Memorie scientifiche - Trattamenti Termici

Multi-scale modeling of aging

of Waspaloy superalloy: prediction
of microstructure evolution and coupling
with mechanical properties
Betül Gövercin, Caner Şimşir

Ni-based superalloys operating under challenging conditions require high mechanical strength at elevated tempe-
ratures where heat treatment processes are crucial for those materials including solutionizing and aging. The yield
strength of these alloys arises concurrently from different strengthening mechanisms and the main strengthening me-
chanism for an alloy can change depending on the composition and processing methods. Starting from solidification,
the optimum solutionizing temperature for Waspaloy is determined and isothermal aging parameters were set with
ICME methods where results were compared with physical experiments. By using the modeling results, yield strength
estimation was conducted from room temperature to operational temperatures and validated with thermomechanical
experiments. Orowan and coherency strengthening were each found to have a great impact on yield strength, showing
the importance of heat treatment processes on Waspaloy. The methods described and the model developed can be
used for refining composition and microstructure to have the desired strength.

KEYWORDS: WASPALOY - NI-BASED SUPERALLOY - HEAT TREATMENT - PANDATTM - MODELING

INTRODUCTION
Ni-based superalloys are designed and developed to
operate under high temperatures, high mechanical loads,
and corrosive environments, in regard to the Brayton cycle
where higher efficiency systems such as turbine engines
are required (1). To provide these challenging properties,
these materials are designed by including many alloying
elements for phase transformations that contribute to
corrosion resistance and material strength at elevated
Betül Gövercin
temperatures arising from solid solution hardening and Middle East Technical University, Türkiye

grain boundary strengthening of ɣ-matrix, precipitation [email protected]

hardening, and coherency strengthening due to ɣ'

Caner Şimşir
particles. Heat treatment processes adequately designed
Simultura Material Technologies Inc, Türkiye
have a great impact on overall strength with respect to
the amount and distribution of L12 ɣ' particles. Since there
are many different mechanisms contributing to overall
strength, establishing a physically based model becomes
more crucial in alloy design fields due to the difficulty
of investigating the contribution of each strengthening
mechanism in experiments by isolating the mechanism

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Scientific papers - Heat Treatments

which is also affected by chemical composition and phase In this study, isothermal aging of Waspaloy is applied
fractions. to model the effect of each strengthening mechanism
The coherency and solid solution strengthening calculated by using the thermodynamic and precipitation
contribution on overall yield strength is found to be modeling outputs. For the validation of modeling studies,
a subject open for discussion in some studies (2-11); physical experiments were performed both at room
however, according to the authors’ knowledge, coherent temperature and around operational conditions. The
and semi- coherent particles’ interaction with ɣ-matrix model is expected to be used in alloy design in the future
and strain fields occurring due to substitutional and for the optimization of material performance with the
interstitial alloying atoms create obstacles for dislocation related composition and microstructure.
movement and increases the material strength. Therefore,
the combined effects of grain boundary, coherency, and METHOD
solid solution strengthening should be considered to Chemical, Microstructural, and Thermomechanical
predict the yield strength of the material. Experiments
Although computational alloy design studies with related To investigate the microstructural variations during heat
software give a prediction on yield strength, the results treatment and predict the yield strength accordingly, the
obtained in such simulations have shown overprediction composition of the as-received Waspaloy was analyzed
where optimization of the heat treatment parameters to with optical emission spectroscopy (OES) from 5 different
obtain desired properties is crucial for the design of such locations on diameter.
materials.

Tab.1 - Chemical composition of the as-received Waspaloy (without P and S).

Since the ingot studied was procured in hot forged and size determination. The samples cut in 0.35 mm
condition, the microstructure of the as-received ingot thickness were used for the extraction of 3mm diameter
was also analyzed from the same 5 locations with optical discs by using a disc punch and further prepared with
microscopy (OM) for the determination of mean grain size grinding and twin-jet electrolytic polishing with 10 vol. %
in accordance with ASTM E-112 and secondary electron perchloric acid at 20.5V at -5°C.
microscopy (SEM) together with energy dispersive Aged samples were subjected to CNC machining for tensile
spectrometry (EDS) for microstructural analysis including test preparation with SMR311 geometry. Gleeble 3800
ɣ', carbide size and amount determination that will affect system was used for tensile testing at room temperature,
the desired time for solutionizing. The samples were cut 580°C, 650°C, and 720° with 10 -3 strain rate.
with electrical discharge machining (EDM) and embedded
in conductive bakelite. Grinding with SiC abrasive papers Solidification Modeling
and polishing with diamond suspensions were applied for The PANDATTM software with the PanNi2023_all database
surface preparation. All samples were etched with 2 gr and chemical composition given in Table 1 were used
CuSO4 + 40 ml HCl + 40 ml Ethanol (95%) etchant (12). to predict the equilibrium and Scheil solidification
Heat treatment applications at 1080°C for 1-hour for phase compositions and phase fractions in regard to
solutionizing followed by water quenching and aging at the CALPHAD method. The thermodynamic equilibrium
850°C for 18-hours followed by water quenching were of a given system with multiphase equilibria at constant
conducted with THERMNEVO – Nevola Curing Furnace pressure is determined with respect to the summation
on 12 mm diameter rods prepared with EDM. After of molar Gibbs energies of the stable phases, leading to
solutionizing and aging, high-resolution transmission minimum Gibbs energy.
electron microscopy (HRTEM) was used for the ɣ' fraction

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 Memorie scientifiche - Trattamenti Termici

(1)

In the given formula above, nφ stands for the number of the liquid takes place at an infinite rate and there is no
moles and Gφm is for the molar Gibbs energy of phase φ diffusion in the solid phases where equilibrium is held at
(13). the liquid-solid interface. (14-16). The solute profile can
In the Scheil method, it is assumed that the diffusion in be found as:

(2)

where C S is the concentration of solute in the solid, at the modeling study and the kinetic database for Waspaloy
a fractional distance along the bar, fS, C0 is the initial is constructed by using the property model calculation
concentration of the liquid, and k is the partition results conducted by PANDAT TM. The input data for
coefficient. the precipitation modeling studies are given in Table 2,
below. The molar volume, interfacial energy, dislocation
Precipitation Modeling density and atomic spacing values are obtained from the
The CALPHAD method is developed to perform property model calculation results of PANDAT TM. Grain
thermodynamic calculations and determine the phase size is determined by using the as-received ingot as
diagrams accordingly. As this method is improved in time, mentioned in Microstructural Experiments Part; the aspect
applying kinetic calculations has also become possible by ratio and contact angle for the precipitates were used as
using the related databases formed either experimentally
the default values which is applicable to almost all the Ni-
or together with ab-initio calculations. The PANDATTM
based superalloys. By using these parameters, aging
software with the PanNi2023_all database and chemical
modeling is performed at 850°C for 18-hours by using the
composition given in Table 1 were also used in this part of
KWN model.
Tab.2 - Input parameters for precipitation modeling of Waspaloy by using PANDATTM.

Simulation Parameter ɣ-matrix ɣ' precipitates

Molar Volume [m3/mole] 7.1E-6 7.1E-6

Grain Size [µm] 35 -

Dislocation Density [m ]-2

1E-12 -

Aspect Ratio 1 1

Interfacial Energy [J/m2] - 0.030

Atomic Spacing [m] - 3.621E-10

Contact Angle [°] - 90

Langer-Schwarz-Kampmann-Wagner approach also matrix and the precipitates form in spherical shape (17-
known as KWN (Kampmann-Wagner Numerical model) 22).
is used which is a mean-field model assuming that the The nucleation rate [3] and growth rate [4] with the KWN
nucleation takes place homogeneously through the model are constructed with the formula:

(3)

(4)

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Scientific papers - Heat Treatments

Where Js is stationary nucleation rate, 𝜏 is incubation time, Yield Strength Modeling

N 0 is number of potential nucleation sites per unit volume, The overall yield strength is obtained by summing
𝛽∗ is the rate of solute atoms in matrix joining the nucleus, Orowan strengthening due to dislocation looping around
𝐶𝑃 is the concentration of the solute in the precipitate, 𝐶(𝑡) the precipitates (𝜎 𝑜𝑟𝑜), coherency strengthening arising
is the concentration of the solute in the matrix and 𝐶𝑅 is from lattice misfit between matrix and precipitates (𝜎 𝑐𝑜ℎ),
the concentration of the solute in the interface boundary. solid solution strengthening of ɣ matrix (𝜎𝑠𝑠), grain size/
boundary strengthening (𝜎 𝑔ℎ) and lattice strength of pure
nickel (𝜎0).

(5)

The linear summation method is applied by taking n=1 has penetration of dislocations to precipitates - usually, the
been found to show a better fit with experimental data. incoherent precipitates with larger precipitate sizes are
seen in the microstructure -, Orowan bowing is seen in
Precipitation Hardening the microstructure where the dislocations with lower
Precipitation hardening mechanisms such as stress bow between the particles (26,27). An extended
particle cutting and bowing were explained with the equation for the calculation of Orowan dislocation looping
implementation of the role of dislocations (23-25). strengthening is also introduced as (28-30):
In the case where the applied stress is smaller for the

(6)

(7)

where 𝐺 is matrix shear modulus, 𝜐 is the Poisson’s ratio boundary hardening occurring from the coherency of
of the matrix, 𝑓 is the volume fraction of precipitates, 𝑟 ɣ', some studies are conducted to investigate the effect
is the mean radius of precipitates, λ is mean interparticle of the coherency strains arising from the lattice misfit on
spacing and b is burgers vector. the overall yield strength of the material. Strengthening
due to lattice misfit arises from the stress fields around
Coherency Strengthening the interface at which the precipitate is coherent with the
Due to the cutting of particles or with the looping of matrix. Those stress fields restrict the dislocation gliding,
dislocations around the precipitates, Ni-based superalloys and the contribution of this misfit is explained by Brown
are mostly hardened with the precipitation of ɣ' phase. and also by (23,24,30):
Although those mechanisms rely on the antiphase

(8)

(9)

(10)

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 Memorie scientifiche - Trattamenti Termici

where χ is material constant changing from 2 to 3, ε is the distortions. These distortions interact with the dislocations
misfit strain parameter, 𝐺𝑃 is shear modulus of precipitates and strengthen the material either by dislocation locking
and 𝜐 𝑃 is the Poisson’s ratio of the precipitates, δ is the due to size mismatch, modulus mismatch, and stacking-
difference between lattice parameters of precipitate 𝑎𝑃 fault interaction, or dislocation friction (31-35)
and matrix 𝑎. The solid solution strengthening formula varies for the
ordered and disordered phases (36-38). Since both
Solid solution strengthening ɣ-matrix and ɣ' precipitates have ordered structures,
Strengthening due to solid solution occurs when the below formula introduced by Fleischer can be used for
solute element with higher strength dissolves in the the prediction of strength contribution via solid solution
solvent metal and either replaces the host atom or (39):
places between the host atoms, causing localized lattice

(11)

Where is a constant set for each element and depends blocking the dislocation motion by absorbing its
on the atomic size and modulus, is the atomic percent energy or dividing the dislocations into pieces due
of the element in the ɣ-matrix. to the misorientation between consecutive grains in
polycrystalline materials. The grain size effect on yield
Grain boundary strengthening strength is described by the Hall-Petch equation (40):
Grain boundary strengthening is often explained by

(12)

Where ky is the Hall-Petch constant that varies depending Some carbide transformations such as Cr 23C6, Cr7C3, and
on the alloy and D is the grain size. Mo3B2 boride formation were also expected to form
during the solidification. Trace amounts of Mo 3B2 that
RESULTS AND DISCUSSION formed after the material is fully solidified are expected to
In order to define the solutionizing and aging temperature positively affect the creep/tension rupture strength due
for Waspaloy, solidification under equilibrium and non- to controlling grain coarsening during heat treatment and
equilibrium conditions is analyzed. As the as-received slowing down the grain boundary sliding mechanism.
specimen’s chemical composition is compared with the
patent, it is observed that the amounts of all the alloying Differently from the equilibrium cooling conditions,
elements were within the limits. non-equilibrium solidification is expected to complete at
1142°C which is about 170°C lower than the equilibrium
With the obtained chemical composition from OES, cooling as given in Table 3-b. Due to the liquid enrichment,
equilibrium cooling solidification is conducted between solidification does not end when the solid composition is
500 to 1750°C as given in Table 3-a and it is observed equal to the initial composition. Also, the solidification
that the Waspaloy for the given composition is expected does not complete homogeneously since the segregation
to fully solidify with a low amount of TiC and ɣ-matrix at of some elements occurs during a high solidification rate.
1312°C where the obtained results are similar with the
literature, and the cause of this difference arises from The Scheil-Gulliver approach by assuming an infinitely
chemical composition and software database, mainly (41). high cooling rate for the given specimen has shown that

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Scientific papers - Heat Treatments

the ɣ-matrix is the former phase, which is expected to that is lost as the solidification is completed. TiB2
form, followed by the TiC carbides. ɣ' particles are seen borides are also expected to form as close to the end of
beginning at 1180°C and the phase transformations are solidification.
followed by Eta phase which is a metastable intermetallic

Tab.3 - Solidification modeling results completed with PANDATTM.

(a) Phase transformations in Waspaloy between 500 – (b) Phase transformations in Waspaloy between 1400 -
1750°C with equilibrium cooling conditions. 1100°C with non-equilibrium cooling conditions.

SEM analysis completed on 5 specimens and on 5 different the as-received material contains TiC and MoC carbides
locations in each specimen has shown that the material through the material on grain boundaries varying between
had undergone heat treatment since ɣ' precipitates are 0.05 to 1.5 μm size with almost spherical morphology. ɣ'
seen in the microstructure as can be observed in Figure 1. precipitates were seen in two different morphologies:
On the other hand, SEM and EDS analysis has shown that cuboidal and spherical.

Fig. 1 - Matrix SEM image with SE detector taken under 5000X magnification with ɣ and ɣ'.

Spherical phase particles’ diameter varies between 20 about 1360 MPa tensile strength at room temperature. This
to 90 nm, whereas cuboidal ɣ' precipitates are found measurement has also shown that the as-received part
in the microstructure between 30 to 200 nm. Hardness has undergone an aging process after wrought condition
measurements from those five specimens with 5 points in compared to the commercial-aged Waspaloy specimens
each have a result of 454.6 ±6.5 HV, which corresponds to seen in the literature (42-44).

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 Memorie scientifiche - Trattamenti Termici

Fig. 2 - TEM image of the as-solutionized sample

The equilibrium and non-equilibrium solidus temperatures particles occurred, dislocation pileups were observed on
are considered as the lower and upper end states for the grain boundary, and partial dislocations were found in
solidification. This approach is widely used for the the ɣ-matrix as given in Figure 2.
estimation of solidification structures and, accordingly,
for the design of the homogenization process. The As the modeling that is done with respect to KWN
solutionizing temperature is set as 1080°C and the related nucleation and growth has shown a volume fraction of 22
modeling studies have shown that the material contains % of ɣ' particles are expected in the material (Table 4-a),
only ɣ-matrix with 99.67 volume fraction and TiC particles TEM analysis has shown that the ɣ' precipitates are found
with 0.33 volume fraction is expected at that temperature. in the microstructure with about 80.9 area percent.
TEM images have shown that total solutionizing of ɣ'

Tab.4 - Isothermal aging modeling outputs (a-c) and TEM image of the specimen that aging is applied physically.

(a) Change of ɣ' volume fraction throughout the (b) Change of ɣ' particle size throughout the aging
aging of Waspaloy. of Waspaloy.

(d) TEM image of ɣ' particles after isothermal

(c) Distribution of ɣ' particles with varying sizes.
aging at 850°C for 18-hours.

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Scientific papers - Heat Treatments

Although the fraction of ɣ' precipitates did not reflect With respect to the equations described before,
the real heat treatment process as understood from the yield strength estimation at different temperatures is
TEM images, the size of the ɣ' particles was predicted completed by using the outcomes obtained in modeling
almost the same as the aging process continues. Both studies conducted with PANDATTM. In order to complete
the simulation and TEM analysis gave similar results for ɣ' the yield strength predictions at elevated temperatures
precipitate radius of 24.8 nm and 25.2 nm, respectively as more accurately, some terms such as lattice strength of
shown in Table 4. However, although the simulation setup pure Nickel, Poisson’s ratio, shear modulus, Burger’s
is prepared for homogeneous nucleation and growth, vector, lattice parameters of ɣ-matrix and ɣ' particles,
from the TEM images the nucleation characteristic is seen interparticle spacing and 𝑘𝑦 parameters were calculated
as semi-homogeneous in the microstructure. Lastly, by using JMatPro software from room temperature to
although the model expected a wider LSW distribution for elevated temperatures and used in the yield strength
the radius of the particles with varying sizes, TEM analysis modeling as a function of temperature. The model
has shown a narrower size distribution mainly focusing on parameters used for the determination of the effect of
18 to 30 nm ɣ' particles. strengthening mechanisms and overall yield strength are
given in Table 5, below.

Tab.5 - Model parameters for strengthening mechanisms.

Used Parameters Numeric Value

Lattice strength of pure Ni: 𝜎 0 69 MPa @ RT

Poisson’s Ratio: v 0.26 @ RT

Shear Modulus: G 80 GPa @ RT

Burger’s vector 2.04 Å at RT (a/2<110>)

Interparticle spacing: 𝜆 36.31 nm @ RT [7]

Lattice Parameter of ɣ 3.59 @ RT

Lattice Parameter of ɣ ' 3.57 @ RT

ɣ' radius 25 nm

ɣ' volume fraction 22 volume %

𝑘𝑦 (T) 250.36 - 0.0738T

Grain size: D 35 µ m

As the critical radius is stated as 10*b by Kelly et al. (45), and incoherent (46). Therefore, coherency strengthening
the critical radius for this procedure is obtained as is also calculated and found as much effective as
2.5 nm whereas the ɣ' particles after 18 hours aging at precipitation hardening mechanism to the yield strength
850°C are expected to have a 25 nm mean radius. Thus, of Waspaloy with the applied heat treatment.
dislocations moving along the matrix favor Orowan Solid solution strengthening calculations are completed
looping since the particle radius is greater than the critical by using the solidification model results under equilibrium
radius. cooling with the elements Cr, Co, Mo, Fe, and Al to the
Additionally, although the ɣ' particles are expected to Nickel matrix and by using the solid solution hardening
show coherent and homogeneous nucleation on the coefficients found in the literature (26).
ɣ- matrix, the growth of these precipitates changes the The least effective mechanism among the others is found
interface characteristic from coherent to semi-coherent to be grain-size hardening. In the literature, it is observed

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 Memorie scientifiche - Trattamenti Termici

that the grain size of Waspaloy changes from 30 to 90μm and precipitates as in coherency strengthening. The
(47-49). Variation of the grain size affects the hardening due contributions of all strengthening mechanisms calculated
to the increasing/decreasing length of grain boundaries by using the outputs of modeling studies are given in
interacting with dislocations. However, the grain size Figure 3.
range of Waspaloy indicated above is calculated to cause For the experiments applied with 0.001 strain rate, it has
a very little difference in strength as between 24 to 42 MPa been seen that the room temperature properties of the
where the as-received ingot with an average grain size of material are superior to the ones at elevated temperatures
35 μm is expected to have 38.6 MPa strength from grain in terms of both in yield and ultimate tensile strength.
size hardening. After that, the property of this alloy shows better
Lastly, the lattice strength of nickel is calculated as a deformation kinetics and strength at 650°C than 580°C
function of temperature. Due to the Shockley partials in and 720°C. This also explains the design criteria of this
the material, the lattice strength of nickel decreases as the alloy where it operates in the turbines generally around
temperature increases. 650°C. The modeling and experimental results have
By considering the fraction of these precipitates in the shown a good agreement varying from 7 to 55 MPa
microstructure, it can be said that the matrix strength from room temperature to operating temperatures.
arises from the solid solution strengthening, grain size These differences are expected to occur due to the
hardening, and matrix lattice strength whereas the carbides and borides formed during solidification and the
second phase provides strength due to the formation heterogeneities in the microstructure where in the model
of dislocation looping. Lastly, the alloy strength also the microstructure is assumed to be homogeneous.
increases from the interaction between the matrix

Fig. 3 - Yield strength results from modeling studies and experiments.

CONCLUSION yield strength of Waspaloy from room temperature to

The effect of heat treatment on yield strength for operational conditions also shows that the matrix strength
polycrystalline Waspaloy was investigated and the is mainly composed of solid solution hardening, grain
corresponding modeling studies have shown that boundary strengthening, and lattice strength of nickel.
heat treatment applications with the parameters set by Linear summation of the contributions of each of these
considering the related thermodynamic modeling results strengthening mechanisms gave a correlation with less
constitute around 60 % of the overall yield strength. The than 8% variation with the experimental data where the

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Scientific papers - Heat Treatments

microstructural modeling results have also shown a good ACKNOWLEDGEMENT

agreement with experimental analysis results. The given We thank CompuTherm-PANDATTM for providing the
model can be used for the determination of compositional related licences for this study. We also thank Lukasiewicz
and microstructural changes ’effect on yield strength. Research Network – Institute for Ferrous Metallurgy
However, more polycrystalline alloys with ɣ' precipitates for supporting the thermomechanical tests conducted
should be investigated to create a generic approach that with Gleeble system and Fatih Kalıp Makine San. for the
can be applied to a larger group of Ni-based superalloys. specimen preparation for Gleeble tests.

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