Materials at High Temperatures

ISSN: 0960-3409 (Print) 1878-6413 (Online) Journal homepage: https://www.tandfonline.com/loi/ymht20

Microstructural studies of NiAl-based model

alloys and commercial coatings after isothermal
oxidation

H. Svensson, J. Angenete, K. Stiller & V. Langer

To cite this article: H. Svensson, J. Angenete, K. Stiller & V. Langer (2003) Microstructural
studies of NiAl-based model alloys and commercial coatings after isothermal oxidation,
Materials at High Temperatures, 20:3, 421-427, DOI: 10.1179/mht.2003.049

To link to this article: https://doi.org/10.1179/mht.2003.049

Published online: 02 Jan 2014.

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MAHT/Svensson 31/10/03 12:08 pm Page 421

Microstructural studies of NiAl-based model

alloys and commercial coatings after
isothermal oxidation

H. Svensson1, J. Angenete1, K. Stiller1 and V. Langer2

1Departmentof Experimental Physics and 2Department of Inorganic Chemistry,
Chalmers University of Technology and Göteborg University, SE-412 96 Göteborg
Sweden

Four commercial aluminide diffusion coatings (one Pt-free) and four polycrystalline NiAl model materials,
isothermally oxidised in laboratory air at 1050°C for 1 hour, have been investigated. The coatings were
deposited on a single crystal Ni-based superalloy, CMSX-4. Two of the model materials are binary
alloys containing different Al amounts. The two other have the same Ni/Al ratio as the binary alloys
but were alloyed with 4 at% Pt. In order to control the surface roughness, all materials were polished
prior to oxidation. Microstructural studies have been conducted using X-ray diffraction and scanning
electron microscopy. To get a deeper insight on the platinum influence on the oxide structure, two com-
mercial coatings (one Pt free and the other modified with Pt) were also investigated using transmission
electron microscopy. The results obtained are discussed according to the influence of Al and Pt con-
tents in the materials.
Keywords: aluminide diffusion coatings, isothermal oxidation

Numerous studies have also demonstrated beneficial

INTRODUCTION
High temperature (above 900°C) oxidation protection of
Ni-base superalloy components in gas turbines and aero-
engines is commonly achieved by application of -NiAl
based coatings. The underlying idea is that -NiAl (or
alloys thereof) easily forms protective and slow growing
-Al2O3 scales, through which transport of oxygen
and/or aluminium is greatly retarded. This means that
further growth of the oxide becomes slow and the depletion
of Al from the bulk of the metallic component is limited
[1].
In order to better understand the mechanisms by which
-NiAl alloys and coatings form a protective scale, a large
number of scientific investigations have been undertaken.
It has been shown that at temperatures <1100°C several
transient oxide phases such as -Al2O3 and -Al2O3 may
form during early stages of oxidation of NiAl [2,3].
Upon further oxidation these metastable alumina phases
transform irreversibly to the stable -Al2O3, but the
nucleation sites of -Al2O3 phase are still under debate.
At higher temperatures a layer of -Al2O3 forms on the
NiAl immediately [4]. The morphologies of the alumina
modifications are different. Typical for -Al2O3 and
-Al2O3 are needle- or blade-shaped grains (indicating
preferential transport direction during the growth of these
crystals). For -Al2O3 a structure with thick ridges is
formed [3,5–7]. These ridges indicate faster oxidation
along the oxide grain boundaries.
effects on oxidation of NiAl alloys by additions of vari-
ous elements. One such elements is platinum which is
known to prolong the total useful lifetime of the NiAl
coatings. It has been proposed that platinum increases
diffusivity of aluminium and decreases diffusivity of other
elements thereby promoting rapid formation of alumina
scale also at low aluminium concentrations [8]. It has
been also reported that platinum improves oxide adherence
[9–11]. However, the exact mechanisms behind this
improvement are not known.
In our recent work on commercial coatings (exposed
to oxidation in air at 1050°C for times ranging from 20
hours to 20000 hours) it was observed that deleterious
spinel phases were not present in the oxide scales on Pt
modified coatings [2,12]. These investigations were per-
formed on coatings in the as-received condition, which
means that their surface roughness (defined by the coat-
ing process) was different. However, surface roughness
plays an important role not only for the microstructure of
the scales, but also for which phases that will be present
in the scale. Thus, in these investigations it was difficult
to be conclusive concerning the influence of platinum.
Moreover, the presence of significant amounts of alloy-
ing elements from the substrate in the commercial coat-
ings that may affect oxidation made separation of the
role of Pt from other effects difficult (if not impossible).
Therefore, to further clarify the oxidation of coating
materials, comparison between the oxidation of complex

0964-3409/03/03/00035–12
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Microstructural studies of NiAl-based model alloys and commercial coatings: H. Svensson et al.

commercial materials with simple model alloys is neces-
sary. Moreover, since the initial (transient) stages of
oxidation play an important role for the continuing oxi-
dation [2,12], short-term oxidation experiments must be
carried out. Thus, in the present study, short-term oxidation
of model NiAl alloys with varying Al content with and
without addition of Pt was compared to that of two com-
mercial aluminide diffusion coatings. In order to exclude
the effect of initial surface roughness, all materials were
polished before oxidation. The results presented in this
paper are still quite preliminary, but clearly indicate the
importance of such studies for a more complete under-
standing of the oxidation mechanisms of real coating
systems.
EXPERIMENTAL
Materials
Four polycrystalline NiAl model materials were investi-
gated. Two of the materials were binary alloys contain-
ing different Al amounts. The two other had the same
Ni/Al ratio as the binary alloys but were alloyed with
4 at.% Pt. The material compositions are reported in
Table 1. According to scanning electron microscopy
(SEM) and energy dispersive X-ray spectrometry (EDS),
all the model materials consisted of only -NiAl phase,
prior to oxidation.
Besides, one Pt free and three Pt modified aluminide
diffusion coatings, on a commercial single crystal super-
alloy material, CMSX-4, were analysed. The composition
of the substrate material is presented in Table 2. The
compositions of the coatings close to the surface, deter-
mined by TEM-EDS, are listed in Table 3. Only major
elements are presented. The simple coating, PWA73, was
produced by inward growth pack aluminisation as well
as the Pt modified RT22 coating. SS82A is an inward
Table 1 Composition of the model materials (at%)
Alloy Ni Al
NiAl 50.0 50.0
NiAl(lowAl) 61.0 39.0
NiAlPt 48.0 48.0
NiAlPt(lowAl) 58.6 37.4
grown above pack coating and the MDC150L coating is
an outward grown chemical vapour deposited coating.
Further details concerning these coatings are given else-
where [13–15]. PWA73 can be considered as a Pt-free
equivalent to RT22 in terms of process parameters and
Al content.
Methods
All materials were polished with diamond paste down to
1 m prior to oxidation in order to control the surface
roughness. The samples were then cleaned in methanol
and acetone. The model materials were in the shape of
discs with a thickness of 300 m, comparable to the
thickness of the commercial coatings. An isothermal oxi-
dation of 1 hour at 1050°C was performed in laboratory
air.
The existence of different oxide phases was investi-
gated by X-ray diffraction (XRD). A Siemens D5000
instrument equipped with a Göbel mirror was used. To
minimise the contribution from the bulk material, a low
incidence angle (5°) was used. The diffractograms were
evaluated with help of the PDF-1 database [16].
Surface morphology of the oxides was studied with a
LEO 1550 Gemini SEM equipped with a field emission
gun (FEG) and a CamScan S4-80DV SEM equipped with
a Link eXL EDS system.
To investigate the platinum role on the oxidation rate,
the weight gain of the two model materials (NiAl and
NiAlPt) was measured using a Sartorius R160P balance
with 10 m readability and the weight gain per unit area
was calculated. Such an investigation was not possible to
perform on commercial coatings since available sample
of the Pt free PWA73 was the too small in size to provide
reliable information and be compared with Pt containing
RT22 sample. Moreover, to get deeper insight on the Pt
influence on the oxide structure, the two commercial
coatings (RT22 and PWA73) were analysed by trans-
mission electron microscopy (TEM) in a Philips CM200
FEGTEM instrument, equipped with a Link ISIS EDS
Pt system. Unfortunately the shape of the model materials
samples proved to be unsuitable for preparation of TEM
– specimens. The TEM foils were produced by focused ion
– beam (FIB) milling [17] in a Fei FIB200THP workstation,
4.0
4.0 using Ga ions at 30 kV. Further details regarding the
specimen preparation are given elsewhere [2,17,18].

Table 2 Nominal composition of CMSX-4

RESULTS AND DISCUSSION
CMSX-4 Ni Al CoCr Ti
Ta Mo W Re Hf Oxide scale

At.% 63.7 12.6 9.3 7.6

Model materials
1.3 2.2 0.4 2.0 1.0 Results from SEM surface observations of model materials
0.03
are presented in Figures 1–5. The micrographs reveal that
the oxide developed on the stoichiometric -NiAl
Table 3 Matrix composition close to the surface of the coatings before
sample (Figure 1) contains blades or whiskers protruding
oxidation (at%)
in different directions, while the oxide formed on the Al-
poor sample (Figure 2) displays a very flat surface. The
Coating Ni Al Pt Co Cr morphology of the oxides on the Pt containing materials
(Figure 3 and Figure 4) was similar to those on the Pt
PWA73 44.5 48.2 – 6.5 0.8
RT22 35.0 42.8 15.7 4.8
free equivalent alloys. No ridges were observed on the
1.8 oxide surface of any model material.
SS82A 23.4 55.0 13.3 3.7 Blade and whisker forms are typical for transient oxide
4.7 phases such as- -, and γ-Al2O3 while -Al2O3 grains are
MDC150L 48.8 40.1 3.7 5.1 block-shaped [19]. Thus, SEM studies indicate the pres-
2.2
ence of several different oxide phases.

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Microstructural studies of NiAl-based model alloys and commercial coatings: H. Svensson et al.

Figure 1 Oxide formed on NiAl sample. Blades typical for transient Figure 4 Flat oxide formed on NiAlPt(lowAl) sample. The
Al2O3 phases such as  or  are clearly visible. NiAl(lowAl) sample shows a similar oxide morphology.

Figure 2 Flat oxide surface of NiAl(lowAl). (Notice the difference in Figure 5 Spallation of the oxide on NiAl(lowAl) sample.
magnification.)

then grows to consume the rest of the oxide scale and

also into the metal. In present investigation ridges, typical
for -Al2O3 surface morphology, were not observed. This
phase was, however, clearly present according to XRD
results in three of the investigated materials: NiAl(lowAl),
NiAlPt(lowAl) and NiAlPt. It is thus probable that 1 h of
oxidation at 1050°C is too short to completely transform
metastable alumina up to the surface of the oxide.
Detailed TEM investigations are planned to confirm this
statement.

Commercial materials
Figures 6–9 show SEM surface view of PWA73, SS82A,
RT22 and MDC150L respectively. The surface mor-

Figure 3 Oxide formed on NiAlPt material showing similar morphol- Table 4 Phases detected by XRD analysis of the model materials. , 
ogy as NiAl material. and  are Al2O3 phases

Material Al at.% Pt at.%   

The results from XRD analyses are summarised in NiO NiAl2O4 -NiAl ´-Ni3Al
Table 4. It is clear that in most cases the oxide consists
of several Al2O3 phases and also of Ni-rich oxides. The NiAlPt(lowAl) 37.4 4.0 x
x x
only exception is the NiAlPt(lowAl) material on which NiAl(lowAl) 39.0 – x x
-Al2O3 is a predominant oxide phase. Further investiga- x x x
tions to clarify this issue are planned. NiAlPt 48.0 4.0 x x x
As mentioned earlier, the nucleation site for α-Al2O3 x x
has been under debate. Recently Yang et al. [7] showed NiAl 50.0 – x x
x x x
that this phase nucleates at the metal–oxide interface and

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Microstructural studies of NiAl-based model alloys and commercial coatings: H. Svensson et al.
Figure 6 Irregular oxides formed on PWA73.
Figure 7 Irregular oxide, with blades and needles protruding, formed
on SS82A.
Figure 8 Oxide formed on RT22.
phology of the oxide on the MDC150L material looks like
that on the NiAl and NiAlPt model materials, indicating
the presence of transient alumina phases. However, such
an observation cannot be confirmed by the SEM surface
analysis of the three others coatings.
The results from XRD analyses are summarised in
Table 5. The phase depicted as a spinel is most probably
a mixed spinel since its diffraction peaks are slightly dis-
placed with respect to peaks from pure spinel phases,
such as NiAl2O4, CoAl2O4 and CoCr2O4. It is also clear
424 MATERIALS AT HIGH TEMPERATURES 20(3)
Figure 9 Oxide formed on MDC150L with characteristic needles pro-
truding from the surface.
that, as in the case of model materials, transient alumina
phases are still present in all coatings after 1 h of oxidation.
The presence of  phase in two samples (PWA73 and
MDC150L) is somewhat unexpected since this phase is
usually observed at temperatures below 1000°C in binary
NiAl alloys [19]. Its existence in the commercial materials
might be explained by the presence of alloying elements
influencing the stability of the transient phases.
Another interesting observation is that the Pt-free
material, PWA73, is the only commercial coating develop-
ing NiO and spinel phases. NiO phase was reported by
[20] to form during early stages of oxidation at 1000°C
on Ni–Al–Cr alloys. The occurrence of this oxide is also
detected in the model materials, but was not observed in
our previous investigations of PWA73 (concerning 100 h
of oxidation) in which only the spinel phase was found.
The comparison of the different oxide phases (Tables 4
and 5) present in the model and commercial materials
reveals that the presence of Pt seems to suppress the for-
mation of spinel phases. This result is also consistent
with previous investigations on commercial coatings [2].
On the other hand, Pt seems to have no such effect on the
formation of NiO phase.
Figure 10 shows TEM images of the oxides formed on
15.7% Pt containing RT22 (a) and on Pt-free PWA73 (b).
The oxide on Pt-rich material consists mostly of about
0,5 m large, quite equiaxed grains with faceted voids.
This contrast is typical for -Al2O3. On the other hand, the
oxide on the Pt-free material contains many elongated
0.1 m  0.7 m grains with many planar defects.
Analyses of diffraction patterns and analytical analyses of
these grains show that they are -Al2O3. The oxide thick-
ness on the Pt-free material is about 2 m, i.e. larger that
on the Pt-rich RT22, 1 m. This is in good agreement
Table 5 Phases detected by XRD analysis of the commercial
materials. (x) determined by TEM
Al at.% Pt at.%   
NiO Spinel NiAl
PWA73 48.2 – x x (x)
x x x
RT22 42.8 15.7 x x
x
SS82A 55.0 13.3 x x
x
MDC150L 40.1 3.7 x x x
x
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Microstructural studies of NiAl-based model alloys and commercial coatings: H. Svensson et al.

Figure 10 (a) TEM cross-section of oxide on RT22 (15 at% Pt). The oxide contains mostly -Al2O3. The oxide thickness is about 1 m. (b) TEM
cross-section of PWA73 (without Pt). Other phases than -Al2O3 (such as ) are present. The oxide thickness is about 2 m.

with gravimetrical investigations of the Pt-free and Oxide/metal interface and underlying metal
Pt-rich model materials showing that the calculated
weight gain for NiAl and NiAlPt was 6.7  10–4 g/cm2 XRD investigations of the materials (Tables 4 and 5) show
and 3.25  10–4 g/cm2 respectively. that, in the case of model materials with low Al content,

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Microstructural studies of NiAl-based model alloys and commercial coatings: H. Svensson et al.
some ′-Ni3Al grains are present close to the metal sur-
face indicating a transformation of −NiAl phase. Among
the commercial materials, MDC150L has the lowest Al
content, 40.1 %, about the same as that of the NiAl(low
Al) model material in which  transformation to ′ is
observed. According to the NiAlPt phase diagram [21],
the phase border between  and ′ is at 37 at% of Al. It
is thus expected that minor depletion of Al at the metal
oxide surface will result in ′ formation in both
NiAlPt(lowAl) and NiAl(lowAl) materials as it is
observed. The reason for suppressed transformation of
-NiAl in MDC150L is due to the presence of alloying
elements, Co and Cr, in this material. Both of these
elements are known to stabilise  phase with respect to
transformation to ′ [22]. On the other hand, small
amounts of Pt (3–4%) do not have any influence on for-
mation of ′.
The spallation resistance of the oxide scale is con-
trolled by several factors. Firstly, the amount of stresses,
that build up at the oxide/metal interface during oxide
growth and (perhaps, more important) during cooling
from oxidation temperature, have a great influence. These
stresses will be higher for a thicker oxide scale. Besides,
the mechanical properties of the scale and of the under-
lying metal will have an influence on the resulting
stresses. Secondly, the presence of voids at the oxide/
metal interface will greatly reduce the spallation resistance
of the oxide. Thirdly, the strength of the interface itself
(the adhesion between the scale and the metal) will also
play a role.
The degree of spallation on model materials was
different, being highest for NiAl(lowAl) (Figure 5) and
NiAlPt(lowAl) samples on which typical voids in the
spalled areas were observed. Spallation on stoichiomet-
ric -NiAl occurred only occasionally. This is in accor-
dance with at least the two first mechanisms mentioned
above, since (1) a lower Al content is expected to increase
the oxidation rate , which in turn should increase result-
ing mechanical stresses and (2) in an Al-poor -NiAl
alloy, the diffusivity of Ni is greater than that of Al [24],
which should give back diffusion of Ni from the inter-
face and subsequent void formation at the interface
[12,25,26].
In the case of the commercial materials, no significant
spallation was observed. However, during FIB preparation
of the TEM foils from the RT22 and PWA73 samples,
voids were observed at the metal/oxide interface in both
samples. Figure 11 is a TEM micrograph showing the
presence of voids in RT22. The observation of voids
both in the Pt free PWA73 and in the Pt-containing RT22
materials shows that the presence of this element does
not prevent formation of interfacial voids. The FIB image
in Figure 12 confirms that these voids did not arise dur-
ing the specimen preparation since they are already
present at an early stage of ion milling.
Figure 11 TEM image of the rectangular area marked in Figure 12.
The bright areas at the oxide/metal interface are voids formed during
oxidation.
426 MATERIALS AT HIGH TEMPERATURES 20(3)
Figure 12 Secondary electron image of RT22 by FIB showing that the
voids have not been created during the specimen preparation.
SUMMARY
Four commercial aluminide coatings and four NiAl
model materials, isothermally oxidised in 1050°C for 1h,
have been investigated using SEM, XRD and TEM.
After this short oxidation time complex oxide scales
containing stable -Al2O3 and transient phases such as 
and  were observed on most of the investigated materials.
This shows that oxidation at 1050°C for 1 hour is too short
to completely transform metastable alumina phases. The
obtained results clearly show that Pt positively influences
oxidation of both NiAl model alloys and commercial
coatings by suppressing the occurrence of deleterious
NiAl2O4 and other spinel phases. These phases allow
outward diffusion of cations and contribut to faster
oxidation rate. On the other hand no effect of Pt on for-
mation of voids at the oxide/metal interface was observed.
Spallation of the oxide as a consequence of interfacial
void formation was observed on all the investigated
model materials. The spallation was most severe on the
Al-poor samples.
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