because its value per unit square was almost the same for all
posited 共on all sides兲 with a 50 ␮m thick film of Ni–Cr composite
samples兲. Heavy scale spallation started on the Ni–10Cr alloy after
from a bath containing an appropriate content of Cr nanoparticles.
only 2 h exposure, whereas scale spallation was not significant on
The bath compositions and plating parameters are listed in Table I.
the other two specimens, particularly the Ni–11Cr nanocomposite.
During coating processing a reciprocating perforated plate main-
The scaling rate of the Ni–11Cr nanocomposite was much lower
tained the nanoparticles suspended in the bath, as described in our
than that of the Ni–20Cr alloy.
previous work.32 The electrodeposited nanocomposite contained a
mean Cr content of 11 wt % with a standard deviation of ±3 wt % Investigation of corroded specimens.— Figure 6 shows the
from place to place. The as-deposited composite was characterized XRD patterns of the samples after 40 h hot corrosion. Stronger
using scanning electron microscope 共SEM兲/energy dispersive analy- peaks from the metal base were clearly seen on the two arc-melted
sis by X-ray 共EDAX兲, X-ray diffraction 共XRD兲, and transmission alloys, particularly on the Ni–10Cr. This suggests that heavy scale
electron microscopy 共TEM兲, respectively. Ni–10Cr and Ni–20Cr spallation occurred. The scale on the arc-melted Ni–10Cr alloy was
specimens with dimensions of 10 ⫻ 10 ⫻ 2 mm were cut from the mainly composed of NiO 共Fig. 6a兲. Compared with the XRD pat-
cold-rolled alloy buttons, which were prepared by electro-arc melt- terns of the Ni–10Cr, intensities of peaks from NiO and substrate
ing pure Ni 共⬎99.9%兲 and Cr 共⬎99.9%兲 in vacuum with magnetic were relatively weaker and those of peaks of Cr2O3 stronger for the
stirring at temperature over 1600°C and subsequently by 2 h anneal- Ni–20Cr 共Fig. 6b兲. This demonstrates that the scale was more pro-
ing at 900°C. tective. In contrast, as can clearly be seen from Fig. 6c, chromia
After being rinsed using distilled water and ultrasonically appeared to be the major phase of the scale on the Ni–11Cr nano-
cleaned in acetone, the as-deposited Ni–11Cr nanocomposite and the composite. In the meantime, stronger peaks of chromate were seen.
Ni–10Cr and Ni–20Cr alloys were coated with salt which was syn- Chromate solute was formed as a result of the preferential reaction
thesized using 25 wt % NaCl and 75 wt % sulfates 共Na2SO4 plus of chromia with oxides 关共Na,K兲2O兴 in the molten salt.35,36
10 wt % K2SO4兲. Its liquidus temperature is close to 650°C. The Figure 7 presents the cross sections of various samples after hot
salt solution was prepared using distilled water and analytical re- corrosion. Severe scale cracking and separation between the scale
agent NaCl, Na2SO4, and K2SO4. The specimens were coated using and the metal occurred on the Ni–10Cr alloy 共Fig. 7a兲. EDAX
a paintbrush, and the water was evaporated by heating the speci- analysis clearly showed that the scale was composed of an outer
mens on a hot plate with a temperature over 200°C. Afterward, NiO layer and a thin inner Cr-rich oxide layer 共darker area兲. This
1.2 mg/cm2 salt was present on the surface of the specimens. Cor- double-layered scale also formed on the Ni–20Cr alloy 共Fig. 7b兲.
rosion tests were conducted in a muffle furnace up to 40 h at 700°C, However, the scale was denser and the inner Cr-enriched oxide layer
at which temperature the salt is molten. Samples were not placed in much thicker compared with the scale formed on the Ni–10Cr alloy.
the furnace until it was at temperature. After various times, samples From Fig. 7a and b, the scale was detached from the metal in most
were withdrawn from the furnace for weighing. The oxide scales on areas and internal corrosion occurred in the metal. The internal cor-
various specimens were investigated using SEM/EDAX and XRD. rosion products were sulfides; an example is shown in Fig. 8 共where
the surface scale has spalled兲. However, there were no internal sul-
fides in the corroded Ni–11Cr nanocomposite 共see Fig. 7c兲. The
scale on the nanocomposite was mainly composed of a thin layer of
Cr-rich oxides, which agreed well with the XRD characterization
Results
result. Moreover, the scale adhered well to the metal.
Characterization of the deposited nanocomposite.— Figure 1
shows the TEM image of the nanoparticles, most of which were
spherical but some appeared to be cubic. The particle size ranged
from 10 to 115 nm with a mean value of 33 ± 20 nm. Figure 2
shows the SEM surface morphology of the as-deposited Ni–11Cr
nanocomposite. Clearly, the surface of the as-deposited nanocom-
posite was very smooth 共Fig. 2a兲. At higher magnification, fine sur-
face protrusions, as indicated by the arrow, can be seen 共Fig. 2b兲.
EDAX analysis showed that the protrusions had higher Cr content
than the other area, suggesting that they were the fresh deposits
enriched with the nanoparticles, while in the other areas the code-
posited nanoparticles were engulfed by Ni deposits. Figure 3 shows
a cross section of the as-deposited nanocomposite. The Cr nanopar-
ticles 共dark dots兲 were in general homogeneously dispersed in the
electrodeposited Ni matrix. Agglomeration of nanoparticles into
larger clusters was occasionally observed. The grain size of Ni de-
posits in a direction perpendicular to the diffraction plane was char-
acterized by XRD using Cu K␣ radiation and calculated using the
full peak width at half-maximum 共fwhm兲 on the basis of the Scher-
rer equation.33,34 The average grain size was ⬃40 nm. Figure 4
shows the TEM bright-field image of the nanocomposite. The Cr
nanoparticles codeposited, as indicated by arrows, were in general Figure 1. TEM image of as-produced Cr nanoparticles.
 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲 B323

Figure 2. 共a兲 Surface morphology of as-

deposited Ni–Cr nanocomposite. 共b兲 At
higher magnification.

Discussion the internal sulfides in the Ni–20Cr alloy appeared to be less in

Many internal sulfides formed in the arc-melted Ni–10Cr and number and shallower compared with the Ni–10Cr alloy 共see Fig. 7a
Ni–20Cr alloys 共see Fig. 7a, 7b, and 8兲, demonstrating that the al- and b兲. This result suggests that the scale on the Ni–20Cr alloy was
loys suffered heavy attack by the sulfates in the molten salt during more hot corrosion resistant than that on the Ni–10Cr alloy. The
corrosion. Compared to this, the effect of the chlorides at this con- reason is that the former has a higher content of chromium, which
centration at 700°C on the hot corrosion of the three samples may favors the formation of chromia scale. Chromia is the most impor-
not be significant. According to Bornstein,35,36 Goebel,37 and Rapp tant oxide to combat hot corrosion in molten salt with sulfates, be-
et al.,38,39 the alloys may be attacked through the following route: cause it preferentially reacts with O2− in molten sulfates to form
the molten salt penetrates the growing oxide scale through defects chromate by the following equilibrium:
共like pores and microcracks兲 and arrives at the scale/alloy interface;
SO2− 2Cr2O3 + 2 O2− + 3 O2 = 4CrO2−
4 关3兴
4 is then reduced there by the following chemical equilibrium:
The chromate will stabilize the melt chemistry, and consequently
2SO2−
4 = 2O
2−
+ 3 O2 + 2S 关1兴 prevent the dissolution/reprecipitation of the protective oxide
scale.35-37,41 Yet, the internal sulfides occurred on the Ni–20Cr alloy,
This leads to internal sulfidation of the alloy substrate. This interfa-
suggesting that higher Cr content is needed to prevent the internal
cial silfidation causes a reduction of S activity and, as a result, an
corrosion.
increase of O2− activity, resulting in basic fluxing of oxide scale. As
In contrast, internal sulfides did not appear in the corroded
a negative gradient of the O2− activity exists across the fused salt
sample coated with the Ni–11Cr nanocomposite 共see Fig. 7c兲. The
layer, the dissolution of oxide scale at the salt/scale interface and the
formation of protective chromia scale was easier on the Ni–11Cr
reprecipitation of oxide particles at the gas/salt interface can be sus-
nanocomposite than the arc-melted alloys. To confirm this assump-
tained. For the arc-melted Ni–Cr alloys, surface NiO layer normally
tion, a comparison of initial scale on both the arc-melted alloys and
fast develops at the onset of exposure.40 The defects in this NiO
the nanocomposite for 30 min exposure in the hot corrosion condi-
layer make it feasible that the molten salt penetrates into the internal
tion was performed. As is evident from Fig. 9, XRD gave more
interface, where the increase of O2− activity by Reaction 1 will
intense chromate peaks from the corroded nanocomposite. This in-
dissolve the oxide by the reaction below:
dicates that the concentration of the chromate produced in the mol-
ten salt by Reaction 3 was higher than that in the molten salt on the
NiO + O2− = NiO2−
2 关2兴 arc-melted alloys. This result is also consistent with the observation
Reaction 2 again decreases the O2− activity, which further increases that XRD presented more intense peaks of chromia on the nanocom-
the S activity. In this case, the alloy is repeatedly attacked by sulfur. posite 共Fig. 9c兲 than on the arc-melted alloys 共Fig. 9a and b兲. Cross-
Therefore, the inward penetration of sulfur caused the formation of sectional investigation revealed that a continuous layer of chromia
the internal sulfides in the arc-melted Ni Cr alloys. Nevertheless, had formed in this case, as shown in Fig. 10a. No continuous chro-

Figure 3. Cross-sectional morphology of as-deposited Ni–Cr nano-

composite. Figure 4. Bright-field TEM image of as-deposited Ni–Cr nanocomposite.
B324 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲

Figure 5. Mass-change vs time curves of the Ni–11Cr nanocomposite, the

arc-melted Ni–10Cr, and Ni–20Cr alloys exposed in air at 700°C for 40 h
under molten salt of Na2SO4–K2SO4–NaCl.

mia layer had formed on the arc-melted alloys as seen in Fig. 10b
for the Ni–20Cr alloy, and as a result, internal sulfides were formed.
Therefore, the ability to form a continuous chromia scale is a
crucial factor affecting the hot corrosion behavior. Whether the
Ni–Cr alloys can grow chromia scale or not depends on the Cr
content. For the oxidation of Ni–Cr alloys, the minimum Cr content
required for selective oxidation of chromium to form a chromia
layer is 20 wt %.40 On Ni–10Cr, nonprotective Ni-rich oxides form,
which inevitably permit attack of the metal by the molten salt.
Hwang and Rapp42 described this synergistic hot corrosion. Thus,
the arc-melted Ni–10Cr alloy exhibited the poorest resistance
against hot corrosion and formed many internal sulfides 共Fig. 5兲.
Although Ni–20Cr alloy is a chromia former, development of a con-
tinuous layer took a long time 共see Fig. 9 and 10b, during which the
molten salt attacked the alloy.
Although the Cr contents of the Ni–Cr nanocomposite and the
10 wt % arc-melted alloy were similar, the composite formed a con-
tinuous chromia scale. Although Cr content of the nanocomposite
was far lower than that of the 20 wt % alloy, the transient stage for
the formation of continuous chromia scale was shorter. This demon-
strates that not only the Cr content but the unique structure of the
Ni–11Cr nanocomposite was responsible for its superior corrosion Figure 7. Cross-sectional images of the arc-melted alloys of 共a兲 Ni–10Cr
performance. This unique structure leads to a different oxide growth and 共b兲 Ni–20Cr, and of 共c兲 the Ni–11Cr nanocomposite-coated sample after
mechanism from those for the arc-melted Ni–Cr alloys. It is gener- 40 h hot corrosion in air at 700°C under the Na2SO4–K2SO4–NaCl molten
ally accepted that during high-temperature exposure, unless the Cr salt.

Figure 6. XRD characterization of the corroded scale on 共a兲 the arc-melted Figure 8. 共a兲 SE image of cross section of the arc-melted Ni–10Cr alloy
Ni–10Cr and 共b兲 Ni–20Cr alloys, and 共c兲 the Ni–11Cr nanocomposite for after the 40 h hot corrosion and 共b兲 X-ray map of sulfur showing the forma-
40 h hot corrosion in air under molten salt of Na2SO4–K2SO4–NaCl. tion of internal sulfides.
 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲 B325

Figure 9. XRD characterization of the

corroded scale on 共a兲 the Ni–10Cr alloy;
共b兲 the Ni–20Cr alloy; and 共c兲 the Ni–
11Cr nanocomposite for 30 min hot corro-
sion in air under molten
Na2SO4–K2SO4–NaCl.

content is 艌50%,43,44 NiO and Cr2O3 simultaneously nucleate, and Conclusions

a continuous outer NiO layer forms before a continuous inner chro-
mia layer because NiO grows faster than Cr2O3. By contrast, the A Ni–11Cr nanocomposite was fabricated through co-
growth mechanism of the oxide scale on the nanocomposite may be electrodeposition of Ni with Cr nanoparticles. Comparison of the hot
different due to its unique structure. First, Cr nanoparticles which corrosion of the nanocomposite and the arc-melted Ni–10Cr and
were dispersed on the surface of the electrodeposited Ni matrix were Ni–20Cr alloys in air at 700°C under molten Na2SO4–K2SO4–NaCl
present to oxidize, and hence would act as sites for the fast nucle- demonstrated that the hot corrosion resistance of the three materials,
ation of chromia. Second, these sites and the metal grain boundaries, from worst to best, is in the order of Ni–10Cr ⬍ Ni–20Cr
which are also nucleation sites for chromia, are much closer together
⬍ Ni–11Cr nanocomposite. Microstructural investigation of the cor-
which will shorten the time needed for the linking of adjacent oxide
islands, compared with the situation for the arc-melted alloys. Third, roded samples indicated that a denser and higher chromia-enriched
which may be more important, is that the greatly increased number scale formed on the Ni–11Cr nanocomposite, whereas the scales on
of grain boundaries in the nanocomposite enhances the flux of Cr to the Ni–Cr alloys were less protective, although the Cr contents of
the oxide/gas interface and consequently accelerates the lateral the alloys were similar to or much higher than that of the nanocom-
growth of the chromia islands to form a continuous layer. posite. The explanation lies in the exclusive formation of a continu-
The more rapid formation of a continuous chromia scale on the ous chromia scale on the Ni–11Cr nanocomposite. This is probably
Ni–11Cr nanocomposite leads to better protection of the metal due to the easy nucleation of chromia on chromium nanoparticles, a
against attack by aggressive species. Thus, internal corrosion was high concentration of metal grain boundaries, which are also nucle-
prevented when the Ni–11Cr nanocomposite-coated sample was ex-
ation sites, and then fast linking of the nuclei as a result of enhanced
posed to the synthetic salt. However, for the rapid formation of a
continuous scale, a critical content of Cr nanoparticles is required. diffusion of Cr from the coating to the interface through those nano-
Presumably, according to the present work, at any given temperature composite grain boundaries. Therefore, a dense chromia scale is
this critical content is dependent upon the particle size and the grain formed before attack by the molten salt can occur. Although the
size of the nanocomposite. This relationship will be explored in our Ni–20Cr alloy forms a continuous chromia scale; a longer time is
future work. needed for its development, which allows the molten salt to attack

Figure 10. Cross-sectional morphologies

of 共a兲 the Ni–11Cr nanocomposite and 共b兲
the arc-melted Ni–20Cr alloy after 30 min
corrosion in air at 700°C under molten
Na2SO4–K2SO4–NaCl.
 B326 Journal of The Electrochemical Society, 152 共9兲 B321-B326 共2005兲

the metal. The Ni–10Cr alloy never forms a continuous chromia 16. F. Easterly, A. Verstak, S. Baranovski, and T. Shmyreva, NACE Corrosion/97,
Paper 141, New Orleans, LA, April 1997.
scale; therefore, the internal attack was the most significant in this 17. M. A. Unsitalo, P. M. J. Vuoristo, and T. A. Mäntylä, Mater. Sci. Eng., A, 346, 168
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The results of the present work suggest that it will be possible to 18. C. H. Lee and K. O. Min, Surf. Coat. Technol., 132, 49 共2000兲.
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Andersson, J. Therm. Spray Technol., 9, 513 共2000兲.
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