A. LISIECKI, A. KURC-LISIECKA: EROSION WEAR RESISTANCE OF TITANIUM-MATRIX COMPOSITE Ti/TiN ...
29–34
EROSION WEAR RESISTANCE OF TITANIUM-MATRIX
COMPOSITE Ti/TiN PRODUCED BY DIODE-LASER GAS
NITRIDING
ODPORNOST KOMPOZITA PROTI EROZIJSKI OBRABI Ti/TiN
IZDELANEGA S PLINSKIM NITRIRANJEM S POMO^JO
DIODNEGA LASERJA
Aleksander Lisiecki1, Agnieszka Kurc-Lisiecka2
1Silesian University of Technology, Faculty of Mechanical Engineering, Welding Department, Konarskiego 18A, 44-100 Gliwice, Poland
2University of D¹browa Górnicza, Rail Transport Department, Cieplaka 1c, 41-300 D¹browa Górnicza, Poland
aleksander.lisiecki@polsl.pl
Prejem rokopisa – received: 2015-06-30; sprejem za objavo – accepted for publication: 2016-02-05
doi:10.17222/mit.2015.160
A prototype experimental stand equipped with a novel high-power direct diode laser (HPDDL), characterized by unique
properties of the laser beam, was applied for producing titanium-matrix composite (TMC) surface layers during the laser gas
nitriding (LGN) of the titanium alloy Ti6Al4V in the liquid state. The erosion wear characteristic of the substrate and nitrided
surface layers was investigated. It was found that the erosion wear resistance of the composite surface layers is significantly
higher than the substrate of titanium alloy Ti6Al4V. The erosion wear resistance depends on the angle of incidence. Reducing
the angle of incidence decreases the weight loss of the composite surface layers and simultaneously increases the weight loss of
the Ti6Al4V. It was found that the weight loss of the composite surface layer with the highest resistance is over six times lower
compared to the Ti6Al4V, at an incident angle of 15°.
Keywords: laser nitriding, titanium alloy, diode laser, erosion wear, composite
Prototipno eksperimentalno stojalo opremljeno z novim diodnim laserjem velike mo~i (HPDDL), zna~ilnem po edinstvenih
lastnostih laserskega `arka, je bilo uporabljeno za izdelavo povr{inske plasti kompozita na osnovi titana (TMC), med plinskim
nitriranjem z laserjem (LGN) titanove zlitine Ti6Al44V, v staljenem stanju. Preiskovane so bile zna~ilnosti erozijske obrabe
podlage in nitrirane povr{ine. Ugotovljeno je bilo, da je odpornost na erozijsko obrabo kompozitne povr{inske plasti ob~utno
ve~ja v primerjavi s podlago iz titanove zlitine Ti6Al4V. Odpornost na erozijsko obrabo je odvisna od vpadnega kota.
Zmanj{anje vpadnega kota zmanj{uje izgubo te`e povr{inke kompozitne plasti in hkrati pove~a izgubo te`e Ti6Al4V.
Ugotovljeno je, da je izguba te`e kompozitne povr{inske plasti, z najve~jo odpornostjo, pri vpadnem kotu 15°, ve~ kot {est krat
manj{a v primerjavi z Ti6Al4V.
Klju~ne besede: nitriranje z laserjem, titanova zlitina, diodni laser, erozijska obraba, kompozit
1 INTRODUCTION
Titanium alloys, thanks to their excellent strength-
to-weight ratio and excellent corrosion resistance, are
widely used in aerospace, automotive, power plant,
maritime, and many other industries.1–6 The most
commonly used titanium alloy is Ti6Al4V (Grade 5
according to ASTM). Light metals and alloys are of
particular importance in aerospace. For example, more
than half of the rotating parts of a modern turbofan
aircraft engine are made of titanium alloys, including the
rotors and fan blades.7–9 Similarly, the blades made of
titanium alloys are commonly used in the steam turbines
of high-power generators.10–13 Titanium alloys are also
used for manufacturing parts for turbochargers, air and
hydraulic pumps, turbines and impellers, etc.14–16 In each
of the above cases, the working surfaces are exposed to
wear, mainly by erosion or cavitation erosion.1,17 For
example, the engines of planes, helicopters, and other
aircraft, as well as rocket engines are often subjected to
severe erosion from sand and dust particles, drops of
rain, or other solid and hard particles in flight and also
during manoeuvres at the airport or landing pad.18–20
However, titanium alloys, and particularly pure
titanium, do not possess high resistance to erosive wear
because of the relatively low surface hardness.1–6 There-
fore, various methods to modify the surface of the tita-
nium alloys are used in industry, and also new methods
and techniques are being developed.1–6,21
Among the many methods of surface modification of
titanium alloys, one of the most efficient is laser gas
nitriding (LGN).2 Y. Fu et al.2 have studied different
methods for improving the erosion resistance of pure
titanium. They have found that the laser surface treat-
ment of titanium in a nitrogen atmosphere provides the
best results and a significant improvement of the erosion
resistance compared to other methods of surface treat-
ment and the deposition of surface lasyers.2
Although the LGN method was invented in 1983, it is
still being developed. The reason for this is the conti-
nuous development of laser devices and associated with
this advances in laser technology.1,4 The LGN process for
Materiali in tehnologije / Materials and technology 51 (2017) 1, 29–34 29
MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967-2017) – 50 LET/50 YEARS
UDK 620.168:620.19:662.2.032 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 51(1)29(2017)
titanium and titanium alloys has been widely studied by
scientists, and also there are plenty of articles in this
field. However, most of the articles concern the structure,
morphology, corrosion resistance, tribology and mecha-
nical properties of the surfaced layers produced by
gaseous CO2 and solid-state YAG lasers.4,22 There are
only a few publications on the application of high-power
diode lasers (HPDLs) in the process of titanium nitriding
and also there is no information on the erosion wear
resistance of surface layers nitrided by HPDLs.23–25
In the present work, a novel continuous wave (CW)
HPDL emitted in the near-infra-red band at 808 nm, with
a rectangular laser beam spot and a uniform energy dis-
tribution across the spot was applied for producing sur-
face layers on the titanium alloy Ti6Al4V during LGN.
The erosion wear resistance of the Ti6Al4V alloy before
and after the LGN process at different angles of inci-
dence was investigated.
2 EXPERIMENTAL PART
The titanium alloy Ti6Al4V (Grade 5 according to
ASTM B265) with the nominal chemical composition
6.29 Al, 4.12 V, 0.14 C, 0.18 Fe in % of mass fractions
and balance Ti was chosen for investigations of the
nitriding process. The specimens of titanium alloy for
the nitriding tests and for the erosion tests were cut into
coupons 50.0×100.0 mm from a hot-rolled sheet having
a thickness of 3.0 mm. The specimens of titanium alloy
used for the erosion tests were mechanically ground by
180-grit SiC paper and cleaned. In turn, the specimens
for LGN tests were mechanically ground and degreased
with acetone prior to the nitriding tests.
The trials of LGN were carried out by means of a
fully automated prototype stand equipped with a novel
high-power direct diode laser (HPDDL) characterized by
direct emission of the laser beam, rectangular laser-beam
spot with a width of 1.8 mm and a length of 6.8 mm at a
given configuration of optics and a short wavelength of
808 nm.
The short wavelength is advantageous because of the
efficiency of the heat transfer to the metal surface as a
result of Fresnel absorption. In this case the absorption
coefficient on the surface of the titanium alloy for the
808 nm wavelength is significantly higher compared to
the wavelength of gaseous CO2 lasers and even com-
pared to the solid-state lasers. Additionally, the multi-
mode and even energy distribution of the laser radiation
along the longer side of the beam spot ensures the uni-
form irradiation of the laser-treated surface and a uni-
form temperature distribution across the processing
track.4 In order to ensure the full control of the process-
ing atmosphere, the samples were placed in a nitrogen-
filled chamber. The pure nitrogen (99.999 % purity) was
supplied into the chamber at flow rate of 10.0 L/min and
a pressure of 1.0 atm. The nitrogen flow was switched in
advance of about 90 s to remove the air from the
chamber. The laser beam was delivered into the chamber
through a transparent cover made of tempered glass. The
rectangular beam was focused on the top surface of the
specimens and the beam spot was set transversely to the
scanning direction. The test surface layers were pro-
duced as single stringer beads during linear scanning of
the surface by the laser beam in a pure nitrogen atmo-
sphere. The test surface layers were produced at different
processing parameters, and thus a different heat input of
nitriding. The processing parameters are given in Table 1.
Table 1: Parameters of the laser gas nitriding of the titanium alloy
Ti6Al4V by the HPDDL
Tabela 1: Parametri plinskega nitriranja z laserjem titanove zlitine
Ti6Al4V z HPDDL
No. of
surface
layer
Scanning
speed,
mm/min
Laser out-
put power,
W
Heat
input,
J/mm
Power
density,
kW/cm2
S1 200 1000 300 8.17
S2 200 800 240 6.54
S3 200 600 180 4.90
The erosion tests were performed in accordance with
the ASTM G76 standard for a determination of the ero-
sion rate by solid particles’ impingement in a gas stream.
The apparatus used to carry out the erosion tests was
built strictly in accordance with the requirements of the
standard. The solid particles used for the erosion tests
were natural angular alumina sands with a size of 50 μm.
The erodent particles were fed from a disk powder feeder
and accelerated from a nozzle by pressured dry air. The
pressured air was supplied from a cylinder and the pres-
sure was stabilized by a two-stage pressure reducer. The
air pressure was adjusted to provide the particle velocity
of 70 m/s. The feed rate of the abrasive sand was set at
2.0 g/min. The distance from the nozzle tip to the tested
surface was kept at 10.0±0.5 mm. A nozzle having an in-
ner diameter of 1.5 mm and a length of 50 mm was ap-
plied. A rotary sample holder allowed for a change in the
angle of the particles’ impingement on the surface from
15° to 90°. Prior to the erosion test of the surface layers
and the base metal, a calibration of the particles’ velocity
was performed according to the procedure given in the
ASTM G76 standard. The material used for the calibra-
tion was C22 annealed steel, according to EN 10250-2
(1020 steel according to AISI).
All the erosion tests were performed under ambient
conditions with a temperature of about 25 °C and a rela-
tive humidity of 45–50 %.
The base metal Ti6Al4V titanium alloy and the sur-
face layers were eroded for 5 and 10 minutes at impact
angles of 15°, 30°, 45° and 90°.
The weight of the samples was measured before and
after the erosion test using a laboratory scale with an
accuracy of ±0.01 mg. Prior to the measurements of
weight, each sample was cleaned with compressed air
and the weight was measured three times in order to
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determine the mean value and to provide the high accu-
racy of the measurement.
Subsequently, the eroded surfaces were analysed with
a scanning electron microscope (SEM) to identify the
mechanisms of wear and mass loss.
3 RESULTS AND DISCUSSION
The relationship between the mass loss and the im-
pingement angle after 10 min of erosion test of the base
metal Ti6Al4V is shown in Figure 1. As can be seen, the
mass loss of the base metal is clearly dependent on the
angle of alumina particles’ impact (impingement angle),
and the mass loss increases with a decreasing the angle.
Such dependence is typical for ductile materials, as indi-
cated in the literature.1–3
On the other hand, in the case of the laser gas nitrided
surface layers the relationship between the mass loss and
impingement angle is different, as can be seen in Figure 2.
For all of the nitrided surface layers the lowest mass loss
occurred at the lowest impingement angle of 15°, while
increasing of the angle resulted in increasing of the mass
loss, reaching the maximum at an angle of 90°, as shown
in Figure 2. Thus in general, the nitrided surface layers
exhibited brittle-type behaviour, characteristic for hard
and brittle materials.1–3 The obtained results are different
from those presented by J. R. Laguna-Camacho et al.3 in
the case of TiN coatings deposited by PVD on the
substrate of steel. In addition, the data in Figure 2
indicate a clear relationship between the laser processing
parameters and the erosion behaviour of the nitrided
surface layers. For example, the surface layer produced
at the lowest laser output power of 600 W (Sample S3)
and so the lowest heat input of 180 J/mm exhibited the
lowest mass loss so the best erosion resistance (Re) at the
highest angle of 90°, as can be seen in Figure 2a. In this
case the mass loss was about 5 mg. In contrast, the
surface layer produced at the highest heat input of 300
J/mm (laser power 1000 W, Sample S1) exhibited the
highest mass loss of about 8 mg, (Figure 2c). For com-
parison, the surface layer produced at the medium heat
input of 240 J/mm (Sample S2) also showed a medium
mass loss below 7 mg, (Figure 2b). Here, it is possible
to conclude that in the range of the investigated parame-
ters the erosion resistance of the laser nitrided surface
layers at the impingement angle of 90° is almost directly
proportional to the heat input of the LGN process. This
phenomenon can be explained by the differences in the
microstructure of the surface layers nitrided at different
parameters (heat inputs). At a high impingement angle
(e.g., 90°) the particles impact both the hard TiN nitrides
and the softer metallic matrix. So in this case the mass
loss, thus the erosion resistance Re, is dependent on the
properties of the titanium nitrides’ precipitations (brittle
material type), but equally on the properties of the me-
tallic matrix (a rather ductile material type). SEM micro-
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Figure 1: Relationship between the mass loss and impingement angle
for erosion of the base metal Ti6Al4V
Slika 1: Odvisnosti med izgubo mase in vpadnim kotom pri eroziji
osnovne kovine Ti6Al4V
Figure 2: Relationship between the mass loss and impingement angle
for different erosion times of the nitrided surface layers: a) S3, b) S2
and c) S1
Slika 2: Odvisnost med izgubo mase in vpadnim kotom pri razli~nih
~asih erozije nitirirane povr{inske plasti: a) S3, b) S2 in c) S1
graphs of the nitrided surface layers at the same magni-
fication are presented in Figure 3. As can be seen, the
morphology and size of the TiN dendrites, as well as the
proportion between the nitrides (population) and the
metallic matrix, are different for every surface layer. The
microstructure and morphology of every single surface
layer correlate with the microhardness profile on the
cross-section, (Figure 4). The surface layer produced at
the highest heat input of 300 J/mm is composed of long
and densely packed TiN dendrite precipitations with a
relatively small amount of metallic matrix (Figure 3a).
Therefore, the microhardness in this case reaches the
maximum value and remains at a high level to a depth of
about 1.4 mm, (Figure 4). The high amount of TiN
dendrites characterized by a very high microhardness is
responsible for the erosion behaviour of the surface layer
at the angle of 90°. In turn, the nitrided surface layers
produced at lower heat inputs have fewer TiN dendrite
precipitations (Figure 3b, c). Additionally, these surface
layers are thinner and also the size of the TiN dendrites
is smaller and the share of metallic matrix is significant-
ly higher. These differences in the structure and morpho-
logy of the surface layers cause a change in the micro-
hardness distribution as well as in the erosion behaviour
(Figure 2, 4). In this case, the softer metallic matrix has
a greater influence on the erosion wear mechanism
(erosion behaviour).
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Figure 4: Microhardness distribution on the cross-section of nitrided
surface layers and the base metal of titanium alloy Ti6Al4V
Slika 4: Razporeditev mikrotrdote na preseku nitrirane povr{inske
plasti in osnovne kovine, titanove zlitine Ti6Al4V
Figure 3: SEM micrographs of the nitrided surface layers, showing
the composite structure consisting of TiNx dendrites in a metallic ma-
trix of samples: a) S1, b) S2 and c) S3; TiN Layer – a homogenous
layer of titanium nitrides on the top surface, MM – metal matrix of Ti
(N), TiNx – titanium nitrides precipitation with various stoichiome-
tric concentration (-TiN, -Ti2N)
Slika 3: SEM-posnetek nitrirane povr{inske plasti, ki ka`e kom-
pozitno strukturo, ki sestoji iz TiNx dendritov v kovinski osnovi
vzorcev: a) S1, b) S2 in c) S3; TiN plast – homogena plast titanovih
nitridov na povr{ini, MM – kovinska osnova Ti(N), TiNx – izlo~anje
titanovih nitridov z razli~no stehiometri~no koncentracijo (-TiN,
-Ti2N)
Figure 5: A view of eroded surfaces of titanium alloy Ti6Al4V at the
incident angle of: a) 90° and b) 15° and nitrided surface layer S1
eroded at the incident angle of c) 90° and d)15°; EC – erosion crater,
SD – secondary damage ("halo effect")
Slika 5: Izgled erodirane povr{ine titanove zlitine Ti6Al4V pri
vpadnem kotu: a) 90° in b) 15° in nitrirana povr{inska plast S1,
erodirana pri vpadnem kotu c) 90° in d) 15°; EC – erozijski krater, SD
– sekundarne po{kodbe ("halo efekt")
On the other hand, in the case of the lowest im-
pingement angle of 15°, the surface layer produced at the
maximum heat input, having the maximum depth and
maximum microhardness, exhibited the lowest mass loss,
and thus the highest erosion resistance Re, (Figure 2c).
However, the relationship between the mass loss at the
angle of 15° and the processing parameters of the LGN
process (in general, the heat input) is not as clear and
simple as in the case of the angle 90°. The reason for this
is the different way of impacting the surface by the alu-
mina erodent particles. When the erosive stream impacts
the surface at a low angle of 15°, the alumina particles
are partially bounced and slide on the top surface. In
such conditions the erosive wear of the composite
surface layer is limited by the erosion rate of the hard
and wear-resistant titanium nitride precipitations, and the
softer metal matrix is not exposed to such strong erosion
as at high angles of impact. Thus, the amount of metallic
matrix has less effect on the overall erosion rate at a low
angle of impact. The eroded craters produced at different
incident angles on the surface of the titanium alloy
Ti6Al4V and on the nitrided surface layers are shown in
Figure 5. The shape and area of the craters depend on
the incident angle. The circular craters characterized by
the smallest area were produced at an angle of 90°. The
increase in the erosion angle changes the shape of the
crater to an elliptical shape and simultaneously increases
the wear area. The secondary erosion damage zone can
be observed around the deep eroded craters (Figure 5).
This secondary damage is caused by the scattered parti-
cles of the erodent stream. This phenomenon is called, in
the literature, the "halo effect".3
The SEM morphology of the bottom surface of the
eroded craters is shown in Figure 6, 7. The worn sur-
faces of the titanium alloy Ti6Al4V eroded at high inci-
dent angles show irregular indentations, craters and deep
pits (Figure 6a). Additionally, fragments of erodent
particles embedded in the surface were identified in the
bottom of the eroded craters (Figure 6a). On the other
hand, the worn surfaces eroded at low incident angles
show deep and long scratches and plastically deformed
ploughing trenches (Figure 6b). Besides the fragments
of erodent particles embedded in the surface, also some
wear debris inside the trenches were found. The appear-
ance of the eroded surfaces and traces of wear indicate
two different mechanisms of wear during erosion at low
and high incident angles. At low incident angles the
material loss is mainly caused by the abrasive wear by
plastic deformation of the material, cutting and plough-
ing the surface by the angular erodent particles. In turn,
at high incident angles, the material loss is mainly
caused by plastic deformation and extrusion of the ma-
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Figure 7: SEM morphology of the bottom surface of eroded craters of
nitrided surface layer S1 at the incident angle of 90° a) and 15° b); P –
pits, PT – ploughing trenches, EP – erodent particles
Figure 7: SEM morfologija povr{ine dna erozijskega kraterja na nitri-
rani povr{inski plasti S1, pri vpadnem kotu a) 90° in b) 15°; P –
jamice, PT – brazde, EP – delci nastali pri eroziji
Figure 6: SEM morphology of the bottom surface of eroded craters of
titanium alloy Ti6Al4V at the incident angle of: a) 45° and b) 15°;
P – pits, PT – ploughing trenches, EP – erodent particles
Slika 6: SEM morfologija povr{ine dna kraterja titanove zlitine
Ti6Al4V, pri vpadnem kotu, a) 45° in b) 15°; P – jamice, PT – brazde,
EP – delci nastali pri eroziji
terial. The worn surface morphology of the nitrided sur-
face layer eroded at a low incident angle is clearly diffe-
rent compared to the base metal of titanium alloy, as can
be seen in Figure 7b. In this case the ploughing trenches
are shorter because the erodent particles rebound from
the hard surface. Large erodent particles embedded in the
surface were also found. The worn surface of the nitrided
surface layer eroded at a high angle were more rough-
ened with pits and craters, but without traces of cracks
(Figure 7a). The erodent particles embedded in the
surface were found also. In this case the material loss is
caused by brittle ruptures of the composite layer, espe-
cially the hard TiN precipitations.
4 CONCLUSIONS
The base metal of titanium alloy Ti6Al4V exhibited
ductile-type behaviour, reaching the maximum erosion
rate at the lowest angle of 15° of the alumina particles’
impact. Unlike the titanium alloy, the nitrided surface
layers exhibited brittle-type behaviour, reaching the
maximum erosion rate at the high angle of 90°.
Nevertheless, the erosion resistance (Re) of the nitrided
surface layers is higher for all the angles of impingement
compared to the base metal of titanium alloy.
Additionally, in the range of the investigated processing
parameters, the heat input of the LGN process has a
strong influence on the microstructure, morphology and
microhardness distribution across the surface layers, and
also on the erosion behaviour, especially at the angle of
90°. It was found that the erosion rate of the composite
surface layers at an angle of 90° depends on the
properties of hard nitrides and the softer metal matrix
equally. In turn, the erosion rate of the composite surface
layers at a low angle of 15° depends mainly on the
properties of the hard nitride precipitations. In this case
the amount and properties of the metallic matrix has less
effect on the overall erosion rate.
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A. LISIECKI, A. KURC-LISIECKA: EROSION WEAR RESISTANCE OF TITANIUM-MATRIX COMPOSITE Ti/TiN ...
34 Materiali in tehnologije / Materials and technology 51 (2017) 1, 29–34
MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967-2017) – 50 LET/50 YEARS