metals
Article
Microstructure of Butt Joint of High-Silicon Steel Made Using
CO2 Laser Welding and Inconel 82 Filler
Ming-Feng Chiang 1 , Ping-Hui Chien 2 , Tzu-Yuan Lo 2 and Ren-Kae Shiue 2, *
Citation: Chiang, M.-F.; Chien, P.-H.;
Lo, T.-Y.; Shiue, R.-K. Microstructure
of Butt Joint of High-Silicon Steel
Made Using CO2 Laser Welding and
Inconel 82 Filler. Metals 2023, 13, 234.
https://doi.org/10.3390/
met13020234
Academic Editors: Xiangdong Gao
and Aleksander Lisiecki
Received: 18 December 2022
Revised: 24 January 2023
Accepted: 24 January 2023
Published: 26 January 2023
Copyright: © 2023 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Metals 2023, 13, 234. https://doi.org/10.3390/met13020234
1 Iron and Steel Research & Development Department, China Steel, Kaohsiung 812, Taiwan
2 Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan
* Correspondence: rkshiue@ntu.edu.tw
Abstract: A nickel-based filler wire, Inconel 82, was applied to weld a high-silicon steel plate with
a chemical composition in wt% of 2.6 Si, 0.5 Al and Fe balance. The chemical composition of
the heterogeneous weld bead was deviated from that of the conventional alloy due to incomplete
mixing/convection between the filler wire and base metal in the weld pool. The microstructure of
the weld bead was examined in greater depth by FESEM/EBSD, EPMA/WDS and STEM/EDS in
the experiment. The heterogeneous weld bead was primarily composed of austenite and martensite,
and mainly governed by the Ni concentration. A Schaeffler diagram based on the ratio of Cr and Ni
equivalents in the selected positions of the weld bead was used to predict the structure and phase(s)
of the Fe-based weld bead. A methodology for the analysis of a weld metal with an unconventional
alloy composition has been proposed in the study.
Keywords: laser welding; microstructure; austenite; martensite; ferrite
1. Introduction
Lasers have been widely used in many industrial applications, such as heat treatment,
ablation, surface modification, precision cutting, cladding, welding and 3-D printing in
recent years, and they demonstrate great potential in many areas of advanced materials
processing [1–7]. With the rapid advancement of laser technology, many lasers have been
used in the fabrication of metallic engineering components [8,9]. There is no clear definition
of high-power laser in the industry, for it depends on many factors, such as the types
of lasers, laser beam quality, efficiency of the laser optical system, laser mode and laser
application. For industrial welding, CO2 lasers of several kWs are sufficiently powerful
for most applications. Therefore, a 10 kW CO2 laser can be considered a high-power laser.
High-power CO2 laser welding has the characteristics of high heat flux and low total heat
input [10,11]. Compared with traditional fusion welding, high-power laser welding can
produce a high-quality weld bead with reasonable production and tooling costs [12,13].
In high-power laser welding in the keyhole mode, the high-energy-density laser
beam causes extensive mixing of the filler metal and base metal (BM). However, the
convection of the molten weld pool is incomplete due to the rapid thermal cycle of laser
welding. Therefore, the elemental distributions in the weld bead (WB) are not uniform on a
macroscopic scale [14]. The chemical composition of the heterogeneous WB will be quite
different from those of the filler wire and base metal. The chemical composition of the WB
is strongly related to the dilution of the BM, and it plays a crucial role in the microstructure
of the solidified WB after laser welding [10,11,14].
The IN82 filler wire has the characteristics of high strength, good toughness, and
resistance to solidification cracking after welding, so it was used in the study [11,12]. It has
been successfully applied in welding many ferrous and nickel-based alloys [15–18]. The
microstructure of the heterogeneous WB of a ferrous BM welded with the nickel-based IN82
filler wire is quite complex because of the phase transformation of the WB is involved in
https://www.mdpi.com/journal/metals
Metals 2023, 13, 234 2 of 13

the fusion zone. Austenite, ferrite and martensite can all be observed in the WB, depending
on the dilution of the weld pool [14]. The Schaeffler diagram illustrates the microstructure
of a welded stainless steel with the aid of Cr/Ni equivalents [10,11]. For the ferrous alloys,
chromium element can stabilize the ferrite with a body centered cubic (BCC) structure, and
the nickel element stabilizes austenite with a face-centered cubic (FCC) structure. With the
aid of the Schaeffler diagram, the microstructure of the WB can be predicted by calculating
the ratio of Cr and Ni equivalents in the fusion zone of the laser WB.
In order to observe the effect of weld pool convection after laser welding, a het-
erogeneous WB was particularly designed in the experiment. The combination of the
nickel-based IN82 filler wire and high-silicon steel BM plate was applied in the test. The
chemical composition of IN82 filler wire primarily consists of Ni, Cr, Mn and Nb, and the
high silicon BM is alloyed with Fe, Si and Al. Alloying elements in the BM are quite differ-
ent from those in the filler wire. A high-silicon steel plate with the chemical composition
of 97.4 Fe, 2.6 Si and 0.5 Al in wt% was laser welded using the IN 82 filler wire to make
a heterogeneous WB. Redistribution of elements and the related phase transformations
in the WB that resulted from the convection of the weld pool induced by the irradiation
of the high-power CO2 laser beam can be accurately identified with aid of advanced mi-
crostructure analysis methods. The validity of the Schaeffler diagram in predicting the
microstructure in the CO2 laser WB was also clarified in the study. The methodology
proposed in the investigation provides an alternative approach to the WB analysis.

2. Material and Experimental Procedures

A high-silicon steel plate with a thickness of 1.8 mm was used in the experiment, and
its chemical composition in wt% was 2.6 Si, 0.5 Al and Fe balance. The diameter of the IN82
filler wire was 1 mm, and its chemical composition in wt% was 0.04 C, 19.99 Cr, 1.28 Fe,
2.97 Mn, 2.51 Nb, 0.09 Si, and Ni balance. The laser power was kept at 10 kW. The maximum
stable IN-82 wire feeding rate was 4 m/min. The traveling speed of the laser head was
optimized in order to obtain full penetration of the weld in a preliminary study, and a travel
speed of 6.5 m/min was used in the experiment [19]. Figure 1a shows the laser welding
station and a schematic diagram of laser welding. A butt joint with a single-square-groove
weld without a gap zone was used in the experiment. Figure 1b displays the top view of
the specimen after laser welding, and the red arrow shows the direction of welding. The
top view of the laser welded seam is included at the center of the specimen next to the red
arrow. Figure 1c shows the cross-section of the heterogeneous WB, including the image of
the weld roots, and full penetration was achieved after laser welding.
After laser welding, the WB was cut and mounted in the conductive resin. The
specimen was roughly ground with 400 grit SiC sandpaper of number 400, and it was
subsequently polished by diamond suspensions with different diamond sizes of 9, 3,
1, and 0.1 µm, respectively. After the polishing, a dilute SiO2 suspension was used to
perform slight chemical etching so as to relieve the surface stress before the electron back
scattered diffraction (EBSD) analysis was performed. A JEOL JXA-8530F Plus electron
probe micro-analyzer (EPMA, JEOL, Tokyo, Japan) combined with a wavelength dispersive
spectrometer (WDS) was used to quantitatively analyze the chemical compositions of
selected positions in the WB. Both secondary electron image (SEI) and back-scattered
electron image (BEI) were used in the analyses. A JEOL JSM-7800F Prime field emission
scanning electron microscope (FESEM, JEOL, Tokyo, Japan) equipped with an Oxford
Nordlys Max 3 EBSD (Oxford Instruments, Abingdon, UK) was applied for crystal structure
analyses of the WB. An ultrahigh resolution electron microscope, the JEOL JEM-2100F
Cs scanning transmission electron microscope (STEM, JEOL, Tokyo, Japan), was used to
examine the complex microstructures of the investigated sample in greater depth. The
specimen was prepared by using a twin jet polisher.
Metals 2023, 13, 234 3 of 13

Metals 2023, 13, 234 3 of 13

Japan), was used to examine the complex microstructures of the investigated sample in
greater depth. The specimen was prepared by using a twin jet polisher.

(a)

(b) (c)
Figure1.1.(a)
Figure (a)The
Thelaser
laserwelding
weldingstation
stationand
andaaschematic
schematicdiagram
diagramof
oflaser
laserwelding,
welding,(b)
(b)top
topview
viewof
ofthe
the
specimen after laser welding, and (c) the cross-section of the WB.
specimen after laser welding, and (c) the cross-section of the WB.

Microhardness measurements
Microhardness measurements of of the
the WB
WB and
andBM
BMwere
wereperformed
performedwith
withthe
theStruers
Struers
Duramin-100 AC 3 hardness tester (Struers, Ballerup, Denmark) with a load of 100 ggand
Duramin-100 AC 3 hardness tester (Struers, Ballerup, Denmark) with a load of 100 and
duration of 15 s. Tensile test was performed according to the ASTM-E8M specification
duration of 15 s. Tensile test was performed according to the ASTM-E8M specification with
with
the the miniature
miniature specimenspecimen
size. size.

3.3.Results
Resultsand
andDiscussion
Discussion
Figure
Figure2a 2ashows
showsthethecross-section
cross-section of of
thethe
WBWBafter CO2CO
after laser welding,
2 laser and and
welding, bothboth
the BMthe
and
BMWBandareWBlabelled in thein
are labelled figure. The microstructure
the figure. along along
The microstructure the longitudinal direction
the longitudinal of the
direction
weld seam
of the weldcannot
seamclearly
cannotexpress
clearlythe convection
express of the weldofpool
the convection theduring laser during
weld pool welding. In
laser
contrast,
welding.theIn cross-section
contrast, the microstructure of the WB in the
cross-section microstructure of central
the WBportion of the weld
in the central seam
portion of
presents
the weldthe best presents
seam effect of weld pooleffect
the best convection
of weldduring
poollaser welding.
convection Therefore,
during laserthe cross-
welding.
section of the
Therefore, theWB was selected
cross-section ofinthe
theWBanalysis. The corresponding
was selected EBSD
in the analysis. Thecrystallographic
corresponding
and
EBSD crystallographic and boundary misorientation maps of the WB are respectively.
boundary misorientation maps of the WB are presented in Figure 2b,c, presented in
The shape
Figure of the
2b,c, WB was easily
respectively. The identifiable
shape of the in the
WBEBSDwasboundary misorientation
easily identifiable in the map,
EBSDas
illustrated
boundary in Figure 2c. Themap,
misorientation trumpet-like WB isinthe
as illustrated result2c.
Figure of joint melting of theWB
The trumpet-like laterally
is the
advanced fillermelting
result of joint wire in of
thethe
laser beamadvanced
laterally and of thefiller
basewire
materials
in theedges, during
laser beam and theofwelding
the base
process.
materialsAccording to Figure
edges, during the 2b,c, the BM
welding microstructure
process. According contains ferrite2b,c,
to Figure withthea BCCBM
structure, having grain size from about 50 to 250 µm.
 be studied later. The upper portion of the WB appears to be rich in austenite, and the
middle/lower portions of the WB are primarily dominated by the BCC structure. Based
on Figure 2b,c, there were few boundaries in the austenite. In contrast, the BCC structure
in the WB contained a high density of high-angle boundaries (>10°). The presence of high-
Metals 2023, 13, 234 4 of 13
density boundaries in the BCC structure of the WB was very different from those in the
ferrite of the BM. It is obvious that the BCC structure in the WB was not a simple ferrite.

Figure 2. Cross-section images of the high-power CO2 laser WB: (a) EPMA SEI image; FESEM EBSD
Figure 2. Cross-section images of the high-power CO2 laser WB: (a) EPMA SEI image; FESEM
(b)EBSD
crystallographic map; (c) boundary misorientation map; EPMA WDS quantitative element
(b) crystallographic map; (c) boundary misorientation map; EPMA WDS quantitative element
mappings in wt%: (d) Cr, (e) Fe, (f) Nb, (g) Ni, (h) Si.
mappings in wt%: (d) Cr, (e) Fe, (f) Nb, (g) Ni, (h) Si.

Because of the
There are twoincomplete convection
different structures, of thethe
namely, weld
redpool
BCCduring
structuretheandlaser welding,
blue FCC the
structure,
chemical are readily distinguishable
composition from theWB
of the heterogeneous WB.was
The not
bluehomogeneous
FCC structure isafter the austenite.
solidification.
However,
Figure 2d–hthe red BCC
present thestructure here could
quantitative be martensite
element mappings orofferrite,
Cr, Fe,andNb,it will
Ni beandstudied
Si in wt%.
later. The upper portion of the WB appears to be rich in austenite, and the
It is evident that WB contains the dominant austenite, which is located in the upper part middle/lower
portions of the WB are primarily dominated by the BCC structure. Based on Figure 2b,c,
of the weld, having higher concentrations of Cr, Nb and Ni compared to the middle and
there were few boundaries in the austenite. In contrast, the BCC structure in the WB
root zones, where
contained a high the low-alloyed
density BCCboundaries
of high-angle structure predominates. Sinceofthe
(>10◦ ). The presence BM was free of
high-density
these
boundaries in the BCC structure of the WB was very different from those in the the
elements, the existence of Cr, Nb and Ni must have originated from IN82
ferrite of filler
wire.
the The nickel-based
BM. It is obvious thatIN82thefiller was melted
BCC structure and
in the WB diluted
was notwith the high
a simple ferrite.Si BM during the
welding. The trace
Because of theof the convection
incomplete vortex
convection in the
of the weldweld
pool pool
during during laser
the laser welding
welding, thecould
chemical composition of the heterogeneous WB was not homogeneous after
easily be identified from quantitative element mappings of Cr, Fe and Ni, as illustrated in solidification.
Figure2d,e,g.
Figure 2d–h present
As shown the quantitative
in Figure 2e,element mappings composition
the chemical of Cr, Fe, Nb, Ni of and
Fe in Si the
in wt%.
WB was
It is evident that WB contains the dominant austenite, which is located
between 50 and 97 wt%. In contrast, the Ni concentration in the WB was between 0 and in the upper part
of the weld, having higher concentrations of Cr, Nb and Ni compared to the middle and
root zones, where the low-alloyed BCC structure predominates. Since the BM was free of
these elements, the existence of Cr, Nb and Ni must have originated from the IN82 filler
wire. The nickel-based IN82 filler was melted and diluted with the high Si BM during the
welding. The trace of the convection vortex in the weld pool during laser welding could
easily be identified from quantitative element mappings of Cr, Fe and Ni, as illustrated
in Figure 2d,e,g. As shown in Figure 2e, the chemical composition of Fe in the WB was
Metals 2023, 13, 234 5 of 13

between 50 and 97 wt%. In contrast, the Ni concentration in the WB was between 0 and
35 wt%, as shown in Figure 2g. Therefore, the heterogeneous WB was an Fe-based alloy.
Since the melting time was short, Cr and Ni elements did not diffuse to the Fe-rich matrix
of the base material. This effect is well highlighted from the elemental distribution images
in Figure 2d,g, which illustrate the trace of the melt convection driven by the keyhole
mechanism in the entire laser WB in the EPMA/WDS analyses.
Based on the Fe-Ni binary alloy phase diagram, Ni is completely soluble in austenite at
elevated temperatures, but in ferrite the maximum solubility of Ni is only 2 wt% Ni below
200 ◦ C [20]. Table 1 shows quantitative chemical analyses of selected positions, labelled
A~G in Figure 1a,b. Position A is the BM, with a chemical composition of 0.5 Al, 96.7 Fe,
0.1 Mn and 2.6 Si in wt%. The chemical composition of position G in the WB is very similar
to that of the BM at position A. The Ni concentration at position G is as low as 0.7 wt%,
well below the maximum solubility of the Ni in the ferrite [20]. It was deduced that there
were a few resolidified ferrite grains in the WM. Position B and E are austenite alloyed with
26.4 and 28.7 wt% Ni, respectively. In contrast, positions C, D and F are the BCC structure
in the WB. The BCC structure in the WM is featured with high-density boundaries, as
demonstrated in Figure 2c. As shown in Table 1, the range of Ni concentration in the BCC
structure is between 5.1 and 13.2 wt%. Both the high-density boundaries and the wide
range of Ni concentrations in the BCC structure exclude the possibility that simple ferrite
was the BCC structure in the WB.

Table 1. Quantitative chemical analyses of positions A~G in Figure 1a,b.

Element/wt% Al Cr Fe Mn Nb Ni Si Phase/Structure
A 0.5 0.0 96.7 0.1 0.0 0.0 2.6 ferrite (BM)
B 0.4 7.1 60.9 1.3 1.0 26.4 2.5 austenite
C 0.4 3.6 79.3 0.4 0.4 13.2 2.5 BCC
D 0.4 1.7 88.9 0.2 0.2 5.8 2.4 BCC
E 0.5 6.7 55.0 1.6 3.0 28.7 3.8 austenite
F 0.4 1.6 89.9 0.2 0.2 5.1 2.4 BCC
G 0.4 0.1 96.0 0.1 0.0 0.7 2.5 ferrite (WB)

The complete melting of the IN-82 filler wire and the BM in the weld pool was
achieved upon laser irradiation. Strong convection of the weld pool resulted in the mixing
of the various elements between the filler wire and BM. However, the characteristics of
extremely short interaction time during the laser welding resulted in incomplete mixing
of the filler wire and the BM in the weld pool. The dilution of the heterogeneous WB was
not homogeneous after solidification [14]. Therefore, the phase/structure of the WB was
not uniformly distributed after solidification. According to the aforementioned results, the
redistribution of Ni in the WB was mainly driven by convection and dilution of the BM
into the weld pool, and it was strongly related to the formation of the phase/structure of
the WB [14].
The Schaeffler diagram has been successfully applied in welding many stainless
steels [21–27]. The phase/structure prediction of the laser weldment for many Fe-based
alloys has also been reported [28–30]. When the laser welding is performed, the Schaeffler
diagram, consisting of the chromium equivalent (= %Cr + %Mo + 1.5 %Si + 0.5 %Nb) and
nickel equivalent (= %Ni + 30 %C + 0.5 %Mn), can be used to predict the microstructure
of the WB according to the ratio of Ni/Cr equivalents [21,22]. In this study, the Schaeffler
diagram was used to predict the BCC structure of the WB. The WDS quantitative chem-
ical analysis results of the cross-section at positions A ~ G, shown in Table 1, were used
to calculate the Cr and Ni equivalents, and the Cr/Ni equivalents were marked on the
Schaeffler diagram, as shown in Figure 3 [10]. According to Figure 3, positions B and E in
Figure 2b were austenite, marked with blue dots, and positions C, D and F in Figure 2b were
martensite, marked by red dots. The martensite area shown in the Schaeffler diagram has a
wide range of Cr/Ni equivalents. In Figure 2c, the BCC structure has a very high boundary
 Metals
Metals 2023, 13, 234 2023, 13, 234 6 of 13 6 of

result
density, which is of theinEBSD
also crystal
line with thestructure analyses
characteristics were consistent
of martensite. with the
The result Schaeffler
of the EBSD diagram
It can be inferred that the BCC structure of the WB was primarily composed
crystal structure analyses were consistent with the Schaeffler diagram. It can be inferred of martensit
It isstructure
that the BCC worth mentioning that primarily
of the WB was position Acomposed
was BM that neither melted
of martensite. nor solidified
It is worth men- durin
tioning thatthe laser welding.
position A was BM Therefore, it was
that neither ferrite
melted stabilizedduring
nor solidified by 2.6wt% Si without
the laser welding.martensit
Therefore, transformation.
it was ferrite stabilized by 2.6wt% Si without martensitic transformation.

Figure 3. The Schaeffler

Figure 3. Thediagram of the
Schaeffler WB cross-section
diagram at positions at
of the WB cross-section A~G in Figure
positions A~G2ab
in[10].
Figure 2ab [10].

Figure 4 presents
Figure 4EPMA SEIs,
presents EBSDSEIs,
EPMA crystallographic and boundary
EBSD crystallographic and misorientation
boundary misorientatio
maps of selected
maps of selected areas I, II and III in the cross-section of the WB in
areas I, II and III in the cross-section of the WB displayed Figure 2a,b
displayed in Figure 2a
at higher magnification. In Figure 2b, two structures are visible in areas I
at higher magnification. In Figure 2b, two structures are visible in areasand II. Area IIIII. Area
I and
is mainly composed of the BCC structure. Based on the boundary misorientation
is mainly composed of the BCC structure. Based on the boundary misorientation ma maps
illustrated in Figure 4c,f,i, the BCC structure had a high density of boundaries above
illustrated in Figure 4c,f,i, the BCC structure had a high density of boundaries above 2
2o , even at higher magnification. Table 2 presents the quantitative chemical analyses of
even at higher magnification. Table 2 presents the quantitative chemical analyses
positions H~S in Figure 4. Both Cr/Ni equivalents can be calculated according to Table 2.
positions H~S in Figure 4. Both Cr/Ni equivalents can be calculated according to Table
Figure 5 shows the Schaeffler diagram of the WB cross-section at positions H~S marked
Figure 5 shows the Schaeffler diagram of the WB cross-section at positions H~S marke
in Figure 4 [10]. According to Table 2 and Figure 4b,e and Figure 5, positions, H, I and N
in Figure 4 [10]. According to Table 2 and Figures 4b,e and 5, positions, H, I and N we
were austenite with high Ni concentrations of 20.1, 21.2 and 24.9 wt%, respectively. The
austenite with high Ni concentrations of 20.1, 21.2 and 24.9 wt%, respectively. T
chemical composition at position P in wt% was 0.2 Al, 13.1 Cr, 34.8 Fe, 2.4 Mn, 1.5 Nb,
chemical composition at position P in wt% was 0.2 Al, 13.1 Cr, 34.8 Fe, 2.4 Mn, 1.5 Nb, 45
45.8 Ni and 1.3 Si. This result is beyond the range of the Schaeffler diagram due to the
Ni and 1.3 Si. This result is beyond the range of the Schaeffler diagram due to the high N
high Ni equivalent of 47. The high Ni concentration of 45.8 wt% was resulted from low
equivalent of 47. The high Ni concentration of 45.8 wt% was resulted from low dilution
dilution of the BM in area II (Figure 2b) [14]. The accumulation of nickel-based filler in the
the BM in area II (Figure 2b) [14]. The accumulation of nickel-based filler in the top regio
top region of the WB was caused by the nature of insufficient mixing between the filler
wire and BM of the WBweld
in the was pool
caused by the
during thenature of insufficient mixing between the filler wire and B
laser welding.
in the weld pool during the laser welding.
Metals 2023, 13,
Metals 2023, 13, 234
234 77of
of 13
13

Figure 4. EPMA SEIs, EBSD crystallographic and boundary misorientation maps of selected areas
Figure 4. EPMA SEIs, EBSD crystallographic and boundary misorientation maps of selected areas
in the cross-section of the weld bead displayed in Figure 1a at higher magnification: (a–c) area I, (d–
in area
f) the cross-section of the
II and (g–i) area III. weld bead displayed in Figure 1a at higher magnification: (a–c) area I,
(d–f) area II and (g–i) area III.
The BCC structure was identified at the positions K, L, and M (Figure 4b), O (Figure
Table 2. Quantitative chemical analyses of positions H~S in Figure 4.
4e), Q, R, and S (Figure 4h), which was in the martensite region of the Schaeffler diagram,
Element/wt% Al as
Crdemonstrated
Fe in FigureMn5. It is noteworthy
Nb thatNi
the red dot Si
J in Figure 4b is located in
Phase/Structure
the region where martensite and austenite coexist. This is consistent with the region of A
H 0.3 5.9 71.3 0.4 0.2 20.1 1.3 austenite
I 0.3
+6.3M in the68.7
Schaeffler diagram
0.6
(Figure
0.4
5). EBSD
21.2
crystallographic
2.1
analyses, EPMA
austenite
J 0.3 quantitative
5.0 chemical analyses
75.6 0.5 and the 0.2Schaeffler 16.4
diagram were 1.7all in good agreement.
BCC
K 0.3 3.3 83.3 0.3 0.1 10.7 1.8 BCC
L 0.4 Table
2.4 2. Quantitative
85.8 chemical
0.2 analyses of0.3
positions H ~8.2
S in Figure 4.2.4 BCC
M 0.4 2.0 88.5 0.2 0.2 6.2 2.3 BCC
N 0.4 7.0Element/wt%
62.1 Al 1.3Cr Fe1.5 Mn 24.9 Nb Ni 2.2Si Phase/Structure
austenite
O 0.4 2.6 H 85.6 0.3 0.45.9 71.3
0.3 0.4 0.2
8.4 20.1 2.2 1.3 austenite
BCC
P 0.2 13.1 I 34.8 0.3 2.46.3 1.5
68.7 0.6 45.8
0.4 1.3
21.2 2.1 —
austenite
Q 0.4 2.6 85.2 0.3 0.3 8.3 2.5 BCC
J 0.3 5.0 75.6 0.5 0.2 16.4 1.7 BCC
R 0.4 2.7 85.9 0.2 0.2 8.3 2.0 BCC
S 0.4 2.7 K 84.6 0.3 0.33.3 83.3
0.2 0.3 0.1
9.0 10.7 2.4 1.8 BCC
BCC
L 0.4 2.4 85.8 0.2 0.3 8.2 2.4 BCC
M 0.4 2.0 88.5 0.2 0.2 6.2 2.3 BCC
N 0.4 7.0 62.1 1.3 1.5 24.9 2.2 austenite
O 0.4 2.6 85.6 0.4 0.3 8.4 2.2 BCC
P 0.2 13.1 34.8 2.4 1.5 45.8 1.3 ---
Q 0.4 2.6 85.2 0.3 0.3 8.3 2.5 BCC
R 0.4 2.7 85.9 0.2 0.2 8.3 2.0 BCC
S 0.4 2.7 84.6 0.3 0.2 9.0 2.4 BCC
Metals 2023,
Metals 13,13,
2023, 234234 8 of 13 8 of 13

5.The
Figure 5.
Figure TheSchaeffler
Schaefflerdiagram of the
diagram WB WB
of the cross-section at positions
cross-section H~S shown
at positions in Figurein4Figure
H~S shown [10]. 4 [10].

The BCC structure was identified at the positions K, L, and M (Figure 4b), O (Figure 4e),
Q, R,Based on Table
and S (Figure 4h),2,which
the Niwasconcentration played
in the martensite an important
region role in
of the Schaeffler the formation
diagram, as of
austenite
demonstratedandinmartensite
Figure 5. Itin the WB. Austenite
is noteworthy that the red wasdotformed if the
J in Figure Nilocated
4b is concentration
in the was
above 20 wt%.
region where In contrast,
martensite a wide
and austenite rangeThis
coexist. of isNi concentrations
consistent was observed
with the region of A + M in the
martensite. Thediagram
in the Schaeffler Ni concentration
(Figure 5). EBSDat position F was analyses,
crystallographic 5.1 wt% EPMA(Figure 2b), and the Ni
quantitative
chemical analyses
concentration at and the Schaeffler
position J was diagram
as highwere as all in good
16.4 wt%.agreement.
According to Figure 2g, the
Based onmapping
quantitative Table 2, theofNiNiconcentration
best represents played
the an important
strong role in of
convection thethe
formation
weld poolof in the
austenite and martensite in the WB. Austenite was formed if the Ni concentration was above
keyhole mode in laser welding [31].
20 wt%. In contrast, a wide range of Ni concentrations was observed in the martensite.
Figure 6a shows a bright field (BF) image of the BCC structure, and the selected area
The Ni concentration at position F was 5.1 wt% (Figure 2b), and the Ni concentration at
diffraction
position J waspattern
as high(SADP) is also
as 16.4 wt%. provided
According in Figure
to Figure 2g, the6b.quantitative
Lath martensite
mapping is of
visible in
Figure
Ni best 6a. There is
represents thea strong
notable absence of
convection retained
of the austenite
weld pool in the along
keyhole themode
lath in
boundaries
laser of
martensite.
welding [31]. Figure 6c shows a high-angle annular dark-field (HAADF) image, and the EDS
chemical
Figureanalysis
6a shows results
a brightatfield
positions 1–9 are
(BF) image of thelisted
BCCin Table 3.and
structure, ThetheNi concentrations
selected area in
diffraction
the pattern
table are (SADP)
between 8.5 is
andalso
9.5provided
in wt%.inTheseFigureare6b.consistent
Lath martensite
with theis visible in
aforementioned
Figure 6a.
results There is that
indicating a notable absence ofwill
the martensite retained austenite
be formed along
if the Ni the lath boundaries
concentration of
is between 5.1
martensite. Figure 6c shows a high-angle annular dark-field (HAADF) image, and the EDS
and 16.4 wt%. The STEM/EDS analysis results demonstrate that the BCC structure with a
chemical analysis results at positions 1–9 are listed in Table 3. The Ni concentrations in the
high density of boundaries in the EBSD analysis was martensite.
table are between 8.5 and 9.5 in wt%. These are consistent with the aforementioned results
indicating that the martensite will be formed if the Ni concentration is between 5.1 and
16.4 wt%. The STEM/EDS analysis results demonstrate that the BCC structure with a high
density of boundaries in the EBSD analysis was martensite.
 diffraction pattern (SADP) is also provided in Figure 6b. Lath martensite is visible in
Figure 6a. There is a notable absence of retained austenite along the lath boundaries of
martensite. Figure 6c shows a high-angle annular dark-field (HAADF) image, and the EDS
chemical analysis results at positions 1–9 are listed in Table 3. The Ni concentrations in
the table are between 8.5 and 9.5 in wt%. These are consistent with the aforementioned
Metals 2023, 13, 234 results indicating that the martensite will be formed if the Ni concentration is between 5.1 9 of 13
and 16.4 wt%. The STEM/EDS analysis results demonstrate that the BCC structure with a
high density of boundaries in the EBSD analysis was martensite.

Metals 2023, 13, 234 9 of 13

Figure 6. STEM analysis result of the BCC structure: (a) BF image, (b) SADP with the zone axis of
Figure STEM analysis
6.HAADF
[113], (c) image andresult of the BCC
EDS chemical structure:
analyses (a) BF1–9.
at positions image, (b) SADP with the zone axis of
[113], (c) HAADF image and EDS chemical analyses at positions 1–9.
Table 3. STEM/EDS chemical analyses at positions 1~9 in Figure 6c.
Table 3. STEM/EDS chemical analyses at positions 1~9 in Figure 6c.
Element/wt% Al Cr Fe Mn Nb Ni Si
1
Element/wt% 0.4
Al 4.3Cr 83.4 Fe 0.5 Mn 0.1 Nb 9.5 Ni 2.0 Si
2 0.4 4.4 83.5 0.5 0.0 9.3 1.9
1 0.4 4.3 83.4 0.5 0.1 9.5 2.0
2 3 0.4
0.4 4.24.4 83.783.5 0.8 0.5 0.4 0.0 8.8 9.31.8 1.9
34 0.4
0.4 4.54.2 84.183.7 0.6 0.8 0.1 0.4 8.5 8.81.9 1.8
45 0.5
0.4 4.14.5 83.684.1 0.6 0.6 0.4 0.1 9.0 8.51.9 1.9
56 0.4
0.5 4.14.1 84.283.6 0.6 0.6 0.4 0.4 8.5 9.01.7 1.9
67 0.4
0.3 4.14.1 84.384.2 0.5 0.6 0.3 0.4 8.8 8.51.8 1.7
78 0.3
0.4 4.24.1 84.084.3 0.5 0.5 0.3 0.3 8.6 8.81.9 1.8
89 0.4
0.4 4.24.2 84.284.0 0.6 0.5 0.4 0.3 8.5 8.61.8 1.9
9 0.4 4.2 84.2 0.6 0.4 8.5 1.8
Figure 7 shows the Vickers microhardness measurement results of the WB. In Figure
7a, the white7area
Figure showsin the
theWB is austenite,
Vickers and the gray
microhardness area in the WB
measurement is martensite.
results of the WB.There
In Figure 7a,
are two
the white lines in the
area cross-section
in the of the WB.and
WB is austenite, The the
hardness
gray measurements
area in the WB were performed There
is martensite.
from
are twothelines
left to
inthe
theright along the of
cross-section topthe
blue lineThe
WB. andhardness
bottom red line, respectively.
measurements wereTheperformed
distance between two measurements was set at 5 μm. In Figure 7b, the top blue line passed
from the left to the right along the top blue line and bottom red line, respectively. The
white austenite and gray martensite areas. The hardness of the base metal is
distance between two measurements was set at 5 µm. In Figure 7b, the top blue line
approximately 210 Hv0.1. The hardness of martensite ranges from 350 to 400 Hv0.1. In
passed white austenite and gray martensite areas. The hardness of the base metal is
contrast, the hardness of austenite is between 250 and 300 Hv0.1. In Figure 7c, the bottom
approximately
red line primarily210 Hv0.1
passed the. gray
The martensite
hardness of areamartensite ranges
in the WB with from 350above
the hardness to 400350Hv0.1 . In
contrast, the hardness of austenite is between 250 and 300 Hv .
Hv0.1. The hardness distribution in the WB is not uniform due to different combinations
0.1 In Figure 7c, the bottom
red line primarily
of martensite passedinthe
and austenite the gray
WB. Themartensite
martensite area
has in
thethe WB hardness
highest with theinhardness
the WB above
350 Hv0.1 . The with
in comparison hardness distribution
the austenite in the It
and ferrite. WB is not uniform
is deduced due
that the to different
combination of combinations
hard
martensite and soft austenite/ferrite in the WB is beneficial to its strength.
Metals 2023, 13, 234 10 of 13

of martensite and austenite in the WB. The martensite has the highest hardness in the WB
Metals 2023, 13, 234 in comparison with the austenite and ferrite. It is deduced that the combination 10
of of 13
hard
martensite and soft austenite/ferrite in the WB is beneficial to its strength.

(a)

(b)

(c)
Figure
Figure 7. Vickers microhardness
7. Vickers microhardnessmeasurements
measurementsofof thethe
WB:WB: (a) cross-section
(a) the the cross-section
of theofWB,
the (b)
WB, (b)
micro-
microhardness values along the top blue line in Figure 7a, and (c) microhardness values along the
hardness values along the top blue line in Figure 7a, and (c) microhardness values along the bottom
bottom red line in Figure 7a.
red line in Figure 7a.

Figure 8 shows three tensile test specimens perpendicular to the WB after tensile
tests. The BM and WB are labelled in the figure. All specimens were fractured in the BM
with the tensile strengths between 490 and 500 MPa. The necking of BM is observed in all
three specimens. In contrast, three WBs shown in Figure 8 are free of necking after tensile
Metals 2023, 13, 234 11 of 13

Figure 8 shows three tensile test specimens perpendicular to the WB after tensile tests.
The BM and WB are labelled in the figure. All specimens were fractured in the BM with
the tensile strengths between 490 and 500 MPa. The necking of BM is observed in all three
specimens. In contrast, three WBs shown in Figure 8 are free of necking after tensile tests.
Metals 2023, 13, 234 It is obvious that the combination of martensite and austenite/ferrite in the WB is 11 of 13
much
stronger than the ferrite of BM.

BM WB BM

10 mm

Figure8.8.Tensile
Figure Tensiletest
testspecimens
specimensperpendicular
perpendiculartotothe
theWB
WBafter
aftertensile
tensiletests.
tests.

4.4.Conclusions
Conclusions
TheIN82
The IN82filler
fillerwire
wireandandhigh-silicon
high-siliconsteel
steelWB
WBusing
usingaahigh-power
high-powerCOCO laserhas
2 2laser hasbeen
been
investigated with
investigated withthe theaid
aidof of EPMA/WDSquantitative
EPMA/WDS quantitativechemical
chemicalanalysis,
analysis,FESEM/EBSD
FESEM/EBSD
crystallographic analysis,
crystallographic analysis, and
andSTEM/EDS
STEM/EDS structure
structure analysis.
analysis. Important
Important conclusions
conclusions are
are
shownbelow:
shown below:
1.1. The
Theheterogeneous
heterogeneousWB WBwas wasmainly
mainlycomposed
composedofofaustenite
austeniteininthe theupper
upperportion
portionand and
martensite
martensiteininthe themiddle
middleand andbottom
bottomportions
portionsdue duetotoincomplete
incompletemixingmixingofofthe theweldweld
pool
poolduring
duringlaser
laserwelding.
welding.The Thetrace
traceofofconvection
convectionininthe theentire
entirelaser
laserweld
weldpool
poolwas was
successfully identified from the quantitative Ni mapping
successfully identified from the quantitative Ni mapping in the EPMA analysis.in the EPMA analysis.
2.2. The
Theformation
formationofofmartensite
martensiteand andaustenite
austenitewas wasdetermined
determinedby bythe
theNiNiconcentration
concentration
ofofthe
theWB.
WB.The Theaustenite
austenitewaswasalloyed
alloyedwith withNi Niabove
above20.1 20.1wt%.
wt%.The Theaustenite
austenitewas was
unstable
unstableand andtransformed
transformed intointo
martensite
martensite if theifNi
theconcentration
Ni concentration was decreased below
was decreased
16.4 wt%.
below Additionally,
16.4 there wasthere
wt%. Additionally, no retained
was noaustenite
retained observed
austeniteatobserved
the lath boundary
at the lath
ofboundary
martensite.of martensite.
3.3. The
Theaustenite
austeniteininthe theWB
WBwas wassoft
softwith
withthe thehardness
hardnessrangerangebetween
between250 250and
and300300Hv Hv0.10.1..
InIncontrast, the martensite had the highest hardness between
contrast, the martensite had the highest hardness between 350 and 400 Hv 350 and 400 Hv 0.10.1.The
. The
high-silicon BM had the lowest hardness
high-silicon BM had the lowest hardness of 210 Hv of 210 Hv 0.10.1. Therefore, the combinationof
. Therefore, the combination of
high-hardness
high-hardnessmartensite
martensite andandaustenite in theinheterogeneous
austenite the heterogeneous WB wasWB much stronger
was much
than the ferrite
stronger than theBM.ferrite
In theBM.tensile test,tensile
In the all specimens were fractured
test, all specimens were in the BM in
fractured withthe
the
BM with the tensile strengths between 490 and 500 MPa, and the necking of thewas
tensile strengths between 490 and 500 MPa, and the necking of the BM BM
observed after the
was observed tensile
after test. The
the tensile application
test. of the IN82
The application of thefiller wirefiller
IN82 in laser
wirewelding
in laser
awelding
high-silicon steel plate can successfully obtain a robust
a high-silicon steel plate can successfully obtain a robust WB. WB.

Author
AuthorContributions:
Contributions: Experiment,
Experiment,M.-F.C., T.-Y.L.,
M.-F.C., and P.-H.C.;
T.-Y.L., formal analysis,
and P.-H.C.; formal M.-F.C.; writing—
analysis, M.-F.C.;
original draft preparation,
writing—original R.-K.S.; writing—review
draft preparation, and editing, M.-F.C.
R.-K.S.; writing—review and R.-K.S.;
and editing, funding
M.-F.C. and acquisi-
R.-K.S.;
tion, R.-K.S.
funding All authorsR.-K.S.
acquisition, have read and agreed
All authors haveto the
readpublished version
and agreed of the
to the manuscript.
published version of the
manuscript.
Funding: This research was funded by the Ministry of Science and Technology, ROC (Contract No.
MOST 109-2221-E-002-042-MY3).
Funding: This research was funded by the Ministry of Science and Technology, ROC (Contract No.
MOST 109-2221-E-002-042-MY3).
Institutional Review Board Statement: Not applicable.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Data Availability Statement: Not applicable.
Acknowledgments: Thanks to C.S. Lin, Y.T. Lee, H.C. Lin and C.Y. Kao of Instrumentation Center,
National Taiwan University
Acknowledgments: Thanksforto FGSEM/EBSD and H.C.
C.S. Lin, Y.T. Lee, EPMA/WDS
Lin and analyses. The authors
Mr. C.Y. Kao gratefully
of Instrumentation
Center, National
acknowledge Taiwan
the use University
of JEOL JEM-2100F forCsFGSEM/EBSD
STEM of MOST and110-2731-M-006-001
EPMA/WDS analyses. The authors
belonging to the
gratefully
Core Facilityacknowledge the use
Center of National of JEOL
Cheng JEM-2100F Cs STEM of MOST 110-2731-M-006-001
Kung University.
belonging to the Core Facility Center of National Cheng Kung University.
Conflicts of Interest: The authors declare no conflicts of interest.

Nomenclature
BCC Body-centered cubic
Metals 2023, 13, 234 12 of 13

Conflicts of Interest: The authors declare no conflict of interest.

Nomenclature

BCC Body-centered cubic

BEI Back-scattered electron image
BF Bright field
BM Base metal
EBSD Electron back-scattered diffraction
EDS Energy-dispersive spectrometer
EPMA Electron probe micro-analyzer
FCC Face-centered cubic
FESEM Field emission scanning electron microscope
HAADF High-angle annular dark-field
IN82 Inconel 82
SADP Selected area diffraction pattern
SEI Secondary electron imaging
STEM Scanning transmission electron microscope
WB Weld bead
WDS Wavelength dispersive spectrometer

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