F ic ion 12(3): 522–538 (2024) ISSN 2223-7690
h ps://doi.o g/10.1007/s40544-023-0790-2 CN 10-1237/TH
RESEARCH ARTICLE
High- empe a u e ibological pe o mance o unc ionally g aded
S elli e 6/WC me al ma ix composi e coa ings manu ac u ed
by lase -di ec ed ene gy deposi ion
Ma a OSTOLAZA1*, Alai z ZABALA2, Jon Iñaki ARRIZUBIETA1, Iñigo LLAVORI2, Nago e OTEGI2,
Ai zol LAMIKIZ1
1 Depa men o Mechanical Enginee ing, Uni e si y o he Basque Coun y UPV/EHU, Plaza To es Que edo 1, Bilbo 48013, Spain
2 Facul y o Enginee ing, Mechanics and Indus ial P oduc ion, Mond agon Unibe si a ea, Lo amendi 4, Mond agon 20500, Spain
Recei ed: 21 Decembe 2022 / Re ised: 17 Ma ch 2023 / Accep ed: 19 June 2023
© The au ho (s) 2023.
Abs ac : Wea -d i en ool ailu e is one o he main hu dles in he indus y. This issue can be add essed h ough
su ace coa ing wi h ce amic- ein o ced me al ma ix composi es. Howe e , he maximum ce amic con en is
limi ed by c acking. In his wo k, he ibological beha iou o he unc ionally g aded WC-ce amic-pa icle-
ein o ced S elli e 6 coa ings is s udied. To ha end, he wea esis ance a oom empe a u e and 400 °C is
in es iga ed. Mo eo e , he ibological analysis is suppo ed by c ack sensi i i y and ha dness e alua ion,
which is o u mos impo ance in he p ocessing o composi e ma e ials wi h ce amic-pa icle- ein o cemen .
Resul s indica e ha unc ionally g aded ma e ials can be employed o inc ease he maximum admissible WC
con en , hence imp o ing he ibological beha iou , mos no ably a high empe a u es. Addi ionally, a shi
om ab asi e o oxida i e wea is obse ed in high- empe a u e wea es ing.
Keywo ds: ic ion, coa ing, me al ma ix composi e, unc ionally g aded ma e ials, high empe a u e, lase -
di ec ed ene gy deposi ion
1 In oduc ion
I is well known ha he pace o he au omo i e
indus y is s ongly se by go e nmen al es ic ions
conce ning en i onmen al issues. In e ms o emissions,
he Eu opean Commission se a 95 g CO2/km a ge
le el o 2021, while 15% and 37.5% educ ion goals
we e es ablished o 2025 and 2030, espec i ely [1].
Vehicle manu ac u e s ag ee ha ligh ening is a
c i ical ac o o a aining ene gy-e icien ca s,
ega dless o he p opulsion echnology [2]. The mos
p omising solu ion o minimising CO2 emissions,
whils inc easing he sa e y and imp o ing he c ash
pe o mance o ehicles, elies on he implemen a ion
o mode n ad anced high-s eng h s eels (AHSS) as
hey enable he educ ion o he weigh o au omo i e
componen s [3]. Un o una ely, hese ma e ials p esen
low oom empe a u e o mabili y and high sp ing
back [4]. The e o e, empe a u e-assis ed p ocesses,
i.e., ho s amping o p ess ha dening, a e necessa y
o o m AHSS componen s [5].
In ho s amping p ocesses, he ool damage caused
by wea and ic ion du ing he high- empe a u e
o ming p ocess is a hind ance in e ms o
p oduc i i y and ool li e ime [4], and s ems om he
una oidable con ac be ween he ool and he p ocessed
blanks [6]. Un o una ely, con en ional lub ican s
canno be employed o coun e hese phenomena, as
he empe a u e ange o he manu ac u ing p ocess is
a ou side he wo king ange o mos lub ican s [7].
F ic ion p oblems in ho o ming ools can be
o e come by su ace ea men s and deposi ion o
ad anced coa ings [8, 9]. A his poin , he localised
hea inpu and he apid solidi ica ion o ma e ials
* Co esponding au ho : Ma a OSTOLAZA, E-mail: [email p o ec ed]
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inhe en o lase p ocessing, place lase -di ec ed ene gy
deposi ion (L-DED) in an ad an ageous posi ion
compa ed o adi ional coa ing echnologies [10].
Indeed, L-DED yields minimum subs a e a ec ion
and low dis o ion, bu high in eg i y coa ings [11].
Consequen ly, demanding geome ical ole ances can
be me , while p o iding a good bond be ween subs a e
and coa ing. Fu he mo e, he ypically complex
su aces o ooling a e no es ic i e o L-DED
owing o i s ee o m abili y.
In su ace enginee ing, me allic and non-me allic
ma e ials a e o en used o imp o e he wea
esis ance o s eel subs a es. Alloying wi h elemen s
such as niobium, anadium, o ungs en, has been
demons a ed o ex end he li e ime o H13 ool
s eel [12]. The deposi ion o complex alloys such
as FeC MoVC on o ool s eel subs a es has been
in es iga ed oo [13]. Mo eo e , wea - esis an high
en opy alloy (HEA) coa ings ha e been es ed in eal
p ocess condi ions and p omising esul s ha e been
ob ained [14]. On he o he hand, Co-base wea -
esis an alloys, such as S elli e 6, possess high wea
esis ance no only a oom empe a u e bu also
when subjec o high empe a u es [15, 16]. The
solid-solu ion o ca bide- o ming elemen s and he
p ecipi a ion ha dening a e esponsible o he imp o ed
mechanical p ope ies o such alloys [17]. In addi ion,
he good ibological pe o mance a high empe a u es
is due o he o ma ion o an oxide laye , which
ac s as a lub ican and mi iga es ic ion [18]. Finally,
su ace enginee s o en eso o ce amics and ce amic
ha d me al coa ings o u he inc ease he esis ance
o wea due o hei high ha dness [6]. In his ega d,
lase p ocessing echnologies enable a localised
dispe sion o ce amic pa icles [4] o he deposi ion
o ce amic pa icle- ein o ced me al ma ix composi e
(MMC) coa ings [19].
The enhanced ibological pe o mance o WC-
ein o ced MMCs has been ex ensi ely epo ed in he
li e a u e. Nu minen e al. in es iga ed he ab asion
esis ance o di e en ma ix and ein o cemen
ma e ials [20]. They concluded ha sphe ical WC
ein o cemen esul ed in he bes ibological
pe o mance. Ba kowski and Kinal ound ha he
wea esis ance o he S elli e 6 Co-base alloy inc eases
when embedding WC ce amic pa icles [21]. They
concluded ha when he olume ic ac ion o WC
is oo high o he ha dness o he ma ix is oo low,
a mo e in ensi e wea mechanism o he coa ings
is p omo ed. None heless, in gene al e ms, an
enhancemen o he su ace p ope ies o he base
ma e ial was a ained. La e , when applying he
de eloped coa ing o a eal indus ial case s udy in
he ield o ag icul u e, hey ob ained a 25% inc ease
in he du abili y o ooling [22]. Also, Ni-base and
Co-base ma ixes a e o pa icula in e es when
high- empe a u e wea pe o mance is a ge ed [23].
Hence, mo e ecen wo ks ha e ocused on cha ac e ising
he high- empe a u e ibological beha iou o hese
coa ings. E anmanesh e al. in es iga ed he high-
empe a u e pe o mance o WC-Co and Ni/WC-Co
coa ings in e ms o wea [24]. They ob ained a
subs an ial imp o emen in he wea esis ance
and hey concluded ha so ab asi e and adhesi e
wea we e dominan . Wang e al. also ocused on
high- empe a u e wea es ing and con i med he
good beha iou o S elli e 6/WC coa ings [25]. In
addi ion, an imp o emen in he wea esis ance
o he coa ings ollowing he WC con en was
demons a ed. Howe e , coa ings wi h >20 w % o
WC showed a signi ican d op in e ms o he mal
a igue. Las ly, Ka maka e al. in es iga ed he high-
empe a u e ab asi e wea o AISI H13 ool s eel
coa ed wi h S elli e 6 and S elli e 6/WC [26]. Composi e
coa ings showed a highe ab asion esis ance in he
ange o empe a u es up o 650 °C, as compa ed o
he base ma e ial. The imp o emen was mo e e iden
he highe he empe a u e o he wea es .
In e ms o L-DED o MMCs, he p oduc ion o
good quali y coa ings is s ill a challenge. Fo ins ance,
ma e ial incompa ibili y is an issue o ackle [27].
De ec s ela ed o me allu gical in eg i y (po es o
c acking) a e equen ly encoun e ed [28]. As a
esponse, mul iple me hods ha e been p oposed o
elimina e c acking, namely, subs a e p ehea ing, he
addi ion o a e ea h oxides, o he elimina ion o
he sha p ansi ion be ween subs a es and coa ings
h ough unc ionally g aded ma e ials (FGM) [19].
The FGM s a egy is pa icula ly in e es ing o he
L-DED echnology [27]. In ac , he composi ion o
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he eeds ock in he p oduc ion o mul i-ma e ial
s uc u es can be easily con olled. In he case
o MMCs, a laye -wise a ia ion o he olume ic
ac ion o he ein o cemen is eadily a ainable.
Typically, unc ionally g aded ma e ials exhibi
lowe esidual s esses, which a e he main cause
o c acking in MMCs. Hence, he FGM s a egy can
be implemen ed o imp o e he in eg i y o MMC
coa ings p oduced by L-DED. In ac , Xu e al.
epo ed ha he c ack sensi i i y o MMC consis ing
o S elli e 6 and WC was signi ican ly educed when
in oducing unc ionally g aded ansi ions as compa ed
o sha p ma e ial ansi ions [29]. In addi ion, hey
s udied he oom- empe a u e wea esis ance o
mono-composi ional and unc ionally g aded MMCs
and go simila esul s. None heless, o he au ho s’
knowledge, he high- empe a u e wea pe o mance
o unc ionally g aded MMC coa ings as compa ed
o mono-composi ional MMC coa ings has no been
s udied so a .
Mo i a ed by he esea ch gap iden i ied in he
li e a u e, in he p esen wo k, he high- empe a u e
wea pe o mance o unc ionally g aded MMCs is
in es iga ed. Indeed, he FGM s a egy can be used
o inc ease he admissible WC% in MMC coa ings,
wi h subsequen pe o mance imp o emen . The
enhancemen o he wea p ope ies o he coa ed
and uncoa ed samples a bo h oom and high
empe a u es is assessed. Fu he mo e, he pe o mance
o unc ionally g aded and mono-composi ional
coa ings is compa ed. Las ly, he mos ele an
wea mechanisms o each scena io and ma e ial
a e iden i ied. The main con ibu ions o he p esen
esea ch wo k a e as ollows.
1) The c ack sensi i i y o mul ilaye MMC coa ings
deposi ed wi h di e en s a egies (i.e., FGM and
mono-composi ion) is assessed.
2) The wea esis ance o L-DED coa ings is
e alua ed bo h a oom empe a u e and 400 °C.
Coa ings wi h di e en op laye composi ions and
manu ac u ed wi h g aded and no g aded s a egies
a e s udied. All esul s a e compa ed o he uncoa ed
e e ence specimens.
3) The mic os uc u al e olu ion o he ma ix
when a ying he composi ion o he eeds ock is
s udied. Mo eo e , he ha dness o he ma ix and
he su ace ha dness o he p oduced specimens a e
in es iga ed.
2 Ma e ials and me hods
2.1 Ma e ials
In his esea ch, AISI H13 ool s eel was selec ed
as he subs a e ma e ial. The dimensions o he
subs a e bille s a e 45 mm × 35 mm × 8 mm. This
ma e ial is equen ly employed in he die and
mould indus y o high- empe a u e p ocess ooling.
The su ace coa ings applied o he AISI H13 consis
o a Co-base ma ix, simila o S elli e® 6, and a WC
ein o cemen . Comme cial L-DED powde s a e
employed o coa ing p oduc ion, namely, Me coClad
6 and Me coClad 52001 (Oe likon Me co). The
g anulome y o bo h powde s is in he ange o 45
o 106 μm. The composi ion o he subs a e ma e ial
and he L-DED eeds ock is shown in Table 1.
2.2 Tes specimen p epa a ion: L-DED p ocess and
hea ea men o e e ence specimens
The coa ing specimens we e p oduced by means o
a T uLase Cell 3000 L-DED machine. The lase
sou ce is a 3 kW Yb:YAG disk lase , wi h a 1,030 nm
wa eleng h. The lase spo diame e a he ocal
plane was se a 1.75 mm. To enable an adequa e
p ocess pa ame e selec ion, di e en se s o pa ame e s
wi h a ying powe , eed a e, and mass low a e
we e es ed be o e choosing he op imal ones. To ha
end, single-clad expe imen s we e ca ied ou . The
p ocessing condi ions es ed a e shown in Table 2.
Table 1 Composi ion o he ma e ials employed w % [30–32].
Ma e ial Co C W Fe Ni Si C Mo Mn P S V
Me coClad 6 Bal. 28.0 4.0 3.0 3.0 1.5 1.0 1.0 0.0 0.0 0.0 0.0
Me coClad 52001 0.0 0.0 Bal. 0.19 0.0 0.0 4.03 0.0 0.0 0.0 0.0 0.0
AISI H13 0.0 5.13 0.0 Bal. 0.0 1.03 0.39 1.43 0.4 0.03 0.03 1.0
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Table 2 Single-clad expe imen al es s o selec op imal p ocess
pa ame e s.
Tes Powe
(W)
Feed a e
(mm/min)
Mass low a e
(g/min)
1 700 400 2.97
2 600 400 2.97
3 800 400 2.97
4 700 450 3.34
5 700 350 2.60
Once he bes p ocess pa ame e s we e selec ed,
di e en o e lapping condi ions we e es ed, namely
30% and 40%.
Mos p omising esul s we e ob ained o he
i s se o pa ame e s and 30% o e lap. Indeed, such
p ocessing condi ions esul ed in de ec - ee clads
soundly bonded o he subs a e. In Fig. 1, he selec ed
single-clad, single-laye , and mul i-laye es s a e
shown.
The L-DED pa ame e s we e kep cons an o all
expe imen s, a 700 W lase powe and 400 mm/min
eed a e. In addi ion, he olume ic a e o he
eeds ock was ixed a 0.35 cm3/min, which esul s in
a cons an clad geome y (0.38 mm heigh and 1.84 mm
wid h). Thus, he mass lows o he ma ix and he
ein o cemen ma e ial we e calcula ed o each laye
acco ding o he a ge composi ion and he densi y
o he ma e ial. The powde is ed h ough a GTV PF
2/2 disk eede , which comp ises wo independen
hoppe s. In his manne , he powde low o each
one o he hoppe s can be uned independen ly and,
he e o e, he composi ion o he powde mix u e is
con olled p ecisely. The powde lows p o ided by
Fig. 1 Single-clad, single-laye , and mul i-laye samples p oduced
wi h he op imal p ocessing condi ions.
each hoppe a e combined in a mixing chambe
and ed o he mel pool h ough a disc e e coaxial
nozzle. A gon a a a e o 12 L/min and helium a a
a e o 4 L/m we e used as shielding and ca ie gases,
espec i ely. As a as he deposi ion s a egy is
conce ned, a zig pa h (one-way deposi ion s a egy)
was ollowed in each laye , al e na ing he X and Y
deposi ion di ec ions laye upon laye .
The dimensions o he deposi ed coa ings a e
oughly 10 mm×25 mm×2 mm. Fou di e en coa ing
designs we e es ed and each specimen was cons i u ed
by ou laye s (Fig. 2), whose composi ion a ies
acco ding o Table 3. In o al, ou specimens we e
p oduced o each coa ing design, one o me allu gical
and ma ix ha dness cha ac e isa ion and h ee o
wea es ing and su ace ha dness measu emen s.
In addi ion, uncoa ed AISI H13 samples we e also
p epa ed o wea es ing and su ace ha dness
measu emen . To ha end, h ee AISI H13 specimens
we e g ound and hea - ea ed, by quenching and
empe ing in acco dance wi h Fig. 3.
2.3 Inspec ion o he me allu gical in eg i y and
mic os uc u al analysis o he samples
The Nikon Op ipho -100 op ical mic oscope was
employed o mic os uc u al analysis pu poses. To
Fig. 2 Laye disposi ion in mono-composi ional and FGM
specimens.
Fig. 3 Q+T hea ea men o he e e ence uncoa ed AISI H13
specimens.
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ha end, wo c oss-sec ional samples we e ex ac ed
om he i s specimen o each coa ing design by
means o wi e-Elec o Discha ge Machining (w-EDM).
The samples we e subsequen ly moun ed, g ound, and
polished ollowing he app op ia e me allog aphic
p ocedu e. Las ly, he mic os uc u e was e ealed by
elec oly ic e ching wi h 10% oxalic acid solu ion a
10 V and 1 A o 1‒3 s.
In addi ion, he su ace in eg i y o he h ee
emaining specimens was inspec ed by means o
he Leica Z6 AP0 op ical mic oscope igh be o e
ibological cha ac e isa ion. Wi h he aim o de eloping
p ocessing maps o he p oduc ion o MMC coa ings
based on he c i e ion o su ace in eg i y, he su ace
c acking o he manu ac u ed samples was quan i ied
wi h ega d o h ee pa ame e s, i.e., he numbe o
c acked samples (ou o 3), he numbe o c acks,
and he a e age wid h o he c acks. The esolu ion
o he equipmen employed o his inspec ion was
351 LP/mm, ha is, abou 3 μm. Las ly, wi h he in en
o inc easing he eliabili y o hese measu emen s,
he wid h o c acks was measu ed en imes pe
sample. The ul ima e objec i e o hese p ocessing
maps is o de e mine he maximum admissible WC
con en in MMC coa ings, depending on he L-DED
s a egy employed in hei p oduc ion.
2.4 Cha ac e isa ion o he ha dness o he ma ix
and he su ace ha dness o he coa ing
As a as he mechanical cha ac e isa ion is conce ned,
bo h he ha dness o he ma ix and he ha dness
o he coa ing we e measu ed. Fo he i s one, he
c oss-sec ional samples we e employed, as indica ed
in Fig. 4. The Fu u e-Tech FM-800 mic oha dness
es e was employed o he ma ix cha ac e isa ion.
Inden a ions wi h 300 g and 12 s dwell ime ollowing
he scheme in Fig. 4 we e ca ied ou . In each line,
13 inden a ions we e done wi h a 500 μm dis ance
be ween cen es.
Fig. 4 Posi ion o he inden a ions o he mic oha dness
cha ac e isa ion. Measu emen s a di e en dis ances om he
su ace a e indica ed by he ed lines.
On he con a y, he ha dness o he coa ing was
measu ed a he su ace o he samples using a
Compu es SC E ns mac oha dness es e be o e
s ep 6 o Fig. 5. This es e ollows he Rockwell C
p inciple and i e inden a ions we e done o each
coa ing design.
2.5 T ibological cha ac e isa ion o he coa ings
The specimen p epa a ion p ocedu e o ibological
es ing is shown in Fig. 5. A pocke in he subs a e
ma e ial was milled and hen coa ed ollowing he
pa ame e s speci ied in Sec ion 2.2. The la ness o
he sample was ensu ed by means o w-EDM o he
coa ed su ace and backside g inding. Then, he op
su ace o he coa ings o be s udied was manually
polished wi h a SiC ab asi e pape un il a su ace
oughness o Ra 0.70±0.07 μm, Rz 5.00±0.70 μm,
was eached, no e ha he ini ial Ra and Rz we e
3.18±0.25 μm and 19.94±1.60 μm, espec i ely. This
was done be o e he ibological cha ac e isa ion.
Las ly, he pa ame e s o he ibological es ing we e
selec ed o ensu e an adequa e ep esen a ion o eal
ho s amping condi ions.
The p ocess pa ame e s du ing shee me al
o ming can be qui e b oad. A e analysing se e al
componen simula ions, Cillau en e al. obse ed
ha he con ac p essu e on la a eas anges be ween
3‒15 MPa on a e age, while i ises o 20‒100 MPa o
cu ed a eas, wi h maximum alues up o 200 MPa.
Table 3 Laye composi ion o L-DED specimens (MC6 and MC52001 s and o Me coClad 6 and Me coClad 52001, espec i ely).
Laye S elli e 6 Mono 5% WC Mono 5% WC FGM 10% WC FGM
1 100% MC6 95% MC6 5% MC52001 100% MC6 100% MC6
2 100% MC6 95% MC6 5% MC52001 97.5% MC6 2.5% MC52001 95% MC6 + 5% MC52001
3 100% MC6 95% MC6 5% MC52001 95% MC6 5% MC52001 90% MC6 + 10% MC52001
4 100% MC6 95% MC6 5% MC52001 95% MC6 + 5% MC52001 90% MC6 + 10% MC52001
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Simila ly, he sliding eloci ies o he inne a eas
anged be ween 20‒25 mm/s on a e age, whils he
ou e a eas aised o 50 mm/s, wi h maximum alues
eaching up o 200 mm/s [33]. When conside ing
empe a u e anges, i is impo an o pay a en ion
o he maximum empe a u e ha ho - o ming ools
ypically wi hs and. Ho man and S einbeiss obse ed
a cyclic e olu ion o ool empe a u e in ho s amping
p ocesses and eached a s able cycle eme ging a e
abou 10 cycles. Fo he case hey p esen ed, he
maximum empe a u e eached was a ound 375 °C
[34]. Conside ing ha he empe a u e o he ooling
s ongly depends on he cooling sys em design [35],
o his s udy, a empe a u e o 400 °C has been
chosen o ep esen he se e e end o he spec um
o ho s amping p ocesses. In o de o ob ain a
compa a i e ange o wea esis ance and ic ion
beha iou o he newly de eloped unc ionally g aded
S elli e 6/WC me al ma ix composi e coa ings, an
accele a ed es unde s anda dised ball-on- la
linea ecip oca ing sliding con igu a ion [36] agains
a e e ence ce amic coun e pa was pe o med.
T ibological es pa ame e selec ion was also suppo ed
by Wang e al. [25], whe e S elli e-6/WC coa ings
p oduced by lase cladding we e es ed o he
ooling indus y. Tes s we e ca ied ou on he B uke
UMT ibome e , using a 6 mm Ø Si3N4 ball as
he coun e pa wi h a no mal load o 8 N, which
co esponded o 900 MPa a e age He zian con ac
p essu e. Using a 2.5 mm s oke and a ecip oca ing
equency o 20 Hz, es s we e conduc ed a an
a e age o 100 mm/s linea speed un il comple ing
18,000 cycles (15 min), bo h a oom empe a u e
(RT) and 400 °C. The oom empe a u e expe imen s
we e pe o med unde 22±1 °C empe a u e and
48%±4% ela i e humidi y. The pin and he pla e
we e ul asonically cleaned in ace one o 10 min
ollowed by ai -d ying be o e each es . Th ee
eplica es pe condi ion we e ca ied ou o good
s a is ical ep esen a ion
The coe icien o ic ion was compu ed h ough
he ene gy dissipa ion me hod unde he ASTM G203
s anda d [37]. No e ha a e age ic ion coe icien
alues we e compu ed conside ing he las 75%
o he ic ion cu e o accoun solely o he s eady
s a e ic ion beha iou , a e he unning in.
Equa ion (1) shows he o mula ion o he ene gy
coe icien o ic ion (ECoF), being d
E he dissipa ed
ene gy o e a cycle, *
he slip ampli ude, and P he
con ac load [38].
d
*
4
E
E
P (1)
A non-con ac 3D op ical p o ile (Senso a S-Neox,
whi e ligh in e e ome y echnique) was used wi h
an objec i e o 20xDI (op ical esolu ion = 0.41 μm,
e ical esolu ion 1 nm) in o de o measu e he
wea sca s. Wea sca olume was compu ed on he
a eal measu emen s [39] and 2D p o iles we e also
ex ac ed o cha ac e ise he wea sca wid h and
dep h in SensoMap P emium 7 so wa e. Las ly, wo n
su aces we e analysed by scanning elec on mic oscopy
(SEM) and ene gy dispe si e spec ome y (EDX).
Fig. 5 Scheme o he sample p epa a ion p ocess ollowed o ecip oca ing wea es ing.
528 F ic ion 12(3): 522–538 (2024)
| h ps://mc03.manusc ip cen al.com/ ic ion
3 Resul s
3.1 C acking sensi i i y o MMC coa ings p oduced
by L-DED
Su ace c acking is a majo p oblem in he L-DED o
ce amic- ein o ced MMCs. Thus, he maximum
ungs en ca bide con en o MMC coa ings is limi ed
by he c acking sensi i i y o he ma e ial. Figu e 6
shows he su ace quali y o he specimens p epa ed
o ibological cha ac e isa ion, whe e he su ace
c acks a e deno ed by whi e a ows. All h ee
specimens co esponding o monoli hic S elli e 6
coa ings p esen good su ace in eg i y and no c acking
is obse ed (Fig. 6(a)). Good quali y coa ings we e
ob ained also when p oducing unc ionally g aded
coa ings wi h ungs en ca bide con en a ying om
0% o 5% WC (Fig. 6(c)). In con as , wo ou o he
h ee mono-composi ional specimens wi h 5% WC
expe ienced su ace c acking (Fig. 6(b)). Las ly, se e e
c acking was obse ed in all specimens manu ac u ed
ollowing he FGM s a egy wi h a 0% o 10% WC
con en a ia ion (Fig. 6(d)).
The c acking o MMCs deposi ed by L-DED has
been widely s udied in Re . [40]. C acks in hese
coa ings o igina e om he high esidual s esses
gene a ed du ing he deposi ion p ocess. As a
p ocess based on usion and apid solidi ica ion o
ma e ials, pa s manu ac u ed by L-DED wi hs and
high- empe a u e g adien s; hus, high he mal
s esses can be p oduced i no speci ic ca e is aken.
The emb i lemen o he ma ix due o he p ocessing
condi ions is also a ac o ha se e ely a ec s su ace
in eg i y. The loss o duc ili y p e en s he me al
ma ix om abso bing he esidual s esses o he
manu ac u ing p ocess. Addi ionally, he ein o cemen
pa icles ac as s ess concen a o s [26], which u he
exace ba e c acking. Hence, he c ack sensi i i y
o his ma e ial is going o limi he p oduc ion o
MMC coa ings by L-DED and he de elopmen o
p ocessing maps is use ul o be e unde s and hei
p ocessabili y.
Based on he analysis o he in eg i y o he su aces
pe o med, he c acking phenomenon is quan i ied
by means o h ee pa ame e s, namely, he numbe o
samples exhibi ing c acking (ou o he h ee p epa ed
specimens), he numbe o c acks p esen in each
sample, and he wid h o he c acks. Based on such
quan i ica ion, a p ocessing map has been de eloped,
o which he accep ance c i e ion es ablished is he
quali y assu ance based on he su ace in eg i y (Fig. 7).
I is concluded he maximum admissible WC con en
is 5% wi h he FGM s a egy and he employed p ocess
pa ame e s, whe eas his admissible maximum d ops
below 5% wi h no c acking mi iga ion s a egy.
I ollows om he ob ained esul s ha he FGM
s a egy is a use ul ool o p e en c acking. No
de ec s we e obse ed when manu ac u ing coa ings
wi h a 5% WC con en a he op laye s wi h he
FGM s a egy. Howe e , poo esul s we e a ained in
he no -g aded coa ings wi h he same op laye
composi ion. The elimina ion o he sha p ansi ion
alle ia es he esidual s esses gene a ed du ing he
deposi ion o successi e laye s. Thus, he p og essi e
Fig. 6 Su ace in eg i y o p oduced specimens: (a) S elli e 6 MONO, (b) 5% WC MONO, (c) 5% WC FGM, (d) 10% WC FGM.
F ic ion 12(3): 522–538 (2024) 529
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Fig. 7 P ocessing map o he L-DED o MMC coa ings, based
on he L-DED s a egy and he WC% a he op laye .
a ia ion o he composi ion used wi h he FGM
s a egy educes he c ack sensi i i y o ce amic-
ein o ced MMCs.
3.2 Mic os uc u al cha ac e isa ion o he MMC
coa ings
In Fig. 8, he c oss-sec ional images co esponding o
WC- ein o ced coa ings manu ac u ed wi h di e en
s a egies a e shown, namely, 5% WC MONO, 5%
WC FGM, and 10% WC FGM. In addi ion, highe
magni ica ion images o egions o in e es a e
p o ided. In he FGM specimens, he g adual a ia ion
o he WC% is clea ly e idenced, as no ce amic pa icles
a e p esen in he 1s laye , in e media e WC% is ound
in he 2nd laye , and he a ge WC% is eached in
he 3 d and 4 h laye s. Hence, he same olume ic
ac ion o WC pa icles is ound in he op laye o
specimens co esponding o 5% WC FGM and 5%
WC MONO, pe he design depic ed in Table 3.
On he o he hand, he he e ogeneous dis ibu ion
o he WC pa icles is isible in he c oss-sec ional
images o Fig. 8, owing o he Mu akami agen
employed o e ch he ungs en ca bide pa icles
selec i ely. In Fig. 8, he mel pool bounda ies and
limi s o he hea -a ec ed egion a e depic ed o be e
iden i y he clads and laye s o he coa ings. E en
in he 5% WC MONO specimen, egions con aining
a highe olume ic ac ion o WC and egions
con aining a lowe ac ion a e obse ed. This is
a esul o he di e en luid dynamic beha iou
o ce amic and me al pa icles h ough he nozzle.
Mo eo e , he he e ogeneous dis ibu ion o pa icles
is u he exace ba ed by bo h g a i a ional and
Ma angoni e ec s in he mel pool.
In e ms o me al-ce amic in e ac ion, MMCs
manu ac u ed h ough usion-based p ocesses o en
exhibi composi ional and mic os uc u al changes
in he me al ma ix. The he mal na u e o usion-
based p ocesses p omo es he eac ion be ween he
Fig. 8 C oss-sec ional images co esponding o WC- ein o ced coa ings manu ac u ed wi h mono-composi ion and unc ionally g ade
d
s a egy. Le -hand images e ched by Mu akami agen ( ungs en ca bide pa icles a e da kened) and high magni ica ion images a e
elec oly ically e ched wi h 10% oxalic acid.
530 F ic ion 12(3): 522–538 (2024)
| h ps://mc03.manusc ip cen al.com/ ic ion
ein o cemen and ma ix ma e ial. When his
in e ac ion is la ge enough, he ma ix is modi ied
globally. Howe e , when li le WC concen a ions a e
employed o he exposu e ime o he ma e ial o high
empe a u es is con olled, his eac ion is educed.
Consequen ly, he ma ix is only a ec ed locally and
he p ope ies o he base ma e ial emain simila
om a global pe spec i e. This is he case o he
specimens p oduced in he p esen s udy. To alida e
such a hypo hesis, he mic os uc u e o he me al
ma ix co esponding o he composi ions employed
h oughou he expe imen s was in es iga ed (Fig. 9).
The base ma e ial wi h no ce amic ein o cemen ,
co esponding o 0% WC (Fig. 9(a)) shows he ypical
hypoeu ec ic mic os uc u e o he S elli e 6 Co-base
alloy [41]. The whi e dend i es co espond o he
Co- ich γ solu ion, while he da k phase co esponds
o he in e dend i ic eu ec ic s uc u e composed o
Co-, C -, and W-ca bides [42]. The same mic os uc u al
phases and simila olume ic ac ions a e obse ed
in all specimens and o all composi ions (Figs. 9(b)‒
9(d)). Sligh a ia ions o he g ain size a e obse ed,
which can be a ibu ed o di e en cooling a es
and solidi ica ion speeds, bu also o he e ec o
in oducing ein o cemen pa icles. Disc e e ca bides
a e a d i e o g ain e inemen [43]. None heless, no
clea conclusions can be d awn om his obse a ion,
as L-DED clads do ha e a ce ain le el o mic os uc u al
he e ogenei y and he obse ed g ain size a ia ions
all wi hin ha ange. To sum up, no signi ican
modi ica ion o he ma ix mic os uc u e was
obse ed due o he in e ac ion o he ma ix wi h he
ein o cemen phase.
3.3 Cha ac e isa ion o he ha dness o he ma ix
and he su ace ha dness o he coa ing
In he p esen wo k, he ha dness o he MMC coa ings
is in es iga ed a mic oscopic and mac oscopic scales,
o cha ac e ise mechanically he ma ix and he
composi e, espec i ely.
The ha dness o he ma ix is measu ed a 100 μm,
200 μm, and 500 μm om he su ace o he coa ing,
pe Fig. 4. The esul s co esponding o he ma ix
ha dness cha ac e isa ion a e shown in Fig. 10.
Inden a ions loca ed in o close o WC pa icles we e
excluded om he a e aging, as he a ge in his
cha ac e isa ion is he ma ix o he MMC coa ing.
Li le a ia ion is obse ed among he specimens
s udied and all o hem show simila ha dness alues
as compa ed o he e e ence specimen (i.e., S elli e 6
MONO). The e o e, i is concluded ha he e ec o
he ein o cemen pa icles on he ma ix p ope ies
is negligible o he employed p ocess pa ame e s
and eeds ock composi ions.
A sligh ly highe alue in he ha dness o he
ma ix o he 10% WC FGM sample is obse ed in
ce ain p o iles. This is asc ibed o he ein o cemen
pa icles loca ed below he es ed su ace, which,
al hough no isible, s ill suppo he ma ix s uc u ally.
On he o he hand, he 5% WC FGM sample exhibi ed
a sligh ly lowe ha dness a a 100 μm dis ance om
he su ace. The con inuous hea ing and cooling
Fig. 9 Mic os uc u al analysis o he MMC specimens: (a) 100% S elli e 6, (b) 97.5% S elli e 6 + 2.5% WC, (c) 95% S elli e 6 + 5% WC,
and (d) 90% S elli e 6 + 10% WC.
F ic ion 12(3): 522–538 (2024) 537
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Ma a OSTOLAZA. She ob ained
he M.S. deg ees in bo h Mechanical
Enginee ing (UPV/EHU) and
Ae ospace Manu ac u ing (C an ield
Uni e si y) in 2018. She cu en ly
holds a esea ch posi ion a he
Depa men o Mechanical
Enginee ing o he Uni e si y o he Basque Coun y
(UPV/EHU), while simul aneously wo king on he
Ph.D. He esea ch wo k ocuses mainly on mul i-
ma e ial addi i e manu ac u ing and lase di ec ed
ene gy deposi ion p ocesses; pa icula ly, on he
manu ac u ing o unc ionally g aded ma e ials and
composi e ma e ials, o wea esis an coa ing
applica ions. He wo k has esul ed in he publica ion
o h ee indexed scien i ic a icles so a , as well as in
se e al con ibu ions o na ional and in e na ional
con e ences.
