Surface & Coatings Technology 201 (2007) 6239 6246

www.elsevier.com/locate/surfcoat

Study of oxyhydroxides formation on P91 ferritic steel and slurry coated by

Al in contact with Ar + 80%H2O at 650 C by TG-Mass spectrometry
F.J. Prez , S.I. Castaeda
Universidad Complutense de Madrid, Dpto. de Ciencias de Materiales e Ingeniera Metalrgica, Madrid 28040, Spain
Received 3 July 2006; accepted in revised form 16 November 2006
Available online 29 January 2007

Abstract
During the corrosion of P91 steel in a steam atmosphere of Ar + 80%H2O, at 650 C for 100 h the following volatile species were identified by
means of a mass spectrometry: Cr(g), CrO2(g), CrOOH(g), CrO2(OH)2(g), Cr(OH)6(g), FeOOH(g), Fe0.947O(g), Fe2O3(g), CO, CO2, Mo(g), and
HNi(g). Al(g), AlO(g) and FeOOH volatile species were formed on FeAl slurry-coated P91 steel that was oxidized in similar conditions for 200 h.
The presence of the volatile species CrO2(OH)2(g) during oxidation of the uncoated P91 steel indicated that in these initial stages of oxidation, the
sample undergoes a breakdown of chromia scales before the FeAl slurry-coated sample, loosing its protection against oxidation and thus
increasing its oxidation rate. In-situ thermogravimetric measurements indicated that the FeAl-slurry coating increased the oxidation resistance of
the P91 steel up to 40 times. The morphology/composition and structure of the oxidized samples were also studied using SEM/EDS and XRD
techniques.
2006 Elsevier B.V. All rights reserved.
Keywords: Mass spectrometry; Volatile species; Protective coating; Steam oxidation

1. Introduction
Ferritic steels are characterized by its excellent oxidation
resistance, while austenitic steels are characterized by its good
toughness and strength properties. Martensitic 912% chromium steels are used for critical components in steam power plants
such as rotors, piping and valve bodies due to their low thermal
expansion, good thermal conductivity and acceptable corrosion
properties. It is well known that creep strength of some
materials can be increased by reducing its chromium content,
but it is deleterious for the corrosion resistance [1].
Many authors [2,3] have studied the oxidation kinetics of
ferritic/martensitic steels such as the P91 and P92 under different
conditions, including temperatures between 600700 C range
and diverse atmospheres (O2, N2, Ar, water steam, etc.). All these
works investigated the initial stages of oxidation but no attempts
of verifying experimentally the volatile species formed are
performed. F. J. Prez et al. [4] presents early an experimental
work on P91 and P92 steel oxidized at 650 C and 1 atm in Ar +
Corresponding author.
E-mail address: fjperez@quim.ucm.es (F.J. Prez).
0257-8972/$ - see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2006.11.029

10%H2O steam. They combined thermogravimetric measurements and mass spectrometry during oxidation process, determining volatile chromium-hydroxides and oxyhydroxides species
such as: CrOOH(g), Cr(OH)3(g), Cr(OH)6(g) and CrO2(OH)2(g)
in P91 steel and Cr(OH)2(g), Cr(OH)3(g), CrO(OH)2(g), Cr(OH)4
(g) and CrO(OH)4(g) species for P92 steel. These results suggest

Fig. 1.

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F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

Fig. 2.

that evaporation of chromium oxides and oxyhydroxides occurs

when steam is present. In these oxidation conditions, F. J. Perez et
al. did not find evidence of the presence of volatile species
CrO2OH(g) in the ferritics steels P91 and P92 studied, but they
detected CrO2(OH)2(g) species in the P91. These authors also
reported the formation of FeO(g) and FeO1.5(g) volatile species
during the oxidation of P92 steel. They finally conclude that the
breakaway oxidation begins earlier for P92 than for P91 steel.
The oxyhydroxide vapour species, CrO2OH(g) [5,6] and CrO2
(OH)2(g) [7,8] have been identified on volatile of chromium from
Cr(s) and Cr2O3(s) samples oxidized in the presence of air and
steam atmosphere at high temperatures. Also, the species Cr3O9
(g), Cr4O12(g) and Cr5O15(g) have been identified from chromium
volatile in air at temperatures below 500 K [9,10].
H. Asteman et al.,[11] reported the volatile species CrO2
(OH)2(g) during the oxidation of type 304 L stainless at 873 K
in the presence of and O2 + 10%H2O atmosphere and caused by
chromium evaporation.
Several researchers [1215] have attributed the formation of
volatile species such as CrO3(g), CrO2OH(g) or CrO2(OH)2(g) to
the breakdown of chromia scales at temperatures near 1000 C,
and with the subsequent depletion of Cr in the scale formed.
The alloys based on Ni, (Co, Fe) with incorporation of Cr or
Al have very beneficial effect for the formation of protective
alumina oxide (Al2O3), for example, additions of 10% of

chromium they can favour the alloy alumina formation with less
of 5% of Al. Alumina does not suffer from problems of scale
loss at high temperatures and provides very good resistance to
oxidation [1620]. Previous works has looked at Ni-base and
alumina forming alloys for surface recuperators to oxidation to
high temperatures and in water vapour [21,22].
Slurry coatings are suitable for internal and external
application to small (e. g. blades) and large components (e. g.,
steam pipe, casings, valve internals) and can be relatively easily
applied to complex shape objects. Slurries of aluminium layer
can be understood as diffusion coatings since the adhesion
between the deposited layer and the substrate is of chemical
nature, i.e. during the heat treatment of the coating. Migration of
the elements between the coating and the substrate takes place.
The main mechanism of degradation during the oxidation of
these coatings is the interdiffusion with the substrate on which
Al spreads towards the interior of the substrate and the Fe from
the base material goes out, reaching a minimum critical
aluminium concentration in the surface of the coating making
it to loose the capacity to form protective oxide layer [23].
In our present work, oxidation of the P91 steel without and of
FeAl-slurry coating at 650 C and +80%H2O atmosphere is
investigated.
Our main objective is to find a direct relation between TGMS (TG-Mass spectrometry analysis) experiments and the

Fig. 3.

F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

Fig. 4.

formation of volatile inorganic oxyhydroxides species that

appear for these samples in their initial period of oxidation
under the mentioned conditions. Comparison with thermodynamic predictions for the system and previous published works
will also be discussed. All those data will give important inputs
for coating design based on experimental evidences and valid
thermodynamic calculations.
2. Experimental
Oxidation tests at high temperatures were performed on the
samples of ferritic/martensitic steel P91 without and with Slurry
coating of FeAl. The chemical composition of P91 steel:
Fe = 89.35, Cr = 8.10, Mo = 0.92, Mn = 0.46, Si = 0.38, C = 0.10,
Ni = 0.33, P = 0.020, V = 0.18, Al = 0.034, Nb = 0.073, N = 0.049
and S = 0.002 (all composition in weight percentage). Samples
with a size of 10 20 3.5 mm were cut for each test and
polished to 600-grid with SiC paper before of the oxidation and
coating deposition. All samples were cleaned with acetone in
ultrasound bath for 10 min.
The painting used for the Slurries coatings of FeAl was
IPCOTE 9183 (supplied by Indestructible Paint): Cr2O3 (2.5
10%), H3PO4 (1025%) and powder of Al (2550%). Water
and diluted chromic acid was used as dissolvent of the painting.
Previously, the painting is homogenized by thermal agitation,
then placed in a stove at 85 C for 15 min and then to a furnace
at 350 C for 30 min to eliminate the dissolvent. Next, a

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diffusion treatment of the painting is made in furnace for 10 h at

700 C to produce the protective coatings phases. After the
thermal treatment, the samples were slightly polished with SiC
paper (30 m) for to eliminate the excess painting.
Identification of volatile species emanating from samples
during oxidation was performed with the Quadrupole Mass
Spectrometer QMS 422 (PFEIFFER VACUUM instruments)
placed inside of the oxidation system.
Oxidation experiments and thermogravimetric (TG) measurements were performed using a thermobalance (sensitivity of
10 7 g) of symmetrical thermoanalyser (SETARAM-TAG 16
model). Initially, the furnaces were pumped by a membrane
pump to a pressure of 10 2 mbar. A constant flow of 500 ml/
min of high purity Ar gas (99.999% pure) is introduced in the
system, filling both furnaces until reaching the atmospheric
pressure, places where the sample in study and the reference
SiO2 crucible are located.
The steam was introduced to the furnaces by a constant flux
of argon carrier gas (16 ml/min) through a water flask
(humidifier). The distilled water from the flask is heated to
give the desired relative humidity percentage by volume of each
experiment.
Routinely, for the oxidation tests of the samples, we
previously must calibrate the thermobalance (verifying level
zero), measure the sensitivity of the Mass spectrometer and
make the measurement of the background of the system. This is
made with two quartz crucibles as calibration samples placed in
each furnace and also maintaining the same conditions of
oxidation.
Always in all the results of mass spectrometry we subtracted
the measures of the background respective. Thus, to the final
only we would obtain the measures of the sample and not of the
system (the apparatus or any gas contaminants). These
considerations and conditions of calibration were reported
before in another work [4]. In this work only we reported the
final results of each sample.
On the results of composition analysis by mass spectrometry
presented and to the diverse mass numbers assigned to the
volatiles species detected in the oxidation of the samples of this
work it can be stated: first, we to find the probable species
volatile have made a series of simulations for material
assumptions that they will be as the bases of our alloys (Cr,
Fe, Si, Al, Cr2O3, Al2O3, SiO2, etc.). The simulation conditions

Fig. 5.

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F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

3. Results and discussion

Fig. 6.

of oxidation were the same as all the experiments. The Thermocalc program (Software AB:Fundation of Computational
Thermodynamics 19952003, Stockholm Sweden) and the
HSC Chemistry for Windows (Software Outokon: version 3.02,
Finland 1994) have been used for the simulations. All the
theoretical results that we obtained have been compared with
others of the bibliographies.
All specimens were oxidized at 650 C in Ar + 80%H2O
atmospheres and with exposure times of 50 to 200 h. The test of
oxidation of FeAl slurry-coated P91 steel was made in three
stages and oxidized in the same conditions without having to
remove them from thermobalance in all the experiment: the first
stage was of 100 h, after an additional time of 50 h and finally
another time of 50 h until completing 200 h of test.
We have observed an apparent noise in the TG spectrums
when we worked with high percentages of water steam (greater
of 50%H2O) and when the samples were of small size.
Phase component of the surface scales of the oxidized samples
was studied by the X-Ray Diffraction (XRD) of a Philips X'Pert
diffractometer, using Cu K (1.54056 ) radiation and by means
of angle 2 and grazing incidence (GIXRD).
The microstructure observation by scanning electron microscopy (SEM) and X-ray energy dispersive spectrometry
(EDS) measurements were performed in a JEOL-JSM 6400
scanning electron microscope operated at 20 KV.

The mass change as a function of testing time (continuous

lines) of oxidized samples of the P91 steel with and without Alslurry coating at 650 C in Ar + 80%H2O atmosphere and the
temperature profile (dash line) are showed in the Fig. 1. As seen
from the figure, in the first 100 h of oxidation the coated sample
loses mass around of 3.5 mg/cm2 and while the P91 steel
without coating gains mass around of 4 mg/cm2. The results
demonstrate in the initial stages of oxidation under these
conditions, the sample of FeAl-slurry/P91 loses mass by
evaporation of aluminium or perhaps due volatile oxide of
aluminium by chemistry reaction of the coating with the
environment. The loss of aluminium by evaporation of the
coating will finish until this element by diffusion reacts totally
with the substrate (P91 steel), to form protective coatings, as
intermetallics or the alumina (Al2O3) that has formed in all
surface maintains the property of protective coating to the
oxidation. The P91 steel without coating in the initial stages of
oxidation gains great amount of mass, this is due to that it begins
to lose chromium in form of volatile gaseous species as,
chromium-hydroxides and oxyhydroxides, thus losing the
protection to the oxidation and then begins the breakaway of
oxidation with the formation of iron oxides in its surface.
Fig. 2 shows the results of the spectrum of mass spectrometry
made simultaneously during TG measurements of oxidation of
the P91 steel without coating at 650 C in Ar + 80%H2O for 100 h.
The species were identified as, Cr(g), CrO2(g), CrOOH(g), CrO2
(OH)2(g), Cr(OH)6(g), FeOOH(g), Fe0.947O(g), Fe2O3(g), CO,
CO2, Mo(g), and HNi(g). By theoretical calculations, the
evaporation of Cr and Fe in form of volatile species is thermodynamically possible at this temperature in atmospheres with the
desired water vapour percentage. The presence of the volatile
species CrO2(OH)2(g) during the initial stages of oxidation of P91
steel indicated that the sample is in the breakdown of chromia
scale dose occur. It is suggested that this chromium depletion may
have important implications for the long-term stability of the
protective oxide scale formed on P91 steel, as other authors have
been proposed in the case of ferritic steels which were oxidized in
water steam [715]. This may result in Fe2O3 (hematite)/Fe3O4
(magnetite)/FeO (wstite) formation, and breakaway corrosion

Fig. 7.

F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

6243

Fig. 10.

Fig. 8.

that confirmed the mass spectrometer with the appearance of the

other species as: oxides, hydroxides and oxyhydroxide of iron.
This effect could explain the observation by Khanna and Kofstad
[24]. Other investigators also have suggested these results by
thermodynamic calculations for oxidations at higher temperature
(1000 C), but with smaller percentage of water steam [11,12]. In
addition, we have detected the fragmentation of others volatile
species of H2O, O2, N2 and Ar molecules. We make emphasise
here that, in our results of mass spectrums of the samples we will
not enter into details on these species because they are not directly
related with the oxidation process.
Fig. 3 shows the volatile species found by means of the mass
spectrometry of FeAl slurry-coated P91 steel sample oxidized at
650 C in Ar + 80%H2O atmosphere for 14 h. These important
species have been identified as Al(g) and AlO(g). The detection
of these volatile species demonstrates us the loss of mass of the
sample in the first hours of oxidation (until 100 h: Fig. 1) under
these conditions by the evaporation of aluminium of the FeAl
coating in form of gas and oxide.
Thermogravimetric and temperature measurements of an
additional time of 50 h until completing 150 h of test of FeAl-

Fig. 9.

slurry/P91 oxidized sample in Ar + 80%H2O at 650 C are

shown in Fig. 4. In the first test hours of oxidation (6.5 h) the
sample loses 0.05 mg/cm2 of mass. This is due to the
evaporation of Al of the coating in form of gas and oxide, as we
described before. However, in the time interval between 6.5 h
and 50 h we observed an increase of mass up to 0.170 mg/cm2.
These results indicated that initial oxidation stages under these
conditions, FeAl Slurry on P91 steel shows higher oxidation
resistance protection than the P91 steel without coating (substrate).
The P91 steel with slurry FeAl coating during oxidation formed a
protective alumina scale on its surface.
Fig. 5 shows the volatile species found by means of the mass
spectrometry in FeAl-slurry/P91 sample in the second oxidation
stage (sample of Fig. 4), which was exposed at 650 C in Ar + 80%

Fig. 11.

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F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

H2O atmosphere for 110 h. These species have been identified as,
Al(g), AlO(g), and FeOOH(g). The presence of these volatile
species confirms that the initially evaporated species from the
coating are in form of aluminium oxide and gas.
The small mass gain observed by TG measurements of this
sample (Fig. 4) during initial oxidation are related directly with
the presence of volatile species FeOOH and the iron oxide
layers that would have formed in the surface.

Fig. 6 shows thermogravimetric results of the third stage of

50 h of oxidation of FeAl-slurry/P91. The results demonstrate
that the sample continues its oxidation due to the possible losses
of alumina and other protective oxides or intermetallics phases
that had formed initially. Thus the sample gained an additional
mass of 1 mg/cm2 by the formation of iron oxides.
By means of these results we verified that the coating of FeAlslurry plays an important role in the formation of protective layers

Fig. 12.

F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

resistant the water steam oxidation, where the alumina protective

coating and/or the intermetallics phases formed by diffusion or
reaction of aluminium of the covering with environment avoid the
loss of chromia and thus to avoid finally the breakaway oxidation.
The results of the study of mass spectrometry made
simultaneously during TG measurements of FeAl-slurry/P91
sample that was oxidized at 650 C, in Ar + 80%H2O and by
160 h are showed in the Fig. 7. These volatile species have been
identified as Al(g), AlO(g), and FeOOH(g), and were the same
ones that we detected to 110 h of oxidation (Fig. 5). We
observed that in this time of test, the intensities of masses lines
of Al(g) and AlO(g) have diminished respect to the same ones
found to smaller time of oxidation, and while the line of the
FeOOH stays almost constant. This suggests that during this
time of oxidation the aluminium from the coating diffused or
reacted inwards the substrate (P91 steel) and then formed
protective intermetallics coatings. Also, the depletion of
aluminium would be related to the loss of the alumina by
evaporation of the species of Al that were detected during the
test and thus the sample would gradually lose its protectiveness.
These results are verified by means of the TG spectrum (Fig. 6),
where we observed as in this time the sample begins to gain
more mass due to the growth of iron oxides.
Fig. 8ab show the results of the XRD analysis in the 2
mode, of the samples of FeAl-slurry/P91 and to P91 steel that were
oxidized in the same conditions as we explained in the Fig. 1. The
results indicate that both samples present two oxide phases,
consisting of cubic magnetite (Fe3O4) and rhombohedral hematite
(Fe2O3) [25,26]. The sample with FeAl coating presents another
most predominant phase of monoclinic Fe2Al5 [27] when
compared to P91 steel (uncoated sample). By means of XRD
patterns of coated sample we did not observe other phase of
aluminium oxide and therefore we resorted to another technique
known as grazing incidence X-ray diffraction (GIXRD). This
technique helps us to determine the thin layers on the surface of the
oxidized sample. The results of Fig. 9 indicated that the sample
presents another important phase that it belongs to the
rhombohedral alumina (Al2O3) [28]. In addition, the phases of
Fe2Al5, Fe2O3 and Fe3O4 were identified, these phases were
already found before by means of the other technique of XRD
(Fig. 8a).
SEM image of the cross section of the P91 steel without coating
(sample of Fig. 8b) that was oxidized at 650 C in Ar + 80%H2O
for 200 h is showed in the Fig. 10. Observation at this magnification indicates an oxide scale formed in the surface with
thickness between 30 and 50 m. EDS analysis of the cross
section (small area) confirmed that the composition of the oxide is
a mixture of iron oxides and with atomic percentages approximately to hematite (Fe2O3) and magnetite (Fe3O4). Also, there is
internal oxidation layer of thickness between 10 and 20 m
formed between the oxides of iron and the substrate, a type mixed
spinel of iron and chromium (Cr2FeO4).
Fig. 11ab shows the micrographs at different magnification
of surface and the cross section of FeAl-slurry/P91 (sample of
Fig. 8a) after being oxidized under the same conditions as for
the P91 steel sample. In all surface (Fig. 11a) we observed that
the sample presents a granular morphology with a great

6245

roughness. In the image of the cross section of the sample

(Fig. 11b) oxide nodes were observed. The nodes presented a
diameter up to 50 m, approximately. The nodes may form
during the oxidation of the sample by the crack, pores and/or
imperfections of the protective coating.
Elemental mappings of the cross section of the oxidized
sample and of a node by means of EDS analysis are showed in
Fig. 12. The mappings indicated that the aluminium is in the
superior part of the sample and together with the oxygen formed
alumina (Al2O3) as protective layer. In the oxidation node we
observed small amounts of alumina and in other cases it was
absent. In the images of the node we observed that the iron and
oxygen together with aluminium are the elements of great part
of the node and that according to its atomic percentages by
precise analyses indicated two superficial layers: the hematite
Fe2O3 and magnetite Fe3O4. Also, we have observed another
majority Fe2Al5 intermetallic layer. In addition, in the inferior
part of the node with substrate (P91 steel) we have observed a
zone with chromium, iron and oxygen, and of composition
approached to the mixed spinel Cr2FeO4.
These complementary results found by means of the
technique of analysis EDS were verified previously with the
spectrums of XRD for both oxidized samples (Fig. 8ab).
4. Conclusions
The oxidation behaviour of P91 steel with and without FeAlslurry coating was investigated. These samples were oxidized at
650 C in Ar + 80%H2O atmosphere for 50 to 200 h.
The following volatile species as: Cr(g), CrO2(g), CrOOH
(g), CrO2(OH)2(g), Cr(OH)6(g), FeOOH(g), Fe0.947O(g), Fe2O3
(g), CO, CO2, Mo(g), and HNi(g) were identified by means of
mass spectrometry during the oxidation of the P91 steel without
coating. The presence of the volatile species CrO2(OH)2(g)
during 100 h of steam oxidation indicated that the P91 steel
loses its protective chromia (Cr2O3) scale due to the strong
deterioration of steam. This result verifies results by other
authors of the oxidation of these steels and results of by
theoretical calculations under the same conditions [715]. In
addition, when we found the fragmentation of the volatile
species that belong to oxides and oxyhydroxides of iron, they
predict the formation of the majority layer of wstite and
therefore it indicates that the sample is in state of catastrophic
corrosion.
The Al(g), AlO(g), and FeOOH(g) volatile species have been
detected for FeAl-slurry/P91 sample oxidized at the same
conditions for 110 and 160 h. The difference between these
times of the test consisted, that the species of Al(g) and AlO(g)
had diminished at the greater time of oxidation, while the
FeOOH(g) species remained constant. The reduction of Al in
the sample during the oxidation would be related later to the loss
of alumina (Al2O3) and for that reason it would not be protected
to the oxidation. Also, this loss of Al during the oxidation would
be related thermally to its diffusion towards the interior of the
substrate (P91 steel) and after together with the iron would form
Fe2Al5 intermetallic. In the oxidation up to 200 h of FeAl
coating sample we did not found another species volatile of

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F.J. Prez, S.I. Castaeda / Surface & Coatings Technology 201 (2007) 62396246

chromium that could determine the sample in state of

catastrophic corrosion.
Thermogravimetric measurements indicated that the FeAlslurry coating increased the oxidation resistance of the P91 steel
up to 40 times. SEM images of the cross section of the thickness
of oxides in both samples confirmed also the advantages of the
FeAl coating. This sample with coating after the test presented
small oxidation nodes.
The mappings of composition, EDS analysis of the cross
section of small area and X-Ray Diffraction of FeAl-slurry/P91
oxidized confirmed the presence of layers as, alumina (Al2O3),
hematite (Fe2O3), magnetite (Fe3O4), other majority intermetallic Fe2Al5, and finally a protective internal layer Cr2FeO4 of
mixed spinel type. These results help us to understand the
importance that the aluminium enhances in the formation of
protective coatings on ferritic steels.
Acknowledgment
The authors acknowledge the financial support of the
European Community under project No ENK5-CT-2002
00608-SUPERCOAT.
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