Materials Science and Engineering A369 (2004) 144150

Investigation of an as-sprayed NiCoCrAlY overlay coating.

A thermoanalytical approach
K. Fritscher, C. Leyens , U. Schulz
DLR German Aerospace Center, Institute of Materials Research, D-51170 Kln, Germany
Received 2 September 2003; received in revised form 27 October 2003

Abstract
A low pressure plasma sprayed (LPPS) NiCoCrAlY aircraft turbine blade overlay coating was investigated by differential thermal analysis
(DTA). A pronounced irreversible endothermic reaction peak was observed at 975 C for the as-sprayed coating. No equivalent reaction is
observed for the LPPS coating in the annealed state and in NiCoCrAl (Ni:Co = 2:1) compositions after slow furnace cool-down as well. The
reaction scheme for the partial ternary AlNiCrNi system was taken as a reference standard for understanding the irreversible reaction, and
was reexamined where necessary. The four-phase solid state reaction in the ternary system at 995 C, according to -Ni + -NiAl  -Ni3 Al
+ -Cr, is compared with the occurrence of the reaction observed at 975 C on the as-sprayed NiCoCrAlY coating material. It runs most likely
according to -Ni +  -Ni3 Al -Cr + -NiAl. The reaction at 975 C is discussed in terms of metastable phase formation sequences.
2003 Elsevier B.V. All rights reserved.
Keywords: NiCoCrAlY overlay coating; Low pressure plasma spraying; AlCrNi; AlCoCrNi

1. Introduction
Superalloy components in the hottest sections of gas
turbines need the application of overlay coatings like
NiCoCrAlY compositions in order to resist effectively
the environmental attack by hot gases and deposits. The
coatings are commonly deposited by low-pressure plasma
spray (LPPS) or electron-beam physical vapor deposition
(EB-PVD) techniques. To an increasing extent the coatings
are also used as bond coats for ceramic thermal barrier coatings (TBC) to make the parts even more durable in service.
The mechanisms by which these coatings become effective rely on the generation and maintenance of stable
and adherent oxide layers on their surface that form during surface engineering procedures and during service as
well. Service temperatures at and beyond 1000 C necessitate the application of alumina-forming coatings. The
most-suited stable -Al2 O3 phase serves to sustain environmental attacks in at least two respects: (i) it protects
MCrAlY-coated substrates against hot gas corrosion due to
the high chemical stability and low diffusivity, (ii) it can
Corresponding author. Tel.: +49-2203-601-3570;
fax: +49-2203-68936.
E-mail address: christoph.leyens@dlr.de (C. Leyens).

chemically bond to ZrO2 -based TBCs by solving Al3+ in

ZrO2 [1].
There are multiple approaches to make overlay coatings
more effective. They refer to two fundamental lines: to
improve the coatings by chemical modification (e.g. alloying with optimal trace concentrations of reactive elements
for better spallation resistance, introduction of diffusionretarding elements like Re for less substrate/coating interdiffusion as well as better creep resistance, addition of
-Al2 O3 stabilising elements [2], etc.), and by microstructural modification (e.g. microcrystallization for enhanced
oxide plasticity and adhesion and for homogenization of
oxide growth via preferential -Al2 O3 formation [3,4]).
The sputter-deposition of an ordered metastable Ni(Cr, Al,
Ti, Si) phase coating isomorphous to CsCl-type -NiAl has
turned out to be most effective in calming down oxidation
kinetics on SX superalloys, and it was believed that the fine
grain size of the coating promoted formation of a highly
protective oxide scale [5].
It has been shown that the diffusive fluxes in two-phase
alloys depend on the size and the form of second phase
distributed in the matrix phase (e.g. the -phase) which
can fundamentally alter the oxidation behavior [6,7]. Accordingly early -Al2 O3 formation could be successfully
accelerated even at 900 C, if a narrow-spaced lamellar

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doi:10.1016/j.msea.2003.10.319
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K. Fritscher et al. / Materials Science and Engineering A369 (2004) 144150

structure in a NiCoCrAlY coating was provided [8].

Since most MCrAlY-based coatings are multiphase alloys,
the microstructural arrangement of the phases is of uppermost importance. The two main phases -(Ni, Co, Cr) and
-NiAl have the advantageous capability to form aluminia
scales on oxidation. The early stages of oxidation between
900 and 1100 C, however, are different for both phases
in NiCrAlY alloys with regard to kinetics and generation
of transient oxide phases [2]. So the -Al2 O3 forming
-(Ni, Cr) phase is reported to oxidize slower than the
transient-alumina forming -phase. Hence the oxide growth
on NiCoCrAlY coatings will not necessarily proceed cooperatively. Anyway microstructural effects in multiphase
protective coatings should aim at the provision of a homogeneous growth process to attain a single-phase oxide layer
in order to reduce detrimental interphase stresses within
the growing oxide [5,6]. Transient microstructures in the
metallic sublayer, however, appear to be promising probably due to inherent diffusion properties for the formation of
favorable scales. So the potential of any microstructure has
to be considered in terms of its utility. LPPS NiCoCrAlY
coatings are commonly subjected to post-coating abrasive
procedures for better aerodynamic performance via blasting, vibration grinding, or media finishing. Subsequent heat
treatments aim at equalizing the microstructures. Hence
some microstructural features will be lost by this way, that
otherwise may exert a beneficial effect on the performance
of superalloy components.
The aim of the thermoanalytical study is to trace
metastable phases and transient microstructures in as-coated
LPPS coatings, that otherwise are mostly devoid in the
state-of-the-art fully processed NiCoCrAlY coatings and
have not been reported so far. By keeping their potential
usability in mind their formation will be discussed.

2. Material and experimental techniques

NiCoCrAlY coating powder (Amdry 365-1, composition stated by the supplier: Ni base, 22.82Co, 17.93Cr,
12.47Al, 0.010C, 0.53Y, 0.24 others (in wt.%), 636 m
particle diameter size) was LPPS deposited on a moderately
transferred-arc heated (<350 C) superalloy plate. Instead
of common grid-blasting the plate was intentionally polished before to allow subsequent mechanical removal of the
deposit from the plate. More experimental details are given

145

in [9]. Approximately, 100 m thick deposits were rolled

up to 5 mm diameter thick coils of typically 1.5 g weight
and fitted in corundum crucibles for DTA (Netzsch 420) investigations. They were carried out under fluent Ta-gettered
argon gas (nominal purity 99.9997%; Ar flow rate 1 l h1 )
at 5 K min1 .
High purity (>99,99%) aluminum, nickel, chromium and
cobalt (>99.7%) were taken for constitutional investigations
to provide equilibrium reference data in the NiCoCrAl
system. Solidliquid equilibrium phase transformations
were obtained by DTA, eutectic compositions identified by
light microscopy. Details are given elsewhere [9]. Solid state
transformations on annealed and slowly furnace-cooled
VIM cast compositions were followed under high vacuum by dilatometry (Bhr; 50 mm long sample) and DTA
(Setaram TGA 92; typically 0.2 g weight) at 1 K min1 .

3. Results
3.1. Characteristic equilibrium phase transformations,
their implementation in the constitution of the AlNiCrNi
system, and the effect of Co
The constitution of the ternary system AlCrNi has been
critically reviewed and collated in a compendium [10]. A
more recent thermodynamic assessment giving calculated
temperatures for invariant reactions differs appreciably [11],
particularly for melt equilibria. The accuracy of the data,
however, is relevant for this work, which spurred the authors
to reexamine and update the data by DTA, dilatometry and
light microscopy [9,12]. The data of [10,11] and the authors
data are compared in Table 1. The corresponding partial
reaction scheme AlNiCrNi is shown in Fig. 1.
Incorporation of cobalt in the system changes it to a
quaternary system with the consequences due to Gibbss
phase rule: invariant reactions become monovariant (transition temperatures widen to temperature intervals), and phase
compositions are changed. The invariant four-phase reactions E and U2 will be modified through substitution of 1/3
nickel in return for 1/3 cobalt and shifted to other temperature (and composition) regimes according to Table 2. The
solid/liquid reaction E goes up by some 34 K according to
DTA data [9,11]. DTA peaks of both eutectic AlCrNi and
AlCoCrNi alloys establish nearly identical shapes, the
latter being slightly broader; both alloys can be directionally

Table 1
Invariant equilibria in the AlNiCrNi system showing temperature data and compositions (at.%) after [10,11] and data from this work
Reaction

Abbreviation of
the reactions

T ( C), composition (at.%)

(Rogl [10]; Dupin et al. [11])

T ( C); composition (at.%)

(This work )

L + -Ni =  -Ni3 Al
L = -NiAl +  -Ni3 Al
L = -Cr + -NiAl + -Ni
-NiAl + -Ni = -Cr +  -Ni3 Al

p1
e2
E
U2

1372
1370
1320, 15Al, 40Cr, 45Ni; 1283
990; 996

1382
1380
1302; 13.47Al, 37.45Cr, 49.08Ni
995

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K. Fritscher et al. / Materials Science and Engineering A369 (2004) 144150

Fig. 1. Elongation vs. temperature of AlCrNi and AlCoCrNi compositions of Table 2 obtained at 1 K min1 showing the inflection point at 995 C
for the AlCrNi alloy that is attributed to the reaction U2 (-NiAl + -Ni = -Cr +  -Ni3 Al).

solidified to lamellar microstructures the same way indicative of similar solidification modes. Hence a minute solidification interval in the order of 1 K for the quaternary eutectic is supposed). The solid/solid reaction U2 is hypothesized to be represented by the turning point on dilatation
at 995 C for the AlCrNi eutectic alloy in Fig. 2 which
is mainly attributable to the volume gain of voluminous
-NiAl phase forming there at the expense of the more
densely packed  -Ni3 Al phase, and the temperature for U2
is confirmed by the DTA onset point on heating/cooling of
996/987 C in Fig. 4 is reduced by some 200 K (first evidence of  -Ni3 Al phase by microscopy below 800 C). The
range of the interval for this reaction downwards, however,
is addressed, for e.g. in [13] and may be terminated below
700 C.
3.2. Differential thermal analysis (DTA) of as-coated PS
NiCoCrAlY deposits
The occurrence of metastable phases was traced by means
of differential thermal analysis. A noticeable reaction peak of
as-coated NiCoCrAlY samples occurred at 975 C on moderate heating at 5 K min1 , signaling phase transformation
(see Fig. 3). This reaction is an irreversible one: it vanished
on repeated heating of the same sample.

3.3. DTA of slowly solidified bars of the NiCoCrAl

system
No DTA signal was observed in the 975 C range for
annealed and slowly furnace-cooled material (Fig. 4). A
minor DTA peak signal occurred at 1041 C on heating,
which, however, was many times smaller in peak area than
the peak in Fig. 3. It shows no correlation with elongation versus temperature plots at this temperature in Fig. 2,
although identical alloy compositions have been used in
either case. The occurrence of the small peak can hardly
be explained. This signal is not observed on cooling. The
energy release due to the relief of mismatch stresses can
not account for the peak effect on heating, as the coefficient
of thermal expansion of and is practically the same
[14]. The CTE for (15.46 106 K1 , RT to 1000 C)
and NiCoCrAlY (16.9 106 K1 , RT 1000 C), measured by the authors, support this view. Instead the sluggish
orderorder kinetics between vacancy and antisite concentration in -NiAl may possibly be transferred to this
temperature range on heating and give there a minor thermal
effect [15].
The start of the gradual transus of  -Ni3 Al + -Cr to
-Ni + -NiAl in the quaternary alloy system on heating can hardly be identified in Fig. 4 by comparing the

Table 2
Invariant phase equilibria in the AlNiCrNi system with transition points (second column from the left, reexamined data) and corresponding four-phase
reactions in the AlCoCrNi (Ni : Co = 2 : 1) system with transition intervals (right)
Ternary reactions in
AlNiCrNi system

T ( C); composition
(at.%), (wt.%)

Analogous quarternary reaction

T ( C); composition
(at.%), (wt.%) below

L = -Cr + -NiAl + -Ni

1302; 13.47Al, 37.45Cr,

49.08Ni; 7.0Al, 37.5Cr,
55.5Ni

L -Cr + -NiAl + -Ni

-NiAl + -Ni = -Cr +  -Ni3 Al

995

-NiAl + -Ni -Cr +  -Ni3 Al

13051306; 13.47Al,
16.36Co, 37.45Cr, 32.72Ni;
6.75Al, 19.25Co, 35.5Cr,
38.5Ni
800<700

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147

Fig. 2. Reaction scheme in the stable ternary system AlNiCrNi (left side), and sector of the scheme transferred to a distinct compositional case in
the quaternary system Al(Co, Ni)Cr(Co, Ni) (column at the right side). In this particular case, the effect of the substitution of 1/3 Ni in return of 1/3
Co is shown (arrows), above all the gain in temperature of the four-phase solid/liquid reaction E by some 34 K and the decrease of the four-phase
solid/solid reaction U2 by some 200 K for starting a broad transition interval via a monovariant reaction mode.

quaternary and ternary DTA plots taken on DTA samples

of equal mass. It may probably start at approximately
700 C on heating. On cooling now more effects can be
seen.

4. Discussion
4.1. Differential thermal analysis data and deduced
reaction scheme for the as-sprayed coating
Thermoanalytical methods in metallurgy are commonly
devoted to constitutional issues. They are uncommon or
rarely used to investigate microstructural subjects in alloys.
If, however, a distinctive change in the microstructure yields
an outstanding thermal effect the occurrence of a dramatic
variation of the thermodynamic potential, e.g. an unexpected
phase transition can be assumed. This is obviously true for
the as-sprayed coating.
The irreversible endothermic reaction observed at 975 C
will be called into question whether it is related to the
four-phase solid state reaction U2 in the equilibrium ternary
NiCrAl system, according to
-Ni + -NiAl  -Ni3 Al + -Cr

Fig. 3. DTA peak of as-sprayed NiCoCrAlY coating on heating at

5 K min1 attributed to a potential solid-state reaction (2) according to
-Ni +  -Ni3 Al -Cr + -NiAl.

(1)

at 995 C. Three arguments at leasta constitutional and

two kinetic argumentsnegate the validity of this reaction
for the as-sprayed material. The evidence of mainly fcc

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K. Fritscher et al. / Materials Science and Engineering A369 (2004) 144150

Fig. 4. DTA plot of cast slowly furnace-cooled quaternary AlCoCrNi alloy material on heating and cooling at 1 K min1 compared to same-sized
and processed ternary AlCrNi showing absence of essential peaks at the temperature interval under discussion below 1000 C for the quaternary
alloy. Meanwhile the ternary alloy shows distinctive signals on heating at 996 C and on cooling at 987 C indicating an invariant solid-state reaction
according to -Ni + -NiAl -Cr +  -Ni3 Al.

phases of the PS quenched-in structure like the / eutectic

obtained by XRF and TEM [9,16] plead rather for a modification of the reaction (1) according to
-Ni +  -Ni3 Al -Cr + -NiAl

(2)

and correspondingly suggest a very different reaction

scheme for as-sprayed material. The disappearance of
 -Ni3 Al on heating to 975 C is in accord with the constitutional expectations of this quaternary system [13] where
 -Ni3 Al is not stable at this temperature, but rather below
800 C.
The second argument still referring to reaction (1) will
recall that a reaction peak can be transferred on rapid heating to higher temperatures due to sluggish transformation
kinetics, but will never occur at a lower temperature than
that of equilibrium. The transient for the disappearance of
 for Astraloy, e.g. is raised by 125 K at a heating rate of
300 K min1 [16]. So it is not reaction type (1) to occur at
975 C which is essentially lower by 20 K on heating instead.
The third argument, admittedly speculative, is the sharpness of the DTA peak and its high intensity. A sharp DTA
peak is typical for invariant reactions to occur in unary, bi-

nary or ternary metallic systems. It is atypical in quaternary

systems in agreement with Gibbs phase rule (one degree
of freedom left). The apparent contradiction can be solved
like this: the two phases -Ni +  -Ni3 Al identified in the
as-sprayed structure have compositions which, although extremely supersaturated, do not necessarily represent quaternary concentrations, as shown in Table 3. The compositions
are essentially binary at least for the  -Ni3 Al phase. The
phase contains additional Y and Ti impurities, whereas
the Ni and Co atoms may be considered to be very similar
in their basic aspects and can easily replace each other in
nearly most deliberate mixtures. At high solidification rates
of the coating a tendency was observed that ternary and quaternary elements will be rejected from the / structure, and
Table 3
Composition (in at.%) of matrix and  -Ni3 Al second phase in LPPS
eutectic grains analyzed by EDS [9]
Phases

Ni

Co

Cr

Al

Ti

 -Ni

Balance
21.61

Traces
12.07

Traces
64.04

33.0 2

1.94

0.3

3 Al
-Ni, Co

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K. Fritscher et al. / Materials Science and Engineering A369 (2004) 144150

instead extended solid solutions will be established [9]. So

in essence binary phases are supplied to the reaction which
now can be understood to perform analogous to invariant
reactions, for e.g. in ternary systems.
The composition of the supersaturated  -Ni3 Al phase
comes close to that of stable -NiAl in binary -NiAl in
equilibrium with  (37.4 at.% Al at 1000 C [17]), whereas
the supersaturated -Ni phase is represented by + or
even single -Cr phase under the corresponding equilibrium
conditions. So the former fcc / structure will decompose
to bcc phases at reaction temperature and simultaneously
approach quaternary compositions. This accumulation of rearrangements as well of phases and in compositions will result in a pronounced thermal effect as observed. So reaction
(2), although fed by metastable phases in a quaternary system, is essentially of the invariant type due to essentially
binary phases. Consequently it establishes a distinct particular transition temperature, which is different from that of
the stable reaction U2 . And apart of that the reaction itself
is not related in any way to reaction (1). It is irreversible
since the metastable phases become transformed into more
stable phases. They, of course, will follow the stable reaction scheme according to reaction (1) on repeated heating
of the same sample.
The intensity of the DTA peak suggests two items that
refer to the demand for energy: at first excessive energy is
needed for the transformation of metastable (and highly Al
supersaturated)  to -NiAl, which is a compound showing
a particularly high energy of formation. Secondly, transport
energy is needed for the spontaneous provision of matter for
instantaneous formation of the stable phases (and a different
microstructure and composition) that depends on enhanced
diffusivity of matter.
In superalloys,  is commonly stabilized by some more
elements like Ta, Ti and Nb so that the transition U2 occurs
at somewhat higher temperatures than 995 C [18]. The Ti
impurities in the coating, however, cannot account for the
stabilization of the  -phase in the coating as Ti, although
involved in reaction (2), has not been identified in this particular  -Ni3 Al phase but exclusively in the -Ni phase.
Nonetheless involvement of Ti would increase the temperature of reaction (1). What we observe is reaction (2) at a
lower temperature instead. It is obviously one more argument that reaction (2) is not related in any way to reaction
(1).
4.2. Phase composition and solubility range extension
issues
The tendency for the rejection of ternary and quaternary elements from the phases in the / structure during
solidification of the as-sprayed NiCoCrAlY coating, as
documented in [9], is worth while to be considered in more
detail. Either it deals with an effect, that is generally valid
for higher-order systems, but not detected so far; or it is it
typical for this system only. No references report on this dis-

149

tinct effect to the authors knowledge but refer to a shifting

of solubility ranges on splat-cooling in binary and ternary
systems [1921]. So, in spite of mental reservations, it is
considered in the following if this effect is a characteristic
of this NiCoCrAlY coating.
In general, melts on splat-cooling experience the lowest temperatures for solidification attainable. For e.g.
glass-forming deep eutectic systems can attain a special
solid state which is still isomorphous with the liquid
state, without a liquidsolid transition during cooling. Besides the glassy phases from deep eutectics, there are
many examples for systems that form metastable phases
on high cooling rates. Due to this trick they still have
a liquidsolid transition, but at a lower temperature. The
most prominent example for it is the ironcarbon system
and the metastable FeFe3 C variant. So in consequence it
should be asked, if there are some more tricks to get low
solidification temperatures.
Moderate undercooling at the melt front is necessary to
initiate eutectic solidification. The undercooling interval
on quenching of regular eutectic structures forming melts,
however, is limited to a few degrees, e.g. to approximately
15 K for the NiAlTi system [22]. In cases where the eutectic reactiona complex long-range ordering processis
the only one feasible in a system, it may pay off in the end,
however, to support the melting-point depressant tendency
of this reaction by introducing a variant of eutectic reactions
(equal to preference of binary instead of multi-elemental
phases) to lower the solidification temperature for this
particular case below the regular limit for undercooling
eutectics even more. In this system, the formation even of
two metastable phases and  (instead of one e.g. for
the FeFe3 C system) is just involved for this very purpose.
More melting point depression is still desirable. As shown
in Fig. 1 and Table 2, the lowest melting temperature (reaction E) in the (stable) ternary system AlNiCrNi is 34 K
lower than in the quaternary Co-containing system. This is a
gain of 20% for a potential lowering of the temperature necessary for undercooling, provided that a similar tendency of
temperature depression is valid for the metastable solidification reaction by following a ternary scheme. In essence, the
trick on splat-cooling the quaternary system is assumed
to be the switching over to a ternary reaction mode in order
to benefit from the lower solidification temperature. The
compositions of the phases need to become pre-adjusted
towards binary compositions to apply to the requirements in a ternary system, e.g. for performing invariant
reactions.
An explanation, different to constitutional issues, may refer to kinetic arguments. It may be mentioned that crystals
grow more easily from multi-component melts on solidification if they are composed of no more than two elements.
Under stringent conditions of rapid solidification they will
do it even more. But examples showing the opposite can be
cited [21]. Which of the explanations is more likely is beyond the scope of this work.

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K. Fritscher et al. / Materials Science and Engineering A369 (2004) 144150

5. Conclusions
As-sprayed NiCoCrAlY coatings exhibited an irreversible
thermal reaction peak on DTA heating at 975 C. It is
attributed to the reaction of metastable  -Ni3 Al and supersaturated -(Ni,Cr) phases to stable -Cr + -NiAl. The
formation of the metastable and supersaturated phases is
discussed with reference to the transformation temperatures
of the reaction schemes in which the respective phases are
involved.
Acknowledgements
The authors thank Dr. Rudolf Henne, DLR Institute of
Applied Physics, for procuring plasma sprayed samples. We
highly appreciate Horst Gedanitz for conscientious conducting the thermoanalytical experiments.
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