L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
341–350
MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR
BEHA VIOR OF FE-BASED AMORPHOUS COATINGS BY LASER
CLADDING
MIKROSTRUKTURA IN VISOKOTEMPERATURNA MEHANSKA
OBRABA AMORFNIH PREVLEK NA OSNOVI @ELEZA,
IZDELANIH Z LASERSKIM NAPR[EV ANJEM
Lu Xie
1*
, Yueming Wang
2
, Jianlin Yang
1
, Chenlong Li
2
, Xuhang Han
2
, Jie Huang
2
1
School of Management Engineering, Jiangsu Urban and Rural Construction Vocational College, Changzhou 213147, China
2
Hunan Provincial Key Defense Laboratory of High Temperature Wear-resisting Materials and Preparation Technology, Hunan University of
Science and Technology, Xiangtan 411201, PR China
Prejem rokopisa – received: 2023-01-24; sprejem za objavo – accepted for publication: 2023-06-04
doi:10.17222/mit.2023.803
FeCrMoCB amorphous coatings were prepared on 316 stainless steel via an amorphous powder. Scanning electron microscopy
(SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) were used to analyze the microstructure, composi-
tion, and phase structure of the coatings. Hardness and friction wear testers were applied to investigate the microhardness and
wear behavior of the coatings. Results show that the Cr 23C 6,C r 15Fe 7C 6 and Fe 3Mo crystal phases appeared after laser cladding
relative to the complete amorphous powder, and the amorphous phase fraction of the coating was calculated up to 68.4 % using
the Verdon method. The coating exhibited a dominating adhesive wear mechanism under room temperature (RT) and trans-
formed to a fatigue wear mechanism as wear test temperature increased to 600 °C. As the temperature was elevated from RT to
600 °C, the wear rate increased from 26 × 10
–6
mm
3
/N·m to 79 × 10
–6
mm
3
/N·m. The laser-cladded Fe-based amorphous coating
exhibited much stronger wear performance than the 316 stainless steel, even the wear rate reached one third of that of steel.
Keywords: laser cladding, Fe-based amorphous coating, test temperature, wear behavior
V ~lanku avtorji opisujejo izdelavo in karakterizacijo amorfnih prevlek FeCrMoCB na podlagi iz nerjavnega jekla vrste 316.
Izdelava prevlek je potekala z laserskim napr{evanjem amorfnega prahu. S pomo~jo vrsti~ne elektronske mikroskopije (SEM),
energijske disperzijske spektroskopije (EDS) in rentgenske difrakcije (XRD) so analizirali mikrostrukturo ter dolo~ili kemijsko
in fazno sestavo izdelanih prevlek. Obrabno odpornost prevlek so ocenili z meritvami trdote in testne naprave za dolo~itev
obrabe zaradi trenja. Rezultati preiskav so pokazali, da so med laserskim napr{evanju nastale kristalini~ne faze Cr 23C 6,
Cr 15Fe 7C 6 in Fe 3Mo, S pomo~jo Verdonove metode pa so ugotovili, da je nastali dele` amorfne faze v prevlekah do pribli`no
68,4 %. Prevladujo~i obrabni mehanizem do sobne temperature je adhezivna obraba in prehaja v mehanizem obrabe zaradi
utrujanja materiala do temperature 600 °C. Od sobne temperature pa do 600 °C je hitrost obrabe narasla s 26 × 10
–6
mm
3
/N·m na
7 9×1 0
–6
mm
3
/N·m. Izdelana lasersko napr{ena amorfna prevleka na osnovi `eleza je mnogo bolj odporna proti obrabi kot
podloga iz jekla vrste 316 in je ocenjeno za do tretjino manj{a.
Klju~ne besede: lasersko nana{anje, amorfne prevleke na osnovi `eleza, temperatura preizkusa, visokotemperaturna obraba
prevleke
1 INTRODUCTION
Amorphous alloys have gained increasing attention
because of their high hardness and excellent mechanical
properties.
1–5
Among those amorphous alloys, Fe-based
amorphous alloys have attracted much interest due to the
relative low cost and high wear resistance for industrial
applications.
6–22
However, the production and application
of Fe-based amorphous alloys were restricted because of
dimension limitations and room-temperature brittle -
ness.
23–27
An amorphous coating, as an alternative form of
amorphous alloy, can overcome the dimensional limita-
tion and avoid the room-temperature brittleness of an
amorphous block, receiving more and more attention in
surface engineering.
28–32
Various methods have been ap-
plied to fabricate Fe-based amorphous coatings, includ-
ing plasma spraying, high-velocity oxygen fuel (HVOF)
spraying, laser cladding and so on. The microstructure,
mechanical properties, and elevated-temperature tribolo-
gical performance of an Fe-Cr-Mo-W-C-B-Y amorphous
coating that was prepared via activated combustion
high-velocity air fuel (AC-HV AF) spraying was investi-
gated by Liang et al.
33
The wear mechanism changed
from abrasive wear accompanied by delamination and
adhesive wear to the delamination and adhesive ones as
temperature rose from 293 K to 673 K. The evolutions of
microstructure, fracture toughness and the sliding-wear
behaviors of APS Fe
43
Cr
16
Mo
16
(C,B,P)
25
amorphous
coatings, which were fabricated by air plasma spraying
(APS) with various powers, were investigated by Cheng
et al.
34
Laser cladding has gained much attention due to
super high bonding strength and coating density relative
Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350 341
UDK 686.4:544.022.6:620.193.95 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 57(4)341(2023)
*Corresponding author's e-mail:
xielucsu@163.com

to other fabricating technologies. Lu et al.
35
prepared
crack-free Fe-based amorphous coatings by laser clad-
ding, which adopted a triple laser scanning strategy. The
deposited Fe-based amorphous coating displayed a stable
wear process and a low wear loss for a much longer ser-
vice time under dry-sliding wear conditions, which was
much superior to 45 steel. Fe-Cr-Si-P/La
2
O
3
amorphous
composite coatings were prepared on 304L substrates by
laser cladding, as reported by Lu et al.
36
The effects of
La
2
O
3
content on the microstructure, phase composition
and microhardness of composite coatings were investi-
gated. Hou et al.
37
synthesized a novel amorphous com-
posite coating on 3Cr13 stainless steel by laser cladding
an Fe-Cr-Mo-Co-C-B amorphous powder. The highest
hardness of the cladding layer was 1179 HV
0.5
, which
was about 6 times that of the 3Cr13 stainless-steel sub-
strate (200 HV
0.5
). As a result, the wear resistance of the
substrate was greatly improved by the cladding layer.
However, there are few reports on the effects of tem-
perature on the wear behavior of a laser-cladded
Fe-based amorphous coating, especially the high-temper-
ature wear friction behavior was rarely studied. As a re-
sult, an FeCrMoCB amorphous coating was deposited on
316 stainless steel by laser cladding. And systematic
study was carried out to investigate the effects of various
test temperatures on the microstructure and wear proper-
ties of the Fe-based amorphous coating.
2 EXPERIMENTAL
2.1 Synthesis of powder and coating
A commercial Fe-based amorphous powder (Liquid
metal company, USA) with a particle size of 16–54 μm
was adopted to fabricate the Fe-based amorphous coat-
ings. The nominal composition of the feedstock is listed
in Table 1. The 316 stainless steel plates with dimen-
sions of 100 × 30 × 10 mm
3
were selected as substrates.
The substrates were sand blasted to activate the surface
and remove the grease for a higher bonding strength. The
substrate surface roughness (R
a
) was controlled to about
5 μm. Subsequently, they were ultrasonically cleaned and
dried in air. The spray experiments were conducted via a
commercially available laser system (LDF-3000,
Laserline, Germany), an operating optical fiber (600 μm,
Laserline, Germany), a laser integrated control system
(S7-1200, Siemens, Germany), a laser-cladding coaxial
powder-feeding nozzle (OTS-2, Laserline, Germany) and
a water-cooling system and a powder-feeding system.
The pressure of powder feeding gas (N
2
) and the height
of the nozzle from the sample surface was 6 Mpa and
12–14 mm, respectively. The nozzle was made of red
copper. The laser cladding parameters are listed in Ta-
ble 2.
Table 1: Nominal composition of the Fe-based amorphous powder
Element Cr C Mo B Fe
FeCrMoCB 26.0 2.3 17.0 2.1 Bal.
Table 2: Laser cladding parameters from Fe-based amorphous powder
Element
Laser
power
/kW
Scanning
speed
/(mm·s
–1
)
Spot diam-
eter
/mm
Over-
lapping ra-
tio /%
FeCrMoCB 1.4 12 3 50
2.2 High-temperature friction and wear testing
Dry sliding tribological properties of the laser
cladded Fe-based amorphous coatings were investigated
by a reciprocating friction-and-wear tester (GF-I,
Lanzhou ZhongkeKaihua Technology Development Co.,
Ltd., China) in accordance with ASTM D6279-2003
(2013) at room temperature, 200 °C, 400 °C and 600 °C.
Si
3
N
4
balls with diameter of 6 mm were selected as the
counterparts. New balls were used for each test. All the
coating samples were grinded and polished to a mirror
surface with roughness of R
a
= 1 μm. The wear debris
was collected after wear testing for subsequent observa-
tion.
The load, rotating speed, friction time and sliding
distance were 60 N, 600 min
–1
, 30 min and 5 mm, re-
spectively. The wear rate Ws of the coating can be esti-
mated using the equation of Ws = V/DL, where V is the
volume loss, D is the sliding distance, and L is the load
applied to the specimen. The volume loss V = m/ ,
where is the density of the coating material, m is the
mass loss measured after each test. The surfaces of the
coatings before and after the wear friction were charac-
terized by SEM.
2.3 Microstructural characterization
The surface morphologies of the feedstock, la-
ser-cladded coatings, wear debris, friction and wear sur-
faces of the amorphous coating and Si
3
N
4
dual grinding
balls were characterized using a scanning electron mi-
croscope (TescanMira4, Tescan Orsay Holding, Czech
Republic). The phase structure was studied by X-ray dif-
fraction (XRD, Rigaku D/max-2550VB) using Cu-K
 ra-
diation. The diffraction angle was from 20° to 80°. The
coating porosity was evaluated using the Image Pro-Plus
6.0 software. At least ten cross-sectional SEM images at
a magnification of 1000 times were randomly selected
for the porosity calculation of each coating.
3 RESULTS AND DISCUSSION
3.1 Microstructural characterization
The particle size distribution of the Fe-based amor-
phous powder ranging from approximately 15 μm to
80 μm (most of particles ranged from 35 μm to 40 μm) is
suitable for laser cladding, as shown in Figure 1a.
Spherical and dense microstructures with few pores can
be found as Figure 1b and 1c. This kind of compact
microstructure of feedstock is beneficial to obtain a uni-
form melting effect during the laser cladding. Finally, a
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
342 Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350

coating with a homogeneous microstructure can be de-
posited.
38,39
Figure 2 shows Fe, Cr, Mo, C and B element-map
distributions on the cross-section of the powder particle.
The main elements including Fe, Cr and Mo are homo-
geneously distributed in the particle. The composition
homogeneity of the laser-cladded amorphous coating can
be improved by this kind of powder.
Figure 3 shows the XRD patterns of Fe-based amor-
phous powder and coating. A broad diffused scattering
peak appears between 40° and 50°, as shown in Fig-
ure 3, which is the typical pattern of an amorphous
phase, indicating almost complete amorphization of the
iron-based powder. Several sharp peaks appear in the
XRD pattern of the coating, which is related to the for-
mation of some crystal phases during laser cladding. The
crystal phases were found to be Cr
23
C
6
,C r
15
Fe
7
C
6
and
Fe
3
Mo via the MDI Jade. The amorphous phase fraction
of the coating was about 68.4 %, after calculation using
the Verdon method. The appearance of crystal phases
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350 343
Figure 1: Particle size distribution and cross-section morphology of the Fe-based amorphous powder: a) particle size distribution, b) panorama
morphology and c) high-magnification morphology of a single particle
Figure 2: Fe, Cr, Mo, C and B element-map distributions on the cross-section of a single Fe-based amorphous particle

can be ascribed to part of the powder being melted dur-
ing the laser cladding, and then crystallization occurred
in the subsequent cooling and solidification process.
Moreover, a portion of crystallization of cladded coating
occurred due to being heated during subsequent deposi-
tion.
Figure 4 shows the SEM photographs of the center
and bottom of the cross-section of cladded Fe-based
amorphous coating. From Figure 4a and 4b,l a r g e
amounts of crystalline grains appeared in the amorphous
matrix, representing rectangular and triangular shapes.
The three phases are indicated by the colors of light grey,
white and dark grey, respectively. The interface morphol-
ogy of the coating and substrate is shown in Figure 4c
and 4d. A planar layer appeared in the bonding region
with a thickness of about 2 μm. With increasing distance
from the surface of substrate, the planar layer was gradu-
ally restrained, and several columnar dendrites were
formed. With increasing distance from substrate surface,
the columnar dendrites transformed to ellipsoid grains.
Subsequently, rectangular and triangular grains were pre-
cipitated at the center of the cladded coating as in Fig-
ure 4a and 4b.
According to the classical theory of the rapid solidifi-
cation, the phase and the morphology of material
microstructure are basically related to the ratio of tem-
perature gradient G to solidification rate R, i.e. G/R.
40,4
In
the initial stage of laser cladding, the powder was melted
by laser beam, and conducted the heat to the substrate
surface, which led the metallurgical bonding of the coat-
ing and coating. In this condition, the G was large and R
was small, therefore, the G/R was huge, leading the pla-
nar layer growth in the bonding area. With increasing
distance from the substrate surface, the G/R decreased,
and then the growth of dendrites and fine grains was sup-
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
344 Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350
Figure 3: XRD patterns of the Fe-based amorphous powder and coat-
ing
Figure 4: SEM photographs of the cross-section of Fe-based amorphous coating prepared by laser cladding: a) the center layer of the cladded
Fe-based amorphous coating, b) magnified image of a), c) the bottom of the cladded Fe-based amorphous coating, d) magnified image of c)

pressed. Meanwhile, coarse ellipsoid grains, rectangular
and triangular grains started to precipitate and grow.
Figure 5 shows EDS mapping of the cross-section of
the interior coating. It should be noted that the white
phase, dark phase and grey phase were the Mo-enriched
area, the Fe-enriched area and the Cr-enriched area, re-
spectively. Oxygen and carbon were uniformly distrib-
uted in the coating. As a result, the rectangular grains
and ellipsoid grains were mainly Fe alloy and Mo alloy,
respectively.
Figure 6 shows the EDS mapping of the interface of
the coating and substrate. The result shows that the grey
phase region is rich in Fe, while the white phase region
is rich in Cr and Mo. This morphology indicates that as
the laser cladding began, the G/R value was huge, result-
ing in large amounts of precipitation of Fe-based crystal-
line material. It is dominated by columnar dendrites near
the substrate surface and ellipsoid grains in the centre
coating, as the above results indicated. The transforma-
tion of morphology did not change the phase composi-
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350 345
Figure 5: EDS mapping of the cross-section of the interior coating
Figure 6: EDS mapping of the interface of coating and substrate

tion according to the element-distribution result. More-
over, oxygen is uniformly distributed, indicating there
was few preferential reactions between the metallic ele-
ments and oxygen.
3.2 Microhardness and wear behavior of iron-based
amorphous coating
3.2.1 Microhardness
Microhardness of various areas from outer coating to
the substrate can be found in Figure 7. The microhard-
ness of the inner coating, outer coating, bonding area and
steel substrate were approximately 1300 HV
0.1
,
1250 HV
0.1
, 300 HV
0.1
and 170 HV
0.1
, respectively. The
microhardness of the iron-based amorphous coating was
much higher than that of steel substrate due to the
atomic-structure randomness in the amorphous phase
42
.
In addition, the hardness of outer coating was a little
lower than that of inner one, which may be due to the re-
sidual thermal stress during laser cladding. Note here,
tensile stress formed in the coating due to rapid solidifi-
cation and shrinkage of the droplet in the process of laser
cladding. The hardness of the bonding area was between
those of the laser cladded coating and the steel substrate
for being composed of the amorphous phase and the sub-
strate.
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
346 Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350
Figure 8: Panorama and local magnification images of the friction surface of amorphous coating after wear test at different temperatures for
30 min: a) and b) RT, c) and (d) 200 °C, e) and f) at 400 °C, g) and h) 600 °C
Figure 7: Microhardness of various areas from outer coating to steel
substrate

3.2.2 Wear behaviour
The morphologies of the friction surface of the amor-
phous coating after wear tests at RT, 200 °C, 400 °C and
600 °C for 30 min are shown in Figure 8. A large area of
cold-welding morphology can be found on the friction
surface of the laser-cladded amorphous coating (see Fig-
ure 8a and 8b). Adhesive wear was the dominant wear
mechanism of the amorphous coating during the RT fric-
tion test. During the wear test, a part of material on the
top surface of amorphous coating was cut off and ad-
hered to the worn surface of the Si
3
N
4
ball due to the
hardness of the latter being higher than that of the for-
mer. And then the coating and grinding ball were
partially bonded and worn together, resulting in
cold-welded regions on the friction surface of the amor-
phous coating. The cold-welding regions decreased, sev-
eral grooves and cracks appeared in the friction surface
of amorphous coating after wear test 200 °C for 30 min
as shown in Figure 8c and 8d. The cold-welded regions
were almost invisible, and delamination occurred as
shown in Figure 8e and 8f. Typical fatigue wear was the
main mechanism as friction temperature increased up to
400 °C. A number of delamination, big cracks and holes
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350 347
Table 3: EDS result on the initial amorphous coating and friction surfaces of the coating after wear test at RT, 200 °C, 400 °C and 600 °C for 30
min
Element
Contents of initial
coating
/(w/%)
Contents of RT
friction surface
/(w/%)
Contents of 200 °C
friction surface
/(w/%)
Contents of 400 °C
friction surface
/(w/%)
Contents of 600 °C
friction surface
/(w/%)
O 0.13 12.59 13.30 13.65 21.75
Fe 80.98 44.90 44.85 44.14 39.45
Cr 7.65 20.75 20.20 20.28 18.15
Mo 5.69 15.89 14.22 15.79 13.76
C 5.54 4.24 6.13 5.04 3.42
N / 0.20 0.30 0.02 0.01
Si / 1.44 1.01 1.09 3.46
Figure 9: Oxygen distributions on wear traces of iron-based amorphous coatings after wear test at different temperatures for 30 min: a) RT,
b) 200 °C, c) 400 °C and d) 600 °C

appeared, while cold-welded regions completely disap-
peared in the friction surface (see Figure 8g and 8h).
The EDS results of the initial amorphous coating and
the friction surfaces of the coatings after the wear tests at
different temperatures for 30 min are shown in Table 3.
The O content (12.59 %) on the friction surface of coat-
ing after wear test at RT is higher than that (0.13 %) of
initial amorphous coating due to self-heating from con-
tinuous friction. Therefore, oxidation wear occurred
throughout the friction experiment. Moreover, the O con-
tents on the friction surfaces gradually increased with the
test temperature. From oxygen distributions on the wear
traces as shown in Figure 9, the oxygen uniformly dis-
tributed on the friction surfaces of the coatings, indicat-
ing the sufficient reaction of oxygen and metal elements
during wear friction. It is notable that several oxy-
gen-rich regions can be seen in Figure 9c. This can be
ascribed to the coating roughness that decided its surface
microscopic height difference, which can cause local
temperature rising, and then the local oxygen content in-
creased.
Wear debris collected from the iron-based coatings
after the wear test at various temperatures for 30 min can
be found in Figure 10. It should be noted that the parti-
cle size of wear debris increased with the test tempera-
tures. In addition, the portion of plate-like particles of
wear debris increased with the test temperature too. Se-
vere abrasion occurred during the 600 °C friction test
and as a result complex micro-cracks were formed in the
plate-like particles, as shown in Figure 10d.
Figure 11 shows the friction coefficient vs. time
curves of the amorphous coating under various wear test
temperatures. There is a long transitional period in the
initial stage of the friction curve of the coating at RT due
to the adhesive wear mechanism, which is consistent
with the above conclusion of a friction surface morphol-
ogy. The average friction coefficients of the coatings are
shown in Figure 12. The average friction coefficients of
L. XIE et al.: MICROSTRUCTURE AND HIGH-TEMPERATURE WEAR BEHA VIOR OF FE-BASED ...
348 Materiali in tehnologije / Materials and technology 57 (2023) 4, 341–350
Figure 11: Friction coefficient vs. time curves of the amorphous coat-
ing under various test temperatures
Figure 10: Wear debris collected from iron-based amorphous coatings after wear test at various temperatures: a) RT, b) 200 °C, c) 400 °C and
d) 600 °C

the coatings at RT, 200 °C, 400 °C and 600 °C are 0.55,
0.68, 0.69, 0.72, respectively. The friction coefficient
was gradually increased with the temperature, which can
due to the increasing of coating roughness caused by the
coating surface oxidation. It is notable that the average
friction coefficient was sharply increased when the tem-
perature was elevated from RT to 200 °C. Nevertheless,
the friction coefficient difference of coating under
200 °C, 400 °C and 600 °C were relative small. This ten-
dency is completely consistent with the conclusion of
oxygen content on the coating friction surface under var-
ious wear temperatures.
Figure 13 shows the wear rates of Fe-based amor-
phous coating and steel substrate after wear tests at vari-
ous temperatures for 30 min. The wear rates of the amor-
phous coatings and iron substrate gradually increased
with the friction temperatures. Note here, the wear rates
of the iron-based amorphous coating were much lower
than those of the steel substrate. As a result, the steel
substrate can be effectively protected by Fe-based amor-
phous coatings prepared by laser cladding.
4 CONCLUSIONS
FeCrMoCB amorphous coatings were successfully
prepared by laser cladding on 316 stainless-steel sub-
strates. The effects of wear temperature on the wear be-
havior of Fe-based amorphous coating were discussed.
The main results are summarized as follows:
The 1300HV
0.1
microhardness of the inner coating
was the highest among the outer coating, inner coating
and bonding area, due to the residual thermal stress dur-
ing the laser-cladding process.
As the wear temperature rose from RT to 600 °C, the
dominating wear mechanism transformed from adhesive
wear to fatigue wear, and the wear rate increased from
26×10
–6
mm
3
/N·m to 79×10
–6
mm
3
/N·m.
The laser-cladded Fe-based amorphous coating ex-
hibited much stronger wear performance than the 316
stainless steel, even the wear rate reached even one-third
of that of steel, indicating the laser-cladded amorphous
coating can protect a steel substrate from wear friction.
Acknowledgment
This work was supported by Natural Science Founda-
tion of Hunan Province of China (Grant No.
2021JJ50025), Key Research and Development Program
of Hunan Province (2022GK2030), Natural Science Pro-
ject of Jiangsu Urban and Rural Construction V ocational
College (XJZK22009/206).
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