See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/294139105

Welding of IN792 DS superalloy by electron beam

Article  in  Surface and Interface Analysis · February 2016

DOI: 10.1002/sia.5946

CITATIONS READS

6 1,523

6 authors, including:

R. Montanari A. Varone
University of Rome Tor Vergata University of Rome Tor Vergata
255 PUBLICATIONS   2,059 CITATIONS    90 PUBLICATIONS   620 CITATIONS   

SEE PROFILE SEE PROFILE

Giuseppe Barbieri Peiman Soltani

ENEA Shahrekord University
53 PUBLICATIONS   213 CITATIONS    26 PUBLICATIONS   239 CITATIONS   

SEE PROFILE SEE PROFILE

Some of the authors of this publication are also working on these related projects:

Microchemical investigations of PbBi alloys; Graphene-based materials; Nanoparticles (AU, Ag, ...) View project

Graphene Quantum Dots for Environment and Energy View project

All content following this page was uploaded by Alessio Mezzi on 16 October 2017.

The user has requested enhancement of the downloaded file.

ECASIA special issue paper
Received: 1 August 2015 Revised: 11 December 2015 Accepted: 8 January 2016 Published online in Wiley Online Library: 10 February 2016

(wileyonlinelibrary.com) DOI 10.1002/sia.5946

Welding of IN792 DS superalloy by

electron beam
R. Montanari,a* A. Varone,a G. Barbieri,b P. Soltani,a,c A. Mezzic
and S. Kaciulisc
Ni-based superalloys are widely used in the components of aeronautic engines and gas turbines operating at the highest temper-
atures. During the service life, surface cracks may form in these mechanical parts; therefore, their repairing by welding is of great
technological relevance.
Seams have been realized by means of electron beam welding (EBW) on plates of IN792 DS superalloy with material pre-
heating. They are free of macro-defects like cracks and pores; however, microstructural changes are observed in molten (MZ)
and heat affected (HAZ) zones. The amount of γ’ phase in MZ is smaller than that in the base metal, and the particles are very fine
with an average size of 20 nm that leads to an increase of hardness. In HAZ particle, coarsening takes place as a consequence of
heating; therefore, hardness slightly decreases with respect the base metal.
X-ray Photoelectron Spectroscopy analyses carried out inside and outside the MZ, and the results show that the distribution of
chemical elements remains homogeneous in the sample. Auger electron spectroscopy line scans with higher lateral resolution ev-
idenced that the center of MZ is depleted of Mo and rich of Cr. Copyright © 2016 John Wiley & Sons, Ltd.

Keywords: IN792 DS superalloy; welding; electron beam; microstructure; XPS; AES

Introduction observations of light optical microscopy (LOM) and scanning elec-

Ni-based superalloys are widely used in the components (disks and
blades) of aeronautic engines and gas turbines operating at the
highest temperatures.[1,2] Their microstructure mainly consists of
cuboidal shaped particles of the ordered γ’-phase embedded in
the disordered γ-phase matrix.[3] During the service life, the me-
chanical parts made of superalloys operate under high stress and
temperature in a quite aggressive environment, therefore, some-
times surface cracks form leading to sudden rupture. Because these
mechanical components are extremely expensive, their repairing
by welding is more advantageous than replacement; however, it
is not an easy task. In fact, the welds must satisfy strict require-
ments: (i) modifying as little as possible the original microstructure;
(ii) do not introduce in the molten (MZ) and heat affected (HAZ)
zones any relevant residual stress; (iii) do not produce cracks in
the MZ and HAZ; (iv) do not cause a massive surface segregation;
and (v) to minimize the elemental diffusion, which can change con-
sequently the chemical composition of γ and γ’ phases.
The present work is part of a general project aimed to determine
the optimal conditions for joining the directionally solidified IN792
DS superalloy by means of high-energy-density welding
techniques;[4–7] here, the electron beam welding (EBW) has been
chosen to produce the seams of molten and solidified metal on
2-mm thick plates of the superalloy. With respect to the conven-
tional welding techniques employing an electric arc, the EBW
enables narrower seams with lower heat input and reduced exten-
sion of the HAZ. A further advantage is the low gas absorption from
liquid metal, because all welding operations are carried out in high
vacuum.
After the EBW, the microstructural features in the MZ, HAZ, and
tron microscopy (SEM), X-ray diffraction (XRD), X-ray Photoelectron
Spectroscopy (XPS), and Auger electron spectroscopy (AES), which
have already demonstrated their effectiveness in studies of
composition profiles connected to diffusion phenomena in
superalloys.[8–10]
Experimental
The chemical composition of examined IN792 DS superalloy is re-
ported in Table 1. The material has been supplied in form of cylin-
drical ingots (diameter 25 mm, length 60 mm) with the [100]
direction of the oriented grains parallel to the ingot axis. The plates
of 2-mm thickness were obtained by spark-erosion cutting the in-
gots along their axis (Fig. 1a).
Some preliminary tests of the EBW at room temperature showed
extended inter-dendritic cracks in the MZ; therefore, all the succes-
sive tests have been performed by using the pre-heating by
defocused and swinging electron beam.
A grid of the samples has been prepared by varying the
pass speed from 1 to 2.5 m/min with pre-heating
* Correspondence to: R. Montanari, Department of Industrial Engineering,
University of Rome “Tor Vergata”, 00133 Rome, Italy.
E-mail: roberto.montanari@uniroma2.it
a Department of Industrial Engineering, University of Rome “Tor Vergata”, 00133,
Rome, Italy
b ENEA, Research Centre of Casaccia, 00196, Rome, Italy
483

base alloy have been investigated by micro-hardness tests, c ISMN – CNR, P.O. Box 10, 00015 Monterotondo Stazione, Rome, Italy

Surf. Interface Anal. 2016, 48, 483–487 Copyright © 2016 John Wiley & Sons, Ltd.
 R. Montanari et al.

Table 1. Chemical composition (wt%) of the IN792 DS superalloy

C Cr Co Ta W Ti Al B Zr Ni

Min 0.07 12.20 8.50 3.85 3.85 3.75 3.15 0.01 — to balance
Max 0.09 12.80 9.50 4.25 4.25 4.15 3.55 0.02 0.01
Si Mn P S Fe Cu Mo Nb Hf
Min — — — — — — 1.70 — 0.80
Max 0.10 0.10 0.015 0.005 0.50 0.05 2.10 0.01 1.20

Figure 1. Sample plates of 2 mm thickness were produced by spark erosion cutting the ingots along their axis corresponding to the [100] direction (a). Cross
section of the welded seam (b).

temperature of 300 °C, while the other EBW parameters were
kept constant: power of 1 kW, acceleration voltage of 50 kV,
and beam current of 20 mA. Preliminarily, the seams have
been checked by X-ray radiography to identify the possible
macro-defects, such as porosities and cracks. Then, the MZ,
HAZ, and base alloy have been examined by LOM and SEM
to investigate the morphology, size, and distribution of γ
and γ’ phases.
XRD measurements were carried out by focussing the beam on
the base alloy, HAZ, and MZ in order to determine the correspond-
ing fraction of γ’ phase and the average size of ordered particles.
The {110} superlattice and {220} fundamental reflections have been
collected by using Mo-Kα radiation (λ = 0.7093 Å) with 2θ angular in-
tervals of 0.005° and counting times of 30 s/step. The degree of or-
dering ζ was calculated from the following relationship:
 
F 2220 L220 I110
ζ ¼
F 2110 L110 I220
where F is the structure factor, I the integrated peak intensity, and L
the Lorentz-polarization factor depending on the Bragg angle θ
and given by
1 þ cos2 2θ
L¼
484
The average size D of ordered particles was determined by
Eq (3):
λ
D¼ (3)
cosθβð2θÞ
where λ is the X-ray wavelength and β(2θ) is the half-height line
width of the {110} superlattice peak.
Vickers micro-hardness tests have been performed across the
seams at equi-spaced distance to determine the hardness in the
base alloy, HAZ, and MZ.
Finally, the micro-chemical distribution of alloying elements in
the different zones has been determined through imaging XPS,
and substantially aimed to verify if the composition of γ and γ’
phases in HAZ and MZ has changed after the welding. XPS experi-
ments have been performed by using a monochromatized spec-
trometer Escalab 250Xi (Thermo Fisher Scientific, UK) equipped
(1) with a 6-channeltron detection system for spectroscopy and multi-
channel plate for chemical imaging. Photoelectrons were excited
by using a standard Al Kα source with a spot size of 900 μm. Photo-
emission spectra were registered at constant pass energy of 50 eV
and electrostatic lens mode with 150-μm diameter of analyzed
area, whereas the chemical images were acquired in electrostatic
lens mode at 150 eV pass energy. Because of the ferromagnetic
properties of the investigated alloy, it was not possible to use the
(2)

sin2 θ cos θ electromagnetic lens mode with much higher lateral resolution.

wileyonlinelibrary.com/journal/sia Copyright © 2016 John Wiley & Sons, Ltd. Surf. Interface Anal. 2016, 48, 483–487
Welding of IN792 DS superalloy by electron beam

The binding energy (BE) scale was calibrated by using C 1s peak of

aliphatic carbon at BE = 285.0 eV. Multipoint analysis by Auger elec-
tron spectroscopy (AES) was carried out using a LEG200 electron
gun mounted on the analysis chamber of an Escalab MkII (VG Scien-
tific, UK) and operated at 10-keV beam energy. Before the measure-
ments, the surface was cleaned by using an Ar+ ion gun at 2.0-keV
energy in order to remove the first few monolayers of contami-
nants. Obtained XPS and AES experimental data were processed
by the Avantage v.5 software (Thermo Fisher Scientific, UK). Shirley
background subtraction and a standard set of Scofield sensitivity
factors were used for XPS quantification. The relative intensities of
principal Auger lines (Mo MNN, Cr LMM, Ti LMM, and Ni LMM) at dif-
ferent analysis points were determined by using the ratio of corre-
sponding peak areas calculated by using a linear background.

Results and discussion

X-ray radiography showed that the EBW seams obtained with ma-
terial pre-heating are of good quality, because no macro-defects
like cracks and pores have been observed. The seam cross section
is shown in Fig. 1b: it exhibits the typical nail-like shape of the
welding. Its width is about 3 mm on the side directly irradiated by
electron beam.
In Fig. 2, the morphological structures (SEM images) of the base
metal (a), HAZ (b) and MZ (c) are compared. In the original alloy,
the volume fraction of the ordered γ’ phase is about 70% (Fig. 2a)
with a mean size of the particles of ~400 nm and the separation
of the channels of ~50 nm. The γ’ phase is almost homogeneously
distributed, but some particle-free (PF) zones in the matrix with a
size of 1–2 μm are also observed.
The amount of γ’ phase in the MZ determined by XRD is ≈ 24%,
i.e. it is smaller than that of the base alloy, whereas this amount
does not change in the HAZ. As it can be expected, the γ’ phase par-
ticles have a larger size in the HAZ (b), than in the original alloy (a)
because of the strong heat flux around the seam that leads to the
coarsening of the ordered phase.
In the MZ, the γ’ particles nucleate after solidification and have a
very short growth time during the cooling to room temperature;
thus, their size is quite small and exhibit a round shape. In Fig. 2c,
only a few particles of about 60 nm can be observed, whereas the
larger part of them is quite finer: an average size of 20 nm has been Figure 2. Morphology of the original material (a), HAZ (b) and MZ (c).
calculated from the broadening of {110} superlattice XRD peak.
The micro-hardness profiles, measured across the seams, re- errors. Their mean values are reported in the Table 2. The chemical
sulted in the higher values for the MZ: the mean value of micro- state of constituent elements was determined by using a peak-
hardness was of 430 HV in base alloy, 415 HV in the HAZ, and fitting routine and chemical shift values from the XPS Handbook.[11]
470 HV in the MZ. This trend depends on the specific microstruc- Even if the most species of metals correspond to their oxides,
tures in the three zones, in particular on the size of γ’ phase parti- the most intense component of O 1-s line has the value of
cles: the smaller the ordered particles, the higher the micro- BE = 531.6 eV, which can be attributed to some oxides[11] (such
hardness. It should be noted that the highest value is observed in as Al2O3 and Ni2O3) as well as to hydroxyl groups,[11,12] whereas
the MZ, in spite of the lower content of ordered phase; therefore, the third component belongs to adsorbed water.[12] As regards
the small particle size seems to play the fundamental role in deter- the constituent elements of alloy, they are mostly in the main
mining the mechanical properties. oxidation state as oxides (Cr, Ni, Ta, and W) or hydroxides (Co and
In order to evaluate whether the distribution of chemical ele- Al). Only the Mo is present completely in its metallic state, whereas
ments remains homogeneous in the welded sample, XPS analyses the Ni and Ta are partially oxidized.
have been carried out in the MZ and out of it. Since the sample sur- Comparison of the spectral regions for the constituent elements
face was contaminated with Ca, Zn and C, it was cleaned by Ar+ that were slightly different in the MZ are shown in Fig. 3. Also the
sputtering for 3 min (2 keV energy, 3 μA sample current) before peak fitting for Ta 4f spectrum out of the MZ is presented in the in-
the XPS line scan across the welding. The results of this scan with sert of this figure. Here are clearly visible two chemical states of Ta:
15 analysis points through both regions of the sample demon- metal and oxide. The main difference between the MZ and the rest
strated that atomic concentrations of the main constituent ele- of alloy is the same as in atomic ratios given in Table 2: the signal of
485

ments in the MZ and out of it is constant within the experimental Co 2p is higher in the MZ than the one in original alloy. The spectra

Surf. Interface Anal. 2016, 48, 483–487 Copyright © 2016 John Wiley & Sons, Ltd. wileyonlinelibrary.com/journal/sia
 R. Montanari et al.

Table 2. XPS quantification (without contaminants) in the molten zone (MZ) and out of it (in original alloy)
In the MZ
Peak BE, eV FWHM, eV Atomic % Weight % Chemical State

Al2p 73.9 0.4 1.4 1.5 Al2O3 and hydroxides

C1s 285.0 1.7 19.3 8.9 aliphatic
Co2p3/2 780.7 6.6 3.4 7.7 oxides and Co(OH)2
Cr2p3/2 576.8 2.8 4 8.1 Cr2O3
Mo3d5/2 227.9 2.4 0.4 1.4 Mo(0)
Ni2p3/2 A 852.5 1.5 4.6 10.3 Ni(0)
Ni2p3/2 B 855.8 3.5 6.6 15 Ni2O3
O1s A 529.8 1.8 13 8 metal oxides
-
O1s B 531.5 1.8 33.6 20.7 oxides and OH
O1s C 533.1 1.8 11.3 7.0 adsorbed H2O
Ta4f7/2 A 22.5 2.7 0.6 4.3 Ta(0)
Ta4f7/2 B 25.3 1.7 0.7 4.7 Ta2O5
Ti2p3/2 458.1 1.4 1.1 2.0 TiO2
W4f7/2 33 0.3 0.1 0.4 WO2
Out of the MZ
Peak BE, eV FWHM, eV Atomic % Weight % Chemical State
Al2p 74.0 1.3 1.8 2.0 Al2O3 and hydroxides
C1s 285.0 2.0 20.1 9.8 aliphatic
Co2p3/2 777.9 0.4 1.5 3.6 oxides and Co(OH)2
Cr2p3/2 577.1 3.1 4.6 9.6 Cr2O3
Mo3d5/2 227.9 2.3 0.5 1.8 Mo(0)
Ni2p3/2 A 852.7 1.4 3.8 9 Ni(0)
Ni2p3/2 B 855.8 3.5 5.6 13.3 Ni2O3
O1s A 530 1.8 14.5 9.5 metal oxides
-
O1s B 531.6 1.8 35.8 23.3 oxides and OH
O1s C 533.2 1.8 9.4 6.1 adsorbed H2O
Ta4f7/2 A 22.4 2.3 0.5 3.6 Ta(0)
Ta4f7/2 B 25.4 1.7 0.8 5.7 Ta2O5
Ti2p3/2 458.3 1.7 1.2 2.4 TiO2
W4f7/2 31.1 0.7 0.1 0.5 W(0)

Figure 3. Comparison of Ta4f, W4f, Ti2p and Co2p spectra in two zones: in MZ and out of MZ (original alloy). In the inset it is shown the peak fitting for Ta 4f
spectrum out of the MZ.

of all other elements were practically identical in the MZ and out of
it. The high noise observed in all photoemission spectra was caused
by the low sensitivity of the instrument in the electrostatic lens
mode combined with the small analysis area. The uniformity of sur-
486
images of constituent metals, where no visible changes between
the MZ, HAZ, and base alloy were revealed.
The elemental line scans with much higher lateral resolution
(about 0.5 μm) have been performed by AES across the seam in dif-

face chemical composition was also confirmed by the XPS chemical ferent positions on the surface. Typical trends of Ni, Cr, Ti, and Mo

wileyonlinelibrary.com/journal/sia Copyright © 2016 John Wiley & Sons, Ltd. Surf. Interface Anal. 2016, 48, 483–487
Welding of IN792 DS superalloy by electron beam
Figure 4. Auger line scan of elemental content (wt%) determined from the
Mo MNN, Cr LMM, Ti LMM, and Ni LMM peak areas, respectively.
concentrations in wt%, obtained from the ratios of respective Auger
peak areas are reported in Fig. 4, where the start position of the
scan corresponds to the center of the seam. The values of content
in wt% (y-axis) were calculated by using as a reference the nominal
composition of alloy, which corresponds to the rightmost analysis
point in this graph.
The amounts of Ni and Ti are almost constant through the scans,
while the significant changes of Cr and Mo concentrations are
observed in the MZ and HAZ. The amount of Mo equals to zero in
the center of the MZ and increases moving toward the HAZ, where
it reaches a nearly stable value. The trend of Cr is opposite, i.e. it is
decreasing from the center of MZ. Such behavior can be ascribed in
part to elemental diffusion in the liquid state and in part to evapo-
ration during EBW passes.
Conclusions
The EBW seams were realized on the plates of IN 792 DS superalloy
by using material pre-heating. They did not exhibit any macro-
defects like cracks and pores,;however, some microstructural
changes were observed in the MZ and HAZ. These variations can
be summarized in a following way:
Surf. Interface Anal. 2016, 48, 483–487 Copyright © 2016 John Wiley & Sons, Ltd.
View publication stats
(i) the amount of γ’ phase in the MZ is smaller than in the base
alloy, also the particles are very fine with an average size of
20 nm that leads to increase of hardness.
(ii) in the HAZ, the fraction of ordered phase does not change,
but particle coarsening takes place as a consequence of
heating; therefore, the hardness slightly decreases with
respect to the base alloy.
XPS analyses, carried out in the MZ and out of it, indicated
the homogeneous distribution of constituent metals on the
sample surface. AES line scans with higher lateral resolution
revealed the constant concentrations of Ni and Ti, while the
significant variations of Cr and Mo content were observed in
the MZ and HAZ, in particular in the center of MZ that was
rich of Cr and completely depleted of Mo.
The results demonstrate that the parameters used to realize
seams guarantee a good quality of welding and are useful to orien-
tate the calibration of post-welding treatments.
References
[1] H. Monjati, M. Jahazi, R. Bahrami, S. Yue, Mater. Sci. Eng. A 2004,
373, 286.
[2] A. M. Ges, O. Fornaro, H. A. Palacio, Mater. Sci. Eng. A 2007, 458, 96.
[3] P. Deodati, R. Montanari, O. Tassa, N. Ucciardello, Mater. Sci. Eng. A
2009, 521-522, 102.
[4] M. T. Rush, P. A. Colegrove, Z. Zhang, B. Courtot, Adv. Mater. Res. 2010,
89-91, 467.
[5] X.-B. Liu, G. Yu, J. Guob, Y.-J. Gu, M. Pang, C.-Y. Zheng, H.-H. Wang,
J. Alloy Comp. 2008, 453, 371.
[6] H.-S. Wang, C.-Y. Huang, K.-S. Ho, S.-J. Deng, Mater. Trans. 2011,
52, 2197.
[7] D. J. Tillack, Weld J. 2007, 86, 28.
[8] S. Kaciulis, A. Mezzi, M. Amati, R. Montanari, G. Angella, M. Maldini, Surf.
Interface Anal. 2012, 44, 982.
[9] M. Amati, L. Gregoratti, S. Kaciulis, A. Mezzi, S.K. Balijepalli, R. Donnini,
R. Montanari, G. Angella, G. Maldini, D. Ripamonti, Metallurgia Italiana
2013, 105/11-12, 21.
[10] A. Mezzi, S. Kaciulis, M. Amati, R. Montanari, G. Angella, R. Donnini,
D. Ripamonti, M. Maldini, L. Zhou, Proc. 35th AIM National
Conference, Rome, November 2014.
[11] J. F. Moulder, W. F. Stickle, P. E. Sobol, K. D. Bomben, Handbook of X-ray
Photoelectron Spectroscopy, Phys. Electronics, Eden Prairie, USA, 1995.
[12] S. Kaciulis, G. Mattogno, A. Galdikas, A. Mironas, A. Setkus, J. Vac. Sci.
Technol. A 1996, 14, 3164.
487
wileyonlinelibrary.com/journal/sia