Andrzej K.

Błędzki1,2,
Adam Jaszkiewicz2,
Biocomposites in the Past
Magdalena Urbaniak3,
Dobrosława Stankowska-Walczak4
and in the Future
West Pomeranian University Abstract
of Technology in Szczecin, Due to increasing environmental awareness nowadays, biocomposites are becoming impor-
1)Institute of Materials Science and Engineering,
3)Department of Mechanics and Machine Elements,
tant and prevalent materials, as they were centuries ago. The development of high-perfor-
mance engineering products made from natural resources is increasing worldwide. Natural
Al. Piastow19, 70-310 Szczecin, Poland fibre composites have become more and more efficient as new compositions and processing
E-mail: [email protected],
[email protected] methods are being intensively researched, developed and consequently applied. This paper,
above all, is intended to provide a brief outline of the development and modification trends
2)Universität Kassel, Institut für Werkstofftechnik, which aim to make biocomposites more user-friendly and eco-friendly by means of novel
Möncheberg str. 3, 34125 Kassel, Germany processing methods. These methods produce biopolymers with an improved melt behaviour
and use naturally occurring raw materials.
4)Pomeranian Medical University in Szczecin,
Medicinal Chemistry Department, Key words: biopolymer, polylactide, chain extender, cellulose fibre, biocomposite.
Al. Powstanow Wlkp. 72, 70-111 Szczecin, Poland

Throughout the centuries, thanks to read- gist Maurice Lemoigne described poly-
ily accessible and easily processable ma- hydroxybutyrate (PHB), which gave rise
terials like a clay, flint or horn, mankind to bioplastic materials used mostly for
n Introduction was able to solve technical problems or medical and later also for packaging ap-
Today, plastic products are an indispen- to achieve artistic effects. However, we plications. However, the last few dec-
sable part of our life, such that recent have always been on lookout for better ades were a time period fully dominated
decades can be described as the plastic materials. In the late Middle Ages, spe-
by petrochemical polymers, since the
age. Therefore, the history of plastics, its cially hardened and filled lactoprotein
growth of chemistry based on crude oil
present and its prospects for the future products were used as a substitute for
are worth presenting to anyone who is natural horn for inlaid work, small me-
interested in developments which have dallions (Figure 1) and other artistic
occurred in materials. wares [1]. The rapidly developing and
constantly changing social structures in
the 18th and 19th centuries then led to an
increase in imitations and surrogate ma-
terials allowing ordinary people access
to those objects which had been reserved
for the wealthy. In this time, a mixture
of linseed oil and powdered cork on a
cloth base (linoleum) was first used as a
floor covering and substitute for a sim- Figure 3. Post card (Portugal - 1905) cel-
luloid [1].
ple wooden floor, and celluloid was used
as synthetic ivory. The first technically
viable plastic product was vulcanised
natural caotchouc, a hard rubber called
Ebonite, became a substitute for ebony
(Figure 2) and replaced natural tortoise
shell [1]. This phase of modified natu-
ral materials derivatives made of casein,
Figure 1. Medallion frame (Germany - cellulose (Figures 3 and 4) and natural
1800), proteinoplast [1]. caotchouc was followed by Bakelite as
the first completely synthetic product.
It was named after Belgian chemist Leo
Hendrik Baekeland who in 1872 dis-
covered this polymer made of phenol
and formaldehyde [1, 2]. However, this
phenolic resin was not initially put into
any practical application. It marked the
starting point for the development of
various synthetic thermoplastic materi-
als from the 1920s and 1930s (Figure 5,
see page 16). The first reports concern-
Figure 2. Writing set (France - 1880) ebo- ing the syntheses of biopolymers dates Figure 4. Table lamp (Germany - 1930)
nite [1]. back to 1925 when French microbiolo- celluloid [1].

Błędzki A. K, Jaszkiewicz A, Urbaniak M, Stankowska-Walczak D. Biocomposites in the Past and in the Future. 15
FIBRES & TEXTILES in Eastern Europe 2012; 20, 6B (96): 15-22.
 able lignocellulosic fibre-based compos-
ites rose significantly (Figure 7).

The main area of increasing usage of

these composite materials has become
the automotive industry, predominantly
in interior applications. Lately, the use
of biocomposites has increased by about
50% per annum in this industry [5] due to
new legislation forcing car makers to re-
use and recycle materials. The increased
importance of renewable resources for
raw materials and recyclability or bio-
degradability of the product at the end
of its useful life is demanding a shift
from petroleum-based synthetics to agro-
based biofibres and biopolymer not only
in automotive applications [6, 7].

As a result of the increased environmen-

Figure 5. Historical diagram of plastics [3].
tal awareness among customers, there
is a growing market for products based
revolutionised the cost-efficient produc- were introduced as agricultural-based on renewable raw materials. This envi-
tion of plastics. As a consequence, lower- polymer materials composed of paper ronmentally conscious motivation has
performance applications have become and soybean resin for automotive parts resulted in the development of stand-
under the aegis of thermoplastics, where- by Henry Ford (1941) (Figure 6). How- ards which determine the percentage
as thermosets have taken over the field of ever, the technologies employed up to of such materials (% bio-based) in the
high-performance composites. the present for producing thermosets do product. Currently, certification of bio-
not comply with the stringent rules and based products has been established in
Accordingly, in long-established tech- regulations concerning preservation of Belgium (OK biobased certification in
nical application areas, the major ther- the environment. This is why, in recent 2009) [8], Germany (DIN Certo certifi-
moplastic engineering composite is still years, many research centres all over the cation in 2010) [9] and the USA (USDA
polypropylene reinforced with glass fi- world have been intensively occupied in Certified biobased products in 2011)
bre, as its cost/performance ratio is one searching out and scientifically examin- [10] (Table 1). Due to this standardisa-
of the best of all. Nevertheless, the most ing new composites based on raw ma- tion, renewable materials are becoming
important polymer construction materi- terials from renewable resources. This attractive alternatives to glass and other
als have become thermosetting compos- is reflected in the increasing number of fibre-reinforced petroleum-based poly-
ites. They have proven to be useful in all publications on natural fibre composites mer composites in the customer market.
branches of the economy and business in recent years. Satyanarayana et al. [4] However, further research is still required
areas, mostly in building of boats, yachts found by entering the words “biodegrad- to overcome obstacles such as moisture
and other sport equipment, in the aviation able, polymer, fibre” in the ISI database absorption and increased long-term sta-
and armaments industries and especially that, after the year 2000, the number of bility for use in exterior components.
in the automotive industry. At first, they publications and patents on biodegrad- New, technically advanced, high quality

Patents
Articles
Number

Year

Figure 6. One of the most famous photographs (1941) of Henry Figure 7. Number of publications and patents on biodegradable lig-
Ford who is trying to crack a rear deck lid composed of paper and nocellulosic fibre based composites (1995–2007) (found in the ISI
soybean resin with a sledge hammer. database by entering the words ‘biodegradable, polymer, fibre’) [4].

16 FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96)
materials from renewable resources, that
are stronger, cheaper and eco-friendly,
should soon be achieved due to the in-
teraction between chemistry, physics and
engineering technology.

n Natural fibres
Total worldwide biomass harvested in
2008 reached ca. 13 billion tons and most
of this was utilised for animal feed (58%),
food (15%), wood energy use (10%) and
wood material use (11%). Utilisation of Figure 8. Worldwide use of renewable resources for materials in 2008 [11].
biomass as renewable raw materials for
energy and material use amounted to
only 2.7 and 3.3%, respectively [11]. The
1 % rapeseed, castor, cotton

use of biomass for renewable raw mate-

rials (as for every other use) throughout
the world is based on a mosaic of differ-
ent types of biomass [11]. These include
3 % linseed
renewable resources from agriculture and
forestry (e.g. timber, plant oils, starches,
sugars, specific components) and biogen-
ic residues (e.g. straw and other waste Figure 9. Worldwide use of natural fibres and vegetable oils for materials in 2008 [11].
from agriculture, wood off-cuts, organic
waste, animal fats and proteins). While were used to reinforce mud bricks. They of selected fibres (flax, hemp, jute, sisal,
the potential use of biomass for energy were, most likely, the first man-made abaca, cotton, man-made cellulose), i.e.
production is limited (direct burning, composites filled with natural fibres those which may successfully compete
biofuels, biogas or biomass gasification), in human history. Classification of the with glass fibres, are shown in Table 2
in contrast, material use of biomass (Fig-
natural fibres used nowadays, including [19, 20]. The chemical and physical
ure 8) can be characterised by a large
excellent raw materials for manufac- structure of natural fibres presented in
spectrum of potential applications. The
turing of so called “green products” as Figure 11 (see page 18) [21] generally
raw materials used to produce biocom-
well as mineral fibres, is shown in Fig- shows an example where its elements
posite components are mostly plant oils
ure 10 (see page 18) [19]. The properties are “designed” for strength and stiffness.
and natural fibres (Figure 9) [11].

Natural fibres surpass the usual reinforc- Table 1. Certification of bio-based products [8 - 10].
ing fibres, for instance glass fibres, with Certification Bio-content Denotation of bio-content
respect to low cost, low density, tough- Belgium 20 - 40%
ness, acceptable specific strength, en- Vinçotte - Certest Products 40 - 60% designated by number
60 - 80% of asterisks on the label
hanced energy recovery, recyclability, bi- ”OK biobased” certification
> 80%
September 2009
odegradability, etc. [12 - 14]. Moreover,
Germany 20 - 50%
natural fillers are able to minimise envi- DIN CERTCO certification 50 - 85%
given on upper semicircle
of the label
ronmental pollution, allowing these com- April 2010 > 85%
posites to play an important role among USA
eco-friendly materials [15, 16]. However, US Dpt. of Agriculture exact % listed on
”USDA Certified min. 25%
natural fibre properties can differ greatly Biobased Products”
the label
depending on type, grade, harvest qual- February 2011
ity, processing method, yield, etc. Only
natural fibres of high technical quality
Table 2. Engineering properties of natural fibres compared to glass fibre [19, 20].
guarantee sufficient reproducibility of the
mechanical characteristics of biocompos- Tensile Young’s Specific Elongation Moisture Diameter of
Density,
ites [17]. The overall characteristics of Fibre
g/cm3
strength, modulus, modulus, to break, absorption, elementary
MPa GPa GPa/g/cm3 % % fibre, μm
reinforcing fibres used in biocomposites,
E-Glass 2.55 2400 73 29 3 - 10 – 20
including source, type, structure, compo- Flax 1.40 800 – 1500 60 – 80 26 – 46 1.2 – 1.6 7 15 – 22
sition, as well as mechanical properties, Hemp 1.48 550 – 900 70 47 1.6 8 17 – 24
are widely reviewed in the literature [18]. Jute 1.46 400 – 800 10 – 30 7 – 21 1.8 12 15 – 35
Sisal 1.33 600 – 700 38 29 2–3 11 15 – 30
Since the beginning of our civilisation, Abaca 1.50 980 - - - - 10 – 30
natural fibres have been used as a rein- Cotton 1.51 400 12 8 3 – 10 8 – 25 15 – 24
forcement in composite materials, such Man-made
1.49 885 27 18 12 8 12
cellulose
as when grass and straw or animal hair

FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96) 17
Figure 10. Classification of natural fibres [19].

Figure 11. Structure of natural fibres [21].

18 FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96)
A fibrous structure made of cellulose, a
natural polymer with high strength and
stiffness per weight with multi-ply con-
struction composed of long fibrils con-
sisting of many microfibrils at different
angles to the fibre axis, can be an effec-
tive reinforcement for a composite ma-
trix, due to hindered polymer flow caused
by the fibre filler [6].
Figure 12. Microbial pathway of polylactic acid
(PLA) production.
n Biopolymers
Public concern about the environment,
climate change and limited fossil fuel re-
Biopolymers
sources are important driving factors to
find alternatives to crude oil. Bio-based
plastics may offer important contribu-
tions by reducing the dependence on fos- From renewable raw materials From crude oil
sil fuels and the related environmental
impacts. Biopolymers have experienced
Vegetable Animal
a renaissance in recent years. A lot of origin
Microbial
origin
new polymers have been developed from
renewable resources and many others,
such as starch, i.e. a naturally occurring Starch, - derivative
Polycaprolactone
polymer, were re-discovered as plastic Cellulose, - Polylactic acid (PLA) Chitin
Polyesteramide
derivative Polyhydroxyalkanoate Collagen
materials. Other examples are polylactic Lignin, - derivative (P(HB), P(HB-co-HV), ... Protein (PBP)
Polyvinyl alcohol
Polyglycolide
Polyamide
acid (PLA) that can be produced from
fermentable sugars, partly by the micro-
biological route via lactic acid formation
Figure 13. Biopolymers classification [22].
and following ring opening polymerisa-
tion (Fig. 11) and polyhydroxyalkanoates
(PHAs) obtained from polysaccharides in the field of medicine. PLA materials use of plastics based on renewable feed-
during metabolic processes in bacteria developed for medical devices such as stocks which are biodegradable is a more
cells. These developments in emerging resorbable screws, sutures and pins re- sensible choice than conventional plastic
bio-based plastics are spectacular not duce not only the risk of tissue reaction recycling, as the end products are organic
only from a technological point of view. but suffering and recovery times of pa- matter, and toxic emissions are avoided.
The biopolymer market has been experi- tients and the costs of the health service Therefore, the growth of plastics which
encing rapid growth. The global average as well. Many biopolymer materials are are compostable or easy degraded must
annual growth rate was 38% from 2003 currently incorporated into adhesives, be encouraged and the infrastructure for
to 2007 and as high as 48% in Europe in paints, engine lubricants and construc- sorting and composting organic waste
the same period. The worldwide capacity tion materials, especially in sport equip- must be developed more intensively [23].
of bio-based plastics will likely increase ment and agricultural applications. There
from 0.36 million in 2007 to 2.33 million are an endless number of areas where bi- Easily degraded biopolymers based on
tonnes in 2013 and to 3.45 million tonnes odegradable polymer materials may find PLA are predestined for conventional
in 2020. The greatest production volumes use. The industrial sectors of agriculture, processing especially by means of extru-
are to be reached by microbial biopoly- automotive, medicine and packaging all sion and injection moulding due to their
mers PLA and PHA, called “starch plas- require environmentally friendly poly- sufficient melt stability provided that the
tics” [6]. mers. Biodegradable plastics containing prescribed processing conditions and
starch and/or cellulose fibres are most procedures are kept. In order to improve
There are a number of other biologi- likely to experience continual growth in the mechanical properties of biopolymers
cal materials, quoted in Figure 13, that usage. Because the level of biodegrada- based on PLA, some research has been
have been examined and manipulated tion may be customised to specific needs, carried out lately. The matrix used was
by biopolymer researches. The design of each industry is able to create its own a polylactide PLA4042D (from Nature-
such materials usually begins with a con- ideal material. The various modes of bio- Works LLC, USA). The PLA was blend-
ceptual application. The renewable and degradation are also a key advantage of ed with PBAT [poly(butylene adipate-
biodegradable polymers that may be em- such materials because disposal methods co-butylene terephthalate)] (trade name
ployed in packaging receive more atten- may be tailored to industry specifica- Ecoflex® from BASF SE, Germany) at
tion than those designated for any other tions. Recycling appears to be a viable a weight ratio of 70/30 (PLA/PBAT). An
application because 41% of plastics are way to reduce pollution and environmen- epoxidised styrene-acrylic copolymer as
actually used in packaging, mostly for tal damage since it was first introduced as the chain extender was delivered from
food products [23]. The most important a waste reduction technique. However, as Clariant Masterbatches, Germany in the
biopolymer applications can be found time has passed, it is now obvious that the form of a masterbatch (CESA-extend®).

FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96) 19
 The matrix was compounded together
3000-3500 60-70
with the chain extender via a coating noz-
3500
2500-3000
2000-2500 70
50-60
40-50
zle and cooled to ambient temperature.
1500-2000 30-40
The pellets were dried and compounded

Tensile strength, MPa

1000-1500 20-30
Tensile E-Modulus, MPa

3000 60

2500
500-1000
0-500
50
10-20
0-10 on a single-screw extruder. All compo-
2000 40
nents were dried in a convection oven
1500 30 with a fan before further processing.
1.0 1.0
1000 20
CESA CESA
Figure 14 shows the results of the ten-
0.5 0.5
500 content,, 10 content,
0.0 % wt % wt
sile test on unreinforced PLA/PBAT
0
0 0.0
0 30 70 100
0 30 70 100
PLA content, % wt PLA content, % wt
blends modified with a chain extender. It
is obvious that with an increasing PBAT
Figure 14. Results of the tensile test on PLA/Ecoflex blends [24]. content, both the E-modulus and the
tensile strength decreased significantly.
This is due to the ductile character of
CESA content
Ecoflex compared to rigid PLA. Further-
% 0 0.5 1
more, the addition of the chain extender
PLA PLA / Ecoflex
had only a negligible influence on these
0 N N N 9
parameters [24].
PLA content

30 N N N 6
By adding CESA, enhanced compatibil-
70 5.92 6.50 8.15
3 ity between two polymer phases (PLA
100 2.88 2.72 2.81
0
as matrix and Ecoflex as modifier) was
0 0.5 1 observed and, consequently, significantly
improved impact strength was achieved
(Figure 15) [24]. The chemical inter-
Figure 15. Results of Charpy A-notch impact strength of PLA/Ecoflex; T=+23°C [24]. action of the epoxy reaction groups of
CESA is depicted in Figure 16 [25],
where a crosslinking reaction of multiple
functional side groups (epoxy or anhy-
dride, respectively) with the end groups
of the polylactide chain (e.g. –COOH or
–OH) leads to non-linear chain extension
Chain of the PLA chains. Primarily, the addition
of PBAT improves the Charpy A-notch
Extender
impact strength by a factor of 2. Fur-
thermore, increasing the chain extender
content increased the impact resistance
up to 8.15 kJ/m², which corresponds to
2.8-fold improvement compared to na-
Figure 16. Mechanisms of chain extension [25].
tive PLA [24].

The molecular architecture of the bi-

opolymer modified using such multifunc-
tional additives affects not only on its
mechanical properties but determines the
melt behaviour during compounding as
well. Due to this innovative modification
with the use of chain extenders, thermo-
mechanical stability of the biopolymer
can be achieved.

n Biocomposites
There is a wide variety of biocomposite
processing techniques, as well as factors
(fibre type and content, additives and
others) affecting these processes [18].
Biocomposites with natural fibres can be
processed using a special coating tech-
nique where dried fibres are introduced
Figure 17. Density of PLA and PP composites with various content of natural or glass into a coating nozzle and covered with
fibres [24]. the melted polymer using a screw ex-

20 FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96)
 Tensile E-Modulus, MPa Tensile strength, MPa
PLA/Ecoflex PLA/Ecoflex/Man-made cellulose
6000 6000 120 PLA/Ecoflex PLA/Ecoflex/Man-made cellulose 120

5000 5000 100 100

4000 4000 80 80

3000 native PLA = 3416 3000 60 60

native PLA = 66

2000 2000 40 40

1000 1000 20 20

0 0 0 0
0 0.2 0.4 0.6 0.8 1 0 0.2 0.4 0.6 0.8 1
CESA content, % CESA content, %

Figure 18. Tensile test results of PLA/PBAT composites with man-made cellulose fibres [24].

A-Notch impact strength, kJ/m²

25 PLA/Ecoflex PLA/Ecoflex/Man-made cellulose 25

20 20

15 15

10 10

5 native PLA = 2.71 5

0 0
0 0.2 0.4 0.6 0.8 1
CESA content, %

Figure 19. Charpy A-notch impact strength of PLA/PBAT compos- Figure 20. Global production capacity of bioplastics [28].
ites, T=+23 °C [24].

truder. Biocomposites are up to 20-30% of reactive processing via special chain by increasing the CESA concentration,
lighter than their glass fibre counterparts extenders by which chain extension is another tendency can be observed, i.e.
(Figure 17), whereas other mechanical done by the reactive end groups of poly- a greater amount of branching occurs,
parameters can be comparable or even condensates with a bi- or multifunctional which leads to gelling. As a result, the
enhanced [26]. In order to improve the reactive component. composite becomes more ductile and
mechanical properties of cellulose-fibre stiff but its strength decreases [24].
reinforced polymers, the combination Research focused on improving the me-
of optimised processing conditions and chanical properties of reinforced PLA/ By adding CESA to the PLA/PBAT com-
customised additives is a matter of great- PBAT blends with man-made cellulose fi- posites, obviously not only increased
est importance. Another essential aspect bres (30% by weight) from the Cordenka compatibility occurs between PLA and
is the detailed analysis of the material’s company (Germany) delivered as indus- PBAT, but also a kind of chemical inter-
micromechanical behaviour compris- trial yarn (Cordenka® 700 Super 3; lin- action at the matrix/fibre interphase. It
ing an analysis of the microstructure, ear density /nominal/dtex=2440, number is possible that the epoxy groups of the
load-displacement curves, and finally of filaments 1350, breaking force 128.6 chain extender react chemically with the
determining the influence on the macro- N, single fibre diameter 12 μm) shows hydroxyl groups of cellulose, increasing
properties of the biocomposites. Since that a meaningful enhancement in me- bonding between the fibre and the matrix
impact strength is one of the most impor- chanical behaviour of the biocomposite (Figure 19) [24].
tant properties for biocomposite techni- can be achieved (Figure 18). Analogous
cal applications, all reinforcing effects of to unreinforced blends, CESA slightly
cellulose fibre on brittle polylactide com- influences the mechanical parameters.
n Future of biocomposites
posites must be utilised in every possible At lower chain extender contents, a lit- The demand for supplies of biocompos-
manner. One of them is the utilisation tle improvement can be seen; however, ites is growing in the world from year

FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96) 21
to year. This growth in Europe is actu- new processes or materials can be devel- Europe and the world, NOVA-Institut,
ally estimated at 32% per annum, from oped. The production costs consisting of 2012.
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22 FIBRES & TEXTILES in Eastern Europe 2012, Vol. 20, No. 6B (96)