DOI 10.

1007/s11041-022-00781-2
Metal Science and Heat Treatment, Vol. 64, Nos. 3 – 4, July, 2022 (Russian Original Nos. 3 – 4, March – April, 2022)

UDC 669.018.58:621.785.5:621.793.6:669.781

SPECIAL FEATURES OF THE KINETICS OF BORIDING

OF BINARY Fe – Ni ALLOYS

N. Ucar,1 C. Ekinci,2 A. Calik,3 and M. Keddam4

Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 3, pp. 43 – 48, March, 2022.

Original article submitted April 23, 2021.

The kinetics of boriding of Fe – Ni alloys containing 60, 70, 80, and 90 wt.% Ni at 1073 – 1373 K for 2 – 8 h
in powdered mixtures with the use of Ekabor-3 boriding agent has been investigated. It has been established
that a compact multiphase layer represented by nickel silicides, borosilicides, and borides is formed on the al-
loy surface. The hardness of the layer depends on the nickel concentration in the substrate. It is shown that the
growth of the boride layer with time can be described by a parabolic dependence. The activation energy of the
boron diffusion in Fe – Ni alloys is also a function of the nickel content.

Key words: boriding, permalloy, nickel borides, kinetics, activation energy, microhardness.

INTRODUCTION
High nickel-content permalloys containing from 35 to
90 wt.% Ni are probably the most versatile soft magnetic al-
loys [1] due to a combination of high corrosion resistance,
magnetic and mechanical properties [2, 3]. They are widely
used in advanced technological devices, including recording
heads, mobile phones, transformers and magnetic sensors.
Numerous studies have shown that the magnetic and elastic
properties of Fe – Ni system alloys are extremely sensitive to
their microstructure, chemical composition, temperature and
pressure. Thus, it was established in [4] that both magnetic
and mechanical properties of alloys increase significantly af-
ter annealing at 900°C for 20 min, and the formation of
intermetallic Fe – Ni compounds at annealing temperatures
below 900°C adversely affects these properties. It was shown
in [5] that the formation of ordered Ni3Fe and NiFe phases in
the structure significantly changes the mechanism of Fe – Ni
alloys deformation. At that, binary Fe – Ni permalloys,
which have a short-range ordered structure at temperatures
below the Curie point, are not suitable for industrial produc-
1
Faculty of Arts and Sciences, Physics Department, Suleyman
Demirel University, Isparta, Turkey.
2
Rectorate, Bozok University, Yozgat, Turkey.
3
Isparta University of Applied Sciences, Faculty of Technology,
Mechanical Engineering, Isparta, Turkey.
4
Materials Technology Laboratory, Faculty of Engineering and
Technological Engineering, USTHB, Bab-Ezzouar, Algeria
(e-mail: keddam@yahoo.fr).
tion [6]. Alloying of Mo, Cr, and Cu permalloys allows re-
ducing the effect of structure ordering [7] and, as a result, im-
proving the magnetic properties at frequencies from 300 Hz
to more than 1 kHz at a reduced field strength [8].
In recent years, boriding has been used to improve the
magnetic and mechanical properties of permalloys. It was
shown in [9] that with an increase in temperature and
boriding time, a decrease in the saturation magnetization
(Ms ) of alloys due to the formation of a borides/borosilicides
layer on their surface is observed. In addition, a significant
decrease in Ms occurs with an increase in the nickel content
in the alloy due to depletion of the solid solution. It was es-
tablished in [10] that under optimal boriding conditions (se-
veral hours at 1000°C in an H2 atmosphere), a boride layer
with a thickness of more than 200 mm is formed on the alloys
surface. The layer consists mainly of Ni2B boride, its micro-
hardness is 800 – 1000 HV0.1, and its wear resistance is about
6 times higher than that of the original permalloy.
The objective of this research is to analyse the kinetics
and study the specific features of the boriding process of
Fe – Ni system alloys with different nickel content in saturat-
ing powder mixtures containing silicon silicide.
METHODS OF STUDY
The binary Fe – Ni alloys with a 60, 70, 80, 90% Ni con-
tent,5 from which samples with dimensions of 2 ´ 2 ´ 10 mm
5
Hereinafter, the elements content (except for specified cases) is
given in mass fractions expressed in %.

176
0026-0673/22/0304-0176 © 2022 Springer Science+Business Media, LLC
Special Features of the Kinetics of Boriding of Binary Fe – Ni Alloys
50 mm
Fig. 1. Structure (SEM) of boride coatings on Fe – 60% Ni (a), Fe – 70% Ni (b ), Fe – 80% Ni (c), and
Fe – 90% Ni (d ) alloys after boriding at 800°C, 5 h.
were cut, were used as a substrate for boriding. Boriding was
carried out in a solid medium, i.e. in powdered mixtures with
the use of the Ekabor 3 agent containing 90% SiC, at atmo-
spheric pressure in electric resistance furnaces according to
the modes: for 2, 4, 6, 8 h at 1223 K and for 5 h at
1073 – 1373 K.
The microstructure of alloys was studied using light and
scanning electron (JEOL 5600LV) microscopes. The thick-
ness of the borided layer was determined using a digital me-
ter connected to a light microscope (Nikon MA100). The
phase composition of the layer was assessed on an x-ray
diffractometer (Rigaku D-MAX 2200) in copper Ka radiation
(l = 0.15418 nm). The microhardness was measured in the
cross section of the samples perpendicular to the borided sur-
face using a Vickers indenter at a load of 100 g and a holding
time of 15 sec. Elemental profiling along the samples thick-
ness was carried out using radio frequency spectrometry with
optical emission of a glow discharge (Horiba Jobin Yvon-RF
GDOES) under the following discharge conditions: 600 Pa
for Ar pressure, 75 W for direct wave radio frequency power,
pulse frequency of 10 kHz.
RESULTS AND DISCUSSION
Figure 1 shows the structure (SEM) of the cross section
of borided samples of Fe – Ni alloys with different nickel
contents after annealing at 800°C for 5 h. One can see that
the formed coatings are compact and dense. The coating
177
a b
c d
thickness in the Fe – 60% Ni alloy was 27 mm and reached
49 mm in the alloy with 90% Ni.
Figure 2 shows the structure of the coatings formed on
the surface of the Fe – 90% Ni alloy after boriding at 950°C
for 2, 4, and 6 h. After boriding according to such modes,
compact and continuous coatings are also formed; however,
they contain pores due to the formation of nickel silicides
[11, 12]. At that, porosity is observed at the longest holding
time of 6 h. The coating thickness after boriding at 950°C for
2 h was 63 mm and reached 128 mm after treatment for 6 h.
Figure 3 shows x-ray diffraction patterns of the Fe –
60% Ni alloy borided at 800, 950, and 1000°C for 5 h. After
boriding at 800 and 950°C, nickel silicide Ni2Si, presented
together with the Ni6Si2B phase, was found on the alloy sur-
face (Fig. 3a and b ). After boriding at 800°C, in addition, the
Ni3B phase is formed (Fig. 3a ). The Ni6Si3 phase was de-
tected only on the surface of the alloy treated at 1000°C, in
which iron boride Fe2B was also observed (Fig. 3c ).
Figure 3d shows the x-ray diffraction pattern of the Fe –
90% Ni alloy after boriding at 1100°C for 5 h. In this case,
the formation of two phases, Ni4B3 and Ni6Si2B, was de-
tected in the surface layer. It is characteristic that the Ni6Si2B
phase was also observed on the surface of the Fe – 60% Ni
alloy borided for 5 h at 800 and 950°C. However, nickel
boride Ni4B3 is formed only in the Fe – 90% Ni alloy, which
is explained by the thermodynamic stability of the boride
containing 11.6% B at high temperatures [13].
178 N. Ucar et al.

100 mm a 100 mm b 100 mm c

Fig. 2. Structure (SEM) of boride coatings on Fe – 90% Ni alloy after boriding at 950°C for 2 h (a), 4 h (b ) and 6 h (c).

Analysis of the obtained x-ray diffraction patterns of the
alloys allows concluding that the phase composition of the
coatings formed during boriding depends on the nickel con-
tent in the Fe – Ni alloy and its treatment temperature and
may include various compounds: silicide, borosilicide or
nickel boride and iron boride of Fe2B type.
Measurement of microhardness in the cross section of
the studied samples showed that the hardness of the boride
layer depends on the parameters of boriding (temperature
and time) and varies in the range from 1011 to 1350 HV0.1
(Table 1), while the hardness of the alloy matrix is
176 ± 20 HV0.1. This level of surface hardness corresponds to
coatings formed with nickel silicides and/or borosilicides.
The minimum value of the surface layer microhardness of
1011 ± 73 HV0.1 was obtained in the Fe – 70% Ni alloy after
boriding at 800°C for 5 h, and the maximum value of
1350 ± 95 HV0.1 was obtained in the Fe – 90% Ni alloy after
treatment at 950°C for 5 h.
In [14], when boriding Fe – Mn alloys containing 0.42,
0.76 and 1.94% Mn, a surface layer, consisting of iron bor-
ides FeB, Fe2B and manganese boride MnB, was obtained.
The hardness of such a layer reached the values of 1400 –
1270 HV0.1. The slightly lower hardness of the boride layer
in the alloys investigated in this research is explained by the
formation of nickel silicides and borosilicides in it, as well as
a small number of pores. In [12], when studying nickel with

I, arb. units I, arb. units

2500 1000
Ni2Si à Ni2Si b
SiC Ni6Si3
2000 Ni3B 800 Ni6Si2B
Ni6Si2B

1500 600

1000 400

500 200

0 0
20 30 40 50 60 70 80 90 20 30 40 50 60 70 80 90
2q, deg 2q, deg
I, arb. units I, arb. units
400
1000
NiSiO2 c d
Fe2B Ni6Si2B
300 Ni6Si3 800 Ni4B3

600
200
400
100
200

0 0
20 30 40 50 60 70 80 90 20 30 40 50 60 70 80 90
2q, deg 2q, deg

Fig. 3. Diffraction patterns of the surface layer of Fe – 60% Ni (a – c) and Fe – 90% Ni (d ) alloys after boriding for 5 h at
the following temperatures: a) 800°C; b ) 950°C; c) 1000°C; d ) 1100°C.
Special Features of the Kinetics of Boriding of Binary Fe – Ni Alloys 179

Fe; B; Si, at.% u, mm

160
100 Fe
90 140

80
120
70
60 100

50 80
40
60
30
20 B 40
10 Si
20
0
5 10 15 20 25 30 35 40 h, mm

Fig. 4. Change in the Fe, Si and B content in the cross section of the 0 1 2 3 Ö t, h
boride coating (h is the distance from the surface) on the Fe – 80% Ni Fig. 5. Dependence u = F ( t) (u is the surface layer thickness; t is
alloy after boriding at 950°C for 2 h.
the boriding duration at 950°C) for Fe – Ni alloys with different
nickel contents: M) 60% Ni; :) 70% Ni; &) 80% Ni; p) 90% Ni.

a purity of 99.5% after boriding at 950°C for 2, 4, and 8 h in

an Ekabor 2 powder mixture, it was established that three fusion coefficient of boron through the coating layer. Fi-
different zones are formed on the samples surface: external gure 5 shows the dependences of the thickness of the formed
— from Ni5Si and Ni2Si silicides, internal — from Ni2B surface layer on the boriding time at 950°C for the Fe – Ni
boride, and transitional. At that, the microhardness of the system alloys with different nickel contents. The kinetic
surface was 747 – 805 HV. curves correspond to the parabolic law of boride layers
Figure 4 shows the results of elemental profiling of the growth, i.e. the layer thickness is proportional to the square
surface layer of the Fe – 80% Ni alloy after boriding at root of the treatment time. Consequently, the boriding pro-
950°C for 2 h. One can see that reactions of silicides and cess is controlled by the diffusion of boron atoms through the
borosilicides formation occur in the surface layer of the alloy coating layer in the solid state.
during treatment.
To analyse the growth kinetics of borided coatings of
Fe – Ni alloys in powdered mixtures containing SiC, the fol-
lowing empirical relationship was used [15, 16]:
TABLE 2. Thickness (u ) of Surface Layer of Fe – Ni Alloys after
u = k t = Dt, (1) Boriding at Tb = 800 – 1100°C for 5 h
Alloy Tb , °C u, mm
where u is the layer thickness; k is the parabolic growth con-
Fe – 60% Ni 800 27
stant; t is the treatment time. Parameter D represents the dif-
900 38
1000 64
1100 118
TABLE 1. Microhardness of Surface Layer of Fe – Ni Alloys after Fe – 70% Ni 800 32
Boriding According to Different Modes 900 50
Alloy Boriding mode HV0.1 , kgf/mm2 1000 92
1100 134
Fe – 60% Ni 800°C, 5 h 1212 ± 56
Fe – 80% Ni 800 41
Fe – 60%Ni 1000°C, 5 h 1165 ± 120
900 74
Fe – 60% Ni 1100°C, 5 h 1088 ± 27
1000 110
Fe – 70% Ni 800°C, 5 h 1011 ± 73 1100 154
Fe – 80% Ni 800°C, 5 h 1157 ± 124 Fe – 90% Ni 800 49
Fe – 90% Ni 950°C, 4 h 1240 ± 80 900 67
Fe – 90% Ni 950°C, 6 h 1350 ± 95 1000 119
Fe – 90% Ni 950°C, 8 h 1190 ± 51 1100 174
180 N. Ucar et al.

ln D, m2/sec ln D, m2/sec
–27 –27
ln D = – 119.58kJ/RT – 17.6376 ln D = – 119.94kJ/RT – 17.1346
R 2 = 0.967 R 2 = 0.991
–28 –28

–29 –29

–30 –30

à b
–31 –31
7 ´ 10–4 8 ´ 10–4 9 ´ 10–4 1/T, K – 1 7 ´ 10–4 8 ´ 10–4 9 ´ 10–4 1/T, K – 1

ln D, m2/sec ln D, m2/sec
–27 –27
ln D = – 107.56kJ/RT – 17.8832 ln D = – 106.44kJ/RT – 17.8534
R 2 = 0.996 R 2 = 0.977
–28
–28

–29

–29
–30

c d
–31 –30
7 ´ 10–4 8 ´ 10–4 9 ´ 10–4 1/T, K – 1 7 ´ 10–4 8 ´ 10–4 9 ´ 10–4 1/T, K – 1

Fig. 6. Arrhenius equations obtained for Fe – Ni alloys with a 60% (a), 70% (b ), 80% (c), 90% (d ) Ni content: D is
the boron diffusion coefficient in the coating; 1/T is the reciprocal of the absolute temperature.

The temperature dependence of the boron diffusion coef- Q varies in the range of 106.45 – 119.94 kJ × mol – 1, which
ficients in the coating layer is described by the equation can be interpreted as the range of minimum values of the ac-
tivation energy required for boron diffusion during boriding
æ Q ö
D = D0 exp ç - ÷, (2) of the studied alloys in powder mixtures. It should be noted
è RT ø that the results obtained are almost the same for all investi-
where D is the boron diffusion coefficient in the coating gated Fe – Ni alloys under the used boriding modes.
layer; D0 is the frequency factor of the diffusion process; Table 4 presents the results of a comparative analysis of
Q is the activation energy; T is the temperature, K; R = the values of the boron activation energy given in
8.314 J × mol – 1 × K – 1 is the universal gas constant. The re- [14, 17 – 21] and obtained in this research. One can see that
sults of measuring the boride layer thickness presented in Ta-
ble 2 were used to calculate the boron diffusion coefficients
through the coating layer for each investigated Fe – Ni sys- TABLE 3. Calculated Values of Q and D0 in Eq. (2) for Fe – Ni Al-
loys during Boriding
tem alloy. The calculations were performed according to
Eq. (1), according to which the D values are the square of the Alloy D0 , m2 × sec – 1 Q, kJ × mol – 1
parabolic growth constant k. Fe – 60% Ni 2.18 ´ 10 – 8 119.58
Figure 6 shows the Arrhenius equations of the calculated Fe – 70% Ni 3.61 ´ 10 – 8 119.94
D values, constructed according to Eq. (2) for Fe – Ni alloys. –8
The values of Q and D0 for Fe – Ni system alloys are
Fe – 80% Ni 1.71 ´ 10 107.56
presented in Table 3. One can see that the activation energy Fe – 90% Ni 1.76 ´ 10 – 8 106.45
Special Features of the Kinetics of Boriding of Binary Fe – Ni Alloys 181

TABLE 4. Activation Energy of Boron Diffusion in Various Alloys

Alloy Boriding method Tb , K Phase composition of the boride layer Q, kJ × mol – 1 Reference
Fe – 0.42% Mn; Powder 1073 – 1373 Fe2B; FeB; MnB 116.06 – 122.94 [14]
Fe – 0.76% Mn;
Fe – 0.94% Mn
Nickel 201 Powder 1123 – 1223 NiB; Ni2B; Ni3B; Ni4B3 203.87 [17]
Ni3Al Electrochemical 1073 – 1223 Ni3B; Ni4B3; Ni20AlB14 185.95 [18]
Ni3Al Powder 1073 – 1223 Ni3B; Ni4B3; Ni3Al 188 ± 14.4 [19]
Fe – 4% Ni Powder 1023 – 1273 (Fe, Ni)B 311 [20]
(Fe, Ni)2B 178
Fe – 10% Ni Powder 1023 – 1273 (Fe, Ni)B 286 [20]
(Fe, Ni)2B 157
Ni – 3% Mg Powder 1173 – 1273 NiB; Ni2B 158.843 [21]
Ni – 7% Mg Ni3B 136.506
Fe – (60 – 90)% Ni Powder with Ekabor 3 agent 1073 – 1373 Ni2Si; Ni6Si2B; AlNi6Si3; Ni4B3; Fe2B 106.44 – 119.94 Current
research

Notations: Tb is the boriding temperature; Q is the activation energy of boron diffusion.

the value of the boron activation energy depends signifi-
cantly on the method of boriding, the substrate chemical
composition, and the process temperature. Thus, in [14], the
boriding kinetics of Fe – Mn alloys containing 0.42, 0.76 and
0.94% Mn was studied. It has been established that Fe2B,
FeB, and MnB borides are formed in the surface layer of the
alloys during boriding, and the boron activation energy va-
ries in the range Q = 116.06 – 122.94 kJ × mol – 1. The activa-
tion energy values obtained in [14] are very close to those es-
tablished in the present research. In [17], when boriding the
Nickel 201 alloy at 1123 – 1223 K, a multiphase surface
layer was obtained, which contained four types of nickel bor-
ides: NiB, Ni2B, Ni3B, and Ni4B3, while the calculated boron
activation energy was Q = 203.87 kJ × mol – 1.
In [18], ultrafast electrochemical boriding of nickel
aluminide substrates at 1073 – 1223 K and a current density
of 0.1 – 0.5 A × cm – 2 has been carried out. The value
Q = 185.96 kJ × mol – 1 has been calculated. In [19], boriding
was carried out in a mixture of Ekabor – Ni powders in the
temperature range of 1073 – 1223 K for 2 – 8 h in a nickel
aluminide suspension. A boride layer containing Ni3B and
Ni4B3 phases was formed, while Q = 118.8 ± 14.4 kJ × mol – 1.
In [20], Fe – Ni alloys with 4 and 10% Ni were subjected to
boriding at 1023 – 1273 K with the formation of a two-phase
boride layer: FeB and Fe2B. However, x-ray studies confirm-
ing the presence of nickel borides and other phases have not
been carried out. At that, the values of the boron activation
energy in FeB and Fe2B were determined using a kinetic
model. Comparative analysis showed that the activation en-
ergy values calculated in [20] are higher than those obtained
in the present research. This is probably due to the lower
nickel content in the Fe – Ni alloys used in [20]. In [21], bi-
nary alloys Ni – 3% Mg and Ni – 7% Mg were borided in
powder mixtures with the Ekabor 2 agent at 900 – 1000°C.
X-ray analysis showed the formation of NiB, Ni2B and Ni3B
nickel borides in the surface layer, while Q = 158.843 and
136.506 kJ × mol – 1 in alloys with 3 and 7% Mg, respec-
tively.
CONCLUSIONS
The research investigates the effect of boriding at 1073 –
1373 K for 2 – 8 h in powdered mixtures using the Ekabor-3
agent containing 90% SiC on the structure, phase composi-
tion and hardness of the surface layer of Fe – Ni alloys with a
60, 70, 80 and 90% Ni content. It is shown that in the
boriding process, compact, dense and practically non-porous
multiphase layers are formed on the alloys surface, consist-
ing of nickel silicides, borides and borosilicides, the compo-
sition and ratio of which depend on the chemical composi-
tion of the alloy, temperature and boriding duration.
The thickness of the coating of borided alloys is 27 –
174 mm, the surface microhardness is 1011 – 1350 HV0.1.
The value of these characteristics largely depends on the
boriding duration and temperature, as well as the nickel con-
tent in the substrate.
The increase in the thickness of the boride layer with the
boriding time is described by a parabolic dependence, and
the value of the activation energy of boron diffusion in the
studied Fe – Ni alloys is in the range of 106.45 –
119.94 kJ × mol – 1.
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