Trans Indian Inst Met
DOI 10.1007/s12666-016-0906-8
TECHNICAL PAPER
Corrosion Behaviour of Uncoated and Ceramic Coated 9Cr1Mo
Steel in Molten LiClKClUCl3 Salt
Ch. Jagadeeswara Rao1 T. P. Ismail2 A. Ravi Shankar1 Atul Ramesh Ballal2
C. Mallika1 U. Kamachi Mudali1
Received: 1 January 2016 / Accepted: 13 May 2016
The Indian Institute of Metals - IIM 2016
Abstract 9Cr1Mo steel has been proposed as the con-
tainer material for the electrorefining process of pyro-
chemical reprocessing of spent metallic fuels from the
future sodium cooled fast breeder reactors. The electrore-
fining process was carried out using LiClKClUCl3
molten salt as the electrolyte at 500 C under argon
atmosphere. To protect the electrorefining vessel, made of
9Cr1Mo steel from the attack by the electrolyte, yttria
stabilized zirconia (YSZ) ceramic coating was deposited on
9Cr1Mo steel by thermal spray process. The corrosion
behavior of 9Cr1Mo steel with and without YSZ coating
was evaluated in LiClKClUCl3 molten salt at 600 C
under argon atmosphere for various durations (100, 250,
500 and 1000 h). The results revealed that with increase in
exposure time, the weight loss of uncoated 9Cr1Mo steel
samples increased, while YSZ coated 9Cr1Mo steel
samples exhibited insignificant weight loss. SEM exami-
nation of exposed uncoated 9Cr1Mo steel samples
showed Cr depletion on the surface and formation of
chromium based oxides as corrosion products. After the
corrosion experiment, SEM/EDS and XRD analyses of
both coated and uncoated samples showed the presence of
FeCr and UO2.
Keywords Molten salt corrosion  9Cr1Mo steel 
Plasma spray coating  Yttria stabilized zirconia 
Corrosion behavior
& U. Kamachi Mudali
kamachi@igcar.gov.in
1
Corrosion Science and Technology Group, Indira Gandhi
Centre for Atomic Research, Kalpakkam 603102, India
2
Visvesvaraya National Institute of Technology, Nagpur, India
1 Introduction
Non-aqueous pyrochemical process is proposed for the
reprocessing of spent metallic fuels to be discharged from
the future sodium cooled fast breeder reactors in India [1,
2]. Among the various processes such as salt purification,
electrorefining, cathode processing, etc., in pyrochemical
reprocessing, electrorefining and cathode processing are
the key steps. Molten LiClKCl eutectic salt is used as the
electrolyte at 500 C under inert argon atmosphere for the
separation of uranium, plutonium and minor actinides from
the fission products through electrorefining process [2, 3].
To initiate the electrorefining process, 56 wt% UCl3
containing molten LiClKCl salt is used as the electrolyte.
The container material used for electrorefining process
should withstand the highly aggressive molten salt envi-
ronment along with UCl3 at high temperatures and it
should not undergo degradation. Since pyrochemical
reprocessing is a batch process and it involves the handling
of highly radioactive materials, the vessel used for the
electrorefining process should also possess the endurance
for longer operation. Ferritic steels are proposed for the
fabrication of electrorefining vessel. Previous studies on
the corrosion behavior of 2.25Cr1Mo and 9Cr1Mo steels
exposed to molten LiClKCl salt at 600 C revealed that
2.25Cr1Mo steel is more prone to corrosion attack com-
pared to 9Cr1Mo steel [4]. Hence, 9Cr1Mo steel is
proposed as container material for the electrorefining pro-
cess because of its relatively better corrosion resistance in
molten chloride environment.
Thermal spray [5] coatings on metallic substrates are
used widely for improving their oxidation and wear resis-
tance. Atmospheric plasma spray (APS) coatings have been
developed on various structural materials and their corro-
sion resistance has been evaluated for pyrochemical
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reprocessing applications [610]. Ceramic coatings devel-
oped by plasma spray process on the structural materials
for pyrochemical reprocessing have been found to protect
the substrate materials from molten salt corrosion. Besides
being corrosion resistant, the overlay coating on the sub-
strate is also expected to have good adhesion/bonding with
the substrate, no interaction with the environment in which
it is used, minimum wettability and ability to withstand
thermal cycles.
Periasamy et al. [11] evaluated the durability of ZrN and
HfN in molten LiClKClNaClUCl3 at temperatures
ranging from 525 to 900 C for durations in the range
4485 h under argon atmosphere. They observed that ZrN
and HfN experience weight loss under all experimental
conditions due to the formation of volatile products and/or
electrochemical dissolution. Formation of the volatile zir-
conium and hafnium chlorides may be attributed to the
reaction of the nitrides with chlorine gas or chloride ion,
which in turn is generated by the reaction of UCl3 species
present in the salt with oxygen. The corrosion behavior of
yttria stabilized zirconia (YSZ) coating on various struc-
tural materials such as 2.25Cr1Mo steel, 9Cr1Mo steel,
Ni-based alloys 600, 625, and 690 has been studied by Ravi
Shankar et al. [4] and they reported that the YSZ-coated
specimens exhibit better corrosion resistance than the
uncoated specimens; however, premature spallation of the
coating is observed, probably due to either imperfections in
the coating or accidental ingress of oxygen and moisture
during the corrosion test. Recently, we have investigated
the corrosion behavior of the structural materials, stainless
steel 410 (SS 410), alloy 600 and 9Cr1Mo steel in LiCl
KCl molten salt at 500 and 600 C by thermogravimetry in
inert (argon) and reactive (argon ? oxygen) atmospheres
and observed the attack by molten salt to be more in 9Cr
1Mo steel than in SS 410, followed by alloy 600 under both
the atmospheres [12]. As the corrosion behavior of these
structural materials in high temperature molten LiClKCl
UCl3 salt has not been reliably reported in literature, the
present study has been undertaken to evaluate the corrosion
behavior of 9Cr1Mo steel and YSZ coated 9Cr1Mo steel
in LiClKClUCl3 molten salt at 600 C under argon
atmosphere for their application in electrorefining process.
2 Materials and Methods
2.1 Specimen Preparation
The chemical composition of 9Cr1Mo steel specimen is
given in Table 1. As-received and YSZ coated 9Cr1Mo
steel specimens of dimensions 50 9 10 9 5 mm were
used for the corrosion studies in molten LiClKClUCl3
salt. The 9Cr1Mo steel specimens were polished with SiC
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emery papers up to 1200 grit. The polished specimens were
grit blasted and 250 micron thick NiCrAlY interlayer
coating and 50 micron thick YSZ top coat were deposited
by plasma spray process using a METCO 3 MB plasma
gun at M/s. Spraymet Surface Technologies Pvt. Ltd.,
Bengaluru. The plasma spray parameters used to deposit
the coatings are given in Table 2. The coating was
deposited on all faces of the rectangular specimens up to a
height of 35 mm.
2.2 Molten Salt Corrosion Test
The electrorefining process in the pyrochemical repro-
cessing of spent nuclear metallic fuels was carried out in
molten LiClKCl salt at 500 C. As the molten salt was
highly hygroscopic, traces of moisture or oxygen present in
the molten salt would affect the performance of the elec-
trorefining process. Therefore, actual pyrochemical repro-
cessing was carried out in inert atmosphere glove boxes. To
simulate the real conditions of the electrorefining process,
the present study was carried out under inert argon atmo-
sphere. The LiCl (44.48 wt%)KCl (55.52 wt%) eutectic
mixture was initially purified by passing chlorine gas at
500 C for about 30 min. Molten LiClKCl salt containing
UCl3 was prepared by equilibrating uranium metal with
cadmium chloride in LiClKCl eutectic salt at 500 C [13].
Uranium content in the LiClKClUCl3 salt was estimated
by Davies and Gray method [14]. The LiClKCl molten
salt containing 4 wt% UCl3, thus produced was loaded in a
recrystallised alumina crucible along with the 9Cr1Mo
steel specimens and thermocouple and the loaded crucible
was sealed in a stainless steel cell inside an argon atmo-
sphere glove box. The cell assembly containing 9Cr1Mo
steel specimens in the molten salt was heated in a furnace
to 600 C and corrosion testing was carried out for 100,
250, 500 and 1000 h under argon gas atmosphere. The
uncoated and coated 9Cr1Mo steel specimens were tested
in the molten salt separately under identical experimental
conditions. Before and after the immersion test, the spec-
imens were ultrasonically cleaned using water and acetone
and allowed to air dry. The initial and final weights of the
specimens exposed to the molten LiClKClUCl3 salt were
recorded to assess the extent of corrosion.
2.3 Characterization
During the course of corrosion test, the 9Cr1Mo steel
specimens were removed from the molten salt at various
durations such as 100, 250, 500 and 1000 h and were
examined visually. The surface morphology and elemental
analysis were carried out using scanning electron micro-
scope coupled with energy dispersive spectroscopy (SEM
EDS, Mini SEM). The tested specimens were mounted in
Trans Indian Inst Met

Table 1 Chemical composition of 9Cr1Mo steel specimen in wt%

Fe Cr Mo C Si Ni Mn V Nb

Balance 8.97 0.94 0.104 0.41 0.20 0.55 0.20 0.09

Table 2 Plasma spray parameters used for depositing NiCrAlY bond
coat and YSZ top coat on 9Cr1Mo steel specimens
Process parameters (unit) NiCrAlY/YSZ coatings
Plasma arc current (A) 450
Arc voltage (V) 60
Primary gas Ar
Secondary gas H2
Powder feed rate (g/min) 4045
Spraying distance (mm) 100
Ar gas flow rate (l/min) 8090
Type of gun used 3 MB
epoxy and used for cross-section examination and ele-
mental mapping by SEMEDS. X-ray diffraction (XRD)
patterns of the tested specimens were recorded using
monochromatic Cu Ka radiation and the phases (corrosion
products) were identified using the standard JCPDS files.
The XRD pattern of the 1000 h exposed sample was
obtained in glancing incidence X-ray diffraction (GIXRD)
mode, while all the other samples were characterized by
normal XRD mode.
3 Results and Discussion
3.1 Weight Loss Measurements
The percentage weight loss of the uncoated 9Cr1Mo steel
specimens exposed to LiClKClUCl3 molten salt at 600 C
for 100, 250 and 500 h durations were 0.5, 3.1 and 7.6,
respectively. Weight loss of the specimens increased with
immersion time. The percentage weight loss for 100 h dura-
tion was higher compared to the percentage weight loss of
9Cr1Mo steel specimen (0.31) exposed to LiClKCl molten
salt for the same duration [4]. The percentage weight loss of
YSZ coated 9Cr1Mo steel specimens exposed to LiClKCl
UCl3 molten salt for different durations were insignificant.
3.2 Surface Characterization
3.2.1 Uncoated 9Cr1Mo Steel Specimens
The SEM images of the uncoated 9Cr1Mo steel specimen
before and after the molten salt corrosion test are shown in
Fig. 1a, c, respectively. The 9Cr1Mo steel specimen
before corrosion test appeared to be uniform with some
polishing lines and the corresponding EDS profile (Fig. 1b)
showed 9.03 wt% Cr, 1.00 wt% Mo and balance Fe. The
SEM examination of the molten salt corrosion tested
uncoated 9Cr1Mo steel specimen revealed both porous
and corrosion product regions (Fig. 1c). The surface mor-
phology with surface roughening indicated the dissolution
and etching of 9Cr1Mo steel. The attacked region showed
porous structure, which might have formed due to the
removal or dissolution of alloying elements into the molten
salt from the exposed surface. These dissolved elements
migrated to other regions of the substrate and formed the
corrosion product layer on the exposed surface of the
substrate. Dissolution of metal at hot spot and metal
deposition at colder regions due to thermal gradient, as
reported in literature [15, 16] upheld the observation in the
present study.
The SEM images of the porous region of uncoated 9Cr
1Mo steel specimens after molten salt exposure for 100,
250, 500 and 1000 h durations are shown in Fig. 2ad. It is
evident from these images that the extent of attack of the
9Cr1Mo steel specimens increased with increase in the
duration of exposure to molten salt. Grain boundary attack
and grain pull out were visible in the SEM images. With
increase in the exposure time, the attack became more
uniform and the attack was not only restricted to grain
boundary but also caused preferential surface dissolution.
The surface morphology of 1000 h exposed sample
(Fig. 2d) showed a highly porous structure. The molten salt
attack and the leaching of alloy elements were higher for
1000 h exposed sample compared to other specimens. The
increase in porosity could be due to higher penetration of
molten salt that had resulted in the higher dissolution or
leaching of alloying elements.
The SEM images of the corrosion product region of
9Cr1Mo steel specimens exposed to molten salt for dif-
ferent durations are shown in Fig. 3ad. Significant quan-
tity of corrosion products were observed as the duration of
exposure increased. Cracks were visible on the corrosion
product region at higher magnification. No significant
difference was observed between the corrosion product
regions of exposed samples for various durations. It is
observed from Figs. 2 and 3 that the surface morphology of
9Cr1Mo steel specimens exposed to molten salt for dif-
ferent durations had similar features except that the

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Fig. 1 SEM image of a plain 9Cr1Mo steel substrate, b EDS elemental analysis of plain 9Cr1Mo steel substrate and c uncoated 9Cr1Mo
steel specimen after exposure to LiClKClUCl3 molten salt at 600 C for 100 h
corrosion attack was more penetrating and prominent all
over the surface with increase in the duration of exposure.
The results of the EDS elemental analysis, given in
Table 3 revealed that the porous and corrosion product
regions of the molten salt tested uncoated 9Cr1Mo steel
specimens had different chemical composition. The
amount of Cr found in the corrosion product region was
lower than that in the porous region, which could be
attributed to either the dissolution of Cr or the formation
of volatile Cr compounds. Presence of high oxygen con-
tent in the corrosion product region might be due to the
formation of oxides of Fe and/or Cr. The oxygen content
in the argon cover gas was maintained at less than 2 ppm.
Formation of oxides of Fe and Cr were possible at low
concentrations of oxygen [17]. Hence, the abundant cor-
rosion products formed on the exposed surface of 9Cr
1Mo steel specimens could be of iron oxide and chro-
mium oxide.
Cross section examination of the tested uncoated 9Cr
1Mo steel specimens at different durations showed similar
features. The cross section image of the sample exposed to
molten salt for 100 h duration is shown in Fig. 4. The
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exposed surface had irregular and deep cavities, which
were visible at severely attacked regions. Some of the
regions were surrounded by corrosion product which could
be due to the preferential attack of grain boundaries. It
could be inferred from the EDS analysis that selective
diffusion of Cr was the mechanism for the corrosion of
uncoated 9Cr1Mo steel in LiClKClUCl3 molten salt.
3.2.2 Coated 9Cr1Mo Steel Specimens
The surface morphology of the as-received YSZ coated
9Cr1Mo steel specimens and those exposed to LiClKCl
UCl3 molten salt at 600 C for different durations of 100,
250, 500, and 1000 h are shown in Fig. 5ae. After expo-
sure to molten salt the surface became more rough and
some pores were formed. The surface morphology of the
samples changed with increase in duration of molten salt
exposure, as shown in Fig. 5ae. The samples exposed for
100 and 250 h exhibited irregular surface than 500 and
1000 h exposed samples, probably because of the removal
of loosely held coating particles from the surface after long
exposure.
Trans Indian Inst Met

Fig. 2 SEM images showing porous regions of uncoated 9Cr1Mo steel specimens after exposure to LiClKClUCl3 molten salt at 600 C for
a 100 h, b 250 h, c 500 h and d 1000 h

The standard Gibbs free energy change, DGr for the are shown in Fig. 6. In the EDS mapping, layers of coating
reactions of ZrO2 and Y2O3 with chlorine have been shown elements were visible in all the tested samples, indicating
in the reactions (1) and (2) [18]. Since the values of DGr for that even after corrosion test, the coating did not peel off
these reactions were positive at 600 C, no possible reaction from the specimen. However, in the case of 1000 h tested
was expected between the YSZ coatings and chlorine. sample, the YSZ coating thickness had reduced signifi-
cantly and became discontinuous (not found in some
ZrO2 2 Cl2 g ! ZrCl4 g O2 g; DGr kJ/mol locations). The bond coat was clearly distinguishable from
185 1 the EDS mapping of Ni and Al elements. As the bond coat
2 Y2 O3 6 Cl2 g ! 4 YCl3 g did not undergo any type of degradation and was intact on
3 O2 g; DGr kJ/mol the substrate, it was confirmed that the base metal had no
730 2 contact with molten salt, thereby preventing the corrosion
of 9Cr1Mo base metal.
The elemental analysis of the YSZ coated 9Cr1Mo steel
specimens tested in molten salt for 1000 h, by EDS (shown in 3.3 X-Ray Diffraction Analysis
Fig. 5f) confirmed the presence of elements from top coat
(YSZ), bond coat (NiCrAlY) and LiClKClUCl3 molten 3.3.1 Uncoated 9Cr1Mo Steel Samples
salt even after thorough cleaning of the samples for a couple
of times. Fe peaks detected on the tested YSZ coated Figure 7 shows the XRD patterns of uncoated 9Cr1Mo
specimens might be due to the deposition of iron oxide from steel specimens before immersion studies and after 100, 250,
the uncoated region of the specimen. Presence of uranium on 500 and 1000 h exposure in molten salt. The XRD results of
the tested YSZ coated specimens indicated that deposition of the 9Cr1Mo steel specimen before the molten salt exposure
salt had occurred on the surface of the coating. showed the peaks corresponding to FeCr (JCPDS no. 34-
The EDS elemental mapping of the cross sectional SEM 0396). The XRD results obtained for the exposed surfaces of
image of YSZ coated 9Cr1Mo steel specimen after uncoated 9Cr1Mo steel specimens were identical and the
exposure to molten LiClKClUCl3 salt for 100 h duration patterns revealed the presence of FeCr (JCPDS no. 34-

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Fig. 3 SEM images showing corrosion product regions of uncoated 9Cr1Mo steel specimens after exposure to LiClKClUCl3 molten salt at
600 C for a 100 h, b 250 h, c 500 h and d 1000 h

Table 3 Composition of porous and corrosion product regions (in

wt%) obtained from EDS elemental analysis
Region Elements Exposure time (h)
100 250 500 1000

Porous region Fe 77.40 86.00 82.48 41.13

Cr 7.00 7.34 7.03 0.31
O 12.71 6.17 9.46 49.29
Corrosion product region Fe 74.68 76.44 67.34 73.07
Cr 2.35 1.33 1.48 0.69
O 22.56 22.22 29.23 26.24

0396) and UO2 (JCPDS no. 41-1422) on the surface of the

samples. The reason for the formation of UO2 on tested
samples has been explained as follows: Among the salt
mixture components, thermodynamically, UCl3 was the least
stable component and was susceptible to oxidation. Upon
oxidation of UCl3 in the salt mixture, UO2 was produced as
per Eq. (3) [11]. The possible source of oxygen for this
reaction could be from any one of the following: (a) oxygen
Fig. 4 Cross section SEM image of uncoated 9Cr1Mo steel
specimen after exposure to LiClKClUCl3 molten salt at 600 C
for 100 h duration
dissolved in the salt mixture, (b) ingress of oxygen through
the joints in the molten salt test assembly or (c) residual
oxygen impurity in the argon gas in ppm range.

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Trans Indian Inst Met

Fig. 5 SEM images of a as-received and YSZ coated 9Cr1Mo steel specimens after exposure to LiClKClUCl3 molten salt at 600 C for
b 100 h, c 250 h, d 500 h and e 1000 h and f EDS elemental analysis of 1000 h exposed YSZ coated 9Cr1Mo steel specimens

2 UCl3 2 O2 g ! 2 UO2 3 Cl2 g; DGr kJ/mol
501600  C
3.3.2 Coated 9Cr1Mo Steel Specimens
The XRD pattern of as-sprayed YSZ coating on 9Cr1Mo
steel specimen, as shown in Fig. 8 consisted of tetragonal
and cubic phases. The X-ray diffraction patterns of YSZ
coated 9Cr1Mo steel specimens after exposure to LiCl
KClUCl3 molten salt for 100, 250, 500 and 1000 h are
3
shown in Fig. 8. All the XRD patterns showed the peaks
corresponding to YSZ and UO2. The cubic and tetragonal
phases of ZrO2 were present and no phase transformation
of zirconia occurred after the exposure to molten LiCl
KClUCl3 salt.

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Fig. 6 EDS elemental mapping of YSZ coated 9Cr1Mo steel specimen after exposure to LiClKClUCl3 molten salt at 600 C for 100 h
duration
4 Conclusions
Corrosion behavior of YSZ coated and uncoated 9Cr1Mo
steel samples was investigated in molten LiClKClUCl3
salt at 600 C for 100, 250, 500 and 1000 h. With increase
in exposure time, the percentage weight loss in uncoated
9Cr1Mo steel specimen increased and YSZ coated 9Cr
1Mo steel specimen showed insignificant weight loss.
Surface morphological examination revealed that the tested
uncoated samples exhibited porous region with low Cr and
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corrosion product region enriched with Cr. The mechanism
of corrosion in the uncoated 9Cr1Mo steel material was
the selective diffusion of Cr from the exposed surface.
Surface morphology of the molten salt tested YSZ coated
samples showed more smooth surface compared to the as-
coated sample. The XRD patterns of tested uncoated
samples revealed the presence of base metal FeCr and
UO2, while the tested YSZ coated samples revealed the
presence of zirconia and UO2. Based on the weight loss and
surface characterization results, it was concluded that YSZ
Trans Indian Inst Met
Fig. 7 X-ray diffraction patterns of uncoated 9Cr1Mo steel spec-
imens before and after exposure to LiClKClUCl3 molten salt at
600 C for 100, 250, 500 and 1000 h duration
Fig. 8 X-ray diffraction patterns of YSZ coated 9Cr1Mo steel
specimens before and after exposure to LiClKClUCl3 molten salt at
600 C for 100, 250, 500 and 1000 h duration
coating had provided adequate protection to 9Cr1Mo steel
specimens against corrosion in LiClKClUCl3 molten
salt.
Acknowledgments The authors acknowledge Dr. B. Prabhakara
Reddy, Scientific Officer H and Shri. P. Venkatesh, Scientific
Officer F, Chemistry Group, IGCAR for providing the molten salt.
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