Corrosion Engineering, Science and Technology

The International Journal of Corrosion Processes and Corrosion Control

ISSN: 1478-422X (Print) 1743-2782 (Online) Journal homepage: https://www.tandfonline.com/loi/ycst20

High-temperature oxidation resistance of Ni–P and

Ni–B electroless coatings on mild steel after long-
term tests

Juan G. Castaño, Sandra Arias & Oscar Galvis

To cite this article: Juan G. Castaño, Sandra Arias & Oscar Galvis (2019): High-temperature
oxidation resistance of Ni–P and Ni–B electroless coatings on mild steel after long-term tests,
Corrosion Engineering, Science and Technology, DOI: 10.1080/1478422X.2019.1684020

To link to this article: https://doi.org/10.1080/1478422X.2019.1684020

Published online: 30 Oct 2019.

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CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY
https://doi.org/10.1080/1478422X.2019.1684020

RESEARCH ARTICLE

High-temperature oxidation resistance of Ni–P and Ni–B electroless coatings on

mild steel after long-term tests
Juan G. Castaño , Sandra Arias and Oscar Galvis
Centro de Investigación, Innovación y Desarrollo de Materiales –CIDEMAT-, Medellín, Colombia

ABSTRACT ARTICLE HISTORY

The oxidation resistance of Ni–P and Ni–B electroless coatings applied on mild steel has been Received 31 May 2019
determined by means of isothermal oxidation tests at 600°C for up to 400 h for uncoated and Accepted 19 October 2019
coated samples. The oxidation rate is evaluated by means of gravimetric analysis. SEM, EDS, XRD
KEYWORDS
and Raman Spectroscopy characterisation allows establishing the morphological and chemical Electroless coatings; mild
features of the coatings and the oxidation products, as well as their relationship with the oxidation steel; isothermal oxidation;
resistance at high temperature. Coated samples show higher oxidation resistance than un-coated Ni–B; Ni–P
samples, being better the behavior of Ni–P coatings. The protective behaviour of electroless
coatings is associated with factors such as the formation of a Ni–Fe interdiffusion layer, the
incorporation of NiO into the oxide layer and the formation of crystalline phases of Ni3P.

Introduction [12] performed oxidation tests of Ni–P and Ni–B coatings

on mild steel, found that, after 10 h, the oxidation in Ni–B
Despite being one of the most used engineering materials in
coatings at 600°C and 700°C was lower than in Ni–P coatings.
industry, mild steels have low oxidation resistance at high
An interdiffusion inner layer consisting of Ni and Fe was
temperatures and their utilisation is restricted at these con-
observed with different researchers in both coatings [12,13].
ditions [1]. Nevertheless, since this material has a lower
In Ni–P coatings, phosphorus is not present in this layer,
cost if compared with other materials used in different corros-
and according to Lin and Lai [13], who performed studies
ive environments [2], a great variety of surface treatments for
at temperatures between 400 and 900°C and times between
improving its oxidation resistance have been developed.
1 and 50 h, this interdiffusion mainly takes place through
Among the alternatives for using mild steels in high-temp-
grain boundaries below 690°C and through the lattice at
erature applications, electroless coatings are considered due
higher temperatures.
to their properties [3,4]. Ni–P electroless coatings, deposited
Tan et al [1] studied the oxidation of Ni–P–ZrO2 coatings
from sodium hypophosphite baths, are dense, with low por-
at 650°C between 1 and 6 h, and Farrokhzad [14] investigated
osity and high thickness uniformity, exhibiting high micro-
behaviour of Ni–P–BN coatings at 500, 600 and 700°C for up
hardness and excellent corrosion resistance [5,6]. on the
to 96 h. In both cases, the composite coatings applied on low
other hand, Ni–B electroless coatings, deposited from sodium
carbon steels exhibited higher oxidation resistance than Ni–P
borohydrides, also have low porosity and high uniformity
coatings.
[5,7] and, if compared with Ni–P coatings, Ni–B coatings
In all the oxidation tests found in the literature for Ni–P
possess enhanced microhardness and wear resistance, as
and Ni–B coatings, exposure times are no longer than
well as lower friction coefficients [8].
100 h. There is no available information about the behaviour
Currently, most corrosion studies are focused on improv-
of electroless coatings on carbon steel in oxidation tests at
ing the corrosion resistance of electroless Ni coatings on steels
long exposure periods, despite this kind of studies are useful
at room or low temperatures [9,10]. However, there are few
for establishing the durability of these coating in high-temp-
studies available about the oxidation resistance at high temp-
erature conditions. For this reason, a comparative analysis of
erature. High-temperature behaviour of Ni–P coatings
the oxidation resistance at high temperature of electroless Ni–
applied on carbon steels was studied at temperatures between
P and Ni–B coatings on mild steel, as well as un-coated steel,
120°C and 1000°C [1,11–15]. To date, to the best of the
was done. Isothermal oxidation tests were performed at 600°
knowledge of the present authors, only two works had been
C and up to 400 h, with a gravimetric evaluation at different
published about the high-temperature behaviour of Ni–B
exposure times. The characterisation of the coatings and the
coatings applied on carbon steels [11,12].
oxidation products were performed by X-Ray Diffraction,
In an early work about oxidation of Ni–P and Ni–B coat-
Scanning Electron Microscopy, Energy Dispersive X-Ray
ings on mild steels, Tomlinson and Wilson [11] conducted
Spectroscopy and Raman Spectroscopy.
tests between 800°C and 1000°C during 440 min (7 h
approx.). They found that Ni–P coating had the highest oxi-
dation rate, following both coatings the parabolic oxidation
Experimental procedure
law. The authors claimed that the higher oxidation rate of
Ni–P coatings was due to their relatively lower amount of AISI 1008 mild steel bars (0.086% C, 0.084% Ni, 0.041% Si,
nickel if compared with Ni–B coatings. Eraslan and Ürgen 0.152% Cu (wt-%)) were employed as substrate material.

CONTACT Juan G. Castaño juan.castano@udea.edu.co Centro de Investigación, Innovación y Desarrollo de Materiales –CIDEMAT-, Universidad de Antioquia
UdeA, Carrera 53 # 61–30, Medellín, Colombia
© 2019 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
2 J. G. CASTAÑO ET AL.
The samples were cut with dimensions of 10 mm in diameter
and 0.4 mm in thickness. Before the coating deposition, the
samples were mechanically grounded with 80-grit SiC paper
and grit-blasted at 60 psi with SiC (177–210 µm) in order
to improve the adhesion of the coatings. Subsequently, they
were degreased in ultrasonic bath with ethanol for 10 min
and deoxidised for 10 min in a solution containing HCl and
hexamethylenetetramine. Finally, the samples were rinsed
with distilled water and dried in hot air steam.
The prepared samples were transferred into the corre-
sponding Ni–P or Ni–B electroless-plating bath. The chemi-
cal composition and operating conditions of the baths are
given in Table 1. The plating solutions were carried out in
polypropylene (Ni–P) and glass (Ni–B) beakers, with two
steel samples in a content of 80 cm3 of each solution. To guar-
antee a homogeneous deposition, the steel samples were held
with a steel wire to immerse them into the electroless sol-
ution. After the deposition process (two hours in both
cases), the coated samples were washed with neutral soap
and dried with hot air. Before and after the electroless process,
the samples were weighed in a Mettler Toledo UMX5 micro-
balance, with a precision of 0.1 µg, for the determination of
weight gain during the coating process.
Ni–P and Ni–B coated samples, as well as un-coated steel
samples, were submitted to isothermal oxidation tests at
different times. The samples were heated in air at a rate of
5°C min−1 up to 600°C. Then, they were kept at this tempera-
ture during 25, 75, 150, 250 and 400 h. Finally, the cooling of
the samples was carried out inside the furnace to room temp-
erature. At each time, three samples of each condition were
withdrawn from the furnace. The samples plus their spalled
scales were weighed again. Based on weight gains obtained
in the three samples of each condition removed in each
time, the oxidation-rate constants (k) were obtained for the
substrate and the coated specimens. Statistical analysis
using the method of least squares was used for calculating
k. The standard deviations, the P-values and the 95% confi-
dence intervals with lower and upper limits were calculated
for the fitted curves.
Characterisation of un-coated and coated samples was
performed before oxidation tests and after 400-hour oxi-
dation tests. A JEOL JSM 6490-LV scanning electron micro-
scope, coupled with an Oxford Inca PentaFET x-3 electron
microprobe, was used to assess the morphology, elemental
composition and thickness of the coatings before and after
the oxidation tests, as well as the characteristic of the oxi-
dation layers. On the other hand, the coatings and oxidation
layers were analysed by means of X-ray diffraction (XRD) in a
X’Pert PANalytical Empirean Series II diffractometer, model
Table 1. Chemical composition and operating conditions of Ni–B and Ni–P
electroless baths.
Ni–B Ni–P
Chemical composition
NiCl2·6H2O 20 g/L NiSO4·6H2O
NaBH4 8 g/L NaH2PO2·H2O
CH4N2S 1 mg/L C3H6O3
C2H8N2 35 ml/L C3H6O2
NaOH 110 g/L C4H6O4
NH4HF2 5 g/L NH4HF2
Operating conditions
pH >12 pH
Temperature 80°C Temperature
Plating time 2h Plating time
2012, with a PIXcel 3D detector and Cu Kα anode radiation
(0.1541874 nm). The data were collected in the 2⍰ range
from 10° to 100°, at a scanning rate of 0.03° min−1.
After oxidation tests, Micro-Raman spectroscopy analysis
of the oxidation layers was performed in a Horiba-Jobin
Yvon, model Labram HR, high-resolution spectrometer,
equipped with a confocal microscope Nikon BX41, through
a 50X objective, with a laser of He/Ne (632.5 nm). Raman
spectra were registered with pinhole of 1000 µm, slit of
200 µm and scanning range from 100 to 2000 cm−1.
Results and discussion
Characterisation of coatings before oxidation tests
In Figure 1, XRD spectra of Ni–P and Ni–B coatings are
shown. Both spectra show a low and broad peak centred at
45°, corresponding to Ni (111). These peaks are attributed
to either a nanocrystalline [16] or an amorphous [17] phase
in the coatings. In the Ni–B spectrum, two sharp peaks associ-
ated with steel substrate are also evidenced.
SEM plain images of Ni–P and Ni–B coatings (Figure 2(a))
show hemispherical growth features of nodular structure
typical for electroless deposited coatings. Cross-sections of
the coatings are shown in Figure 2(b). The measured average
thickness was 18 ± 2.5 μm for Ni–P coatings and 16 ± 4.2 μm
for Ni–B coatings. EDS analyses performed in cross-sections
of Ni–P coating indicated an average P content of 9.95 wt-%.
On the other hand, boron content in the Ni–B coatings
obtained was assessed elsewhere between 1 and 4.5 wt-% by
means of DSC [18].
Gravimetric analyses after oxidation tests
In Figure 3, the growth rate of the oxide layers, expressed as
weight gain per area unit (mg cm−2) and obtained at different
hours, are showed for un-coated and coated steels. In general,
electroless coatings exhibited better performance at high
temperatures than mild steel substrate, especially Ni–P coat-
ings. The weight gain per area unit of Ni–P coatings after
400 h was 1.2 mg cm−2, while in Ni–B coatings was
8.5 mg cm−2 and bare steel reached approximately
56 mg cm−2. For Ni–B coatings, the weight gain after 400 h
was approximately seven times higher than that obtained in
Ni–P coatings. On the other hand, the weight gain in the
21.2 g/L
24.2 g/L
26.5 ml/L
2.2 ml/L
12 g/L
13.3 g/L
4.65
90°C
2h
Figure 1. XRD spectra of Ni–P and Ni–B coatings applied on mild steel.

Figure 2. Plain (a) and cross-section (b) views of Ni–P and Ni–B coatings.
substrate after 400 h was approximately 6.5 times higher than
in Ni–B coatings.
Tan et al. [1] found slightly higher values for the weight
gain of Ni–P coatings for similar temperatures but low oxi-
dation time. At 650°C and 6.5 h, they reported a weight
gain of 2.841 mg m−2. The comparison of this value with
our results could be associated with the protective nature of
Ni–P coatings even at long times. To date, there is no pub-
lished data on weight gain for Ni–B coatings at 600°C or
nearby temperatures.
The oxidation rate constants (k) calculated from weight
gains for the substrate and the different coatings are included
in Table 2. Data were fitted using the Statgraphics Centurion ®
program, based on the parabolic behaviour of the oxidation
curves [9,12,19].
The results for k from Table 2 indicate that the magnitude
of the oxidation rate constant decreases significantly in coated
specimens. In comparison with the substrate, k values in Ni–
B coatings are lower in two orders of magnitude. On the other
Figure 3. Weight gain of un-coated and coated (Ni–P and Ni–B) mild steels in
oxidation tests from 0 h to 400 h at 600°C.
CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 3
hand, the lowest value of k is found in Ni–P coatings, being
three orders of magnitude lower than that obtained for the
substrate and one order of magnitude lower than in Ni–B
coatings. The reduction in the magnitude of k indicates that
electroless coatings improve the oxidation resistance at 600°
C, being much better the protection provided to the steel by
the Ni–P coating.
Only Tan et al. [1] reported a k value of 0.1508 mg2 cm−4 h,
calculated at 650°C and up to 6.5 h. This value is similar to
that found in our research and could be associated with little
changes over time in the protective nature of Ni–P coatings at
600°C or nearby temperatures. This comparison was not
possible for Ni–B due to the lack of published data.
Characterisation after oxidation tests
Figure 4 shows SEM plain views of the surface of the different
coatings and the substrate, after oxidation tests at 600°C and
400 h, at different magnifications. On the other hand, oxide
layers were characterised by XRD (Figure 5) and Raman
Spectroscopy (Figure 6).
On the substrate, crystalline oxidation products with glob-
ular forms and whiskers randomly oriented are observed
(Figure 4). These structures are associated with haematite
(α-Fe2O3) [20,21]. XRD and Raman analyses confirm that
haematite is the main oxidation product formed in the un-
coated steel (Figure 5(a) and Figure 6(a)). Magnetite
(Fe3O4) or maghemite (γ-Fe2O3) is also detected (Figure 5(a)).
In XRD and Raman analyses, the differentiation between mag-
netite and maghemite is not possible. However, a scale made of
Table 2. Calculated oxidation rate constant (k) for un-coated and coated steels
at 600°C.
Fitting result P-value for slope R2 k (mg2/cm4 h)
Substrate 7.2336t 0.0000 0.9727 7.2336
Ni–B 0.1433t 0.0000 0.9600 0.1433
Ni–P 0.0039t 0.0025 0.9189 0.0039
4 J. G. CASTAÑO ET AL.

Figure 4. Scanning electron micrographs of steel substrate, Ni–P and Ni–B coatings. The images in column (b) are enlargements of those in column (a).

an inner magnetite layer and an outer haematite layer is usually zone, with a thickness between 10 and 15 µm, is observed
reported in steels oxidised at high temperatures [20]. in an inner region between the coating and the substrate.
On the surface of the Ni–P coatings, which exhibited the
best behaviour in the oxidation tests, the cauliflower mor-
phology is still distinguishable, covered with very fine crystals
(Figure 4). XRD analysis (Figure 5(b)) allows the identifi-
cation of magnetite/maghemite, NiO and Ni3P. Raman analy-
sis (Figure 6(b)) confirms the presence of magnetite/
maghemite and NiO.
The surface of Ni–B coatings is completely covered with
oxidation products with similar appearance to those found
in the substrate, although the size of haematite globular struc-
tures is higher (Figure 4). The degree of surface oxidation is
consistent with the results found in the gravimetric tests.
XRD and Raman analyses allow the identification of haematite
and magnetite/maghemite (Figure 5(c) and Figure 6(c)), as
well as some NiO. Nevertheless, there is no evidence about
nickel borides or other boron compound in the oxide layer.
Figure 7 shows cross-section views of the coatings after
oxidation tests at 600°C and 400 h, as well as EDS linear
profile graphs. There is an important difference in the thick-
ness of the oxide scale between the two coatings. For Ni–P
coating, the thickness of the oxide scale was around 4 μm,
while for Ni–B coating was around 28 μm (7 times higher).
In Ni–P coating, EDS linear profile analysis (Figure 7(b))
evidenced the incorporation of Fe, Ni, P and O into the
oxide scale. The relative content of Fe in the outer zone of Figure 5. XRD spectra of un-coated and coated (Ni–P and Ni–B) mild steels after
the coating is low, although a Ni and Fe interdiffusion oxidation tests: (a) un-coated steel, (b) Ni–P, (c) Ni–B.

Figure 6. Raman spectra of un-coated and coated (Ni–P and Ni–B) mild steels
after oxidation tests: (a) un-coated steel, (b) Ni–P, (c) Ni–B.
Tomlinson and Wilson [11] found that oxidation of Ni–P
coatings starts above 400°C. They observed a thin film of NiO
at 600°C after 7.3 h. NiO is the first corrosion product formed
on electroless Ni coatings at high temperatures [15, 19]. The
formation of NiO is slow and depends on the outward diffu-
sion of Ni cations and the inward diffusion of oxygen ions via
doubly charged cationic vacancies, being the diffusion rate of
oxygen smaller by several orders of magnitude [14]. NiO acts
as a passivation layer and hence improves the oxidation
resistance of the Ni–P coating [22].
At the first stages of the oxidation process, the Ni–P coat-
ing prevents the rapid upward migration of Fe cations from
the substrate by lowering their rate of diffusion; however,
due to its progressive diffusion through the coating, iron is
incorporated into the oxide structure and substitutes nickel.
As consequence, the corrosion products are progressively
converted into iron oxides [12, 15]. However, NiO is still
detected in the oxide layer in oxidation tests up to 96 h
[14]. In our study, NiO remained in the oxide layer and hae-
matite was not detected after 400 h, which could be associated
with the low oxidation of the steel coated with Ni–P coating at
600°C.
The exposure at 600°C allowed the crystallisation of
nickel and the precipitation of fine particles of Ni3P phase,
as reported by other authors [5, 23]. According to Tan
et al. [1], Ni3P prevents the inward oxygen diffusion and
enhances the oxidation resistance of the coatings. The
amount of P into the coating was almost constant and
there was no evidence about the formation of phosphorus
oxides (i.e. P2O5) into the oxide layer. The migration of
phosphorus to the surface and its subsequent oxidation
occurs at temperatures higher than 600°C, while the
decomposition of Ni3P and the subsequent evaporation of
phosphorus occurs only at temperatures above 800°C [11].
The above explains the presence of phosphorus in the
coating after the oxidation tests.
CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 5
Ni–Fe interdiffusion layer formed at the coating-substrate
interface (Figure 7(a)) has been reported by different authors
at 600°C [11,12,15]. These authors also reported the lack of P
in this layer, which was corroborated in EDS profile analy-
sis performed after oxidation at 600°C during 400 h. Weiss
[15] claims that this layer is the most influential factor in
the protection against oxidation of Ni–P coatings, because
it acts as a diffusion barrier for diffusion of iron to the sur-
face. According to Lin and Lai [13], interdiffusion between
steel substrate and Ni–P coating mainly takes place through
grain boundaries below 690°C and through the lattice at
higher temperatures. The low amount of iron observed in
the Ni–P coating could be associated with the diffusion of
iron through the grain boundaries. On the other hand,
Kirkendall voids are observed in the interdiffusion layer,
due to the difference in the diffusion rates between Fe
and Ni [24].
Therefore, there is four influential factors in the protection
of Ni–P coatings over mild steel: the barrier effect of the
coating itself, the passivation associated with the formation
of NiO, the decrease in the inward oxygen diffusion due
to the formation of Ni3P and the decrease in the outward
iron diffusion associated with the formation of the interdiffu-
sion layer.
In the Ni–B coating (Figure 7(c)), the innermost part of
the oxide scale is mixed with the coating. EDS linear profile
analysis (Figure 7(d)) evidenced the presence of Fe and O
in the scale, associated with iron oxides detected by XRD
and Raman (Figure 5(c) and Figure 6(c)). B and Ni were
not detected in the oxide layer, despite NiO was identified
by XRD and Raman analyses.
In a previous study [12], based on Glow Discharge Optical
Emission Spectroscopy and XRD analyses, neither boron nor
nickel borides were observed in the top of Ni–B coatings after
10-hour oxidation at 600°C, due to the loss of boron from the
structure by its evaporation. Boron atoms diffusing and react
with oxygen in the surface of the coating to form boron
oxides, and these oxides start to evaporate at 450°C. Arslam-
bekov et al. [25] reported that the diffusion mobility of boron
atoms is many times higher than the diffusion of nickel
atoms, at high temperatures. It is possible that the lack of
boron compounds in Ni–B coatings after oxidation at 600°
C is due to diffusion and oxidation of boron and boron crys-
talline phases at initial stages, and the complete evaporation
of these boron oxides after long-term oxidation.
The relative content of Fe in the coating was significant
(Figure 7(d)), indicating that iron was diffusing through the
coating to oxidise in the outermost zone. On the other
hand, the relative content of Ni was higher in the outside of
the coating, which would indicate the diffusion of Ni towards
this zone. Unlike Ni–P coatings, in Ni–B coatings the inter-
diffusion zone between Fe and Ni is not clearly defined and
it seems to include the entire coating.
Ni–B coatings applied on mild steel showed a higher oxi-
dation resistance than un-coated steels, probably due to the
remaining NiO that influences the protective behaviour of
the oxide layer. According to previous observations [11] the
resistance to oxidation of this coating is more related to its
purity (or nickel content) than with the formation of boron
compounds. Therefore, despite the protection of Ni–B coat-
ings over mild steel is lower than that observed in Ni–P coat-
ings, it can be associated mainly with the formation of NiO, as
well as the barrier effect of the coating itself. The greater
6 J. G. CASTAÑO ET AL.

Figure 7. SEM cross section images and element profiles after oxidation tests of coated steels at 600°C during 400 h: (a, b) Ni–P, (c, d) Ni–B.

outward diffusion of Fe explains the higher oxidation rate
found for these coatings and the greater thickness of the
oxide layer, if compared with Ni–P coatings.
Conclusions
The oxidation resistance at 600°C of Ni–P and Ni–B
coated mild steels after 400 h was higher than that in
un-coated samples. In comparison with the substrate, the
oxidation rate constant (k) value in Ni–P coated mild
steel was lower in three orders of magnitude, while in
Ni–B coated mild steel this value was lower in two orders
of magnitude.
The protection of Ni–P coatings over mild steel was
mainly due to the decrease in the outward iron diffusion
associated with the formation of an interdiffusion layer of
10–15 µm between the coating and the substrate. Other influ-
ential factors were the barrier effect of the coating itself, the
passivation associated with the formation of NiO and the
decrease in the inward oxygen diffusion due to the formation
of Ni3P.
The protection of Ni–B coatings over mild steel was
mainly due to the formation of NiO, as well as the barrier
effect of the coating itself. Nevertheless, the amount of iron
diffusing through the coating to oxidise in the outermost
zone was significant. The lack of boron compounds at 600°
C was probably due to the diffusion and oxidation of boron
at initial stages, and the complete evaporation of these
boron oxides after long-term oxidation.
Disclosure statement
No potential conflict of interest was reported by the authors.
Funding
The authors gratefully acknowledge to CODI-Universidad de Antioquia
for the financial support of the project ‘Influencia del tratamiento tér-
mico en las propiedades tribológicas de recubrimientos autocatalíticos
Ni-B’, under grant [2014-914].
ORCID
Juan G. Castaño http://orcid.org/0000-0002-7972-8293
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