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Characterization and Boronizing Kinetics of EN-GJL-250 Lamellar Gray Cast

Iron

Article · March 2020

DOI: 10.18280/acsm.440103

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 Annales de Chimie - Science des Matériaux
Vol. 44, No. 1, February, 2020, pp. 23-28
Journal homepage: http://iieta.org/journals/acsm

Characterization and Boronizing Kinetics of EN-GJL-250 Lamellar Gray Cast Iron

Chaima Zouzou1, Mourad Keddam1*, Boudjema Bouarour1, Adam Piasecki2, Andrzej Miklaszewski2, Michal Kulka2
1
Laboratory of Materials Technology, Faculty of Mechanical and Process Engineering, University of Sciences and Technology
Houari Boumediene, Bab-Ezzouar, Algiers, Algeria
2
Institute of Materials Science and Engineering, Poznan University of Technology, Poznan, Poland

Corresponding Author Email: mkeddam@usthb.dz

https://doi.org/10.18280/acsm.440103 ABSTRACT

Received: 18 August 2019 The aim of the present study is to generate the boride coatings at the surface of the
Accepted: 5 November 2019 lamellar gray cast iron (EN-GJL-250). This material was hardened by pack-boriding in
the powders mixture of 50% B4C, 49.5% Al2O3 and 0.5% AlF3 at 800, 900 and 1000°C
Keywords: for 4, 6 and 8 h. The produced borided layers were characterized by Scanning electron
pack-boriding, kinetics, activation energy, microscopy (SEM) and XRD analysis. The boriding kinetics of EN-GJL-250 lamellar
design of experiments, integral diffusion model gray cast iron was also investigated. Based on the experimental data, the value of
activation energy for boron diffusion was calculated as 163.86 kJ mol-1 for the EN-GJL-
250 cast iron by using the integral diffusion model. The regression model based on the
design of experiments (DOE) was also employed in order to predict the total boride layer
thickness as a function of boriding parameters (the treatment time and the boriding
temperature). The experimental values of total boride layer thickness were in agreement
with the results from the regression model.

1. INTRODUCTION powders containing 90% SiC, 5% B4C, and 5% NaBF4 to get

a double boride layer (FeB+Fe2B). In this paper, a kinetic
The boriding process is a thermochemical treatment applied analysis was done by using the design of experiments
to produce a hard layer composed of borides on ferrous and approach. Sen et al. [9] have borided in salts bath three types
non-ferrous alloys. In case of ferrous alloys (steels and cast of ductile cast irons at 850 and 950°C for 2 to 8 h. They
irons), two kinds of iron borides can be formed depending on analyzed the growth kinetics of formed boride layers at 850
the chemical composition of boriding agent and on the process and 950°C. Sen et al. [10] have borided a ductile cast iron in
parameters (the time duration and the boriding temperature). salts bath and have studied its boriding kinetics. Azouani et al.
As a result of this thermochemical process, the surface [11] have analyzed the boriding kinetics of EN-GJS-400-15
properties and wear performance of treated parts are improved ductile cast iron by using the mixture of powders composed of
due to a high hardness of boride layers [1]. The boriding 90% SiC, 5% B4C, and 5% NaBF4
process requires high temperatures to be carried out (between In the current work, the EN-GJL-250 lamellar gray cast iron
800 and 1050°C) and a treatment time from 0.5 to 10 h. was hardened by the powder-pack boriding in the temperature
Various methods of boriding can be found in the literature. range 800-1000°C for a treatment time of 4-8 h.
Among them, the powder pack-boriding as the frequently used The morphology of produced boride layers was observed by
method, owing to its simplicity and cost effectiveness [2, 3]. SEM. The crystallographic nature of iron borides was
For instance, Sen et al. [4] have used the liquid boriding (in identified by XRD analysis. Furthermore, the activation
salts bath) to produce the boride layers on GGG-80 ductile cast energy for boron diffusion in EN-GJL-250 lamellar gray cast
iron and investigate the wear behaviour. iron was estimated by using the integral diffusion model and a
Nodular cast iron 500-7 was laser borided by a CO2 comparison was made with the literature results.
molecular laser with a continuous wave and using amorphous A comparison of experimental total boride layers’
boron as an alloying element [5]. In the literature, a few thicknesses with the simulated values from the regression
information about the growth kinetics of gray and ductile cast model was finally done.
irons exists. In this context, Campos-Silva et al. [6] have pack- The present research paper is organized in 5 sections.
borided the gray cast iron material between 1173 and 1273 K Section 1 presents an overview of existing research
to form a single boride layer (Fe2B). They applied a diffusion background and significance of the studied problem. The
model to estimate the boron diffusion coefficients in the Fe2B mathematical formulation of the integral diffusion model is
layers formed on gray cast iron. Mu et al. [7] have hardened a addressed in Section 2.
gray cast iron by powder pack-boriding in the temperature The details regarding the material and experimental
range 1123-1223 K to get a single Fe2B layer using a mixture procedure are given in Section 3. The estimated value of boron
of powders composed of 88% SiC, 8% B4C, and 4% KBF4. activation energy was compared to the data taken from the
Azouani et al. [8] have treated the EN-GJL-250 gray cast literature in Section 4. A conclusion gathering the main results
iron in the temperature range 800-1000°C with a mixture of was given in the last Section.

23
2. THE INTEGRAL DIFFUSION MODEL where, DBL
B is the boron diffusion coefficient in the entire boride

layer (FeB+Fe2B). The expression of the boron-concentration

This kinetic approach, based on the integral diffusion model, profile along the entire boride layer was taken from the
Türkmen et al. [12] was adopted to be applied for the growth Goodman’s method [21] as follows:
kinetics of entire boride layer (FeB+Fe2B) formed on the
lamellar gray cast iron substrate. The integral diffusion model C BBL [ x, t ] = Clow
Fe2 B
+ a(t )[u (t ) − x] + b(t )[u (t ) − x]2
has been successfully used to simulate the kinetics of Fe2B
layers on different substrates [12-18]. The developed boron for 0 xu (5)
concentration-profile through the entire boride layer is
schematically shown in Figure 1. The three time-dependent unknowns a(t), b(t) and u(t) are
subjected to the boundary conditions given by Eqns. (2) and
(3). Eq. (6), which is the first algebraic constraint, was
obtained by considering the boundary condition on the surface:

a(t )u(t ) + b(t )u(t ) 2 = (CupFeB − Clow

Fe2 B
) (6)

The ordinary differential equation (ODE) given by Eq. (7)

was CFe B
low obtained after integration of Eq. (4) with respect to
2

the diffusion distance x(t) from 0 to u(t):

d u (t )2 da(t ) u (t )3 db(t )
[ + ] = 2DBBL b(t )u(t ) (7)
dt 2 dt 3 dt

The second algebraic constraint was derived from the mass

Figure 1. A schematic illustration of boron-concentration balance equation at the (FeB+Fe2B/substrate) interface:
profile through the entire boride layer
(CupFeB + Clow
Fe2 B
)b(t ) = a(t )2 (8)
FeB
C denotes the upper limit of boron concentration in the
up

FeB phase (=16.40 wt.%) while represents the lower limit of Eqns. (6), (7) and (8) represent a system of differential
boron concentration in the Fe2B phase (=8.83 wt.%) and the algebraic equations (DAE) whose unknowns are the variables
variable u represents the entire boride layer thickness a(t), b(t) and u(t). By considering the analytic solution of this
(FeB+Fe2B). The term Cads is the adsorbed boron diffusion problem, the expression of boron diffusion
concentration in the entire boride layer during the boriding coefficient in the total boride layer (FeB+Fe2B) was deduced
treatment [19]. C0 is the boron solubility in the matrix which as follows (Table 1):
can be neglected because of its very low concentration (0
wt.%) [20]. DBBL =  k 2 (9)
The assumptions considered during the formulation of this
diffusion model were given elsewhere [12-18]. The initial and
With:
boundary conditions for this diffusion problem are represented
as:
1 Cup + Clow2 CupFeB − Clow
FeB Fe B Fe2 B

 = [( )( FeB )(1 + 1 + 4( ))
t = 0, x 0, with C BBL [ x(t ), t = 0] = C0  0 16 Cup − Clow
Fe2 B
CupFeB + Clow
Fe2 B
(1)
wt.%B 1
+( )]
12
Boundary conditions:
k represents the parabolic growth constant at the (FeB+Fe2B
CBBL[ x(t = 0) = 0, t = 0] = CupFeB /substrate) interface or the slope of the straight line relating the
(2) entire boride layer thickness u(t) to the square root of time.
for Cads  16.23 wt.% B
u(t ) = k t (10)
C BBL [ x(t = t ) = u (t ), t = t ] = Clow
Fe2 B

(3)
for Cads  8.83 wt.% B The  constant was found to be equal to 0.60061. The
expression of entire boride layer thickness from the integral
method can be finally re-written as follows:
The change in the boron concentration inside the entire
boride layer (FeB+Fe2B) as a function of the distance x(t) at a
given boriding temperature is described by the Second Fick’s DBBL
u (t ) = t (11)
law: 

 2CBBL [ x, t ] CBBL [ x, t ]
DBBL = (4)
x 2 t

24
 Table 1. The experimentally determined parabolic growth
constants and the calculated values of boron diffusion
coefficients by using the integral diffusion model (Eq. (9))

T (°C) k (µm s -0.5) DBL 2 -1

B (µm s )
800 0.27009 0.04381
900 0.60792 0.22197
1000 1.1413 0.78239

3. EXPERIMENTAL PROCEDURE

3.1 The material and the boriding treatment

The substrate to be hardened by the powder-pack boriding

was the EN-GJL-250 lamellar gray cast iron whose chemical
composition is displayed in Table 2. Figure 2. SEM micrograph showing the initial
microstructure of EN-GJL-250 lamellar Gray cast iron
Table 2. Chemical composition of EN-GJL-250 lamellar
Gray cast iron (given in weight percent)

C Si Mn P S Fe
3.1-3.4 1.9-2.3 0.6-0.9 0.05 0.02 Bal.

The samples to be borided were cut from an ingot in cubic

form with dimensions of 10x10x10 mm3. The SiC abrasive
papers of different granulometry (of 180 to 400) were used for
grinding. They were finally cleaned with acetone to remove
any residue of grease and dirt. The pack-boriding process was
realized in a sealed stainless steel container placed in an
electrical resistance furnace. The container was filled with the
powders mixture composed of 50 wt.% B4C, 49.5 wt.% Al2O3
and 0.5 wt.%AlF3. The samples to be borided were placed in
contact with the powders mixture. The process temperatures
were 800, 900 and 1000°C for treatment times of 4, 6 and 8h.
Once finished, the borided samples were removed from the
furnace and cooled in air.

3.2 Characterization of the borided samples

The SEM observations were performed on polished and

etched cross-sections of pack-borided samples using TESCAN
VEGA 5135 scanning electron microscope. The
measurements of boride layer thickness were made by
employing a practical procedure proposed by Kunst and
Schaaber [22] along the cross-sections of borided samples. A
minimum of 20 measurements was taken to ensure a good
reproducibility. The formation of iron borides at the surface of
borided samples was confirmed by using an X-ray
diffractometer (PHILIPS X’PERT PRO MPD) with a Cu-K
radiation source with a wavelength of 0.154 nm. To determine
the crystalline nature of phases from the diffraction peaks, the
data taken from the JCPDS database were used [23].

4. RESULTS AND DISCUSSIONS

4.1 SEM observations of the boride layers

Figure 2 shows the SEM image of the initial microstructure

of EN-GL-250 lamellar cast iron after etching with 2% Nital
solution. The lamellar graphite is seen inside a fully pearlitic
matrix. Figure 3. SEM images of the cross-sections of borided
samples of EN-GJL-250 lamellar gray cast iron for 8 h at
different temperatures: (a) 800°C, (b) 900°C and (c) 1000°C

25
 Figure 3 shows the cross-sections of boride layers formed Figure 4 represents the XRD patterns obtained at the
on EN-GJL-250 lamellar gray cast irons at 800, 900 and surfaces of borided EN-GJL-250 lamellar cast iron for the
1000°C during 8 h of treatment after etching with 2% Nital boriding conditions (800, 900 and 1000°C for 8 h of treatment).
solution. The boride layers exhibited a less pronounced saw- The presence of iron borides was verified by use of JCPDS
tooth morphology because of the presence of alloying database [23]. Two kinds of iron borides were identified as
elements with high contents compared to borided low alloy FeB and Fe2B at the surface of treated lamellar gray cast iron.
steels, carbon steels and Armco iron. The formation of borides The same phases were also found for all boriding conditions.
needles was ascribed to the preferred pathway for boron It is seen that the Fe2B phase has the strongest peak
diffusion along the crystallographic direction [0 0 1] [24]. corresponding to the crystallographic plane (002) whatever the
Furthermore, the thickness of boride layers was increased with boriding temperature. The boride layer is composed mainly of
the rise of boriding temperature since the diffusion Fe2B phase with a minor presence of FeB phase based on the
phenomenon of boron atoms at the surface of treated material XRD results.
is thermally activated. The boride layer thickness reached a
value of 190.398.3 µm at 1000°C while it is only 49.193 µm 4.3 Estimation of the value of activation for boron diffusion
at 800°C for a treatment time of 8 h. No contrast could be
distinguished between the both layers (FeB and Fe 2B) in the The boriding kinetics is controlled by the diffusion rate of
SEM images since the volume fraction of FeB phase is very boron atoms inside the substrate. Therefore, the values of
low. It can be concluded that the Fe2B phase is dominant in the parabolic growth constants can be obtained from a linear
formed boride layers whatever the boriding conditions. fitting of the experimental entire boride layer thickness u(t)
versus the square root of time according to Eq. (10). The
4.2 XRD analysis variation of total boride layer as a function of square root of
time is depicted in Figure 5 for different boriding temperatures.
3500
(b)
Gray cast iron borided at 900°C for 8 h

Total boride layer thickness (µm)

◼
3000 800°C
❑ FeB
200 900°C
Intensity ( counts)

◼ Fe B
2500 2
1000°C

2000 150

1500
100

1000
◼
❑ ◼ 50
❑
500 ◼

◼ ◼ ◼
0 0
20 30 40 50 60 70 80 90 120 130 140 150 160 170
0.5
Angle 2 theta (°) Square root of time (s)
3000
(a)
Gray cast iron borided at 800°C for 8 h

2500 ◼ Figure 5. Time dependence of the square of total boride layer

❑ FeB
thickness at different process temperatures
Intensity ( counts)

◼ Fe B
2
2000
The parabolic character regarding the growth kinetics of
1500 boride layers is confirmed. The relationship describing the
evolution of boron diffusion coefficient with the boriding
1000 temperature can be expressed by Eq. (12):
◼
❑

500 ◼
Q
DBBL = D0 exp(−
❑

◼ ❑ ❑◼ ❑
◼
❑ ◼
❑
) (12)
0 RT
20 30 40 50 60 70 80 90
Angle 2 theta (°)
3600
where, D0 is the diffusion coefficient of boron extrapolated at
3200
(c) Gray cast iron borided at 1000°C for 8 h
◼ a value of (1/T) = 0. The Q parameter represents the value of
❑ FeB activation energy for boron diffusion which gives the quantity
2800
of energy (in kJ mol-1) necessary for the reaction to occur, and
◼ Fe B
Intensity ( counts)

2400
R is the ideal gas constant (R=8.314 J mol-1. K-1). Figure 6
2000
describes the evolution of natural logarithm of the calculated
1600
values of boron diffusion coefficients through the entire boride
1200 layer as a function of reciprocal temperature.
800
◼
❑
The value of activation energy for boron diffusion Q can be
400 ❑
◼
◼
readily obtained from the slope of the curve relating the natural
◼ ◼

logarithm of DBBL to the inverse of temperature. Eq. (13) was

◼
0
20 30 40 50 60 70 80 90
Angle 2 theta (°) obtained from the graph displayed in Figure 6 by a linear
fitting of data with a coefficient of determination close to unity.
Figure 4. XRD patterns recorded at the surfaces of pack-
borided EN-GJL-250 lamellar gray cast iron for 8 h of 163.86kJ / mol
treatment at the three temperatures: (a) 800°C, (b) 900°C and DBBL = 4.2317 10−6 exp(− ) (13)
RT
(c) 1000°C

26
Table 3. Values of activation energies for boron diffusion in layers’ thicknesses agree with the experimental results.
the pack-borided cast irons

Material Q (kJ mol -1) References

ASTM A-536 197.28 [3]
Gray cast iron 177.4 [6]
Gray cast iron 209.0 [7]
EN-GJS-400-15 212.28 [11]
ASTM A-536 155.7 [25]
EN-GJL-200 163.86 This work

In Table 3 are gathered the values of activation energies for

boron diffusion in some pack-borided cast irons [3, 6, 11, 25]
with the value of activation energy for boron diffusion in EN-
GJL- 250 lamellar gray cast iron estimated in this work. The
found value of activation energy for boron diffusion (=163.86 Figure 7. Iso-thickness diagram showing the variation of
kJ mol-1) is required to overcome the energetic barrier total boride layer thickness as a function of the boriding
allowing the diffusion of boron atoms inside the material parameters
substrate.
Table 4. Comparison between the experimental values of
-27 total boride layers’ thicknesses and those provided by
BL
D=exp(-163.86 kJ/RT - 12.3729) regression model (Equation (14)) in the temperature range
B
800-1000°C
-28
2
Ln (D (m s ))

R=0.999 Total boride layer thickness (µm)

2 -1

T (°C) t (h) Experimental values Simulated values

-29
800 4 29.391.6 30.36
BL

6 38.293.4 40.07
8 49.193.0 48.39
-30
900 4 73.856.2 72.24
6 88.087.1 89.55
8 103.637.9 105.48
-31
1000 4 140.17.6 142.46
7.6E-4 8.0E-4 8.4E-4 8.8E-4 9.2E-4 9.6E-4
-1 6 169.07.2 167.42
Inverse of temperature (K ) 8 190.398.4 190.98

Figure 6. Arrhenius relationship between the boron diffusion

coefficient and the process temperature 5. CONCLUSIONS
4.4 Prediction of total boride layer thickness with the In this work, the substrates made of EN-GJL-250 lamellar
regression model gray cast iron were pack-borided in the temperature range 800-
1000°C between 4 and 8 h. The formed boride layers on EN-
A full factorial design with two factors at three levels was GJL-250 lamellar gray cast iron were composed of FeB and
used to predict the total boride layers’ thicknesses depending Fe2B phases with a less pronounced saw-tooth morphology.
upon the boriding parameters (time and temperature) by means The XRD results indicated that Fe2B is the dominant phase in
of ANOVA analysis [26, 27]. Based on the experimental data, the boride layer in accordance with the SEM observations. The
Equation (14) was obtained as follows:
total boride layer thickness attained a value of 190.39 8.4 µm
during 8 h for 1000°C, while it was only 29.391.6 µm for 4
u (T , t ) = 816.31167 − 2.14797  T
h at 800°C.
−23.88917  t + 0.03812  T  t + Based on the integral diffusion model, the value of
0.00142  T 2 − 0.17500  t 2 activation energy for boron diffusion in EN-GJL-250 lamellar
gray cast iron was found to be 163.86 kJ mol -1 and compared
for 800 T 1000°C and 4 t 8 h (14) with the values of energy available in the literature.
Furthermore, an iso-thickness diagram yielding the total
where, t represents the time duration (h) and T the process boride layer thickness (FeB+ Fe2B) as a function of boriding
temperature in degree Celsius. parameters (time and temperature) was suggested based on the
Equation (14) can be used to get the iso-thickness diagram design of experiments. It could be used as a simple tool to
shown in Figure 7. select the optimum values of total boride layer thickness for a
This Figure allows selecting the optimum value of total practical use of EN-GJL-250 lamellar gray cast iron in the
boride layer thickness according to the practical utilization of industry. Finally, the experimental values of total boride layer
EN-GJL-250 lamellar gray cast iron. thickness were in agreement with the values given by the
Table 4 provides a comparison between the experimental regression model.
values of total boride layers’ thicknesses and the predicted As a prospect, this applied integral diffusion model can be
values using Equation (14) in the temperature range 800- used to investigate the boriding kinetics of any borided ferrous
1000°C. It is noticed that the predicted values of total boride alloys.

27
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