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A Review
on Natural Fibre Based Composites–
Part I:
Structure, Processing and Properties
of Vegetable Fibres
J. Biagiotti
D. Puglia
José M. Kenny

ABSTRACT. Natural fibre-based composites have been intensely stud-

ied in the last years due to their specific properties and their clearly posi-
tive environmental impact. Other advantages of using vegetable fibres
are related to their economical production and processing, their safe han-
dling and working conditions. Therefore, lignocellulosic natural fibres
constitute an interesting alternative to traditional synthetic fibres in
composite materials. This work is intended to present an overview of the
main results presented in literature on this topic, focusing the attention
on the fibres properties in terms of physical and chemical structure, ther-
mal and mechanical properties. Some aspects related to the production
of vegetable fibres for composites are also presented. [Article copies avail-
able for a fee from The Haworth Document Delivery Service: 1-800-HAWORTH.
E-mail address: <docdelivery@haworthpress.com> Website: <http://www.
HaworthPress.com>  2004 by The Haworth Press, Inc. All rights reserved.]

J. Biagiotti, PhD Student, University of Perugia (E-mail: jerico@unipg.it). D.

Puglia, PhD Student, University of Perugia (E-mail: dpuglia@unipg.it). José M.
Kenny, Prof., University of Perugia (E-mail: kenny@unipg.it), all at the Materials En-
gineering Centre, University of Perugia, Loc. Pentima Bassa, 21 05100-Terni (Italy).
Part of the presented results has been obtained in the research work of the
ECOFINA Project, in the framework of the 5th European Research Program. We
would like to thank all the partner of the Project for the useful researches, and the other
colleagues that have kindly furnished their contributes.
Journal of Natural Fibers, Vol. 1(2) 2004
http://www.haworthpress.com/web/JSF
 2004 by The Haworth Press, Inc. All rights reserved.
Digital Object Identifier: 10.1300/J395v01n02_04 37
38 JOURNAL OF NATURAL FIBERS

KEYWORDS. Natural fibres, cellulose fibres, fibre processing, retting,

steam explosion, mechanical properties, thermal properties, composites

INTRODUCTION

After decades of high-tech development of artificial fibres such as carbon,

aramid and glass, it is remarkable that natural fibres such as kenaf, flax, jute,
hemp and sisal are still attracting renewed interest (English, Youngquist and
Krzysik 1994; Bledzki and Gassan 1999; Nabi Saheb and Jog 1999; Eichhorn
et al. 2001; Mohanty, Misra and Drzal 2002). In Figure 1 is shown the increas-
ing trend of the production of fibre crops in the world for all industrial applica-
tions along the last forty years.
The main advantages of using natural reinforcements in composite materi-
als, if compared with conventional synthetic fibres, can be summarized in the
following (Brower 2000; Peijs 2000):

• biodegradability, therefore they can be eliminated from the environment

after the life cycle;
• they can also be incinerated with energy recovery;
• lower specific weight which results in a higher specific strength and
stiffness than glass;
• renewable resource, so the production thereof requires little energy; CO2
is used while oxygen is given back to the environment;
• produced with low investment at a low cost which makes the material an
interesting product for low-wage countries;
• friendly processing with reduced wearing on tools;
• better working conditions and no skin irritation;
• good thermal and acoustic insulating properties.

On the other hand, some disadvantages may limit their application on an in-
dustrial level:

• variable quality depending on several factors including unpredictable in-

fluences, such as weather;
• moisture absorption which causes swelling of the fibres;
• limited maximum processing temperature;
• lower strength properties, in particular, impact strength;
• lower durability but fibre treatments can improve this considerably;
• poor fire resistance;
• prices may fluctuate according to harvest results or agricultural politics.
 Peer Reviewed Papers 39

FIGURE 1. Global fibre crops primary among the last forty years.

3 107

7
2.5 10
Fibre crops primary (Mt)

2 107

1.5 107

1 107
1960 1970 1980 1990 2000

Year

Most of the available information published over the last few years on natu-
ral fibre/wood composites dealt with several topics like identification and
classification of fibres, treatments and adaptation of natural fibres, study of
compatibility between fibre and matrix in composites, determination of fibre
and composite mechanical properties, humidity effects and, finally, potential
applications as substitutes for other materials. However, more extensive re-
search is necessary to assess the standard quality of the fibres that is a function
of raw material optimisation, growth-maturity-retting-decortication processes
and the use of advanced methods for the preparation and processing of fibres.
Moreover, in the case of their utilization as reinforcements in composite tech-
nology, it is also fundamental to improve the compatibility between the (hydro-
phobic-thermoplastic or hydrophilic-thermoset) matrix and the hydrophilic
cellulose-based natural fibres (Rowell 1995; George, Sreekala and Thomas
40 JOURNAL OF NATURAL FIBERS

2001; Joseph et al. 1996). The purpose of composite materials development is,
in fact, to obtain a product able to combine the positive properties of each con-
stituent component. In this sense, lignocellulosic reinforcements have been of
growing interest in the last few years due to their environmentally friendly as-
pect (Rowell 1998). In fact, environment legislation as well as consumer de-
mands are all increasing the manufacturing requirements of these materials
and final products to consider the virtual impact of the products at all stages of
their life cycle. The latter aspect validates the renewed interest that natural re-
inforcements have gained, especially as a glass fibre substitute in the automo-
tive industries (Brouwer 2000, Kenny 2001). Furthermore, the development
of specific manufacturing technologies has to be addressed in order to obtain
reliable products based on these materials.
Natural bio-based fibres may be classified in two main categories: non-
wood fibres and wood fibres (see Figure 2). Even so, the basic chemical struc-
tures of these kinds of fibres are similar in terms of the constituents varying
their composition fibre-to-fibre (Mohanty, Misra and Drzal 2002). Most natu-
ral leaf, bast and seed fibres are actually used as reinforcements in the composite
industry. Bast fibres (flax, jute, hemp) are typically the bests for improve-
ments in tensile and bending strength and modulus. Instead, coarse fibres such
as sisal and coir (coconut husk fibre) are better for toughness. In addition,
other kinds of fibres and fillers, obtained from the processing of wood, coir,
agave, hemp, jute, etc. as well as rice and nut hulls, cereal straws (oat, rye,

FIGURE 2. Classification of natural fibres.

NATURAL FIBRES

NON-WOOD FIBRES WOOD FIBRES

STRAW BAST LEAF SEED/FRUIT GRASS

i.e.: Flax, i.e.: Coir, i.e.: Soft and

Jute, Hemp Cotton Hard Woods

i.e.: Corn, i.e.: Sisal, i.e.: Bamboo,

Wheat, Rice Henequen Elephant grass
 Peer Reviewed Papers 41

wheat, etc.) and corn cobs can be used to improve dimensional stability and
stiffness.
The objective of this first part is to introduce the main aspects of vegetable
fibres used for composite materials by means of a general overview of the re-
sults presented in literature concerning this new typology of reinforcements,
focusing the attention on the fibre properties in terms of chemical and physical
structure, and on their thermal and mechanical characteristics. The second
parting will be devoted to the final utilization of vegetable fibres as reinforce-
ment of polymeric matrices (thermoplastics, thermosets and biodegradables),
and to the review the most used methods for the improvement of fibre-matrix
compatibility (physical and chemical treatments) with particular attention to
the application of natural fibre composites in the automotive industry.

NATURAL CELLULOSIC FIBRES

Chemistry

Cellulose based fillers are simple materials, both chemically and physi-
cally. If one ignores the absorbed water, the main constituents of cellu-
lose-based reinforcements consist of three types of chemicals: approximately
half thereof is cellulose and approximately a quarter thereof is hemicellulose
and lignin. Other extractives present in plant-sources include pectin and waxes
(Hon 1991; Bledski and Gassan 1996). The compositions of some plant-fibres
are shown in Table A.

Cellulose

The existence of cellulose as a common material in plant cell walls was first
discovered by Anselm Payen in 1838 (Payen 1838a, 1838b). A natural poly-
mer consisting of D-glucose (C6H12O6) monomer units, cellulose contains
glucose units which link together to form long unbranched chains. A schema-
tisation of cellulose structure is reported in Figure 3 (Nevell and Zeronian
1985). There are roughly 4,000 to 8,000 glucose molecules strung together.
The polymer chains in cellulose have a linear structure due to the 1,4-b
glycosidic linkages. The repeating unit in cellulose is actually made up of two
glucose units with each glucose unit in the linear chain being “turned over”
when compared with its preceding unit. Due to the positioning of the three
hydroxyl groups in each glucose monomer, strong hydrogen bonds are formed
between these groups and the hydroxyl groups on adjacent chains. Cellulose is
largely crystalline, organised into microfibrils and is very stable in normal en-
vironments. The H-bonding of many cellulose molecules to each other results
in the formation of microfibres that can interact to form fibres. Cellulose fibres
42 TABLE A. Chemical composition of some vegetable fibres.

Fibre Latin name Cellulose Hemi-cellulose Lignin Pectin References*

(wt.%) (wt.%) (wt.%) (wt.%)
Flax Linum usitatissimum 60-81 14-18.6 2-3 1.8-2.3 1
Jute Corchorus capsularis, C. olitorius 51-72 12-20.4 5-13 0.2 2
Abaca Musa textilis 60.8-64 21 12 0.8 3
Sisal Agave sisalana Perrine 43-88 10-13 4-12 0.8-2 4
Kenaf Hibiscus Cannabinus 36 21 18 2 5
Ramie Boehmeria nivea Gaud, variety tenacissima 68.6-76 13.1-15.0 0.6-1 1.9-2 6
Hemp Cannabis sativa L. 70-78 17.9-22 3.7-5 0.9 7
Cotton Gossypium spp.(commonest G. hirsutum) 82.7-92 2-5.7 0.5-1 5.7 8
Coir Cocos nucifera L. 43 0.3 45 4.0 9
Banana Musa acuminata L. 60-65 6-19 5-10 3-5 10
Henequén Agava fourcroydes Lemaire 60-78 4-28 8-13 3-4 5
Bagasse Saccharum officinarum L. 40 30 20 10 5
Pineapple Acanas Comosus 80-81 16-19 12 2-2.5 11
Wood - 45-50 23 27 - 11
*1. (Gassan, Chate and Bledzki 2001; Smeder and Liljedahl 1996; Bledski and Gassan 1999; Bledski, Reihmana and Gassan 1996 ; Mwaikambo and Ansell 2002).
2. (Gassan, Chate and Bledzki 2001; Smeder and Liljedahl 1996; Bledski and Gassan 1999; Bledski, Reihmana and Gassan 1996).
3. (RunCang Sun et al. 1998; Rowell et al. 1997).
4. (Joseph et al. 2002; Bledski and Gassan 1999; Rowell et al. 1997; Bledski, Reihmana and Gassan 1996; Mwaikambo and Ansell 2002).
5. (Klemm, Schmauder and Heinze 2001).
6,. (Bledski and Gassan 1999; Bledski, Reihmana and Gassan 1996; Mwaikambo and Ansell 2002).
7. (Bledski, Reihmana and Gassan 1996).
8. (Smeder and Liljedahl 1996; Bledski and Gassan 1999; Mwaikambo and Ansell 2002; Klemm, Schmauder and Heinze 2001).
9. (Gassan, Chate and Bledzki 2001; Bledski, Reihmana and Gassan 1996).
10. (Gassan, Chate and Bledzki 2001; Smeder and Liljedahl 1996)
11. (Gassan, Chate and Bledzki 2001).
 Peer Reviewed Papers 43

usually consist of over 500,000 cellulose molecules. So, if a fibre consists of

500,000 cellulose molecules with 5,000 glucose resides/cellulose molecules,
the fibre would contain about 2.5 billion H-bonds. Even if a H-bond has about
1/10 the strength of a covalent bond, the cumulative bonding energy of 2.5 bil-
lion of them is awesome. It is the H-bonding that forms the basis for the high
tensile strength of cellulose.
Cellulose I is the most common crystalline form (allomorph) of native cel-
lulose. Cellulose I is metastable and can be irreversibly converted into another
crystalline state, cellulose II, the most stable allomorph known (Ranby 1952)
differing from cellulose I in unit cell dimensions and, possibly, in chain polar-
ity (see Table B). Cellulose I has parallel glucan chains and strong intra-
molecular hydrogen bonds. In nature, cellulose I exist as two crystalline
sub-allomorphs, cellulose I-α and cellulose I-β (Atalla and Vanderhart 1984).
Cellulose II is seldom found naturally and is generally the product of re-pre-
cipitation after swelling and dissolution of cellulose I with various solvents. It
is more commonly known as “Rayon” (Roberts, Saxena and Brown 1989)
?The glucan chains of cellulose II are anti-parallel, probably as a result of
chain folding (Kuga, Takagi and Brown 1993). Other allomorphs of cellulose
such as cellulose III and IV are known but seldom, if ever, occur in nature.
Meyer, Mark, and Misch (Meyer and Mark 1928; Meyer and Misch 1937) pro-
posed a unit cell of the crystal lattice, already 60 years ago, that is still applica-

FIGURE 3. Haworth projection formula of cellulose. (Nevell and Zeronian 1985).

6
OH CH2OH OH
HO O 3⬘ 1⬘ CH2OH
O HO OH
HO 5 2 5⬘ 2⬘ O
O HO O H
3 4⬘ O HO
CH2OH OH 1 CH2OH OH
6⬘ n-2 O
Non-Reducing Anhydroglucose unit, AGU Reducing
End-Group (n = value of DP) End-Group

TABLE B. Unit cell dimensions of various cellulose allomorphs (Krassig, 1993).

Polymorph a-axis (Å) b-axis (Å) c-axis (Å) -axis (Å)

Cellulose I 7.85 8.17 10.34 96.4
Cellulose II 9.08 7.92 10.34 117.3
Cellulose III 7.74 7.74 10.30 122
Cellulose IV 8.11 8.11 10.30 90
44 JOURNAL OF NATURAL FIBERS

ble for practical purposes today (Figure 4). The dimensions of the cell are
reported in Table B.

Hemicellulose

A fourth form of sugar polymers found in biomass is hemicellulose.

Hemicellulose consists of short, highly branched chains of sugars (Figure 5). It
contains five-carbon sugars (usually D-xylose and L-arabinose), six-carbon
sugars (D-galactose, D-glucose and D-mannose) and uronic acid. The sugars are
highly substituted with acetic acid. Its branched nature renders hemicellulose
amorphous and relatively easy to hydrolyse to its constituent. When hydro-
lysed, the hemicellulose from hardwood releases products high in xylose (a
five-carbon sugar). The hemicellulose contained in softwood, in contrast, yields
more six-carbon sugars. In contrast to cellulose that is crystalline, strong and

FIGURE 4. Unit cell of cellulose I according to the Meyer-Misch model.

c = 79 Å
b = 103 Å

␤ = 84°

a = 8.35 Å
 Peer Reviewed Papers 45

FIGURE 5. Some monomers of hemicellulose.

H C O H C O H C O
HCOH CH2OH HCOH COOH CH2OH
HO C H
HOCH O HOCH O HOCH O
HCOH HCOH HCOH
HCOH HCOH HCOH
CH2OH COOH CH2OH
D - glucose D - glucuronic acid D - mannose

H C O H C O
HOCH HCOH
HCOH HOCH
HCOH HCOH
CH2OH CH2OH

D - arabinose D - xylose

resistant to hydrolysis, hemicellulose has a random, amorphous structure with

little strength. It is easily hydrolysed by dilute acid or base, but nature provides
an arsenal of hemicellulase enzymes for its hydrolysis. These enzymes are
commercially important because they open the structure of wood for easier
bleaching leading to the substitution of older methods of bleaching that con-
sume larger amounts of chemicals dangerous for the environment, such as
chlorine (Kuhad, Singh and Ericksson 1997).
All of the changes in the fibres dimensions with changing environmental
conditions can be attributed to hemicellulose swelling with adsorbed water.
Small ions like lithium and sodium can join and stabilise adsorbed water mole-
cules (the effects of sodium ions is more significant at low moisture contents
as they can raise the equilibrium moisture content by up to 2%). In dry condi-
tions, hemicellulose breaks down into carbon dioxide and water. At 20°C, this
degradation can already reduce wood weight by 1%. Under wet conditions,
acid hydrolysis accelerates the hemicellulose degradation into mostly sugar
molecules. Obviously, these degradation processes are faster at higher temper-
atures (Stamm 1971).

Lignin

Lignin is formed by the removal of water from sugar to create aromatic

structures. These reactions are not reversible. There are many possible mono-
46 JOURNAL OF NATURAL FIBERS

mers of lignin and the types and proportions depend on the source in nature.
Some typical monomers are shown in Figure 6a and an early stage in the con-
densation process of these monomers to form lignin is shown in Figure 6b. In
this last figure several chemical groups that may react further are highlighted.
Large lignin molecules are three-dimensional and are heavily cross-linked.
Sometimes lignin is isolated as a brown powder, but more often it is a gummy
mixture of lignins with a wide range of molecular weights. Lignin resists at-
tack by most microorganisms and anaerobic processes tend not to attack the
aromatic rings at all. The aerobic breakdown of lignin is slow and may take
months. Lignin together with hemicellulose is nature’s cement in the exploita-
tion of the strength of cellulose while conferring flexibility.

Physical Structure

Physically, vegetable fibres are a collection of long, thin, pointed cells

made up of cell walls on the outside and air on the inside. A simplified scheme
of the cell wall is shown in Figure 7a-b. Each cell wall has four layers, with the
“primary” layer on the outside and three “secondary” layers inside. The
amount of hemicellulose is about the same in each layer because the layers
need to swell and contract together without stress between them when the
moisture content changes. The cellulose content of each layer increases
steadily from the outer “primary” layer to the innermost “secondary” layer.
The lignin content consequently decreases in that sequence. The cellulose
microfibrils lie parallel to each other within each layer and spiral around the
cell’s long direction. Different layers have different angles of spiralling. The
hemicellulose combined with the lignin acts as glue that holds the layers to-
gether and the cellulose microfibrils within each layer. Most cells have their
long directions parallel to the direction of plant growth. The wall of each cell
has a cross-sectional shape that is rectangular with slightly rounded corners.
Adjacent cells have their walls glued to one-another by a mixture of about
three-quarters lignin and a quarter hemicellulose. The glue layer is about as
thick as an individual cell-wall layer except at the rounded corners, where it
fills the space. Pairs of glued-together adjacent cell walls act as structural
units. There are evenly-spaced holes in the cell walls called “pits” which usu-
ally line up with similar holes in adjacent cell walls. These holes allow the pas-
sage of water or air between the cells and ultimately between the inside and
outside of the fibre.
So, vegetable fibres can be considered as advanced composite materials
themselves with a taylor made distribution of structural cellulose fibres in a
functional hemicellulose-lignin matrix that has also taylor-made mechanical
and diffusion control properties.
 Peer Reviewed Papers 47

FIGURE 6. Some typical monomers of the lignin (a) and early stage in their
condensation (b).

CH3 HC O CH2OH

CH2 CH C O
CH2
CH HCOH

CH3O CH3O HO
O O O
H
CH3 CH3

(a)

CH2OH

C O

HCOH

HC O
CH2OH
CH CH3O
C O
CH
CH2 O
HCOH OH
C O

CH3O HCOH
O
HCOH
O
C O

O CH2OH
H

(b)
48

FIGURE 7. Scheme of the morphological architecture of a cotton fibre (a) and a delignified spruce wood (b).

Secondary wall
Lumen Secondary wall
Inner layer (S1)
Inner layer (S1)

Middle layer (S2)

Middle layer (S2)

Outer layer (S1)
Primary wall

Outer layer (S1)

Primary wall
Middle lamella
Cuticle

(a) (b)
 Peer Reviewed Papers 49

Fibre Production

After the planting and growing phase, which takes about one year, depend-
ing on the variety of the plant and the final desired quality, the fibres are har-
vested. In general, the harvesting should tend to preserve the maximum final
length of the fibre. In fact, as in the case of their application as composite rein-
forcements, the greater the aspect ratio (length/diameter) of the fibre, the
better the improvement of the final mechanical properties.
A simple process, named decortication, is also normally used to extract leaf
fibres. Leaves are crushed and beaten by a rotating wheel set with blunt
knives, so that only the fibres remain. All the other parts of the leaf are washed
away by water. Decorticated fibres are then washed before drying them in the
sun or with hot air. The dry fibres are machine combed and sorted into various
grades, largely on the basis of the previous in-field separation of leaves into
size groups (Yayock, Lombin and Owonubi, 1988).
The extraction of bast fibres from the stems of the plant-fibres is in general
accomplished through retting processes, described hereunder.

Retting

Retting is a microbial process that breaks the chemical bonds that hold the
stem together and allows separation of the bast fibres from the woody core.
The two traditional types of retting are field retting and water retting. With
field or dew retting, plant stems are cut or pulled up and left in the field to rot.
Farmers monitor the process closely to ensure that the bast fibres separate
from the inner core without much deterioration in quality. Moisture is needed
for the microbial breakdown to occur, but then the weather must be dry
enough for the stalks to dry for bailing. Although varying weather conditions
affect the quality of the fibre, field retting has been used extensively because it
is inexpensive, mechanized and does not use water. Currently, dew-retting,
which depends on indigenous, aerobic fungi to colonize pulled plants in the
fields, is the accepted practice in European countries and accounts for much of
the fibres used in textiles. However, the disadvantages of dew retting include:
(1) the dependence on particular geographical regions that have the appropri-
ate moisture and temperature ranges for retting, (2) coarser and lower quality
fibres than those produced with water-retting, (3) less consistency in fibre
characteristics and (4) the occupation of agricultural fields for several weeks
(Van Sumere 1992). Dew-retting further results in a heavily contaminated fi-
bre that is particularly disadvantageous in cotton textile mills. On the other
hand, water retting produces more uniform and high-quality fibre but the pro-
cess is very labour and capital intensive. In this case, stems are immersed in
water (rivers, ponds or tanks) and monitored frequently. Not only is this labour
intensive, but farmers and/or workers must also have the necessary knowledge
50 JOURNAL OF NATURAL FIBERS

regarding fibre quality. Furthermore, the process uses large volumes of clean
water that must be treated before being discharged. Water retting, which was
formerly the method of choice because of high quality fibre, produces envi-
ronmentally unacceptable fermentation waste (Sharma and Van Sumere, 1992a;
Sharma and Van Sumere, 1992b). This practice was mostly discontinued in
western countries several decades ago because of the pollution from fermenta-
tion products and the high cost of drying (Brown, 1984).
An alternative that has had long-term consideration is the use of enzymes in
controlled reactors. Scientists speculate that improved microorganisms or di-
rect use of enzymes may allow countries in Europe and North America to pro-
duce textile-quality bast fibres. The cost of the enzymes, and perhaps other
less obvious reasons, have prevented a further development of a commercial
enzyme-retting process and dew-retting remains the most widely used practice
in Europe to obtain fibres commercially for industrial use, despite continuing
research on other methods. In this scenery, the work performed by the Finnish
factory Finflax, as a partner of the European Project ECOFINA (Ecoefficient
Technologies and Products based on Natural Fibre Composites) as a provider
of flax fibre can be mentioned as they uses a controlled enzymatic retting of
flax fibre to obtain a higher quality fibre for composite materials (Kenny
2003). In this process, the anatomy of the fibres and fibre bundles determines
on a large extent the final fibre quality and yield and it is also dependent on the
flax cultivation and growth conditions within the stem. The quality of the
fibres is also largely determined by the shape of the bundles; oval or kid-
ney-shaped fibre bundles being characteristics of good quality flax, while ir-
regular bundles are indicative of poor quality flax. Furthermore, both fibre
yield and quality are strongly dependent on the characteristics of the cell
walls, for example, better fibre quality and higher yields correspond with
thicker cell walls, while fibre strength is mainly determined by the cell shape
and the characteristics of the middle lamellae.
In order to achieve good quality fibre, it is important to focus on all the
steps in the refining process. The selection of flax, to be retted industrially,
must start already at beginning of the production of the raw material, in partic-
ular microbiological and microscopical (light and electron microscopy) exam-
inations should be taken into account. Microbiological tests are performed
using standard plate culture methods in order to investigate the quality of the
fibre. This was examined with an optical microscope (Figures 8a-b). A well
formed fibre bundle, oval cross section form of fibres and well packed fibre
cells are signs of good quality fibres. The number of fibre bundles vary from
stem to stem and depend on which part of the stem is used. For example, bun-
dles are less numerous at the top of the plant than at the root, while most bun-
dles are found in the middle part of the stem. The number of fibre bundles
varies from 15 to 35. A fibre bundle usually contains from 10 to 40 fibre cells
 Peer Reviewed Papers 51

FIGURE 8. Before retting cross-section, of (a) portion of the flax stem and
(b) flax fibre bundle with surrounding tissue.

(a)

(b)
52 JOURNAL OF NATURAL FIBERS

having a diameter of 20 to 30 µm. The amount of fibre cells differ from bundle
to bundle, the largest amount being found in the middle part of the stem. The
primary wall of the flax fibre cell contains pectic substances, occasionally
with traces of lignin, whereas the secondary layers consist mainly of cellulose.
The retting time may easily vary (12-24 hours) depending on the enzyme con-
centration, the type of fibres to be retted and the final quality of fibres required
for different technical applications. Figures 9a-b show the quality of the flax
fibres retted enzymatically by the Arctic-Flax Process used by Finflax. The
enzymes break the pectin substances of the flax fibre cell walls. The retting
time is over 22 hours, because the aim is to break off the fibre bundle and pro-
duce elementary fibres.

Fibre Separation

Once the stalks are retted, dried and baled, they are processed by mechani-
cal separation, in a process called scutching that include two operations:
breaking and swingling. In the breaking, stalks are passed between fluted roll-
ers to crush and break the woody core into short pieces of less than 1 cm
length, called shives. Swingling is the removal of the shives and is achieved by
tangential scraping of the broken stems. The process of long fibre scutching
produces two kinds of fibres, scutched flax (long fibre) and tow (short fibre).
Although partially mechanized, these procedures are functionally identical to
traditional methods by hand of preparing line fibre and tow for twisting into
twine or rope or for spinning into yarn. Not only are these methods time con-
suming but they also require skilled workers and a considerable investment in
capital equipment.
It is also possible to mechanically convert virtually all of the bast fibre di-
rectly into tow using flax breaking and tow processing machinery. This elimi-
nates traditional scutching and allows the processing of randomly-oriented
baled straw. Compared to scutching machinery, tow-processing equipment
usually has a higher throughput, requires fewer and less skilled workers and
costs less. However, a tow processing system cuts all of the bast fibre into
short lengths, making it appropriate only for lower value uses, such as pulp
and paper, instead of textiles or composites.

Hackling

This is the final process before spinning. It is the removal of all bits of fibre
straw and all short fibres (tow). There are three to four sets of hackles, starting
with the very coarse set and continuing on to the very fine toothed set. The
fibres are flicked over the coarsest hackle first until no coarse fibres can be re-
moved from the fibres held in hand. This process is repeated with the second
coarsest hackle, using only the fibre remaining in the hand. Flicking and draw-
 Peer Reviewed Papers 53

FIGURE 9. The end-point of the enzymatic retting (a), followed by the breaking
of pectic substances of the flax fibre cell (b).

(a)

(b)
54 JOURNAL OF NATURAL FIBERS

ing continues through the various hackles until the fibre remaining in the hand
is of a smooth and consistent length.
The fibre remaining in the hand is called a line, strick, hank or lint. The fi-
bre remaining in the hackles is removed and the hackling process is repeated.
This fibre is called tow and is used for sacking, candle wicks, tow ropes and
other similar coarse materials. The straw remaining is used in bedding and is
considered to repel fleas and lice.

Spinning, Weaving and Finishing

In spinning, the fine fibres are twisted together to obtain a yarn. Finer yarns
are generally spun with water (wet spun) and the coarser yarns are dry spun.
The weaver will generally use wet spun yarns for nicer apparel and household
fabrics and dry spun (tow) for coarser upholstery items. The basic principles of
weaving have not changed since linen was first invented. However, technol-
ogy has changed considerably over the centuries, and today weaving is a very
sophisticated operation. The non-wovens were manufactured by a full-scale
scutching, opening, carding and needle-punch process. The technological pa-
rameters have an extended influence on the fabric and the later composite
properties; needle penetration and stitch density in needling can change the
tensile strength, the flexing resistance and the E-modulus. The objective of
carding is to open the processed fibre without damaging its technical proper-
ties. The carding functions are:

• opening the fibre bundles into single fibres and cleaning of the fibres
• unidirectionaling and straightening of the fibres
• removal of very short fibres
The fibres can be processed with the non-woven carding process. After
carding, the fibres can be also processed into different square-weighted mats
by needle-punching.

Steam Explosion

Research in Europe has sought methods for separating bast fibre that by-
pass traditional retting and scutching. Steam explosion and ultrasound are un-
der investigation in Germany, but the processes produce short fibres only
(D’Agostino, Richard and Taylor 1996; Kessler et al. 1998). In the early
1930’s, Charles V. Rowell published a patent, which used the technique of
steam explosion to extract fibres from agricultural wastes (Rowell 1932). In
the 1970’s and 1980’s, several commercial and academic organizations began
conducting research and development that explored other applications for
steam explosion, including the production of cattle-feed, ethanol and specialty
 Peer Reviewed Papers 55

chemicals from wood fibres. Certain heat transfer limitations which hinder
process optimisation are associated with batch steam explosion. In 1986, an
experimental station that uses steam explosion (STEX) started in Germany to
produce short staple linen fibres and can be processed on a highly productive
cotton line in mixtures. The processing of flax by STEX can be adjusted to
variable raw material quality and provides short fibres of high purity and
free-ness due to a chemical treatment during steaming and a mechanical action
when the material is expelled from the reaction chamber.
Steam explosion generally refers to the process of exposing fibres to
high-pressure steam (typically 200-450 psi) for a period of 1-10 minutes and
then explosively discharging the product to atmospheric pressure. The process
has, in the past, been mistakenly described as a physical treatment. However,
it is now well accepted that the process is chemical in nature and is controlled
by temperature and time. In order to utilize the fibres, it is necessary to sepa-
rate the lignin from the cellulose. In the past, it was only possible to break the
bonding between the cellulose and the lignin through very expensive and high
polluting chemical pulping processes. Continuous steam explosion pulping
uses high-pressure steam, under controlled conditions of time and tempera-
ture, to alter the natural structure of lignocellulosic materials and achieves sig-
nificant reductions in chemical requirements and refining energy. The strength
characteristics of the resulting pulps are improved and respond well to bleach-
ing with hydrogen peroxide. In Figure 10, a schematic diagram of the steam
explosion treatment of decorticated flax fibre is shown (Kessler et al. 1998).
The decorticated fibre bundles are impregnated with NaOH at a concentration
range of 0.1-0.5% wt at different temperatures (20-120°C) in the reaction
chamber. After releasing the surplus base, the material is subjected to satu-
rated steam. According to the specified steam treatment, the material is ex-
truded into a cyclone by suddenly opening the extrusion valve at the defined
release pressure. The degraded materials, like pectin and hemicellulose are
then extracted by alkaline scouring. Following the wash cycle, the fibres are
dried at room temperature, opened on a standard opener and carded.
In conclusion, natural fibres processed by steam explosion offer the oppor-
tunity for high-tech applications in textiles as well as in technical applications
which may balance farming and productions costs, for its better spinnability in
comparison to mechanically cottonized flax, due to a higher degree of free-
ness, homogeneity and purity.

Thermal Properties

Main thermal properties of vegetable fibres for composite materials are

thermal expansion and thermal degradation. In spite of other clear advantages,
the thermal properties of vegetable fibres represent a clear drawback in com-
56 JOURNAL OF NATURAL FIBERS

FIGURE 10. Schematic representation of the flax steam explosion treatment.

Processing and Variables

Low Decorticated Flax Straw High

disintegration (Maturity, retting degree, variety, etc.) disintegration

Impregnation
(Chemicals, temperature, time, etc.)

Steam Explosion
(Temperature, time, extrusion speed)

Scouring
(Procedure, chemicals, etc.)

Hemicellulose, Hemicellulose,
Pectin, Lignin Pectin, Lignin,
Cellulose
Knots, fibre Opening, Carding Fibre fragments,
bundles trash

Short Staple Fibres

parison with synthetic fibres. Regarding thermal expansion only few data are
available in the scientific literature with values of the corresponding coeffi-
cient ranging in the order of 3⭈10⫺5, while glass fibres are in the order of
5⭈10⫺6. On the other hand, thermogravimetric and differential scanning calo-
rimetric analysis demonstrate that noticeable mass loss in natural fibres start at
about 200-220°C; above this temperature irreversible degradation of the fibres
occurs (Wielage et al. 1999). The relative low degradation temperatures of
vegetable reinforcements, in comparison with the process temperatures of
polymeric matrices, represents the most important limit for their use in plastics
with the conventional processing equipments (extruder, injection moulding,
etc). However, the thermal stability of the cellulose-based fibres can be im-
proved with several physical and chemical treatments as described in the sec-
ond part of this work. Therefore, an intense research activity on the thermal
degradation of vegetable fibres for composites has been reported in the scien-
tific literature. Only some results, related to the effects of chemical treatments
on the thermal stability of natural fibres are reported here as examples. Rana et
al. investigated the thermal behaviour of untreated and acetylated jute fibres,
characterizing the hemicellulose and α-cellulose decomposition temperatures
 Peer Reviewed Papers 57

(found also in DSC tests) and showing the missing of the first peak and the in-
crease of the second peak temperature for treated fibres, due to higher thermal
stability (Rana et al. 1997). Albano et al. studied the effect of acetylated and
non-acetylated sisal fibres on the thermal degradation of blends of PP and
polyolefins, especially PP/HDPE/functionalized EPR and PP/HDPE/non-
functionalized EPR (Albano et al. 1999). The studies have shown that the
starting temperature of the decomposition of the fibre, whether treated or not,
was maintained almost at the same level and acetylated fibre stability was also
found to increase with a higher activation energy value (for acetylated fibre).
A change in the degradation mechanisms with two stages degradation for the
treated fibres was also observed.
Thermogravimetric analysis, TGA, of untreated and different surface mod-
ified jute fibres was also performed by Mohanty et al. (Mohanty, Khan and
Hinrichsen 2000) for the realization of composites based on a Biopol matrix;
all surface modified fabrics show the same or better thermal stability com-
pared to untreated fabrics. Typical TGA curves of some untreated vegetable
fibres are illustrate in Figure 11. In any case processing and service tempera-
tures for vegetable fibres cannot exceed 200-200°C limiting the availability of
suitable polymeric matrix. These aspects will be specifically addressed in the
second part of this review.
Although many research reports indicate that natural fibres exhibit a com-
plicated anisotropic structure, unfortunately the anisotropy property of most
natural fibres has been left undetermined. For example, the jute fibres investi-
gated by Cichocki and Thomason exhibited considerable elastic and thermal
expansion anisotropy (Cichocki and Thomason 2002). The longitudinal Young’s
modulus of the fibre was determined to exceed the transverse fibre modulus by
as much as an order of magnitude in certain temperature regimes. The fibres
exhibited negative thermal expansion coefficients along their lengths; how-
ever, large positive thermal expansion coefficients, similar in magnitude to
many polymeric materials, have been estimated in the transverse directions.

Mechanical Properties

The properties of the fibres are determined by the physical, mechanical and
chemical properties of the morphological constituents and their interfaces.
Main physical characteristics found in literature regarding the most widely
known natural fibres are reported in Table C. Natural fibre consists of highly
crystalline cellulose fibrils spirally wound in a matrix of amorphous hemi-
cellulose, lignin and, eventually, pectin. Lignin and pectin act mainly as bond-
ing agents. The characteristic values of the structural parameters vary from
one fibre to another. In the case of flax fibre, they are oriented with a tilt angle
of 10° to the axis of the fibre and hence display a unidirectional structure (Bos
58 JOURNAL OF NATURAL FIBERS

FIGURE 11. Typical thermogravimetric curves for some natural fibres.

100 0.16

0.14

80 flax
jute
sisal 0.12
abaca

0.1

DTG (µg/µgi min)

Weight loss (%)

60

0.08

40
0.06

0.04
20

0.02

0 0
100 150 200 250 300 350 400 450 500
Temperature (°C)

and Donald 1999). In a recent research the Young’s modulus of a flax fibre
was estimated by taking into account the composition of the fibre and the evo-
lution of the orientation of the fibrils during a tensile test, using micro-me-
chanical equations well compared with experimental results (Baley 2002).
The calculation of the elastic properties of cellulose based natural fibres
was performed by Gassan et al. (Gassan, Chate and Bledzki 2001) by means of
different mechanical models. The results shown how the modulus in fibre axis
decreases with an increasing spiral angle and degree of anisotropy, while shear
modulus reached a maximum value at a spiral angle of 45°. Moreover, the de-
gree of anisotropy was only affected by the cellulose content in the range be-
tween 35 and 90%, which is the typical content for most natural fibres.
Eichhorn et al. (Eichhorn, Sirichaist and Young 2001) utilized Raman spec-
troscopy in order to probe the deformation mechanism of cellulose fibres.
During tensile deformation, the 1095 cm⫺1 Raman band, corresponding to the
 TABLE C. Main physical properties of cellulose based fibres compared with conventional synthetic fibres.

Fiber Density Diameter Elongation Tensile Young’s Specific Price References*

(g/cm3) (µm) at break strength Modulus modulus (€/Kg)
(%) (MPa) (GPa) (GPa⭈cm3/g)
Flax 1.40-1.50 40-620 2.7-3.2 343-1035 27-80 19-53 2.29-11.47 1
Jute 1.30-1.50 30-140 1.4-3.1 187-773 3-55 2-37 0.12-0.35 1
Abaca 1.50 17-21 10-12 980 72 48 0.81-0.92 2
Sisal 1.30-1.50 100-300 2.0-2.9 507-855 9.0-28.0 7-19 0.70-1.02 3
Kenaf 1.22-1.40 40-90 3.7-6.9 295-930 22-53 18-38 0.53-0.61 2
Ramie 1.50 40-60 3.6-3.8 400-938 44-128 29-85 1.44-2.40 4
Hemp 1.40-1.50 16-50 1.3-4.7 580-1110 3-90 2-60 0.57-1.73 5
Cotton 1.50-1.60 16-21 2.0-10.0 287-597 5.5-12.6 4-8 1.61-4.59 6
Coir 1.25-1.50 100-450 15.0-47.0 106-270 3.0-6.0 2-4 0.24-0.48 7
Banana 1.30-1.35 50-280 3-10 529-914 7.7-32.0 6-24 0.7-0.9 8
Henequén 1.49 20-500 3.0-5.0 430-580 10.1-16.3 7-11 0.38-0.67 8
Bagasse 0.55-1.25 200-400 0.9 20-290 2.7-17.0 5-14 0.15 9
Pineapple 1.52-1.56 200-8800 0.8-3.0 170-1627 6.21-82 4-53 0.36-0.72 10

E-glass 2.50-2.55 10-20 2.5 2000-3500 73.0 29 1.25 11

Aramide 1.40-1.45 12 3.3-3.7 3000-3150 63.0-67.0 45-48 7.20 11
Carbon 1.40-1.75 5.5-6.9 1.4-1.8 4000 230.0-240.0 164-171 12.0 11
*1. (Gassan and Bledzki 1999; Van Rijswijk and Brouwer 2002).
2. (Karus, Kaup and Lohmeyer 2000).
3. (Gassan and Bledzki 1999; Kalaprasad, Joseph and Thomas 1997; Nabi Saheb and Jog 1999).
4. (Gassan and Bledzki 1999; Van Rijswijk and Brouwer 2002; Vázquez and Domínguez 1999).
5. (Van Rijswijk and Brouwer 2002).
6. (Gassan and Bledzki 1999; Baley, D’Anselme and Guyader 1997).
7. (Van Rijswijk and Brouwer 2002; Baley, D’Anselme and Guyader 1997; Geethemma et al. 1998).
8. (Baley, D’Anselme and Guyader 1997).
9. (Vázquez, Domínguez and Kenny, 1999).
10. (Nabi Saheb and Jog 1999; Uma Devi, Bhagawan and Thomas 1997; Satyanarayana et al. 1990; Geethemma et al. 1998).
59

11. (Saechtling 1987).

60 JOURNAL OF NATURAL FIBERS

stretching of the cellulose ring structure, shifted towards a lower wavenumber

due to molecular deformation.
In contrast with more uniform synthetic fibres, whose properties can be eas-
ily and univocally determined, natural fibres are characterized by a large dis-
persion of their characteristics, as evidenced in Figure 12. Tensile properties
of natural fibres exhibit considerable scatter thus requiring statistical analysis
(Bledski and Gassan 1999; Biagiotti et al. 2003). The two-parameter Weibull
distribution (Weibull 1951), which expresses the cumulative density function
of the studied property of the fibres as:

 E a
( )
F Ef = 1 − exp −
f
 
  E0  
(1)
 

FIGURE 12. Comparison between Weibull distributions of flax and glass fibres.
(Biagiotti et al. 2003).

Flax fibre
Glass fibre
Weibull model
0.8
Probability of failture

0.6

0.4

0.2

0
101 102 103 104 105
Tensile strength (MPa)
 Peer Reviewed Papers 61

where a is a dimensionless shape parameter and E0 is a location parameter, is

found to provide good agreement with the natural fibres tensile data (elastic
modulus and tensile strength) (Van de Weyenberg, Ivens and Verpoest 2000).
However, for a more accurate modelling the three-parameter Weibull model is
some times adopted (Kompella and Lambros 2002; Joffe, Andersons and
Wallstrom 2002). Such features make it necessary to utilize a more systematic
statistical approach to define their properties and those of their relative com-
posites (Hu and Hsieh 1997). In order to describe the mechanical characteris-
tics of natural fibres, a preliminary study was conducted using statistical
representations based on the probability density functions of the quantities of
interest (Biagiotti et al. 2003). The variation of the elastic modulus and the ten-
sile strength of the natural fibres with the diameter size were predicted in a first
approach, by means of the model proposed by Griffith (Griffith 1921). Then,
the statistical approach presented utilized the distribution of the geometric
properties of the measured fibres, over a post-processed composite, to obtain a
statistical distribution of the mechanical response of the composite through
the non-linear equations arising from the combination of mechanical models.
The true distribution functions were explicitly estimated with the help of
semi-parametric algorithms, drawn from the neural network literature.

Influence of Environmental Conditions on Fibre Properties

It is well established that natural fibres are susceptible to moisture (McKenzie

1979; Maldas and Kokta 1989). Cellulose, which is the main constituent of the
cell wall of natural reinforcements, in fact, contains numerous hydroxyl
groups that are strongly hydrophilic. The moisture content of natural fibre is
also a function of the fraction of non-crystalline regions and of void content
(Bledzki and Gassan 1999). Therefore, natural fibre-reinforced composites
can absorb a great amount of water, which generally causes a reduction in their
mechanical properties (Karmaker 1994). Generally, the water content in these
systems is about 10-20 %wt. under standard conditions. The rate of water ab-
sorption in a composite depends on many factors: the kind of fibre and matrix,
temperature conditions, differences in water distribution within the compos-
ite, reaction between water and the matrix and others variables (Wolff 1993).
Both the rate of water pick-up and the total amount of moisture absorbed de-
pend on the chemical structure of the resin and crosslinking agent together
with the temperature and relative humidity. The moisture absorbed not only
plasticizes the matrix resin, but also changes the state of stress in favour of
cracking through swelling (Pritchard and Speake 1987). Moisture effects in fi-
bre-reinforced plastic composites have been studied extensively during the
lasts two decades (Mahlberg et al. 2001). This drawback represents one of the
major restrictions of natural fibre in durable composite applications for the
62 JOURNAL OF NATURAL FIBERS

consequent poor dimensional stability (swelling) and their susceptibility to

rotting (Peijs et al. 1998). Swelling of fibres can lead to microcracking of the
composite and degradation of the mechanical properties. Moreover, the pro-
cessing of thermoplastic matrix based composites and the moisture content
can lead to poor processability and porous products due to the evaporation of
water during the conventional thermal steps of the process. At the fibre/matrix
interface, moisture may reduce the bond strength by breaking the bonds
(Chua, Dai and Piggot 1992).
Other environmental factors, such as solvents, oil and radiation can also in-
fluence the properties of natural materials during their service-life (George,
Bhagawan and Thomas 1998). At lower temperatures, the translational free-
dom of water molecules is slowly hindered by the stiffness of polymer chain
segments. Moisture diffuses into a polymer to varying degrees depending on
molecular and microstructural aspects such as polarity, the extent of crystal-
linity of thermoplastics and the presence of residual hardeners or other water-
attracting species (Jones 1994). In the absence of radiation, the environmental
degradation of the mechanical properties of polymers is generally associated
with plasticization, weight loss, micro-mechanical damage and blistering, in-
duced by the sorbed solvents. Loss of material by leaching after longer time
periods also leads to effective damage.
The moisture absorption of fibres can be minimized in the composite by en-
capsulation by the polymer and good fibre-matrix adhesion. Good adhesion
can also reduce the rate and amount of water absorbed in the interphase region
of the composite. It is difficult to entirely eliminate the absorption of moisture
without using expensive surface barriers on the composite surface (Rowell et
al. 1999). The moisture resistance of natural fibres can, however, be improved
through fibre treatments like acetylation and a novel upgrading process based
on three steps: hydro-thermolysis, drying and curing of flax fibre (Stamboulis,
Baillie and Peijs 2001).

CONCLUSIONS

The recent environment-conservative regulations have motivated new ef-

forts in research and development of new products and processes reducing fur-
ther dependency on oil reserves. The possibility to use natural fibres as
reinforcements for composite materials offers an adequate reply to these con-
siderations. The lower specific gravity of the cellulosic-based fibers (approxi-
mately 1.4 g/cm3 as compared to about 2.5 g/cm3 for mineral based systems)
leads to weight savings in composite structures with direct implications in
transport applications. Moreover, their specific mechanical properties appear
to be competitive to the other conventional fibres. Costs of natural fibres are,
 Peer Reviewed Papers 63

in general, close or lower than plastic and high fibre loading can result in sig-
nificant material cost savings. Other advantages can be found in their non-
abrasive nature. In fact, reduced equipments abrasion and the subsequent re-
duction of re-tooling costs through the use of natural fibres is a factor that will
be considered by the plastics industry when evaluating the use natural fibres.
On the other hand, despite the numerous advantages that vegetable fibres
present in a first approach, the series of drawbacks discussed in previous para-
graphs (scattered mechanical properties, low process temperatures, easy mois-
ture absorption, etc) can limit their utilisation in industrial scale. Then, although
extensive research efforts have been dedicated to the production of industrial
vegetable fibres suitable for composite materials several aspects still require
attention before this industrial sector can be considered as mature.

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