Valorization of Marine Sediments in a

Proteinic Biopolymer: Modeling of the

Mechanical Behavior

I. Zarrad, M. Jeridi, N. Montrelay,

R. M. Dheilly, J. Houesson, J. Bouaziz,
M. Queneudec & K. Saï

Journal of Polymers and the

Environment
formerly: `Journal of Environmental
Polymer Degradation'

ISSN 1566-2543

J Polym Environ
DOI 10.1007/s10924-014-0700-9

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 Author's personal copy
J Polym Environ
DOI 10.1007/s10924-014-0700-9
ORIGINAL PAPER
Valorization of Marine Sediments in a Proteinic Biopolymer:
Modeling of the Mechanical Behavior
I. Zarrad • M. Jeridi • N. Montrelay •
R. M. Dheilly • J. Houesson • J. Bouaziz •
M. Queneudec • K. Saı̈
 Springer Science+Business Media New York 2014
Abstract Biocomposites, which consist of renewable
resources like proteins, have been extensively investigated.
However, studies on the combination of marine sediments
and proteinic biopolymer have not been conducted yet. In
this work, marine sediments were added to the matrix in
proportions ranging from 0 to 20 %. The mechanical
properties in terms of tensile, flexural and compressive
strength tests were investigated. Thermogravimetric ana-
lysis were also used to assess the thermal stability of the
produced composites. The hemoglobin marine sediments
(HESM) may be dedicated to ground coating or to wall
covering, it is then necessary to perform a preliminary
structure analysis. A multi-phase mechanical model able to
reproduce the compressive behavior of the HESM is
developed in order to simulate the HESM coating at dif-
ferent marine sediments ratios and different strain rates.
The incorporation of sediments increases the stiffness of
the material and improves the compressive properties of
the composite.
Keywords Biocomposite  Marine sediments 
Hemoglobin of beef protein  Multi-phase model
I. Zarrad  J. Bouaziz
LCI, Ecole Nationale d’Ingénieurs de Sfax, 1173 Sfax, BP,
Tunisia
M. Jeridi  K. Saı̈ (&)
UGPMM, Ecole Nationale d’Ingénieurs de Sfax, 1173 Sfax, BP,
Tunisia
e-mail: kacemsai@yahoo.fr
N. Montrelay  R. M. Dheilly  J. Houesson  M. Queneudec
EPROAD (EA3669), Université de Picardie Jules Verne-7, rue
du Moulin Neuf, 80039 Amiens Cedex 1, France
Introduction
The research and development of biological material have
seen an increased interest during the two last decades. These
eco-materials are designed to replace the petroleum-based
polymers which have become more and more scarce and
will be more expensive. Biopolymers can be derived from
non petroleum sources like polysaccharides, starch, cellu-
lose pectins and proteins [1] or chemically synthesized from
natural monomers such as poly lactic acid [2]. A non-
exhaustive list of researches, devoted to biopolymers and
mainly to those derived from vegetable proteins such as soy
protein, was studied in the works [3–5]. The present work is
devoted to the investigation of a biopolymer newly devel-
oped by the IMaP team from EPROAD and has already
been patented [6]. Marine sediments (SM), as solid wastes,
can be added to this biopolymer in order to be valorized.
Several studies which were conducted for their valorization
in civil engineering applications can be cited as follows.
Tran [7] has valorized marine and river sediments designed
for road construction. Brakni [8] has investigated artificial
aggregates elaborated from marine sediments devoted to
coastal engineering. In addition, marine sediments can play
the role of a mineral filler thanks to their clay composition.
On the other hand, inorganic fillers are often incorporated in
bio-polymers to improve their thermal stability and even-
tually their mechanical properties [9–11]. According to the
authors’ knowledge, the biocomposite HESM has not yet
been investigated in the literature. The main goal of the
present paper is to reveal the effect of the incorporation of
marine sediments in proteinic biopolymer on the thermal
characteristics and mechanical properties of the composite.
With the HESM being used for ground coating or to wall
covering, it is then necessary to perform a preliminary
structure analysis. It will be shown that flexural and tensile
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behaviors are elastic brittle, whereas promising ductile Table 1 Tensile properties of the HESM biocomposite for different
behavior is noticeable under compressive loading. A SM ratios
mechanical model able to reproduce the compressive SM Cross Young’s Tensile Elongation at
behavior of the HESM is developed in order to simulate the ratio head- modulus (MPa) strength break (%)
HESM coating using the finite element (FE) method. This (%) speed (MPa)
(mm/min)
paper is organized in the following manner: in ‘‘Experi-
mental Results’’ section, experimental data on HESM bio- 0 2 1,600 ± 61 13.19 ± 2.3 1.05 ± 0.3
composite are provided. In this section, in addition to the 20 1,700 ± 240 15.88 ± 2.33 1.08 ± 0.29
thermogravimetric analysis, the compressive, tensile and 100 1,620 ± 303 9.86 ± 2.92 0.63 ± 0.28
bending strengths are discussed. In ‘‘Modelling’’ section, 5 2 1,450 ± 164 8.14 ± 2.52 0.66 ± 0.19
the mechanical model formulation devoted to the descrip- 20 1,780 ± 237 6.50 ± 1.60 0.46 ± 0.15
tion of the HESM behavior is shown in detail. Based on the 100 1,750 ± 334.51 4.35 ± 1.09 0.23 ± 0.08
experimental results related to compressive tests at different 15 2 1,580 ± 125 7.04 ± 1.71 0.55 ± 0.17
SM ratios and different strain rates, the identification of the 20 2,100 ± 113.13 8.47 ± 0.12 0.46 ± 0.033
model parameters is shown in ‘‘Results’’ section followed 100 1,610 ± 190.175 5.38 ± 2.42 0.32 ± 0.20
by the presentation of the numerical results. A FE analysis 20 2 2,120 ± 296 3.21 ± 1.27 0.25 ± 0.04
of the case study of HESM coating is finally investigated.

Experimental Results
Raw Materials
In this study, the protein used is an atomized hemoglobin
beef provided by the French company ‘‘VAPRAN’’ and
commercialized under the name ‘‘Vepro 95 BHF.’’ with a
bulk density of 1:37 g/cm3 . The marine sediments used in
this work are dredged in the area named ‘‘Naval Repair’’ in
the port of Dunkirk (France). Their absolute bulk density is
2:78 g/cm3 . Particle size analysis of sediments was carried
out by a laser particle type ‘‘Fritsch Analysette 22 Micro
Tec’’ which allows to identify particles in the range of 0.08
to 2,000 lm. Sediments composed mainly of silty materi-
als have a maximum grain boundary up to 300 lm.
Preparation of Biocomposites
The material investigated herein is a biocomposite. The
matrix has been elaborated according to the patent [6].
Mineral fillers have been introduced in the biocomposite by
a mass substitution of the matrix with mass fractions of 0,
5, 15 and 20 % and the whole mixture is mixed for 90 s.
The powder mixture is subjected to a pre-molding and
transferred to a metal frame to be subjected to thermo-
compression. The prepared mixture is poured into a cube of
10 cm in side and compacted by a punch. Finally, the
square plate is introduced into a thermo-compression-
machine (MIB HYDRO) with a capacity of 35 tonnes. The
mixture is then submitted to a load of 80 kN for 120 s
followed by a load of 128 kN for 240 s at a temperature of
70  C.
Mechanical Testing
• Tensile tests recommended by the ISO 527-1 norm
were conducted on a SHIMADZU AGX tensile
machine with a maximal load of 10 kN. This measuring
device was equipped with an extensometer type
SSG50-10 SHIMADZU. X. Trapezium software was
used for the control of the machine and data acquisi-
tion. Tensile tests were performed at three cross-head
speeds of 2, 20 and 100 mm/min. The variation of the
Young’s modulus, tensile strength and elongation at
break with the substitution percentage of SM are shown
in Table 1 and illustrated in Fig. 1a, b. The substitution
of the marine sediments slightly enhances the Young’s
modulus but it decreases the tensile strength of the
composite, thereby not giving a reinforcing effect of the
marine sediments in the matrix. The plummeted
strength is due to the insufficient interaction and the
weak chemical bonds between the matrix and the sed-
iments. Indeed, and in addition to the incompatibility
between the organic and inorganic phases [12], the
mineral fillers contain halite that crystallizes and
inhibits the adhesion between the matrix hemoglobin
(HE) and the mineral fillers.
• Three point bending tests in conformity with ISO
14125 norm were performed using the same machine
and acquisition system as for the tensile tests with a
constant cross-head speed of 3 mm/min. Trends of
flexural modulus are almost identical to those of tensile
modulus. However the flexural strength was reduced
compared to pure biocomposite but it stabilized starting
from 5 % of marine sediment ratio (Table 2, Fig. 1c, d).
Fillers have no effect on the flexural strength because of
the poor adhesion or bonding at the interface between

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Fig. 1 Mechanical properties of 25

2500

tensile strength(MPa)
tensile modulus(MPa)
the HESM biocomposite for
different SM ratios, a tensile 2000 20
elastic modulus, b tensile
strength, c flexure elastic 1500 15
modulus, d flexure strength,
e compressive elastic modulus, 1000 10
f compressive yield stress
500 5

0 0
0 5 10 15 20 25 0 5 10 15 20 25
SM% SM%
(a) (b)
2000 40
flexure modulus(MPa)

flexure strength(MPa)
1500 30

1000 20

500 10

0 0
0 5 10 15 20 25 0 5 10 15 20 25
SM% SM%
(c) (d)
compressive yield stress(MPa)
compressive modulus(MPa)

1500 50

40
1000
30

20
500
10

0 0
0 5 10 15 20 25 0 5 10 15 20 25
SM% SM%
(e) (f)

the matrix (organic) and the marine sediment inorganic Table 2 Flexural properties of the HESM biocomposite for different
particles. It can also be explained by the incompatibility SM ratios
between the organic and inorganic phases [12].
SM ratio Cross head-speed Fexural modulus Flexural
• Compressive tests were conducted on a WDW-10E (%) (mm/min) (MPa) strength (MPa)
Microcomputer–controlled electronic universal testing
machine with a maximal load of 10 kN. A WinWdw 0 3 1,402 ± 110 30.61 ± 4.24
Electonic universal testing machine and a control 5 3 1,625 ± 41.12 19.16 ± 1.3
system software were used to control the machine and 15 3 1,619 ± 131.97 19.19 ± 1.21
for data acquisition. Cross-head speeds of 3, 30 and 20 3 1,805 ± 55 16.47 ± 1.22
100 mm/min were selected. Figure 1e, f illustrate the
variation of the compressive Young’s modulus and the increases linearly with the marine sediment ratios.
compressive strength with the different marine sedi- Indeed, the vertical load exerted is supported by the
ment ratios. It can be seen that the compressive strength matrix and the hardness of the particles [13] even if

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Table 3 Compressive properties of the HESM biocomposite for 10

different SM ratios 0%SM
0
5%SM
SM ratio Speed Compressive Compressive yield -10 15%SM
(%) (mm/min) modulus (MPa) stress (MPa)

weight loss(%)
-20

0 3 667.11 ± 61 32 ± 2.82 -30

30 666.69 ± 0.02 40.88 ± 2.92 -40

100 729.21 ± 0.02 39.40 ± 1.66 -50

5 3 773.80 ± 84 32.55 ± 1.25 -60
30 1,055.55 ± 78 43.5 ± 3.53 -70
100 1,388.88 ± 392 47.25 ± 3.34 -80
15 3 953.79 ± 45 38.66 ± 4.71 -90
30 1,275.25 ± 379 42.22 ± 6.54 0 100 200 300 400 500 600 700 800

100 909 ± 0.007 58.45 ± 2.77 Temperature(◦ C)

20 3 954.54 ± 64.28 36.43 ± 0.32
Fig. 2 Thermogravimetric analysis of the HESM 0 %, HESM 5 %,
HESM 15 % biocomposites

there is no adhesion between them, which is not the
case of the tensile test where the stress exerted is
entirely supported by the matrix. It can also be inferred
that the HESM 20 % has a better compressive strength
compared to the composites with other percentages.
However, because of the poor tensile properties, the
mechanical modeling of the compressive behavior will
be restricted to HESM 0, 5 and 15 % (Table 3).
loss is 54 % instead of 64.6 % which shows that the
thermal stability of the biocomposite was improved com-
pared to HESM 0 % and HESM 5 %. Such thermal sta-
bility improvement for a polymer clay composite has been
reported for instance in [9, 14]. In other words, the deg-
radation of the biocomposite improved significantly with
the addition of 15 % SM (Fig. 3).

Thermogravimetric Analysis Modelling

Thermogravimetric analysis allows the recording of the
change in mass in relationship to the temperature cycle.
Thermogravimetric results were obtained under a helium
flow at 80 ml/min in a temperature range from 25 to
800  C, at a rate of 10  C/min, on a SETARAM Ligne 96
TGA apparatus. The thermal degradation behavior of the
HESM 0 %, HESM 5 % and HESM 15 % biocomposites
were investigated. The Thermograms are shown in Fig. 2.
As it can be seen, three regions of weight loss can be
distinguished with the increase of temperature. The weight
loss, for the polymer matrix (HESM 0 %) of about 20.4 %
in the temperature range of 25–110  C was attributed to the
adsorbed ethanol. The degradation of the biopolymer
matrix occurs in two steps with a weight loss of 15.2 and
40.3 % respectively. For the biocomposite containing 5 %
of SM, there are three weight losses: 19.30, 14.13 and
38.23 %. The total weight loss decreases compared to
HESM 0 %. The addition of 5 % SM does not have a great
effect on the thermal stability since a total weight loss of
71.7 % was found instead of the expected value of 72 %
(deduced by linear interpolation based on the total weight
losses at 100 %). On the contrary, the addition of 15 % SM
in the biopolymer reduces the three weight losses to 11.23,
5.80 and 37.91 % respectively. In this case, the total weight
The following notations are adopted for the description of
the constitutive equations of the material behavior:
• x denotes a single scalar,
• denotes a second order rank tensor,
• denotes a fourth order rank tensor,
• x_ is the derivative of x with respect to the time,
• denotes the tensor product contracted over one
indices of and .
The proposed model devoted to describe the mechanical
behavior of the HESM should:
• take the volume fraction substitution of the marine
sediment into account,
• account for the rate sensitivity of the material,
• provide local information such as, plastic strains and
stresses on the phases level.
The multi-phase model type is a good candidate to describe
this behavior. The proposed model belongs to a large class
of models known as the multi-mechanism (MM) model
type. The first version of the MM model, developed in the
general thermodynamical framework which in itself was
developed by Germain et al. [15], has been proposed by
Cailletaud and Saı̈ [16]. Several improvements of this

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(a) (b)
(c) (d)
(e) (f)
(g) (h)
Fig. 3 Photos of the biocomposite HESM with different contents of
marine sediments before and after compressive tests, a 0 % SM
(before), b 0 % SM (after), c 5 % SM (before), d 5 % SM (after),
e 15 % SM (before), f 15 % SM (after), g 20 % SM (before), h 20 %
SM (after)
model have been performed successively in [17–24] among
others. A review of these mechanical models can be found
in [23]. Since HESM consists of an HE phase and an SM
phase, the MM model is a good approach to model the
mechanical behavior of the HESM composite while taking
into account the influence of the SM volume fraction in the
HE phase. Moreover, the MM model is selected to preserve
the possibility to separate the two different behaviors in the
constitutive equations.
The use of a finite strain formulation through updated
lagrangian formalisms is needed to model the large-strain
deformation of the studied HESM composite. The material
behavior is based on Green-Naghdi transformation of the
stress-strain problem into an ‘‘equivalent material referen-
tial’’. This kind of formulation can be applied to materials
with tensorial internal variables without modifying the
local evolution rules [25]. The model is described by:
ð1Þ
where is the deformation gradient, is the rate of
deformation, is the stretch rate and is the rotation rate.
The stretch rate tensor is transported into a local rotated
referential following the expression:
ð2Þ
where the rotation tensor is determined by the polar
decomposition of the deformation gradient . and
describe a pure rotation and a pure stretch tensor respec-
tively. The integrated strain tensor is decomposed into both
elastic and inelastic parts. Thanks to updated lagrangian for-
mulation, constitutive relations can be expressed as in the small
strain hypothesis. Therefore, dealing with the elastic strain
tensor is equivalent to a hypoelastic formulation in agreement
with a Green-Naghdi stress rate. The stress measure here is the
Cauchy stress obtained by using the conjugate stress which
results from the material behavior integration:
ð3Þ
Under the small deformation assumption, the total strain can
be decomposed into an elastic part and an inelastic one:
ð4Þ
The elastic strain is calculated by using to the generalized
Hooke’s law: where is the Cauchy stress tensor
or macroscopic stress resulting from the material behavior
integration and is the the fourth-rank tensor of elastic
moduli. The inelastic strain is the average of the irrevers-
ible deformations of the two considered phases according to:
ð5Þ
where z denotes the volume fraction of the SM phase in the
composite. In the MM models, each phase I is associated to a
stress tensor calculated from a stress concentration rule.
Several approaches were used to obtain through different
transition rules. For the sake of simplicity and to reduce the
number of material coefficients, it is assumed in the present work
that the macroscopic stress is equal to the stress in each phase:
ð6Þ
The kinematic hardening is not considered here since these
variables are devoted to describe material behavior under
cyclic loading. The present study being only dedicated to
HESM behavior under monotonic loading, the HE and SM
criteria are written simply as:
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ð7Þ

where and is the deviatoric part of the of these parameters is performed with the help of Zset FE
tensor . The material parameters RHE SM
0 and R0 characterize code provided with an optimizer routine [26]. From the
the initial size of the two elastic domains, whereas RHE and compressive tests, the apparent Young’s moduli are
RSM denote the size change in the elastic domain related to checked by calculating the initial slope of the stress-strain
each yield surface. curve. The parameters used for the simulations of the


numerical results (Table 4) are found to fit best to the
RHE ¼ QHE 1  ebHE :vHE RSM ¼ QSM 1  ebSM :vSM
ð8Þ
(a) 60
where QHE ; bHE ; QSM and bSM are material parameters.
According to the normality flow rule, the viscoplastic strain

stress σ(MPa)
rates may be expressed as:
40

20 10−2 s−1
ð9Þ sim 7.5
exp 7.5 10−2 s−1
where v_HE and v_SM are two viscoplastic multipliers. They sim 7.5 10−3 s−1
exp 7.5 10−3 s−1
can be written using a classical Norton law to account for 0
the strain rate sensitivity: 0 0.05 0.1 0.15 0.2 0.25
 HE nHE  SM nSM strain ε
f f
v_HE ¼ v_SM ¼ ð10Þ
KHE KSM (b) 60
The McCauley-brackets hi denotes the positive part: hxi ¼ 0
if x\0 and x otherwise. KHE ; nHE ; KSM and nSM , are visco-
stress σ(MPa)

40
plastic parameters related to the viscosity of the two phases.

Results 20 sim 7.5 10−2 s−1

exp 7.5 10−2 s−1
sim 7.5 10−3 s−1
In the previous section Eqs. 1–10 display some material exp 7.5 10−3 s−1
coefficients that have to be determined. The identification 0
0 0.05 0.1 0.15 0.2 0.25
Table 4 Identified parameters of the proposed model dedicated to the strain ε
mechanical behavior of the HESM biocomposite
Parameters Units (c) 80
z 0.0 0.05 0.15
stress σ(MPa)

60
E 730 750 900 MPa
HE phase RHE
0 28.46 28.46 38.46 MPa
nHE 2.3 40 sim 2.5 10−1 s−1
KHE 59.32 MPa exp 2.5 10−1 s−1
sim 7.5 10−2 s−1
QHE 38.98 MPa 20 exp 7.5 10−2 s−1
bHE 2.1 sim 7.5 10−3 s−1
SM phase RSM 39.09 39.09 49.09 MPa exp 7.5 10−3 s−1
0
0
nSM 2.8 0 0.05 0.1 0.15 0.2 0.25
KSM 75.73 MPa strain ε
QSM 16.75 MPa
bSM 59.76 Fig. 4 Compressive tests of the HESM biocomposite, a 0 % SM,
b 5 % SM, c 15 % SM

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normal pressure P =10MPa
coating
y
substrate
Ux =Uy =0
Fig. 5 Finite element modeling of the HESM coated surface subjected to mechanical loading
Fig. 6 Contour plot of the von
Mises stress (MPa) in the
HESM coating and the substrate
at the end of the loading stage
0 9 18
experimental compressive tests as given in Fig. 4. These
parameters are unique for all the SM phase levels except
for the initial size of the elastic domain RHE SM
0 and R0 and
Young’s modulus E. Good agreement is encountered by
both simulations and experimental curves for the whole
range of the SM ratio and strain rates. It can be seen that
strength is increased by the addition of SM particles. This
result is confirmed by the photographs of each specimen (0,
5, 15, 20 %) after compressive tests (Fig. 3). The model is
implemented in the FE code Zébulon. The constitutive
equations of the model can then be used to analyze the
inelastic behavior of structures made of HESM composite.
In the following step, a FE simulation of a case study is
performed using the MM model described and identified in
the previous section. This simulation is to predict the
mechanical behavior and the resulting stress strain
detailed view of the contact zone
x
(0% of SM)
(5% of SM)
(15% of SM)
27 36 45 55 64 73 82 91 100
distribution of structures composed of HESM coating and
stiffer substrate subjected to a contact pressure imposed by
an indenting body. A plain strain mesh (Fig. 5) is used for
the FE analysis of the coating. The coating and the indenter
include 448 and 580 three node elements respectively
refined in the contact zone, whereas, the substrate is
modeled with 102 three node elements. The base of the
substrate is clamped. Pressure imposed on the top surface
of the indenter along the x2 direction increases linearly
during the time lapse and reaches 10 MPa after 1 s. The
contact between the indenter and the coating surface is
modeled by the classical Coulomb law with a friction
parameter l ¼ 0:1. Figure 6 shows the contour plot of the
equivalent von Mises stress at the end of the loading stage
for the three SM ratios. A deeper cavity is obtained for the
natural SM. A progressive strength of the HESM takes
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place when the SM substitution ratio increases and the
height of the print decreases (0.145, 0.144, 0.13 mm for 0,
5, 15 % respectively). The stress distribution is also more
convenient for the coating. Experimental investigation
should be conducted in order to assess the previous results.
Conclusion
The biocomposite from SM and the biopolymer based beef
HE using the thermo-compression molding technique were
successfully fabricated. The incorporation of sediments
with different percentages of marine sediments (0, 5, 15
and 20 %) increases the stiffness of the material and the
compressive strength while tensile and flexural strengths
decrease but maintain acceptable values. The TGA analysis
shows that the thermal stability improved with the addition
of marine sediments. Contrarily to the elastic-brittle
behavior obtained under tensile and flexure loading, the
compressive behavior of the HESM is ductile (visco-elasto-
plastic). A multi-phase model is then developed to char-
acterize this compressive behavior taking into account the
SM ratio and the strain rate effect. The proposed model is
implemented in an FE code in order to simulate the strain
and stress distribution in ground coating submitted to
compressive loading. The results are encouraging to use the
HESM biocomposite as a coating element.
Acknowledgments The author would like to thank Pr. Noredine
Abriak, Pr. Rachid Zentar and Dr. Mahfoud Benzerzouar from Mines
de Douai for providing marine sediments. The authors also gratefully
acknowledge the support of Dr. Nader Haddar from ENI Sfax for the
realization of the compressive tests.
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