Surface & Coatings Technology 204 (2010) 2410–2416

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Surface & Coatings Technology

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / s u r f c o a t

Cemented carbide surface modifications using laser treatment and its effects on hard
coating adhesion
José Manuel Arroyo ⁎,a, Anselmo Eduardo Diniz b, Milton Sergio Fernandes de Lima c
a
Dep. Ingeniería Mecánica y Mecatrónica, Universidad Nacional de Colombia, Carrera 45 No 26-85, Bogotá, Colombia
b
Faculdade de Engenharia Mecânica, Universidade Estadual de Campinas, Rua Mendeleyev, 200, Caixa Postal 6122, CEP 13083-970, Campinas, SP, Brazil
c
Instituto de Estudos Avançados, Centro Técnico Aeroespacial.; P. Marechal Eduardo Gomes, 50, Caixa Postal 6044, CEP 12231-970, São José dos Campos, SP, Brazil

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

Article history: A pulsed HyBrID copper laser (510 nm, 30 ns, 13.8 kHz) was used for the treatment of cemented carbide
Received 18 August 2009 substrate before deposition of TiCN/Al2O3/TiN coating by the MT-CVD process. The influence of the laser
Accepted in revised form 7 January 2010 treatment on the surface morphology, surface structure and coating adhesion was investigated based on the
Available online 14 January 2010
laser irradiation dynamics used here. The experimental results showed that a large variety of cemented
carbide surface textures could be obtained, depending on the laser intensity and number of applied laser
Keywords:
pulses. Moreover, this laser process was found to produce some less carbon non-stoichiometric WC phases
Coated cemented carbide
Laser surface treatment
such as β-WC1 − x and α-W2C. Finally, using the Rockwell C adhesion test as output criteria, two sets of laser
Adhesion parameters were identified that produced a surface with adhesion strength comparable to that of
commercial tools pretreated by micro-sandblasting.
© 2010 Elsevier B.V. All rights reserved.

1. Introduction thermally sprayed WC–Co coatings over metallic substrates to

Coated cemented carbide is a material with a broad range of
applications, especially in cutting tools for machining several kinds of
metallic alloys. In addition to substrate and coating materials with
suitable properties, the treatment of substrates before coating
deposition, as well as high quality rounding of cutting edges, are
essential factors for durable cutting tools [1]. Several technologies and
combinations of technologies have been investigated for substrate
precoating preparation and can be loosely classified into chemical
processes, mechanical treatments, interlayers, thermal treatments
and laser ablation. Among these technologies laser ablation has
attracted interest for substrate precoating preparation because it
allows for precise removal of material with minimal thermal impact
on adjacent zones and high process stability, since no tool wear occurs
[2]. Laser ablation is also easily automated, does not produce waste
effluents and can be used for treating three-dimensional tools like
drills and saws [3].
Laser treatment is efficient in improving the adhesion strength of
PVD-AlTiN coating deposited on laser-irradiated cemented carbide
substrates [4], and is also a successful technique for improving the
adhesion strength of CVD-deposited diamond on cemented carbide
substrates [5–7]. Other noteworthy applications of laser processing of
cemented carbide materials include the application of WC–Co coat-
ings through laser cladding or alloying and laser remelting of
⁎ Corresponding author. Tel.: +57 1 3165684; fax: +57 1 3165641.
E-mail addresses: jmarroyoo@unal.edu.co (J.M. Arroyo), anselmo@fem.unicamp.br
(A.E. Diniz), milton@ieav.cta.br (M.S.F. de Lima).
improve their hardness and wear resistance [8]. Moreover, direct
fabrication of WC–Co parts using a rapid prototyping process known
as laser-engineered net shaping allows one to overcome the
disadvantages of the conventional sintering process [9].
In this work, the laser irradiation technique was used to prepare
the substrate surface of carbide inserts subsequently coated with
TiCN/Al2O3/TiN deposited by moderate temperature chemical vapor
deposition (MT-CVD). The objective was to establish a suitable
substrate surface preparation method to replace conventional
sandblasting method. The substrate surface topography produced by
the laser and the structural modifications were analyzed by scanning
electron microscopy (SEM), roughness measurements and X-ray
diffraction. Different surfaces, produced with various laser intensities
and number of laser pulses, were considered. The coating adhesion
strength of each surface was compared qualitatively by the Rockwell C
indentation test and two sets of laser process parameters were
identified that showed qualitatively the best adhesion strength, which
was comparable to that of commercial micro-sandblasted tools.
1.1. Laser-cemented carbide interaction
When metals are irradiated with laser pulses of nanosecond pulse
duration, the transfer of energy occurs within the pulse duration
under conditions of thermal equilibrium. Moreover, unlike other
metals, in WC–Co cemented carbide, the absorption of laser
irradiation energy varies slightly with the wavelength, from 76–77%
at 1064 nm to 85% at 355 nm [10]. Table 1 summarizes the thermal
properties of WC and Co. The WC and Co phases exhibit comparable

0257-8972/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2010.01.009
 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416
Table 1
Thermal properties of WC and Co [10–12].
WC
Density [g cm− 3] 15.7
Heat of melting [J g− 1] 192.4
Thermal conductivity (room temp.) [W m− 1 K− 1] 60–84
Specific heat capacity (room temp.) [J g− 1 K− 1] 0.210
Boiling temperature [K] 6273
Melting temperature [K] 3070–3140
WC–Co binary eutectic temperature [K] 1583
thermal conductivities but show different melting and boiling points.
In the description of thermal phenomena induced by laser energy, the
depth of material exposed to heat transfer during a laser pulse is
called the thermal penetration depth (l), which can be estimated by
Eq. (1), where τp: pulse duration, k: thermal conductivity, ρ: material
density and c: specific heat. In high intensity processing, the thickness
of the modified layer is not necessarily equal to the thermal
penetration depth because the material is ejected in this condition.
sffiffiffiffiffiffiffiffiffiffiffi
k intensity, I0 [MW cm− 2], and the quantity of laser pulses irradiating a
l≈2 τ ð1Þ
ρc p
With τp = 30 ns, the thermal penetration depth of both WC and Co
is l ≈ 1.5 μm; therefore, the different ablation behaviors of WC and Co
under laser irradiation in the ns time regime is determined only by the
difference between their melting points. Thus, when WC–Co
cemented carbide is laser-processed, the Co phase melts and
vaporizes first, after which ablation of the material occurs mainly by
selective removal of binder material. WC grains are removed by liquid
and/or by the ejected Co vapors. The WC melting temperature can be
reached with high intensities, leading to growth of larger WC grains
(few μm) during solidification [10].
2. Experimental
2.1. Substrate materials
Ground substrates of commercial coated cemented carbide cutting
tools (ISO equivalent P25, M15 and K30) were used as specimens for
the laser surface processing experiments. These substrates were
composed of 9% cobalt binder, 90% tungsten carbide and 1% complex
carbides (TiC, TaC, and NbC), with a grain size of 3–5 μm. Tool coating,
which was deposited at the tool manufacturing facility using the
moderate temperature chemical vapor deposition process (MT-CVD),
consisted of a multilayer TiCN/Al2O3/TiN coating with a total thickness
of approximately 5 μm. Before and after laser processing, the sample
substrates were subjected to an ultrasonic bath in deionized water for
5 min. Before coating, the samples were also treated with the standard
ultrasonic cleaning bath that the tool manufacturer applies to its
entire product line.
2.2. Laser irradiation process
A HyBrID copper laser source was used for surface irradiation,
which delivers a laser beam with a wavelength λ = 510 nm, pulse
duration τp = 30 ns, focus diameter df = 30 μm, repetition rate fr =
13.8 kHz and high beam quality M² ≈ 3.5. The diameter of beam focus
was measured experimentally by irradiating a thin opaque bronze
sheet with one laser pulse at the maximum mean power used
(1.2 W); after, the diameter of the affected area was measured by
scanning electron microscopy. Using the same laser facility, Gião et al.
[13] reported that the beam waist after the lens did not change
considerably with iris aperture, within a fluctuation of about 10%.
2411
Therefore, for intensity calculations, only the laser's mean power
could be recorded in the experiments without appreciable error.
Co The main components of the laser system comprise the laser
cavity, an iris diaphragm for laser intensity control, a computer-
8.8
259.6 controlled scanning head to guide the laser beam over the workpiece,
69–75 and the necessary optics to direct the laser energy onto the workpiece
0.440 surface.
3200
Fig. 1 shows the laser surface irradiation dynamics applied. Laser
1768
surface texturing was performed by scanning the workpiece with
parallel laser tracks spaced 15 μm from each other and was applied in
an open atmosphere. As indicated in Eq. (2), the feed rate (vf) can be
expressed as a function of the number of pulses (np) irradiating a
particular point of the work surface, the path superposition, the focus
diameter and the repetition rate. Multiplication by 2 is due to fact that
the path superposition is equal to half the diameter of the beam.
2fr df
vf = ð2Þ
np
The controlled input parameters for laser processing were the
particular point of the work surface, np. The morphology of the
fabricated surfaces was examined under a JEOL-JXA-840A scanning
electron microscope (SEM) equipped with an energy dispersive X-ray
spectrometer (EDX).
The RZ-ISO roughness was measured with a Mitutoyo SJ-201P
roughness meter. A Rigaku Dmax 2200 X-ray diffractometer (XRD)
and the JCPDS (Joint Committee for Powder Diffraction Studies) cards
15_0806, 42_0853, 35_0776, 31_1408, 25_1047, 20_1316, 32_1383,
35_0801 and 38_1364 were used for the structural analyses. The
indentation adhesion Rockwell C tests were performed with a Pantec
durometer. A very stable laser with high beam quality was used, and
the evolution of surface morphology was gradual as a function of the
intensity and number of pulses. None of the surfaces deviated from
the observed tendency, so each set of process parameters was tested
only once and replications of the tests were considered unnecessary.
3. Results and discussion
3.1. Laser-produced morphologies
In order to evaluate the effect of laser intensity (I0) and the number
of pulses (np) on the surface topography, two groups of samples were
laser-irradiated. In the first group, the number of pulses was constant
(np = 32) while the laser intensity varied (I0 = 137, 239, 273, 308 and
410 MW cm− 2). In the second group, the intensity was constant
(I0 = 273 MW cm− 2) while the number of pulses varied (np = 16, 32,
64, 128 and 256). As can be seen in Figs. 2 and 3, depending on the
laser intensity and on the number of pulses, the effect of the laser's
interaction with the cemented carbide can range from an almost
Fig. 1. Laser surface irradiation dynamics used.
2412 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416

Fig. 2. Cemented carbide surfaces irradiated with 32 pulses and varied laser intensities.

imperceptible surface change to violent ablation with instantaneous
vaporization of large volumes of material.
The SEM images in Fig. 2 show the morphology of cemented
carbide surfaces laser-treated with np = 32 fixed laser pulses and
varying laser beam intensity. Fig. 2A corresponds to the ground
surface. At 137 MW cm− 2 (Fig. 2B), ablation of the material was
almost imperceptible. Part of Co at the surface melted and evaporated
and WC melted. A thin resolidified layer with a few small blowholes
was visible. This layer was probably composed of new WC coalescent
grains. At an intensity of 239 MW cm− 2 (Fig. 2C), a uniform structure
of peaks and valleys superimposed with resolidified materials was
observed, probably caused by vapor expansion and by the differen-
tiated ablation threshold of Co and WC. Many 0.5 μm blowholes were
observed, suggesting vapors and/or gases exiting from the surface. At
273 MW cm− 2 of intensity (Fig. 2D), the peak-valley structure with
blowholes appeared more interlaced and the orientation of the laser
beam feed rate was visible. At a laser intensity of 308 MW cm− 2, a
channel oriented in the direction of the laser beam path was formed
on the surface (Fig. 2E). The peak-valley topography was still present,
but with parallel mountain ranges apparently formed by melted
materials displaced by the momentum originated by the laser beam.
Complex gas-dynamic processes occur when a high power laser beam
interacts with an absorbing solid surface since the processes are very
similar to those in explosions. The momentum arising outside the

Fig. 3. Cemented carbide surfaces irradiated at 273 MW cm− 2 with varied number of pulses.
 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416
irradiated spot contributes considerably to the recoil of the irradiated
surface [14]. Moreover, with a Gaussian laser beam, the intensity of
the laser is highest at the center of the beam, which could also explain
the ablation of material at the centerline. At a laser beam intensity of
410 MW cm− 2 (Fig. 2F), the morphology of the irradiated surface was
very irregular and appeared to have undergone massive unstable
evaporation–sublimation of both WC and Co. The flow of melted
material was evident and the surface showed violent ablation, with
irregular channel patterns and drops of resolidified material.
Fig. 3 shows the effect of the number of pulses on the surface
morphology subjected to a laser beam intensity of 273 MW cm− 2.
Sixteen laser pulses (Fig. 3B) produced a clearly visible channel
topography oriented in the same direction as the laser beam feed on
the surface. Parallel channel mountain ranges and numerous blow-
holes were formed by displaced melted materials. An interlaced peak-
valley structure with blowholes appeared at 32 laser pulses (Fig. 3C),
and the mountain range was less evident, possibly because the
accumulated laser pulses produced more evaporation. Sixty-four and
128 pulses (Fig. 3D and E) produced an interlaced peak-valley
morphology, evidencing the laser beam feed direction. The mountain
range observed previously (Fig. 3B) was absent and there was no
evidence of melted material flow. The main ablation mechanism
seemed to be direct evaporation–sublimation. The structure of the
surface processed with 256 pulses (Fig. 3F) showed a spontaneous
row of holes with a mean diameter of 6 μm and periodicity of 14 μm.
The large number of laser pulses probably explains the formation of
holes resulting from the intensive accumulated reflection of laser
energy at the bottom of the valleys created initially. This reflection
produced localized vaporization with ejection of material from the
interaction zone due to an evaporation recoil pressure gradient. It is
also possible that bubbles emerging from the layer just below the
melted layer produced this volcanic aspect.
According to Yilbas et al. [15], when cemented carbide is laser-
irradiated, the rapid melting and evaporation of Co binder phase
accelerates the cooling of the affected volume, which slows the melting
and evaporation of WC phase. After that, the rapid cooling of WC induces
thermal stresses that promote the formation of cracks in the resolidified
WC. Fig. 4 shows the SEM images of the top and cross section (fractured)
of the original surface and of the surface laser-irradiated with 32 pulses
—273 MW cm− 2. Blowholes produced by vapors and/or gases exiting
from the surface are visible. Although these holes relieve stresses, there
were also cracks propagating in every direction, probably originated
during solidification of the molten layer.
Fig. 4. SEM images of the top and cross section (fractured) of the original surface and the surface laser-irradiated with 32 pulses—273 MW cm− 2.
2413
As Fig. 4 also shows, the layer of the material melted by laser
processing was very thin, with a thickness of less than 1 μm (the
calculated thermal penetration depth of WC and Co is ≈1.5 μm).
Apparently, in a process similar to that proposed by Dumitru et al.
[10], WC grains melted totally or partially and then solidified in the
form of larger thin grains.
The roughness values RZ-ISO, measured perpendicularly to the laser
feed orientation on each manufactured surface are also included in
Figs. 2 and 3. The intensity of the laser beam and the number of laser
pulses directly affected the roughness of the irradiated cemented
carbide surfaces, as indicated in Fig. 5. At a fixed number of 32 pulses,
the surface roughness values presented a slight increase at intensities
of 137 to 250 MW cm− 2 and a sharp rise at higher intensities. The
surfaces fabricated with a fixed laser intensity of 273 MW cm− 2, after
a sharp increase with 0 to 32 pulses, showed the slope of the curve
decreasing between 32 and 256 pulses. The initial pulses appear to
define the roughness, while the subsequent ones have a limited
contribution.
3.2. Surface structural changes
Fig. 6 shows the diffractograms of the surfaces processed with 32
fixed laser pulses and beam intensities of 0, 137, 239, 273, 308 and
410 MW cm− 2. The original surface (marked with 0) presented
typical sharp WC and tenuous Co diffraction lines. Due to the ground
condition, the surface did not exhibit an excess of segregated Co from
the sintering process. The surface processed at 137 MW cm− 2
presented incipient β-WC1 − x diffraction lines. At 239 MW cm− 2,
there was a rise in β-WC1 − x diffraction lines and a tenuous α-W2C
diffraction line appeared. The majority of diffraction lines on the
surfaces processed with higher beam intensities were still of WC,
albeit with progressively lower heights, while the number and height
of β-WC1 − x and α-W2C diffraction lines increased.
Fig. 7 shows the diffractograms of the surfaces processed with 0,
16, 32, 64, 128 and 256 laser pulses and a fixed laser intensity of
273 MW cm− 2. Similar to the structural changes produced by
increasing the laser intensity, increasing the number of pulses led to
an increase in the number and height of β-WC1 − x and α-W2C
diffraction lines, as well as a W3C diffraction line on the surfaces
processed with 128 and 256 pulses.
Therefore, the tungsten carbide phase transformation WC → β-
WC1 − x → α-W2C was observed with increasing laser intensity, while
the transformation WC → β-WC1 − x → α-W2C → W3C was observed
2414 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416

Fig. 6. X-ray diffractograms of surfaces irradiated with 32 pulses and with increasing
laser intensity, where: ➀:Co, ➁:WC, ➂:β-WC1 − x, and ➃:α-W2C.

to identify the set of laser parameters that produced high adhesion

strength of hard coatings deposited on cemented carbide substrates,
the trial-and-error method was applied, using the Rockwell C inden-
Fig. 5. Number of laser pulses and laser intensity influence the surface roughness.
tation test as output criteria.

with increasing number of pulses. Due to the high temperatures

reached and because the process was carried out in open air, it is
reasonable to assume that the oxygen in air promoted the formation
of COx gases, causing surface carbon to escape and forming these
tungsten carbide phases with progressively lower carbon content.
Because the W2C phase is thermodynamically unstable below 1300 °C
[16], an explanation for its presence at room temperature is the high
cooling rate of surface melted materials. The β-WC1 − x diffraction
lines observed could also be interpreted as the triple compound
Co6W6C, but due to the rapid direct evaporation of Co under the high
laser intensities applied, this phase formation is unlikely.
To estimate the Co compositional changes, all the irradiated surfaces
were analyzed by EDX. This analysis indicated that the concentration of
Co was slightly increased as the intensity and/or number of pulses
increased. Despite the semi-quantitative results of the EDX, this
conclusion was drawn because the percentage of Co increased
continuously as the intensity and/or number of pulses increased from
a minimum of 7.27% for the untreated surface to 8.4% at the maximum
intensity and to 8.7% at the maximum number of pulses. This result is
consistent with the findings of Kano and Inoue [17]. Who reported not
only Co evaporation but also Co diffusion from the bulk to the subsurface
due to the high temperature gradient generated by the laser pulses,
causing Co to concentrate close to the surface.

3.3. Effect of laser pretreatment on hard coating adhesion

To the best of knowledge, no laser surface ablation model exists, so

the experimental trial-and-error method is important to find a Fig. 7. X-ray diffractograms of surfaces irradiated with a laser intensity of 273 MW cm− 2
desired result and is widely used in industrial research [18]. Therefore, and several numbers of pulses, where: ➀:Co, ➁:WC, ➂:β-WC1 − x, ➃:α-W2C, and ➄:W3C.
 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416 2415

Fig. 8. Indentations on laser pretreated coated substrates and on the commercial substrate.

A total of 21 cemented carbide surfaces were laser-processed and sets of 64 pulses—239 MW cm− 2 and 02 pulses—410 MW cm− 2,
subsequently coated in four sequential groups, A, B, C and D. Fig. 8 which is even lower than that observed on a commercial coated
shows the Rockwell C indentations on those surfaces. This figure cemented carbide surface also tested and depicted in Fig. 8. Commercial
shows that minimal coating failure occurred with the laser process surfaces are typically prepared for coating by micro-sandblasting.

Fig. 9. Details of the coating deposited on the substrate treated with 32 pulses—308 MW cm− 2 (left) and the substrate treated with 32 pulses—239 MW cm− 2 (right).
2416 J.M. Arroyo et al. / Surface & Coatings Technology 204 (2010) 2410–2416
It can be seen in Fig. 8 that specific regions of sets of laser process
parameters produced almost no ablation with small surface modifica-
tions, or no differential effect with incremental number of pulses, or
even violent and irregular ablation. Therefore, no coated surface was
manufactured in these process regions.
The laser-prepared surfaces with high surface roughness generally
exhibited low adhesion strength, probably due to the loss of cohesion in
the growth of the coating. This can be observed in Fig. 9, which shows
details of the coating deposited on the substrate treated with 32 pulses—
308 MW cm− 2 (left), whose roughness was RZ-ISO = 4.75 μm, and the
substrate treated with 32 pulses—239 MW cm− 2 (right), whose
roughness was lower, i.e., RZ-ISO = 2.53 μm. Note that the coating has a
typical nodular growth mode on the rougher surface. This loss of coating
cohesion may lead to the type of failure observed on several surfaces in
Fig. 8, where portions of coating parallel to the tracks produced by the
laser process were removed from the substrate during the indentation
test.
4. Conclusions
Based on the results reported here, the irradiated cemented
carbide surfaces showed different surface topographies, variable
amounts of non-stoichiometric β-WC1 − x, α-W2C and W3C phases
and Co segregated from the bulk to the subsurface, depending on the
laser intensity and/or the number of laser pulses. Two sets of laser
parameters determined by the trial-and-error method for the
substrate, coating process and coating materials used in this work
presented good coating-substrate adhesion strength (64 pulses—
239 MW cm− 2 and 02 pulses—410 MW cm− 2), which was compara-
ble to that obtained with commercial micro-sandblasted tools. Hence,
the laser irradiation process can be considered an effective alternative
for the precoating treatment of cemented carbide cutting tools.
Acknowledgments
The authors gratefully acknowledge the support of the National
University of Colombia (UNCB), University of Campinas (UNICAMP),
the Photonics Division of the Institute for Advanced Studies (CTA-
IEAv), Sandvik Coromant Brazil and Villares Metals S.A.
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