Solar Energy Materials & Solar Cells 146 (2016) 8–15

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Solar Energy Materials & Solar Cells

journal homepage: www.elsevier.com/locate/solmat

Slurry aluminizing: A solution for molten nitrate salt corrosion

in concentrated solar power plants
A. Soleimani Dorcheh n, M.C. Galetz
Department of High Temperature Materials, DECHEMA-Forschungsinstitut, Theodor-Heuss-Allee 25, 60486 Frankfurt am Main, Germany

art ic l e i nf o a b s t r a c t

Article history: Molten nitrate salts (KNO3–NaNO3) are used extensively as heat transfer fluids in concentrated solar
Received 13 August 2015 power (CSP) applications. The oxidative character of nitrate salts at high temperature conditions leads to
Received in revised form challenges in the corrosion protection of CSP installations in contact with molten salts. This work reports
6 October 2015
efforts to protect low-cost ferritic–martensitic P91 (Cr9–Mo1) and austenitic stainless steel 304SS
Accepted 13 November 2015
materials against molten salt corrosion using slurry aluminizing. The gravimetric results show a sig-
nificant improvement for aluminized alloys up to 1700 h immersion in molten nitrate salt at 600 °C. The
Keywords: extent of protection in P91 becomes comparable with the most competitive resistant materials e.g.
Nitrate salt Inconel 625. Metallographic investigations and scanning electron micrographs reveal no sign of corrosion
Concentrated solar power
in the substrates beneath the aluminide coatings during the immersion test. Electron probe micro-
P91
analysis results reveal Na(Fe,Al)O2 as the protective corrosion product forming on the surface of both
Aluminizing
Slurry aluminized steels.
Solar salt & 2015 Elsevier B.V. All rights reserved.

1. Introduction calculated as:

Concentrated solar power (CSP) has recently gained increased
interest as a major renewable energy technology. It provides not
only clean electricity, but can also provide continuous, reliable and
flexible power systems using an unlimited source of energy i.e.
Sun. The most common CSP technologies are parabolic dishes,
power towers, parabolic troughs, and linear Fresnel reflectors
which are based on point focus and line focus concentration of
solar radiation. To date, more than 95% of the CSP systems are
based on parabolic trough collectors [1,2]. However, recent trends
show that the solar power tower system is the preferred CSP
system for the future due to its capability to achieve higher tem-
peratures [2]. Fig. 1 demonstrates the schematic cycle for a solar
power tower system. The principle of this technology is based on
the concentration of solar radiation using mirrors focused on the
receiver tank. Inside the receiver the heat transfer fluid (HTF)
absorbs the heat and transfers it to a storage tank (hot tank). This
stage is followed by a heat exchange process which finally ends
with a conventional steam power generating process. The cold
fluid is transferred to the cold tank and is again pumped to the
receiver tank [3]. Based on basic thermodynamic principles, the
amount of heat produced in a central receiver CSP can be
n
Corresponding author. Tel.: þ 49 69 7564 363; fax: þ 49 69 7564 388.
E-mail address: soleimani@dechema.de (A. Soleimani Dorcheh).
Q ¼ mC P ðT H  T C Þ
where Q is the heat energy, m is the mass, C P is the specific heat of
the storage medium i.e. HTF (which is assumed to be independent
on temperature), T H is the temperature in the hot storage, and T C
is the temperature in the cold storage.
Thus, higher energies can be stored by a) high density storage
media, b) HTFs with higher specific heat, and c) higher tempera-
tures in the hot storage tank. All of these parameters are related to
the characteristics of heat transfer fluids. To date, molten nitrate
salts (so called solar salt) based on alkali nitrates with a compo-
sition of 40 wt% KNO3–60 wt% NaNO3 are the main HTFs used for
CPS applications. They offer a combination of high density, high
specific heat (C P ), low melting point, high thermal stability, and
low vapor pressures. The physical properties of the solar salt are
listed in Table 1.
Currently, the thermal efficiency of the power tower CSP plants
is between 30% and 40% [1]. Increasing thermal efficiency requires
lower salt melting points and elevated hot storage temperatures.
Efforts to develop novel salt mixtures with lower melting points
and higher heat capacities are increasing [2,7,8]. However, degra-
dation of nitrate salts which starts above 600 °C does not allow an
increase in the hot storage temperature beyond the stability of
such molten salts [2].
The circulation of salt in the power cycle relies on the molten
state of the nitrate salts and this can only be granted by keeping
the temperature in all transport and storage parts above the

http://dx.doi.org/10.1016/j.solmat.2015.11.024
0927-0248/& 2015 Elsevier B.V. All rights reserved.
 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15 9

steels (e.g P91 or X20CrMo-V11-1) which significantly affect the

price of the output electricity [1].
More than 75 years ago iron-aluminides emerged as resistant
materials for highly oxidative environments [18–28]. The high Al
concentration of these alloys induces the formation of a protective
aluminum oxide scale which guarantees their high resistance to
oxidation [22], sulfidation [23,29] at high temperatures and hot
corrosion in molten salts [27,30,31]. Tortorelli et al. showed that
iron aluminides show significant resistance to molten nitrate salt
corrosion [13,31]. They reported that aluminides with more than
30 at% Al show superior oxidation resistance in KNO3–NaNO3–
Na2O2 molten salt at temperatures lower than 600 °C.
In iron-based alloys, aluminizing can significantly increase
corrosion resistance by promoting alumina scale formation in
oxidizing atmospheres [18,19,21,23,26,28,32–35]. Pack cementa-
tion (chemical vapor deposition) and slurry process are the major
Fig. 1. Schematic of the energy conversion cycle in a concentrated solar aluminizing techniques. Recently, interest in slurry aluminizing
power plant. processes has increased due to its simplicity, economic efficiency,
environmentally friendly process, and higher flexibility compared
Table 1 to a pack cementation method [36]. The process starts with
Physical properties of the solar salt (60 wt% NaNO3–40 wt% KNO3). spraying or painting of a suspension of Al particles on the sub-
strate surface followed by a heat treatment process which forms
Property Melting ΔHfusion (J/g) Thermal Viscosity Heat Capa-
point (°C) stability (at 300 °C, city (at an aluminide diffusion layer on the substrate surface. The classical
(in air, °C) cP) 300 °C, J/ heat treatment is performed under an inert atmosphere at mod-
kg K) erate temperatures. Recent technical advances, however, increased
the process flexibility including on-site treatment (eg. post weld-
Value 221 123.9 650–700 3.26 1495
Reference [4] [4] [5] [6] [6]
ing treatment) by utilizing local induction, hot blanket, and flame
treatment under atmospheric conditions [37].
Experimental results on the effect of aluminizing on molten salt
freezing point of the salt (  225 °C). In this condition, the corro- corrosion resistance of ferritic and austenitic steels are very lim-
sion resistance of the storage tanks and piping in CSP installations ited. Carling et al. studied the molten salt corrosion behavior of
is one of the most challenging engineering issues in CSP plants pack cemented aluminized steels [38].
[4,9–13]. Molten nitrate salts contain oxidizing agents such as In this work, slurry aluminizing is used to enhance the molten
NO2 and NO3 oxide species, and O2 (from air). Corrosion of steel salt corrosion of ferritic–martensitic steel P91 and austenitic
parts in contact to molten nitrate salts at high temperatures can stainless steel 304 materials in NaNO3–KNO3 molten salt mixtures.
occur via the following reactions: The focus is primarily on the comparative corrosion performance
of uncoated and aluminized steel substrates. Furthermore, the
NO3 þ 2e  2NO2 þ O2  ð1Þ evolution of coating microstructure and corrosion products during
the corrosion test is evaluated.
Feþ O2  2FeO þ 2e  ð2Þ

3FeO þ O2  2Fe3 O4 þ2e  ð3Þ 2. Experimental

2Fe3 O4 þ O2  2Fe2 O3 þ 2e  ð4Þ 2.1. Substrate materials

2Cr þ3O2  2Cr2 O3 þ 6e 
Feþ Cr2 O3 þO2  2FeCr2 O4 þ2e 
Moreover, commercial salts contain levels of impurities which
can accelerate the rate of corrosion. Thus, the mechanism of cor-
rosion has to be investigated and the life time of these materials
has to be correctly estimated.
The performance of different materials in molten salt corrosion
at different temperature ranges has been studied [12,14]. It has
been found that high chromium Ni-base alloys (e.g. IN625) and
high chromium austenitic steels (e.g. 304 and 316) have lower
corrosion rates in molten salt compared to the low chromium
steels [11–13,15–17]. The influence of chromium on molten salt
oxidation behavior is controversial. It is known that high chro-
mium alloyed steels show higher corrosion protection via forma-
tion of a slow growing continuous chromium oxide or chromate
spinel layer [4,12]. On the other hand, depletion of chromium in
the substrates and Cr-dissolution in molten salt (however slow)
has been evident [13]. In addition, alloys with high chromium
contents are usually more expensive than the low-chromium
ð5Þ Rectangular coupons of ferritic–martensitic steel P91 and
stainless steel 304 with 25  10  4 mm3 dimensions were cut by
ð6Þ an electric discharge machine. Coupons were ground to 320 grit
SiC paper, sand blasted, degreased with acetone in an ultrasonic
bath, and finally dried in air. The compositions of the studied
alloys were obtained using optical emission spectroscopy (OES)
(see Table 2).
2.2. Slurry aluminizing procedure
Two groups of specimens from both steels were used for the
slurry coating process. To prepare the coating slurry, aluminum
powder was mixed with polyvinyl alcohol and distilled water. The
slurry was air brushed onto the specimen's surface. Dried samples
were heat treated at 300 °C for 4 h (to cure the binder) and then
heat treated at 700 °C for 10 h under an Ar atmosphere. After heat
treatment samples were washed and weighed before being used
in the corrosion test.
Two different salt mixtures composed of NaNO3 (60 wt%) and
KNO3 (40 wt%) were used for the corrosion test. The salt mixtures
were different in the level of impurities, primarily the chloride
10 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15

content. Details of the impurity levels in the salts are listed in products and the microstructural evolution of the coating were stu-
Table 3. died using electron probe microanalysis.
Corrosion tests were conducted for non-coated and aluminized
alloys under similar conditions. The corrosion behavior of alloy-
steel P91 was studied in salt A and that of austenitic steel 304SS in 3. Results and discussion
salt B with higher chloride levels.
The corrosion test was conducted according to ISO/NP 17245 – 3.1. Microstructure of the aluminized steels
Corrosion of Metals and Alloys – Test method for high-temperature cor-
rosion testing of metallic materials by immersing in molten salt or other Former studies on aluminized low-chromium ferritic steels
inorganic liquids. The immersion test was conducted on 5 coupons of (e.g. P91 and P92) illustrated their promising oxidation perfor-
each alloy immersed in molten salt at 600 °C under flowing laboratory mance in steam environments [18,34]. Aluminum enrichment of
air for up to 2500 h. Only one sample was removed after each time the sub-surface region in steel substrates results in the formation
of Al-rich intermetallic phases which are prone to the formation of
interval (100, 500, and 1000, 1700, and 2500 h) and the weight change
a protective alumina scale [18,22].
kinetics of oxidation was investigated. The chemistry of corrosion
After the heat treatment process, an aluminide coating with a
thickness of  80 mm formed on the P91 ferritic substrate. The
structure of the aluminide coating is already known on P91 sub-
Table 2
Chemical composition of the studied steels. strates [22,26,39]. It is composed of an outer Fe2Al5 layer with Cr-
rich precipitates and underneath a much thinner FeAl layer as
Alloy P91 304SS shown in Fig. 2a. Vertical cracks in the aluminide coating (Fig. 2a)
are typical features in such coatings on ferritic steels [22,26]. These
EN number 1.4903 1.4301
C 0.102 0.037 cracks form during aluminizing due to the mismatch between the
Si 0.356 0.649 coefficient of thermal expansion of the ferritic substrate and the
Mn 0.412 1.21 phases in the aluminide coatings [26].
P 0.014 0.013
A thinner aluminide coating of  52–65 mm thickness was
S 0.01 0.021
Cr 8.75 18.37 formed on 304SS. A larger thickness of the aluminide coating on
Ni 0.17 8.69 steel P91 can be explained by a higher diffusivity of Al in bcc ferrite
Mo 0.944 0.32 compared to the fcc austenitic structure of 304. The inward dif-
Fe 88.7 69.92
fusion of Al leaves pores in the coatings [26]. The amounts of these
Al 0.001 0.002
Ti 0.002 0.005 pores depend on the diffusion rate of Al during the heat treatment
V 0.203 0.065 process. As the Al diffusion rate in the ferrite structure is higher
Co o 0.002 0.058 than in austenite, a higher porosity level in the steel P91 diffusion
W 0.008 0.02
Cu 0.119 0.493
zone should not be surprising (see Fig. 2).
Nb 0.08 0.013 The coating on austenitic steel 304 has a different morphology.
The SEM micrograph (see Fig. 2b) illustrates three distinct layers
composed of a single phase layer with a dark gray level, a two
Table 3 phase layer with a lighter gray scale and underneath a thin single
Levels of impurities in nitrate salt mixtures. phase layer. EDS results revealed that the outer layer resembles
Impurity Salt 1 (wt%) Salt 2 (wt%)
the Fe2Al5 phase containing similar Al and Fe contents. The dif-
ference in their gray scale was attributed to the higher Ni content
Nitrite (NO2  ) o0.01 o 0.02 (2 at%) in the inner Fe2Al5 layer. A higher phase fraction of the Cr-
Chloride (Cl  ) o0.02 o 0.25 rich precipitates due to the higher Cr content is found in alloy 304
Magnesium (Mg2 þ ) o0.0007 o 0.05
o0.1 o 0.1
compared to that of P91. EDS results revealed the formation of an
Carbonate CO23 
o0.01 o 0.1 FeAl layer under the Fe2Al5 layer in both steels. The aluminide
Sulfate SO24 
Insolubles o0.01 o 0.05 coating on the 304SS substrate did not reveal vertical crack for-
Moisture o0.2 o 0.1 mation. This can be due to the smaller mismatch between the
coating and the substrate [26,36].

Fig. 2. Back scattered SEM micrographs of (a) as-coated P91 and (b) as-coated 304.
 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15
Fig. 3. (a, b) Gravimetric results for uncoated and aluminized P91 and 304SS immersed in molten nitrate salt at 600 °C and (c) corresponding macrographs of uncoated and
aluminized substrates at t ¼1000 h.
To study the corrosion behavior, the aluminized and un-coated
ferritic steel P91 and the austenitic 304SS were immersed in salt A
and salt B at 600 °C, respectively.
3.2. Corrosion kinetics
3.2.1. Un-coated alloys
Fig. 3 illustrates the gravimetric weight change result for coated
and un-coated alloys immersed in the molten salt at 600 °C.
Results represent the net weight of coupons after rinsing with
water and drying. In accordance with previous works [40], it was
shown that P91 does not act protective in molten nitrate salts as
its weight gain increases massively during the exposure. Moreover,
the oxide scales formed on the un-coated P91 substrates are prone
to buckling and blistering as shown in Fig. 3b.
The austenitic steel 304, however, shows notably higher cor-
rosion resistance with parabolic behavior (see Fig. 3). Higher
chromium content results in the formation of a protective chro-
mium oxide layer which accounts for the lower mass gain in 304
[11,15].
3.2.2. Aluminized alloys
Slurry aluminide coatings provide an alumina forming layer on
the surface of alloys which significantly increases the corrosion
behavior of low chromium alloys in oxidizing environments. The
weight change curves of the un-coated and aluminized steels in
salts A and B reveal the beneficial influence of the coating on
corrosion resistance of both steels. In the case of P91, the protec-
tive behavior of the coating is much more pronounced to an extent
that is comparable with the protective behavior of the high-
chromium stainless steel 304 (see Fig. 3a). The coated 304 steel
shows about 2.5 times less mass gain compared to un-coated 304
in salt B. Higher molten salt corrosion protection in aluminized
steels is in agreement with the results of Carling et al. on pack
cemented aluminide coatings on low and high-chromium steels
[38]. However, detailed observation of the weight change curves of
11
both aluminized alloys reveals that up to 100 h, an initial mass-
gain occurs followed by a slow rate mass-loss after 500 h (Fig. 3a).
The initial weight gain was not observed in Carling's gravimetric
curves [38]. The difference can be attributed to the FeAl aluminide
formation in the pack cemented P91 of Carling's work and Fe2Al5
aluminide formation in slurry aluminized P91 of this work. The
higher Al activity in Fe2Al5 aluminide is more prone to form an
aluminum rich scale during the course of corrosion. Thus, it is
expected to observe increased protection in this work. Partial
dissolution of aluminum and iron-oxide to sodium-aluminate and
sodium-ferrite (NaAlO2 and NaFeO2) is expected for the alumi-
nized steels under long term exposure in molten nitrate salts [38]
which can describe the weight loss in the gravimetric curves. The
corresponding macrographs of specimens did not show signs of
local spallation, buckling, or blistering (see Fig. 3b).
3.3. Corrosion products
The contrast in corrosion behavior of coated and un-coated
alloys can be reflected by comparing their metallographic cross
sections after 1000 h immersion in molten salts (Fig. 4).
The massive weight gain of the un-coated P91 gravimetric
results is reflected as a thick scale composed of multi-layers of iron
oxides (Fe2O3, Fe3O4) on top and inner layers of iron chromium
spinel FeCr2O4 (see Fig. 4) [38]. The major oxidation product in
304SS is FeCr-spinel and sodium ferrite as a continuous protective
layer that prevents molten salt access to the substrate. This
behavior is typically observed in other stainless steels with high
chromium contents (e.g. 316SS and 347SS) [11,13]. Despite the
acceptable corrosion resistance of the un-coated 304SS, further
improvements are achieved by aluminizing 304SS.
Fig. 5 shows scanning electron micrographs of the aluminized
steels after 100 and 1000 h immersion. Thin layers of corrosion
products on top of the coatings on both steels are evident. On both
aluminized steels the corrosion front could not penetrate the
coating and the substrate remained protected. The aluminized P91
12 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15
Fig. 4. Metallographic cross section of (a) uncoated P91 (b) aluminized P91, (c) uncoated 304SS, and (d) aluminized 304SS after 1000 h immersion in molten nitrate salts at
600 °C.
and 304SS show higher porosities in the aluminide layers adjacent
to the salts compared to their as-coated samples. Continuous
inward diffusion of aluminum from the high activity region during
the course of exposure leaves these pores at the outer parts of the
aluminide layer. Further diffusion process during exposure results
in a thicker coating. In addition, the reaction between the inward
diffusing oxygen and Al fills pores and vertical cracks with internal
oxides (Fig. 5). The austenitic structure of 304SS provides lower
CTE mismatch between the Fe2Al5 aluminide layer and the sub-
strate preventing vertical crack formation (Figs. 4 and 5) [41,42].
The evolution of coating microstructure during the corrosion test
in both steels is much the same. They are composed of a homo-
geneous Fe2Al5 layer with more porosities and Cr-rich precipitates
at longer immersion times. The precipitation-free zone of the as-
coated 304SS (see Fig. 2b) is altered to a single zone with dis-
persed Cr-rich precipitates after 1000 h exposure.
3.3.1. Aluminized P91
Element distribution maps and quantitative EPMA line scans of
the aluminized P91 after 100 and 1000 h immersion in molten salt
at 600 °C (Fig. 6) reveal details of the compositional evolution of
corrosion products and coatings. After 100 h, a complex layer with
relatively similar O and Na contents is observed. After 1000 h,
however, the oxygen content dominates forming a more protective
layer of  5 μm thickness. Mutual solubility of elements in the
oxide and ferrite/aluminate structure makes it difficult to conclude
the stoichiometric composition of this layer using EPMA results. X-
ray diffraction analysis (not shown) could also not resolve the
different phases as the existing peaks corresponding to the can-
didates (Al2O3, sodium aluminate) were too weak and overlapped.
It may be attributed to a complex aluminate (Na(Fe,Al)O2) based
on distribution profiles (see Fig. 6b). This is in agreement with
thermodynamic calculations of Tortorelli et al. for Al–K–O–N–Na
system at 507 and 677 °C (Fig. 7) revealing that NaAlO2 is the only
stable phase at this temperature range [13]. Since the temperature
used in this work lies in the range used for the calculations, it is
safe to say that no Al2O3 phase can form under the conditions
used. The microstructure of the coating also underwent an evo-
lution during the course of exposure. Due to ongoing inter-
diffusion in the aluminide layer, after 1000 h, Fe2Al5 thinned
while the underlying FeAl layer thickened compared to their
thicknesses after 100 h immersion.
3.3.2. Aluminized 304SS
Fig. 8 shows the element distribution maps and line scan pro-
files of the aluminized 304SS after 100 and 1000 h immersion in
salt B. Similar to the behavior of aluminized P91, the 304SS forms a
continuous corrosion product with a thickness similar to that of
aluminized P91. A comparison of the Na/O signal ratio after 100 h
and 1000 h reveals that similar to the observations for the alu-
minized P91, the initially formed sodium-rich phase tends to form
oxide as the course of exposure continues. This is illustrated as a
significant reduction in the Na/O ratio in the line scan profiles.
Several differences can be noted, however, by comparing to the
results of the aluminized P91 steel. EPMA results reveal higher
oxygen/sodium ratios in the oxidation products and notable Fe
depletion within the Fe2Al5 in aluminized 304SS after 1000 h (see
Figs. 6 and 8). Moreover, co-diffusion of chromium and Ni in the
aluminide layer is evident in the distribution profiles. The effect of
substrate Cr content does not seem to be significant on the alu-
minide corrosion performance.
 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15 13

Fig. 5. Back-scattered micrographs of the aluminized P91 and 304SS steels after (a, c) 100 h and (b, d) 1000 h immersion in molten salts at 600 °C. Note the evolution of
coating during the course of exposure.

Fig. 7. Predominance diagram for Al–Na–K–N–O system for the temperature range
507–677 °C (after Tortorelli et al. [13]).

4. Conclusions

The effect of aluminizing on corrosion behavior of ferritic–

martensitic P91 and austenitic 304 in molten nitrate salts at 600 °C
was studied. It was found that the slurry aluminized substrates
Fig. 6. Element distribution maps and quantitative line-scan profiles of the alu-
minized P91 after (a) 100 h and (b) 1000 h immersion in molten salt A at 600 °C. achieved higher protection against molten salt corrosion. During
14 A. Soleimani Dorcheh, M.C. Galetz / Solar Energy Materials & Solar Cells 146 (2016) 8–15
Fig. 8. Element distribution maps and quantitative line-scan profiles of the alu-
minized 304SS after (a) 100 h and (b) 1000 h immersion in molten salt A at 600 °C.
the course of exposure, the Fe2Al5 aluminide was solely in contact
with the molten salt while the substrate steel remained unaf-
fected. Although the uncoated stainless steel provided higher
protection than the uncoated P91, both aluminized steels per-
formed equally well in terms of molten salt corrosion. By resolving
the corrosion issue of low-chromium P91, the aluminized P91
could be a promising candidate for CSP applications as it can offer
a significant cost-saving. However, besides the isothermal corro-
sion studies, further studies on coating optimization, thermo-
cyclic corrosion behavior, and mechanical stability of the alumi-
nized steels in the molten salt environment should be considered.
Acknowledgments
Authors thank Ferrostaal GmbH for supporting this project. Dr.
Rick Durham is thanked for his valuable discussions.
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