Surface & Coatings Technology 386 (2020) 125482

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Surface & Coatings Technology

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A new approach to sintering and boriding of steels “Boro-sintering”: T

Formation, microstructure and wear behaviors
⁎
Azmi Erdogana, , Bilal Kursuncub, Ali Günenc, Müge Kalkandelend, M. Sabri Gokb
a
Department of Metallurgy and Materials Engineering, Faculty of Engineering Architecture and Design, Bartın University, Bartın, Turkey
b
Department of Mechanical Engineering, Faculty of Engineering Architecture and Design, Bartın University, Bartın, Turkey
c
Department of Metallurgy and Materials Engineering, Faculty of Engineering and Natural Sciences, Iskenderun Technical University, Hatay, Turkey
d
Department of Metallurgy and Materials Engineering, Institute of Engineering and Sciences, Iskenderun Technical University, Hatay, Turkey

A R T I C LE I N FO A B S T R A C T

Keywords: In this study, sintering and boriding methods are applied as a single step, and it is aimed to gain time and
Sintering economic advantage. For this purpose, powder mixtures prepared in suitable compositions were subjected to
Boriding sintering and boro-sintering processes. In the boro-sintering process, the sintering was carried out in the boriding
Boro-sintering atmosphere and the two processes were carried out together. The processing, microstructure, hardness and dry
FeB
sliding wear behavior of the samples were studied. The powders were pressed under different pressures, and
Fe2B
Dry sliding wear
their effects on the properties of the final component were investigated. The sintering process was carried out for
AISI 1010 2 h at 1000 °C, and the boro-sintering process was carried out at 1000 °C for 2, 4 and 6 h. Fe2B and Fe2B + FeB
boride phases occurred depending on the boro-sintering process duration. Boride layer thickness varied between
120 and 400 μm according to boro-sintering duration and cold press pressure. Vickers micro-hardness and Ball-
on-disc wear tests were performed on the samples. Whereas 205–215 HV hardnesses were obtained in the
sintered samples, 1252–1705 HV hardness values were reached by boro-sintering process. Increased cold
pressing pressure reduced wear losses. However, the long boro-sintering time increased surface hardness, but
reduced wear resistance.

1. Introduction and wear resistance by changing the microstructure properties [8].

The powder metallurgy (P/M) method offers many advantages for
many types of materials in the manufacture of finished parts over other
manufacturing methods. Production with powder metallurgy eliminates
the need for many machining processes required for castings and forged
products, thus achieving the production of structural parts with higher
precision structural. For these reasons, it is both more cost-effective and
more environmentally friendly production method for materials. [1,2].
Important advantages of P/M include high dimensional accuracy, high
surface quality, repeatability, low cost and material savings due to the
absence of secondary processes [3–5]. This method does not require
melting to form complex components unlike conventional manu-
facturing methods, and high alloy components can be used due to the
rapid solidification of powder production [6]. P/M is one of the easiest
methods of producing metallic parts closest to the final shape. This
method is widely used in the production of structural materials and
many automobile parts [7]. The P/M production method allows the
formation of a good combination of mechanical properties, corrosion
However, the mechanical properties of the steels produced by this
method may be lower than those of other steels with the same com-
position due to the porosity found after production [9].
Boriding is a thermo-chemical surface treatment that allows the
production of a boride layer near the substrate surface without creating
an additional layer on the surface [10–12]. Boriding can be applied to a
wide range of steel alloys as well as materials such as cobalt-based al-
loys, nickel-based alloys, titanium and molybdenum to achieve the very
high hardness and wear resistance on their surfaces [13,14]. Borided
steel components have excellent performance in many industries due to
their superior tribological properties [15,16]. Parameters such as boron
potential of the medium, process temperature and duration, chemical
composition of the substrate control the phase structure of the formed
boron layer. Depending on these parameters, tetragonal Fe2B (8 wt% B)
and orthorombic FeB (16 wt% B) phases can be formed according to the
amount of boron diffused into iron alloys [17–19]. Generally, single-
phase Fe2B layer is preferred over double phase FeB+Fe2B layer for
parts operating at high loads [20,21].

⁎
Corresponding author.
E-mail address: aerdogan@bartin.edu.tr (A. Erdogan).

https://doi.org/10.1016/j.surfcoat.2020.125482
Received 8 January 2020; Received in revised form 13 February 2020; Accepted 17 February 2020
Available online 19 February 2020
0257-8972/ © 2020 Elsevier B.V. All rights reserved.
A. Erdogan, et al.
In a study, Yazici and Çavdar [22] compared 30MnB5, 28MnCrB5
steels with borided steel which was produced by powder metallurgy
and boriding process. They carried out the sintering process at 1120 °C
and boriding process at 950 °C. After boriding, they obtained 1400 HV
hardness in the sintered steel sample which contained 0.3% C and 2%
Cu. As a result of their abrasive wear tests, sintered and borided steel
yielded favorable results among other steels. In another study, Çavdar
et al. [1] sintered samples containing iron-based powders at 1120 °C for
30 min. The samples containing different amounts of copper and gra-
phite were borided after the sintering process. As a result of hardness
tests, they obtained hardness values between 950 and 1550 HV de-
pending on the varying graphite and copper ratio. Serafini et al. [8]
investigated the mechanical and microstructural properties of sintered
316 L steel by the addition of different boron amounts. After the sin-
tering process was carried out at 1240 °C for 30 min, microstructure,
hardness and micro abrasion properties of the samples were tested.
Thanks to the liquid phase formed during sintering, the parts produced
were found to have lower porosity and a higher density. They also
found that the hardness increased due to the phases such as M2B
(M = Metal) and M23(B1.5C4.5) and wear coefficient decreased. Franco
et al. [23] applied boro-niobizing heat treatments on P/M AISI M2, and
compared the properties and wear behavior of obtained coatings. They
obtained coatings composed of iron borides, niobium borides and nio-
bium carbides with higher hardness (3000 HV). The authors also in-
vestigated the wear behavior of coatings obtained on P/M AISI M2 steel
and reported that the highest wear resistance was obtained in iron
boride coatings. In addition to these studies, boriding of iron-based
materials produced by powder metallurgy [24,25] or adding boron
[26,27] directly to the composition has been tried in many other stu-
dies. Furthermore, it has been proven in many studies [28–30] that the
surface coatings by boriding process contribute to the mechanical
properties of many non-ferrous metals. However, in literature ex-
aminations, no studies have been found in which boriding process is
applied simultaneously with powder metallurgy production method
[23,31,32].
Sintering is an alternative production technique made by bringing
the powder particles together under or above the melting temperature.
Boriding is a crucial surface treatment to improve the mechanical and
oxidation properties of steels. In this study, as a new approach, si-
multaneous application of sintering and boriding process is aimed. By
applying the boriding process during sintering, it can be ensured that
the substrate material is free from problems such as grain growth and
loss of mechanical properties during subsequent boriding treatment.
Besides, it is possible to save costs due to the absence of additional
boriding treatment which is conducted at temperatures of 800 °C or
above. For this purpose, in this study, the effect of sintering and bor-
iding in a single process step on microstructure, phase formation,
hardness and wear behavior of AISI 1010 steel was investigated. In this
study, the term “boro-sintering” is used for boriding and sintering op-
erations which were conducted in one step.
2. Experimental
Inıtially, commercially available powders with Fe – 0.6Mn – 0.4Si –
0.1C chemical composition and 50–150 μm particle size were subjected
to mechanical alloying for 6 h to ensure homogeneous mixing powders.
Then, the powder blend was weighed and poured into the mold to
produce samples 40 mm in diameter and 5 mm in thickness by cold
pressing under varying pressure at 1500, 2000 and 2500 Psi. Finally,
the cold-pressed samples were boro-sintered 1000 °C for 2, 4 and 6 h in
the presence of EKabor 2 powder or sintered at 1000 °C for 2 h in the
pure Al2O3 powder medium.
After the sintering and boro-sintering process, metallographic
samples were prepared with a precision cutting device for SEM, EDS
and XRD analyzes. Then, the samples were subjected to conventional
grinding with 320, 400, … 1500 SiC paper and polishing steps with
2
Surface & Coatings Technology 386 (2020) 125482
1 μm Al2O3 solution and then etched with 2% Nital solution to reveal
microstructural details. Metallographic studies were conducted on the
polished and etched cross-sections of the samples using Thermo
Scientific Apreo S SEM equipped with Ultra Dry EDS Detector and
Quasor II EBSD equipped with EDS. The thicknesses of the boride layers
were determined by the SEM, and the presence of Fe-B phases formed
on the surface were verified by X-ray diffraction (XRD) analyses using a
computer-controlled RIGAKU Smart LabTM device, for which the op-
eration values were as follows; Cu Kα radiation λ = 0.154 nm; 2θ range
from 10° to 90°; step size Δ2θ = 0.006°; 121 integration time 280 s.
Microhardness measurements were conducted on a cross-section of
the boro-sintered samples by using the FM-700, Future-Tech hardness
tester with Vickers pyramid indenter along the cross-section using 100 g
load and 15-s dwell time by the ASTM- E384 standard. A Wave System
Hommelwerke T8000 2D profilometer was utilized to evaluate the
surface roughness (Ra) of the samples with at the speed of 1 mm/s and
the length of 6 mm.
Sliding friction and wear experiments were performed using a ball-
on-disk tribometer (TURQUOISE 2.0 Tribometer T10/20) under dry
conditions against 6 mm diameter WC (1917 HV hardness) ball. Wear
tests were performed at room temperature under 5, 10, 15 N loads with
a sliding speed of 5.5 cm/s along a circular path of 7.5 mm in radius for
a total of 200 m sliding distance. Three wear tests were conducted for
each sample. After the wear experiments, worn surfaces of each sample
were analyzed by using SEM (TESCAN MAIA3 XMU) equipped with
energy dispersive X-ray (EDS) spectrometer operating at an accelerating
voltage of 20 kV. Volume losses were calculated from the average of the
measurements which were taken from 10 different profiles of wear
tracks.
3. Results and discussion
3.1. Microstructure and formation behavior
SEM images taken from the cross-sectional surface of AISI 1010 steel
samples sintered for 2 h in Al2O3 medium at 1000 °C are given in Fig. 1.
The effects of pressing pressure on the microstructure were investigated
by applying 1500 (Fig. 1a), 2000 (Fig. 1b) and 2500 (Fig. 1c) Psi
pressures, while the powders were cold pressed. When the Fig. 1 is
examined, it is seen that after sintering, the bonding between the
powder particles is formed, the pores between the particles are de-
creased, and the grain boundaries are formed significantly due to the
neck formation. It is seen that the discontinuities in the microstructure
become more homogenous, and the porosity decreases due to the in-
creasing pressing pressure. It was concluded that the sintering tem-
perature of 1000 °C and 2 h could be sufficient to obtain the desired
metallographic appearance.
Since sintering for 2, 4 and 6 h at 1000 °C is sufficient to obtain the
desired metallographic appearance, it was decided to apply boro-sin-
tering at this temperature and durations. SEM microstructure taken
from the surface of the samples subjected to boro-sintering process at
1000 °C for 2 h is given in Fig. 2. When Fig. 2 is examined, a single-
phase Fe2B layer in the range of 100–120 μm can be observed on the
surface of boro-sintered samples. However, it is seen that a boride layer
containing Fe2B+FeB phases were formed (between 375 and 400 μm)
in the samples subjected to 6 h boro-sintering process (Figs. 3a–c and
6).
It was found that the boride layer obtained by P/M contained
compressed islets of oxide and yielded a higher hard or boride layer
thickness than the boride layers obtained on cast steels. This is attrib-
uted to the fact that, samples produced by powder metallurgy contain
some porosity in their internal structure, which makes easier diffusion-
based coating operations. On the other hand, although there was a
slight decrease in the thickness of the coating layers due to the in-
creasing pressing pressure, it was found that the oxide islets were also
decreased. This has resulted in the formation of a denser material by
A. Erdogan, et al.
Fig. 1. SEM microstructures of AISI 1010 steel which were taken from the cross-section surfaces after sintering for 2 h in Al2O3 medium at 1000 °C. Cold-pressed at a)
1500 Psi b) 2000 Psi c) 2500 Psi.
sintering of the powder particles, which were bonded better due to the
increased pressing pressure. Therefore, as a result of increasing pres-
sure, the amount of grain boundaries decreased and a result, reduced
diffusion of boron towards the interior of coating is thought to result in
a reduction of the coating layer and oxide islets (Fig. 2). Because dif-
fusion process occur more quickly in the grain boundaries than the
grain [33]. While this is stated in the form of some porosity in the
coatings in steels [10–13], it is expressed as the continuation of the
presence of graphite nodules in the coating layer in spherical graphite
cast irons [34,35].
In the EDS analyzes obtained from the coatings produced by boro-
sintering, it was determined that a single-phase (Fe2B) structure was
formed in 2 h boro-sintering process (Fig. 4) and a double phase (Fe2B
+FeB) structure was formed in 4 h boro-sintering process. In Fig. 4, it is
seen that “B” element was constant along with the coating layer, and
shows a sudden decrease after the coating layer. Fe content shows an
increase from the surface to the inner parts but shows sudden decre-
ments and increments in some regions. The opposite distribution of the
amount of oxygen in the specified areas confirms that these are oxide
islets trapped in the structure. This can be attributed to the penetration
of “O” into the P/M material at high temperatures during the boro-
sintering process since the cold-pressed powders are connected to each
other only by mechanical bonding (no chemical bonding) before the
boro-sintering process.
Fig. 5 shows that the Pt1 and Pt2 regions contain wt. 22.97% and
wt. 23.54% “B”. This amount is sufficient for the amount (wt. 16.23%)
required for FeB phase formation, which has been indicated in Fe-B
equilibrium diagram. B amount of Pt3 is below the amount required for
FeB formation, but this region has the amount of boron (wt. 8.93%)
required to form Fe2B. In Pt 4, the amount of oxide is more than 30%. It
is seen that the Pt5 and Pt6 regions taken from the bottom of the
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Surface & Coatings Technology 386 (2020) 125482
coating layer consist mainly of Fe.
XRD analysis of sintered and boro-sintered samples after cold
pressing under 2500 Psi pressure is given in Fig. 6. It was observed that
only α-Fe iron phase formed in the sintered sample in Al2O3 medium. α-
Fe phase was observed in all boro-sintered samples for 2, 4 and 6 h.
However, the peak intensity of this phase decreased with increasing
boriding time. This is due to the penetration of the X-ray beam to a
certain distance. Because the X-ray beam reached the Fe layer in the
substrate less due to the increased boride layer thickness, which was
formed on the surface. Fe2B and α-Fe phases were formed in boro-
sintered samples for 2 h. In addition to Fe2B and α-Fe phases, FeB phase
was formed in samples subjected to boro-sintered for 4 and 6 h. In
addition, the intensity of FeB phase increased with increasing proces-
sing time. Because, as mentioned in the steel-based materials produced
by casting, firstly the Fe2B phase is formed during the boriding process
due to the diffusion of the boron atom. Sufficient conditions are pro-
vided for the formation of FeB layer on the surface with increasing
boriding duration or temperature [36].
After the sintering process, surface roughness was measured on the
surface of the samples, and coating thickness and hardness were mea-
sured from the cross-sections (Table 1). In boro-sintered samples, the
thickness of the boride layer varied over a wide range of 105–420 μm
depending on the pressing and boriding parameters. The hardness va-
lues of the boride layer varied between 1252 and 1705 HV. Thanks to
boro-sintering process, the hardness values of P/M AISI 1010 samples
(120 ± 20 HV) were 12.5–17 times higher than the sintered samples
(Fig. 7). However, when the boride layer hardness values were com-
pared with the boride layer hardness values obtained on the low carbon
steels (FeB 1900–2100 HV, Fe2B 1650–1900 HV) [37–39], it was seen
that the hardness values were lower. This is related to the porosity and
oxide content of materials, which are characteristic properties of the P/
A. Erdogan, et al. Surface & Coatings Technology 386 (2020) 125482

Fig. 3. SEM microstructures of AISI 1010 steel which were taken from the
cross-section surfaces after sintering for 6 h in B4C medium at 1000 °C. Cold
pressed at a)1500 Psi b)2000 Psi c)2500 Psi.

Fig. 2. SEM microstructures of AISI 1010 steel which were taken from the 3.2. Dry sliding wear behavior
cross-section surfaces after sintering for 2 h in B4C medium at 1000 °C. Cold
pressed at a)1500 Psi b)2000 Psi c)2500 Psi. When the wear loss graph (Fig. 8) is examined, it is seen that wear
losses increase in all samples with the increase of the load. The hardness
of the materials may also be defined as the extent of exhibiting re-
M materials and are clearly visible in the SEM and EDS figures. This
sistance to objects that want to sink to the surface. High hardness re-
may be due to the fact that the tip coincides with the oxide during
duces the plastic deformability of the material. Therefore, the increase
hardness testing of the boride layer. Because, due to the trapped oxide
in the load means more penetration into the opposite surface. Thus, the
layers in the boride layer (Fig. 2), sufficient resistance against the tip
abrasive ball penetrates more against the opposite surface and cuts the
may not be established. As can be seen from the standard deviations of
layer formed in front of it, causing material loss. However, the fact that
the obtained hardness values (Table 1), there are differences in dis-
volume losses do not increase linearly with increasing load can be ex-
persion values between the especially low pressure applied (high oxide
plained as follows: First of all, the more immersion of the ball on the
content) samples. On the other hand, the increase in the applied pres-
opposite surface and the increased contact area between the interactive
sure increased the densities [40]. With the increase of boro-sintering
surfaces play a role in the non-linearity of wear losses. Furthermore, the
time, a slight increase occurred in the surface roughness values.

4
A. Erdogan, et al.
Fig. 4. EDS line analysis is taken from the cross-sectional surface of the sample, which was cold pressed by applying 1500 Psi pressure and then subjected to boro-
sintering for 2 h in B4C medium at 1000 °C.
faster and more stable formation of oxide films formed on the surface
with increasing load also explains the nonlinear increase. Wear debris
which was separated from the surface by the movement of mutual
surfaces can be embedded into the surface compactly under the effect of
the load [41,42]. This may play an artificial role in changing the wear
resistance of the material.
The processes that the powders undergo before sintering can affect
the final properties. Bolokang et al. [43]. studied the effect of me-
chanical milling and cold pressing on Co powders. They have found that
mechanical milling and cold pressing process caused changes in
thermal properties, phase formations and lattice parameters of the
phases. The volume losses of the sintered samples decreased with in-
creasing cold pressing pressure. The same condition was also observed
in boro-sintered samples. The deformation of the powder particles oc-
curs with the application of pressing, and the particles are inter-
connected by weak mechanical bonds. Increased cold pressing pressure
increases the density of both green and sintered samples. The increase
in compression pressure leads to an increase in the particle contact area
where high densification can be achieved. Increasing the compression
pressure affects the work hardening of the green compact. In addition,
as the compression pressure increases, the increased density due to the
decrease in the pores causes an increase in hardness [40]. When the
volume losses of the sintered and boro-sintered samples were examined,
the increased pressing pressure reduced wear losses due to the men-
tioned reasons.
Although the hardness of the samples increases with increasing
boro-sintering time, it is seen that the volume losses increase. Increase
in the hardness of the test piece generally contributes to the wear re-
sistance and reduces wear losses [15,44,45]. However, apart from the
hardness, material properties such as fracture toughness must also be
considered. It has been shown in many studies that FeB phase is harder
than Fe2B phase but has lower fracture toughness. [20,29]. It is known
that the Fe2B phase is more desirable, especially when the material is
subjected to a high load [17,46]. From this perspective, it can be un-
derstood that the wear losses increase despite the increased hardness
with increasing boro-sintering time. For samples produced by powder
metallurgy, the brittle FeB phase may be more easily separated from the
5
Surface & Coatings Technology 386 (2020) 125482
surface during the friction process. Generally, saw-tooth shaped single
phase (Fe2B) layer formation is preferred over a layer with both FeB and
Fe2B. Fe2B boride layer adheres to the substrate material more strongly
because of saw-tooth morphology. Brittleness of the boronised layer
increases with layer thickness. Also, since the FeB and Fe2B phases have
different thermal expansion constants (TEC; FeB – 23 × 10−6 °C−1,
Fe2B – 7.85 × 10−6 °C−1), crack formations are frequently found on
the FeB/Fe2B phase interfaces in two phase layers. These cracks fre-
quently cause spalling and scaling under a mechanical load and this
cause a low wear resistant [47,48]. In addition, the surface roughness of
samples increased with increasing boro-sintering time (Table 1). Dif-
ferent surface roughness values affect the wear results. Especially at the
beginning of the test, only the asperities are in contact, and the material
is removed relatively easily [49,50]. After these asperities are removed,
wear can progress steadily. Increased surface roughness values with
increasing boro-sintering time are also likely to play a role in increasing
wear loss.
In the tests carried out under 5 and 15 N load, friction coefficient
graphs of cold-pressed samples at 2000 Psi are given in Fig. 9. No
correlation was found between friction coefficients and wear losses. The
highest friction coefficient was observed in the boro-sintered sample for
2 h. Especially at the beginning of the test, there was a rapid increase in
the friction coefficient. This increase is due to the removal of asperities
between the interactive surfaces. The rate of growth in the friction
coefficient slowed down by removal of the surface asperities and in-
crease in the contact area between the abrasive ball-the counter surface.
The fluctuations that occur after this point are due to the formation and
breakage of the oxide layers. The lowest friction coefficient was seen in
the sintered sample. SEM wear track (Fig. 10a) also show that the ball
was in low contact with the opposite surface due to a large number of
spill areas. The low contact area between the ball and the opposite
surface caused the friction coefficient to remain low in this sample. The
friction coefficient values of the boro-sintered samples for 4 and 6 h
were between samples which were sintered and boro-sintered for 2 h.
When the wear marks (Fig. 11) are considered, it is seen that the sur-
faces of these samples have fewer asperities to prevent movement of the
ball. When the wear marks are examined, it is seen that the surfaces of
A. Erdogan, et al. Surface & Coatings Technology 386 (2020) 125482

Fig. 5. EDS analysis of the sample, which was cold-pressed by applying 2000 Psi pressure and then subjected to boro-sintering for 4 h in B4C medium at 1000 °C.

6
A. Erdogan, et al. Surface & Coatings Technology 386 (2020) 125482

Fig. 6. XRD analysis of the samples which were cold-pressed by applying 2500 Psi pressure and then subjected to sintering and boro-sintering at 1000 °C. a) Sintered
at Al2O3 medium for 2 h. b) Sintered at B4C medium for 2 h c) Sintered at B4C medium for 4 h d) Sintered at B4C medium for 6 h.

Table 1
The thickness, surface hardness, roughness and density of the P/M specimens subjected to sintering and boro-sintering heat treatment.
Sample Heat treatment Treatment Pressure Treatment Coating thickness Max. surface hardness Surface roughness Density (g/cm3)
temperature (°C) (PSi) duration (h) (μm) (HV0.1) (Ra, μm) (Relative porosity %)

S1 Sintering 1000 1500 2 – 105 ± 20 3.10 5.90 (25)

S2 (Al2O3) 2000 2 – 110 ± 20 2.95 6.01 (24)
S3 2500 2 – 115 ± 15 2.90 6.20 (21)
S4 Boro-sintering 1000 1500 2 120 ± 15 1252 ± 175 4.58 5.60 (29)
S5 (B4C) 1500 4 360 ± 20 1390 ± 130 5.70 5.66 (28)
S6 1500 6 420 ± 20 1505 ± 130 5.94 5.75 (27)
S7 Boro-sintering 1000 2000 2 110 ± 15 1350 ± 155 3.96 5.63 (28)
S8 (B4C) 2000 4 348 ± 18 1590 ± 120 5.45 5.72 (27)
S9 2000 6 405 ± 20 1685 ± 125 5.78 5.80 (26)
S10 Boro-sintering 1000 2500 2 105 ± 15 1358 ± 145 3.80 5.65 (28)
S11 (B4C) 2500 4 340 ± 18 1627 ± 130 5.35 5.80 (26)
S12 2500 6 400 ± 17 1705 ± 130 5.50 5.92 (24)

Fig. 7. The variation in hardness from the surface to the interior of sintered and boro-sintered samples.

7
A. Erdogan, et al. Surface & Coatings Technology 386 (2020) 125482

Fig. 8. Volume losses of sintered and boro-sintered samples as a function of the sliding load.

Fig. 9. Friction coefficient curves of cold pressed samples at 2000 Psi pressure. a)5 N, b)15 N.

Fig. 10. Wear tracks of samples which were tested under 10 N load. a) Sintered for 2 h, b) Boro-sintered for 4 h.

8
A. Erdogan, et al.
Fig. 11. SEM micrographs of the worn surfaces of sintered and boro-sintered samples. a) Sintered for 2 h, b) Boro-sintered for 2 h, c) Boro-sintered for 4 h, d) Boro-
sintered for 6 h.
these samples have fewer asperities to prevent movement of the ball.
For this reason, it can be understood that the friction coefficient is
lower than the sample boro-sintered for 2 h. The increase in the applied
load had no significant effect on the friction coefficients. However, the
rise in load reduced the fluctuations in the coefficient of friction to a
lesser degree. This can be related to the fact that the sample becomes
more compact under high load and the oxide layer on the surface forms
more quickly.
Fig. 10 shows the wear tracks of the sintered and boro-sintered
samples. On the surface of the sintered sample (Fig. 10a), black areas
that can be expressed as oxides and white areas due to spills caused by
friction are seen. Fig. 10b shows that the boro-sintered sample is much
smoother, and almost the entire surface is covered with oxide.
Fig. 11 shows the wear scar morphology of the samples subjected to
wear test under 10 N load. The wear pattern of the sintered sample
showed wear due to fractured junctions (Fig. 11a). The microstructure
of the sample shows the structure formed by pressing and sintering of
approximately 50–150 μm grains. When a load is applied to the sample
during the wear test, ruptures occur at the weakest part of the sample.
Therefore, fractured areas occur in regions where the powders bond
with each other. Fig. 11b shows the wear track of the boro-sintered
sample for 2 h. A smoother surface is seen when compared to the sin-
tered sample. There are flaking areas with micro-scratches on the sur-
face. It can be said that micro-scratches were formed by wear particles
separated from the surface. The reason for the less damage of the
sample compared to the sintered sample can be attributed to the pro-
tection of the sample surface with the Fe2B layer. Furthermore, it is seen
in Fig. 2 that boro-sintering forms a denser layer on the surface. This
caused less damage to this sample and a change in the wear mechanism.
When the wear tracks of the boro-sintered samples for 4 (Fig. 11c) and
6 h (Fig. 11d) are examined, similar wear mechanisms are seen. The
surfaces of these samples are much smoother than other samples.
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Surface & Coatings Technology 386 (2020) 125482
Flaking areas and high oxidized regions are seen as the wear me-
chanism. These flaking areas were formed because of the higher FeB
phase on the surface of these samples, which causing brittleness.
Fig. 12 shows the EDS analysis taken from the wear track of the 4 h
boro-sintered sample. A dense oxide layer is observed on the surfaces of
4 and 6 h boro-sintered samples. The lower friction coefficient in these
samples can be attributed to this dense oxide layer. When two surfaces
move on top of each other, most of the work done by friction turns into
heat. This leads to local temperature peaks on the surface and an overall
increase in temperature. This increase in surface temperature may
cause oxidation or possible melting, which may alter the mechanical
and metallurgical properties of the sliding surfaces [51]. It is well
known that the oxide layer formed during sliding can be buried to the
deformed surface and affect its friction and wear properties [52]. These
oxide layers formed during sliding are called tribo-oxides. It is believed
that the amount of oxides determines the function of the tribo-oxides,
ie, whether they affect the wear behavior and mechanism of the alloys.
In addition, the properties of tribo-oxides such as continuity, com-
pactness and thickness have an undeniable effect on wear behavior and
wear resistance [41]. If an oxide layer prevents metal-to-metal contact,
a reduction in friction and wear can be expected.
4. Conclusion
Sintering and boriding operations were successfully performed in
one step. The powders were pressed under different pressures, and their
effects on the properties of the final component were investigated. The
sintering process was carried out for 2 h at 1000 °C, and the boro-sin-
tering process was carried out at 1000 °C for 2, 4 and 6 h. In addition,
dry sliding tests were carried out under different loads to determine the
wear resistance of the samples. Formation, microstructure and hardness
properties of sintered and boro-sintered samples were investigated. The
A. Erdogan, et al.
Fig. 12. EDS line analysis of wear track of 4 h boro-sintered sample.
results obtained are summarized below;
• Increased cold pressing pressure increased the density and hardness
of all samples. In addition, increased cold press pressure caused a
slight decrease in coating thickness of the samples.
• In boro-sintered samples for 2 h, a single phase (Fe2B) in the range
of 100–120 μm, and in the samples boro-sintered for 4, 6 h, a
double-phase (Fe2B+FeB) phase in the 340–420 μm range was ob-
served.
• In sintered samples 205–215 HV hardness values and in boro-sin-
tered samples 1252–1705 HV hardness values were obtained.
Increased boro-sintering time resulted in increased hardness due to
the FeB phase formation.
• Wear resistance of cold pressed samples at high pressure was higher.
The wear resistance of boro-sintered samples was better than that of
sintered samples. The increase in load applied in the wear tests
10
Surface & Coatings Technology 386 (2020) 125482
increased the wear losses.
• Increased boro-sintering duration increased hardness but decreased
wear resistance. This was attributed to the FeB layer which was
formed in long duration boro-sintering process.
CRediT authorship contribution statement
Azmi Erdogan: Conceptualization, Methodology, Software,
Writing - review & editing, Writing - original draft. Bilal Kursuncu:
Data curation, Writing - original draft, Software. Ali Günen: Writing
- original draft, Visualization, Investigation, Writing - review &
editing, Supervision. Müge Kalkandelen: Writing - original draft,
Conceptualization, Software, Validation. M. Sabri Gok: Writing -
original draft, Validation, Supervision.
A. Erdogan, et al.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgement
This work was supported by Scientific Research Funds of Bartın
University (Project Number: 2018-FEN-A-023).
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