Artículo 1 - Aleación Ferrosa.
Artículo 1 - Aleación Ferrosa.
748
Article
Artur Czupryński, Damian Janicki, Jacek Górka, Andrzej Grabowski, Bernard Wyględacz,
Krzysztof Matus and Wojciech Karski
Special Issue
Advanced Technologies of Welding, Surfacing, and Thermal Spraying of Modern Materials
Edited by
Dr. Artur Czupryński, Dr. Marcin Adamiak, Prof. Dr. Antonín Kříž and Dr. Tünde Anna Kovács
https://doi.org/10.3390/ma15051915
materials
Article
High-Power Diode Laser Surface Transformation Hardening of
Ferrous Alloys
Artur Czupryński 1, * , Damian Janicki 1 , Jacek Górka 1 , Andrzej Grabowski 2 , Bernard Wygl˛edacz 1 ,
Krzysztof Matus 3 and Wojciech Karski 1
1 Department of Welding, Silesian University of Technology, Konarskiego 18A, 44-100 Gliwice, Poland;
damian.janicki@polsl.pl (D.J.); jacek.gorka@polsl.pl (J.G.); bernard.wygledacz@polsl.pl (B.W.);
wojciech.karski@polsl.pl (W.K.)
2 Institute of Physics—CSE, Silesian University of Technology, Krasińskiego 8, 40-019 Katowice, Poland;
andrzej.grabowski@polsl.pl
3 Materials Research Laboratory, Silesian University of Technology, Konarskiego 18A, 44-100 Gliwice, Poland;
krzysztof.matus@polsl.pl
* Correspondence: artur.czuprynski@polsl.pl
Abstract: A high-power direct diode laser (HPDDL) having a rectangular beam with a top-hat
intensity distribution was used to produce surface-hardened layers on a ferrous alloy. The thermal
conditions in the hardened zone were estimated by using numerical simulations and infrared (IR)
thermography and then referred to the thickness and microstructure of the hardened layers. The
microstructural characteristics of the hardened layers were investigated using optical, scanning
electron and transmission electron microscopy together with X-ray diffraction. It was found that
the major factor that controls the thickness of the hardened layer is laser power density, which
determines the optimal range of the traverse speed, and in consequence the temperature distribution
in the hardened zone. The increase in the cooling rate led to the suppression of the martensitic
transformation and a decrease in the hardened layer hardness. The precipitation of the nanometric
Citation: Czupryński, A.; Janicki, D.; plate-like and spherical cementite was observed throughout the hardened layer.
Górka, J.; Grabowski, A.; Wygl˛edacz,
B.; Matus, K.; Karski, W. High-Power Keywords: laser surface transformation hardening; high-power diode laser; ferrous alloys; thermog-
Diode Laser Surface Transformation raphy; cooling rate
Hardening of Ferrous Alloys.
Materials 2022, 15, 1915. https://
doi.org/10.3390/ma15051915
a relatively homogeneous austenite structure in the hardened zone during a very short
period of the laser-induced thermal cycle. This requires notably higher temperatures on
the hardened surfaces than those during conventional hardening to achieve a sufficiently
high diffusion rate for the homogeneous austenitic structure [18]. As a result, to obtain
the desired layer thickness and to avoid partial melting, precise control of the surface
temperature is needed. However, scant data are available on the effect of LSTH parameters
on the thermal conditions during the processing of DCIs and the resulting microstructure
of the hardened layers.
The main objective of this work was to assess the effect of the LSTH parameters on
the thermal conditions in the hardened zone and the resulting change in the thickness and
the microstructure of the surface-hardened layer. The LSTH process was performed on a
pearlitic DCI using a high-power direct diode laser having a rectangular beam with a top-
hat intensity distribution. The thermal conditions in the hardened zone were determined
by using infrared (IR) thermography and numerical simulations. The surface-hardened
layers were characterized in terms of their surface finish, microstructure and hardness.
C Si Cu Mn Cr Ni S P Fe
3.52 2.62 0.80 0.24 0.02 0.04 0.008 0.016 balance
(a) (b)
Figure 1. (a) Optical image showing the microstructure of the as-received DCI grade EN-GJS-700-2;
(b) In-lens SEM image showing the perlite matrix.
The reflectivity of the DCI specimens at room temperature was measured using a
setup comprising an Ocean Optics PC2000-ISA-PC Plug in Fiber Optics Spectrometer
Materials 2022, 15, 1915 3 of 17
(wavelength range 500–1000 nm; resolution: ±0.5 nm), an ISP-REF Integrating Sphere and
a WS-1 diffuse reflectance standard (Ocean Optics Inc., Dunedin, FL, USA). Reflectance
measurements were made using both diffuse and specularly reflected light.
The thermographic measurements were carried out with the use of a FLIR A655SC
thermal camera (Teledyne FLIR LLC., Wilsonville, OR, USA). The camera works in the
7.5–14.0 µm wavelength range and a 16-bit dynamic range at a 50 Hz polling rate and has
an accuracy of ±2% of reading.
The hardening trials were carried out with a high-power direct diode laser (HPDDL)
with a rectangular beam with a top-hat intensity distribution in the slow-axis direction
(HPDDL, Rofin-Sinar Laser GmbH, Hamburg, Germany). The dominant wavelength of
HPDDL used was 808 nm. The HPDDL beam spot size was 1.5 × 6.6 mm (length × width).
The focal plane of the laser optics was located at the DCI specimen and the slow HPDDL
beam axis was set to be perpendicular to the scanning direction. Argon (at a flow rate
of 10 L/min) was used during all hardening trials to prevent oxidation of the surface.
Additional details of the HPDD laser source have been previously given [21]. The selected
hardening conditions are listed in Table 2. The selection of the optimal range of processing
conditions was aimed at avoiding the finish grinding operation in potential industrial
applications. For this reason, the occurrence of partial surface melting was not accepted.
The hardness measurements were performed with a Wilson Wolpert 401 MVD micro-
hardness intender (Wilson Wolpert Instruments, Aachen, Germany). The measurements on
the hardened surface and the polished SHB cross-sections were conducted using 500 g and
100 g loads, respectively.
The laser hardening process was simulated by means of a nonlinear 3D transient
thermal simulation in Visual Weld 16 (Sysweld core-ESI Group). The material database con-
sisted of specific heat and thermal conductivity over the range of 20 ◦ C to the melting point.
– – –
The simulations take into consideration solid-state transformation with the Johnson–Mehl–
–
Avrami–Kolmogorov equation for diffusive transformations and the Koistinen–Marburger
equation for non-diffusive transformation. The equation parameters were chosen to fit the
simulated TTT diagram to the experimental TTT diagram. A 3D Model with 691,620 el-
ements and 187,640 nodes was developed (Figure 2). The dimensions of the developed
3D model were consistent with those of the specimens used in the experimental stage.
The model was prepared in such a manner that where the simulated laser processing took
place, hexa elements with a 0.05 × 0.05 × 0.05 mm size were used, and the rest of the
model was composed of tetra elements with element size increasing with the distance
from the processed area. Only half of the planar symmetrical sample was simulated to de-
crease computational complexity. This did not affect the simulation accuracy. The thermal
boundary conditions were set to free air with a temperature of 20 ◦ C exchange on the outer
surfaces of the model excluding the symmetry plane. The process was simulated with
the usage of a modified load 3D double ellipsoidal heat source proposed by Kik [22]. The
double ellipsoidal heat source dimensions were calibrated to achieve the 800 ◦ C isotherm
dimensions equal to the dimensions of the hardening zone. The heat source parameters
were as follows: length of 1.6 mm, depth of 0.1 mm and load zone width of 6.6 mm. The
results of reflection measurements (Figure 3) were taken into account during the selection
–
of energy input. The final heat source efficiency was in the 0.5–0.6 range.
Figure 3. Spectral reflectance curve for a test plate of the DCI having an average roughness (Ra ) of
approximately 0.05 µm.
3. Results
3.1. Surface Condition Analysis
Figures 4 and 5 show the appearance of the laser hardened surface of the selected
DCI in different processing conditions. The results of the hardness measurements on the
hardened surfaces are listed in Table 2. The laser power level, determining the laser power
density, has a direct impact on the optimal range of the traverse speed. With an increasing
laser power density, the lower limit of the traverse speed, which ensures avoidance of
partial melting, is notably increased (Table 2). The partial melting occurred in the regions
directly adjacent to the graphite nodules and led to the formation of ledeburite eutectic
structures on the processed surface (Figures 4a and 5a). The presence of ledeburite eutectic
regions increased the overall surface hardness of the processed layers (Table 2). Note
that, to avoid finish grinding operations, surface melting is undesirable in transformation
hardening. The surface hardness of the SHB fabricated in the optimal range of parameters
(providing no surface melting) was in the range of 755 to 684 HV0.5. It should be noted that
with increasing traverse speed, the maximum surface hardness decreased. To understand
the effect of the processing conditions on the microstructure and the hardness of the laser
surface-hardened layers on DCI, the next sections present detailed investigations on the
microstructure and hardness of the SHBs produced under processing condition no. H2 and
H8, as well as the thermal conditions in the hardened zone under those two processing
conditions (Table 2).
(a) (b)
)
Figure 4. SEM images of the hardened surface at laser power of 400 W and traverse speed of:
(a) 0.1 m/min; (b) 0.2 m/min.
Materials 2022, 15, 1915 6 of 17
(a) (b)
Figure 5. SEM images of the hardened surface at a laser power of 800 W and a traverse speed of:
(a) 0.4 m/min; (b) 0.6 m/min.
(a)
(b)
Figure 6. Optical macrographs of the SHBs no. (a) H2; (b) H8 (Table 2).
Materials 2022, 15, 1915 7 of 17
(a) (b)
Figure 7. Low magnification optical micrographs of the SHB no. (a) H2; (b) H8 (Table 2). Dashed
lines indicate an approximate boundary between the hardened layer and the core material.
(a) (b)
Figure 8. Optical micrographs showing the undersurface area of the SHB (in the center of the bead)
no. (a) H2 (hardened layer and transition boundary) and (b) H8 (hardened zone) (Table 2).
The micrographs in Figure 7 suggest that the thickness of the hardened layer was
approximately 60 and 200 µm for conditions no. H2 and H8, respectively. Based on the
optical micrographs presented in Figure 8, one can observe that the microstructure of the
hardened layer is composed of graphite nodules and the martensitic matrix. The XRD
analysis indicated the additional presence of the retained austenite phase in the matrix of
the hardened layer produced under processing condition no. H8 (Figure 9c). Note that
the retained austenite fraction in the hardened layer produced under processing condition
no. H2 was negligible (Figure 9b). Moreover, XRD patterns from all hardened layers gave
peaks that can be identified as belonging to the cementite phase.
Materials 2022, 15, 1915 8 of 17
(a)
(b)
(c)
Figure 9. XRD patterns of the (a) as-received DCI and after the LSTH under conditions no. (b) H2 and
(c) H8 (Table 2).
SEM investigations (Figures 10 and 11) indicated that the hardened layer can be di-
vided into two sub-regions: the region of complete dissolution of cementite lamellae and the
region of partial dissolution of cementite lamellae. Directly beneath the hardened surface,
there was a region exhibiting a complete dissolution of cementite lamellae (Figure 11a). The
thickness of this region was approx. 22 and 135 µm in the SHB no. H2 and H8, respectively.
The microstructure of this region was composed of the graphite nodules and the martensitic
matrix (the martensitic/austenitic matrix in the case of SHB no. H8). The region of the
hardened layer adjacent to the core material had a matrix that was, in general, composed
of partially dissolved cementite lamellae and fine martensite laths (Figure 11b,c). The
thickness of the region of partial dissolution of cementite lamellae was approx. 39 and
61 µm in the SHB no. H2 and H8, respectively.
Materials 2022, 15, 1915 9 of 17
(a) (b)
Figure 10. In-lens SEM images taken from the undersurface area of SHB no. (a) H2 and (b) H8
(Table 2).
(a) (b)
(c)
Figure 11. In-lens SEM images taken from the SHB no. H8 (Table 2) showing: (a) the region of
complete dissolution of cementite lamellae; (b) the region of partial dissolution of the cementite
lamellae; (c) a boundary between the region of partial dissolution of the cementite lamellae and the
core material.
40 nm (Figure 12c). Both types of nanometric cementite precipitates were observed at the
martensite lath boundaries. Further research will be required to clarify the mechanism of
cementite precipitation during the investigated LSTH process.
(a) (b)
(c) (d)
Figure 12. (a) Dark-field and (b) bright-field STEM HAADF images showing a distribution of plate-
like (P) and spherical (S) cementite precipitates formed in the matrix of the SHB no. H8 (the region of
complete dissolution of the cementite lamellae); (c) Bright-field TEM image taken from a marked area
in (a); (d) SAED pattern obtained from region (1) in (a).
Materials 2022, 15, 1915 11 of 17
(a) (b)
(c) (d)
Figure 13. (a) Dark-field and (b) bright-field STEM HAADF images showing spherical (S) cementite
precipitates formed in the matrix of the SHB no. H8 (the region of complete dissolution of the
cementite lamellae); (c,d) SAED patterns obtained from regions (1) and (2), respectively, in (a).
Figure 14. Hardness profiles of the SHBs no. H2 and H8 (Table 2).
(a) (b)
Figure 16. Temperature profiles for the hardened surface in (a) the longitudinal (along the SHB cen-
terline) and (b) traverse directions (along the slow-axis of the HPDDL beam). Processing conditions
no. H2 (Table 2).
(a) (b)
Figure 17. Temperature profiles for the hardened surface in (a) the longitudinal (along the SHB cen-
terline) and (b) traverse directions (along the slow-axis of the HPDDL beam). Processing conditions
no. H8 (Table 2).
Figure 18. Calculated temperature fields in the cross-section of the SHB (a half of the bead) no.:
(a) H2, (b) H8 (Table 2).
Materials 2022, 15, 1915 14 of 17
Figure 19. Calculated temperature distributions beneath the surface of the SHB (along the central
vertical plane) under processing conditions no. H2 and H8 (Table 2).
The thermal data indicated that the maximum temperature on the hardened surface
(on the SHB centerline) was about 1000 and 1100 ◦ C for processing conditions no. H2 and
H8, respectively. The average heating rate for the above two cases was 2300 and 8500 ◦ C/s,
respectively. The time spent above the critical temperature (i.e., the matrix structure
becomes entirely austenitic; assuming approximately 800 ◦ C) for processing conditions
no. H2 and H8 was 0.33 and 0.14 s, respectively. The average cooling rate within the
temperature range –of 800–500 ◦ C for processing conditions no. H2 and H8 was 1300 and
3400 ◦ C/s, respectively. The thermal data errors due to simplification of the modelled
process, limited mesh density, idealisation of the simulation and variety of emissivity
of the sample can be present. Although small deviations between the simulation and
thermographic experimental measurements are present, their convergence is high, which
increases the confidence of investigated thermal parameters.
4. Discussion
The laser power density, determining the optimal range of the traverse speed (ensuring
no surface melting), had a direct impact on the hardened layer thickness. The power density
for processing conditions no. H2 and H8 was 40.4 and 80.8 W/mm2 , respectively. Despite
a notably lower HI level (80 J/mm), the processing condition no. H8 provided an almost
3.5 times higher thickness of the hardened layers in comparison to that achieved under the
processing condition no. H2 (HI = 120 J/mm). Similar relationships between the processing
parameters and the hardening depth have been reported for LSTH of different grades of
steel [23,24]. It should be noted that the maximum hardness produced in the hardened layer
was affected by the traverse speed. The increase in the traverse speed led to a reduction in
the maximum layer hardness. Comparing the surface hardness of the SHBs no. H2 and
H8 shows that the lower traverse speed (0.2 and 0.6 m/min for H2 and H8, respectively)
provided about 10% greater surface hardness (Table 2). This trend of decreasing hardness
with increasing traverse speed is associated with an increase in the cooling rate and the
resulting suppression of the martensitic transformation. The lower hardness of SHB no. H8
(651 HV0.1, Figure 14) in comparison to that of SHB no. H2 (755 HV0.1) is attributed to the
presence of the retained austenite phase. The suppression of the martensitic transformation
under non-equilibrium cooling conditions has been reported in several works on the casting
and surface treatment of different cast iron grades [25,26]. It indicates that, from the point of
view of the maximum surface hardness, the lower traverse speeds, ensuring lower values of
the cooling rate, are beneficial in producing more wear-resistant layers [27,28]. On the other
hand, to avoid surface melting with increasing power density, the elevation of traverse
speed is required. The above results show that both the laser power density (determined by
the laser power level and laser spot size used) and the traverse speed are equally important.
Materials 2022, 15, 1915 15 of 17
5. Conclusions
Surface-hardened layers were produced on ductile cast iron via laser surface transfor-
mation hardening. The laser source used was a high-power direct diode laser having a rect-
angular beam with a top-hat intensity distribution. The thermal conditions in the hardened
zone were examined by using numerical simulations and infrared (IR) thermography. The
results showed that the major factor controlling the thickness of the hardened layer is the
laser power density, which determines the optimal range of the traverse speed and in con-
sequence the maximum surface temperature. The hardening depth was found to increase
with increasing power density. To avoid surface melting with increasing power density,
the lower limit of traverse speed notably increases. The resulting increase in the cooling
rate led to a suppression of the martensitic transformation and a decrease in the hardened
layer hardness. In the investigated range of the laser power density (40.4–80.8 W/mm2 ),
the maximum hardening depth was approx. 200 µm. The hardness in the hardened layer
was increased by almost three times in comparison with the as-received condition.
Author Contributions: Conceptualization, A.C. and D.J.; methodology, A.C., D.J., J.G., A.G., B.W. and
K.M.; formal analysis, A.C., D.J., J.G., A.G. and B.W.; investigation, D.J., A.C., A.G., B.W., K.M. and
W.K.; resources, A.C. and D.J.; writing—original draft preparation, A.C. and D.J.; writing—review
and editing, A.C. and D.J.; visualization, A.C., D.J. and B.W.; supervision, A.C. and D.J.; project
administration, A.C. and D.J.; funding acquisition, D.J. and A.C. All authors have read and agreed to
the published version of the manuscript.
Funding: The research was funded by the Silesian University of Technology Rector’s habilitation
grant 10/050/RGH_20/1006 and pro-quality grant 10/050/RGJ_22/1029.
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.
Materials 2022, 15, 1915 16 of 17
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