Applied Surface Science 285P (2013) 72–85

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Tribological behaviour and statistical experimental design of sintered

iron–copper based composites
Ileana Nicoleta Popescu a , Constantin Ghiţă b , Vasile Bratu a,∗ , Guillermo Palacios Navarro c
a
Valahia University of Targoviste, Faculty of Materials and Mechanics Engineering, 18-24 Unirii Boulevard, 130082, Targoviste, Romania
b
Valahia University of Targoviste, Faculty of Science and Arts, 18-24 Unirii Boulevard, 130082, Targoviste, Romania
c
University of Zaragoza, Department of Electronic Engineering and Communications, Zaragoza, Spain

a r t i c l e i n f o a b s t r a c t

Article history: The sintered iron–copper based composites for automotive brake pads have a complex composite com-
Received 12 April 2013 position and should have good physical, mechanical and tribological characteristics. In this paper, we
Received in revised form 30 July 2013 obtained frictional composites by Powder Metallurgy (P/M) technique and we have characterized them
Accepted 1 August 2013
by microstructural and tribological point of view. The morphology of raw powders was determined by
Available online 11 August 2013
SEM and the surfaces of obtained sintered friction materials were analyzed by ESEM, EDS elemental and
compo-images analyses. One lot of samples were tested on a “pin-on-disc” type wear machine under
Keywords:
dry sliding conditions, at applied load between 3.5 and 11.5 × 10−1 MPa and 12.5 and 16.9 m/s relative
Tribological characteristics
ESEM
speed in braking point at constant temperature. The other lot of samples were tested on an inertial test
EDS stand according to a methodology simulating the real conditions of dry friction, at a contact pressure of
X-ray maps and compo image of surface 2.5–3 MPa, at 300–1200 rpm. The most important characteristics required for sintered friction materials
friction materials are high and stable friction coefficient during breaking and also, for high durability in service, must have:
Statistical experimental design low wear, high corrosion resistance, high thermal conductivity, mechanical resistance and thermal stabil-
ity at elevated temperature. Because of the tribological characteristics importance (wear rate and friction
coefficient) of sintered iron–copper based composites, we predicted the tribological behaviour through
statistical analysis. For the first lot of samples, the response variables Yi (represented by the wear rate
and friction coefficient) have been correlated with x1 and x2 (the code value of applied load and relative
speed in braking points, respectively) using a linear factorial design approach. We obtained brake friction
materials with improved wear resistance characteristics and high and stable friction coefficients. It has
been shown, through experimental data and obtained linear regression equations, that the sintered com-
posites wear rate increases with increasing applied load and relative speed, but in the same conditions,
the frictional coefficients slowly decrease.
© 2013 Elsevier B.V. All rights reserved.

1. Introduction The brake friction materials have a complex composition that

The increasing consumer demand for low-cost performing and
non-polluting materials, with a favourable price/quality ratio,
has determined, in the past decades, development of exten-
sive researches in automotive brake friction industry. The efforts
include the development of ferrous (composites with iron based
matrix) and non-ferrous based materials such as copper, alu-
minium or carbon composites, as new candidates of brake friction
materials [1–6].
Friction materials are used for converting the kinetic energy of
the automotive to thermal energy (heat), resulting from two sur-
faces in contact of the brake pads and brake disc, which is absorbed
and dissipated by the materials [7].
∗ Corresponding author. Tel.: +40 245206106.
E-mail address: vasilebratu.uvt ro@yahoo.com (V. Bratu).
includes both metallic and non-metallic components. Also, brake
pads typically comprise the binders, the lubricating components
and frictional additives [7]. The purpose of a binder is to maintain
the brake pads’ structural integrity (to hold the components of a
brake pad together) under mechanical and thermal stresses. The
binders could be synthetic resins, metallic ingredients or mixture
of metallic and organic ingredients. The synthetic resin based fric-
tion materials is cheap to produce, but it has as a disadvantage that,
in high-energy braking applications (operating up to 370–450 ◦ C)
when the induced temperature can be high enough, the material
decomposes or breaks down. As a result, the friction coefficient with
the brake disc is compromised leading to decreasing road safety
[7,8]. In case of using metallic binders as iron, cooper, aluminium
and their alloys, we can improve the wear resistance, thermal dif-
fusivity and strength of the brake friction material. The lubricating
components such as graphite, molybdenum disulphide, etc. have
the objective to: (i) stabilize the developed friction coefficient

0169-4332/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2013.08.007
 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85
during braking, particularly at high temperatures, (ii) decrease
wear of counterparts and also (iii) increase grippe resistance
[1–14]. The frictional additives, such as oxides (Al2 O3 , SiO2 , ZrO2 ,
Mullite, and Spinel), nitrides (TiN and Si3 N4 ), carbides, (SiC, TiC,
B4 C, and VC), determine the frictional properties of the brake pads.
Also the frictional components increase and stabilize the fric-
tion coefficient values, respectively increase the wear resistance
[1–12,15]. Composites with iron or steel matrix and ceramic rein-
forcements used like friction materials bring new possibilities in the
production of wear resistant materials because they provide good
wear resistance and maintain friction effectiveness at elevated
temperature [7,11,15]. Iron could be alloyed with Cu, Cu–Sn–(Zn),
Ni, Mo, Al, Co, Mn, etc. for improving resistance of the metal-
lic matrix [7–11,15]. Cooper and Cu alloys are chosen mainly to
improve the thermal conductibility at the friction interface and for
sustaining the level of the coefficient of friction at elevated temper-
atures by producing copper oxides at the friction interface [1,8].
Aluminium or aluminium alloys are used in frictional materials
because of lightweight and good thermal diffusivity [12,16–18].
The proportion and granulation of these components, was and is
still the subject of numerous investigations in various countries
in order to achieve the optimal characteristics of brake friction
materials. The processing of brake friction materials is realized by
a diversity of methods [6–8,13–23] including powder metallurgy
(P/M) techniques. The P/M techniques give (i) a good uniformity
distribution of lubricated and frictional components in metallic
matrix, (ii) near net-shape parts fabrication, (iii) high productiv-
ity (iv) dimensional accuracy and (v) allows a good control of brake
friction require characteristics. Among the required market per-
formance criteria for brake pads materials, we mention [8]: (a)
maintaining a high and stable friction coefficient with the brake
disc, in various conditions, including at high temperatures; (b) very
good wear resistant material and implicit very good durability in
service; (c) good strength at elevated temperatures; (d) high ther-
mal conductivity; (e) high corrosion resistance; (f) smooth braking
assurance.
In this paper we obtained frictional composites by conventional
P/M technique and we have characterized them by microstructural
and tribological point of view.
2. Materials and compositional selection
The raw powders chosen for frictional materials were Fe
(reduced), Cu (electrolytic) as metallic ingredients, graphite and
MoS2 as solid lubricant, respectively, mullite and spinel as fric-
tional components, with a particles size situated up to 100 ␮m.
The raw powders selected must be non-polluting material from
compositional point of view and have required characteristics.
Using iron/steel based material in comparison with Cu-based
material improved strength, hardness, ductility and heat resis-
tance properties. Iron as a matrix of the automotive brake material
has been chosen due of its stability under higher temperatures
(1100 ◦ C), which imply very good tribological behaviour under
heavy duty dry operating conditions. The selection of copper as
alloying element gives additional strength of sintered steels (the
elemental copper at 1083 ◦ C promotes sintering and enhances the
strength of the steel) [10]. In order to improve cold and hot strength
of sintered friction materials a tight ratio between cooper and iron
was chosen. Generally for the friction sintered materials for auto-
motive brakes, the cooper ratio in the material is majority [3].
Graphite + MoS2 have the role to stabilize the developed friction
coefficient during braking, particularly at elevated temperatures.
Additions of graphite to Fe–Cu sintered steels are desirable because
the carbon promotes the formation of a pearlitic microstructure,
resulting in additional strength and hardness of steel [9].
73
The high proportion in lubricating components was chosen
due to (i) easy pressing of the mixture, at medium pressure of
500–600 MPa; (ii) improvement of sliding properties, by forming
a lubricant layer on the opposing counter friction material at speed
of 20–30 m/s [3,7,14].
The new chemical compositions (new proportion of compo-
nents) established after a number of preliminary tests [15] of
iron–copper based friction material (SFM1 and SFM2) samples
preparation and the chemical composition of a commercial brake
pad, used as reference material (RM) are presented in Table 1.
3. Materials and experimental procedure
3.1. Powder analysis
The following characteristics of powders were analyzed: (i) the
apparent density according to SR EN 23923-1: 1998 standards, (ii)
flow rate, in concordance with the standard method SR EN ISO
3953: 1998; (iii) particle size distribution, according with SR 13203-
94 and ISO 4497:1983; (iv) the morphology of powder particles
determined by scanning electronic microscopy (SEM).
3.2. Composite preparation
We used P/M as a technique for preparation of composites for
automotive brake pads because this technology allows us to obtain
sintered friction materials with a large variety of chemistry in
concordance with different conditions of solicitation. Before the
manufacturing of the composite, the oxides of iron copper pow-
ders were reduced in “Siemens–Plania” type furnace in presence
of H2 atmosphere at temperature near 980 ◦ C for iron and 280 ◦ C
for copper, during 60 min, in order to obtain reduced metallic pow-
ders. The ceramic powders were heated for 300–400 ◦ C, holding
120 min, for elimination of adsorbed gases, moisture and organic
contaminants.
The dosage of mixtures was made gravimetric and the elemen-
tal powder of the mixtures was dry blended using the Double
Cone Blender (10 kg capacity) at a rotation speed of 20 rpm, dur-
ing 6–8 h. The mixed homogenous powders were compacted at
room temperature in a double action hardened steel die with a
automate hydraulic press of 30 tone force, Meyer Type, at pres-
sure of 500–600 MPa. According to literature [23–25] there are a
diversity of process parameters (sintering temperature, sintering
time, and protective environment). For our experiments, the com-
pacts were sintered in a sintering furnace, Balzers type, at 1050 ◦ C
sintering temperature, 90 min holding time, in vacuum atmosphere
under a pressure of 0.1–0.3 mmHg, in limits mentioned of scientific
literature.
The composite processing flow-sheet is presented schematically
in Fig. 1.
3.3. Sintered friction material characterization
The obtained sintered SFM1, SFM2, composites and reference
material RM were analyzed from physical, mechanical, micro-
structural (SEM) and micro-compositional (SEM, EDS and X-ray
maps) point of view, according with specific techniques presented
in [26].
The quantitative X-ray microanalysis of obtained sintered
iron–copper based composite as frictional material was carried
out using the energy dispersive X-ray spectroscopy (EDS) of the
environmental scanning electron microscopy (ESEM), FEI XL-30
and FEG SEM Inspect F, FEI. The density of the sintered compos-
ites was measured by physical measurements and also using the
Archimedes method. The Brinell Hardness test was done according
ISO 4498/1 standardization.
74 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85

Table 1
Raw powders chemical composition (wt.%) of brake friction materials.

Friction material type Metallic binder Lubricant component Frictional components

Fe Cu Sn Graphite MoS2 Mullite (3Al2 O3 ·2SiO2 ) Spinel (MgAl2 O4 )

SFM1 24–30 21–25 – 18–22 4–8 Balanced

SFM2 30–35 20–30 – 13–17 5–7 Balanced
RM 30–32.5 30–32.5 2–3 9–11 4–6 Balanced −

The tribological (friction and wear) tests of sintered iron–copper
based composite for automotive brake pads were performed
using a “pin-on-disc” tribometers. One lot was tested with a tri-
bometer (with a grey cast iron of 300 HB as counterparts), on
10 mm × 10 mm × 7 mm samples, in dry friction conditions, applied
normal load between 0.35 and 1.15 MPa, during 15–20 min per
sample, at 12.5–16.9 m/s relative speed in braking points (sliding
distance between 8125 and 14733 m) and at constant tempera-
ture. The test machine consists of a balanced pendulum in which
is mounted the sample into a box. The sample rubs on a cast iron
disc and the disc is acted through the main body of a transmission
belt, by an electric motor of 1.4 kW power. The peripheral speed of
the disc can be varied by positioning the sample box (sample posi-
tion) at different distances from the axis of the machine through
a variable ratio transmission. The frictional force was determined
by measuring the angular movement (˛) of pendulum from the
vertical position (Fig. 2).
The correlation between applied pendulum weight (G) in Kg,
total length (L) in mm and the distance from the spindle axis to
pendulum test box (e) in mm is given by the relation.
F = L · G · sin ˛/e
It is known that:
 = F/N
where F is the frictional forces;  is the coefficient of friction and N
is the normal forces.
From Eqs. (1) and (2) result that the coefficient of friction is
determined by the relationship:
 = L · G · sin ˛/Ne (3)
The wear rate was measured, respectively, by height loss
(mm/h) and weight loss (g/cm2 h). The wear of the friction materials
was expressed by weight/height loss percent as:
W % = (W0 − W1 )/W0 · 100% (4)
where W0 and W1 are the weight/height of the specimens before
and after testing, respectively.
The other lot of samples were tested on an inertial test stand
according with Fermit S.A. methodology [15]. In this type of test-
ing the real conditions of dry friction of automotive brake pads
were simulated (cold and hot testing, grinding and endurance con-
ditions) on dry sliding wear conditions, at a contact pressure of
2.5–3 MPa, depending on braking parameters as: (i) number of bra-
king stops (25–500) and (ii) speed 300–1200 rpm. The temperature
during braking ranged between 75 and 350 ◦ C.
The dimensions of sintered friction samples of the second lot,
(1) for test samples on inertial stand, fixed on a metallic pad, were
2500 mm2 × 12 mm (Fig. 3).
3.4. Factorial design
(2)
Because of the tribological characteristics importance (wear rate
and friction coefficient) of sintered iron–copper based composites,
we predicted the tribological behaviour through statistical analysis
[27–30]. For that purpose, a factorial design of experiment of the
type Pn [30] was used in the present paper, for the testing sintered
frictional material from the first lot, in dry friction conditions. The
“n” corresponds to the number of factors and “P” stands for the
number of levels.

Fig. 2. Schematic diagram of the forces which activate during the wearing of sam-
Fig. 1. The P/M technology route of SFM1 and SFM2 materials for braking pads. ples (pin-on-disc).
 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85 75

Table 3
The average values concerning physical and mechanical characteristics of
iron–copper sintered composites for automotive brakes.

Sintered friction material Density, g/cm3 Hardness, HB

SFM1 3.8 16.5

SFM2 3.9 19.2
RM 3.6 11.8

graphite and MoS2 have the particles shape as flaws, especially

Fig. 3. Sintered friction materials (second lot), fixed on a metallic pad, for test sam-
ples on inertial stand.
In this design, n = 2 (i.e. applied load and relative speed in braking
point) and P = 2 (i.e. upper and lower level of each variable). Thus,
the minimum number of trial experiments to be conducted for each
material is four. If wear rate is represented by Y1 and Y2 (Y1 mea-
sured by height loss of material and Y2 measured by weight loss)
and friction coefficient is represented by Y3 , the linear regression
equation for these experiments could be written as:
Yi = bi0 + bi1x1 + bi2x2 + bi3x1x2 (5)
where bi0 is the response variable of wear rate and friction coef-
ficient, respectively, at the base level (i.e. at the applied load
7.45 × 10−1 MPa and relative speed in braking points 14.7 m/s); bi1
and bi2 are coefficients associated with each variable x1 (applied
load) and x2 (relative speed in braking point) and bi3 is interaction
coefficient between x1 and x2 , within the selected levels of each of
the variables.
The parameters of Eq. (5) have been estimated by the method
of least squares using a Excel programme package. The coefficients
were determined statistically using the Student criterion and the
accordance degree of the regression equations was verified with
the Fischer criterion. The mathematical model of wear behaviour
once established, the problem of the models optimization is to
determination of the mathematical function extreme [30].
4. Results and discussion
the molybdenum disulphide particles have the tendency of coales-
cence. The average values of apparent densities of the mixtures for
frictional materials were 1.39 g/cm3 for SFM1 powder mixture and
1.46 g/cm3 for SFM2 mixture. The physical and mechanical charac-
teristics (Brinell hardness and density) of the obtained composite
friction material, in comparison with reference material, are pre-
sented in Table 3.
The structure of iron–cooper composites, the ESEM, EDS anal-
ysis and X-ray mapping of the elements from SFM1 samples are
presented in Figs. 5–8.
The analyses were made on the surface of the frictional compos-
ite material, from different white and grey compact areas.
In Figs. 5 and 6 we can observe the components and elements
from the surface of sintered iron–copper based composite. The
microstructure and elemental analysis shows a basic mass formed
by iron and copper (white compact areas) as we observed in Fig. 5(a)
and (c), respectively and in Fig. 7(a) and (b). The mechanical inclu-
sions, especially mullite, spinel, are identified from X-ray mapping
(Al, O, Si, and Mg elements) and EDS elemental analysis (the propor-
tion of them), in Fig. 6, and we observed them from microstructural
point of view as light grey compact particles, Fig. 7(a) and (d),
respectively and Fig. 8. We can notice the graphite (C) as dark grey
compact particles in all ESEM microstructure and confirmed by
X-ray mapping (Ck) and EDS elemental analysis.
Due to the combined influences of powder mixtures compo-
nents, it is not possible to determine precisely the influence of each
component on the basic structure. The most pregnant structural
modifications are determined especially by the copper additives.
The equilibrium diagram of Fe–Cu shows that copper is liquid at
1083 ◦ C and can easily infiltrate between the Fe particles. There
is a partial diffusion in iron and, thus, the net is reinforced (liq-
uid copper ensures a better connection between alloy particles
and resulted that by action of capillary force). The above described
phenomena can take place at lower temperatures than the melting
points of copper, due to the iron-solubility of 8.5% at 1094 ◦ C and
of 4.5% at 833 ◦ C.

4.1. Powders and frictional material characteristics 4.2. Influence of braking parameters on friction coefficients

In Table 2 the physical characteristics of raw powders are pre-
sented and in Fig. 4 the morphology of elemental powders is
presented.
We observed in Fig. 4 that iron powders have spherical and
egg-shape morphology, the dendrites particle shape is specific for
electrolytic copper powders, the mullite has irregular form and the
The braking parameters used were number of braking stops
(25–500) and speed of 300–1200 rpm.
The friction coefficient variation depending on temperature, the
speed and number of brakes for test samples on the inertial stand
is presented in Fig. 9. The values obtained by simulating the condi-
tions of real friction, on the inertial test-stand, were brought close

Table 2
The physical characteristics of raw powders.

Powder type Particle size distribution, % Apparent density, g/cm3 Flow rate, s/50 g

>100 ␮m 100–63 ␮m 63–50 ␮m 50–40 ␮m <40 ␮m

Fe 23.4 28.1 28.3 11.9 8.3 2.55 39

Cu – 54.4 24.7 12.2 8.7 1.34 41.2
Graphite – 69.8 20.4 5.1 4.7 0.49 Not flowing
MoS2 – 44 29 12.5 14.5 0.43 Not flowing
Mullite (3Al2 O3 .2SiO2 ) – – 23 42 35 0.72 Not flowing
Spinel (MgAl2 O4 ) – – 36 32.1 31.9 0.81 Not flowing
76 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85
Fig. 4. Morphology of (a) Fe powder (1000×), (b) Cu powder (1000×), (c) graphite powder (3000×), (d) MoS2 powder (2000×) and (e) Mullite powder (1000×).
to the maximal allowed amount of 0.5–0.6 at the cold testing, under
speed increasing conditions (Fig. 9(b)).
4.3. Linear regression equations
The upper level and lower level of each variable along with their
code values used in these investigations are presented in Table 4.
Experiment planning matrix, the values of individual variables with
their wear rate and friction coefficient response in each trial tested
for SFM1, SFM2 and RM samples (results of random experiments
along with theoretical value) are presented in Tables 5–7 (where
y1 , y2 and y3 are the experimental values and y1calc , y2calc and y3calc
are the calculated ones).
The calculation of dispersal reproducibility for y1 , y2 – wear rate
and y3 – friction coefficient was made in cases in which the values
of Z1 xZ2 have the base level.
The four parallel experiences are presented in Table 8, where u is
the number of experience; n is the number of parallel experiments
 is the arithmetic average of obtained results for k = 1, 2 or
(n = 4); yuk
3, the type of variable response; v2 is the degrees of freedom at n − 1.
The calculation of reproducibility dispersion is based on the Eq.
(6):
n
u=1
yu
S02 = (6)
n−1
Result for variable response Y1 is S02 = 0.00071875, for variable
response Y2 is S02 = 0.000583 and for variable response Y3 is S02 =
0.000475, for sample SFM1.
The coefficients were determined statistically using the Student
criterion and the accordance degree of the regression equations
was verified with the Fischer criterion.
 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85 77

Fig. 5. The structure of iron–copper based composites (SFM1): (a) microstructure ESEM, (b) EDS elemental analysis, and (c) compo image of samples, 500× magnification.

Thus, the coefficients of each variable from Eq. (5) were calcu- Y2,SFM1 = 0.535 + 0.101x1 + 0.037x2 − 0.0325x1 x2 (10)
lated with Eqs. (7) and (8).
n
x · yu
u=1 iu Y3,SFM1 = 0.454 − 0.083x1 − 0.0138x1 x2 (11)
bi = , for linear effects, (7)
(xiu )2
where Y1,SFM1 , Y2,SFM1 represent the response variables (wear rate
n of SFM1 samples measured by height loss and weight loss, respec-
x
u=1 iu
· xju · yu
bij = , for interaction effects, (8) tively; Y3,SFM1 represents the friction coefficients of SFM1).
(xiu · xju )2 The dispersion in determination of coefficients is calculated with
relations:
By introducing the calculated coefficients (7) and (8) in Eq. (5)
the following regression equations result: S02

2
Sbi =  and Sbi = 2
Sbi (12)
Y1,SFM1 = 1.37 + 0.45x1 + 0.07x2 + 0.03x1 x2 (9) x
j=1 ij

Table 4
Levels of each factor and their coded values.

SI. no. Variables

Factor levels Z1 – Applied load (×10−1 MPa) Z2 – Relative speed in braking point (m/s)

Coded values x1 x2
1 Upper level (+1) 11.5 16.9
2 Base level, Z10 (0) 7.5 14.7
3 Lower level (−1) 3.5 12.5
Variation interval, Z1 4 2.2
78 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85

Fig. 6. The X-ray mapping of the elements (a) and EDS elemental analysis of the frictional sintered iron–copper based material (SFM1) (b).

Result for variable response Y1 , Sbi = 0.013404757, for vari- from zero; therefore, the term comprising interaction, or another
able response Y2 , Sbi = 0.012076, and variable response Y3 , factor from equation, will be neglected. In this case, the calculated
Sbi = 0.010897. (predicted) linear model of the processes will be: for the wear, Eqs.
The Student criterion t0.05;4 = 2.776 and bi – confidence inter- (13) and (14) and friction coefficients Eq. (15), respectively, of the
val is bi = 2.776·Sbi . friction material SFM1 can be expressed as follows:
After calculation, result for variable response Y1,SFM1 ,
bi = 0.0372, for variable response Y2,SFM1 , bi = 0.0335 and Y1,SFM1 = 1.37 + 0.45x1 + 0.07x2 (13)
for variable response  , bi = 0.0302. But according to [30],
   Y3,SFM1 Y2,SFM1 = 0.535 + 0.101x1 + 0.037x2 (14)
if the relation  b0  , b1 bi is not accomplished, result for the
calculated value of the coefficient is not statistically different Y3,SFM1 = 0.454 − 0.083x1 (15)
 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85 79

Fig. 7. The microstructure ESEM (SFM1), 500× maginification (a) and EDS elemental analysis taken from the compact white phase (b), from small white particles (c) and
light grey compact particles (d).

In this equation x1 and x2 are coded values of the factors, which

Verification of the model concordance: The computation of dis-
are calculated from natural values, with the formula: 2
persion produced by the linear equations of regression Sconc is
zi − zio presented in Table 9, where
xi = (16)
zi
Substituting in Eq. (16), the values from Table 4, we will  
z −7.5 z −14.7 yu = yexp − y (18)
obtain(17)x1 = 1 4 and x1 = 2 2.2

Fig. 8. The microstructure ESEM (SFM1), 2000× maginification (a) and EDS elemental analysis taken from the light grey compact particles (b).
80 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85

Fig. 9. The variation friction coefficient depending on temperature, speed and number of brakes for test samples on the inertial stand in: grinding (a), cold testing (b), hot
testing (c), recovery testing (d), and endurance conditions (e).

and
Introducing the values of yu from Table 9 in Eq. (19) and then

n
2 introducing the resulted Sconc2 and values of reproducibility disper-
(yu ) 2
sion S0 in Eq. (20) result that the calculated Fisher is Fc1 = 5.01 (for
2 u=1
Sconc = (19) variable response Y1 ); Fc2 = 7.307 (for variable response Y2 ) and
1
Fc3 = 5.05 (for variable response Y3 ).
From tabulated values of optimization book annexes in [29]
The calculated Fischer criterion is:
resulted in F˛ , 1 , 2 = F0.05,1.3 = 10.13. Because Fci < F0.05,1.3 , i = 1.2
2
Sconc or 3 ⇒. The linear models for all three variables of sin-
Fc = (20) tered friction material SFM1 are in concordance with analyzed
S02
process.
Table 5
The values of individual variables with their wear rate and friction coefficient response in each trial tested for SFM1 samples.

Trial no. Applied load Relative Wear rate Calculated wear Wear rate Calculated wear Friction Calculated friction
(×10−1 MPa) speed (m/s) (mm/h) rate (mm/h) (g/cm2 h) rate (g/cm2 h) coefficient coefficient
x0 x1 x2 x1 x2 y1 y1calc y2 y2calc y3 y3calc

1 (+1) 11.5 (+1) 16.9 (+1) (+1) 1.92 1.89 0.64 0.673 0.337 0.3709
2 (+1) 3.5 (−1) 16.9 (+1) (−1) 0.96 0.99 0.503 0.471 0.53 0.537
3 (+1) 11.5 (+1) 12.5 (−1) (−1) 1.72 1.75 0.631 0.599 0.405 0.371
4 (+1) 3.5 (−1) 12.5 (−1) (+1) 0.88 0.85 0.364 0.397 0.543 0.537

I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85

Table 6
The values of individual variables with their wear and friction coefficient response in each trial tested for SFM2 samples.

Trial no. Applied load Relative Wear rate Calculated wear Wear rate Calculated wear Friction Calculated friction
(×10−1 MPa) speed (m/s) (mm/h) rate (mm/h) (g/cm2 h) rate (g/cm2 h) coefficient coefficient
x0 x1 x2 x1 x2 y1 y1calc y2 y2calc y3 y3calc

1 (+1) 11.5 (+1) 16.9 (+1) (+1) 1.4 1.424 0.52 0.491 0.295 0.295
2 (+1) 3.5 (−1) 16.9 (+1) (−1) 1.1 1.078 0.29 0.321 0.395 0.395
3 (+1) 11.5 (+1) 12.5 (−1) (−1) 1.25 1.228 0.368 0.399 0.32 0.32
4 (+1) 3.5 (−1) 12.5 (−1) (+1) 0.86 0.882 0.26 0.229 0.46 0.46

81
82 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85

In the same way the 4 parallel experiences for variable response

Calculated friction
for SFM2 and RM samples were calculated and the following lin-
ear regression equations (21)–(26) were obtained which are also in
concordance with analyzed process:

coefficient
Y1,SFM2 = 1.153 + 0.173x1 + 0.098x2 (21)

0.353
0.529
0.287
0.463
y3calc
Y2,SFM2 = 0.359 + 0.085x1 + 0.046x2 (22)

Y3,SFM2 = 0.368 − 0.06x1 (23)

coefficient
Friction

0.39 Respectively:
0.49
0.25
0.5
y3

Y1,MR = 1.383 + 0.113x1 + 0.063x2 (24)

Y2,MR = 0.538 + 0.203x1 − 0.073x1 x2 (25)

Calculated wear
rate (g/cm2 h)

Y3,MR = 0.408 − 0.088x1 (26)

From Eq. (21) deduced that the height loss increase with
0.723
0.317
0.759
0.353
y2calc

increasing of applied load, relative speed in braking point

and no depends with interaction of those variables. Eq. (22)
showed that the weight loss of SFM2 material depends direct
proportional with applied load and no depend of relative
speed (witch means that regardless of automotive speed, bra-
Wear rate
(g/cm2 h)

king to accomplish in safe condition depending on pressing

0.65
0.39
0.83
0.28

force.
y2

Eq. (23) showed that the friction coefficient of SFM2 material

increased with increased all the variables inclusive with interaction
of them.
We noticed that wear rate measured by height loss for
Calculated wear

reference material (Y1,MR ), weight loss of material increased

rate (mm/h)

with increasing of applied load and relative speed in accor-

The values of individual variables with their wear and friction coefficient response in each trial tested for RM samples.

dance with Eq. (24) and wear rate measured by weight loss
1.559
1.333
1.433
1.207
y1calc

(Y2,MR ) increased with increasing of applied load and with

decreasing of interaction of applied load and relative speed, in
accordance with Eq. (25). Eq. (26) shows that the friction coef-
ficient of reference material decreases with increasing of applied
Wear rate

load.
(mm/h)

The calculated (theoretical) values of wear rate and friction coef-

1.56
1.33
1.43
1.21

ficient were obtained replacing in Eqs. (13)–(15) and (21)–(26) the

y1

coded values corresponding of each trial for all types of material

tested.
Through the statistical experimental design presented before,
(−1)
(−1)
x1 x2

(+1)

(+1)

we can describe the evolution of tribological characteristics of sin-

tered frictions samples (SFM1, SFM2 and RM) at different applied
load, different relative speed and constant temperature.
Thus, for comparison, the statistical results of response vari-
speed (m/s)

12.5 (−1)
12.5 (−1)

ables, represented by wear rates and friction coefficients, and the

16.9 (+1)
16.9 (+1)
Relative

experimental data of them, are presented in Figs. 10 and 11.

For better understanding of tribological behaviour of the
x2

three types of samples depending on all factors: applied load

(3.5 × 10−1 MPa and 11.5 × 10−1 MPa) and relative speed (16.9 m/s
and 12.5 m/s), we presented all the results of experimental and cal-
(×10−1 MPa)
Applied load

culated data in Fig. 11. From these figures we observed that the
3.5 (−1)

3.5 (−1)
11.5 (+1)

11.5 (+1)

difference between experimental values and the calculated one are

the majority ±3–6%.
x1

Comparing the wear rates of SFM1 and SFM2 samples with ref-
erence material RM we noticed that values for all materials are
not great; in addition at maximum values of applied load and rel-
(+1)
(+1)
(+1)
(+1)

ative speed, wear rate measured by loosing weight per hour is

x0

0.64 g/cm2 h for SFM1, 0.32 g/cm2 h for SFM2, 0.65 g/cm2 h for MR,
and wear rate measured by loosing height per hour is 1.92 mm/h
for SFM1, 1.4 mm/h for SFM2 and 1.56 mm/h for RM. We have seen
Trial no.

that the lowest values of wear rate have friction materials SFM2,
Table 7

which have a lowest value in comparison with the reference mate-

1
2
3
4

rial. The values of friction coefficients at maximum solicitations are:

 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85 83

Table 8
The 4 parallel experiences for variable response for SFM1 sample.
     
    2     2     2
No. y ’ u1 yu1 = y u1 − yu1 (yu1 ) y ’ u2 yu2 = y u2 − yu2 (yu2 ) y’3 yu3 = y u3 − yu3 (yu3 ) 2

1 1.52 0.0275 0.00075625 0.51 0.01 0.0001 0.47 0.035 0.001225 3

2 1.6 0.0525 0.00275625 0.48 0.04 0.0016 0.42 0.015 0.000225 3
3 1.64 0.0925 0.00855625 0.59 0.07 0.0049 0.47 0.035 0.001225 3
4 1.43 0.1175 0.01380625 0.5 0.02 0.0004 0.38 0.055 0.003025 3

Table 9
The computation of dispersion Sconc
2
produced by the linear equation of regression, for SFM1 sample.

No. y1exp ȳ1 y1u (y1u )2 y2exp ȳ2 y2u (y2u )2 y3exp ȳ3 y3u (y3u )2 1 = N − k

1 1.92 1.89 0.03 0.0009 0.64 0.673 0.033 0.001089 0.337 0.371 0.034 0.001156 1
2 0.96 0.99 0.03 0.0009 0.503 0.471 0.032 0.001024 0.53 0.537 0.007 0.000049 1
3 1.72 1.75 0.03 0.0009 0.631 0.599 0.032 0.001024 0.405 0.371 0.034 0.001156 1
4 0.88 0.85 0.03 0.0009 0.364 0.397 0.033 0.001089 0.543 0.537 0.006 0.000036 1

0.337 for SFM1, 0.36 for SFM2, 0.39 for MR respectively. We noticed
that SFM1 has a constant and higher value of friction coefficient;
this value is closer to a coefficient of friction value of MR mate-
rial. From Figs. 10 and 11, we can see that the values of friction
coefficients have a low decrease with increasing of strains (load
and speed), decreasing from 0.543 to 0.337 for SFM1, from 0.46
to 0.295for SFM2, from 0.5 to 0.39 for RM (maximum value was
obtained for applied load of 3.5 × 10−1 MPa and 16.9 m/s speed);
all values of frictional coefficients are in admitted domain (0.5–0.3)
for automobile friction materials.
From statically point of view, after we analyzed Eqs. (13)–(15)
for SFM1 sintered friction material, Eqs. (21)–(23) for SFM2 sin-
tered friction material and Eqs. (24)–(26) for reference material RM
respectively were found them “in accordance” on the basis of the
Fischer criterion which means that the model is good and supports
the reproducibility of the trial experiments.

Fig. 10. The experimental and statistical calculated values of response variables: (a) wear rates of samples as a function of applied load, at constant speed (16.9 m/s), (b)
friction coefficients of samples as a function of applied load, at constant speed (16.9 m/s), (c) wear rates of samples as a function of applied load, at constant speed (12.5 m/s);
(d) friction coefficients of samples as a function of applied load, at constant speed (12.5 m/s).
84 I.N. Popescu et al. / Applied Surface Science 285P (2013) 72–85
Fig. 11. The experimental and calculated values of wear rate and friction coefficient respectively of all three types of materials as a function of applied load (3.5, 11.5 × 10−1 MPa,
respectively), for relative speed (a) 16.9 m/s and (b) 12.5 m/s.
5. Conclusions
We obtained a sintered friction iron–copper based material,
with new chemical compositions and proportion of components
(SFM1 and SFM2 samples) and non-polluting constituents (ecolog-
ically friendly). The chosen composition and proportion of these
components ensured good physical and mechanical characteris-
tics, confirmed also by the morphological and microcompositional
investigation (uniform distribution of constituents and good adhe-
sion between them, due to changes occurring during liquid phase
sintering in the Fe–Cu system).
We established after different conditions of tribological tests,
including the tests on inertial stand (inertia dynamometer) which
simulate the real conditions of dry friction, that the obtained fric-
tional materials for braking pad have:
(i) high and stable friction coefficients (0.3–0.5), according to the
requirements imposed by brake pads materials for automotive
application (Fig. 9);
(ii) high durability of SFM2 materials in comparison with RM and
SFM1 samples; the values of wear rate, in the same experi-
mental conditions for SFM2 is maximum 25% lower than RM
(Figs. 10 and 11).
(iii) increase of applied load or increase of the relative speed in
braking points induces moderate increase of wear rate and
slow decrease of the frictional coefficients of the composites
(shown through experimental data and obtained linear regres-
sion equations in Figs. 9–11).
Acknowledgements
The authors are grateful to the Metallurgical Research Institute
Bucharest and BIOMAT Research Centre, Bucharest for providing
equipments and also thank Full Professor Ph.D. Dionezie Bojin from
Electron Microscopy Laboratory, Science and Engineering Faculty,
POLITEHNICA University of Bucharest for advice and support.
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