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Studies of magnetic properties of iron-based coatings produced by a high-

velocity oxy-fuel process

Article  in  Materials Chemistry and Physics · August 2005

DOI: 10.1016/j.matchemphys.2005.01.047

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 Materials Chemistry and Physics 92 (2005) 419–423

Studies of magnetic properties of iron-based coatings produced by a

high-velocity oxy-fuel process
M. Cherigui a,∗ , S. Guessasma a , N. Fenineche a , R. Hamzaoui b , O. El-Kedim b , C. Coddet a
a LERMPS—UTBM (Site de Sévenans), F-90010 Belfort, Cedex, France
b Nanomaterials Research Group (NRG)—UMR 5060 CNRS-UTBM, Site de Sévenans, F-90010 Belfort, Cedex, France

Received 4 October 2004; received in revised form 28 December 2004; accepted 9 January 2005

Abstract

The paper studies the effect of high-velocity oxy-fuel thermal spraying parameters, in particular spray distance and oxygen flow rate, on
coating porosity and magnetic properties of FeSi and FeSiB deposits using the artificial neural network methodology. The magnetic properties
correlated to coating porosity were obtained using an optimized network structure. The predicted results permitted to point out the role of
porosity for varying the coercivity and saturation magnetization and the stability of magnetic properties with respect to the considered spray
parameters.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Magnetic materials; Coatings; Computer modelling and simulation; Magnetic properties

1. Introduction magnetic losses. These losses decompose to loss by hysteresis

Magnetic materials are elaborated by various techniques,
in particular rapid quenching and mechanical alloying. The
major problem of these techniques is their limited field of
application. An alternative can be found to solve this lim-
itation. Indeed, thermal spraying can be considered as one
of the processes, allowing the realization of deposits accord-
ing to various techniques conferring specific functionalities
to the parts to be covered by integrating a broad material
range (metallic, ceramic and polymeric alloys and composite
materials).
The high-velocity oxy-fuel (HVOF) technique has been
widely used mainly due to its high flame velocity (up to
Mach 5) and moderate temperature (below 3000 ◦ C). The
moderate flame temperature is especially suitable for coat-
ing deposition of materials with low melting temperatures
[1].
FeSi alloy is selected for its good magnetic properties.
In the dynamic mode, the soft magnetic materials dissipate
energy in the form of heat. FeSi alloys can also decrease
∗ Corresponding author. Tel.: +33 3 84 58 3243; fax: +33 3 84 58 3286.
E-mail address: mohamed.cherigui@utbm.fr (M. Cherigui).
and loss by Foucault current, from where the interest of these
alloys in engines, generators and transformers [2].
The choice of FeSiB is justified by the thermal stability of
the residual amorphous phase enriched in boron and the good
magnetic properties related to the presence of silicon, where
the boron increases the possibility of having an amorphisation
phase [3]. Moreover, FeSiB alloys have been widely used as
a magnetic core material for electric generator construction
[3–5].
In order to quantify the role of the porosity of coating on
the magnetic properties of FeSi and FeSiB, a model of data
processing is considered based on the artificial neural network
methodology. Such a methodology is an adequate tool for the
study of complex processes with parameter interdependen-
cies [6]. In addition, this technique proved to be applicable
in the domain of materials science [7] and especially in the
case of thermal spraying [8].
In this context, a network structure is used to relate HVOF
process parameters to both porosity and magnetic properties
of FeSi and FeSiB coatings. The predicted magnetic proper-
ties are then correlated to the porosity level for each material,
taking into account the interdependency revealed by the op-
timized network structure.

0254-0584/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.matchemphys.2005.01.047
420 M. Cherigui et al. / Materials Chemistry and Physics 92 (2005) 419–423

Table 1
Spraying parameters
Fuel flow rate “methane” (SLPM) 145 145
Oxygen gas flow rate (SLPM) 290 350
Oxygen rate in the mixture (fuel/O2 ) 0.5 0.41
Nitrogen carrier gas flow rate (SLPM) 20 20
Powder feed rate (g min−1 ) 35
Spray distance (mm) 250–300
Scanning step (mm) 12
Torch-substrate relative velocity 245
(m min−1 )
Scanning velocity (mm s−1 ) 50
Substrate thickness (mm) 0.8
Spray gun CDS 8944, 3 psi
Deposit thickness (␮m) 200
Number of passes 30

The XRD patterns revealed the basically cubic structure

Fig. 1. X-ray diffraction patterns of the: (a) FeSi and (b) FeSiB powders.
2. Experimental procedure
2.1. Powders
Two types of nanocrystalline powders were used (in at.%):
Fe–6.5Si and Fe–6.5Si–18.5B as alloys with average gran-
ulometries of 45 and 40 ␮m, respectively. These nanocrys-
talline powders were produced from FeSi microcrystalline
powder with an average particle size of 65 ␮m using mechan-
ical alloying during 48 h. FeSiB powder was obtained from
Fe, Si and B elementary powders using the same process. The
ball milling was carried out using a planetary high-energy ball
milling (Retsch PM 400). Steel balls (diameter: 20 mm) and
50 ml volume jar were used. Four jars were mounted on a
planar disc. With the rotation of the disc, the vials moved in
a circular and opposite direction compared to the disc rota-
tion. The rotation speed of disc was equal to 400 rpm and the
rotation speed of jar was equal to 800 rpm. The grain size of
the resulting powders was estimated using X-ray diffraction
(XRD) and applying the Scherrer formula. They were about
10 and 12 nm for FeSiB and FeSi, respectively (Fig. 1).
Fe3 Si (DO3) which is characteristic for the low-silicon con-
tent FeSi alloys. These results agree with those obtained for
rapidly quenched Fe100 − x Six alloys [5] and mechanically al-
loyed FeSi [9]. Concerning FeSiB powder, it has noticed that
the XRD pattern is similar to that of FeSi.
2.2. Coating preparation
A Sulzer Metco CDS 8944 system was used for coating
preparation. Methane was used as a fuel gas with a flow rate of
145 SLPM (standard litre per minute). The flow rate of oxy-
gen was either 290 or 350 SLPM. Powder carrier gas was ni-
trogen with a flow rate of 20 SLPM. Two spray distances were
used, 250 and 300 mm. The powders were coated on cop-
per substrates using sheet sizes of 70 mm × 25 mm × 0.8 mm.
The experiments were carried out using an air-cooling sys-
tem. Table 1 shows the spray parameters.
2.3. Characterization
Optical microscopy was used to calculate the porosity
level by image analysis, using a NIH image free software.
Ten images were used to assess mean and standard deviation
of the porosity level. Magnetic measurements were realized
using a hysteresismeter Bull M2000 SIIS, which enabled to
draw the hysteresis loop of the considered samples. It per-

Table 2
Magnetic measurements of the coatings
Material Spray distance (mm) Oxygen flow rate (SLPM) Coating porosity (%) Coercivity (Oe) Saturation magnetization
(A m2 kg−1 )
FeSi 250 290 4.48 ± 0.53 15.008 ± 2.10 1170 ± 11
FeSiB 250 290 3.208 ± 1.10 26.008 ± 3.40 1600 ± 9
FeSi 250 350 4.518 ± 0.55 15.068 ± 2.12 1165 ± 10
FeSiB 250 350 3.408 ± 1.00 26.408 ± 3.50 1595 ± 10
FeSi 300 290 4.608 ± 0.53 15.158 ± 2.06 1160 ± 11
FeSiB 300 290 3.508 ± 0.90 26.508 ± 3.60 1590 ± 11
FeSi 300 350 4.628 ± 0.51 15.218 ± 2.10 1155 ± 10
FeSiB 300 350 3.608 ± 1.10 26.508 ± 3.30 1580 ± 12
 M. Cherigui et al. / Materials Chemistry and Physics 92 (2005) 419–423
mitted also to calculate the magnetic properties, particularly
coercivity and saturation magnetization. Table 2 shows the
experimental porosity levels and magnetic properties for the
studied conditions. The coating porosity varied from 3.9 to
4.6%, the coercivity from 21 to 27 Oe and the saturation mag-
netization from 1376 to 1600. The variation recorded for each
property represented 15, 29 and 17% from the average value,
respectively.
2.4. Statistical analysis
An artificial neural network was used to analyze the exper-
imental data. The input parameters were material type, spray
distance and fuel rate. The output parameters were porosity
level, coercivity and magnetization saturation. The optimiza-
tion process of the network structure was rigorously identical
to that of another work [10]. Such an optimization consid-
ered a training and a testing process based on a submitted
database. The optimization steps were run for 1000 cycles
after which 100% of the experimental sets were learnt cor-
rectly (difference between predicted and experimental values
was less than 5%). The average error was less than 0.002.
Fig. 2. Morphology of the coatings: (a) FeSi and (b) FeSiB.
421
3. Results and discussion
3.1. Coating microstructure
Based on previous experiences using a single parameter
variation, the most significant spray parameters were adjusted
to minimize the oxygen content as well as the porosity of the
coatings. Fig. 2 a and b shows the cross-section of dense FeSi
and FeSiB coatings, respectively. Denser coatings were ob-
tained in the case of FeSiB as FeSi deposit structure presents a
large amount of porosity. In addition, the presence of several
non-molten particles in the FeSi deposit is clearly observed
as shown in Fig. 1a. The porosity values are about 4.5 and
3.5% for FeSi and FeSiB, respectively.
3.2. Porosity level related to spray parameters
The optimized artificial neural network structure was used
to predict the correlation between porosity and spray distance
and oxygen flow rate for FeSi and FeSiB coatings. Fig. 3
shows the porosity evolution as a function of spray distance
and oxygen flow for FeSi and FeSiB coatings. It is noticed that
Fig. 3. Porosity level predicted evolution vs. spray distance and oxygen flow
rate for: (a) FeSi and (b) FeSiB coatings.
422 M. Cherigui et al. / Materials Chemistry and Physics 92 (2005) 419–423

the coating porosity remains nearly unchanged when spray

distance increases from 160 to 340 mm. The same magnitude
can be observed when varying the oxygen rate of the two
materials. This increase of porosity with the increase of spray
distance can be related to the following considerations:

- When the spray distance increases, particles leave the flame

and begin to solidify before they impinge the substrate and
thus their temperature is low;
- The decrease of particle temperature has the consequence
to decrease the flattening process as their viscosity is high
and wetability is low;
- The incomplete flattening process increases the amount of
porosity.

The oxygen flow rate seems to have no significant effect on

coating porosity especially for the FeSi material. Roughly
speaking, an oxygen flow rate increase is related to a decrease
of the flame temperature for a fixed fuel flow rate [11]. This
decrease favours the presence of the no-molten particles in
the coating and an increase of porosity if the fuel flow rate is
not sufficient.

Fig. 5. Predicted evolution of saturation magnetization vs. spray distance

and oxygen flow rate for: (a) FeSi and (b) FeSiB coatings.

3.3. Magnetic properties related to spray parameters

Fig. 4 shows the predicted coercivity variation when vary-

Fig. 4. Predicted evolution of coercivity vs. spray distance and oxygen flow
volume for: (a) FeSi and (b) FeSiB coatings.
ing spray distance and oxygen flow for FeSi and FeSiB coat-
ings. It seems that the coercivity increases with both oxygen
flow rate and spray distance. The increase of coercivity fol-
lows the increase of porosity level (Fig. 3), which suggests a
correlated variation between magnetic properties and poros-
ity level. In fact, this represents a partial correlation as the
coercivity variation is also dependent on the oxygen flow
rate.
The saturation magnetization exhibits the same trend with
respect to spray parameters (Fig. 5). As the porosity is mostly
affected by the increase of spray distance, this parameter is
considered as a control factor of the magnetic properties.
Previous studies permitted to point out the role of the spray
distance on the microstructure because of the large sensitivity
of particle velocity and temperature [12,13].
In order to investigate more deeply the role of porosity in
the modification of magnetic properties, one has to withdraw
the spray parameter variables. This is done by collecting the
ANN responses for any process parameter combination and
plotting the porosity versus the magnetic properties. Fig. 6
 M. Cherigui et al. / Materials Chemistry and Physics 92 (2005) 419–423
Fig. 6. Predicted evolution of coercivity vs. porosity level for FeSi and FeSiB
coatings.
Fig. 7. Predicted evolution of saturation magnetization vs. porosity level for
FeSi and FeSiB coatings.
shows the coercivity response as a function of porosity level
response for FeSi and FeSiB coatings. The coercivity ex-
hibits parabolic relationships with the porosity level. The in-
crease of coercivity is explained by the fact that the porosity
acts against the continuity of magnetic properties through the
coating structure. These are considered as defects anchoring
Bloch walls and involving consequently an increase of co-
ercivity [14]. One can conclude that an improvement of the
coercivity can be related to a low-porosity content.
Fig. 7 shows the predicted variation of the saturation mag-
netization as a function of porosity level. A low decrease of
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423
saturation magnetization is noticed. Generally, in magnetism
studies, a decrease of this parameter is related to an increase
in coercivity [15].
4. Conclusions
This study examined the effect of HVOF thermal spray-
ing parameters on the porosity and magnetic properties of
coatings using the artificial neural network methodology.
- The spray distance was the control factor for varying the
porosity for both FeSi and FeSiB as the increase of this
parameter permitted to increase the spray distance. The
oxygen flow rate was not sensitive to porosity variation.
- Coercivity and saturation magnetization were dependent
on both spray parameters.
- Structural modifications related to spray distance variation
permitted to predict the increase of coercivity with the in-
crease of porosity.
- The saturation magnetization is correlated to the coercivity
and is thus affected by the porosity level.
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