Surface & Coatings Technology 328 (2017) 344–354

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Surface & Coatings Technology

journal homepage: www.elsevier.com/locate/surfcoat

Microstructure related enhancement in wear resistance of tool steel AISI

D2 by applying laser heat treatment followed by ultrasonic
impact treatment
D.A. Lesyk a, S. Martinez b, B.N. Mordyuk c,⁎, V.V. Dzhemelinskyi a, А. Lamikiz b, G.I. Prokopenko c,
Yu.V. Milman d, K.E. Grinkevych d
a
Department of Laser Systems and Applied Technologies, National Technical University of Ukraine “Igor Sikorsky Kyiv Polytechnic Institute”, 37 Peremohy ave., UA-03056 Kyiv, Ukraine
b
Department of Mechanical Engineering, University of the Basque Country, Alameda Urquijo s/n, SP-48013 Bilbao, Spain
c
Department of Physical Fundamentals of Surface Engineering, Kurdyumov Institute for Metal Physics, NAS of Ukraine, 36 Academician Vernadsky blvd., UA-03142 Kyiv, Ukraine
d
Department of Physics of Metastable Alloys and High-Strength Materials Destruction, Frantsevich Institute for Problems of Materials Science, NAS of Ukraine, 3 Krzhizhanovsky st., UA-03142 Kyiv,
Ukraine

a r t i c l e i n f o a b s t r a c t

Article history: The surface layers of tool steel AISI D2 were modified by laser heat treatment (LHT) conducted using the solid
Received 18 May 2017 state fiber-laser, by ultrasonic impact treatment (UIT) and by the combined LHT + UIT process. The paper is
Revised 1 August 2017 focused on the establishing the correlation between the microstructure, hardness and wear resistance of the
Accepted in revised form 19 August 2017
modified layers. XRD analysis and TEM observations show that the LHT process results in the formation of micro-
Available online 24 August 2017
structure comprised submicronic ferrite/austenite grains, martensitic needles and secondary carbides while the
Keywords:
combined LHT + UIT process leads to the formation ultra-fine grained structure (~ 80–250 nm) with grain
Laser heat treatment boundaries fixed with fine secondary carbides (~20 nm), and some areas of martensitic feathers. The observed
Ultrasonic impact treatment microstructural features and phase compositions are shown to affect the wear resistance of the AISI D2 steel
Tool steel surface measured both in quasi-static and dynamic conditions. The modified layers demonstrate almost double,
Microstructure triple and four times decrease in the wear losses in dynamic conditions with regard to the initial surface after the
Hardness LHT, UIT, and combined LHT + UIT processes, respectively. Theoretical evaluations of the wear resistance W−1th
Wear using the Archard expression correlate well with the experimental data W−1exp, especially when the local
plasticity characteristics δН describing the retained plasticity was taken into account.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction means of the structure modifications and phase transformations related

The reliability and durability of die tools are largely provided with
both the surface microrelief and microstructure/phase composition of
tool steels. These characteristics determine the hardness of the surface
layers, which undergo the most significant loads during the operation
life [1]. The working surfaces of tools are exposed to impact loads of
highly concentrated stresses. As a consequence, the surface layers be-
come the weakest sites prone to thermal or mechanical fatigue, oxida-
tion and mechanical wear, especially at the elevated temperatures.
Therefore, the enhanced wear resistance of the working surfaces of
tool steels is currently a goal of high topicality in mechanical
engineering.
Laser treatment is one of the most common methods for surface
modification. It can be used for the laser heat treatment (LHT) of the
surfaces of the end-products [1–5], which results in the hardening by
⁎ Corresponding author.
E-mail address: mordyuk@imp.kiev.ua (B.N. Mordyuk).
to the formation of fine-grained martensitic structures [2–9] and fine
carbides [2,5]. Additionally, the surface layers can be restored owing
to the LHT induced alloying/cladding [3,5,7–11]. A lot of studies regard-
ing the impact of laser radiation on the structure and properties of tool
steels can be found in the literature [6,8,10], which however mainly de-
voted to laser melting treatment [5,7–10]. In particular, the authors of
[5] have shown that the melting zone was characterized by the reduced
microhardness due to complete dissolution of carbides and a significant
increase in the volume fraction of the retained austenite. It was there-
fore suggested to perform LHT of highly alloyed steels without or with
a minimal melting of superficial microasperities [12]. The influence of
LHT on the wear resistance of tool steels was also analyzed [13,14].
However, the outcomes of the LHT performed using a fiber laser and
scanner without melting of the surface layer were addressed insuffi-
ciently [15,16].
Recently, to reduce mechanical wear of metallic products by the hy-
brid processes consisted of the laser-mechanical hardening [17],
alloying [18,19], cladding [11] and severe plastic deformation (SPD)

http://dx.doi.org/10.1016/j.surfcoat.2017.08.045
0257-8972/© 2017 Elsevier B.V. All rights reserved.
 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
attracted more attention. When the plastic straining of the surface is im-
plemented at the cooling stage of the subsurface layers previously heat-
ed to the austenitization temperature [20], then it promotes the
simultaneous improvement of the parameters of the surface microrelief
and the formation of ultra-fine grained microstructure in the surface
layer, which may possess an enhanced microhardness, increased plas-
ticity, and compressive residual macrostresses [12,18]. It was shown
that previous heating promotes plastic deformation to higher extents
owing to the temporary softening of the material [12,20].
Another technological solution is to apply the SPD methods after the
laser hardening [21–24]. Ultrasonic burnishing treatment [21,22], ultra-
sonic impact treatment [16,23] or shot peening [24], and surface me-
chanical attrition treatment (SMAT) [25] are the most common
dynamic SPD methods, which were used to remove possible disadvan-
tages of LHT.
Use of LHT followed by roller-burnishing resulted in more
fragmented grain structure and in a higher increase in the surface hard-
ness and wear resistance as compared to the solely applied LHT. For in-
stance, the wear resistance and friction coefficient of steel AISI 420 were
significantly increased using such a hybrid treatment [2,12]. It was
shown that the combined (hybrid) laser-mechanical process for surface
hardening is effective for improvement of the wear resistance of both
small [21,22] and large [16,19,23,24] parts made of tool steel. Though,
the laser transformation hardening combined with shot peening does
not provide uniform hardening depth and regular surface microrelief
[24].
This work is aimed to evaluate the wear and friction behaviours of
the tool steel AISI D2 hardened by laser heat treatment, ultrasonic im-
pact treatment and laser heat treatment followed by ultrasonic impact
treatment by means of the quasi-static and dynamic wear tests. The
special attention was given to identify the correlation between the
wear resistance and hardness of the surface layers both caused by
microstructural and phase transformations induced by thermal (LHT)
and deformation (UIT) hardening.
2. Experimental procedures
2.1. Material
The AISI D2 tool steel often employed for production of the parts
working in extreme conditions and contained high contents of chromi-
um and carbon was studied in this paper. The nominal chemical compo-
sition of the steel given in wt% is the following: 11.5% Cr, 1.5% C, 0.83%
Mo, 0.72% V, 0.46% Mn, 0.42% Si, 0.15% Ni, 0.06% Cu and balance Fe.
Specimens were machined in the plate shape of 69 × 9 × 69 mm.
Prior to the laser and ultrasonic treatments, the specimens were
subjected to annealing at 850 °С, then they were slowly cooled in the
furnace to 650 °C (10 °C per hour), and then they were cooled in the
Fig. 1. General views of equipment and schemes for LHT (а) (Vsc is scanning speed, bsc is the track width, S is the feed rate of specimen) and UIT (b) (Fs is static loading of head, Ausv and fusv
are the vibration amplitude and frequency of ultrasonic horn, S is the specimen feed rate, nt is the rotation frequency of the head, Rt is the distance between the pin and the head rotation
axis, ωt is the rotational speed of the pin).
345
ambient air. The original structure of the steel after heat treatment
contained the alloyed α-ferrite and carbide phases.
2.2. Treatment details
2.2.1. Laser heat treatment
Preliminary the LHT process was performed by single passes without
overlapping of the laser tracks to avoid formation of the over-tempered
microstructures with inhomogeneous and reduced hardness in the o-
verlapped areas [26]. Then, the laser hardened surfaces were subjected
to ultrasonic strain hardening taking into account that the UIT produced
track completely covers the LHT induced one.
The LHT process was implemented using a strategy of the remote
surface hardening (Fig. 1(a)) using a machine tool with numerical con-
trol specially designed for laser processing of the material surfaces. A
solid state fiber laser Rofin Sinar FL010 of 1 kW power output and of
1.064 μm wavelength was used to heat treatment of the specimens. A
focusing head (scanner) produced by SCANLAB was mounted on the
machine tool as shown in Fig. 1(a), which work area is 120 × 120 mm.
The laser beam was guided to the focusing head by an optical fiber
that provides a beam diameter of 100 μm. The focal plane was adjusted
to obtain a defocused laser spot of dlb = 1 mm on the specimen surface.
Then, the track of the required width (bsc = 10 mm) and length
(60 mm) was treated using the same scanning parameters (the scan-
ning speed Vsc along the width bsc) of the laser beam controlled by spe-
cial software [16] and by the chosen feed rates S of specimen,
respectively.
The LHT process was performed using a strategy of constant heating
temperature, which was controlled by means of a digital proportional-
integral-differential (PID) controller and infrared pyrometer Impac
Igar 12LO. In particular, the surface temperature in real time was mea-
sured without contact by two-spectral radiation that gives the actual
value of the surface temperature. Then, the measured surface tempera-
ture was delivered through the PID controller to a special board that
transforms the digital signal into the analogous signal inducing the
required laser power needed to maintain a constant temperature in
the area affected by the laser beam [27].
The appropriate heating temperature range was previously deter-
mined taking into account the ternary iron carbon chromium phase
diagram and the magnitudes of the laser power density, as well as the
thermo-kinetic [28] and thermo-physical [29] models, the limiting
maximum of the heating (surface) temperature (AC3 b Т (°С) b Тm)
and the duration of the laser action (0.01 b tl (s) b 1.5) that provide a
thermal hardening without melting of the surface.
In the present work, the experimental results of the laser surface
hardening of tool steel AISI D2 are given for the heating temperature
of T = 1270 °C, the scanning speed Vsc = 1000 mm/s, the laser track
width bsc = 10 mm, and specimen feed rate S = 40…140 mm/min. At
346 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354

Table 1 The surface hardness of the specimens was determined using a

Laser heat treatment parameters. Computest SC digital tester at a load on indenter of 10 N and a dwell
T S dlb Vsc bsc tlb tLHT ELHT time of 3 s and microhardness in the near-surface layers was registered
(°С) (mm/min) (mm) (mm/s) (mm) (s) (s) (kJ/cm2) using a FM800 digital tester at a load on Vickers indenter of 0.5 N and
1270 40 1 1000 10 1.50 90 78 dwell time of 12 s was used for all the measurements. The microhard-
90 0.66 40 40 ness of the surface layer (surface hardness) was determined as average
140 0.42 25 29 magnitude based on the results of 4–5 measurements. The depth profile
of microhardness in the heat affected zone was defined by the results on
the base of measurements.
these regimes, the magnitudes of the energy density of laser beam ELHT, The hardening intensity gradients in the surface layers of 25, 50 and
specific duration of the laser beam action tlb, and overall LHT duration 100 μm thickness were calculated by the following ratio:
tLHT are given in Table 1.
Ihard ¼ ðHVhard −HVin Þ=hhard ; ð1Þ

2.2.2. Ultrasonic impact treatment

Ultrasonic surface hardening was realized using a machine tool with
numerical control, ultrasonic generator (with a frequency fusv of
21.6 kHz and a power output of 0.3 kW), ultrasonic vibration system
and electromotor [16]. The ultrasonic oscillatory system contained a
piezoceramic transducer, step-like horn and impact head with seven
cylindrical pins producing impacts with frequency fi [30]. These pins
were made of steel AISI 52100 and their shapes were the rods of 5 mm
in diameter and 18 mm in length. During the UIT process, the ultrasonic
vibration system was loaded to the treated surface by a static force Fs,
and multiple-pins head was forcedly rotated by the motor with the rota-
tion speed ωt. The scheme of the UIT loading unit is shown in Fig. 1(b).
Based on the previous experimental studies, the range of the vibra-
tion amplitudes Ausv of ultrasonic horn in (15–18 μm), the UIT duration
t (60…240 s), and the limiting static loading Fs of the ultrasonic vibra-
tion system (30 b Fs (N) b 100) to the treated specimen were adopted
[16]. The UIT parameters are listed in Table 2. The UIT duration t =
120 s (S = 600 mm/min) was chosen to be optimal. For this regime,
the specific mechanical energy applied EUIT to the specimen by ultrason-
ic tool was estimated to be ≈53 mJ (Table 2).
2.3. Structure and hardness examinations
The X-ray diffraction (XRD) analysis of the surface layers of about
10…20 μm thick was carried out using a DRON-3M diffractometer in ra-
diation Cukα with a graphite monochromator. To estimate the peak
broadening β the registered diffraction peaks were fitted with Pseudo-
Voigt function using Origin Pro 8 software, and the width, intensity
and the centroid position of the fitted peaks were obtained and ana-
lyzed. The changes of β were analyzed to evaluate the lattice
microstrains and the size of the coherent scattering areas (CSA). The
treatment induced macrostresses were also estimated by analyzing
the angular positions of the diffraction peaks.
The cross-sections of the treated specimens were mechanically
polished and chemically etched using a 4% Nital reagent to reveal the
grain boundaries and carbides' distribution. Analysis of the microstructure
in the near-surface layers was carried out using Nikon Optiphot-100 opti-
cal microscope. A JEOL-CX-II 100 transmission electron microscope (TEM)
was also used to observe the microstructures of the samples. The plane-
view TEM foils from the sub-surface layer ~10–15 μm below the outmost
surface were analyzed. They were prepared by mechanical polishing of
the sample on the untreated side until it was about 30 μm in thickness
and then by one-side electro-polishing using a twin-jet technique.
Table 2
Ultrasonic impact treatment parameters.
Fs (N) Ausv (μm) fusv (kHz) fi (kHz) ωt (rpm) tUIT (s) EUIT (mJ/cm2)
50 18 21.6 2±1 76 60 26
120 53
180 77
240 105
where HVin and HVhard are the microhardness magnitudes of the origi-
nal and modified layers (MPa), respectively, hhard is the thickness of the
considered layer possessing enhanced hardness (μm).
The local plasticity characteristic δН as a fraction of the plastic strain
in the total elastoplastic strain (the ability of the material to plastic de-
formation) was determined by the indentation method by a Vickers py-
ramidal indenter according to the formula [31–33]:

HV
δH ¼ 1−14:3 1−ν−2ν 2 ; ð2Þ
E
where HV is the microhardness of the surface layer (GPa), ν is the
Poisson coefficient, E is the Young's modulus (GPa).
2.4. Wear tests
Considering a wide application of the studied steel for production of
stamps or cutting tools working usually under cyclic loads, wear tests of
the hardened surfaces were carried out using an automated tribolog-
ical complex at the quasi-static and dynamic loading conditions
(Fig. 2(a)). A detailed description of the used equipment is given
elsewhere [34–36]. The quasi-static tests (at a constant load Fs =
30 N applied to the WC-Co indenter (hardness of 94 HRA)) were per-
formed by reciprocating sliding of the indenter (8 mm in diameter)
with the frequency of ~ 1 Hz along the track of 4 mm. Two types of
tests lasted for 15 min (~ 950 cycles) and 45 min (~ 2850 cycles)
were performed. Eight duplicate runs were conducted for each
wear condition (each material) studied, and then statistically aver-
aged. The variable of the test method was not exceed 4%. In the
dynamic conditions, the wear tests were implemented along the
track of the same length by means of the application of the same stat-
ic load F s plus additional dynamic load applied in a sinusoidal
manner (with the frequency of 25 Hz and amplitude of ΔF ~ 3 N).
All the tests were conducted at the sliding speed of 0.013 m/s that
was sustained to be constant during each half-cycle outside the
transient stages around the turning points owing to the used cam
mechanism of Archimedes' spirals shape (14 in Fig.2a). In addition,
all the tests were carried out at room temperature (20 °C) in ambient
atmosphere.
After each test, the magnitude of the wear loss WL (the depth of the
wear track) was evaluated by measuring the surface topography
(Fig. 2(b)) and profile (Fig. 2(с)) across the worn track using the optical
profilometer Leica DCM3D [16]. The friction force F was determined
using the data recorder connected to the induction transducer and the
displacement sensitive elastic element.
The theoretical magnitude of the wear resistance W−1 R of the hard-
ened layer, which is inversely proportional to the wear loss magnitude
WL (estimated as a worn volume in mm3) according to the Archard
expression, was evaluated using the formula [34]:
HV
W −1
R ¼ ; ð3Þ
KF s l
 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354 347

Fig. 2. Scheme of the automated tribological complex (a) consisting of frame (1), transducer (2), clip (3), two pairs of balls (4), the stand with a slide (5), support (6), ring spring (7), flat
sample (8), indenter (9), stock (10), set of weights (11), pair of springs (12), lever (13), the cam mechanism (14), and the carriage (15), 3D texture (b) and 2D texture (c) of the worn track
after dynamic test (hW is the magnitude of the wear loss WL).

where HV is the microhardness hardened layer (N/mm2), K is the wear
coefficient, Fs is the static load (N), and l is the length of the worn track
(mm).
3. Experimental results
3.1. Hardening of heat/strain affected zones
To achieve the increased wear resistance it is of great importance to
enhancing not only the hardness magnitude HV of the modified layer,
which according to the Archard expression (Eq. (3)) is inversely propor-
tional to the wear. The thickness h of the hardened layer should also be
enlarged. The preparative experiments carried out in this study allowed
determining the optimum regimes of the LHT and UIT processes in the
view of the HV to h ratio. The latter varies depending on the set temper-
ature and the feed rate of the treated specimen at the LHT process, on
the one hand, and depending on the duration of the UIT process applied
to the specific surface area (the number of impacts per unit area), on the
other hand. After different regimes of the LHT and UIT processes, the op-
tical images of the microstructure in the cross-sections of the specimens
(Fig. 3), which were made along the central axis of the treated track (Fig.
1(a)), were also analyzed.
The results show that the hardening zone is formed owing to ther-
mal influence (Fig. 3(a–d)). The LHT induced transformation hardening
of the studied tool steel occurs due to rapid heating to a temperature
slightly below the melting temperature followed by rapid cooling. The
increase of the scanning speed of the laser beam applied to the treated
surface from 40 to 140 mm/min leads to the reduction of the thickness

Fig. 3. Hardened zones in the surface layers of tool steel AISI D2 after the LHT (1270 °С) (a–d) and UIT (e–f) processes: а) LHT at S = 40 mm/min, b) LHT at S = 90 mm/min, c) LHT at S =
140 mm/min, e) UIT for t = 60 s, f) UIT for t = 120 s, g) UIT for t = 180 s.
348 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
Fig. 4. Dependences of the hardness magnitudes (1, 2) and thickness of the hardened layer
(3, 4) of tool steel AISI D2 on the feed rate at LHT (1270 °С) (1, 3) and on the duration of
the UIT (2, 4) and combined LHT + UIT (5) processes.
of the hardened layer from 380 to 240 μm with only slight increase in
the microhardness magnitudes (Figs. 3(a–c), 4). In view of the HV to h
ratio, the optimum regime of the LHT process applied to the tool steel
AISI D2 is the heating temperature 1270 °C and the specimen feed rate
of 90 mm/min (Figs. 3(b), 4).
The increase of the UIT process duration also leads to the surface
hardening and to the increase in the thickness of the deformed layer
(Figs. 3(е–h), 4). However, both the hardness magnitude (~29.5 HRC)
and the thickness of the hardened layer (60…80 μm) after UIT treatment
for 120 s are smaller than those produced by the LHT process (see the heat
affected zone (HAZ) indicated in Fig. 3(d) and the strain affected zone
(SAZ) shown in Fig. 3(h). At the same time, the prolonged UIT process
(for 150–180 s) can lead to overstraining, which manifests itself with
the formation of the pores and cracks that can coagulate, form the breaks
and delaminations of the deformed layer (Fig. 3(g)). As a result, the hard-
ened layer with such defects can even deteriorate the wear resistance sur-
face because of the destruction of the friction surface and removal of the
wear products. Therefore, it is inappropriate to continue the UIT process
despite some increase in the surface hardness and hardening depth due
to the beginning of irreversible destruction processes in the overstrained
material. Moreover, the over-processing above the optimum duration can
lead to the crack formations and intensive wear at the test/operation.
Fig. 5 compares the magnitudes of the surface hardness HRC (curve
2) and microhardness HV0.05 (curve 1) of the layers modified by optimal
LHT (T = 1270оС, S = 90 mm/min), optimal UIT (Ausv = 18 μm, tUIT =
120 s), and the combined LHT + UIT processes with those of the initial
state. A good correlation of both the curves should be noticed. In com-
parison with the UIT process, which causes surface strain hardening
by 40…50% with regard to the initial state, the LHT process leads to
Fig. 5. Microhardness HV (1), surface hardness HRC (2), local plasticity characteristics δН
(3) and hardness intensity gradient Ihard (4–6) for the layer thicknesses of 25 μm (4), 50
μm (5) and 100 μm (6) for the initial and LHT, UIT and LHT + UIT processed specimens
of tool steel AISI D2.
more significant surface hardening that relates to the structure and
phase transformations under conditions of the limited diffusion during
rapid heating/cooling of the material. The finishing UIT of the LHT hard-
ened layer leads to a slight increase in the hardness (lower than that in
the case of the UIT processing of the initially annealed specimen).
Fig. 5 also shows a curve describing the change of the local plasticity
characteristics δН (curve 3) calculated using the expression (2). A reduc-
tion in the δН magnitude after LHT indicates more depletion of the mate-
rial plasticity in the LHT modified surface layer in comparison with those
in the initial and UIT processed states. Thus, the predisposition of the mod-
ified layers to a brittle destruction would be increased at the UIT finishing
process or at subsequent wear tests. The dependences of the hardness in-
tensity gradient Ihard presented in Fig. 5 (curves 4–6) can also characterize
the effectiveness of the surface treatment used in view of the HV to h ratio
of the modified layers. It is seen that the Ihard after the combined LHT
+ UIT process remains high enough in the surface layers of various
thicknesses up to 100 μm (Fig. 5, curves 4–6). Thus, in view of the hard-
ness intensity gradient, the LHT and combined LHT + UIT processes
would result in the longest operation life of the processed product.
3.2. XRD and TEM observations of surface microstructures
The presented dependences of hardness achieved after different sur-
face treatments correlate well with the data related to the structure and
phase state of the modified layers obtained using XRD (Fig. 6) and TEM
(Figs. 7, 8) analysis. A comparison of XRD spectra shows that the chang-
es of phase composition occur in the surface layers of the studied steel
(thickness is ~ 10…20 μm). In the XRD spectrum of the initial surface
(Fig. 6(a), spectrum 0) the lines of trigonal chromium carbide Cr7C3
and/or a complex carbide (Cr,Fe)7C3, as well as traces of austenite, are
observed additionally to the lines of α-phase. According to XRD analysis,
the total volume fraction of the carbides is about 5% that is slightly
smaller than the magnitude (~10%) estimated using the optical images
of the microstructure in the cross-sections of specimens (Fig. 3). The
volume fraction of austenite is about 8%. An oxide layer is formed after
the LHT process (Fig. 6(a), spectrum 1), which contains a number of
the iron (FeО, Fe2О3, Fe3О4) and chromium (Cr2О3) oxides. The rather
large thickness of the oxide layer masks the reflections from other
phases (ferrite, austenite and carbides) and leads to appeared reduction
of the intensities of their peaks. The combined LHT + UIT process causes
a significant decrease in the intensity of the diffraction peaks related to
oxides and carbides (Fig. 6(a), spectrum 2). The lower peak intensities
are associated especially with the destruction of the oxide film as well
as with the deformation effects. Detail analysis of (211)α diffraction
maximums in the spectra registered for the LHT (Fig. 6(b)) and LHT
+ UIT (Fig. 6(c)) specimens shows that they are splitting on two
submaximums (112)αT and (211)α, i.e. a lot of martensitic phase is
formed in the surface layers of these specimens. These data well corre-
late to the TEM observations of these specimens (Fig. 8(b), (d)).
Analysis of TEM images of the microstructure of tool steel AISI D2
shows that in the initial state (Fig. 7(a)) the alloyed ferrite is character-
ized by insignificant dislocation density (~108 cm−2). Besides, it con-
tains a large number of light areas of significantly smaller thickness
than that of a whole foil. They were seemingly formed in the sites
where the chromium carbides were etched and pulled out. These
areas and the carbide particles remained in the field of view indicate
that the size of primary carbides is about 350 nm. Selective area electron
diffraction (SAED) pattern contains the system of carbide reflexes (indi-
cated by white arrows). It should be mentioned that the small spherical
carbides are considered here. They are located in the alloyed ferrite in
addition to the large strip-like carbides that were observed in the optical
images of the cross-sections of specimens (Fig. 3).
The UIT process inducing SPD leads to a significant increase in dislo-
cation density (1010 cm−2) and some reduction in the size and number
of carbides in the microstructure of the surface layer of 15…20 μm thick.
The latter may be associated with the strain induced dissolution of
 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
Fig. 6. X-ray diffraction profiles (a) of the initial (1) and the LHT (2) and LHT + UIT
processed (3) specimens of the tool steel AISI D2 and martensite doublets (112)/(211)
after LHT (b) and LHT + UIT (c) processes.
Fig. 7. TEM images of the microstructure and electron diffraction patterns of the tool steel AISI D2 in the initial state (a) and after UIT process (b) .
349
carbon from the carbide particles in the ferrite matrix. The dense dislo-
cation nets are seen in the subgrains of the alloyed ferrite, which size is
~0.8 μm (Fig. 7(b)). The increase in the number of defects in the crystal
structure (the dislocation density, number of vacancies, etc.), as well as
the fragmentation of grains and carbides (Fig. 3(h)), manifest them-
selves in the increase of the surface hardness HRC and microhardness
HV of the surface layer. After UIT, this increase is about 40…50% in com-
parison with the initial specimen (Figs. 4, 5).
After LHT, the surface layer of this steel contains two types of struc-
tures. The most typical is the fragmented grain structure with many fine
secondary carbides (~150 nm) and some quantity of primary carbides
on the grains/subgrains boundaries (Fig. 8(a)). The dislocation density
does not high inside the most grains. The existence of the carbide phases
is also confirmed by the reflexes on the SAED pattern. In some areas, the
systems of elongated grains of martensitic nature (~ 250 nm) are ob-
served (Fig. 8(b)). The observed structural and phase transformations
induced by LHT provide the ~2.5 times increase in the surface hardness
HRC (Figs. 4, 5) as compared to the initial state.
The combined LHT + UIT process of the studied steel leads to the
formation of ultra-fine grained structure (~ 80–250 nm) with grain
boundaries fixed by many fine secondary carbides (~ 20 nm)
(Fig. 8(c)). The existence of a large number of highly misoriented grains
in the structure of the surface layer is confirmed by the significant azi-
muthal dispersion of the ferrite diffraction spots in the SAED pattern.
An additional factor of the hardening is the increased dislocation density
inside grains/subgrains. Somewhere, the systems of the elongated mar-
tensitic grains are observed (Fig. 8(d)), which are similar to those regis-
tered in the LHT-processed layer (Fig. 8(b)).
The formation of the ultra-fine grained structure with the grain
boundaries fixed by the fine carbides together with the high density of
dislocations and their bundles result in a maximum increase of the micro-
hardness value (~8 GPa) and can provide the highest wear resistance,
which will be considered in the next section. This result is consistent
with the data reported for the tool steel SKD11 nanostructured by the
combination of laser melting and friction stir processing (FSP) [37]. A
nanometer-sized microstructure (grain size: ~200 nm) containing fine
M7C3 carbide (particle size: ~100 nm) had an extremely high hardness
of ~9 GPa in spite of the high amount of retained austenite.
3.3. Wear and friction behaviours
The tribological tests of the hardened surfaces of tool steel AISI D2
were carried out in different regimes (quasi-static and dynamic condi-
tions) for 15 and 45 min. The experimental magnitudes of wear losses
were determined by analyzing the surface profile and topography of
the worn tracks using laser confocal microscopy.
350 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
Fig. 8. TEM images of microstructure and SAED patterns of the LHT (a, b) and combined LHT + UIT (c, d) processed specimens of the tool steel AISI D2.
Fig. 9 shows the 3D micrographs of the worn tracks on the modified
surfaces of tool steel AISI D2 after testing for 45 min at different test re-
gimes (quasi-static and dynamic tests). It is seen that after dynamic test
the depth of the worn tracks is always larger regardless the surface
treatment used. Moreover, the depth of the worn tracks is reduced
after the LHT (Fig. 9(b, e), 10) and combined LHT + UIT (Fig. 9(c, f),
10) processes in comparison with those for the initial (Fig. 2(b, c), 10)
and UIT processed (Fig. 9(a, d), 10) specimens.
The experimentally registered wear losses WL after quasi-static and
dynamic tests lasted for 15 and 45 min are given in Fig. 10. Generally,
the results of the wear tests of both types demonstrate that all the
used surface treatments result in the decrease of the WL as compared
to the initial state. This observation correlates well with the hardness
behavior. The lowest WL magnitudes were registered after the com-
bined LHT + UIT process. Measured in the quasi-static and dynamic
tests, they are respectively 2 and 4 times lower than those of the initial
state. At dynamic test, the magnitudes of wear loss WL are naturally
higher than those after the quasi-static test owing to the additional
pulse component of the load applied to the indenter during the tests.
Herewith, the dynamically tested WL magnitude for the LHT + UIT-
processed specimen is lower than that of the initial specimen tested in
the quasi-static conditions and four times lower than that of the dynam-
ically tested initial specimen.
An interesting feature is observed after the quasi-static test for
15 min. In spite of the higher hardness of the LHT processed surface,
its WL magnitude is larger than that for the UIT processed surface of
lower hardness. This effect may be associated with the fact that the
hard/brittle oxide layer is formed at the LHT process, and it can be
easily destroyed by UIT (Fig. 6). Destruction of the LHT induced
oxide film and micro-asperities of the surface profile can occur at
the wear tests, and it can cause the excessive abrasion of the tested
surface in the running-in stage by the broken oxide particles or
parts of micro-asperities (three-body wear). In the case of the UIT
finishing process, the destruction of the oxide layer occurs owing
to the multiple impacts (before the wear tests). Therefore, the
LHT + UIT processed surface, which has already deprived the
oxide layer and micro-asperities, demonstrates the lowest WL mag-
nitudes owing to the highest hardness and absence of negative fac-
tors neutralized by the UIT finishing process.
When the wear tests are prolonged till the finish of the running-in
stage of the wear process, the LHT hardened surface layers, which are lo-
cated under the destroyed oxide layer, mainly contribute to the WL
magnitude. In particular, after wear test lasted for 45 min the WL mag-
nitude of the LHT processed surface already lower than that for the
UIT processed one owing to the significantly higher surface hardness
after LHT in comparison with that after UIT.
 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
Fig. 9. 3D micrographs of the worn tracks of the UIT (a, d), LHT (b, e) and LHT + UIT (c, f) processed tool steel AISI D2 after quasi-static (a–c) and dynamic (d–f) tests lasted for 45 min.
Arrows indicate worn tracks.
Fig. 11 compares the friction force magnitudes registered for the spec-
imens of tool steel AISI D2 modified by different surface treatments. It is
seen that the friction force F registered in the dynamic test is significantly
smaller than that observed in the quasi-static test. Such difference is con-
nected to a lower quantity of the contacted areas between the surfaces of
the indenter and tested specimen in the dynamic regime. In other words,
the probability of the adhesive component of friction/wear is reduced.
Analysis of the friction forces registered in the quasi-static test shows
that for the initial and UIT processed states F become slightly larger
with increasing duration of the tests. After the LHT process, the F observed
in the quasi-static regime becomes higher with respect to the other treat-
ments owing to abrasion component of friction/wear. It slightly decreases
with increasing test duration. These effects are also related to the adhe-
sion of the surface layers of the specimen and indenter, which seemingly
exists in the first two cases and is absent in the last two ones. After the
combined LHT + UIT process, F becomes lower again indicating on the re-
duced adhesive and abrasive components of friction/wear.
4. Discussion
As-cast tool steels of the die equipment with a significant carbon
content (1.25…1.65%) including the tool steel AISI D2, contain the
Fig. 10. Wear losses of the initial and LHT, UIT and LHT + UIT processed specimens of tool
steel AISI D2 registered in quasi-static (S) and dynamic (D) conditions.
351
carbide eutectic. The mechanical properties, including wear resistance,
depending on the thermo-mechanical treatment, which determines
the formation of various phases of different sizes. Heating of these tool
steels above the temperature of pearlitic transformation (800…820
°С) results in dissolution of the secondary carbides and in saturation
of austenite with chromium. The higher the temperature, the lower
the volume fraction of carbides is, and the higher the concentrations
of carbon and chromium in austenite are. On the one hand, high volume
fraction of (CrFe)7С3 carbides provides a high wear resistance of the
hardened steels, but on the other hand, significant carbide heterogene-
ity can also reduce their toughness and strength [1].
Furthermore, the maximum hardness (62…64 HRC), which is
achieved by quenching, makes mechanical treatment impossible [1].
Therefore, to obtain the required properties and surface microrelief pa-
rameters the preliminary deformation treatments should be conducted
on the specimens/parts underwent annealing (HRC1 = 19.6) or
quenching from other temperatures (HRC1 = 45…52) [16]. The strain
hardening of tool steel is related to the generation and rearrangement
of dislocations in the alloyed ferrite, which contains both large and
fine carbides (Fig. 7b), and it is not as high as the thermal hardening.
It is well known that the laser surface melting of high-alloyed steels
causes the reduction in the surface hardness due to complete
Fig. 11. Friction force magnitudes registered for the initial and the LHT, UIT and LHT + UIT
processed tool steel AISI D2 in the quasi-static (S) and dynamic (D) conditions.
352 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
dissolution of carbides and a significant increase in the volume fraction
of the retained austenite [10]. The melted layer of the tool steel AISI D2
contained dendritic austenite structure and interlayers of the cementite
type [12]. As a result, the diffusion of chromium occurs quite slowly.
Therefore, the formation of the chromium carbides is retarded due to
high cooling rate from the liquid state [6]. In this study, the LHT induced
thermal hardening occurred without melting of the surface layer (Fig.
3(a–d)).
It is known that among the factors that affect the wear resistance,
the surface roughness/waviness and microrelief features play a crucial
role on the beginning stages of tests/operation (on the running-in
stage) [16]. Another factor, which determines the long-term operation
life, is the surface hardness. Its correlation with the wear resistance is
usually well described by the Archard expression (Eq. (3)). The results
obtained in this study indicate that the hardness of the surface layer of
tool steel AISI D2 can be effectively changed by selecting the preliminary
heat treatment and regimes of subsequent LHT, UIT and combined LHT
+ UIT processes, which cause different structural and phase transfor-
mations. Thus, the volume fractions of fine carbides and ultra-fine
grained martensite can be managed by choosing the regime of the
LHT process, which will affects the strain hardening at subsequent SPD
induced by the UIT process [16,38] or by other methods such as shot
peening [24], SMAT [25], FSP [37] or ball/roller-burnishing [39].
The experimental magnitudes of wear resistance W−1exp (estimated
as a reciprocal worn volume in mm−3) after the short-term (15 min)
and long-term (45 min) tests and the theoretically assessed wear resis-
tance W−1th of the studied steel are given in Fig. 11 depending on the
surface microhardness HV. The theoretical estimates were conducted
using the Archard expression (Eq. (3)), taking into account the duration
of the tests (curves 3, 5) and the local plasticity characteristics δH
(curves 4, 6), which was used as a factor inserted in the denominator
Fig. 12. Dependences of experimental (1, 2) and theoretical (3–6) wear resistance
(estimated as a reciprocal worn volume) of the tool steel AISI D2 on microhardness
registered after 15 (1) and 45 (2) min wear tests in quasi-static (a) and dynamic (b)
conditions and estimated using classical (Eq. (3)) (curves 3, 5) and modified (Eq. (4))
(curves 4, 6) Archard expressions.
of the expression (3):
W −1
R ¼ HV=δH KF S l: ð4Þ
Additionally, the magnitudes of K were chosen to be different in Eq.
(4) for various studied cases [34,40]. It was ~10−4 for the cases of initial
and UIT- or LHT + UIT processed surfaces underwent a mild wear (as-
perity deformation, adhesion, ploughing) and ~ 10−2 for the case of
the LHT processed surface severely worn by abrasion or micro-machin-
ing. Comparing the trends of the W−1exp and W−1th shows a good cor-
relation. Generally, according to Eqs. (3) and (4) the wear resistance
increases when the HV grows. The enhanced HV of the UIT processed
surface layer is caused by the strain hardening owing to the increased
dislocations density and their fixing with fine carbides (Fig. 7(b)). The
sequence comprising an accumulation of dislocations, their interaction,
and formation of dislocation cell structures is one of the main mecha-
nisms for hardenings of steels [41–44]. In view of the hardness increase,
the structural and phase transformations induced by the LHT process
appear more effective [13,27–29,45–48]. They manifest themselves in
the formation of the ultra-fine grained martensite-ferrite structure
(Fig. 6(b, c)) and fine secondary carbides (Fig. 8(a, b)). Wear resistance,
however, appears lower due to abrasion by the broken oxides and
microasperities. The theoretical W−1th correctly describes the W−1exp
curves owing to the increased friction force registered experimentally
(and used in Eq. (4)) for this case. The finishing UIT process only slightly
increases the hardness due to additional fragmentation and misorienta-
tion of grains/subgrains of the alloyed ferrite and martensite, which
boundaries are fixed by fine secondary carbides (Fig. 8(c, d)). Moreover,
it results in the oxides' removal and roughness reduction, i.e. it pre-
serves the LHT + UIT processed surface from extensive wear during
the subsequent test. Good correlation of W−1exp and W−1th is also ob-
served in dynamic conditions. It should also be noted that the use of
δH Eq. (4) results in a better concordance of the W−1exp and W−1th de-
pendencies. Thus, this parameter can reflect the effect of toughness/
brittleness on the wear resistance of the studied surfaces.
Let's consider the results of the 15 min wear tests carried out in the
quasi-static conditions. It is worth to drawn attention to the fact that in
spite of the higher surface hardness the LHT processed surface demon-
strates lower W−1exp than that of the UIT processed one, which pos-
sesses a lower surface hardness. The results of XRD analysis (Fig. 6)
show that this effect can be associated with the formation of the hard/
brittle oxide layers on the LHT processed surface and their destruction
during the wear tests. The broken oxide particles cause excessive abra-
sion of the tested surface and increase the wear losses at the short-term
tests. Herewith, if the oxide layer and micro-asperities would be re-
moved by some way, then it would lead to the increase in the W−1.
The W−1exp curves obtained after the long-term wear tests (for
45 min) confirm this supposition. The running-in stage finished, and
the oxide layer was removed in this case. As a result, the essential in-
crease in W−1exp occurs. Moreover, the finishing UIT process (i.e. LHT
+ UIT) is also effective in this sense. Both destruction and removal of
the oxide layer occur, and significant enhancement in W−1exp is
observed.
5. Conclusions
In this work, the relationship between the structure and phase trans-
formations, hardness HV (HRC) and wear resistance W−1 of the tool
steel AISI D2, modified by the separately applied UIT by multiple-pins
head (strain hardening) and LHT by scanning beam without melting
(thermal hardening), as well as by the combined LHT + UIT process
(thermo-mechanical hardening) was studied. The obtained results
allow making the following conclusions:
1. About 1.5 times increase in the hardness of the UIT processed surface
layer up to 80 μm thick is observed due to the strain hardening of the
 D.A. Lesyk et al. / Surface & Coatings Technology 328 (2017) 344–354
surface. A double increase in the hardness of the LHT processed sur-
face layer of ~300 μm thick is caused by the formation of fine-grained
ferritic-martensitic structure and secondary carbides. The highest in-
crease in the surface hardness (about 2.5 times) after the combined
LHT + UIT process is caused by the formation ultra-fine grained
structure (~80–250 nm) with grain boundaries fixed with fine sec-
ondary carbides (~20 nm).
2. In the dynamic wear tests lasted for 15 and 45 min, the experimen-
tally registered magnitudes of the wear loss of the tool steel AISI D2
are reduced in 2, 3 and 4 times in comparison with the initial state
after the LHT, UIT, and combined LHT + UIT processes, respectively.
3. In the quasi-static wear tests lasted for 45 min, the experimentally
registered magnitudes of the wear loss of the tool steel AISI D2 are re-
duced in ~1.5 times only after the combined LHT + UIT process. The
solely applied UIT and LHT result in the wear losses almost identical
with that of the initial surface. However, the reasons of the latter are
different. It is the insufficient surface hardness of the UIT processed
surface, and the excessive abrasive wear of the LHT processed surface
induced by the broken parts of the oxide layer.
4. Theoretical evaluations of the wear resistance W− 1th using the
Archard expression correlate well with the experimental data
W−1exp, although they are slightly underrated. The best correlation
of the W−1th and W−1exp was achieved after taking the local plastic-
ity characteristics δН into account, which reflects the ability of the
material to be deformed plastically without destruction.
Acknowledgements
This study is financially supported by the East-West European
Network on higher Technical education (EWENT) programme
Erasmus Mundus Action 2 Lot 8, as well as partially supported by
National Academy of Sciences of Ukraine (Project 0114U001127)
and Scientific Program of NASU “Reliability and durability of mate-
rials, structures, equipment, and buildings Resource 2” (Projects
9.8.1 and 9.8.2).
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