metals
Article
Influence of Electron Beam Welding Parameters on the
Microstructure Formation and Mechanical Behaviors
of the Ti and Ni Dissimilar Metals Welded Joints
Beáta Šimeková 1, * , Erika Hodúlová 1 , Pavel Kovačócy 1 , Ingrid Kovaříková 1 , Miroslav Sahul 2 , Martin Sahul 3 ,
Matej Pašák 3 and Florian Pixner 4
Citation: Šimeková, B.; Hodúlová, E.;
Kovačócy, P.; Kovaříková, I.; Sahul,
M.; Sahul, M.; Pašák, M.; Pixner, F.
Influence of Electron Beam Welding
Parameters on the Microstructure
Formation and Mechanical Behaviors
of the Ti and Ni Dissimilar Metals
Welded Joints. Metals 2022, 12, 894.
https://doi.org/10.3390/
met12060894
Academic Editors: Marcello Cabibbo
and Paolo Ferro
Received: 22 March 2022
Accepted: 19 May 2022
Published: 24 May 2022
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Copyright: © 2022 by the authors.
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Attribution (CC BY) license (https://
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4.0/).
Metals 2022, 12, 894. https://doi.org/10.3390/met12060894
1 Department of Welding and Joining of Materials, Institute of Production Technologies, Faculty of Materials
Science and Technology in Trnava, Slovak University of Technology in Bratislava, J. Bottu 25,
917 24 Trnava, Slovakia; erika.hodulova@stuba.sk (E.H.); pavol.kovacocy@stuba.sk (P.K.);
ingrid.kovarikova@stuba.sk (I.K.)
2 Department of Manufacturing Technology, Faculty of Mechanical Engineering, Czech Technical University in
Prague, Technická 4, 166 07 Prague, Czech Republic; miroslav.sahul@fs.cvut.cz
3 Institute of Materials Science, Faculty of Materials Science and Technology in Trnava, Slovak University of
Technology in Bratislava, J. Bottu 25, 917 24 Trnava, Slovakia; martin.sahul@stuba.sk (M.S.);
matej.pasak@stuba.sk (M.P.)
4 Institute of Materials Science, Joining and Forming, Graz University of Technology, Kopernikusgasse 24/I,
8010 Graz, Austria; florian.pixner@tugraz.at
* Correspondence: beata.simekova@stuba.sk; Tel.: +421-908-119-601
Abstract: Commercially pure titanium Ti Grade 2, 2 mm in thickness, was welded to 2 mm thick
nickel alloy 201 with electron beam welding. Various welding parameters were used to create the
butt-welded joints. The innovation herein consists of welding two dissimilar metals that are declared
non-weldable. The welding current used for electron beam welding was 40–70 mA and welding
speeds were 20–50 mm/s. In this experiment, we tested two offsets of the electron beam, which were
100–300 µm to the nickel side and 200 µm to the titanium side. It was observed that the offset of the
beam had no effect on the weld joint’s strength. The samples were subjected to a visual test in which
longitudinal and transverse cracks were recorded along the whole weld. Only four samples retained
the integrity of the joint. Microstructures of the weld joints were examined by scanning confocal and
scanning electron microscopy. Energy dispersive spectroscopy (EDS) analysis confirmed the phase
constitution inside the weld regions and the fusion interfaces. Tensile strength and microhardness
tests were used to evaluate the mechanical parameters of the Ti/Ni welded joint. The results showed
that cracking of brittle Ni–Ti intermetallic phases in electron beam welded joints occurred. The
microstructure in the fusion zone’s center part was primarily NiTi and Ti2 Ni. No clear correlation
was found between heat input or welding parameters—welding current and welding speed—and
tensile strength. The strain–tensile strength curve resulted in brittle fracturing. The hardness of the
weld zone was five times higher than that of the base metal and heat-affected zone. The amount of
heat input into the welded metal is as critical as the large asymmetry in heat transport that controls
the process of solidification from each side of the base metal.
Keywords: electron beam welding; dissimilar materials; microstructure; mechanical properties
1. Introduction
Titanium alloys are popular construction materials in the aerospace industry due to
their high specific strength [1,2]. Above 600 ◦ C, the favorable mechanical properties of these
materials diminish significantly [3]. On the contrary, Ni-based alloys can maintain their
mechanical properties at higher temperatures, even above 1000 ◦ C [4–6]. The dissimilar Ti
and Ni weld joints in manufactured and assembled components [7,8] reduce material costs
compared to the application of a single material, provide design flexibility, and frequently
https://www.mdpi.com/journal/metals
Metals 2022, 12, x FOR PEER REVIEW 2 of 20

Metals 2022, 12, 894 2 of 18

ilar Ti and Ni weld joints in manufactured and assembled components [7,8] reduce mate-
rial costs compared to the application of a single material, provide design flexibility, and
frequently lead to improved performance [7]. It is important to gain knowledge about
lead to improved performance [7]. It is important to gain knowledge about joining Ti and
joining
Ni alloysTiandandcreating
Ni alloys and creating
a quality welded a quality welded
joint. When thejoint. When the
difficulties difficulties
arising from the arising
high
from the high affinity of titanium to oxygen have been overcome,
affinity of titanium to oxygen have been overcome, then a major metallurgical problem then a major metallur-
gical problem
arises arises from
from the formation ofthe
the formation
intermetallic of phases
the intermetallic
in the Ti–Ni phases
systemin[9].theThe
Ti–Ni system
principals
[9]. The principals for understanding the welding process
for understanding the welding process of Ti and Ni are in the binary diagram shown of Ti and Ni are in the binary
in
Figure 1. The NiTi phase is represented as hatching, and it only covers a very smallcovers
diagram shown in Figure 1. The NiTi phase is represented as hatching, and it only area;
a very630
under small
◦ C, area; under
it is just a line630at°C, it is%just
50 at. Ni, a50line
at. %at Ti.
50 Inat.accordance
% Ni, 50 at.with % Ti.
theInTi–Ni
accordance
binary
with the Ti–Ni binary phase diagram, outside of this narrow
phase diagram, outside of this narrow central zone, many kinds of Ti–Ni intermetallic central zone, many kinds of
Ti–Ni intermetallic
compounds (IMC) will compounds
form in the (IMC)
weldwill[10].form
If theinredundancy
the weld [10]. of If
Ti the
andredundancy
Ni in the matrixof Ti
and Ni in the matrix are in the brittle phases, Ti Ni and TiNi arise.
are in the brittle phases, Ti2 Ni and TiNi3 arise. The phases Ti2 Ni and TiNi3 are stable
2 3 The phases Ti2 Ni and
TiNi are stable intermetallic phases that have unacceptable
intermetallic phases that have unacceptable properties besides the base metal (BM). The
3 properties besides the base
metal (BM).
welded joint The
willwelded
becomejoint will become
unacceptable unacceptable
if the volume ofifthese the volume of these
precipitates precipitates
grows. These
grows. Thesephases
intermetallic intermetallic phases are
are subsidized by subsidized
the heat input by the
andheat
the input and the contamination
contamination with oxygen,
with oxygen,
nitrogen, nitrogen,
and iron andChatterjee
[11–15]. iron. [11–15].et al.Chatterjee
[16] found etbrittle
al. [16]NiTi
found brittle
2 and NiTi
Ni3 Ti 2 and Ni3Ti
intermetallic
intermetallic compounds in laser welding butt
compounds in laser welding butt joints of dissimilar Ti–Ni metals. joints of dissimilar Ti–Ni metals.

Figure1.1.Binary
Figure Binarydiagram
diagramof
ofNi–Ti
Ni–Tidata
datafrom
from[2].
[2].

Solid-statewelding
Solid-state weldingmethodsmethodsare areused
usedforfordissimilar
dissimilarmetal
metaljoining
joiningduedueto tothe
thefact
factthat
that
thebase
the basemetals
metalscan canbebe kept
kept solid
solid during
during these
these procedures.
procedures. Solid-state
Solid-state welding
welding of nickel
of nickel and
and titanium
titanium is very
is very difficult
difficult to perform
to perform successfully,
successfully, due due
to theto limited
the limited solubility
solubility of nickel
of nickel in
in alpha
alpha titanium
titanium at room
at room temperature
temperature [17].[17]. Although
Although solid-state
solid-state welding
welding approaches
approaches ap-
appear
pear
to to be promising
be promising for addressing
for addressing brittleness
brittleness caused caused
by thebycreation
the creation
of an ofIMCan layer,
IMC layer,
they
they significant
have have significant limitations
limitations and areandnotareadvised
not advised
for somefor some situations.
situations. Consequently,
Consequently, it is
it is necessary
necessary to study
to study the fusion
the fusion processprocess for welding
for welding dissimilar
dissimilar metals metals
for the for
nextthe next re-
research.
search.
The fusion welding method of dissimilar metals brings a set of difficulties which
do noThe appear
fusionin welding
the welding methodof similar metals.metals
of dissimilar One significant
brings a setdistinction in dissimilar
of difficulties which do
metal welding
no appear (DMW)
in the welding is that the various
of similar metals.thermo-physical properties of
One significant distinction in the base metals
dissimilar metal
(melting point, thermal conductivity, specific heat, density) influence
welding (DMW) is that the various thermo-physical properties of the base metals (melting the macrostructure
and microstructure
point, formation.specific
thermal conductivity, The binary
heat,diagram
density)of a Ti/Ni couple
influence provides a model
the macrostructure for
and mi-
all systems, forformation.
crostructure example, TiThe to stainless steel (SS)of
binary diagram [18–20],
a Ti/Ni Ti3Al alloyprovides
couple to Ni alloy [21], Ti6Al4V
a model for all
to SS [22–24],
systems, NiTi to Ti6Al4V
for example, [25], Ti6Al4V
Ti to stainless to Inconel
steel (SS) [18–20],718 [7], NiTi
Ti3Al alloytotoSSNi[26–30], andTi6Al4V
alloy [21], NiTi to
Ni alloy
to SS [21], for
[22–24], theto
NiTi investigation
Ti6Al4V [25], of Ti6Al4V
the fundamentals
to Inconelof718 microstructure
[7], NiTi to SS formation.
[26–30], and NiTi
Some of the first attempts to joint Ti/Ni by electron
to Ni alloy [21], for the investigation of the fundamentals of microstructure beam welding (EBW) reported
formation.
the creation of intermetallic phases which caused brittleness in
Some of the first attempts to joint Ti/Ni by electron beam welding (EBW) reported these welding joints [30].
“The most common fusion welding technology for joining different
the creation of intermetallic phases which caused brittleness in these welding joints [30]. metals is electron beam
welding
“The most because
common of itsfusion
benefits, which technology
welding include a high for density
joining of energy, metals
different vacuum, is heating
electron
position,
beam weldingand area control”
because of [31]. Among which
its benefits, other things,
include a very
a highnarrow
densityHAZ of is produced.
energy, The
vacuum,
electron beam welding method was successfully used for the joining of Ti3Al–TC4 titanium
alloys [32]. In the creation of welded joints with IMC formed, for electron beam welding
and laser beam welding, filler metals are frequently required. Gao et al. [33] performed
the laser beam welding of the Ti6Al4 titanium alloy and 304L stainless steel using an Mg
Metals 2022, 12, 894 3 of 18

interlayer. As a result, the welded joint in terms of 221 MPa tensile strength was achieved.
An intermetallic phase of Mg17Al12 was observed in the Ti–weld interface, but there was
no intermetallic phase in the SS–weld interface. Wang et al. [34,35] reported electron beam
welds without cracks and with 310 MPa tensile strength. The welded joint was mainly
formed by a Cu solid solution. The thin Cu–Ti IMC was formed in the titanium–weld
interface. Tomashchuk et al. [22] came to the conclusion that the interlayer of a pure copper
used in the Ti/Fe welds produced by electron beam welding reduced but did not eliminate
the formation of brittle phases of Ti–Fe and Ti–Cr. The local cumulating of Cu–Ti and
Cu–Fe–Ti phases decreased the strength of the welds, and it was allowed to join.
Compared to other joining processes, fusion welding is always a preferable choice due
to its potential ability to produce joints with good metallurgical bonding and mechanical
integrity. However, in terms of dissimilar Ti and Ni metals, technical challenges remain,
such as process-induced brittle intermetallic compounds (IMCs) and thermal stress [36,37],
resulting from not only their different thermo-physical-mechanical properties, but most
importantly, also their limited metallurgical miscibility in room temperature [7,30,38]. In
this paper, the composition of phases, microstructures, and mechanical properties of the
welded joints are analyzed.
The experimental works were part of comprehensive research which has been moti-
vated by the necessity to adjust welding parameters carefully and to protect the materials
by vacuum. No comprehensive study dealing with careful investigation of the effects of
different welding conditions on the microstructure and properties of these materials had
been performed prior. The paper brings some novel and important findings. First, it should
be mentioned the used welding parameters affected the penetration depth, the fusion zone
width, and also the width of heat affected zone in the welded joints. Second, we determined
the relationships between the obtained microstructures, hardness, ultimate tensile strength,
and ductility. Finally, the obtained results from the tensile strength testing were coupled
with fractographical analysis of the specimens from the tensile tests.

2. Materials and Methods

Titanium Grade 2 (a technically pure material with favorable mechanical properties
and high corrosion resistance) and commercially pure Nickel Ni 201 (with high resistance
to corrosion and good toughness) with dimensions of 50 × 100 × 2 mm were used as
base materials. Tables 1 and 2 show the chemical compositions of the base materials. The
chemical compositions of these base materials were measured using a Bruker Q4 TASMAN
optical emission spectrometer (Bruker, Madison, WI, USA). The average values of three
different places were calculated for chemical composition. Energy dispersive spectroscopy
(EDS) (JEOL Ltd., Tokyo, Japan) analysis confirmed the phase constitution inside the weld
regions and the fusion interfaces. The base material’s mechanical properties are given
in Tables 3 and 4. Milling was done on the weld surfaces to ensure precise contact, and
acetone was used to remove the oxidation coating. The plates to be welded were clamped
in the fixture with minimum restraint in a butt weld geometry and placed into the vacuum
chamber (Figure 2). PZ EZ 30 STU electron beam welding complex (First Welding Company,
Bratislava, Slovakia) was used for joining dissimilar metals. The maximum accelerating
voltage of the equipment is 60 kV. An accelerating voltage of 55 kV was used in the study.
A vacuum of 10−2 Pa was created in the chamber, and the vacuum in an electron gun
was 10−5 Pa. With the help of a technological computer, the welding parameters were set,
which were designed on the basis of literature reporting the same or similar issues, and we
performed tests. The experiments consisted of 16 welds. The value of the welding current
was changed in the range of 40 to 70 mA, and the welding speed was 20 to 50 mm/s. The
electron beam was focused on the top surfaces of the materials to be welded, i.e., a focusing
current of 890 mA was used. Positive beam offset was set to Ni 100, 200, and 300 µm
(samples 2, 3, 4), and negative beam offset was to the Ti side 200 µm (sample 5) (Table 5).
Furthermore, samples 15 and 16 were welded using circular oscillation.
Metals 2022, 12, 894 4 of 18

Table 1. Chemical composition of Ni 201 alloy (in wt. %).

Fe Mn Si C S Cu Ni
0.40 0.35 0.35 0.15 0.01 0.25 Balance

Table 2. Chemical composition of Ti Grade 2 (in wt. %).

Fe C O H N Ti
0.30 0.08 0.25 0.015 0.03 Balance

Table 3. Mechanical properties of Ni 201 alloy.

Tensile Strength Rm (MPa) Yield Strength Rp0.2 (MPa) Ductility (%)

345 70 40

Table 4. Mechanical properties of Ti Grade 2.

Metals 2022, 12, x FOR PEER REVIEW Tensile Strength Rm (MPa) Yield Strength Rp0.2 (MPa) Ductility (%) 5 of 20

485 350 20

(a) (b)

Figure
Figure 2.
2. Electron
Electron beam
beam welding
welding workplace—vacuum
workplace—vacuumchamber
chamber(a);
(a); setup
setup and
and clamping
clamping of
of welded
welded
materials
materials (b).
(b).

5. Electron
TableTables 5 andbeam welding
6 list parameters.
the welding parameters used in the experiment with calculated
heat inputs. The following equation [25] was used to calculate the heat input in electron
Welding Welding Focusing Heat Beam
beam welding:
Welded Accelerating
Current Speed Current Input Offset
Joint No. Voltage [kV]
[mA] . .
[mm/s] [mA] [J/mm] [µm]
Q= (J/mm) (1)
1 55 60 30 890 110 0
where2 is welding 55 current in mA;
60 U is accelerating
30 voltage
890 in kV; k is110
thermal efficiency,
+100 Ni
which3 can be 0.9–1.0
55 [37]; and v60is welding speed
30 (mm/s).890 110
Thermal efficiency +2001.0
k was Ni in
4
our calculations. 55 60 30 890 110 +300 Ni
5 55 60 30 890 110 −200 Ti
6 55 50 30 890 91.67 0
Table 6. Oscillation parameters.
7 55 40 30 890 73.33 0
8
Welded 55
Channel Voltage A 70 30
Channel Voltage B 890 128.3 0
9 55 50 20 890 Frequency [Hz]0
137.5
Joint No. [mV] [mV]
10 55 50 40 890 68.75 0
15 200 200 200
11 55 50 50 890 55 0
16 200 200 200
12 55 40 40 890 55 0
13 55 40 30 890 73.33 0
Visual
14 inspection
55 was performed
40 for all20sixteen samples.
890 Based 110
on the results0of the
visual
15inspection,55 samples 1, 6,608, and 10 were
20 selected890 for more detailed
165 analysis.
0 The
16 55 60 30 890 110
cross-sections of weld joints were analyzed by ZEISS LSM 700 laser scanning confocal 0
microscope. An etchant with the composition HCl, 50 mL; H2O, 40 mL; HNO3, 10 mL; and
CuCl2, 2.5 g, was used to indicate the microstructures of the base metals and Ni-rich weld
metal. This process took about 20 s. After purification, the samples were prepared for
macroscopic and microscopic analysis. JEOL JSM 7600 F scanning electron microscope
(SEM) was applied for the study of chemical composition and microstructure analysis. On
etched samples, EDS evaluation was carried out. Microhardness was measured across
weld joints by a Buehler IndentaMet 1100 Series tester with the loading of 0.98 N (HV0.1).
 Metals 2022, 12, 894 5 of 18

Tables 5 and 6 list the welding parameters used in the experiment with calculated
heat inputs. The following equation [25] was used to calculate the heat input in electron
beam welding:
I·U·k
Q= (J/mm) (1)
v
where is welding current in mA; U is accelerating voltage in kV; k is thermal efficiency,
which can be 0.9–1.0 [37]; and v is welding speed (mm/s). Thermal efficiency k was 1.0 in
our calculations.

Table 6. Oscillation parameters.

Channel Voltage A Channel Voltage B

Welded Joint No. Frequency [Hz]
[mV] [mV]
15 200 200 200
16 200 200 200

Visual inspection was performed for all sixteen samples. Based on the results of the
visual inspection, samples 1, 6, 8, and 10 were selected for more detailed analysis. The
cross-sections of weld joints were analyzed by ZEISS LSM 700 laser scanning confocal
microscope. An etchant with the composition HCl, 50 mL; H2 O, 40 mL; HNO3 , 10 mL;
and CuCl2 , 2.5 g, was used to indicate the microstructures of the base metals and Ni-rich
weld metal. This process took about 20 s. After purification, the samples were prepared
for macroscopic and microscopic analysis. JEOL JSM 7600 F scanning electron microscope
(SEM) was applied for the study of chemical composition and microstructure analysis. On
etched samples, EDS evaluation was carried out. Microhardness was measured across weld
joints by a Buehler IndentaMet 1100 Series tester with the loading of 0.98 N (HV0.1). The
distance between gaps was 100 µm. Across the middle of samples 1, 6, 8, and 10, thickness
was measured. Dwell time was 10 s. The hardness measurements for the contour plot of
samples 8 and 10 were performed with an automated EMCO M1C (EMCO Test, Kuchl,
Austria) hardness machine due to the standard DIN EN SO 6507-4: 2006-03. Vickers (HV)
indentations with a load of 1.96 N (HV0.2 ) were performed in a dwell time of 15 s. The
distance between indentations was 0.3 mm, and contour plots were derived using Matlab
Metals 2022, 12, x FOR PEER REVIEW 6
routine (The Mat Works, Natick, MA, USA). For tensile strength tests, we used the LabTest
5.250 SP1-VM tensile testing machine (LABORTECH s.r.o., Opava, Czech Republic). The
specimens are in Figure 3. The crosshead speed was 3 mm/s.

Figure
Figure 3.3.The
The tensile
tensile test test specimens’
specimens’ schematic
schematic (a), andtest
(a), and fractured fractured test
specimens specimens
after after
tensile testing (b).tensile te
(b).

3. Results
3.1. Weld Bead and Root Appearance
The samples visually assessed, during which longitudinal and transverse cracks w
 Metals 2022, 12, x FOR PEER REVIEW 6 of 20
Metals 2022, 12, 894 6 of 18

3. Results
3.1. Weld Bead and Root Appearance
The samples visually assessed, during which longitudinal and transverse cracks were
recorded along the whole weld. Cracking in the weld after solidification led to a loss of
the integrity of the welded joint. The welds fell apart. Only four samples 1, 6, 8, and 10
retained the integrity of the joint and were prepared by the parameters shown in Table 5.
Figure 4 shows the appearance of the weld bead and root for dissimilar welded joints
1, 6, 8, and 10. The width of the weld bead was in the range of 2.402–2.686 mm (Table 7).
The weld bead surface of sample 1 was where the crack was located. For sample 8, the
weld root was located in the crack. In both samples, the heat input was higher than in
samples 6 and 10. A low heat input per unit length of an EBW weld can significantly reduce
residual strains and prevent cracking of the bead and root of the weld joint. The surfaces
of the weld bead and root of samples 6 and 10 (Figure 4) were uniform and smooth. The
mentioned welded
Figure 3. The tensilejoints were produced
test specimens’ with
schematic (a),lower heat inputs
and fractured of 68.75 and
test specimens after91.67
tensileJ/mm.
testing
The
(b).welding speed was constant at 30 mm/s, but for sample 10 it was increased, thereby
reducing the heat input as much as possible. The results in relation to heat input and weld
width are shown in Figure 5.
3. Results
3.1. Weld Bead and Root Appearance
3.2. Analysis of Weld Cross-Sections
Thesides
The samples visually
of each assessed, during
full penetration weld which longitudinal
were nearly parallel.and
Thetransverse cracks
weld profile onwere
the
Ti side was straighter than that of the Ni side. This was visible mainly in samples 6 and 8of
recorded along the whole weld. Cracking in the weld after solidification led to a loss
the integrity
(Figure 6). Theofgeometry
the welded joint. The
of welds waswelds fell depending
different apart. Onlyon four
thesamples
welding1,parameters
6, 8, and 10
used. The dependence on calculated heat input and weld width can be seen on in
retained the integrity of the joint and were prepared by the parameters shown theTable
chart5.
Figure 4 shows the appearance of the weld bead and root for
in Figure 5. The macrostructure images clearly show the melting asymmetry—Ti is more dissimilar welded joints
1, 6, 8, and 10. The width of the weld bead was in the range of 2.402–2.686
susceptible to melting than Ni. Additionally, in the welds can be observed the segregated mm (Table 7).
The weld bead surface of sample 1 was where the crack was located.
Ni-rich regions (brighter contrast). The asymmetric weld pool with a greater extent of For sample 8, the
weld root
melting was on
formed located
the Tiinside.
the The
crack. In both
reason samples,
for weld poolthe heat input
asymmetry is was higherthermal
the lower than in
samples 6of
diffusivity and 10. A low heat
Ti compared to thatinput perwhich
of Ni, unit length
resultsofinan EBW
more weld can
localized significantly
heating, and as re-
a
duce residual strains and
consequence, more melting of Ti. prevent cracking of the bead and root of the weld joint. The
surfaces of the weld bead and root of samples 6 and 10 (Figure 4) were uniform and
3.3. Analysis
smooth. Theofmentioned
the Microstructure
welded joints were produced with lower heat inputs of 68.75 and
91.67 J/mm. Theofwelding
Monitoring speed was constant
the microstructures at 30 mm/s,
of the samples but for sample
was performed in the10following
it was in-
creased,
areas: BM thereby reducing
(base metal) titaniumthe Grade
heat input
2–HAZas much as possible.
(heat affected zone)The results
of the in relation
BM Ti, BM–WMto
heat input
(weld metal),and weld width
BM–HAZ of theareBMshown
Ni, andin Figure 5.
HAZ–BM–nickel 201 (Figure 7).

Welding Welding Focusing Beam

Weld Heat Input
Current Speed Current Offset
Joint No. (J/mm)
(mA) (mm/s) (mA) (µm)
Weld Face Root Surface
1 60 30 890 0 110

Figure 4. Cont.
Metals 2022,12,
Metals2022, 12,894
x FOR PEER REVIEW 77 of
of1820

6 50 30 890 0 91.67

8 70 30 890 0 128.3

10 50 40 890 0 68.75

Figure4.4.Weld
Figure Weldbead
beadand
androot
rootview
viewfor
forjoints
jointsproduced
producedwith
withelectron
electronbeam
beamwelding
weldingwith
withdifferent
different
parameters (samples 1, 6, 8, 10).
parameters (samples 1, 6, 8, 10).

Table7.7.Measured
Table Measuredwidths
widthsofofthe
thebead
beadand
androot
rootfor
fordissimilar
dissimilarweld
weldjoints.
joints.

Welded Joint
Welded No.No.Width ofWidth
Joint the Weld Bead
of the [mm]
Weld Bead [mm] Width of the
Width Weld
of the Root
Weld [mm]
Root [mm]
1 2.485 2.104
1 2.485 2.104
6 2.402 1.424
6 2.402 1.424
8 2.686 1.493
8 2.686 1.493
10 10 2.670 2.670 1.580
1.580

Titanium Grade 2 has a polyhedral morphology. In terms of chemical composition, it

is pure titanium with a small amount of alloying elements. The microstructure contains fine
grains with slight heterogeneity in grain size: grains are 5 to 30 µm. The heat-affected area
from the base material differs by significant coarsening of the grain (two to three times).
The grains have a polyhedral structure, and at some boundaries, it is possible to see the
undulations which may have been caused by the heat. The weld metal of samples had a
predominantly dendritic morphology. Dendrites are formed by the substitution of a solid
solution of the γ phase, which contains nickel and titanium, or a small amount of alloying
elements of used alloys.
PEER REVIEW 8 of 20
Metals 2022, 12, 894 8 of 18

2.75

2.7 10. 8.

2.65
Weld width (mm)

2.6

2.55
1.
2.5

2.45
6.
2.4

2.35
60 80 100 120 140
Metals 2022, 12, x FOR PEER REVIEW Heat input (J/mm) 9 of 20

Figure 5. Dependence of heat input (J/mm) on weld width (mm) for samples 1, 6, 8, and 10.
Figure 5. Dependence of heat input (J/mm) on weld width (mm) for samples 1, 6, 8, and 10.

3.2. Analysis of Weld Cross-Sections

The sides of each full penetration weld were nearly parallel. The weld profile on the
Ti side was straighter than that of the Ni side. This was visible mainly in samples 6 and 8
(Figure 6). The geometry of welds was different depending on the welding parameters
used. The dependence on calculated heat input and weld width can be seen on the chart
in Figure 5. The macrostructure images clearly show the melting asymmetry—Ti is more
susceptible to melting than Ni. Additionally, in the welds can be observed the segregated
Ni-rich regions (brighter contrast). The asymmetric weld pool with a greater extent of
melting formed on the Ti side. The reason for weld pool asymmetry is the lower thermal
diffusivity of Ti compared to that of Ni, which results in more localized heating, and as a
consequence, more melting of Ti.

Cross-sections of weld joints produced with different welding parameters.

Figure 6. Cross-sections parameters. Samples
Samples 11 (a),
(a),
6 (b), 8 (c), 10 (d).

3.3. Analysis of the Microstructure

Monitoring of the microstructures of the samples was performed in the following
areas: BM (base metal) titanium Grade 2–HAZ (heat affected zone) of the BM Ti, BM–WM
(weld metal), BM–HAZ of the BM Ni, and HAZ–BM–nickel 201 (Figure 7).
Titanium Grade 2 has a polyhedral morphology. In terms of chemical composition,
it is pure titanium with a small amount of alloying elements. The microstructure contains
Metals 2022, 12, x FOR PEER REVIEW 10 of 20
Metals 2022, 12, 894 9 of 18

Figure
Figure 7. Nickel–HAZtransition
7. Nickel–HAZ transition zone
zone of
of weld
weld88(a);
(a);weld
weldmetal
metal8 (b); titanium–HAZ-base
8 (b); metalmetal
titanium–HAZ-base of of
weld 8 (c).
weld 8 (c).

Ni structures have a polyhedral character. The matrix is made of nickel austenite. The
3.4.austenite
SEM Analysis
grains are about 10 to 200 µm. The boundaries of grains are clear without the
The microstructure
precipitation of secondaryof phases.
the weld pool is composed
Annealing twins could ofbe different
observed in phases, which are de-
nickel austenitic
grains. Their presence is typical for metals and alloys with a K12 lattice.
termined via EDS analysis. Welded joints produced with a heat input of 128.3 J/mm (8) or
68.75 J/mm (10) were analyzed. As the phases in the Ti–Ni system have distinct composi-
3.4. SEM Analysis
tions, the EDS analysis allowed for unmistakable phase identification (Figures 8 and 9);
The microstructure of the weld pool is composed of different phases, which are deter-
this was verified with results from previous studies using the same conditions for the
mined via EDS analysis. Welded joints produced with a heat input of 128.3 J/mm (8) or
electron beam welding. The intermetallic phases in this system have a wide range of com-
68.75 J/mm (10) were analyzed. As the phases in the Ti–Ni system have distinct composi-
positions.
tions, theThe
EDSmeasurements
analysis allowedhelped in the phase
for unmistakable phaseidentification. The intermetallic
identification (Figures 8 and 9); this com-
pounds are referred
was verified to byfrom
with results their respective
previous studiesstoichiometric
using the sameratios, and for
conditions thethe
terminal
electron solid
solutions with varied
beam welding. solute content
The intermetallic areinreferred
phases to ashave
this system (Ti)aand
wide(Ni).
range of compositions.
The measurements helped in the phase identification. The intermetallic compounds are
referred to by their respective stoichiometric ratios, and the terminal solid solutions with
varied solute content are referred to as (Ti) and (Ni).
Metals
Metals 2022,
Metals2022, 12,
12,xx894
2022,12, FOR PEER
FOR PEER REVIEW
REVIEW 11
10 of11 of 20
18 of 20

Figure8.8.
Figure
Figure 8.Measurement
Measurement
Measurement of
ofof chemical
chemical
chemical composition
composition
composition by EDS
by by
EDSEDS analysis
analysis
analysis (weld
(weld
(weld 8).
8). 8).

Figure9.9.
Figure
Figure 9.Measurement
Measurement
Measurement of chemical
of chemical
of chemical composition
composition
composition by EDS
by EDS(nickel–weld
by EDS analysis analysis (nickel–weld
analysis (nickel–weld metal
metal
metal interface) interface)
(weldinterface)
10).
(weld 10).
(weld 10).
SEM-EDS was used to analyze each phase of the weld in more depth, and the results
are presented
SEM-EDS
SEM-EDS inwas
Tables
was used
used 8 and
to 9. The weld
to analyze
analyze microstructure
each phase
each phase of of the
the weldnear
weld inthe
in more
moretitanium
depth,isand
depth, shown
and in
the results
the results
Figures 10 and
are presented
are presented in 11. Based
in Tables on
Tables 88 and the
and 9. Ti–Ni
9. The binary
The weld phase diagram
weld microstructure
microstructure near (Figure
near the1), the microstructure
the titanium
titanium is is shown
shown in in
near Ti Grade
Figures
Figures 10 and211.
10 and side
11. consisted
Based
Based on the
on ofTi–Ni
the a mixture
Ti–Ni binary
binary of phase
β–Ti and
phase Ti2 Ni (Figure
diagram
diagram produced
(Figure 1),by
1), thethe
the eutectic
microstructure
microstructure
reaction
near Ti
near L → β-Ti
Ti Grade
Grade + Ticonsisted
22 side
side Ni. The content
2consisted of titanium
of aa mixture
of mixture of β–Ti
of β–Ti wasand
andabout 71produced
Ti22Ni
Ti Ni at. % andby
produced thethe
by nickel
the eutectic
eutectic
content of 29
reaction LL → at.
→ β-Ti % was
β-Ti ++ Ti detected
Ti22Ni.
Ni. The (Figure
The content
content of 8). Then,
of titanium
titanium wasin the direction
was about
about 71 towards
71 at.
at. %
% and the
and the Ni side, con-
the nickel
nickel
reaction con-
the microstructure evolved into a mash-up of TiNi and Ti2 Ni which was given by the
tent of
tent of 29
29 at.
at. % % waswas detected
detected (Figure (Figure 8). 8). Then,
Then, in in the
the direction
direction towards
towards the the NiNi side,
side, the
the
reaction L → TiNi and peritectic reaction L + TiNi → Ti2 Ni. In this location, the titanium
microstructure evolved
microstructure evolved into into aa mash-up
mash-up of of TiNi
TiNi andand Ti Ti22Ni
Ni which
which was was given
given by by the
the reaction
reaction
content decreased to 65 at. % and nickel content raised to 35 at. %. The brittle intermetallic
LL→ → TiNi
TiNi and
and peritectic
peritectic reaction
reaction LL ++ TiNi TiNi → → Ti Ti22Ni.
Ni. In
In this
this location,
location, the the titanium
titanium content
content
compounds (IMCs) TiNi and Ti2 Ni created cracks more easily in the phase interface and
decreased
decreased
finally to 65
to 65inat.
resulted at. % and
the%joint’s nickel
and nickel content
failure.content raised
raised
EDS results to
ofto 35 at.
the35cracked %.
at. %. The The brittle
brittle
interface intermetallic
intermetallic
(Figure 11c) alsocom-com-
pounds (IMCs)
pounds
confirmed (IMCs) TiNi and
TiNi
the existence and aTinumber
of Ti Ni created
22Ni created cracks more
cracks
of different more easily
Ti–Nieasily
basedin in the phase
the
IMCs. phase interface and
interface
The microstructure and finally
finally
of
resulted in the joint’s failure. EDS results of the cracked interface
the weld metal center is shown in Figures 10b and 11b. The dendritic structure contained con-
resulted in the joint’s failure. EDS results of the cracked interface (Figure
(Figure 11c)
11c) also
also con-
firmed
firmed
the the
TiNitheand existence
existence
TiNi3 IMCs, of a number
of a number
which were of different
of different Ti–Ni
given byTi–Ni based IMCs.
based IMCs.
the reaction of L →TheThe
TiNi microstructure
microstructure
+ TiNi3 , which of the
of the
weld metal
weld
became metal
the basecenter
center is shown
is
phase. shown
As shown in Figures
in Figures
n Figure 10b
10b
10a,and
and 11b.
the11b. The dendritic
The
microstructuredendritic structure
structure
in the weld near contained
contained
Ni side the the
TiNimainly
was
TiNi and TiNi
and TiNi
formed IMCs,
by the
33 IMCs, which
threewere
which were given
different
given by the
shapes
by the reaction
of solid solution
reaction of LLof→
of →γ-Ni.
TiNi
TiNi ++ TiNi
ThereTiNi
was33,, which
which be-
about be-
21.92 at.
came the
came % of
the base elemental
base phase.
phase. As Ti in
As shown the γ-Ni
shown nn Figure (Figure
Figure 10a, 9 and
10a, the Table 9),
the microstructurewhich
microstructure in was considered
in the
the weld
weld near as
near Ni the
Ni side
side
mixture
was of phases
was mainly
mainly formed
formed Ni by+ TiNi
by the three
the .
3three different shapes
different shapes of of solid
solid solution
solution of of γ-Ni.
γ-Ni. There
There was was about
about
21.92 at.
21.92 at. %
% of
of elemental
elemental Ti
Ti in
in the
the γ-Ni
γ-Ni (Figure
(Figure 99 and
and Table
Table 9),
9), which
which was
was considered
considered as
as the
the
mixture of
mixture of phases
phases Ni
Ni ++ TiNi
TiNi33..
x FOR PEER REVIEW 12 of 20

Metals 2022, 12, 894 11 of 18

Table 8. EDS point analysis of weld 8 (Ni—weld metal interface) (in at. %).

Spectrum Ti Ni
Table 8. EDS point analysis of weld 8 (Ni—weld metal interface) (in at. %).
1. 0.00 100.00
2. Spectrum 0.00 Ti 100.00 Ni
3. 1. 0.31 0.00 99.69 100.00
4. 2. 4.59 0.00 95.41 100.00
5. 3. 45.45 0.31 54.55 99.69
4. 4.59 95.41
6. 5.
65.07 45.45
34.93 54.55
7. 6. 50.73 65.07 49.27 34.93
8. 7. 66.52 50.73 33.48 49.27
9. 8. 51.44 66.52 48.56 33.48
9. 51.44 48.56
10. 50.85 49.15
10. 50.85 49.15

Table 9. EDS point analysis weld 10 (nickel–weld metal interface) (in at. %).
Table 9. EDS point analysis weld 10 (nickel–weld metal interface) (in at. %).
Spectrum Ti Ni
Spectrum Ti Ni
1. 0.00 100.00
2. 1. 21.92 0.00 78.08 100.00
2. 21.92 78.08
3. 3.
45.91 45.91
54.09 54.09
4. 4. 49.35 49.35 50.65 50.65

SEM
Figureof10.the
Figure 10. SEM analysis analysis of themetal
Ni–HAZ–weld Ni–HAZ–weld
interface metal interface
of weld 8 (a); of weld
high 8 (a); high magnification
magnification of of
weld metal area (b);weld
weldmetal area (b);
metal–Ti HAZ weld metal–Ti(c).
interface HAZ interface (c).
022, 12, x FOR PEER
Metals 2022,REVIEW
12, 894 13 of 20 12 of 18

Figure 11. SEM Figure

analysis11.ofSEM
the Ni–HAZ–weld
analysis of the metal of weld 10metal
Ni–HAZ–weld (a); higher magnification
of weld 10 (a); higherofmagnification
weld of weld
metal interface (b); weld
metal metal–Ti
interface (b);HAZ
weldinterface
metal–Ti(c).
HAZ interface (c).

Figure 10a shows the 10a

Figure fusion line the
shows on the Ni side.
fusion The
line on thebase metalThe
Ni side. grains
basedid not grains
metal grow did not grow
intosolidification
into the weld. The the weld. The solidification
process began with process began with
the formation of a the
solidformation
solution layerof a solid solution
(Ni) on the purelayer (Ni) onofthe
Ni grains thepure
base Ni grains
metal andof the base
passed metal
to the and passed
formation of the to the formation of the
interme-
intermetallic
tallic phase TiNi in HAZ. The phase TiNi was
Ni layer in HAZ. The Based
wetted. Ni layeronwas
the wetted. Based onthe
phase diagram, theNi phase
3Ti diagram, the
Ni
+ (Ni) phase region 3 Ti was not observed. However, faceted primary Ti2Ni dendrites were 2 dendrites
+ (Ni) phase region was not observed. However, faceted primary Ti Ni
also observed. were also observed.
The microstructure
The microstructure of the center ofofweld the center
metal of weld metal
consisted mainly consisted
of NiTimainly
and Tiof 2NiNiTi and Ti2 Ni

phases. Figurephases.
10b shows Figure 10b shows
a typical a typical microstructure
microstructure characteristic of characteristic
this region. of Thethis region. The light
light
grey contrast’sgrey contrast’s
dendrites weredendrites
NiTi, while werethe NiTi, whileparts
dark grey the dark
were grey
Ti2Ni,parts were Ti
according to2 Ni, according
composition analyses. Frequently, alternate layers of coarse and fine NiTi formed NiTi formed
to composition analyses. Frequently, alternate layers of coarse and fine
throughout thethroughout
central region the central regionThe
of the weld. of the
NiTiweld. The
layer’s NiTi layer’s
growth in the growth
formation in the
of formation of
dendrites was sandwiched betweenTi Ni layers. The
dendrites was sandwiched betweenTi2Ni layers. The2NiTi phase also occurred as a large NiTi phase also occurred as a large
area of the weld pool. The NiTi phase also created cellular/dendritic
area of the weld pool. The NiTi phase also created cellular/dendritic morphology that re- morphology that
reflected
flected the remaining the remaining characteristics
microstructural microstructuralofcharacteristics
bright contrastofinbright contrast in the figure.
the figure.
Figure 10c shows the Ti fusion interface microstructure.
Figure 10c shows the Ti fusion interface microstructure. It was characterized by It was characterized
Ti2Ni by Ti2 Ni
dendrites in the interdendritic space and β-Ti + Ti 2 Ni
dendrites in the interdendritic space and β-Ti + Ti2Ni eutectic. The inset of this picture eutectic. The inset of this picture
shows the disintegration of the Ti 2 Ni solidification front
shows the disintegration of the Ti2Ni solidification front growing toward the Ti base metal growing toward the Ti base metal
from within the weld pool. The microstructure of the
from within the weld pool. The microstructure of the weld pool from the Ti interface weld pool from the Ti interface shows
shows the NiTithe NiTi dendrites
dendrites growinggrowing in opposite
in opposite directions,
directions, i.e., intoi.e.,
the into
weldthe weld
pool shownpool shown in the
next
in the next picture. picture.
We can see a Ti fusion interface with the wide area of the HAZ containing the Ti2 Ni
We can see a Ti fusion interface with the wide area of the HAZ containing the Ti2Ni
layer, which grew further into the base metal. The interface of the base material and the
layer, which grew further into the base metal. The interface of the base material and the
HAZ was linear and separated into pure forms. The HAZ created from the Ni side was
HAZ was linear and separated into pure forms. The HAZ created from the Ni side was
about 7 µm; in the case of the Ti side, it was wider, around 80 µm.
about 7 μm; in the case of the Ti side, it was wider, around 80 μm.
The fusion line on the Ni side in Figure 11a reveals only a small amount of base metal
The fusion line on the Ni side in Figure 11a reveals only a small amount of base metal
development into the weld. The base metal formed a cellular morphology and grew as a
development into the weld. The base metal formed a cellular morphology and grew as a
solid solution phase γ-Ni containing up to 21.92 at. % of Ti. It can be seen that a Ni3 Ti layer
solid solution phase γ-Ni containing up to 21.92 at. % of Ti. It can be seen that a Ni3Ti layer
Metals 2022, 12, x FOR PEER REVIEW 14 of 20
Metals 2022, 12, 894 13 of 18

and the eutectic region grew. In this image, the rest of the microstructure, and the majority
and
of thethe eutectic
weld, region grew.
are composed In this
of the Ni3image, theeutectic.
Ti + NiTi rest of the microstructure, and the majority
of the weld, are composed of the Ni3 Ti + NiTi eutectic.
3.5. Microhardness Measurements
3.5. Microhardness Measurements
The distribution of microhardness across the welded joints was analyzed to further
studyThe the distribution of microhardness
microstructure vs. mechanicalacross the welded
properties joints was
relationships, analyzed to
as illustrated in further
Figure
study the microstructure vs. mechanical properties relationships, as illustrated
12. By keeping the weld centered, microhardness measurements were taken of prepared in Figure 12.
By keeping
weld joints. the
Theweld centered,
hardness microhardness
of weld measurements
metal was determined were taken
to have a peakofhardness
preparedvalue
weld
joints. The hardness of weld metal was determined to have a peak hardness value in
in the range 660.3–483.4 HV, as shown by the hardness profile. The microhardness of base
the range 660.3–483.4 HV, as shown by the hardness profile. The microhardness of base
metal was compared to the manufacturer’s reported values. The values of measured mi-
metal was compared to the manufacturer’s reported values. The values of measured
crohardness of HAZ were somewhat similar to microhardness values of the base metal.
microhardness of HAZ were somewhat similar to microhardness values of the base metal.
From the above values, it is clear that the microhardness of the weld metal was five times
From the above values, it is clear that the microhardness of the weld metal was five times
higher than that of the base metal.
higher than that of the base metal.

Figure 12.
Figure The distribution
12. The distributionof
ofmicrohardness
microhardnessacross
acrossthe
theTi–weld
Ti–weldmetal–Ni
metal–Niinterface
interfaceof
ofsample
sample88(a)
(a)
and sample
and sample 10
10 (b).
(b).

By achieving
By achieving lower
lower microhardness
microhardness inin the
the Ti/Ni
Ti/Niweld,
weld,the
theductility
ductility of
of the
the joint
joint and
and its
its
crack stop property can be improved.
crack stop property can be improved.
Figure 13a
Figure 13a presents
presents the
the microhardness
microhardness map
map ofof welded
welded joint
joint 8.
8. This
This weld
weld joint
joint sample
sample
was created with the welding speed of 30 mm/s, welding current of 70 mA, which
was created with the welding speed of 30 mm/s, welding current of 70 mA, which was the was the
highest welding current used in these samples, and the heat input of 128.3
highest welding current used in these samples, and the heat input of 128.3 J/mm. J/mm.
Nickel and titanium, as the base metals, had homogenous distributions of hardness
corresponding to their microhardness values as predicted by theory, according to a mi-
crohardness contour map generated from microhardness measurements over the weld
cross-section. The base metals Ti and Ni and their heat-affected zones microhardness
were identical, due to the small heat input by the electron beam welding, as opposed to
traditional fusion welding. It effectively eliminates grain development close to the weld
metal interface. In the weld metal, the microhardness rapidly grew, which was expected
because of the presence of the intermetallic layer. In the weld metal, the average microhard-
ness was much higher than the average microhardness of the base metals. The increase
in microhardness in the weld metal was most likely associated with the presence of the
brittle intermetallic compound TiNi3 . Using a filler metal prevents brittle intermetallic
Ti–Ni system compounds from forming, and the hardness decreases [38]. The influence
of heat input is clear. Based on the microhardness maps, when the higher heat input was
used, higher microhardness in the weld metal was recorded. Microhardness map for weld
joint 10 produced with a heat input of 68.8 J/mm is given n Figure 13b. In this case, lower
Metals 2022, 12, 894 14 of 18

microhardness values were measured in the weld metal. When taking a closer look at
the microhardness course across the mid-thickness of both welded joints, it is necessary
to underline some important remarks. The microhardness of titanium Grade 2 averaged
194 HV and that of nickel 201 averaged 123 HV. The average value of microhardness of the
weld metal in the case of heat input 128.3 J/mm (8) reached the value of 603 HV. The drop
Metals 2022, 12, x FOR PEER REVIEW 15 of 20
of the heat input to 68.8 J/mm (10) resulted in a decrease in the weld metal microhardness
to 376 HV. This could be associated with the greater intermixing of both metals when high
heat input was used.

Figure 13. Microhardness map of weld joints 8 (a) and 10 (b) produced with various heat
heat inputs.
inputs.

NickelStrength
3.6. Tensile and titanium,
Resultsas the base metals, had homogenous distributions of hardness
corresponding to their microhardness
Tensile testing was used to determine values as predicted
the mechanical by theory, due
characteristics according to a mi-
to the standard
crohardness contour map generated from microhardness measurements
STN 6892-1. The same welding conditions were employed to prepare representative samples over the weld
cross-section.
for the tensile The
test base
as formetals
other Ti and Ni Four
samples. and their heat-affected
samples zones microhardness
of each weldment were subjected wereto
identical, due to the small heat input by the electron beam welding,
tensile tests. All samples ruptured at the HAZ of the Ti side. The tensile test measurementas opposed to tradi-
tional
valuesfusion
are shownwelding.
in theItgraph
effectively eliminates
of heat input vs.grain development
tensile strength. Noclose cleartotrend
the weld metal
was found
interface. In the weld metal, the microhardness rapidly grew, which
between heat input, beam current, or welding speed and tensile strength. The values of was expected because
of the presence
tensile of thesample
strength were: intermetallic
10—175 layer.
MPa;Insample
the weld6—155metal,
MPa;thesample
average microhardness
1—190 MPa; and
was much
sample higher
8—160 MPa.than the average microhardness of the base metals. The increase in mi-
crohardness in theappears
Each sample weld metal
to havewasbroken
most likely associated
soon after with
the yield the presence
point was reached.of the brittle
Further-
intermetallic compound
more, the ultimate TiNiand
strength 3. Using
the afracture
filler metal
pointprevents
were bothbrittle intermetallic
coincident. Ti–Ni
There wassys-
no
tem compounds from forming, and the hardness decreases [38]. The
necking in this scenario. Figure 14a,b illustrates the influences of heat input on the weldinfluence of heat in-
put is clear.
strength and Based on thecurves
stress–strain microhardness
of electronmaps,
beamwhen welded thejoints
higher heat
8 and 10.input was used,
higher microhardness in the weld metal was recorded. Microhardness map for weld joint
3.7.produced
10 Fracture Surfaces
with a heat input of 68.8 J/mm is given n Figure 13b. In this case, lower mi-
crohardness
The SEMvalues
imageswere measured
in Figure 15a,b in
showthe the
weld metal.surface’s
fracture When taking a closer
interface look 8atfrom
in sample the
microhardness
the Ti side and course
the weld across
metal the mid-thickness
side. We know from of both welded
previous joints, it is that
experiments necessary
the base to
metal Ti results
underline some in an evident
important ductile The
remarks. dimple fracture, andofthe
microhardness interface
titanium of the
Grade base metal194
2 averaged Ti
andand
HV weldthat
metal had a brittle
of nickel cleavage123
201 averaged fracture
HV. The on the fracture
average valuesurface with river markings.
of microhardness of the
Theremetal
weld were in
several crack
the case initiations
of heat in theJ/mm
input 128.3 traverse course. the
(8) reached Thevalue
cracksofwere initiated
603 HV. by a
The drop
cleavage
of the heatprocess.
input to 68.8 J/mm (10) resulted in a decrease in the weld metal microhardness
to 376 HV. This could be associated with the greater intermixing of both metals when high
heat input was used.

3.6. Tensile Strength Results

Tensile testing was used to determine the mechanical characteristics due to the stand-
 trend was found between heat input, beam current, or welding speed and tensile strength.
The values of tensile strength were: sample 10—175 MPa; sample 6—155 MPa; sample 1—
190 MPa; and sample 8—160 MPa.
Each sample appears to have broken soon after the yield point was reached. Further-
more, the ultimate strength and the fracture point were both coincident. There was no
Metals 2022, 12, 894
necking in this scenario. Figure 14a,b illustrates the influences of heat input on the15weld
of 18

strength and stress–strain curves of electron beam welded joints 8 and 10.

Figure 14. Heat input influences the weld strength (a). Stress–strain curves of electron beam welded
joints 8 (128.3 J/mm) and 10 (68.8 J/mm) (b).

3.7. Fracture Surfaces

The SEM images in Figure 15a,b show the fracture surface’s interface in sample 8
from the Ti side and the weld metal side. We know from previous experiments that the
base metal Ti results in an evident ductile dimple fracture, and the interface of the base
metal Ti and weld metal had a brittle cleavage fracture on the fracture surface with river
Figure 14.
markings.
Figure 14. Heat
Heat
There input
input influences
were the
severalthe
influences weld
crack strength (a).
initiations
weld strength (a). Stress–strain
in Stress–strain curves
the traversecurves of The
course.
of electron beam
cracks
electron welded
were
beam in-
welded
joints
itiated 8
joints 8 by(128.3 J/mm)
a cleavage
(128.3 and
J/mm) and 10 (68.8
process. J/mm) (b).
10 (68.8 J/mm) (b).

3.7. Fracture Surfaces

The SEM images in Figure 15a,b show the fracture surface’s interface in sample 8
from the Ti side and the weld metal side. We know from previous experiments that the
base metal Ti results in an evident ductile dimple fracture, and the interface of the base
metal Ti and weld metal had a brittle cleavage fracture on the fracture surface with river
markings. There were several crack initiations in the traverse course. The cracks were in-
itiated by a cleavage process.

Figure 15. Morphology of the fracture surface at the interface of Ti Grade 2 and weld metal (a,b).
Figure 15. Morphology of the fracture surface at the interface of Ti Grade 2 and weld metal (a,b).

Several
Several secondary
secondary cracks
cracks were
were stopped
stopped by by grain
grain boundaries.
boundaries. ForFor the
the fracture
fracture ofof the
the
welded joint at room temperature, the brittle fracture was situated exactly at the interface
of base metal Ti and weld metal. This means that this interface was the weakest position
of the
the welded
weldedjoint,
joint,essentially
essentiallydueduetoto
thethe
larger grains.
larger There
grains. waswas
There no plastic area area
no plastic that was
that
visible. Furthermore,
was visible. Furthermore, EDSEDSpoint analysis
point was
analysis carried
was carriedout
outononthe
thefracture
fracture surface.
surface. The
chemical composition analysis revealed that about 67 at. % of titanium and 33 at. % of
nickel
Figure were present inofthe
15. Morphology theanalyzed locations,
fracture surface corresponding
at the to the2presence
interface of Ti Grade and weld of Ti2 Ni
metal MC
(a,b).
decreasing the mechanical properties of the welded joint.
Several secondary cracks were stopped by grain boundaries. For the fracture of the
4. Discussion
welded joint at room temperature, the brittle fracture was situated exactly at the interface
of base
Themetal Ti and
research wasweld metal.
focused onThis means
joining that this
different interface
Ti/Ni was using
materials the weakest
electronposition
beam
of the welded
welding joint, essentially
technology. due towere
Two substrates the larger
used grains. There was noTiplastic
for the experiment, Grade2area
andthat was
Ni201
alloy, both
visible. measuring 50
Furthermore, EDS× 100 × 2analysis
point mm. Welding parameters
was carried out onwerethe designed on the basis
fracture surface. The
of literature facing the same or similar issues. The experiments consisted of 16 welds.
The values of welding current varied from 40 to 70 mA and the welding speed from
20 to 50 mm/s. The electron beam was focused on the upper surfaces of the materials to
be welded, using a focusing current of 890 mA. For samples 15 and 16, circular oscillation
was used in welding. The analysis of the welded joints took place in several stages. The
geometry and shape of the surface and root of the weld were monitored by visual inspection.
The width of the weld on the surface and on the root side was measured. Longitudinal
and transverse cracks were recorded along the weld on the surface of the weld joint and
Metals 2022, 12, 894 16 of 18

on the root side. Cracking in the weld after solidification led to a loss of the integrity of
the welded joint, and there was a change in the consistency of the joint. As a result of the
visual inspection, it was possible to subject samples 1, 6, 8, and 10 to subsequent analysis,
as they retained their integrity according to the designed and used welding parameters
(Table 7). The width of the surface weld was in the range of 2.402–2.686 mm. Low heat input
per unit length of EBW weld can significantly reduce residual deformation and prevent
cracking of the surface and the root of the welded joint. For a more detailed analysis, we
selected sample 8 with a heat input of 128.3 J/mm and sample 10 with a heat input of
68.75 J/mm. The geometry of the welds varied depending on the welding parameters
used, but samples 8 and 10 showed approximately the same values of surface width and
weld root, in spite of their different heat input values. The resulting microstructure and
the proportion of intermetallic phases in the weld were affected by the cooling rate of
the liquid. The cooling rates of melted material in the fusion zones of the weld joints of
samples 8 and 10 were estimated by computing Equation (2) [39]:
 2
s
R = −2πκρC (T − T0 )3 (2)
Q

where R is the cooling rate (K/s); T is the liquid’s temperature (1583 K for NiTi)); T0 is
the room temperature (293 K); κ is the thermal conductivity (8.6 W/m K); ρ is the density
of material (6450 kg/m3 ); C is the specific heat (837 J/kg·K); s is the thickness of welded
specimen (0.002 m); Q is heat input (J/m).

Joint 8 (Q = 128300 J/m) R = 152 K/s

Joint 10 (Q = 68750 J/m) R = 530 K/s

Cracking can be suppressed by increasing the cooling rate of the liquid. At high cooling
rates, a supersaturated solid solution is formed (NiTi diagram Figure 1), which reduces the
formation of intermetallic phases NiTi, Ni3 Ti, and NiTi2 . An increase in cooling rate can
be achieved by reducing the heat input (Equation (2)). This corresponds to the results in
Figure 2. The influence of heat input is clear. Based on the microhardness maps, when the
higher heat input was used, higher microhardness of the weld metal was recorded.
The macrostructural analysis confirmed higher asymmetry of Ti melting. The cause
of the asymmetry of the weld pool was the lower thermal diffusion of Ti compared to Ni.
The microstructures of the samples were monitored in the areas: BM (base metal) titanium
Grade 2–HAZ (heat affected zone) of the BM, Ti BM–WM (weld metal), Ti BM–HAZ of the
BM Ni, and HAZ–BM–nickel 201. Ti Grade 2 and Ni 201 had polyhedral morphology. The
microstructure of Ti contained fine grains with slight heterogeneity. The heat-affected area
differed by significant grain coarsening. The grains had a polyhedral structure, and waves
could be seen at some borders. This could have been due to higher heat. The weld metal
had a predominantly dendritic morphology. Dendrites were formed by the substitution of
the solid solution of the γ phase. The Ni matrix was made of austenite. Austenite grains
showed heterogeneity of about 10 to 200 µm. The grain boundaries were clear without
precipitation of secondary phases. Annealing twins could be observed in austenitic grains.
The subjects of further research will be the monitoring of the proportions of intermetal-
lic phases in the weld metal, depending on the cooling rate, and attempts at stabilizing the
structure and minimizing stresses in the weld metal by means of heat treatment.

5. Conclusions
Dissimilar Ti Grade 2–Ni 201 welds were prepared by EBW by using different weld-
ing parameters. The macrostructures and microstructures, microhardness, and tensile
properties have been analyzed. The following conclusions can be drawn:
• The samples were subjected to visual testing, in which longitudinal and transverse
cracks were recorded along the whole weld. Cracking in the weld after solidification
led to a loss in integrity of the welded joint.
Metals 2022, 12, 894 17 of 18

• Fully penetrated welds had near parallel fusion lines on both sides. The weld profile
on the Ni side was straighter than on the Ti side.
• The weld metal had a predominantly dendritic morphology. Dendrites were formed
by a substitution solid solution of the γ phase, which contained nickel and titanium,
or a small number of alloying elements used n alloys.
• The microstructure of the weld pool was composed of various phases, which were
detected by SEM composition analysis. The microstructure in the weld pool’s middle
section was largely made up of NiTi and TiNi3 .
• The microhardness of the base material was compared to the producer’s declared
values. The values of the measured hardness of HAZ were somewhat similar to the
hardness values of the base material. The hardness of weld metal was five times higher
than that of the base material.
• No clear trend was found between heat input and tensile strength. Brittle fracturing
was observed after tensile testing. There were several crack initiations in the traverse
course. The cracks were initiated by a cleavage process due to the formation of
intermetallic compounds, namely, Ti2 Ni.

Author Contributions: Conceptualization, B.Š. and E.H.; methodology, P.K.; software, F.P.; validation,
P.K., I.K. and M.S. (Miroslav Sahul); formal analysis, M.P.; investigation, P.K.; resources, B.Š.; data
curation, M.S. (Martin Sahul); writing—original draft preparation, B.Š.; writing—review and editing,
E.H.; visualization, M.P.; supervision, P.K.; project administration, I.K.; funding acquisition, E.H. All
authors have read and agreed to the published version of the manuscript.
Funding: The research was carried out under the support of the Vedecká grantová agentúra VEGA
grant agency of the Ministry of Education, Science, Research and Sport of the Slovak Republic,
project 1/0499/21; by the Slovak Research and Development Agency under the contract APVV-SK-
AT-20-0013 (Bilateral project Slovakia—Austria SK-AT 2020); and by the International Cooperation in
Higher Education Department of the OeAD (“Research on electron beam weldability of hard to join
dissimilar materials” SK14/2021).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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