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Licentiate Thesis

Production Technology
2021 No. 35

Tribological behaviour of
HVAF-sprayed WC-based coatings:
Role of process variables and binder chemistry

Kaveh Torkashvand
NMÄR
NEN M Ä R KE
VANE KE
VA
SS

TT

Trycksak
Tryck: Stema Specialtryck AB, September 2021 Trycksak
3041 0234
3041 0234
Licentiate Thesis
Production Technology
2021 No. 35

Tribological behaviour of
HVAF-sprayed WC-based coatings:
Role of process variables and binder chemistry

Kaveh Torkashvand
University West
SE-46186 Trollhättan
Sweden
+46 52022 30 00
www.hv.se

© Kaveh Torkashvand 2021


ISBN 978-91-89325-02-9 (Print)
ISBN 978-91-89325-01-2 (Electronic)
Dedicated to my family for their unconditional love…
Acknowledgements

I would like to express my sincere gratitude to my supervisors Assoc. Prof. Mohit


Gupta and Prof. Shrikant Joshi for their continuous guidance and endless
patience. Their countless support since the early stages of my PhD program has
kept me enthusiastic and motivated in this exciting learning journey, more than
ever. This is halfway through my PhD so I still have a lot left to learn from them.

I would like to sincerely thank Mr. Stefan Björklund for his help with spraying
process of the samples, for the useful discussions and for sharing his valuable
knowledge and experience of thermal spraying with me. Thanks to Mr. Magnus
Sandberg for his kind assistance in preparing samples. I would like to express my
sincere gratitude to Prof. Luca Lusvarghi for the discussions and invaluable
comments on this thesis. I would like to thank Mr. Filippo Ghisoni and Ms. Lidia
Baiamonte for their great assistance during the beginning stages of this work.

Financial support of the Knowledge Foundation, Sweden is gratefully


acknowledged. I also would like to thank Ms. Olivia Danielsson and Mr. Owe
Mårs from Höganäs for supporting this study through useful discussions and by
providing feedstock powders.

A heartfelt thanks to all my friends and colleagues at Production Technology


Centre (PTC) for creating a wonderful learning environment.

Finally, I would like to thank my family members for their continuous love and
support.

Kaveh Torkashvand
September 2021

v
vii
Populärvetenskaplig Sammanfattning

Cermet-beläggningar består av WC-partiklar inbäddade i ett metallbindemedel,


sprutat med High Velocity Air Fuel (HVAF) uppvisar utmärkt tribologisk
prestanda under olika slitage förhållanden. Med HVAF-tekniken kan partiklarnas
flygtemperatur och hastighet påverkas av konfigurationen av den utrustning som
används såväl som partikelstorleksintervallet för råmaterialet. Därtill kan kemin
hos det metalliska bindemedlet spela en nyckelroll för beläggningarnas egenskaper
och prestanda. I denna avhandling undersöktes egenskaper och tribologiskt
beteende hos HVAF-besprutade WC-baserade beläggningar. Undersökningen
gjordes genom att använda fyra olika uppsättningar av ändra sprutparametrar för
HVAF-processen där fyra olika munstyckskonfigurationer (4L2, 4L4, 5L2 och
5L4) och tre olika partikelstorleksintervaller av WC-CoCr råvarupulver (5/20,
5/30 och 15/45 µm). Studieegenskaper och prestanda för alla deponerade
beläggningar, påverkan av processvariabler (olika munstyckskonfigurationer och
olika partikelstorlekar) undersöktes. Dessutom undersöktes egenskaper och
prestanda för tre olika WC-baserade råvaror med alternativa bindemedel till CoCr
(NiMoCrFeCo, FeNiCrMoCu och FeCrAl) och jämfördes med WC-CoCr-
beläggning som referens. Beläggningens egenskaper undersöktes genom att
genomföra SEM-analys, mikroindragningstest och röntgenanalys. Beläggningens
prestanda utvärderades genom att utföra glidförslitning, erosionsslitage under
torra förhållanden och test med torr sand/gummihjulanordning. Vidare
undersöktes mekanismer för materialavlägsning i beläggningarna med
ovanstående tester genom analys efter slitage.

Ingen avsevärd fasförändring observerades för alla beläggningar som besprutades


med HVAF-teknik. Det avslöjades att minskning av pulvrets genomsnittliga
partikelstorlek resulterade i en förbättring av mikrostrukturella egenskaper, såsom
homogenitet och densitet, samt beläggningarnas hårdhetsvärde. Dessutom leder
det till en avsevärd förbättring av beläggningens slitageförmåga. Det visades att
användning av olika munstycken till HVAF-processen inte resulterar i en avsevärd
förändring i egenskaper eller prestanda hos WC-CoCr-beläggningarna. När det
gäller förslitningsmekanismer visades det att genom att minska partikelstorleken
från grov till medium eller fin sågs en avsevärd skillnad. För beläggningar
besprutade med fina och medelstora partiklar dominerades
förslitningsmekanismer av plöjningsslitage och sprickor av enskilda
hårdmetallkorn. För grova beläggningar observerades plöjningsslitage och
spårning tillsammans med avlägsnande av material.

Ingen signifikant skillnad i mikrostruktur eller fasförändring observerades i alla


beläggningar med alternativa bindemedel såväl som WC-CoCr som
referensbeläggning. Hårdhetsvärdet för alla de fyra beläggningarna låg inom

ix
intervallet 1100 - 1300 HV0.3. NiMoCrFeCo och FeNiCrMoCu visade bättre eller
jämförbar glidförmåga med referensbeläggningen. FeNiCrMoCu och FeCrAl
visade jämförbara prestanda under erosionsförhållanden och alla de tre
undersökta beläggningsmaterialen visade något sämre prestanda under
nötningsslitage jämfört med referensbeläggningen. Medan plöjningsslitage var
den vanliga förslitningsmekanismen i alla de fyra beläggningarna noterades
gropning i beläggningarna CoCr och FeNiCrMoCu vid glidförslitning.

Nyckelord: Tribologisk Prestanda; HVAF; WC-baserade Beläggningar;


Parametervariabler; Bindemedelskemi

x
Abstract

Title: Tribological behaviour of HVAF-sprayed WC-based coatings: Role


of process variables and binder chemistry

Keywords: Tribological Behaviour, HVAF; WC-Based Coatings; Process


Variables; Binder Chemistry
ISBN: ISBN 978-91-89325-02-9 (Print)
ISBN 978-91-89325-01-2 (Electronic)

Tungsten carbide (WC) based metallic matrix coatings sprayed using high velocity
air fuel (HVAF) technique have attracted increasing attention as they show
excellent tribological performance in various wear conditions. In the HVAF
method, particles’ in-flight temperature and velocity can be influenced by the
process variables including nozzle configuration as well as feedstock particle size
range. On the other hand, the chemistry of metallic binder can also play a key role
in determining both properties and performance of these coatings. In this thesis,
characteristics and tribological behaviour of HVAF-sprayed WC-based coatings
were investigated employing four different nozzle configurations (4L2, 4L4, 5L2
and 5L4), and three different feedstock particle sizes of WC-CoCr feedstock
powder (5/20, 5/30 and 15/45 µm). Also, characteristics and performance of
coatings processed with four different WC-based feedstocks comprising
alternative binders to traditionally used CoCr (namely CoCr, NiMoCrFeCo,
FeNiCrMoCu and FeCrAl) were investigated. Characteristics of the coatings were
explored by conducting scanning electron microscopy observations, micro
indentation testing and X-ray diffraction analysis. Performance of the coatings
was evaluated by conducting sliding wear, dry jet erosion wear and sand rubber-
wheel abrasion wear testing. Moreover, material removal mechanisms in the
coatings subjected to the above tests were investigated through post wear analysis.

X-ray diffraction analysis showed that no considerable phase change compared


to the starting feedstock was observed in any of the coatings sprayed by HVAF
technique. It was revealed that decrease in powder particle size range can result in
an improvement in microstructural characteristics, such as homogeneity and
density, as well as hardness of the coatings. Besides, it can lead to a substantial
improvement in wear performance of the coatings. It was shown that using
various nozzle configurations does not result in any considerable change in
characteristics or performance of the HVAF-sprayed WC-CoCr coatings. It was

xi
further shown that, by decreasing particle sizes from coarse to medium or fine, a
significant difference can be observed. While wear mechanisms for medium and
fine feedstock coatings were dominated by ploughing and fracture of individual
carbide grains, for the coarse feedstock coatings ploughing and grooving along
with the local removal of coating material were observed.

Hardness values for all the four coatings with different binder chemistries were
in a narrow range of 1100 – 1300 HV0.3. WC-NiMoCrFeCo and WC-
FeNiCrMoCu coatings showed better or comparable sliding wear performance
compared to WC-CoCr coating (as reference). WC-FeNiCrMoCu and WC-
FeCrAl coatings showed comparable performance under erosion conditions
while all the three binder alternatives yielded slightly inferior coating performance
under abrasion wear, compared to the reference coating. While ploughing was the
common wear mechanism in all the four coatings, pitting was noted in coatings
with CoCr and FeNiCrMoCu binders in case of sliding wear.

xii
xiii
Appended Publications

Paper A. Advances in thermally sprayed WC-based wear resistant coatings:


Co-free binders, processing routes and tribological behaviour, Submitted
to Journal of Thermal Spray Technology (under revision).
Kaveh Torkashvand, Shrikant Joshi, Mohit Gupta
Conceptualization, K.T., S.J. and M.G.; literature review, summarizing and analysis,
K.T.; writing—original draft preparation, K.T.; review and editing, S.J. and M.G.;
funding acquisition, S.J.

Paper B. Influence of test conditions on sliding wear performance of high


velocity air fuel-sprayed WC-CoCr coatings, Materials 14, no. 11 (2021):
3074.
Kaveh Torkashvand, Vinod Krishna Selpol, Mohit Gupta, Shrikant
Joshi
Conceptualization, K.T., M.G. and S.J.; methodology, K.T., M.G. and S.J.; investigation,
K.T. and V.S.; data curation, K.T and V.S.; writing—original draft preparation, K.T.;
review and editing, S.J. and M.G.; funding acquisition, S.J.

Paper C. Influence of nozzle configuration and particle size on


characteristics and sliding wear behaviour of HVAF-sprayed WC-CoCr
coatings, Surface and Coatings Technology (2021): 127585.
Kaveh Torkashvand, Mohit Gupta, Stefan Björklund, Francesco Marra,
Lidia Baiamonte, Shrikant Joshi
Conceptualization, K.T., M.G. and S.J.; methodology, K.T., M.G., S.B and S.J.;
investigation, K.T., S.B, F.M and L.B.; data curation, K.T; writing—original draft
preparation, K.T.; review and editing, S.J. and M.G.; funding acquisition, S.J.

Paper D. Tribological behaviour of HVAF-sprayed WC-based coatings


with alternative binders (under preparation).
Kaveh Torkashvand, Veronica Testa, Filippo Ghisoni, Luca Lusvarghi,
Giovanni Bolelli, Francesco Marra, Shrikant Joshi, Mohit Gupta
Conceptualization, K.T., V.T., F.G., L.L., S.J., G.B., and M.G.; methodology, K.T.,
V.T., F.G., L.L., S.J., G.B., F.M., and M.G.; investigation, K.T., V.T., F.G. and
F.M.; data curation, K.T., V.T. and F.G.; writing—original draft preparation, K.T.
and V.T.; review and editing, L.L., S.J., G.B., and M.G.; funding acquisition, S.J. and
L.L.

xiv
Table of Contents

Acknowledgements..........................................................................v
Populärvetenskaplig Sammanfattning ............................................. ix
Abstract .......................................................................................... xi
Appended Publications ................................................................. xiv
Abbreviations ............................................................................... xvii
1 Introduction .................................................................... 1
1.1 Research motivation and objectives ..................................... 1
1.2 Research questions ............................................................. 2
2 Background .................................................................... 3
2.1 WC-based coatings.............................................................. 3
2.2 Spraying processes ............................................................. 3
2.3 Size range of feedstock powder ........................................... 7
2.4 Alternative binders ............................................................... 7
3 Experimental procedure ................................................ 9
3.1 Spraying samples .............................................................. 10
3.2 Material characterization .................................................... 11
3.3 Micro indentation................................................................ 12
3.4 Tribological tests ................................................................ 12
3.4.1 Sliding wear test ............................................................. 12
3.4.2 Erosion wear test ............................................................ 13
3.4.3 Abrasion wear test .......................................................... 14
4 Summary of results ...................................................... 15
4.1 Coating characterization .................................................... 15
4.2 Test parameters for ball-on-disk experiment ...................... 16
4.3 Influence of process variables ............................................ 16
4.3.1 Wear performance .......................................................... 16
4.3.2 Wear mechanism ........................................................... 17

xv
4.4 Influence of binder chemistry ............................................. 19
4.4.1 Performance under sliding wear ..................................... 19
4.4.2 Sliding wear mechanisms ............................................... 20
4.4.3 Performance under erosion wear.................................... 21
4.4.4 Erosion wear mechanisms.............................................. 22
4.4.5 Performance under abrasive wear .................................. 23
5 Conclusions and future works .................................... 25
5.1 Summary and conclusions ................................................. 25
5.2 Future works ...................................................................... 26
6 References .................................................................... 27

Appended Publications

Paper A. Advances in thermally sprayed WC-based wear resistant


coatings: Co-free binders, processing routes and tribological
behaviour
Paper B. Influence of test conditions on sliding wear performance of
high velocity air fuel-sprayed WC-CoCr coatings
Paper C. Influence of nozzle configuration and particle size on
characteristics and sliding wear behaviour of HVAF-sprayed WC-
CoCr coatings
Paper D. Tribological behaviour of HVAF-sprayed WC-based
coatings with alternative binders

xvi
Abbreviations

HVAF: High Velocity Air-Fuel

HVOF: High Velocity Oxy-Fuel

APS: Atmospheric Plasma Spray

VPS: Vacuum Plasma Spray

LPPS: Low-Pressure Plasma Spray

HPPS: High Power Plasma Spray

SPS: Suspension Plasma Spraying

CS: Cold Spray

DG: Detonation Gun

WLI: White Light Interferometry

xvii
xviii
xix
1 Introduction

Ceramic/metal-matrix or cemented carbides are defined as “a class of hard, wear-


resistant, refractory materials in which the hard carbide particles are bound
together, or cemented, by a ductile metal binder” by ASM International’s Metals
Handbook [1]. Cemented carbides can be deposited in form of a coating by
thermal spray technology which is defined by ASM as “a group of coating
processes that provide functional surfaces to protect or improve the performance
of a substrate or component” [2]. In this technique, using a spraying torch, coating
materials (in powder, wire, or suspension form) are heated and accelerated
towards a prepared surface [2]. Accumulation of numerous sprayed feedstock
particles results in formation of the coating. Particulate composite coatings, also
known as cermet coatings, are widely used for wear-resistant applications since
1960 [2]. There has been a consistent progress in processing this class of materials
for tribological applications. However, it demands further attention to adapt the
existing technology with current concerns such as environment issues. This
becomes even more crucial when considering huge challenges posed by wear
phenomenon in a vast variety of industries [3].

1.1 Research motivation and objectives


High velocity oxy-fuel (HVOF) processing technique is the current state-of-the-
art method in industry for depositing WC-based coatings to combat wear, and is
the most widely used thermal spray route for applying cermet feedstock materials.
In this technique, Oxygen and fuel in form of gas or liquid are used to generate a
combustion jet at a temperature up to around 3000 ºC [2]. It can fabricate dense,
homogeneous, highly coherent and well-bonded coatings which perform
outstandingly in wear environments. However, high velocity air-fuel (HVAF)
technique is now poised to challenge its position. It has shown a great potential
in fabricating high-quality coatings with negligible ratio of material alteration. In
HVAF method, there are various torch configurations designed to achieve desired
in-flight velocity and temperature for feedstock powder particles. Different torch
configurations essentially involve variations in convergent-divergent design and
length of the nozzles. On the other hand, feeding powders with different particle
sizes into an identical gun configuration may also result in variations in in-flight
particle velocity and temperature. One of the advantages of HVAF over other
methods like HVOF is its lower flame temperature, which makes it suitable for
spraying feedstock powders with finer particle size without inducing a significant
decarburization effect in the powder feedstock [4–6]. This can be important since

1
it is shown that employing feedstock powder with reduced particle size can result
in improvement of microstructure characteristics as well as tribological
performance [7]. Therefore, selection of the suitable gun configuration for various
powder feedstocks with different particle size ranges demands a fundamental
understanding of how it influences characteristics and performance of the
resultant coating. Hence, conducting a comprehensive study with the aim of
foundation of a fundamental understanding of influence of process variables by
screening three powders with different particle sizes and spraying them with four
nozzles of varying configuration is the first main objective of this thesis.

In WC-based composite system, the metallic binder acts as a “cement” agent


providing physical support to the individual hard carbide particles. Cobalt has
been traditionally widely employed to act as binder over the past decades [8,9].
However, there are several concerns around this element including supply risk,
price as well as environmental considerations [10]. Therefore, searching for
alternative binders to Co exhibiting comparable performance seems crucial.
Evaluating characteristics and tribological performance of different HVAF
sprayed WC-based coatings utilizing four alternative binders is the second
objective of this study.

Therefore, the two main objectives of this thesis are:

- To develop fundamental understanding of coating process parameters-


microstructure-performance relationships in HVAF sprayed WC-based
coatings by investigating the role of feedstock particle size and nozzle
design
- To evaluate characteristics and performance of new generation
environment friendly WC-based wear resistant coatings by exploring
different binders as potential alternatives to Co

1.2 Research questions


The following research questions are framed based on the objectives of this study;

- RQ1: How do process variables influence characteristics and


performance of HVAF-sprayed WC-based coatings?
- RQ2: How do the proposed binder alternatives (to Co) perform in terms
of tribological properties?
- RQ3: How do process variables and binder chemistry influence wear
mechanisms under different wear environments in HVAF-sprayed WC-
based coatings?

2
2 Background

2.1 WC-based coatings


Hard carbide particles embedded in a metallic binder, deposited on a prepared
surface, are known as cermets or metallic matrix composites coatings. Particulate
composites of tungsten carbide (WC) particles with metallic binder are widely
used for tribological applications [11,12]. Hard WC particles which offer high
hardness to the coating blended together with a ductile metallic binder to provide
toughness to the system, create an excellent combination for tribological
applications [13,14]. Therefore, the composite system offers both high overall
hardness and toughness at the same time, which eventually results in excellent
tribological performance. Figure 1 (a) and (b) show low and high magnification
images of HVAF-sprayed WC-CoCr coating which is a typical view of HVAF
WC-based coating system. In Figure 1 (b), light grey particles are WC, dark grey
areas are identified as metallic binder and black spots are pores.

a b
Figure 1. Cross-sectional SEM images of deposited WC-CoCr coating a) low
magnification b) high magnification image

2.2 Spraying processes


WC-based wear resistant feedstock powders are typically deposited employing
thermal spray techniques. Thermal spray is defined as a process through which
feedstocks powders are heated up in a flame, accelerated and deposited on a
substrate [15]. Thermal spray can be categorized into various techniques
depending on specifications of the process such as source of power, type of
feedstock, etc. In general, the main difference in various thermal spray techniques

3
is reflected in the temperature and velocity produced by the flame. The different
flame temperature and velocity can subsequently influence the amount of thermal
and kinetic energy imparted to the injected feedstock powder particles. Figure 2
presents categories of thermal spray techniques based on the thermal power
source.

WC-based feedstocks are possible to be sprayed through a variety of thermal


spray techniques including plasma spraying (APS, VPS, LPPS, HPPS and SPS)
[16–18], cold spray (CS) [19] and high-velocity spraying routes (HVOF, HVAF
and DG) [20–22]. During the past decades, APS and HVOF techniques have been
more common for spraying WC-based feedstocks than the rest. However,
nowadays it is very well-known that APS sprayed WC-based coatings suffer from
severe decarburization of carbide particles during the spraying process [23,24].
Decarburization, in case of WC-based coatings, can be defined as loss of carbon
from the surface of WC particles due to overheating [2]. High velocity routes such
as HVAF and HVOF are attracting more and more attention, because of their
great potential in spraying this class of materials without an extreme overheating
of the carbides. A very dense, well-adherent WC-based coating can be achieved
by HVOF and HVAF techniques, since they provide a suitable combination of
high kinetic and adequate thermal energy [25,26]. Nevertheless, thermal energy
in HVOF technique, because of employing pure oxygen, is still relatively high
enough to keep the window open for occurrence of decarburization. Instead,
employing compressed air in HVAF technique can keep particles temperature
under 1500 ºC while in-flight particles can reach a high speed of up to 1200 m/s
[7,27,28]. This provides a greater kinetic energy with lower particles temperature
compared to HVOF technique, which helps mitigating decarburization [5,6].
Hence, a very high particle speed combined with relatively low flame temperature
paves the way for fabrication of extremely dense coatings, with significantly
reduced feedstock material degradation due to thermal effects such as oxidation
and/or decarburization [5,6,29]. Moreover, the desired combination of high
kinetic and low thermal energy makes HVAF a suitable method for spraying
feedstock powders with smaller particle/carbide size which can greatly improve
properties and performance of the fabricated coating [26,30,31]. A comparison of
decarburization ratios of the three APS, HVOF and HVAF spraying routes,
reported in literature, is provided in Table 1. Figure 2 shows where HVAF
technique stands among various thermal spray routes.

4
BACKGROUND

Table 1. Decarburization ratio for APS, HVOF and HVAF processing routes

Deposition method Decarburization Chemistry Ref.


ratio (W2C/WC)
APS 0.2 WC-17Co [32]
APS ≈1 WC-17Co [33]
APS 0.46 WC-Ni [34]

HVOF (JK) 0.7 WC-10Co-4Cr [35]


HVOF (JP 8000) 0.12 WC-10Co-4Cr [35]
HVOF (JP 5000) 0.055 WC-10Co-4Cr [36]
HVOF (DJ) 0.14 – 0.16 WC-10Co-4Cr [37]
HVOF (JP 5000) 0.114 WC-12Co [36]
HVOF (DJ 2700) ≈0.6 WC-12Co [38]
HVOF (DJ 2700) 0.13 WC-12Co [39]
HVOF (HV-2000) 0.25 WC-12Co [39]

HVAF (AK) ≈0 WC-10Co-4Cr [35]


HVAF (M2) ≈0 WC-10Co-4Cr [40]
HVAF (M3) ≈0 WC-12Co [38]
HVAF (Aerospray) 0 WC-12Co [39]

Figure 2. various thermal spray techniques [3].

Figure 3 shows schematic sketch of a typical HVAF gun. In this technique,


compressed air and fuel are blended in mixing chamber and directed into the
combustion chamber through a ceramic insert. Feedstock powder is axially
injected into the combustion chamber, heated up and accelerated through flow
stream in a De-Laval nozzle and subsequently deposited on a target surface. In an
HVAF gun, configuration design of combustion chamber and acceleration nozzle
can be varied. Depending on length of combustion chamber, length of employed
nozzle as well as its convergent-divergent configuration (see Figure 4), various in-

5
flight temperatures and velocities for feedstock particles can be obtained [41]. For
instance, equipping an HVAF gun with convergent-divergent nozzle (named 4L4)
can increase average velocity of WC-CoCr feedstock particles by 120 m/s as
compared to a cylindrical nozzle (named 4L0) [41]. Also, in a study by Lyphout
et al. [42], it was shown that employing nozzles with longer length can lead to
improvement in performance of resultant WC-CoCr coating under abrasion test.

Figure 3. Schematic sketch of a typical HVAF gun

Spraying parameters such as air and fuel pressure, powder feeding rate etc. should
be carefully adjusted depending on the employed gun configuration. Moreover,
as discussed above, different gun configurations can result in varying in-flight
particle velocities/temperatures and consequently affect characteristics of the
fabricated coating. Hence, it is crucial to establish a fundamental understanding
of how different gun configurations can potentially influence the characteristics
and performance of the deposited coating.

6
BACKGROUND

Nozzle Schematic
4L2

4L4

5L2

5L4

Figure 4. Schematics of nozzles used for spraying

2.3 Size range of feedstock powder


Feedstock powders can differ in terms of morphology, carbide and particle size
distribution, and apparent density [15,43]. In HVAF process, in-flight velocity and
temperature of particles can be significantly influenced by their size [2,44]. In a
study by Matikainen et al. [45], it was shown that decreasing WC-CoCr feedstock
size range from 10-30 µm to 5-25 µm can result in an increase in the average
velocity of particles by 30 m/s while their temperature was decreased by 50ºC,
when spraying by HVAF technique. This can potentially affect characteristics and
consequently performance of the resultant coating. Bolelli et al. [12] conducted
sliding and abrasive wear tests on HVAF-sprayed WC-CoCr coatings fabricated
from two different feedstock materials with particle size ranges of 5-30 µm and
15-45 µm, to study influence of particle size on tribological behaviour. In the two
wear conditions of sliding and abrasion, feedstock with finer particle size yielded
superior wear performance. Therefore, prior studies suggest the importance of
role of particle size in governing the coating characteristics, and thereby their wear
behaviour. Hence, the influence of particle size needs to be well-understood in
order to achieve best performance in HVAF sprayed WC-based coatings.

2.4 Alternative binders


Conventionally, Cobalt has been widely used in WC-based coatings to act as
binder [46]. WC-12Co and WC-10Co-4Cr are the two most popular compositions
for thermal spray applications. HVOF-sprayed WC-based coatings with Co-based

7
binder can result in a hard coating with high Vickers hardness value in the range
of 1100 to 1700 HV as well as good fracture toughness of 2.5 to 6 MPam0.5 which
is a desired combination for wear applications [47,48]. However, there are several
environmental and supply risk concerns associated with this element, which have
driven extensive research towards proposing suitable alternatives to Co as binder
for WC-based coatings [10,46]. A possible alternative candidate should not only
meet environmental requirements, but also exhibit promising mechanical
properties and tribological performance. During recent years there have been
several investigations with the attempt to propose non-Co-based binders showing
comparable performance with Co. Ni as a stand-alone binder [49,50], with three
main weight ratios of WC-10Ni, WC-12Ni and WC-17Ni [51], is commercially
available as a binder in thermal spray WC-based coatings. Using this element as
binder can result in a coating system with higher oxidation resistance compared
to Co [52]. Although limited reports are available on wear performance of thermal
spray WC with pure Ni as binder [50,51], there are several on Ni-based binders
proposed as alternatives to Co. For thermal spray, because of poor oxidation
resistance [53] and corrosion resistance of pure Ni as binder [49,54] as-well as its
inferior wear performance compared to WC-CoCr [50,55] it is used typically with
addition of other elements such as chromium or chromium carbides [56,57]. A
list of varied WC-based feedstock compositions, investigated in powder
metallurgy and thermal spray studies, and their specifications that can be found
in the literature is provided in Table 2. In case of HVOF spraying, some Ni-based
and Fe-based binders have been reported to show promising characteristics and
performance. For example, NiMoCrFeCo is one of the Ni-based binders that has
shown comparable performance relative to WC-CoCr as reference [56,58].
Similarly, FeNiCrMoCu and FeCrAl are the two Fe-based binders that have
showed promise [40,56,58]. However, a comprehensive study on mechanical
properties and tribological performance of HVAF sprayed WC-based coatings
with proposed binders seems to be a research gap. Therefore, one of the main
objectives of this thesis is to assess tribological behaviour of proposed Ni and Fe-
based binders including FeCrAl, FeNiCrMoCu and NiMoCrFeCo deposited
using HVAF technique.

8
EXPERIMENTAL PROCEDURE

Table 2. Partial list of varied WC-based feedstock compositions investigated in


powder metallurgy (PM) and thermal spray (TS) literature.

Chemical Formula Composition (%Mass) Particle Sizes (µm) Service Powder Type/Hardmetal Reference
Carbide size Temp.
88WC-12Co Co: 10.5-13 Fe: Max. 0.2 30/5 - 90/45 <500 ºC Agglomerated and sintered/ [26,40,59,60]
C: 5.2-5.6 W: Bal. Fine, Medium, Coarse, Sintered
Very coarse and crushed, (TS)
86WC-10Co4Cr Co: 8.5-11.5 C: 5.0-6.0 15/5 - 45/15 <500 ºC Agglomerated and sintered/ [61–63]
Cr: 3.0-5.0 O: Max. 0.2 Nanometric, Sub-micron, Sintered
Fe: Max. 0.6 W: Bal. Fine, Medium, Coarse and crushed, (TS)
WC-12Ni Ni: 11-13 WC: Bal. 45/15 <500 ºC Agglomerated and sintered, [35,36]
Fe:0.2 Fine (TS)
WC-NiCr - 38/53 - Mechanically milled, (TS) [57,64]
WC-NiMoCrFeCo Ni: 11.0 Fe: 1.0 45/15 - Agglomerated and sintered, [56,58]
Mo: 3.0 Co: Max. 0.8 Medium (TS)
Cr: 2.5 W: Bal.
73WC-20CrC-7Ni Cr: 17-21 Fe: Max. 0.3 30/5 – 53/20 <750 ºC Agglomerated and sintered, [65–67]
Ni: 6.5-8 O: Max. 0.2 Fine (TS)
C: 6.3-7.3 W: Bal.
NiCrWMo Cr: 20.5 Fe: <1 53/11 and 53/20 <875 ºC Gas or water atomized, (TS) [68–70]
W: 10 C: 0.75 -
Mo: 9 B: 0.75
Cu: 4 Ni: Bal.
Cr3C2-37WC C: 8.11 Fe: 0.23 30/10-45/15 <700 ºC Agglomerated and sintered, [71–73]
18NiCoCrFe Ni: 11.63 Cr: 40.74 1.6/0.7 (TS)
Co: 3.63 WC: Bal.
85WC–15(FeCrAl) Fe: 10.79 C: 5.58 45/15 Agglomerated and sintered, [40,56,74]
Cr: 5.58 O: 0.16 Fine (TS)
Al: 1.02 W: Bal.
WC-FeNiCrMoCu Fe: 5.1 Mo: 1.0 45/15 - Agglomerated and sintered, [58]
Ni: 4.6 Cu: 0.2 Fine (TS)
Cr: 4.3 WC: Bal.
WC-10, 20FeNi Fe: 9, 18 WC: Bal. - - Hardmetal, (PM) [75]
Ni: 1, 2
WC-15FeCoNi Fe: 9.75 Ni: 2.25 - - Hardmetal, (PM) [76]
Co: 3 WC: Bal. 0.21±0.12
WC-10FeMn Fe: 9.84, 9.69, WC: Bal. - - Hardmetal, (PM) [75]
9.38, 8.4
Mn: 0.16,
0.31, 0.62, 1,
1.6

3 Experimental procedure

All the experimental steps ranging from spraying processes, microstructural


characterization, material and tribological testing as well as post-test analysis are
provided in this chapter. However, a more detailed explanation on each is
provided in the appended papers: Paper B, Paper C and Paper D.

9
3.1 Spraying samples
Table 3 shows all the feedstock powders sprayed in this study. WC-CoCr
feedstock (as the reference) was used in three different particles size distributions.
Also, there were three more powders with alternative binder chemistries. All the
powders, acquired from Höganäs AB, were manufactured by agglomeration and
sintering procedure. Disk-shaped samples (of diameter 25.4 mm and thickness 6
mm) and rectangular samples (of dimension 50×25×6 mm) made from Domex
355 steel were used as substrates.

Table 3. Specifications of the used feedstock (manufactured by Höganäs AB)

Particle size distribution (µm)


Particle
Chemistry WC size Trade name
size (µm) D 10% D 50% D 90%
WC-CoCr 45/15 22 34 52 Amperit®
86-10-4 558.074
WC-CoCr 30/5 12 19 28 Amperit®

Fine
86-10-4 558.059
WC-CoCr 20/5 6 13 22 Amperit®
86-10-4 558.052
WC-NiMoCrFeCo 18-22 30-38 48-58 Medium Amperit®
82-18 529.074
WC-FeNiCrMoCu 17 28 45 Amperit®
45/15

85-15 531.074
Fine

WC-FeCrAl 17-21 29-37 49-57 Amperit®


85-15 618.074

All the samples were sprayed by a M3 HVAF gun (Uniquecoat Technologies LLC,
USA). As shown in Figure 4, four different nozzles with different configurations
were employed for spraying the feedstock powders. The three powders of the
reference chemistry (WC-CoCr) with different particle size ranges (coarse,
medium and fine) were sprayed using all the four nozzles (4L2, 4L4, 5L2 and
5L4), while the three powders with alternative binder chemistries (of identical size
range) were sprayed with only nozzle 5L2.

All the substrates were cleaned and mounted on a rotating fixture for grit-blasting
and coating. The spray gun was always perpendicular to the surface of samples,
moving up and down. After grit-blasting, the three powders of the reference
chemistry were sprayed with the parameters listed in Table 4. Also, all the powders
with alternative chemistries were deposited following the spraying parameters
listed in Table 5.

10
EXPERIMENTAL PROCEDURE

Table 4. HVAF spraying parameters for the WC-CoCr coatings with three different
particle size ranges

Powder WC-10Co-4Cr WC-10Co-4Cr WC-10Co-4Cr


(coarse) (medium) (fine)
Nozzle 4L2 4L4 5L2 5L4 4L2 4L4 5L2 5L4 4L2 4L4 5L2 5L4
Air (psi) 111 114 113 114 111 114 118 118 111 114 - 118
Fuel 1 (psi) 100 100 105 105 100 100 105 105 100 100 - 105
Fuel 2 (psi) 105 105 115 115 105 105 115 115 105 105 - 115
Carrier (l/min) 40 40 50 50 50 50 50 50 50 50 - 50
Feed (g/min) 200 200 200
SoD (mm) 300 300 300
Number of strokes 11 13 11 11 15 17 16 17 26 29 - 26

Table 5. HVAF spraying parameters for the coatings with different binder chemistries
and identical particle size range of 15-45 µm

(WC-CoCr) (WC-NiMoCrFeCo) (WC-FeNiCrMoCu) (WC-FeCrAl)


Nozzle 5L2
Air (psi) 113 113 113 118
Fuel 1 (psi) 105
Fuel 2 (psi) 115
Carrier (l/min) 50
Feed (g/min) 200
SoD (mm) 300
Number of strokes 11 17 12 14

3.2 Material characterization


Scanning electron microscopy (SEM) was performed on powders as well as the
coatings for microstructural characterization. In order to perform cross-sectional
analysis of powders and coatings under SEM (HITACHI TM3000 microscope,
Krefeld, Germany, and ZEISS GeminiSEM 450, Oberkochen, Germany), the
samples were mounted, ground and polished. Detailed information about
preparation procedure of the samples is provided in Paper B, Paper C and Paper
D.

Roughness of the coatings was measured employing a portable roughness tester


(Surftest 301, Mitutoyo, Japan) as per ASME B46.1-2002 standard. Three
measurements were performed on each sample to measure the average Ra value
with standard deviation.

11
3.3 Micro indentation
Vickers hardness of the coatings was measured by micro indentation tests
performed by micro hardness tester (Struers Duramin-40, Cleveland, United
States) following the procedure explained in the standard ASTM E384 [77]. All
the tests were performed on cross-sections of mirror-polished samples. A total of
fifteen indents were conducted on each sample.

3.4 Tribological tests


Tribological tests under three different wear conditions including sliding wear,
three body abrasion and erosion were performed.

3.4.1 Sliding wear test

Sliding wear tests were conducted using a tribometer rig (Tribometer TRB3,
Anton-Paar, Switzerland) on mirror polished surfaces of the coatings by following
the standard ASTM G99 [78]. Alumina balls of diameter 6 mm were used as
counter body. Friction coefficient evolution during the tests was monitored using
an in-situ sensor. After each test, wear debris was collected from the surface of
the tested sample and studied under SEM. Tested samples were ultrasonically
cleaned from debris so that they are ready for post wear analysis. Post wear
analysis included volume loss measurement along with SEM investigation of wear
tracks. White light interferometry (WLI) technique was employed for measuring
volume loss and calculating specific wear rate of the samples therefrom.

Since the employed Profilm 3D equipment does not provide capability of


scanning the whole wear track, the total volume loss was calculated from
measuring volume loss of four regions (Figure 5). The cross-sectional area of the
wear track at each location was determined by dividing measured volume loss by
length of wear track at each segment measurement. From the four measured
values, an average value for the cross-section area of the whole wear track was
calculated along with standard deviation of the four measurements. Having total
length of the wear track and the average value of cross-section area, the total
volume loss from the wear track (equation (1)) and therefrom the specific wear
rate can be obtained according to equation (2).

12
EXPERIMENTAL PROCEDURE

Figure 5. Schematic sketch of volume loss measurements on wear track on coating

1 𝑉𝑉1 𝑉𝑉2 𝑉𝑉3 𝑉𝑉4 (1)


𝑉𝑉 = (𝜋𝜋. 𝑅𝑅). ( + + + )
2 𝑙𝑙1 𝑙𝑙2 𝑙𝑙3 𝑙𝑙4
𝑉𝑉 (2)
𝑊𝑊 =
𝐿𝐿. 𝑑𝑑

where in equation (1) V1, V2, V3 and V4 are volume losses at the four scanned
locations, l1, l2, l3 and l4 are the lengths of the corresponding wear track segments
and R is radius of the wear track. In equation (3), W is specific wear rate, V is
volume loss, L is load and d is total sliding distance.

Due to intrinsic properties of WC-based coatings i.e., high hardness and


exceptional resistance against wear, the amount of material removed during
sliding wear test is usually extremely low [29,79]. A very shallow wear scar (ranging
from hundreds of nanometres up to couples of micro meters) and consequently
low volume loss and specific wear rate can introduce sensitivities to both selection
of test conditions and the employed measurement procedure. These sensitivities
can be firstly regarding repeatability of the results and also about reliability of
volume loss measurement procedure described above. Therefore, it is crucial to
have a good understanding of the role-playing factors in a ball-on-disk test and
their effect on the sliding wear behaviour of WC-based coatings, conducting a
comprehensive investigation is vital. This helps to establish a reliable testing
routine for HVAF-sprayed WC-CoCr coatings. By performing various tests, the
effect of potential influencing parameters including angular velocity, load and
sliding distance on wear behaviour of WC-based coatings fabricated from WC-
CoCr feedstock, was evaluated to achieve a reliable testing routine (refer to Paper
B).

3.4.2 Erosion wear test

Dry jet erosion tests were conducted using an air jet erosion rig (TR-470 test rig,
DUCOM) on mirror-polished samples. Alumina powder with median size of 50
µm were used as erodent media. The test conditions were listed in Table 6.

13
Erosion test was performed under various test conditions (A, B and C). Mass loss
for eroded samples were measured and reported in case of test conditions A and
B. However, because of very wide and shallow pits, it was not possible to measure
volume loss in the cases of test conditions A and B. Therefore, the velocity and
time duration of the test was optimized (test conditions C) in a way that
circumference length of the pit is small enough that provides the possibility of
volume loss measurement by using WLI technique. Each test was repeated three
times and mass loss along with erosion rate, calculated based on volume loss, were
reported. Also, both top surface and cross section of eroded regions were
investigated by SEM.

Table 6. Jet erosion test conditions for volume loss measurement

A B C
Erodent particle size (µm) 50 50 50
Particle velocity (m/s) 30 30 70
Impingement angle (degree) 90 45 90
Duration (min) 10 10 4
Erodent feed rate (g/min) 2 2 2
Standoff distance (mm) 10 10 10
Nozzle diameter (mm) 1.5 1.5 1.5

3.4.3 Abrasion wear test

Dry sand-rubber wheel tests were conducted on the rectangular samples


according to the ASTM G-65 standard [80]. The samples were exposed to three
body abrasion testing in their as-deposited state. Silica Quartz sand with particle
size range of 100 µm – 700 µm was employed as third body abradant. Overall test
duration was 30 min for each sample. The samples were weighed after 10 min
intervals. Other test conditions used in the test are provided in Table 7. Top
surface and cross section of eroded regions were investigated using SEM.

Table 7. Dry sand-rubber wheel test conditions

Parameter Value
Abradant particle size (µm) 100-700
Load (N) 130
Wheel rotational speed (rpm) 200
Erodent feed rate (g/min) 315
Duration (min) 3*10

14
SUMMARY OF RESULTS

4 Summary of results

In this chapter, the attempt is to summarize the main results in a way to answer
the research questions.

4.1 Coating characterization


Uniform and dense coatings were achieved by HVAF method in all the cases.
Homogeneity and density of the coatings do not experience considerable changes
when using various nozzles (Paper C) or when spraying alternative binders
employing the same nozzle (Figure 6). However, as shown in Figure 7, by decrease
in feedstock particle size, homogeneity and density of the deposited coatings
exhibit a substantial improvement (Also see Paper C). Since the overall porosity
content in HVOF/HVAF spray WC-based coatings is less than 1 per cent [81,82],
a quantitative porosity measurement of these coatings is challenging. Hence, the
aforementioned conclusions are drawn based on qualitative SEM analysis.

WC-CoCr WC-NiMoCrFeCo WC-FeNiCrMoCu WC-FeCrAl


Figure 6. Cross-sectional BSE-SEM images of the four coatings with different binder
chemistry

Coarse Medium Fine


Figure 7. Cross-sectional BSE-SEM images of WC-CoCr coatings with three different
particle sizes

Employing various nozzles did not considerably influence hardness of coatings


deposited using a given feedstock, while its value experienced a considerable

15
increase by approximately 400 HV0.3 when powder particle size is reduced (paper
C). Also, the Vickers hardness of all the four coatings with alternative binders was
in the relatively narrow range of 1100 HV0.3 and 1300 HV0.3, with WC-CoCr
accounting for the highest and WC-FeCrAl for the lowest hardness (paper D).

Referring to XRD analysis performed in both the Paper C and Paper D, no


considerable phase change was found to occur in any of the coatings sprayed by
HVAF technique regardless of the feedstock particle size or the nozzle
configuration used for spraying.

4.2 Test parameters for ball-on-disk experiment


As explained in Paper B, a comprehensive investigation was conducted to
establish a practical testing procedure which inspires confidence in the test
conditions utilized to rank different WC-based coatings. By running fifteen tests
on three samples at various wear track radii between 5 – 9 mm, it was shown that
no significant difference is noted in specific wear rate with change in radius from
5 mm up to 9 mm (angular velocity from 1333 rpm up to 2400 rpm), in a way that
the difference in smaller than precision of measurement method itself. Also,
increasing the normal load up to 40 N showed no major change in specific wear
rate or deviation of different specific wear rate values obtained from various
repetitions. Moreover, increase in sliding distance up to 10 km while the applied
load is fixed at 20 N did not show considerable change in specific wear rate
and/or values deviation when compared to other used test conditions (Paper B).
All these were rooted from no major change in dominant wear mechanisms or
wear regime of sprayed WC-CoCr coatings under this window of test conditions.

After performing several tests runs with various test conditions, a ball-on-disk test
under 20 N normal load, 5 km sliding distance and 20 cm/s performed with
angular velocity between 1333 rpm to 2400 rpm seemed to offer a reliable testing
routine to rank various coatings fabricated in terms of difference in processing
parameters, particle size and binder chemistries. In all the cases the specific wear
rate values were fell between 1 to 1.9 × 10-8 mm3.N-1.m-1.

4.3 Influence of process variables


4.3.1 Wear performance

Influence of spraying parameters (by using four different nozzles) along with
effect of particle size (by employing three different size ranges of WC-CoCr
powder) on sliding wear performance of deposited coatings were evaluated.

16
SUMMARY OF RESULTS

While no clear trend was identified for the coating obtained from coarse powder
(Pc), coatings from fine powder (Pf) performed better when using nozzle 4L4 or
5L4 instead of 4L2. On the other hand, wear performance of the coatings
fabricated from medium powder (Pm) showed negligible sensitivity to the
selection of nozzle configuration (Figure 8) in a way that all the four coatings were
showed to have a relatively similar performance.

When considering reduction in particle size for a given nozzle, moving to finer
powder size range from Pc to Pm, regardless of the nozzle type, the average value
of specific wear rate of the coatings was decreased. Further decreasing particle
size (Pm to Pf) leads to further decrease in specific wear rate of the coatings
sprayed employing 4L4 and 5L4. Pf sprayed by 5L4 showed to exhibit the most
excellent resistance against wear.

Figure 8. Specific wear rate of the coatings fabricated from three different particle size
range sprayed with four different nozzles (Paper C)

4.3.2 Wear mechanism

Influence of process variables including nozzle configuration and particle size on


wear behaviour of deposited WC-CoCr coatings is discussed in this section. As
described in Paper C; for every given powder sprayed with different nozzles; no
significant difference was observed in sliding wear behaviour and associated
material removal mechanisms. However, wear mechanism of the WC-CoCr
coatings differs depending on the used powder sizes including coarse (Pc),
medium (Pm) and fine (Pf). Decrease in particle size led to a considerable change
in wear behaviour of the corresponding coating. As shown in Figure 9, wear
mechanism for Pc coatings started from crack propagation around defects within
coatings leading to breakage of batches of coating material into the pit areas.

17
Further sliding of the ball possibly caused fragmentation and removal of these
particles in which could act as third body particles and led to formation of
relatively deep grooves on the surface. As shown in Figure 10 (a) and (b), in Pm
and Pf coatings, no pits were observed. In these two coatings, wear process
seemed to start with removal of binder and consequently fracture and
fragmentation of loosely bounded individual carbides and as a result removal of
submicron carbides.

This difference in removal mechanism can be initiated from the higher number
of defects in form of pores and binder accumulations in Pc coatings, as was
described in 4.1. SEM analysis on debris particles (Paper C) confirmed this
difference as debris for Pc coatings were much coarser as compared to Pm and
Pf.

Figure 9. Breakage mechanism in Pc coatings: breakage of group of carbides into the


adjacent pit (Paper C)

18
SUMMARY OF RESULTS

Figure 10. removal mechanisms in Pm and Pf coatings, a) Pm, b) Pf (Paper C)

4.4 Influence of binder chemistry


Wear performance of HVAF-sprayed WC-based coatings with four different
binder chemistries (see Table 3) was evaluated by exposing them to various wear
environments including sliding, erosion and abrasion.

4.4.1 Performance under sliding wear

Figure 11 shows average specific wear rates along with the standard deviation of
the four coatings (WC-CoCr, WC-NiMoCrFeCo, WC-FeNiCrMoCu and WC-
FeCrAl) under sliding wear test. The wear rate for all the four coatings is in the
order of 10-8 mm3.N-1.m-1, which is considered to be extremely low. The coating
WC-NiMoCrFeCo is clearly showing the best performance, while the coating
WC-FeCrAl shows the least resistance against wear under sliding wear conditions.

20
18
Specific wear rate (mm3/(N.m)), 10-8

16
14
12
10
8
6
4
2
0
WC-CoCr WC-NiMoCrFeCo WC-FeNiCrMoCu WC-FeCrAl

Figure 11. Specific wear rate of the four coatings, with different binder chemistries,
obtained from ball-on-disk testing (Paper D)

19
4.4.2 Sliding wear mechanisms

As was shown in previous sections, chemistry of binder can affect performance


of coatings under sliding wear. Post wear analysis showed that binder chemistry
can greatly influence material removal mechanism of coatings when testing under
sliding wear conditions. Figure 12 shows SEM micrographs, with three different
magnifications, of wear tracks of the four coatings WC-CoCr, WC-NiMoCrFeCo,
WC-FeNiCrMoCu and WC-FeCrAl. Formation of pits (dark areas) on top surface
of the samples WC-CoCr and WC-FeNiCrMoCu clearly indicate local
delamination of coatings material. Looking at the SEM images it is noticeable
that the occurrence frequency of these pits in the sample WC-CoCr is clearly
greater than the coating WC-FeNiCrMoCu. There is no detectable sign of pitting
in the coating WC-NiMoCrFeCo and negligible number of them in the coatings
WC-FeCrAl which are remarkably smaller in size compared to the ones on
samples WC-CoCr and WC-FeNiCrMoCu. This is while pitting of these two
coatings too was found in other studies [58,83] when they are sprayed by HVOF.

20
SUMMARY OF RESULTS
WC-CoCr
WC-NiMoCrFeCo
WC-FeNiCrMoCu
WC-FeCrAl

Figure 12. SEM micrographs of worn surfaces of the four coatings WC-CoCr,
WC-NiMoCrFeCo, WC-FeNiCrMoCu and WC-FeCrAl with three different
magnifications

4.4.3 Performance under erosion wear

According to Table 6, jet erosion tests were conducted under three test conditions
of A (particle velocity: 30 m/s, time: 10 min, impact angle: 90º), B (particle
velocity: 30 m/s, time: 10 min, impact angle: 45º) and C (particle velocity: 70 m/s,
time: 4 min, impact angle: 90º). Figure 13 shows mass loss and erosion rate of the
four coatings under the three jet erosion test conditions A, B and C. For test
conditions A and B, WC-CoCr and WC-NiMoCrFeCo accounts for the least and
the highest average amount of mass loss, respectively. However, the overlap in
error bars (indicating standard deviation) prevents a clear ranking based on the
results from these two test conditions. From the erosion rate of the four coatings,
it is clear that coating WC-CoCr shows the most superior performance against
erosive wear while WC-NiMoCrFeCo exhibits the least resistance to dry jet
erosion. WC-FeNiCrMoCu and WC-FeCrAl coatings, on the other hand, seem to
have similar behaviour under erosive wear environment.

21
A-Mass loss B-Mass loss C-Mass loss C-Erosion rate
8
Mass loss (mg) & Erosion rate (mm3/g), 10-2
7

0
WC-CoCr WC-NiMoCrFeCo WC-FeNiCrMoCu WC-FeCrAl

Figure 13. Erosion rate and mass loss of the four coatings under test conditions of A,
B and C (Paper D)

4.4.4 Erosion wear mechanisms

Post wear analysis on erosion pits showed that binder chemistry can slightly
influence material removal mechanism of coatings when testing under erosion
wear conditions. Figure 14 shows images of surface morphology of erosion pits
at three different magnifications SEM for the four coatings with different binder
chemistries under test condition A. Looking at the low magnification images, a
smooth surface with lower number of pits and bulges is observable in the coating
WC-NiMoCrFeCo. Protuberances in all the other three coatings look roughly
similar. Looking at medium magnification images, removal mechanisms of the
coating exposed to erosion wear conditions can be identified. Four main removal
mechanisms including pitting (I), ploughing (II), shovelling (III) and chipping
(IV) were detectable on all the surfaces [84]. The three coatings WC-CoCr, WC-
FeNiCrMoCu and WC-FeCrAl exhibit mostly similar behaviour.

22
SUMMARY OF RESULTS
WC-CoCr
WC-NiMoCrFeCo
WC-FeNiCrMoCu
WC-FeCrAl

Figure 14. Morphology of the erosion pits for the four coatings tested under A test
condition (Paper D).

4.4.5 Performance under abrasive wear

Figure 15 shows mass loss of the four WC-Co based HVAF coatings with
different binder chemistries when exposed to dry sand rubber-wheel abrasion
wear test. WC-CoCr coating shows the best performance under all the coatings
followed by WC-NiMoCrFeCo, WC-FeNiCrMoCu and finally WC-FeCrAl. It
can be seen that, for all the coatings, the slope of the mass loss vs. time plot is
higher in the first 10 minutes of the test. This could be because of the surface
asperities present in the as-sprayed samples resulting in higher rate of material loss
during early stages of the test. Continuing the tests for two further 10-minute
intervals, the slope of the mass loss is observed to dramatically decrease and
remain almost the same for these last two stages of the test, thereby suggesting
that steady state situation may have been achieved. Nearly same slopes for all the
coatings between 10-30 min indicate that steady state wear rate is approximately
the same for all the 4 coatings.

23
WC-CoCr WC-NiMoCrFeCo WC-FeNiCrMoCu WC-FeCrAl
18
16
14
12
Mass loss (mg)

10
8
6
4
2
0
0 5 10 15 20 25 30
Time (min)

Figure 15. Abrasive performance of the four coatings (Paper D)

24
CONCLUSIONS AND FUTURE WORKS

5 Conclusions and future works

5.1 Summary and conclusions


This study was conducted with the aim of understanding the influence of binder
chemistry and process variables on characteristics and behaviour of HVAF-
sprayed WC-based coatings. The main findings of this study are summarized in
the following three categories, which are answers to the research questions RQ1,
RQ2 and RQ3;

RQ1: Influence of process variables on characteristics and performance:

- Reduction in particle size leads to increase in density and homogeneity


and subsequently hardness value of the coating. No considerable
difference was observed when employing various nozzles to deposit
coatings which affirms the reliability and robustness of the HVAF
technique.
- All these result in general a better wear performance of the coatings by
decreasing in feedstock particle size.

RQ2: Characteristics and performance of alternative binders:

- Comparable hardness values were obtained for all the alternative binders
compared to the reference Co.
- Superior or comparable performance for FeNiCrMoCu and
NiMoCrFeCo binders were achieved compared to the reference Co-
based under sliding wear conditions. Comparable erosion and abrasion
performance of the FeCrAl binder were obtained when comparing the
reference Co-based and other alternatives.

RQ3: Tribological behaviour:

- Ploughing, grooving and pitting are the main removal mechanisms in


coarse feedstock coating (Pc), while ploughing is the only dominant main
wear mechanisms in medium (Pm) and fine (Pf) feedstock coatings when
testing under sliding wear conditions.
- Dominant wear mechanisms for the reference WC-CoCr coating under
sliding wear test was deep grooving, excessive cracking and consequently
pitting. This is while no material removal in form of pitting were
observed for the coatings WC-NiMoCrFeCo and WC-FeCrAl under
sliding wear test, instead material ploughing was the only dominant

25
mechanism. WC-NiMoCrFeCo shows slightly different behaviour in
terms of erosion mechanism.

5.2 Future works


In order to establish a better understanding of behaviour of WC-based coatings
with alternative binders, more investigations will be conducted on mechanical
properties including measurement of hardness of different binders using
nanoindentation. Tribological performance of the coatings will be evaluated
under other wear conditions including slurry abrasion and high temperature
sliding wear. Moreover, studies will be performed on coatings with reduced
thickness (~ 50 µm). Capabilities of HVAF method, such as lower temperature
and higher velocity compared to other methods resulting in extremely dense
coatings, make it possible to produce coatings with reduced thickness utilizing
powders with a finer feedstock particle size that could potentially show similar
performance as the conventional thicker coatings. Reducing coatings’ thickness
to 50 µm can significantly cut feedstock and operation costs and impact economic
viability. The coatings will be comprehensively characterized for microstructure
and mechanical properties and their performance under different wear conditions
will also be studied and compared with regular thick (~200 um) coatings.

26
6 References

[1] H.E. Boyer, T.L. Gall, Metals handbook; desk edition, (1985).

[2] J.R. Davis, Handbook of thermal spray technology, ASM international,


2004.

[3] B.G. Mellor, Surface coatings for protection against wear, Woodhead
publishing limited, 2006. https://doi.org/10.1533/9781845691561.

[4] X. Luo, R. Chidambaram-Seshadri, G.-J. Yang, Micro-Nanostructured


Cermet Coatings, Elsevier Inc., 2019. https://doi.org/10.1016/b978-0-
12-813870-0.00004-8.

[5] O. Lanz, B. Gries, HVAF - Chance and challenge for users and for powder
producers, Proc. Int. Therm. Spray Conf. 2019-May (2019) 15–22.

[6] C. Lyphout, K. Sato, S. Houdkova, E. Smazalova, L. Lusvarghi, G. Bolelli,


P. Sassatelli, Tribological Properties of Hard Metal Coatings Sprayed by
High-Velocity Air Fuel Process, J. Therm. Spray Technol. 25 (2016) 331–
345. https://doi.org/10.1007/s11666-015-0285-4.

[7] K. Torkashvand, M. Gupta, S. Björklund, F. Marra, L. Baiamonte, S. Joshi,


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35
Paper
PaperBB
Influence
Influenceofoftest
testconditions
conditionson
onsliding
sliding
wear
wearperformance
performanceofofhigh
highvelocity
velocityair
airfuel-
fuel- BB
sprayedWC-CoCr
sprayed WC-CoCrcoatings
coatings
Kaveh
KavehTorkashvand,
Torkashvand,Vinod
VinodKrishna
KrishnaSelpol,
Selpol,Mohit
MohitGupta,
Gupta,
ShrikantJoshi
Shrikant Joshi

Published:
Published:”Materials”
”Materials”

MDPI,June
MDPI, June2021
2021

Published
Publishedwith
with
Creative
Creative
Commons
Commons
license:
license:
CCCC
BYBY
4.04.0
materials
Article
Influence of Test Conditions on Sliding Wear Performance of
High Velocity Air Fuel-Sprayed WC–CoCr Coatings
Kaveh Torkashvand * , Vinod Krishna Selpol, Mohit Gupta and Shrikant Joshi

Department of Engineering Science, University West, 46186 Trollhättan, Sweden; vinodselpol@gmail.com (V.K.S.);
mohit.gupta@hv.se (M.G.); shrikant.joshi@hv.se (S.J.)
* Correspondence: kaveh.torkashvand@hv.se; Tel.: +46-(0)-520223375

Abstract: Sliding wear performance of thermal spray WC-based coatings has been widely studied.
However, there is no systematic investigation on the influence of test conditions on wear behaviour
of these coatings. In order to have a good understanding of the effect of test parameters on sliding
wear test performance of HVAF-sprayed WC–CoCr coatings, ball-on-disc tests were conducted
under varying test conditions, including different angular velocities, loads and sliding distances.
Under normal load of 20 N and sliding distance of 5 km (used as ‘reference’ conditions), it was
shown that, despite changes in angular velocity (from 1333 rpm up to 2400 rpm), specific wear rate
values experienced no major variation. No major change was observed in specific wear rate values
even upon increasing the load from 20 N to 40 N and sliding distance from 5 km to 10 km, and
no significant change was noted in the prevailing wear mechanism, either. Results suggest that no
dramatic changes in applicable wear regime occur over the window of test parameters investigated.
Consequently, the findings of this study inspire confidence in utilizing test conditions within the
 above range to rank different WC-based coatings.


Citation: Torkashvand, K.; Selpol, Keywords: tests conditions; sliding wear; HVAF; WC–CoCr; ball-on-disk; wear mechanism
V.K.; Gupta, M.; Joshi, S. Influence of
Test Conditions on Sliding Wear
Performance of High Velocity Air
Fuel-Sprayed WC–CoCr Coatings.
1. Introduction
Materials 2021, 14, 3074. https://
doi.org/10.3390/ma14113074 WC-based cermet coatings sprayed using high velocity thermal spray techniques are
one of the most common protective layers employed in industry for wear applications [1,2].
Academic Editor: Andrzej Dziedzic They are expected to resist various wear environments, namely erosive wear, abrasive wear,
fretting wear, fatigue and sliding wear [1,3]. There are several standardized test procedures
Received: 28 April 2021 to simulate different wear environments, including ASTM G76 [4] for erosive, ASTM G65 [5]
Accepted: 2 June 2021 for abrasive and ASTM G99 [6] for sliding wear conditions. Ball-on-disk is one of the most
Published: 4 June 2021 commonly employed tests to assess sliding wear performance of WC-based coatings [7,8].
In this test, however, there are several parameters that can potentially affect the results. It is
Publisher’s Note: MDPI stays neutral known that a minor change in the contact conditions can influence the process of material
with regard to jurisdictional claims in removal in a tribosystem [9]. Bayer [10] remarks that “Wear is not a material property.
published maps and institutional affil- It is a system response”, and this clearly highlights the importance of test conditions in
iations. a wear experiment. A sliding ball-on-disk test can result in different contact conditions
depending on applied load, the material of the mating surfaces, hardness and size of the
produced debris, which can potentially lead to changes in material removal mechanisms
and, consequently, test results [11,12]. Occasionally, laboratory testing also compels conduct
Copyright: © 2021 by the authors. of multiple tests on a single specimen by varying the wear track radii [13,14]. For a given
Licensee MDPI, Basel, Switzerland. sliding distance, such tests inevitably lead to varying linear sliding velocities as well as
This article is an open access article different number of contact incidents at a specific location. The influence of the above on
distributed under the terms and the test outcome also needs to be well understood. Further, it is pertinent to mention that
conditions of the Creative Commons the influence of test conditions on results could be material-specific. This is expected, since
Attribution (CC BY) license (https:// the threshold for a dramatic change in wear regime is expected to be intimately related to
creativecommons.org/licenses/by/
the materials being tested.
4.0/).

Materials 2021, 14, 3074. https://doi.org/10.3390/ma14113074 https://www.mdpi.com/journal/materials


Materials 2021, 14, 3074 2 of 14

Performing ball-on-disc tests on thermally sprayed WC-based coatings typically re-


sults in a very shallow volume loss and, as a result, extremely low specific wear rate
(in order of 10−8 –10−9 mm3 ·N−1 ·m−1 ) [15,16]. This extremely low material removal in-
troduces potential sensitivities to selection of test conditions as well as measurement
procedure. As stated in the standard [6], chosen test parameters can influence precision
of measurement as well as repeatability of test results. Particularly, great precision is
required when volume loss is extremely low, as typically in the case of WC-based coatings.
According to the standard ASTM G99, linear measures of wear scar should at least have
a sensitivity of 2.5 µm. However, the depth of a typical wear track in a ball-on-disc test
can be below 1 µm [17,18], which demands a higher measurement sensitivity than that
stated in the standard. Generally, in a ball-on-disk test, applied load, test duration and
sliding speed are the three main parameters that can potentially influence test results,
particularly in terms of material loss and coefficient of friction. Some studies can be found
in literature studying influence of these test parameters [19–22]. Based on the selected
test parameters, two main regimes can be achieved during sliding wear test, namely mild
wear and severe wear [1,23]. A transition is known to happen in wear regime from mild
to severe by increasing load and/or sliding speed or running the test for longer distances.
For instance, it has been shown in some studies [24,25] that a full transition in wear regime
can occur in the case of HVOF-sprayed WC–Co samples when increasing the normal
load from 19 to 35 N, resulting in a substantial increase in specific wear rate. Moreover,
Wang et al. [26] performed ball-on-disk tests on high velocity oxy-fuel (HVOF)-sprayed
WC–CoCr coatings at many different loads in the range 15 N–90 N for same test duration,
sliding speed and ball material. They concluded that, despite a huge change in the applied
load, the friction coefficient during the steady state period fluctuated in a small range
of 0.3–0.4. However, their results showed that the mechanism of material removal can
greatly change from carbide pull-outs to massive material exfoliation, depending on the
applied load. Moreover, specific wear rate experienced a substantial increase by a factor
of 102 (from 3.6 × 10−8 to 3.5 × 10−5 mm3 ·N−1 ·m−1 ). Karaoglanli et al. [27] studied wear
behaviour of HVOF WC–Co coatings, employing the ball-on-disk test under loads of 5 N
and 15 N and sliding speeds of 10 and 20 cm/s for the same test duration and ball material.
It was shown that an increase in sliding speed resulted in higher specific wear rate, while
the wear rate decreased on increasing the normal load from 5 N to 15 N. Although these
studies provide an understanding of the influence of test conditions on wear behaviour
of WC–CoCr coatings, there is no published report systematically investigating the effect
of all the aforementioned parameters on wear performance of WC-based coatings. In this
study, we tried to fill this research gap by conducting a systematic study on wear behaviour
of WC-based coatings under various wear conditions.
In order to have a good understanding of the role-playing factors and their effects on
the sliding wear behaviour of WC-based coatings, conducting a comprehensive investiga-
tion is vital. This helps to establish a reliable testing routine for HVAF-sprayed WC–CoCr
coatings. In this study, the effects of potential influencing parameters including angular
velocity, load and sliding distance on wear behaviour of WC-based coatings, fabricated
using high velocity air fuel (HVAF) spraying, are systematically evaluated and discussed.

2. Experimental Procedure
2.1. Deposition of Coating
Commercially available 86WC–10Co–4Cr powder manufactured employing agglom-
eration and sintering technique (trade name: Amperit® 558.059, Höganäs GmbH, Goslar,
Germany) was used as feedstock. Characteristics of the used powder are provided in
Table 1. Domex 355 coupons of 25.4 mm diameter and 6 mm thickness were used as sub-
strate. All the samples were degreased and mounted on a fixture rotating with a 1.66 m/s
linear speed. The samples were grit blasted with alumina particles of average size 220 µm
sprayed with the HVAF gun, resulting in a surface roughness (Ra) of approximately 4 µm.
The grit-blasted substrates were then coated using a 5L2 convergent–divergent nozzle with
Materials 2021, 14, 3074 3 of 14

an M3 HVAF torch (Uniquecoat Technologies LLC, Oilville, VA, USA). Spray parameters
for grit-blasting and coating, both carried out using the above torch, are listed in Table 2.

Table 1. Characteristics of WC–CoCr feedstock powder.

Composition (% Mass) Particle Size Range (µm) Carbide Size Service Temp. (◦ C)
Co: 8.5–11.5 C: 5.0–6.0
5/30 fine <500
Cr: 3.0–5.0 W: Bal.

Table 2. Grit-blasting and spraying parameters employed.

Air Fuel 1 Fuel 2 Carrier Feed SoD Number


Gun/Nozzle
(psi) (psi) (psi) (L/min) (g/min) (mm) of Strokes
Grit-blasting M3/5L2 110 100 80 60 ≈100 350 2
WC–CoCr M3/5L2 118 105 115 50 200 300 16

2.2. Coating Characterization


Coated samples were ground and polished for microstructural characterization of
coating cross-sections and hardness measurements. Surfaces of coated samples were also
polished prior to wear testing. Following grinding using a 45 µm diamond disk, three steps
of polishing were performed successively with 9 µm and then 3 µm Kemet liquid diamond
media, followed by MasterMet 2 dispense to reach a mirror-polished state corresponding
to Ra value less than 0.01 µm. General microstructure analysis of the coatings as well
as post-wear analysis on wear scars were performed by scanning electron microscopy
(SEM) (HITACHI TM3000 microscope, Krefeld, Germany, and ZEISS GeminiSEM 450,
Oberkochen, Germany).
Vickers hardness measurement of the coating was conducted employing Struers
Duramin-40 microhardness tester. Following the standard ASTM E384 [28], a total of
fifteen indentations were performed on coating specimens.

2.3. Ball-on-Disk Sliding Tests


Samples were exposed to sliding wear employing a ball-on-disk testing rig (Tribometer
TRB3, Anton-Paar, Buchs, Switzerland) following the procedure of the standard ASTM G99.
The tests were conducted on mirror-polished samples. Three parameters, namely angular
velocity, load and sliding distance, were varied (see Table 3). A test run conducted at 20 N
of normal load for 5000 m of sliding distance with a linear speed of 0.2 m/s was selected as
the reference. All the test runs were performed at a constant linear speed of 0.2 m/s, which
resulted in various angular velocities corresponding to 2400, 2000, 1700, 1500 and 1333 rpm
when the radii of the wear tracks, made by the sliding ball on the coating surface, were
set to 5, 6, 7, 8 and 9 mm, respectively. That Alumina ball of radius 6 mm was used as the
mating material in all cases.
For each set of tests to assess parametric impact on ensuing results, the parameter of
interest was systematically varied compared to the reference run mentioned above. The
angular velocity was changed by varying the wear track radius and keeping the linear
speed constant during the tests. All the tests conducted to assess influence of angular
velocity (Figure 1a) were repeated three times at each wear track radius on three different
samples (S1, S2 and S3). Figure 1b shows a typical sample after testing on radii of 5, 7 and
9 mm. For the set of tests using the load as variable parameter, the normal applied load was
varied between 20 N and 40 N. Due to limitation in the testing rig, it was not plausible to
increase the load beyond 40 N. In yet another, the sliding distance was increased to 10 km
from 5 km. Finally, in one particular run, both load and distance were simultaneously
increased to 30 N and 10 km, respectively. The tests with load and distance as variables
were conducted on radii of 7 and 8 mm. This was done since the outcome of the tests of
different radii (see Section 3.2) has already established that the wear track radius does not
influence the specific wear rate.
R9 (S1/S2/S3) 9 20 5
L20D5 7 and 8 20 5
L30D5 7 and 8 30 5
Load
L35D5 7 and 8 35 5
L40D5 7 and 8 40 5
Materials 2021, 14, 3074 Distance L20D10 7 and 8 20 10 4 of 14

Load and distance L30D10 7 and 8 30 10


Table Testset
For3.each parameters employed
of tests to during sliding
assess parametric wear on
impact tests.
ensuing results, the parameter of
interest was systematically varied compared to the reference run mentioned above. The
Variable Parameter Code Radius (mm) Load (N) Distance (km)
angular velocity was changed by varying the wear track radius and keeping the linear
R5 (S1/S2/S3) 5 20
speed constant during the tests. All the tests conducted to assess influence of angular 5 ve-
R6 (S1/S2/S3) 6 20 5
locity (Figure 1a) were repeated three times at each wear track radius on three different
Angular velocity R7 (S1/S2/S3) 7 20 5
samples (S1, S2 and S3). Figure 1b shows a typical sample
R8 (S1/S2/S3) 8 after testing
20 on radii of 5,5 7 and
9 mm. For the set of tests using the load as variable9 parameter, the
R9 (S1/S2/S3) 20normal applied 5 load
was varied between 20 N and 40L20D5 N. Due to limitation in the testing rig,
7 and 8 20
it was not plausible
5
to increase the load beyond 40 N. In yet another,7the
L30D5 andsliding
8 distance
30 was increased 5 to 10
km from 5 km.Load Finally, in one particular run, both7 load
L35D5 and 8and distance 35were simultaneously
5
increased to 30 N and 10 km, respectively.
L40D5 The tests
7 andwith
8 load and 40distance as variables
5
were conducted
Distance on radii of 7 and 8 mm. This was
L20D10 done
7 and 8 since the outcome
20 of the 10
tests of
different radii (see Section 3.2) has already established that the wear track radius does not
Load and distance L30D10 7 and 8 30 10
influence the specific wear rate.

(a) (b)
Figure 1. (1.
Figure a) (a)
Schematic diagram
Schematic diagramof of
different
differentradii
radiiand
anddistinct
distinctlocations
locationsfor
for volume
volume loss measure-
loss measurements
ments on the
on the testing
testing samples,
samples, andand
(b) a(b) a typical
typical sample
sample afterafter ball-on-disk
ball-on-disk test.test.

Sliding data
Sliding such
data suchasasfriction
frictionforce
forceandand friction coefficientwere
friction coefficient werecontinuously
continuouslymonitored
moni-
tored during
during the the tests.
tests. After
After eacheach
test, test, the samples
the samples werewere ultrasonically
ultrasonically cleaned
cleaned and theand the
volume
volume loss measured
loss measured employing
employing whiteinterferometry
white light light interferometry (WLI) method
(WLI) method (Profilm(Profilm 3D,
3D, Filmetrics,
Filmetrics, Unterhaching,
Unterhaching, Germany). Germany). The measurement
The measurement was performed
was performed at fourlocations
at four different differenton
locations
the wearontrack,
the wear track, in
as shown as Figure
shown1a. in Figure 1a. The cross-sectional
The cross-sectional area of thearea
wearoftrack
the wear
at each
track at each
location waslocation was by
determined determined by dividing
dividing measured measured
volume loss byvolume
length ofloss
wearby track
lengthat of
each
wear track at
segment each segmentApproximate
measurement. measurement. arcApproximate
length of eacharc length is
segment of1.75
eachmm.
segment
Fromisthe 1.75
four
mm. From the
measured four measured
values, an averagevalues,
value foran theaverage value for
cross-section theofcross-section
area the whole wearareatrack
of thewas
whole wear track
calculated alongwas calculated
with standardalong with of
deviation standard
the fourdeviation of the four
measurements. measurements.
Having total length of
the wear track and the average value of cross-section area, the total volume loss from the
wear track (Equation (1)), and therefore, the specific wear rate, can be obtained according
to Equation (2).  
1 V1 V V V
Vloss = (π.R). + 2+ 3+ 4 (1)
2 l1 l2 l3 l4
Vloss
W= (2)
L.d
where in Equation (1) V 1 , V 2 , V 3 and V 4 are volume losses at the four locations shown in
Figure 1a; l1 , l2 , l3 and l4 are the corresponding arc length of the segments; and R is radius
of the wear track. L and d in Equation (2) are the applied normal load and total sliding
distance, respectively.
𝑉𝑉����
𝑊𝑊 𝑊 (2)
𝐿𝐿𝐿 𝐿𝐿
where in Equation (1) V1, V2, V3 and V4 are volume losses at the four locations shown in
Figure 1a; l1, l2, l3 and l4 are the corresponding arc length of the segments; and R is radius
Materials 2021, 14, 3074 of the wear track. L and d in Equation (2) are the applied normal load and total sliding 5 of 14
distance, respectively.

3. 3.
Results and
Results Discussion
and Discussion
3.1. Coatings
3.1. Coatings Characterization
Characterization
Figure
Figure 2 shows
2 shows low
lowand
and high
highmagnification
magnification images
images ofofthe
theWC–CoCr
WC–CoCr coating
coating used
used
throughout
throughout thisthis study.It It
study. cancanbebe
seenseen that
that a auniform
uniformand anddense
denseWC–CoCr
WC–CoCrcoating coatingis is
achieved
achieved byby thethe HVAFHVAF method.
method. Although
Although there
there areare some
some submicron
submicron pores
pores (as(as indicated
indicated
in in Figure
Figure 2) 2) noted
noted inin the
the coating,
coating, thethe overall
overall porosity
porosity content
content is is less
less than
than 1 percent
1 percent and
and
comparable
comparable with with literature
literature [7,8].
[7,8]. Vickers
Vickers hardness
hardness value
value forfor
thethe coating
coating measured
measured toto
bebe
1410
1410 ± 27
± 27 HVHV 0.3. 0.3
All . All
thethe coating
coating specimens
specimens utilized
utilized forfor subsequent
subsequent ball-on-disk
ball-on-disk wear
wear tests
tests
weresimultaneously
were simultaneouslyHVAF HVAF sprayed
sprayed to to ensure
ensureminimal
minimalvariation,
variation,and andthethe
influence
influenceof each
of
testtest
each parameter
parameter on onensuing results
ensuing is individually
results is individuallydiscussed
discussed below.
below.

(a) (b)
Figure 2. SEM
Figure images
2. SEM of of
images cross-sections of of
cross-sections deposited coatings
deposited at at
coatings (a)(a)
low magnification
low and
magnification (b)(b)
and high magnification.
high magnification.

3.2. Influence
3.2. of of
Influence Angular Velocity
Angular onon
Velocity Wear Behaviour
Wear Behaviour
3.2.1.
3.2.1. Local
Local Variations
Variations within
within a Wear
a Wear Track
Track
AccordingtotoTable
According Table 3,
3, identical
identical coating
coatingspecimens
specimenswere were subjected
subjectedto ball-on-disk
to ball-on-disktests,
withwith
tests, the the
track radius
track being
radius the only
being variable.
the only As mentioned
variable. As mentioned in Section 2.3, 2.3,
in Section specific wear
specific
rates
wear are are
rates calculated
calculated based
basedon on
four local
four measurements
local measurements using
usingWLI
WLI method.
method.Therefore,
Therefore,de-
pending on
depending onvariation
variationininvolume
volumeloss lossfrom
fromthethefour
fourdifferent
differentlocations,
locations,a standard
a standard deviation
devi-
can be defined for specific wear rate measurement corresponding
ation can be defined for specific wear rate measurement corresponding to each wear track. to each wear track. This
deviation
This deviation is aismeasure
a measureof uncertainty
of uncertaintyassociated withwith
associated specific wear wear
specific rate determination
rate determina- due
to local variations within the wear track. The standard deviation values
tion due to local variations within the wear track. The standard deviation values (Sm) for (Sm) for all the radii
allare
thereported
radii3 are−as error bars
reported in Figure
as error bars in3. Figure
It can be3. seen
It canthat a standard
be seen deviationdeviation
that a standard
1 ·m−1 can occur in specific wear rates corresponding to the same wear track,
as high as
4.18 mm · N
as high as 4.18 mm ·N ·m can occur in specific wear rates corresponding to the same
3 −1 −1
calculated based on four local measurements. It is also noticeable that no trend is evident in
wear track, calculated based on four local measurements. It is also noticeable that no trend
magnitude of Sm by changing angular velocity, which means the number of revolutions on
is evident in magnitude of Sm by changing angular velocity, which means the number of
the same wear track as well as angular velocity does not significantly influence uniformity
of the wear track for the radii between 5 and 9 mm and angular velocity corresponding
to 1333 rpm to 2400 rpm. This indicates that the effect on uniformity of wear track due to
change in angular velocity can be considered negligible within this window.

3.2.2. Variation in Specific Wear Rate


Figure 3 shows specific wear rate value for all the 15 test runs (3 each for the five track
radii tested), and the error bars indicate standard deviation (Sm) of the four measurements
on each wear track.
Barring S2R5, S1R7 and S3R8, at least two out of the three tests performed at each
radius on the three samples were found to result in similar specific wear rate values.
Regardless of the different wear track radii, a clear overlap in error bars can also be
Materials 2021, 14, x FOR PEER REVIEW 6 of 15

revolutions on the same wear track as well as angular velocity does not significantly in-
Materials 2021, 14, 3074 fluence uniformity of the wear track for the radii between 5 and 9 mm and angular 6veloc- of 14
ity corresponding to 1333 rpm to 2400 rpm. This indicates that the effect on uniformity of
wear track due to change in angular velocity can be considered negligible within this win-
dow.
recognized. Therefore, the three conditions above (S2R5, S1R7 and S3R8) may be considered
to be outliers. Thus, the ball-on-disk tests are observed to yield consistent specific wear rate
3.2.2. Variation
results regardlessinofSpecific Wearvelocity
the angular Rate being varied over a wide range, as demonstrated
by theFigure
present3 shows specific wearisrate
experiments. This due value
to thefor
factallthat
theno
15change in wear
test runs mechanisms
(3 each for the five
and wear
track regime
radii happened
tested), and thein this bars
error window of tests
indicate conditions.
standard More(Sm)
deviation detailed discussion
of the is
four meas-
provided in Section 3.5.
urements on each wear track.

S1 S2 S3
40.00
Specific wear rate × 10-9 (mm3·N-1·m-1)

35.00

30.00

25.00

20.00

15.00

10.00

5.00

0.00
R5 R6 R7 R8 R9
Figure3.3.Specific
Figure Specificwear
wearrates
ratesfrom
fromall
allfifteen
fifteenball-on-disc
ball-on-disctests
testsconducted
conductedatatvarious
variouswear
wear track
track radii.
radii.
To further highlight the consistency of the specific wear rate results regardless of
angularBarring S2R5,
velocity, S1R7 the
omitting andthree
S3R8, at least
above two outoutlier
mentioned of the values,
three tests performedaverage
the calculated at each
radius
value ofon
thethe three wear
specific samples ratewere
and found to resultstandard
the maximum in similardeviation
specific wear rateoccur
that can values.
fromRe-
gardless of the
measurement aredifferent
depictedwear track 4.
in Figure radii, a clear overlap in error bars can also be recog-
nized. Therefore,
It can be seenthe three
that all conditions
the averageabove values(S2R5, S1R7radius
of each and S3R8)
fall inmay be considered
a range of aroundto
be outliers.
11—18.6 mmThus,
3 ·N−1the
· m−ball-on-disk tests areinobserved
1 . This deviation average to yield consistent
specific wear ratespecific wear
is smaller rate
than
results
the regardless
maximum of thedeviation
standard angular velocity being varied (Max.
from measurement over a Sm
wide =± range, as demonstrated
4.18 mm 3 ·N−1 ·m−1 ).

by the present
Therefore, it canexperiments.
be concluded This is due
that to the fact
maximum that no change
deviation in wear mechanisms
from changing the wear track and
wear regime
radius happened
(and, hence, angularin this window
velocity) of teststhan
is smaller conditions. More detailed
the maximum standarddiscussion
deviationis
provided
from in Section 3.5.method itself. Moreover, standard deviation of the specific wear
the measurement
Toall
rates of further highlight
the twelve the consistency
measurements is 2.9ofunits,
the specific
which wear
is stillrate
muchresults regardless
less than of an-
maximum
gular
Sm. velocity, results
Therefore, omitting fromthe the
three above
tests mentioned
performed outlier
on the same values,
sample thewith
calculated
various average
track
value
radii of the specific
(between 5 and 9wear
mm in rate
theand the maximum
present study and standard deviation
corresponding that can occur
to substantially from
varying
measurement
angular velocity)arecan
depicted in Figure
be consistent and 4.deemed to be representative of wear behaviour of
the coating.

3.2.3. Variation in Coefficient of Friction and Wear Mechanism


The coefficient of friction (CoF) for all the samples reached steady state after around
initial 5000 s of sliding. Figure 5 shows average steady state CoF values for all the 15
test repetitions performed on the 3 samples at different radii, along with the standard
deviation (as error bars) showing fluctuation of CoF values. It can be seen that a majority
of CoF values fall into a narrow range of 0.3 to 0.4. However, looking at S1R6 and S1R8, the
average CoF value can deviate from 0.16 to 0.58 units without any considerable change
in the specific wear rate (see Figure 3). Comparing specific wear rate figures with CoF
values (Figures 3 and 5), no direct correlation can be clearly made between specific wear
rate and its corresponding friction coefficient value. Unlike two studies conducted by
Materials 2021, 14, 3074 7 of 14

Wesmann et al. [29,30] attributing higher coefficient of friction to formation of surface


oxides and tribofilm, no obvious correlation was identified between CoF values and surface
morphology during post-wear analysis. In other words, some wear tracks were found to
be similar, while the corresponding CoF values were different by a factor of 2 or 3. Hence,
the CoF value in the WC–CoCr coating studied in this paper appears to vary without a
clear trend within the aforementioned range. Similar large variation in CoF without any
clear trend was found in a study by Wilkowski et al. [31].
Materials 2021, 14, x FOR PEER REVIEW 7 of 15

Figure 4. Average specific wear rate value of different


Materials 2021, 14, x FOR PEER REVIEW
different wear
wear track
track radii.
radii. 8 of 15

It can be seen that all the average values of each radius fall in a range of around 11—
S1 S2 S3
18.6 mm3·N−1·m−1. This deviation in average specific wear rate is smaller than the maxi-
0.7
mum standard deviation from measurement (Max. Sm = ±4.18 mm3·N−1·m−1). Therefore, it
can be concluded that maximum deviation from changing the wear track radius (and,
0.6
hence, angular velocity) is smaller than the maximum standard deviation from the meas-
Coefficient of friction (µ)

urement method itself. Moreover, standard deviation of the specific wear rates of all the
0.5
twelve measurements is 2.9 units, which is still much less than maximum Sm. Therefore,
results from the tests performed on the same sample with various track radii (between 5
0.4
and 9 mm in the present study and corresponding to substantially varying angular veloc-
ity) can
0.3be consistent and deemed to be representative of wear behaviour of the coating.
3.2.3. 0.2
Variation in Coefficient of Friction and Wear Mechanism
The coefficient of friction (CoF) for all the samples reached steady state after around
initial0.1
5000 s of sliding. Figure 5 shows average steady state CoF values for all the 15 test
repetitions performed on the 3 samples at different radii, along with the standard devia-
tion (as0error bars) showing fluctuation of CoF values. It can be seen that a majority of CoF
values fall into aR5 narrow rangeR6 R7
of 0.3 to 0.4. However, R8 at S1R6 andR9S1R8, the av-
looking
erage CoF value
Figure5.5.Average can deviate
Average CoFvalue
valuefor from
forall
allthe 0.16 to 0.58
the fifteentests.
tests.units without any considerable change in
the specific wear CoF
Figure
rate (see Figure 3). fifteen
Comparing specific wear rate figures with CoF values
(Figures 3 and 5),
Although thenospecific
direct correlation
wear rate values can beappear
clearlyconsistent
made between specific
regardless of wear rateveloc-
angular and
its
itycorresponding frictionitcoefficient
as discussed above, value. Unlike
is also important two studies
to ensure that thisconducted
observation by Wesmann et
is not coinci-
al. [29,30]
dental andattributing
there is nohigher
change coefficient
in wear regimeof friction
overto formation
the of surface
test parameter windowoxides and con-
under tri-
bofilm, no obvious
sideration. correlation
Therefore, in orderwas identified the
to investigate between
wear CoF values and
mechanisms surface morphol-
responsible for mate-
ogy
rial during
removal,post-wear analysis.
wear tracks wereInstudied
other words,
under some
SEM.wear
Figuretracks wereSEM
6 shows found to be similar,
images of wear
while
scars the corresponding
of various radii of CoF
R5, R7 values
and were
R9 ondifferent
the two by a factor
samples, S2ofand
2 orS3.
3. Ploughing
Hence, theisCoF the
value in thewear
dominant WC–CoCr coating
mechanism studied in
regardless of this paper appears
the angular velocitytoofvary without
the test. a clear trend
In addition, some
within
signs of theshallow
aforementioned
grooving range.
can beSimilar
detected large variation
(shown in CoFsided
by double without any clear
arrows). trend
These two
was found in are
mechanisms a study
also by Wilkowski
reported in other et al. [31]. to be the common wear mechanisms in case
studies
of WC-based coatings under sliding wear conditions [26,32]. SEM image on wear scar of
the sample S2R5 shows that the number and depth of the ploughs are extremely higher
than the rest of the test runs, which is the reason for its specific wear rate being too high
(see Figure 3). Moreover, as shown by arrows, there are regions with significant material
removals within this wear track, while no such large-scale removal (in form of pitting
wear) was detected in other wear tracks. The reason for this unique behaviour was not
clear. By comparing SEM images of the wear tracks with various radii (various angular
velocities), it is clear that the quantity and depth of ploughs and grooves are differing
randomly from a case to the other, without any direct correlation with the radius (angular
Materials 2021, 14, 3074 velocity). For instance, number of ploughs on the sample S2R7 are clearly higher than8 ofthe
14
sample S2R9, but this trend is completely reversed in the case of sample 3 (compared S3R7

Materials 2021, 14, x FOR PEER REVIEW 9 of 14


(a) (b)

(c) (d)

(e) (f)
Figure 6. SEM images of wear tracks at different radii of 5, 7 and 9 mm. (a) S2R5; (b) S3R5; (c) S2R7; (d) S3R7; (e) S2R9 and
(f) S3R9.
(f) S3R9.

3.3. Influence
Although of the
Load on Wear
specific Behaviour
wear rate values appear consistent regardless of angular velocity
as discussed
3.3.1. Variationabove, it is also
in Specific important
Wear Rate to ensure that this observation is not coincidental
and there is no change in wear regime over the test parameter window under consideration.
Wear behaviour of the HVAF-sprayed WC–CoCr coating was also evaluated at dif-
Therefore, in order to investigate the wear mechanisms responsible for material removal,
ferent loads applied during ball-on-disk testing. Specific wear rate values corresponding
wear tracks were studied under SEM. Figure 6 shows SEM images of wear scars of various
to various loads are reported in Figure 7. No major change in specific wear rate was de-
radii of R5, R7 and R9 on the two samples, S2 and S3. Ploughing is the dominant wear
tected,
mechanismand it is also clear
regardless that
of the no major
angular variation
velocity of theintest.
the In
range of error
addition, bars
some is noted.
signs This
of shallow
means that increase in load over the range investigated (20 N to 40 N)
grooving can be detected (shown by double sided arrows). These two mechanisms are has no influence on
consistency of the sliding wear test results.

22.00
20.00
oatings

18.00
0-9)

16.00
Materials 2021, 14, 3074 9 of 14

also reported in other studies to be the common wear mechanisms in case of WC-based
coatings under sliding wear conditions [26,32]. SEM image on wear scar of the sample
S2R5 shows that the number and depth of the ploughs are extremely higher than the rest
of the test runs, which is the reason for its specific wear rate being too high (see Figure 3).
Moreover, as shown by arrows, there are regions with significant material removals within
this wear track, while no such large-scale removal (in form of pitting wear) was detected
in other wear tracks. The reason for this unique behaviour was not clear. By comparing
SEM images of the wear tracks with various radii (various angular velocities), it is clear
that the quantity and depth of ploughs and grooves are differing randomly from a case to
the other, without any direct correlation with the radius (angular velocity). For instance,
number of ploughs on the sample S2R7 are clearly higher than the sample S2R9, but this
trend is completely reversed in the case of sample 3 (compared S3R7 with S3R9). All things
considered, it is clear that for none of the samples major wear mechanisms changed, and it
is dominated by ploughing and minor grooving.

3.3. Influence of Load on Wear Behaviour


3.3.1. Variation in Specific Wear Rate
Wear behaviour of the HVAF-sprayed WC–CoCr coating was also evaluated at dif-
ferent loads applied during ball-on-disk testing. Specific wear rate values corresponding
to various loads are reported in Figure 7. No major change in specific wear rate was
detected, and it is also clear that no major variation in the range of error bars is noted. This
means that increase in load over the range investigated (20 N to 40 N) has no influence on
consistency of the sliding wear test results.
Materials 2021, 14, x FOR PEER REVIEW 10 of 15

22.00
20.00
Specific wear rate of coatings

18.00
(mm3·N-1·m-1 × 10-9)

16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
L20D5 L30D5 L35D5 L40D5

Figure7.7.Specific
Figure Specificwear
wearrates
ratesfrom
fromball-on-disc
ball-on-disctests
testsconducted
conductedunder
underdifferent
differentloads.
loads.

3.3.2.
3.3.2. Variation
Variationin inCoefficient
Coefficientof ofFriction
FrictionandandWear
WearMechanism
Mechanism
Figure
Figure 8 shows evolution of friction coefficient of
8 shows evolution of friction coefficient of the
the samples
samples during
during thethe tests
tests per-
per-
formed
formed at atradius
radiusof of77mm.
mm.TheTheheight
heightof ofthe
theCoF
CoFplateau
plateauisisobserved
observedto toclearly
clearlydecrease
decrease
with
withincreasing
increasingnormalnormalload.
load.A Agradual
gradualdecrease
decreasein inthe
theaverage
averagevalues
valuescancanbebeseen
seenwhen
when
increasing
increasingthe theload
loadfrom
from2020NN to to
30 30
N, N,
35 N35and 40 N.
N and 40This indicates
N. This that, in
indicates spite
that, in of increase
spite of in-
in normal
crease in load,
normal friction
load,load doesload
friction not experience any considerable
does not experience change. Although
any considerable change. some
Alt-
studies
hough some can be foundcan
studies reporting
be found a similar
reportingtrend [33], this
a similar trendtrend
[33], can
this also
trendexhibit
can also random
exhibit
behaviour depending
random behaviour on contacton
depending conditions [26] or may
contact conditions even
[26] or be
maycompletely reversed [34]
even be completely re-
based on the number of third-body particles involved in the
versed [34] based on the number of third-body particles involved in the contact contact region. Inregion.
general, In
when
general,fewerwhen third-body particles particles
fewer third-body are involved in the test,
are involved in i.e., when
the test, thewhen
i.e., test condition
the test con-is
close
ditiontoistwo-body wear, with
close to two-body increase
wear, withinincrease
load, the in CoF
load,value
the CoFdecreases.
value decreases.
crease in normal load, friction load does not experience any considerable change. Alt-
hough some studies can be found reporting a similar trend [33], this trend can also exhibit
random behaviour depending on contact conditions [26] or may even be completely re-
versed [34] based on the number of third-body particles involved in the contact region. In
Materials 2021, 14, 3074
general, when fewer third-body particles are involved in the test, i.e., when the test con-
10 of 14
dition is close to two-body wear, with increase in load, the CoF value decreases.

Figure8.
Figure 8. CoF
CoF evolution
evolution for
for the
the coating
coating tested
testedunder
underdifferent
differentnormal
normalloads.
loads.

Toinvestigate
To investigate anyany possible
possible change
change inin mechanism
mechanism of of wear
wear asas aa result
resultof
ofincrease
increasein in
load, SEM
load, SEM analysis
analysis waswas performed
performed on on wear
wear tracks.
tracks. Figure
Figure 99 shows
shows SEMSEM images
images of ofwear
wear
scars of
scars of the
theL30D5
L30D5and andL40D5
L40D5samples.
samples. The
The number
numberof ofploughs
ploughshas hasclearly
clearlyexperienced
experiencedaa
noticeable
noticeable increase
increase byby increasing
increasing the
the load
load from
from 3030 N
N to
to 40
40 N.
N. Comparing
Comparing Figures
Figures 66 and
and 9, 9,
itit is
is clear
clear that,
that, in
in spite
spite of
of the
the increase
increase in
in load
load from
from 20
20 NN to
to 40
40 N,
N,ploughing
ploughing isis still
still the
the
dominant
dominant wear wear mechanism.
mechanism. This This suggests
suggests that
that no
no significant
significant changes
changes occurred
occurred in in the
the
mechanism
mechanism of
Materials 2021, 14, x FOR PEER REVIEW of material
materialremoval
removal[1,26,35].
[1,26,35]. 11 of 15

(a) (b)
different normal
Figure 9. SEM images of wear tracks at different normal loads
loads of
of 30
30 N
N and
and 40
40 N.
N. (a)
(a) L30D5
L30D5 and
and (b)
(b) L40D5.
L40D5

3.4. Influence
Influence of Sliding Distance on Wear Rate
Running the the test
testfor
forlonger
longertimetime(longer
(longersliding
sliding distance)
distance) is another
is another wayway to investi-
to investigate
any changes
gate in wear
any changes rate. rate.
in wear ThreeThree
tests were conducted
tests were for this
conducted formatter: two with
this matter: two the same
with the
load of
same 20 N
load of and
20 Ndifferent sliding
and different distance
sliding of 5 km
distance of 5and
km10 km
and 10(L20D5
km (L20D5and L20D10)
and L20D10)and
one with
and normal
one with loadload
normal of 30ofN30and distance
N and of 10ofkm
distance 10 (L30D10).
km (L30D10). Figure 10 shows
Figure 10 shows specific
spe-
wearwear
cific rate of the
rate ofthree samples.
the three Increasing
samples. sliding
Increasing distance
sliding of the
distance of test fromfrom
the test 5 km5 tokm10tokm
10
(under
km normal
(under normalload of 20
load N)N)
of 20 resulted
resultedininneither
neithera asubstantial
substantialdifference
differencein in specific
specific wear
wear
rate nor
rate nor any
any improvement
improvement in in repeatability
repeatability ofof result
result (bigger
(bigger error
error bar
bar for
for L20D10
L20D10 compared
compared
to L20D5).
to L20D5). As As presented
presented later
later inin Figure
Figure 12,
12, all
all the
the three
three values
values are
are still
still within
within the
the window
window
of maximum
of maximum Sm and thus
Sm and thus dodo not
not differ
differ significantly.
significantly.

24
22
rate of coatings

20
·m-1 × 10-9)

18
16
14
12
same load of 20 N and different sliding distance of 5 km and 10 km (L20D5 and L20D10)
and one with normal load of 30 N and distance of 10 km (L30D10). Figure 10 shows spe-
cific wear rate of the three samples. Increasing sliding distance of the test from 5 km to 10
km (under normal load of 20 N) resulted in neither a substantial difference in specific wear
rate nor any improvement in repeatability of result (bigger error bar for L20D10 compared
Materials 2021, 14, 3074 to L20D5). As presented later in Figure 12, all the three values are still within the window
11 of 14
of maximum Sm and thus do not differ significantly.

24
22

Specific wear rate of coatings


20

(mm3·N-1·m-1 × 10-9)
18
16
14
12
10
8
6
4
2
0
L20D5 L20D10 L30D10

Figure10.
Figure 10.Specific
Specificwear
wearrate
ratevalues
valuesfrom
fromball-on-disc
ball-on-disctests
testsconducted
conductedfor
fordifferent
differentsliding
slidingdistance
distance
and load.
and load.

Figure11a,b
Figure 11a,bshowshowSEM SEM images
images onon wear
wear tracks
tracks of the
of the twotwo
L20D10L20D10 andandL30D10L30D10 sam-
samples.
ples.by
First, First, by comparing
comparing Figure Figure
11a and11a SEMand SEM in
images images
Figurein6,Figure 6, itthat
it is clear is clear that no
no major major
changes
changes
are are detectable
detectable by increasing by the
increasing the sliding
sliding distance from distance
5 km tofrom
10 km 5 under
km to the 10 km
same under
normal the
sameofnormal
load load of 20 N.
20 N. However, However,change
a noticeable a noticeable change
is evident is evident
when when SEM
comparing comparing
imagesSEM of
images11a,b,
Figure of Figure
which 11a,b, whichfrom
is rooting is rooting from an
an increase in increase in applied
applied normal loadnormal
from 20 load
N to from
30 N 20
N to 30N
when when
running forrunning
the same fordistance
the same of distance
10 km. One of 10 km.change
clear One clear change
is that is that
quantity andquantity
depth
and
of thedepth
ploughsof the ploughs experienced
experienced an obvious an obvious
increase, andincrease,
the numberand the andnumber
size of and
pits size
(darkof
pits (dark
regions) regions)
also also considerably
considerably increased. Theincreased. The pits,
pits, which whichup
are filled arewithfilled up products,
wear with wear
products,
indicate
Materials 2021, 14, x FOR PEER REVIEW
indicate
material material[18].
removal removal [18]. Therefore,
Therefore, by a simultaneous
by a simultaneous increase in increase in the
the normal nor-
load
12 of 15
mal load
(from 20 N(from
to 3020 N)Nand to 30 N) and
sliding sliding(from
distance distance
5 km (from
to 105 km),
km to some10 km),signssome signs of
of material
material
removal in removal
form ofinpits form of pitstoisploughing
is added added to as ploughing
dominantaswear dominant
mechanisms.wear mechanisms.
However, as
However, as far
far as the pits areas the pitsand
isolated aretherefore
isolated and therefore
possible possible
to be filled up towithbe wear
filledproducts
up with wearsuch
as oxides such
products of alumina,
as oxides tungsten, cobalttungsten,
of alumina, and chromium,
cobalt and theychromium,
are not taken they into
areaccount
not taken in
volume loss measured
into account in volumeby lossWLI technique
measured and, technique
by WLI consequently, and,not in specific wear
consequently, rate.
not in This
specific
explains
wear noThis
rate. major changeno
explains inmajor
specific wear rate
change value reported
in specific wear rateinvalue
Figure 10 in spite
reported of minor
in Figure 10
change
in spiteinofremoval
minor changemechanisms and, therefore,
in removal mechanismsno changes in wear regime.
and, therefore, no changes As shown
in wearin the
re-
study by
gime. As Wang
shown et in
al. the
[26],study
connection
by Wang of these
et al.pits canconnection
[26], cause a dramatic
of these change in removal
pits can cause a
mechanism
dramatic and result
change in the mechanism
in removal magnitude of andspecific
result wear
in therate.
magnitude of specific wear rate.

(a) (b)
Figure 11.
Figure 11. SEM
SEM images
images of
of wear
wear tracks
tracks performed
performed under
under 20
20 N
N (a)
(a) and
and 30
30 N
N load
load (b).
(b).

3.5. Wear Regime


When the specific wear rate is low and does not substantially change (i.e., remains of
same order of magnitude) by changing test conditions, the wear regime can be termed as
mild [1,26,35]. Moreover, in case of WC-based coatings, it is known that, after a certain
increase in normal load, the specific wear rate experiences a substantial increase by orders
of magnitude [26]. The specific wear rate values for various angular velocities, loads and
Materials 2021, 14, 3074 12 of 14

3.5. Wear Regime


When the specific wear rate is low and does not substantially change (i.e., remains
of same order of magnitude) by changing test conditions, the wear regime can be termed
as mild [1,26,35]. Moreover, in case of WC-based coatings, it is known that, after a certain
increase in normal load, the specific wear rate experiences a substantial increase by orders
of magnitude [26]. The specific wear rate values for various angular velocities, loads and
sliding distances (from a large matrix of ball-on-disk tests conducted, as listed in Table 3)
previously presented in Figures 4, 7 and 10 reveal that the average specific wear rate values
vary from 11 to 18.6 mm3 ·N−1 ·m−1 , which are small enough to be categorized as mild
wear regime. All the specific wear rate values from ball-on-disc testing under different
angular velocities, different loads and/or sliding distances along with the corresponding
average value are depicted in Figure 12. It can be seen that deviation of all the specific
wear rate values (with the only exception of S3R9) from average value is still within the
window of maximum Sm. It should be mentioned that the conclusions in this paper are
specific to sliding wear rate behaviour of HVAF-sprayed WC–CoCr coatings, and the results
may differ for other coatings. Additionally, no significant difference in wear mechanisms
was evident from post-wear analysis, confirming that no transition from mild to severe
wear regime occurs over the investigated test parameter window. Therefore, as shown
in Figure 13, by individually increasing either normal load up to 40 N, angular velocity
up to 2400 rpm, or sliding distance up to 10 km from the ‘reference’ test parameters of
20 N, 2400 rpm and 5 km, no changes in wear regime occur during ball-on-disk testing of
HVAF-sprayed WC–Co-Cr coatings.
Materials 2021, 14, x FOR PEER REVIEW 13 of 15
Materials 2021, 14, x FOR PEER REVIEW 13 of 15

Figure
Figure 12.
12. Specific
Specific wear
wear rate
rate from
from various
various ball-on-disc
ball-on-disc tests
tests conducted under different
conducted under different conditions
conditions according
according to
to Table
Table3.
3.
Figure 12. Specific wear rate from various ball-on-disc tests conducted under different conditions according to Table 3.

Figure 13. Schematic diagram of the mild and severe wear regimes adapted from [1].
Figure
Figure 13.
13. Schematic
Schematic diagram
diagram of
of the
the mild
mild and
and severe
severe wear
wear regimes
regimes adapted
adapted from [1].
from [1].
A comprehensive investigation was conducted in order to understand sliding wear
A comprehensive
behaviour investigation
of HVAF-sprayed WC–CoCr was coatings
conducted in order
under to understand
a variety of differentsliding wear
test condi-
behaviour of HVAF-sprayed
tions, and the WC–CoCr
following conclusions werecoatings
drawn: under a varietydifference
No significant of different
wastest condi-
observed
tions, and the
in specific wearfollowing conclusions
rate when changing were drawn:
angular No significant
velocity difference
from 1333 rpm up to was
2400observed
rpm in a
in
wayspecific wear
that the rate when
difference changing
in smaller angular
than velocity
precision from 1333 rpm
of measurement up toIncrease
method. 2400 rpm in a
in load
way
up tothat
40 the difference
N did not makein smaller thanchange
any major precision
in of measurement
either method.
specific wear rate Increase in load
or deviation of
up to 40
values N did
from not make
different any major
repetitions. change
Increase in either
in sliding specific
distance up wear ratewhile
to 10 km or deviation
the normal of
values from different repetitions. Increase in sliding distance up to 10 km while the normal
Materials 2021, 14, 3074 13 of 14

A comprehensive investigation was conducted in order to understand sliding wear


behaviour of HVAF-sprayed WC–CoCr coatings under a variety of different test conditions,
and the following conclusions were drawn: No significant difference was observed in
specific wear rate when changing angular velocity from 1333 rpm up to 2400 rpm in a way
that the difference in smaller than precision of measurement method. Increase in load up
to 40 N did not make any major change in either specific wear rate or deviation of values
from different repetitions. Increase in sliding distance up to 10 km while the normal load
was fixed at 20 N changed neither specific wear rate nor repeatability deviation. All these
roots from no major change in dominant wear mechanisms or wear regime. Therefore,
conducting ball-on-disc test on WC–CoCr coatings under test conditions within the range
conducted by this study could be considered as a reliable testing routine.

Author Contributions: Conceptualization, K.T., M.G. and S.J.; methodology, K.T., M.G. and S.J.;
investigation, K.T. and V.K.S.; data curation, K.T. and V.K.S.; writing—original draft preparation, K.T.;
review and editing, S.J. and M.G.; funding acquisition, S.J. All authors have read and agreed to the
published version of the manuscript.
Funding: This research was funded by the Knowledge Foundation, grant number 20180197.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Data is contained within the article.
Acknowledgments: The authors would like to thank Stefan Björklund and Magnus Sandberg for
spraying coatings and Owe Mårs and Olivia Danielsson from Höganäs for supporting this study by
providing feedstock powders.
Conflicts of Interest: The authors declare no conflict of interest.

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30. Wesmann, J.A.R.; Espallargas, N. Elucidating the complex role of surface oxides formed during sliding of self-mated warm
sprayed WC-CoCr in different environments. Tribol. Int. 2016, 94, 360–372. [CrossRef]
31. Wilkowski, J.; Marek, B.; Radosław, J.; Zbigniew, W.; Alicja, A. Analysis of sliding friction of WC-Co composite on particleboard.
Ann. Warsaw Univ. Life Sci. For. Wood Technol. 2020, 111, 60–67.
32. Wang, Q.; Zhang, S.; Cheng, Y.; Xiang, J.; Zhao, X.; Yang, G. Wear and corrosion performance of WC-10Co4Cr coatings deposited
by different HVOF and HVAF spraying processes. Surf. Coat. Technol. 2013, 218, 127–136. [CrossRef]
33. Chowdhury, M.A.; Khalil, M.K.; Nuruzzaman, D.M.; Rahaman, M.L. The effect of sliding speed and normal load on friction and
wear property of aluminum. Int. J. Mech. Mech. Eng. 2011, 11, 53–57.
34. Vashishtha, N.; Sapate, S.G.; Gahlot, J.S.; Bagde, P. Effect of Tribo-Oxidation on Friction and Wear Behaviour of HVOF Sprayed
WC–10Co–4Cr Coating. Tribol. Lett. 2018, 66, 56. [CrossRef]
35. Hutchings, I.M. Tribology: Friction and Wear of Engineering Materials; Edward Arnold Publishers: London, UK, 1992; p. 352.
Paper
PaperCC
Influence
Influenceofofnozzle
nozzleconfiguration
configurationand
and
particle
particlesize
sizeon
oncharacteristics
characteristicsand
andsliding
sliding
wear
wearbehaviour
behaviourofofHVAF-sprayed
HVAF-sprayedWC-WC-
CoCr
CoCrcoatings
coatings CC
Kaveh
KavehTorkashvand,
Torkashvand,Mohit
MohitGupta,
Gupta,Stefan
StefanBjörklund,
Björklund,Francesco
Francesco
Marra,Lidia
Marra, LidiaBaiamonte,
Baiamonte,Shrikant
ShrikantJoshi
Joshi

Published:
Published:”Surface
”Surfaceand
andCoatings
CoatingsTechnology”
Technology”

Elsevier,
Elsevier,July
July2021
2021

Published
Publishedwith
with
Creative
Creative
Commons
Commons
license:
license:
CCCC
BYBY4.04.0
Surface & Coatings Technology 423 (2021) 127585

Contents lists available at ScienceDirect

Surface & Coatings Technology


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

Influence of nozzle configuration and particle size on characteristics and


sliding wear behaviour of HVAF-sprayed WC-CoCr coatings
Kaveh Torkashvand a, *, Mohit Gupta a, Stefan Björklund a, Francesco Marra b,
Lidia Baiamonte a, b, Shrikant Joshi a
a
Department of Engineering Science, University West, Sweden
b
Department of Chemical Engineering Materials Environment, Sapienza University of Rome, Italy

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, effect of feedstock particle size and nozzle configuration on deposition, microstructural features,
Particle size hardness and sliding wear behaviour of high velocity air fuel (HVAF)-sprayed WC-CoCr coatings was evaluated.
Nozzle configuration Three different WC-CoCr powders with nominal particle sizes of 5/20 μm (fine), 5/30 μm (medium) and 15/45
HVAF
μm (coarse) were sprayed employing a HVAF gun with four distinct DeLaval nozzle configurations involving
WC-CoCr
different lengths and/or exit diameters. Microstructure, phase constitution and mechanical characteristics of the
Sliding wear
coatings were evaluated using SEM, EDS, XRD and micro indentation testing. Specific wear rate for all the
samples was determined under sliding conditions and a comprehensive post wear analysis was conducted. X-ray
diffraction analysis showed negligible decarburization in all the HVAF-sprayed coatings. It was shown that
decrease in particle size of employed feedstock results in discernible changes in microstructural features of the
coatings as well as considerable improvement in their performance. Also, notable changes in wear mechanisms
were identified on reducing particle size from coarse to medium or fine. Fine and coarse feedstock powders were
found to be sensitive to the type of nozzle used while no major difference was observed in coatings from powders
with medium cut size sprayed with different nozzles.

1. Introduction convergent-divergent design of the nozzles. Therefore, selecting a


proper configuration demands a deep understanding of its effect on
High velocity air-fuel (HVAF) spraying method has been considered properties of the resultant coating. Feedstock characteristics such as
increasingly attractive for spraying WC-based wear resistant coatings morphology, density, and particles size also significantly influence the
and attracting significant research attention. This is largely by virtue of resultant coating properties. Among these, the particle size distribution
its capability to produce high quality coatings and overcoming some of can be considered a prominent feedstock characteristic for a given
the existing problems such as decarburization [1–3]. HVAF spraying chemistry in case of HVAF spraying. Both the temperature and velocity
method typically generates higher particle velocities leading to higher attained in flight by particles are strongly dependent on their size, which
kinetic energy and, due to the lower flame temperature, the particle is also a determining factor in selecting the most appropriate HVAF
temperatures are also lower compared to other spraying techniques like spraying configuration [9,10].
high velocity oxy-fuel (HVOF). The latter is a key factor responsible for Some investigations have been previously conducted to study the
diminishing decarburization [4,5]. Moreover, in the HVAF method, effect of HVAF process parameters on characteristics and performance of
substituting air in place of oxygen not only results in lower spraying WC-based coatings. Matikainen et al. [11] studied the effect of nozzle
costs, but can also effectively mitigate oxidation of the feedstock. configuration on tribological properties of HVAF-sprayed WC-CoCr
Consequently, a finer powder cut size can be used as feedstock [6–8]. coatings deposited using feedstock powder of 10–30 μm size range. They
However, different hardware configurations in the HVAF method result employed a M3 gun (Uniquecoat Technologies LLC, USA) and utilized
in varied particle temperatures and velocities. Different torch configu- three nozzles of the same length but with different exit diameters: one
rations can be achieved particularly through variations in length and the cylindrical (named 4L0) and two convergent-divergent configurations

* Corresponding author.
E-mail address: Kaveh.torkashvand@hv.se (K. Torkashvand).

https://doi.org/10.1016/j.surfcoat.2021.127585
Received 16 April 2021; Received in revised form 29 July 2021; Accepted 30 July 2021
Available online 5 August 2021
0257-8972/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Code Nozzle Schematic Table 1


Specifications of the three powders with different particle size used in the study.
N1 4L2
Code Chemistry Particle Particle size Type Trade
nominal distribution (μm) name
size (μm)
D D D
N2 4L4 10% 50% 90%

Pc WC-Co-Cr 45/15 22 34 52 Agl. Amperit®


86-10-4 & 558.074
Sint.
Pm WC-Co-Cr 30/5 12 19 28 Agl. Amperit®
N3 5L2 86-10-4 & 558.059
Sint.
Pf WC-Co-Cr 20/5 6 13 22 Agl. Amperit®
86-10-4 & 558.052
Sint.
N4 5L4

of nozzle configuration. Matikainen et al. [20] deposited two different


powders with particle size ranges of 10–30 and 5–25 μm using an
Fig. 1. Different nozzle configurations used for spraying. identical HVAF M3 gun configuration. Average measured temperature
of in-flight particles was 50 ◦ C higher for coarser cut size (1410 ◦ C vs.
(named 4L2 and 4L4) with increasing exit diameter as the nozzle 1360 ◦ C) while the particle velocity for the finer powder was around 30
designation changes from 4L0 to 4L2 and 4L4 (see Fig. 1 for 4L2 and 4L4 m⋅s�1 higher than that for the coarser powder (957 m⋅s�1 vs. 929 m⋅s�1).
designs). Their results showed that average particle velocity can rise Average Vickers hardness was slightly higher for coatings sprayed with
from 780 m⋅s�1 for a straight bore nozzle to 900 m⋅s�1 for a convergent- the coarser powder, with a value of 1458 HV0.3 as compared to 1344
divergent nozzle, resulting in substantial improvement in density and HV0.3 for coatings sprayed with a finer cut size. The main focus of this
microstructure of the coating. Lyphout et al. [12], utilizing an identical effort was to evaluate cavitation, slurry and dry particle erosion of WC-
gun with different nozzles varying in length to spray an identical pow- 10Co4Cr and Cr3C2-25NiCr coatings sprayed by HVOF and HVAF and
der, studied mechanical and wear properties of WC-CoCr coatings. Their two different size ranges for the powders were used without considering
results showed that increasing length of the nozzle leads to an influence of nozzle configuration.
improvement in microhardness and abrasion wear resistance of the Different nozzle configurations can potentially affect the quality of
coating. In another study by Kumar et al. [10], it was shown that the deposited coating and need to be properly selected based on particle size
AK06 HVAF gun (Kermetico, USA) with three different nozzle designa- used as feedstock. The studies mentioned above indicate that selection of
tions 5O, 5E and 5L, of varying geometrical design, can result in average an appropriate feedstock particle with a suitable nozzle configuration
particle velocities of 1010, 960 and 895 m⋅s�1, respectively, when could result in an enhanced wear performance. Notwithstanding the
spraying WC-CoCr feedstock powder of the same particle size (20–45 above, none of the existing studies have undertaken a dedicated effort
μm). However, the above investigations were conducted on powders focused on investigating the effects of particle size and nozzle configu-
with an identical particle size and, as a result, do not provide a broad ration when spraying WC-based coatings using HVAF. Hence, con-
view of how the nozzle geometry-particle size combinations can influ- ducting a comprehensive study, involving a wide range of particle size
ence the properties and performance of the resultant coatings. Besides, distributions and a host of different nozzle configurations, to assess how
given the fact that HVAF parameters are primarily hardware dependent each can influence microstructural, mechanical and tribological prop-
[12] as compared to other spraying techniques like HVOF and plasma erties of HVAF sprayed WC-CoCr coatings is deemed crucial and pro-
spraying where other spray variables can play a major role [13,14], vides the motivation for this work. Accordingly, a comprehensive
changing nozzles covers a wide-ranging process window in HVAF investigation is conducted on three powders with different particle size
spraying and is of considerable practical relevance. Consequently, ranges sprayed with four different nozzles with varying length and/or
considering the rapid progress of the HVAF technology and commercial convergent-divergent design to investigate the influence of nozzle
availability of different spray equipment, the influence of nozzle configuration and particle size on characteristics and sliding wear per-
configuration needs to be well established for different powder particle formance of HVAF-sprayed WC-CoCr coatings.
sizes to be sprayed.
During the spraying process, particles attain different temperatures 2. Experiment procedure
and velocities depending on their size. Another key factor is the duration
of high temperature exposure, which itself is dependent on the size 2.1. Spraying process
(mass) of the particles [15,16] since the in-flight residence time is
governed by the particle velocity. Through a modeling simulation, it has Three commercially available WC-10Co4Cr powders with different
been shown that WC-CoCr particles are fully molten during HVOF particle size ranges produced by Höganäs GmbH employing the
spraying when their size is smaller than 15 μm [13,17]. Several studies agglomeration and sintering technique (see Table 1), were used as
have been performed to investigate mechanical properties and tribo- feedstock material. Domex 355 coupons of diameter 25 mm and thick-
logical performance of HVAF WC-based coatings [10–12,18–21], among ness 6 mm were used as substrates.
which a few have investigated influence of particle size [20,21]. Bolelli An M3 HVAF torch (Uniquecoat Technologies LLC, Oilville, VA,
et al. [21] studied sliding and abrasive wear performance of HVAF- USA) was used and four different De Laval nozzles (Fig. 1) were
sprayed WC-CoCr with two different particle size ranges of 5–30 μm employed to spray the feedstock powders. All three powders were
and 15–45 μm employing M3 and M2 guns (Uniquecoat Technologies sprayed with each nozzle configuration in this study, except Pf which
LLC, USA). Their results showed that coatings deposited from powders was not sprayed with nozzle N3.
with finer particle size yield superior wear performance. The main Cleaned samples were mounted on a rotating fixture and grit-blasted
objective of this study was to compare the tribological properties of employing alumina powder. Then the three powders were sprayed with
HVOF and HVAF WC–10Co4Cr coatings and this was conducted by the process parameters mentioned in Table 2 with a targeted thickness of
employing powders of two particle sizes without considering influence 250 μm for all the coatings. The carrier gas was Nitrogen. It is relevant to

2
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Table 2
HVAF spraying parameters used for coating deposition.
Pc Pm Pf

N1 N2 N3 N4 N1 N2 N3 N4 N1 N2 N3 N4

Air (psi) 111 114 113 114 111 114 118 118 111 114 – 118
Fuel 1 (psi) 100 100 105 105 100 100 105 105 100 100 – 105
Fuel 2 (psi) 105 105 115 115 105 105 115 115 105 105 – 115
Carrier (l⋅min�1) 40 40 50 50 50 50 50 50 50 50 – 50
Feed (g⋅min�1) 200 200 200
SoD (mm) 300 300 300
Number of strokes 11 13 11 11 15 17 16 17 26 29 – 26

mention that the HVAF torch technology is critically based on the orifice Duramin-40 microhardness tester (Cleveland, United States). Fifteen
design inside the torch. Moreover, the fuel and air supply are pressure indentations were performed on each sample according to the standard
controlled, not flow controlled. Therefore, an appropriate way to ASTM E384 [22].
describe torch parameters in a M3 MVAF torch would be to indicate the Identification of the crystalline phases was performed by X-ray
nozzle dimensions (as done in Fig. 1) and the supply pressures for Air, diffraction analysis (XRD), with a Philips X'Pert device (PANalytical B.
Fuel 1 and Fuel 2 (provided in Table 2). Nonetheless, it may be added for V., The Netherlands) on as-coated surfaces. XRD measurements were
completeness that, the air and fuel pressures stated in Table 2 for nozzle carried out at 40 kV and 40 mA, with Cu Kα radiation (λKα1 = 1.540598
dimensions indicated in Fig. 1 correspond to flow rates in the range of Å, λKα2 = 1.544426 Å), with a scan range of 20◦ –80◦ (2θ), step size
9000 l/min for Air and 200 l/min for Fuel 1 and 2. 0.02◦ , and an acquisition time of 2 s/step.
AccuraSpray – G3C (Tecnar, Quebec, Canada) was employed to
measure temperature and velocity of in-flight particles at impact. In
order to assess repeatability of measured data, the measurement was 2.3. Ball-on-disk test
repeated three times for Pf sprayed using N1 and N2 nozzles several days
apart. Sliding wear tests were performed on samples with a mirror-polished
surface (ground and polished in the same manner as described in the
Section 2.2), following the procedure prescribed in ASTM G99 standard
2.2. Characterization of powders/coatings [23]. The test was conducted using a tribometer rig (Tribometer TRB3,
Anton-Paar, Switzerland) which monitors friction coefficient during the
Scanning electron microscopy (SEM) analysis was performed on all test. Alumina balls with radius of 6 mm were employed as the mating
powders to examine their morphology and cross-sections. Powders were counterpart. The ball-on-disk tests were conducted under a constant
collected on carbon tapes and observed under SEM (HITACHI TM3000 normal load of 20 N, with a constant linear speed of 0.2 m⋅s�1 and for a
microscope, Krefeld, Germany, and ZEISS GeminiSEM 450, Oberkochen, total sliding distance of 5000 m. At least two repetitions were performed
Germany). In order to perform cross-sectional observations, powders for each test on radius 7 and 9 mm of wear trace. All the tests were done
were mixed with epoxy, cold mounted, ground and polished (employing at room temperature with relative humidity of around 30%. After each
the same procedure explained in next paragraph) before being studied in test, wear products were collected from the surface of the sample in the
the SEM. form of debris, and then the samples were cleaned ultrasonically prior to
Employing a surface roughness tester (Surftest 301, Mitutoyo, surface analysis. The top-surface of the wear tracks as well as the wear
Japan), roughness values of as-deposited coatings (Ra) were measured as debris were characterized using SEM/EDX analysis.
per ASME B46.1 standard. Three measurements were performed on each Volume loss in the samples as a result of sliding wear was measured
coating and average values and standard deviations have been reported employing white light interferometry (WLI) technique (Profilm 3D,
herein. Filmetrics, Unterhaching, Germany). Using WLI, it was not possible to
After sectioning and hot mounting, the samples were ground and capture the whole wear track. Therefore, volume loss in four different
polished. Grinding was performed by employing a 45 μm diamond disk, regions across the wear track was measured (Fig. 2(a)), based on which
while polishing was carried out successively using 9 μm and 3 μm Kemet an average cross-sectional area was obtained for the wear track at once.
liquid diamond solution. Finally, the specimens were mirror-polished Hence, four different wear track locations, approximately 90 degrees
employing MasterMet 2 dispense. General microstructure analysis of apart were scanned on each circular wear track. The overall volume loss
the samples was performed using SEM analysis. was calculated by multiplying the average cross-sectional area by the
Vickers hardness of the samples was measured employing Struers total length of the wear track (Eq. (1)). Also, specific wear rate for balls

Coating Ball

a b
Fig. 2. Schematic sketch of volume loss measurements on a) wear track on coating and b) worn ball.

3
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

a: Pc b: Pm c: Pf

d: Pc e: Pm f: Pf
Fig. 3. SEM images of (a-c) particle surface morphologies and (d-f) particle cross-sections of the three powders used (coarse: Pc, medium: Pm and fine: Pf).

corresponding to wear track radius of 7 mm was measured. For this, the 3. Results
worn surface area of balls (see Fig. 16) was measured using image
analysis [24], then the corresponding radius (r) and volume loss deter- 3.1. Powder characteristics
mined as shown in Fig. 2(b). Consequently, using Eq. (3), the specific
wear rates for both the ball and the coating were obtained by dividing Morphologies of the three used powders are shown in Fig. 3(a), (b)
volume loss over the normal load (L) and sliding distance. and (c). Most of the powder particles of Pc and Pm exhibit a spherical
( ) shape while most of the Pf particles were irregular in shape. Fig. 3(d), (e)
1 V1 V2 V3 V4
Vloss�coating = (π.R) + + + (1) and (f) shows cross-sectional images of Pc, Pm and Pf, respectively. From
2 l1 l2 l3 l4
the SEM visualization, it is clear that by decreasing the particle size, the
number and dimension of the pores within the particles decreases
1 � )
Vloss�ball = (π.h) 3.r2 + h2 (2) because the smaller the dimension the limited number and size of
6
comprising defects [25]. In other words, the density of individual par-
V ticles seemed to increase with decrease in particle size, which can
W= (3)
L.d potentially have an influence on density of the resultant coating.

where in Eq. (1) V1–4 are volume losses at the four scanned locations, l1–4
3.2. Deposition rate
are the lengths of the corresponding wear track segments at these lo-
cations and R is radius of the wear track. In Eq. (2), h and r are the height
Fig. 4 shows the measured in-flight temperatures and velocities of
and radius of the removed spherical cap, respectively. Finally, in Eq. (3),
particles, in case of different powders used and nozzle configurations
W is specific wear rate, V is volume loss, L is load and d is total sliding
employed. Indicative standard deviation values are drawn as error bars
distance.
in the corresponding data points, based on repeat measurements

Fig. 4. Measured in-flight a) temperature and b) velocity, for the three feedstock powders sprayed using four different nozzles.

4
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

efficiency, which could vary with particle size, may not have been
encompassed in the process parameter window that has been investi-
gated herein in case of all powders.

3.3. Coating microstructure

Fig. 6 shows SEM images of surfaces of the Pc, Pm and Pf coatings


sprayed with the nozzle N2. It is clearly noticeable that, with decrease in
particle size, the surface of the coatings attains a finer morphology,
resulting in a lower average roughness. Average Ra value decreases from
around 4.5 μm for Pc coating to around 2.5 μm and 2 μm for Pm and Pf,
respectively. No significant difference was observed in surface
morphology and roughness of the coatings of the same particle size
sprayed with different nozzles.
Fig. 5. Deposition rate for various feedstock powders sprayed using four Fig. 7 shows SEM images of all the eleven coatings. No significant
different nozzles. differences in microstructure were detected by changing the nozzle
configuration for the same powder. However, with decrease in particle
conducted on Pf sprayed using nozzles N1 and N2 to show reliability of size, the homogeneity of the coatings seemed to experience a substantial
data. The particle temperature was not significantly influenced by the improvement. The number and size of the dark regions, which corre-
particle size, varying over a window of 105 ◦ C or less when using the spond to either pores or binder accumulation (see Fig. 17), considerably
same nozzle. Increasing the exit diameter of the nozzle from N1 to N2, decrease with reduced feedstock particle size. In order to differentiate
led to a drop in particle temperature by around 150 ◦ C for Pf and Pm and pores, SE SEM images were taken from the polished surfaces of coatings
by about 100 ◦ C for Pc. The particle velocity was found to increase with from the three different powders (Fig. 8). It was clear that the size and
reducing particle size in case of each of the nozzles. However, for a given number of pores dramatically reduced with decrease in particle size
powder, no significant differences in particle velocity were discernible from Pc to Pm or Pf. The Pf coating exhibited the highest density among
with change in type of nozzle, with the noted variation being limited to a all, with minimal detectable pores observable in the coating at 5000×
maximum of around 100 m⋅s�1. magnification (shown by arrows). There could be two main reasons for
An average targeted thickness of around 250 μm was achieved for all this: first, as discussed before, porosity within the particles decreases
the coatings. From the measured coating thickness and the total number with size and consequently yields a denser coating. Besides, as shown in
of strokes for each coating (see Table 2), the thickness built up per pass Table 2, the number of passes needed to reach the targeted thickness
(deposition rate) can be determined, which is a fair measure of deposi- substantially increased with decrease in feedstock particle size despite
tion efficiency. The deposition rates for all the coatings are provided in the same powder feed rate, which leads to a greater peening effect [26].
Fig. 5. This effect can be even more pronounced considering the higher in-flight
In general, a substantial decrease in deposition rate can be observed particle velocity for smaller cut size powders (see Fig. 4), and conse-
with decrease in particle size from Pc to Pm and from Pm to Pf. This quently result in an improvement in the final density of the corre-
trend was consistent and more clearly evident when comparing the sponding coating.
deposition rates for each nozzle used for spraying the three powders
with varying particle size ranges. The reason for this must be related to 3.4. X-ray analysis
the intrinsic properties of particles associated to their dimension and is
further discussed in Section 4.1. Since all powders were of identical chemistry, X-ray diffraction
Reduction in deposition efficiency may raise concerns around costs. analysis was performed on one of the powders (Pc) as well as two of the
However, it is worth mentioning that deposition efficiency is not the coatings deposited using the coarsest and the finest powders (Pc and Pf)
only determining factor governing the choice of feedstock. For example, employing N1 and N4 nozzles. As shown in Fig. 9, no deviation in phase
a finer feedstock particle size makes it possible to fabricate thinner constitution is recognizable when comparing all the coatings with the
coatings which involve less powder being used in a shorter spraying time starting powder. This implies that negligible decarburization or phase
and can, in turn, reduce total coating costs. Also, a finer particle size change occurs when spraying WC-CoCr feedstock powder through HVAF
makes it possible to achieve smoother coatings, which can potentially within the process parameter window used in this study. This reaffirms
reduce the demand for subsequent machining leading to significant findings from other studies employing the HVAF technique [27].
savings in post-processing costs. On the other hand, in this study,
powders of all particle sizes were sprayed with a fixed set of parameters.
Therefore, the “optimum” spray conditions in terms of deposition

PcN2 PmN2 PfN2

Fig. 6. SE SEM images of surfaces of as-deposited coatings using powders with three different particle sizes (Pc, Pm and Pf) sprayed with the same nozzle (N2).

5
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

PcN1 PcN2 PcN3 PcN4

PmN1 PmN2 PmN3 PmN4

PfN1 PfN2 PfN4

Fig. 7. Cross-sectional BSE-SEM images of all the coatings using powders with three different particle sizes (Pc, Pm and Pf) sprayed with four nozzles (N1, N2, N3
and N4).

PcN2 PmN2 PfN2

Fig. 8. SE SEM images of surfaces of the three coatings using powders with three different particle sizes (Pc, Pm and Pf), sprayed with the same nozzle (N2).

3.5. Microindentation test of the nozzle and/or increasing degree of divergence (larger exit diam-
eter) of the nozzle (N3/N4 vs. N1/N2). The reason for this could be the
Results from indentation testing show that the Vickers hardness slight increase in particle velocity as seen in Fig. 4 and the corresponding
values experience a considerable increase with decrease in particle size, increase in peening effect. This effect of velocity on peening effect has
increasing from around 1100–1300 HV0.3 for Pc coatings, to also been confirmed by other studies [20,25]. For each particle size (Pc,
1350–1450 HV0.3 for Pm coatings, and to 1500–1600 HV0.3 for Pf Pm and Pf), average hardness values are highest for coatings sprayed by
coatings (see Fig. 10). This is attributable to the denser coatings being nozzle N4 as evident from Fig. 10.
formed by decrease in particle size, combined with the stronger peening
effect resulting from higher velocity for finer particles as well as the
higher number of strokes required due to the lower deposition rate to 3.6. Sliding wear
achieve the targeted thickness [28,29]. Average hardness value of the
coatings manufactured from Pc slightly increases with increasing length By calculating specific wear rates of each coating and corresponding
mating ball, as well as monitoring coefficient of friction (CoF) values

6
K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 9. XRD spectra of the Pc powder along with PcN1, PcN4, PfN1 and PfN4.

just an outlier value in CoF which is usual to happen in these coatings, as


it was shown in our other study [30]. It was also shown in the above
study that there was no correlation between the CoF value and the
specific wear rate.
In Fig. 11(b), evolution of friction coefficient of the three coatings
from Pc, Pm and Pf powders sprayed using nozzle N1 is shown. It can be
seen that all the coatings follow the same generic trend, with the CoF
attaining a steady state after around 10,000 s. Also, it is clear that the
CoF value decreases with decrease in particle size. Notably less fluctu-
ation in CoF values (during steady state period) can be observed for Pf
when compared to Pm and Pc, as well as for Pm when compared to Pc. It
is discussed later in Section 4.2 that the reason for reduction in CoF
value as well as its fluctuation can be related to the initial powder
particle size and consequently the size range of the ensuing debris.
Coatings fabricated from smaller feedstock particle size led to produc-
tion of finer wear debris, resulting in lower CoF and less fluctuation.
Fig. 10. Vickers microhardness values for all coatings sprayed with various
nozzles and powders with different particle size. Fig. 12(a) shows specific wear rates of all the coatings. Specific wear
rate was extremely low and of the order of magnitude of 10�8
mm3⋅N�1⋅m�1 in all cases. Moving to finer powder cut size from Pc to
throughout the duration of the wear test, an effort was made to compare
Pm, regardless of the nozzle type, the average value of specific wear rate
all the coatings in terms of their sliding wear performance. Also, a
of the coatings was found to decrease. Further decreasing particle size
comprehensive post wear analysis was performed to shed light on pre-
(Pm to Pf) leads to further decrease in specific wear rate of the coatings
vailing material removal mechanisms.
sprayed employing nozzles N2 and N4. The coatings deposited with
Fig. 11(a) shows average values of friction coefficient for all the
medium and fine sized powders performed similarly, one of the reasons
coatings after the initial running-in period (after 10,000 s). Error bars
being that the difference in particle sizes between the two powders was
show standards deviation in the CoF values calculated based on the test
not as large as that between medium and coarse powders (see Table 1).
repetitions. It can be seen that, with the sole exception PfN2, the average
Among all the three powder cut sizes, Pm showed the least sensitivity to
value for all the other coatings decreases with decrease in powder cut
the type of nozzle, with the average specific wear rates of all the four
size. For Pc and Pm, the average value of friction coefficient was not
coatings deposited with different nozzles being in the narrow range of
found to be dependent on the employed nozzle. Pf sprayed by N2, on the
14 × 10�8 mm3⋅N�1⋅m�1 to 21 × 10�8 mm3⋅N�1.m�1. Pc and Pf sprayed
other hand, had an average coefficient of friction that was about double
by nozzle N1 exhibited the least resistance against wear while Pf sprayed
as that of PfN1 and PfN4. The reason for this is not clear, but it could be
using nozzle N4 accounted for the best performance among all coatings.

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

N1 N2 N3 N4
0.5
0.45
0.4
Coefficient of friction (µ)

0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
Pc Pm Pf

a b
Fig. 11. a) Average steady state CoF values for all coatings, and b) typical evolution of CoF for coatings with different powder cut size.

Fig. 12. Specific wear rates of a) coatings, and b) mating alumina balls.

Comparing specific wear rates of the alumina balls used as counter Lower specific wear rates and consequently smaller contact surface
body in each of the wear tests (Fig. 12(b)), it was difficult to establish a areas of the corresponding balls (see Fig. 16) in case of coatings fabri-
clear correlation. However, a general trend can be observed that higher cated from finer powder cut size, could be correlated with the noted
specific wear rate in the coating leads to a higher specific wear rate in lower coefficient of friction values. This is consistent with other studies
the corresponding ball. Powder Pc sprayed with nozzle N3 was the only reporting that smaller frictional surface can result in lower friction co-
exception in this regard, showing comparable specific wear rate as PcN1 efficient [31,32].
but the counterpart ball exhibiting much lower wear than that of PcN1
counter body.

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 13. Schematic illustration of feedstocks Pc, Pm and Pf (a, b and c) and their respective flattening showing the effect of relative powder particle and WC particle
sizes on flattening behaviour.

4. Discussion Case II:


dp
4.1. Deposition behaviour δ= ≈ 1, ε ≈ 0 (6)
dc
The consistent decrease observed in deposition efficiency for each For Case I, where the particle size is much larger than the carbide size
nozzle when particle size is decreased can be discussed from various (δ ≫ 1), flattening ratio increases with the ratio dp/dc and can be
points of view. According to the literature, it is already known that for calculated theoretically [44]. In this case, the deformability of the par-
WC-based feedstock sprayed by cold spray and HVOF, the size and ticle is governed by equivalent properties of both binder and carbide
content of WC particles [33–36], powder porosity [29,37] as well as particles. However, with decrease in size of powder particle (dp) when
substrate hardness and roughness [38,39] can all significantly influence the carbide size is constant (dc), the flattening ratio progressively de-
the flattening ability of powder particles impacting the substrate and its creases to the point where the powder particle theoretically comprises
deposition rate. Presence of an intimate conformal contact surface only one carbide particle (Case II) and the flattening ratio approaches
occurring as a result of particle flattening is essential for good bonding, zero. As the ratio dp/dc approaches 1, solid carbide particles dominate
and can also be beneficial for enhancing deposition efficiency [36,37]. the flattening behaviour. Hence, because of low flattening ratio, the
Porous particles show better deformation ability or flattening upon chance of the particle being rebounded off increases. This trend is
impact compared to dense particles [37] and, as a result, have lesser observed when reducing particle size from Pc to Pm and Pf (Fig. 13(a, b
chance of being rebounded. As discussed in Section 3.1, in case of the and c)), with decrease in particle size resulting in decrease in δ value and
feedstocks used in the present study, increase in particle size corre- consequently a decrease in flattening ratio (ε) of the particles. This can
sponds to higher porosity content within powder particle and as a result explain how more particles tend to bounce off and result in lower
improves flattening ability. This is in line with the studies conducted by deposition rate for powders with smaller particles, when carbide size is
Gao et al. [37] on cold-sprayed WC-Co coatings, Varis et al. [29] on the same. High chance of particles corresponding to smaller δ values
HVOF-sprayed WC-CoCr coatings and Chivavibul et al. [40] on warm- being bounced off after impacting the surface is consistent with other
sprayed WC-Co coatings. So, better deformability can be one of the studies [33,42].
reasons for higher deposition rates noted when powder particle size is Surface roughness is another factor influencing flattening behaviour
increased (Fig. 5). of particles and, as a result, the deposition rate [45]. It was shown in
However, besides the porosity effect, the size of particles is another Section 3.3, Fig. 6, that the three coatings Pc, Pm and Pf are charac-
key factor determining flattening behaviour. For homogeneous parti- terized by different progressively decreasing surface roughness values.
cles, it has already been shown by experiment and modeling that smaller During spraying, every deposited layer can be considered as the ‘sub-
particles tend to exhibit greater resistance against deformation upon strate’ for the next pass. Higher roughness can result in higher induced
impact [41]. Several studies have been conducted with the aim of un- shear stress on the particle upon impact, which leads to better flattening
derstanding the effect of carbide dimensions on flattening behaviour of and, consequently, improved deposition rate [38,45].
WC-based coatings [33–35,42]. If the particle is assumed to be spherical, According to Accuraspray data (see Fig. 4), decrease in particle size
the flattening ratio can be defined as [41,43]; leads to a substantial increase in particles velocity. This can be another
key parameter influencing deposition behaviour of powders with vary-
h
ε = 1� (4) ing particle size. In case of cold spray, it has been reported that there
dp
exists a critical velocity which the particles must overcome in order to
get deposited successfully onto a substrate [46,47]. Similarly, there have
where dp and h are particle size and the height of flattened particle,
also been studies on metallic powders which reveal that, for velocities
respectively.
beyond a certain value, no major difference is noted in deposition effi-
Depending on the relative size of powder particle (dp) and carbide
ciency [48,49]. In some cases, it has indeed been shown that increase in
particle (dc), the flattening behaviour can be categorized as follows:
velocity can lead to increase in rebounding of particles [35]. Therefore,
Case I:
increase in velocity of powder feedstock containing hard WC particles
dp may not improve deposition rate.
δ= ≫1, ε > 0 (5)
dc

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

PcN1

PmN1

PfN1

PfN4

Fig. 14. SE SEM images of wear tracks on the four tested coatings, revealing changes in wear mechanisms with decreasing feedstock particle size. Pit areas are
indicated by ellipses/circles.

4.2. Wear behaviour within the wear track of the sample PcN1, which are negligible in the
other two samples. These pits could have been formed as a result of
Fig. 14 shows low and high magnification SEM images taken on wear breakage of group of carbides resulting in massive exfoliation. It is
tracks with the same track radii (r = 7 mm) on tested coating specimens plausible that the segregated carbides get stuck between sliding ball and
fabricated from the three feedstocks Pc, Pm and Pf, sprayed with nozzle sample surface leading to chipping of coating and consequently forma-
N1. Comparing the low magnification images with specific wear rate tion of narrow deep grooves. The other two samples do not exhibit
values (Fig. 12(a)), it can be inferred that samples with deeper and presence of such grooves, and wide shallow ploughing tracks are
higher number of grooves account for higher specific wear rate values. detectable instead. The tracks are deeper and higher in number for the
Another clear difference between the three images is the presence of pits sample PfN1 compared to sample PmN1. The ploughing tracks could

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 15. SE SEM image of tribolayer within the wear track of sample CfN1 along with the layered EDS image on tribolayer and EDS maps of O and Al.

PcN1 PmN1 PfN1


Fig. 16. Wear scars on alumina ball counterbody in case of the three coatings PcN1, PmN1 and PfN1.

have formed as a result of the alumina ball sliding over the surface layer which is perfectly bonded to the surface. Fig. 15 shows a typical
leading to coating material being pushed aside as well as beneath tribolayer within the wear track of sample CfN1. The EDS analysis on the
[50,51]. Using nozzle N4 for spraying Pf resulted in the best sliding wear tribolayer reveals presence of W, Co, Cr, Al and O elements, with O being
performance among all the eleven samples. From SEM images of its wear the predominant element and W, Co and Cr showing similar patterns.
track (Fig. 14), extremely shallow ploughing tracks are detectable Hence, the formed tribolayer is essentially a mixture of oxidized ele-
without any sign of grooving and carbide fragmentation. ments from the coating as well as alumina from the ball counterpart.
One feature that was observed in some of the wear tracks (e.g. PcN1 Formation of such oxide rich layers has been reported by others, and
in Fig. 14) was the formation of a thin, narrow and smooth tribolayer referred to as tribolayer or tribofilm [52–54]. Presence of a tribolayer
similar to that reported in a previous study [52]. In some cases, the can effectively separate the coatings surface from the counterpart ball
tribolayer seemed to be thicker and could be distinguished as a distinct and, therefore, change the governing tribological behaviour of the

Fig. 17. SE SEM micrographs revealing a) pores and b) binder accumulation region (with corresponding EDS maps) in regions outside of wear track of sample PcN4.

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 18. BSE SEM and EDS micrographs revealing oxide accumulation in pits within wear track of the sample PcN1.

Fig. 19. Breakage mechanism in Pc coatings, a and b) breakage of a fragment of coating, c) intergranular crack initiated from the pit shown in (b).

surface. It has been reported that the presence of such a tribolayer for material around the pit. Fig. 17(a) shows high magnification SEM
covering the surface of a wear track can significantly decrease the spe- images on shallow and deep pores on the surface of the coating, taken in
cific wear rate [53–56]. However, the presence or absence of this tri- areas outside of the wear track regions. Fig. 17(b) additionally shows
bolayer did not seem to significantly influence the specific wear rate or regions of accumulation of binder (in form of pits) outside of the wear
coefficient of friction of the corresponding samples in this study. The track. EDS analysis on the pits shows accumulation of binder rich in Cr in
reason could be that in none of the samples a continuous and wide tri- these regions. Similar EDS map was performed for Co and no accumu-
bolayer covering a significant fraction of the wear track could be lation of the element was identified. Similar analysis was also performed
distinguished. on pits within the wear track (Fig. 18). It is clear that, unlike the ones
Fig. 16 shows the wear debris accumulated around the leading edge outside the wear track (Fig. 17(b)), the pit within the wear track was
of the contacting region of the balls. Presence of the wear debris can filled with material transferred during wear testing, which was mostly
potentially act as third body particles and facilitate the process of ma- aluminum oxide from the ball counterbody.
terial removal [57,58]. Parallel ploughs on the balls are detectable along SEM analysis at higher magnifications was performed on the wear
the sliding direction and can be attributed to such third body action of tracks to explore breakage mechanism around the pits in more detail.
particles present in the debris. Fig. 19(a) and (b) shows breakage of coating in the form of batches of
It was observed that ploughing was the common mechanism in all carbides. In Fig. 19(a), breakage of a fragment was observable and
the three (Pc, Pm and Pf) coatings. It was also seen that, for coatings transformed along the sliding direction. It may be pointed out that
fabricated from the coarse powder (Pc), several narrow shallow grooves similar behaviour was observed for coatings with WC-CoCr feedstock of
are visible on the wear track apart from some pits. The presence of these identical chemistry sprayed with another HVAF spray gun (Kermetico,
pits was the main identifiable difference between the Pc coatings and the Inc.) [19]. Also, a groove can be detected continuing over the fractured
other two (Pm and Pf). These pits could have initiated from small pores fragment and being closured within the pit (shown by arrow). Existence
and accumulated binder areas (Fig. 17) where there was lack of support of the grooves facilitates breakage of fragments because of high amount

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 20. Breakage mechanisms in coatings a) Pm and b) Pf.

a: Pc b: Pm c: Pf
Fig. 21. Wear debris from: a) Pc coating, b) Pm coating and c) Pf coating.

of stressed induced to the coating due to presence of a third body par- As discussed, the presence of these pits can facilitate the process of
ticle. In Fig. 19(b), breakage of several fragments was observable being material removal. However, the pits are not reflected as removed ma-
separated both along the sliding direction and in the opposite direction terial when measuring volume loss, since they are already filled up with
as shown by arrows. These fragments were possibly fractured in absence wear products. Besides ploughing and grooving as the two common
of any major third body particle since there was no grooving detectable removal mechanisms for Pc coatings, crack initiation and propagation
over these fractured fragments. These pits can introduce some stress around pits leading to breakage of batches or groups of carbides was the
concentrated locations leading to crack propagation (shown by the other main wear mechanism. These batches of carbides can be further
square in Fig. 19(b)) and further breakage into fragments. Fig. 19(c) fragmented into individual carbides as a result of further sliding and
shows a high magnification image of the crack indicated in Fig. 14(b). It removed from the surface. The described mechanisms were similar for
can be seen that an intergranular crack was formed regardless of the the coarse powder sprayed with all the four nozzles (PcN1, PcN2, PcN3
carbide's presence towards the next pore. The fractured carbides are and PcN4). However, in case of Pm and Pf coatings, there was no
identified with red marks. detectable fragmentation of carbides as a batch.

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

Fig. 22. EDS analysis on wear debris from PcN1 coating.

In both Pm and Pf coatings, there were no signs of pits filled up with microstructural characteristics were assessed by conducting micro
wear products. Instead, as shown in Fig. 20, in the first step, binder indentation test, SEM, EDS and XRD analyses. The main conclusions are
around carbides seems to be removed resulting in lack of support around listed as following.
the carbides. Then due to load applied from slider, the individual car-
bides could get fractured, leading to production of submicron sized - For a given nozzle, reduction in particle size leads to increased
carbides (shown by arrows in Fig. 20). The last step would be removal of density, better homogeneity and higher hardness in the coating. At
these nano size wear products. SEM investigation of wear debris con- the same time, the reduction in particle size is accompanied by a
firms these differences in wear mechanism between Pc coatings and Pm/ reduction in deposition efficiency. Despite the decrease in particle
Pf coatings. size, negligible decarburization was detected in all the coatings. All
As shown in Fig. 21, size of debris particles in case of Pc coatings was these result in better wear performance of the coatings by decreasing
much coarser and irregular shaped than that observed in Pm and Pf the feedstock particle size.
coatings. Fig. 21(a) shows debris produced from Pc coatings, which are - Fine feedstock powder sprayed with nozzle 5L4 exhibited the best
mostly in size range of initial carbide particles (1–3 μm). Presence of wear performance among all the coatings. Therefore, nozzle 5L4 is
these micro size carbides acting as third body particles explains higher recommended for spraying fine powder. However, the specific wear
coefficient of friction during the ball-on-disc tests as shown in Fig. 11. rates of coatings with the medium sized feedstock were independent
For Pm and Pf coatings (Fig. 21(b) and (c)), very few micro size particles of nozzle type.
are found in the debris, with a majority of them being in the nanometric - Although no major change was observed in microstructure of the
size range and spherical in shape. coatings deposited from the same feedstock particle size but with
Comparing dimensions of the wear debris with friction coefficient different nozzle configurations, the average hardness value increased
values (Fig. 11(b)), it is clear that CoF value is reduced with reduction in by increasing length of the nozzle and/or its exit diameter (from
debris size. For Pm and Pf, the presence of nano-sized spherical shaped 4L4/4L2 to 5L4) for all the three particle sizes.
debris particles can result in reduction in friction coefficient [31,59,60]. - While shallow and wide ploughing was found to be the common
Also, it can be seen that by reduction in debris size, friction coefficient wear mechanism in all the coatings, decrease in feedstock particle
value as well as its fluctuation was reduced. size led to a major change in material removal mechanism in the
Semi-quantitative EDS analysis was conducted on debris from PfN1 corresponding coating. Wear mechanism for coarse feedstock coat-
samples shown in Fig. 22. Elements of O, W, Al, Co and Cr were ings involved crack propagation around pores and binder accumu-
detectable in debris. The EDS analysis conducted on wear debris from lation areas leading to breakage of batches of carbides with binder
Pm and Pc coatings showed similar result for all. into the pit areas. Further sliding of the ball possibly caused further
fragmentation and removal of these batches of carbides, with the
5. Summary and conclusions debris acting as third body particles to leave narrow deep grooves on
the coating surface. In medium and fine feedstock coatings, no pits
Sliding wear tests were conducted on different HVAF-sprayed WC- were observed. In these two coatings, the wear process seems to start
CoCr coatings with the aim of evaluating effect of feedstock particle size with removal of binder and subsequent fracture and fragmentation of
and spray nozzle configuration on tribological performance of the loosely bound individual carbides resulting in removal of fine-sized
coatings. Moreover, their influence on coatings' hardness and their carbides. SEM analysis of debris particles confirmed this difference,

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K. Torkashvand et al. Surface & Coatings Technology 423 (2021) 127585

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16
Tribological behaviour of HVAF-sprayed
WC-based coatings:
Role of process variables and binder chemistry
Thermally sprayed tungsten carbide (WC)-based metal matrix composite coatings are popular
candidates as wear resistant layers. High velocity air fuel (HVAF) process, which offers specific
advantages in terms of high adhesion strength and minimal in situ degradation/oxidation of powder
feedstock, can be employed to fabricate WC-based coatings.
In HVAF method, particles’ in-flight temperature and velocity can be influenced by the process
variables including nozzle configuration as well as feedstock particle size range. In this thesis, char-
acteristics and tribological behaviour of HVAF-sprayed WC-based coatings were investigated em-
ploying four different nozzle configurations and three different feedstock particle sizes of WC-CoCr
feedstock powder. It was revealed that decrease in powder particle size range can result in an im-
provement in microstructural characteristics as well as wear performance of the coatings.
Conventionally, cobalt has been widely used as binder to provide physical support for WC particles.
However, there have been some environmental, supply and economic concerns around Co for it to
be frequently labeled as a “critical raw material” or “conflict element” by the European Commission
and National Environmental Research Council. Consequently, the need for a substitute binder for
WC-based coatings has assumed some urgency during recent years. In this study, tribological be-
haviour of four HVAF WC-based coatings with alternative binders (WC-CoCr, WC-NiMoCrFeCo,
WC-FeNiCrMoCu and WC-FeCrAl) were investigated. Results suggest that WC-NiMoCrFeCo and
WC-FeNiCrMoCu coatings showed better or comparable sliding wear performance compared to
WC-CoCr coating (as reference).

ISBN 978-91-89325-02-9 (Printed version)


ISBN 978-91-89325-01-2 (Electronic version)

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