Composites Science and Technology 69 (2009) 2163–2168

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Composites Science and Technology

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

New biocomposites based on thermoplastic starch and bacterial cellulose

Ivo M.G. Martins, Sandra P. Magina, Lúcia Oliveira, Carmen S.R. Freire *, Armando J.D. Silvestre,
Carlos Pascoal Neto, Alessandro Gandini
CICECO and Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro, Portugal

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

Article history: Bacterial cellulose, produced by Acetobacter Xylinum, was used as reinforcement in composite materials
Received 23 March 2009 with a starch thermoplastic matrix. The composites were prepared in a single step with cornstarch by
Received in revised form 20 May 2009 adding glycerol/water as the plasticizer and bacterial cellulose (1% and 5% w/w) as the reinforcing agent.
Accepted 24 May 2009
Vegetable cellulose was also tested as reinforcement for comparison purposes. These materials were
Available online 29 May 2009
characterized by different techniques, namely TGA, XRD, DMA, tensile tests, SEM and water sorption
assays. All composites showed good dispersion of the fibers and a strong adhesion between the fibers
Keywords:
and the matrix. The composites prepared with bacterial cellulose displayed better mechanical properties
Bacterial cellulose and thermoplastic starch
B. Mechanical properties
than those with vegetable cellulose fibers. The Young modulus increased by 30 and 17 fold (with 5%
D. Dynamic mechanical thermal analysis fibers), while the elongation at break was reduced from 144% to 24% and 48% with increasing fiber con-
(DMTA) tent, respectively for composites with bacterial and vegetable cellulose.
D. Scanning electron microscopy (SEM) ! 2009 Elsevier Ltd. All rights reserved.
D. Thermogravimetric analysis (TGA)

1. Introduction Starch is one of the most abundant natural polymers and is con-
sidered as a promising raw material for the development of novel
New functional materials obtained from renewable resources materials, including biocomposites. It can be converted into a ther-
have gained much attention in the last decades due to the global moplastic material, known as thermoplastic starch (TPS), through
increasing demand for alternatives to fossil resources [1]. For the disruption of the molecular chain interactions under specific
example, composites based on thermoplastic polymers and natural conditions, in the presence of a plasticizer. Water and glycerol
fibers are very attractive materials because of their good mechan- are the most widely used plasticizers in the production of TPS.
ical properties, sustainability and environmental-friendly connota- When natural fibers are mixed with TPS, its mechanical properties
tion [2]. These materials have been widely used in the automotive are improved, indicating a good adhesion between the reinforcing
and packaging industries [2] and their applications in other areas fibers and the matrix [4,5]. Several studies have been published
are being actively sought. dealing with the preparation and characterization of TPS-based
The use of natural fibers as reinforcing elements in composite composites with different cellulose substrates, namely commercial
materials presents important advantages, when compared with regenerated cellulose fibers [6], vegetable fibers [6–8], microcrys-
their synthetic or inorganic counterparts, namely biodegradability, talline cellulose [9], microfibrillated cellulose [3] and cellulose
high availability, low cost, low energy consumption, low density, nanocrystallites [5]. Apart from the enhanced mechanical proper-
high specific strength and modulus (with fibers possessing an ade- ties of these reinforced TPS materials, a significant improvement
quate aspect ratio), high sound attenuation and comparatively easy in water resistance is also obtained by adding cellulose crystallites
processing ability due to their flexibility and non-abrasive nature [10] or microfibrillated cellulose [3]. In general, these TPS/fiber
[3]. composites also displayed improved thermal stability due to the
In addition, if the natural fibers are combined with biodegrad- higher thermal resistance of cellulose fibers [7].
able matrices, the obtained composite materials are expected to Owing to its unique properties, such as high mechanical
be fully biodegradable. The development of biocomposites gained strength, high crystallinity and a highly pure nanofibrillar network
particular relevance with the increasing availability and diversity structure, bacterial cellulose, produced by Acetobacter Xylinum, is
of biodegradable polymers [4]. becoming a promising biopolymer for several applications. For
example, due to its biocompatibility [11], bacterial cellulose has
been extensively investigated in the biomedical field [12–14].
* Corresponding author. Tel.: +351 234 401 405; fax: +351 234 370084. Other applications include its use as component for audio mem-
E-mail address: [email protected] (C.S.R. Freire). branes [15], electronic paper [16], optically transparent composites

0266-3538/$ - see front matter ! 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2009.05.012
2164 I.M.G. Martins et al. / Composites Science and Technology 69 (2009) 2163–2168

[17], reinforcing agent for paper [18] and other polymeric materi- not improve the modulus to the same extent as cotton or softwood
als and composites [19], among others. counterparts.
However, to the best of our knowledge, only two studies dealing The present paper describes the preparation and characteriza-
with the preparation and characterization of bacterial cellulose- tion of biocomposite materials obtained by the incorporation of
starch composites have been published so far [20,21]. Grande bacterial cellulose into a TPS matrix during the gelatinization pro-
et al. obtained a plasticized starch/bacterial cellulose nanocompos- cess. Similar composite materials reinforced with vegetable cellu-
ite sheets by hot-pressing. The ensuing films were characterized in lose fibers were also prepared for comparison purposes.
terms of their morphology, whereas other important parameters,
such as their mechanical and thermal properties, were not investi-
gated. The incorporation of bacterial cellulose microfibrils, ob- 2. Experimental
tained by the acid hydrolysis of the cellulose network, into
extruded TPS and starch-pectin blends was also studied [21]. How- 2.1. Materials
ever, in this work, the peculiarity of this cellulose substrate was not
fully exploited, since the nano- and micro-fibril three-dimensional Bacterial cellulose (BC) (a tridimensional network of nano and
network morphology was partially destroyed during the hydrolysis microfibrils with 10–100 nm width), in the shredded wet form
step. Indeed, the microfibrils derived from bacterial cellulose did (95% of humidity), was supplied by Forschungszentrum für

100 T d = 327 ºC TPS

90
80
70
m/mi(%)

60
50
40
30
20
10
0
0 100 200 300 400 500 600 700 800
Temperature (ºC)

100
100 T d = 336 ºC
T d = 376 ºC
VC TPS/VC 5%
90 90
80 80
70 70
60 60
m/mi(%)
m/mi(%)

50 50
40 40
30 30
20 20
10 10
0 0
0 100 200 300 400 500 600 700 800 0 100 200 300 400 500 600 700 800
Temperature (ºC) Temperature (ºC)

100 100 T d = 332 ºC

T d = 337 ºC BC T PS/BC 5%
90 90
80 80
70 70
60 60
m/mi(%)
m/mi(%)

50 50
40 40
30 30
20 20
10 10
0 0
0 100 200 300 400 500 600 700 800 0 100 200 300 400 500 600 700 800
Temperature (ºC) Temperature (ºC)

Fig. 1. Thermogravimetric curves for TPS, BC, VC, TPS/BC 5% and TPS/VC 5% composites.
 I.M.G. Martins et al. / Composites Science and Technology 69 (2009) 2163–2168 2165

Medizintechnik und Biotechnologie e.V. (Germany). The vegetable The mixtures were loaded into the mixer chamber pre-heated at
cellulose fibers (VC) (with 0.8–1 mm length and 20–30 lm width) 120 "C and processed at 60 rpm during 6 min, for the unfilled TPS
used in this work were from a Eucalyptus globulus ECF (DEDED) and VC fiber-based composites, and 20–30 min for the BC compos-
industrial bleached kraft pulp, kindly provided by a Portuguese ites, to allow for the release of the moisture excess, in order to
pulp mill. reach comparable water contents of the final composites (about
Corn starch (27% amylose), glycerol (99.5%), stearic acid (95%), 10% and 4% (w/w) for composites with a fiber content of 1% and
magnesium chloride hexahydrate (>99%), magnesium nitrate (pur- 5%, respectively).
um, >99%), and barium chloride (dehydrated, >99.9%) were sup- The composites were then molded in an injection molding ma-
plied by Sigma–Aldrich and used as received. chine (Thermo-Haake Minijet II) for tensile (bar according to ISO
527-2-5A) and DMA analysis.
2.2. Biocomposites preparation Before characterization, all samples were kept in a conditioning
cabinet of 50% relative humidity (RH) at 25 "C to ensure the stabil-
Both vegetable and bacterial cellulose fibers were first dis- ization of their water content.
persed in water in order to avoid the formation of agglomerates.
The excess of water was then removed by vacuum filtration until 2.3. Biocomposites characterization
the desired content required for the plasticization step (25 wt.%
in respect to the total amount of the mixture components, namely The composites were characterized using thermogravimetry
starch, glycerol and water) was reached. However, in the case of (TGA), X-ray diffraction (XRD), tensile tests, dynamical mechanical
bacterial cellulose, due to its natural high water content and mor-
phology, it was not possible to reduce the water content to that le- 24
vel, particularly for 5% of BC. In this case the lowest water content
achieved was about 50%.
Young Modulus (MPa)
20
Starch (45%), glycerol (30%) and the wet fibers (either VC or BC)
(1% or 5%, in dry basis) were then pre-mixed in polyethylene bags 16
until a homogeneous mixture was obtained. Stearic acid (demoul-
ding agent) was also added, at low concentration (0.5 wt.%). TPS 12
samples without fibers were prepared likewise, but adding 25
wt.% of water. 8
The unfilled thermoplastic starch and the corresponding com-
posites were prepared using a Plastograph EC (Brabender) mixer. 4

0
TPS VC 1% VC 5% BC 1% BC 5%

3.5
Starch
3.0
Tensile Strength (MPa)

2.5

2.0
TPS
1.5

1.0

0.5
VC
0.0
TPS VC 1% VC 5% BC 1% BC 5%

TPS/VC 5%
160
Elongation at break (%)

140

BC 120

100

80

60

TPS/BC 5% 40

20

0
5 10 15 20 25 30 35 TPS VC 1% VC 5% BC 1% BC 5%
2θ
Fig. 3. Young modulus, tensile strength and elongation at break of corn starch
Fig. 2. The X-ray diffractograms of Starch, TPS, VC, BC, and TPS composites with 5% thermoplastic composites reinforced with 1% and 5% of bacterial and vegetable
of VC (TPS/VC 5%) and with 5% of BC (TPS/BC 5%). cellulose.
2166 I.M.G. Martins et al. / Composites Science and Technology 69 (2009) 2163–2168

analysis (DMA), scanning electron microscopy (SEM) and water

absorption tests.
TGA essays were carried out with a Shimadzu TGA 50 analyzer
equipped with a platinum cell. Samples were heated at a constant
rate of 10 "C/min from room temperature to 800 "C, under a nitro-
gen flow of 20 mL/min. The thermal decomposition temperature
was taken as the onset of significant (P0.5%) weight loss, after
the initial moisture and glycerol losses.
The X-ray diffraction (XRD) measurements were carried out
with a Phillips X’pert MPD diffractometer using Cu Ka radiation.
Mechanical testing was performed on a TA-Hdi (Stable Micro
Systems Texture Analyser) texturometer using a load cell of 5 kg,
and operating at a deformation rate of 0.5 mm/s. The tensile tests
were performed under ambient conditions. Tensile strength, ten-
sile modulus, and elongation at break were calculated using the In-
Fig. 4. Temperature dependence of storage modulus of the TPS and the TPS/BC 5%
stron Series IX software. and TPS/VC 5% based composites.
DMA measurements were carried on a Tritec 2000 DMA Triton
equipment operating in the bending (dual cantilever) mode. Tests
were performed at 1 Hz and the temperature was varied from !80
to 100 "C by 1 "C steps. The displacement amplitude was set to patibility between the two carbohydrate components of the com-
20 lm. posites. This increased thermal stability has already been
SEM micrographs of the composite fractured surfaces, produced observed with other cellulose substrates, namely microcrystalline
by immersion in liquid nitrogen, were obtained on a SU-70 equip- cellulose and pulp fibers [4,9]. However in those studies, regard-
ment operating at 1 and 4 kV, depending on the sample, while less of the fact that higher reinforcing agent contents were used,
those of the BC and VC substrates were taken in Hitachi S4100 the effects observed were less pronounced than the values re-
equipment operating in field emission. ported here.

2.4. Moisture uptake 3.2. X-ray diffraction

Composite specimens (dimensions 10 " 10 " 2 mm) were con- The X-ray diffraction patterns of native corn starch, vegetable
ditioned at RH of 33%, 52% and 91%, achieved by maintaining the and bacterial cellulose fibers, thermoplastic starch and correspond-
samples in a closed atmospheric equilibrium at room temperature ing biocomposites are shown in Fig. 2. Native corn starch showed a
with saturated solutions of MgCl2, Mg(NO3)2 and BaCl2, respec- typical A-type X-ray diffraction pattern with strong peaks at 2h
tively. A minimum of three samples were tested for each compos- 15.4, 17.4, 18.7 and 23.4, whereas in both VC and BC the main
ite. The weight increase due to water absorption was periodically peaks were observed at 2h 14.3, 15.9, 22.6 and 33.7, which are typ-
assessed for #1 month. The water uptake, Wuptake, at time t, was ical of Cellulose I. Retrograded thermoplastic starch gives both B
calculated as: and V-type diffraction patterns [23], with the main peaks at 2h
! " 16.8, 12.9 and 19.8, respectively.
Wt ! W0 The X-ray diffractograms of TPS biocomposites showed typical
M uptake ¼ " 100
W0 diffraction peaks of both cellulose fibers and retrograded thermo-
plastic starch matrix. The increase in the fiber content seemed to
where W0 is the specimen initial weight and Wt its weight after a favor the retrogradation process, i.e. the improvement of the TPS
time t. matrix crystallinity, since the peaks at 2h 12.9, 16.8 and 19.8 be-
came more pronounced. These results are in agreement with those
3. Results and discussion reported by Ma et al. [22] for composites of TPS plasticized by urea
and formamide, with a fiber content above 20%.
The unfilled TPS and all biocomposites prepared in this study
were in general very homogenous, since the formation of agglom-
erates was not visually observed.

3.1. Thermal properties

Thermogravimetric analysis of the composite materials was

carried out to assess their thermal stability and degradation pro-
files. The TGA tracing of both VC and BC composites are a combina-
tion of those of the corresponding cellulose substrates and of the
TPS matrix (Fig. 1). The two mass losses, at around 100 and
200 "C, before the onset temperature, were related to the volatili-
zation of water and glycerol, respectively, and the maximum deg-
radation step at 330–340 "C assigned to the degradation of starch
and cellulose [22].
The addition of low amounts (1% and 5%) of both vegetable
and bacterial cellulose fibers to the TPS matrix, resulted in a
slight increase in the thermal stability of the composites (9 and
7 "C, respectively), which can be explained by the higher stability Fig. 5. Temperature dependence of tan d of the TPS and the TPS/BC 5% and TPS/VC
of the cellulose substrates and particularly by the excellent com- 5% based composites.
 I.M.G. Martins et al. / Composites Science and Technology 69 (2009) 2163–2168 2167

3.3. Mechanical properties The storage modulus of cellulose fiber-based composites was
also higher than that of the unfilled TPS matrix, but the presence
The effect of the cellulose fiber type and also of the fiber content of BC gave higher storage modulus values than those associated
on the large strain behavior of cellulose fibers/TPS composites was with the vegetable counterpart. These results were in good agree-
investigated up to their failure. The Young modulus and the tensile ment with the tensile tests essays referred to above (Fig. 3).
strength, determined from the typical stress–strain curve, in- Fig. 5 shows the curves of tan d as a function of temperature for
creased considerably with the fiber content, with BC producing the TPS matrix and the corresponding composites, which revealed
the most relevant increments (Fig. 3). At a fiber content of 5%, two main thermal transitions at around !55 and !6 "C, respec-
the Young Modulus was 30 and 17 times higher than that of the tively. The main a relaxation, associated with a broad tan d peak,
unfilled TPS, respectively for BC and VC composites. Additionally, is normally attributed to the starch-rich phase, whereas the second
the presence of cellulose fibers caused a considerable decrease in relaxation (b) is assigned to the glycerol-rich phase [7,25]. The
the elongation at break (Fig. 3), which, as in the case of the Young introduction of VC and BC fibers into the TPS matrix resulted in a
modulus, was more accentuated for BC composites (144–24%) shift in the main relaxation to higher temperatures, which further
(Fig. 3). confirmed the strong fiber–matrix interfacial interactions, particu-
The superior mechanical properties of TPS/BC composites com- larly in the case of the BC reinforced composites. This behavior is in
pared with those filled with VC fibers, confirmed the good interfa- close agreement with previous studies dealing with the prepara-
cial adhesion and the strong interactions between the BC and the tion of natural fiber-based TPS composites [4,9].
TPS matrix. These results can be explained by the inherent mor-
phology of BC with its nano- and micro-fibrillar network. Further- 3.4. Microscopy
more, huge increments in the mechanical performance of several
composite materials have previously been reported by the incorpo- A selection of SEM micrographs of the fractured surface of com-
ration of modest proportions of BC nanofibers in other kinds of posite materials with 5% of VC or BC is shown in Fig. 6. For each
matrices [24]. material, two different magnifications were used in order to dis-
The dynamic mechanical measurements were performed on un- play both the cellulose dispersion within the TPS matrix and the
filled TPS and composite materials filled with 5% VC or BC fibers. interfacial adhesion between the two composite components.
The curves of the log (E’/Pa) (storage tensile modulus) vs tempera- The incorporation of both cellulose substrates had a modest ef-
ture are displayed in Fig. 4. In general, as expected, the storage fect on the plasticization of corn starch, since no residual starch
modulus decreased as the temperature increased. granular structures were observed after the composite processing

Fig. 6. SEM micrograph of vegetable and bacterial celluloses and the fragile fractured surface of TPS filled with VC and BC: (A) vegetable cellulose; (B) bacterial cellulose; (C)
and (D) TPS/VC composites (5 wt.%); (E) and (F) TPS/BC composites (5 wt.%).
2168 I.M.G. Martins et al. / Composites Science and Technology 69 (2009) 2163–2168

16
TPS TPS/VC 5% TPS/BC 5% Acknowledgments
50% RH
14 The authors would like to acknowledge Prof. Cruz Pinto for his
Water absorption (%)

12 valuable contribution with the DMA experiments optimization. L.

Oliveira thanks the Fundação para a Ciência e a Tecnologia (Portu-
10
gal) for a post-doctoral Grant (SFRH/PBD/38515/2007).
8
33% RH
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