Materials Letters 63 (2009) 61–63

Effect of pre-treatment of Luffa fibres on the structural properties

L. Ghali a,⁎, S. Msahli a, M. Zidi b, F. Sakli a
a Textile Research Unit of ISET Ksar Hellal 5070, Monastir, Tunisia b Laboratory of Mechanical Engineering, National School of Engineering of Monastir 5000, Tunisia
a r t i c l e i n f o a b s t r a c t Article history: Received 26 March 2008 Accepted 1 September 2008 Available online 9 September 2008
Keywords: Luffa fibres Electron microscopy X-ray techniques Crystallinity Chemical treatment
⁎ Corresponding author. Tel.: +216 97 66 33 93.
E-mail address: ghali_las@yahoo.fr (L. Ghali).
Recently, the use of lignocellulosic fibres to reinforcing composite has received an increased attention. However, lack of good interfacial adhesion makes
important the treatment of raw materials. Chemical treatment prepared the raw material to be useful by elimination of gummy and waxy substances. In this study,
the Luffa fibres were treated by tow methods: alkali treatment and mixed treatment (sodium hydroxide and hydrogen peroxide). The effect of these treatments on
the structure of fibres was showed using SEM and XRD (X-Ray Diffraction) analysis. The SEM results revealed that both treatments resulted in a removal of
lignin, pectin and hemicellulose substances, and change the characteristics of the surface topography. The XRD analysis shows the increase of crystallinity index
by many treatment conditions. We find that the alkali treatment (120 °C; 3 h; 4% NaOH) shows a good cleaning and the higher crystallinity index of treated fibres.
It is also interesting to note that mixed treatment can change the Luffa fibres from mat structure to fibrils structure.
© 2008 Elsevier B.V. All rights reserved.
1. Introduction
The sponge gourd, fruit of Luffa cylindrica, has a ligneous netting system in which the fibrous cords are disposed in a multidirectional array
forming a natural mat. This fibrous vascular system is composed of fibrils glued together with natural resinous materials of plant tissue. Gianpietro
et al. [1] has reported that the fibres of L. cylindrica were composed of 60% cellulose, 30% hemicellulose and 10% lignin.
Recently, the L. cylindrica have been used as support of immobi- lization for the discolouration of certain solutions [2–10] and dyeing water
[5–9]. Indeed, Akhtar et al. [2–4] showed that the Luffa sponge gave good results during its use as support to produce a new system of sorption to
remove the cadmium, the Chromium III and nickel II ions from the contaminated aqueous mediums.
Some other studies characterized the Luffa fibres [11] for other technical applications such as reinforcing composite materials [12,13]. Tanobe et
al. [11] prepared a data characterizingfibres extracted from Brazilian sponge gourd. It has been found that the physical properties of Luffa fibres
must be enhanced by chemical or physical modifications to make them more useful in composite. In this work, we investigate the influence of
changing chemical treatment parameters on the structure of pre-treated Luffa fibres. The conservation of the mat structure of Luffa fibres and a
high crystallinity index after chemical treatment has a good interest in their technical use. The Luffa fibre samples are characterized by using
Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) to explore the structure change.
2. Materials and methods
2.1. Treatment of Luffa fibres
The Luffa sponge, collected from Tunisia, used in this study was washed three times in hot water, then with 0.2% lauryl sulphate solution under
continuous stirring at 60 °C for 30 min to ensure good cleaning [14]. Cell-fibres of L. cylindrica were extracted from fibrous stands by tow
methods. In the first method, a solution containing both sodium hydroxide and anthraquinone is used to remove waxy and gummy
Table 1 Crystallinity index of untreated and treated Luffa fibres

Treatment method Treatment conditions (T°C–Temps–% of NaOH–% H2O2) Icr (%) Untreated Untreated 50.00 Alkali treatment 80–3–8 66.32 100–3–8 70.56 120–3–4 70.84
120–1–12 68.18 Mixed treatment 100–1–2–10 65.18 100–1–4–10 65.24 100–1–6–10 65.72 100–1–8–5 67.66 100–1–8–10 67.40 100–1–8–15 68.88 100–2–8–10 67.61
100–3–8–10 67.82 100–1–10–10 67.09 120–1–8–5 69.03 120–1–8–10 66.07 120–1–8–15 70.10
0167-577X/$ – see front matter © 2008 Elsevier B.V. All rights reserved. doi:10.1016/j.matlet.2008.09.008
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substances (Table 1). In the second method, cleaned Luffa fibres are treated by solution containing both sodium hydroxide and hydrogen peroxide
mixed treatment (Table 1). In these two methods the sodium hydroxide was used as a reagent for the delignification of Luffa fibres, the
anthraquinone to catalyse the reaction of delignification and the hydrogen peroxide as bleaching reagent. The duration of treatment, the soda
concentration, percentage of hydrogen peroxide and the temperature are variable parameters. The obtained fibres are washed several times with
distilled water and dried at 80 °C during 2 h.
2.2. Scanning microscopy analysis
A Phillips Scanning Electron Microscopy (SEM) is used to examine the morphology and the fibre surface topography before and after chemical
treatments.
2.3. X-Ray Diffraction analysis
The crystallinity index of the tested fibres was calculated from X- Ray Diffraction patterns recorded on an X'Pert pro MPD X-ray diffractometer.
Diffractograms were obtained by varying angle (2θ) from 4° to 65°. The crystallinity index (Icr %) of the fibre was calculated using the following
formula [15]:
I −I
Icr k( )= 002 am ( )
I002 x 100
 where I002 is the maximum intensity of diffraction of the (002) lattice peak at a 2θ angle between 22° and 23° and Iam is the intensity of
62 L. Ghali et al. / Materials Letters 63 (2009) 61–63
Fig. 2. SEM micrographs of a) gross morphology of untreated Luffa fibres; b) fibrillary structure of treated fibres.
Fig. 1. SEM micrographs of a) untreated Luffa fibres; b) Alkali treated Luffa fibres.
diffraction of the amorphous material, which is taken at a 2θ angle between 18° and 19° when the intensity is minimal.
3. Results and discussions
Fig. 1 shows the morphology of treated and untreated Luffa fibres obtained using SEM analysis. We note that the alkali treatment removes the waxy and gummy substances observed
in the untreated Luffa fibres. The topography of the surface of
Fig. 3. X-Ray Diffraction patterns of untreated and treated Luffa fibres.
alkali treated fibre shows the formation of the scratches due to the removal of the lignin ans found
hemicelluloses. This characteristic may improve the adhesion between fibre and matrix when it is use
and showed that their value depended on the parameter's choice. The analysis
in reinforcing composite material. As shown in Fig. 2, the Luffa fibres change their morphology wit
changing treatment parameters. Fig. 2a shows the morphology of untreated Luffa sample. The fibres showed that many treatments conditions enhanced the crystalline structure of
formed by fibrils glued together by gummy substances, are disposed in a multidirectional array formin technical fibres of Luffa. It was shown also that other treatment conditions of mixed

a natural mat. The treatment of this mat by solution containing 4% of NaOH and 10% H2O2 at 120 °C method can damage the crystalline structure of technical Luffa fibres. In this case, a
fine structure of Luffa fibre can be obtained.
during 3 h transforms the technical fibres to fibrils (Fig. 2b).
The XRD examination of treated and untreated Luffa fibres shows that only the crysta
References
polymorph I of cellulose is present [15]. Fig. 3 shows the X-Ray Diffraction patterns of untreated Luf
fibres, alkali treated (120 °C–1 h–12% NaOH) and Luffa fibres treated with mixed treatment. This figur
shows many peaks at 2θ=15.1°, 16.4°, 22.4° and 34.4°. The peaks at 2θ=15.1° and 16.4° correspond t [1] Gianpietro V, Amaducci S, Vannini L. Multi-use Crops, Programme by DG XII of the European
respectively crystallographic planes (110) and (110). Tserki et al. [15] reported that these two peaks wi Commission. Department of Agronomy, University Bologna; 2000. p. 82–3. [2] Akhtar N, Iqbal J,
be confused in the case of the samples showing a high rate of amorphous products such a Iqbal M. Removal and recovery of nickel (II) from aqueous solution by loofa sponge-immobilized
hemicelluloses, lignin and amorphous cellulose. We can see in Fig. 3 that, for alkali treated fibres an biomass of Chlorella sorokiniana: character- ization studies. J Hazard Mater 2004;B108:85–94. [3]
treated fibres with mixed treatments (with exception of the treatment with 2% NaOH), the peaks at 2θ Akhtar N, Saeed A, Iqbal M. Chlorella sorokiniana immobilized on the biomatrix of vegetable sponge
15.1° and 16.4° are not confused indicating a low rate of amorphous products such as hemicellulose of Luffa cylindrica: a new system to remove cadmium from contaminated aqueous medium. Bioresour
lignin and amorphous cellulose. The peaks at 2θ=22.4° and 34.4° indicate respectively the (002) an Technol 2003;88(2):163–5. [4] Akhtar Nasreen, Iqbal Muhammad, Iqbal Zafar Saeed, Iqbal Javed.
(023) crystallographic planes. The peak intensity at 2θ=22.4° increases with the increase of temperatur Biosorption characteristics of unicellular green alga Chlorella sorokiniana immobilized in loofa
in the alkali treatment. This can be explained by the enhancement of the crystallinity index define sponge for removal of Cr(III). J Environ Sci 2008;20(2):231–9. [5] Ali Mazmanci M, Ünyayar Ali.
above. Decolourisation of Reactive Black 5 by Funalia trogii immobilised on Luffa cylindrica sponge.
Process Biochem 2005;40(1):337–42. [6] Nilsson I, Möller A, Mattiasson B, Rubindamayugi MST,
Table 1 presents the data of crystallinity index for several treatments. In the case o
Welander U. Decolorization of synthetic and real textile wastewater by the use of white-rot fungi.
alkali treatment, this index increases from 50% for untreated Luffa fibres to about 70% for treated at 12
Enzyme Microb Technol 2006;38(1–2):94–100. [7] Demir H, Top A, Balköse D, Ülkü S. Dye
°C, 3 h and 4% NaOH.
adsorption behaviour of Luffa cylindrica
As shown in Table 1 the treatment of Luffa fibres with mixed treatment improves the
fibres. J Hazard Mater 2008;153(1–2):389–94. [8] Abdelwahab Ola. Evaluation of the use of
crystalline structure. We note that an increasing rate of sodium hydroxide in the mixed treatment (10
loofa activated carbons as potential adsorbents for aqueous solutions containing dye. Desalination
°C, 1 h and 10% H2O2) from 2% to 10% enhances the crystallinity index to reach a maximum valu 2008;222(1–3):357–67. [9] Ogbonna JC, Liu YC, Liu YK, Tanaka H. Loofa (Luffa-cylindrica) sponge
(67.4%) for 8% of NaOH. Then, this rate decreases to 67.09% for 10% of NaOH. We can conclude th as a carrier for
the chemical reagents react first of all with the chain ends on the surface of the crystallites and elimina
microbial cell immobilization. J Ferment Bioeng 1994;78:437–42. [10] Iqbal M, Edyvean
the amorphous products such as hemicellulose and lignin. When the concentration of sodium hydroxid
RGJ. Loofa sponge immobilized fungal biosorbent: a robust system for cadmium and other dissolved
increases, the reagents can diffuse into the crystalline region, resulting in the rupture of some benzen
metal removal from aqueous solution. Chemosphere 2005;61(4):510–8. [11] Tanobe Valcineide OA,
cycles of cellulose chains by oxidation and transform them into aliphatic chains. In this case, som
Sydenstricker Thais HD, Munaro Marilda, Amico Sandro C. A comprehensive characterization of
amorphous zone of cellulose can be formed. Table 1 shows also that the variation of temperatur
chemically treated Brazilian sponge-gourds (Luffa cylindrica). Polym Test 2005;24(4):474–82. [12]
duration and rate of hydrogen peroxide generally enhance the structure of Luffa fibres.
Demir H, Atikler U, Balköse D, Tıhmınlıoğlu F. The effect of fiber surface treatments on the tensile and
water sorption properties of polypropylene–Luffa fiber composites. Compos Part A Appl Sci Manuf
4. Conclusion 2006;37(3):447–56. [13] Boynard CA, Monteiro SN, d'Almeida JRM. Aspects of alkali treatment of
sponge gourd (Luffa cylindrica) fibers on the flexural properties of polyester matrix composites. J Appl
Polym Sci 2003;87:1927–32. [14] Bal Kheir Eddine, Bal Youcef, Lallam Abdelaziz. Gross morphology
The aim of this work is to investigate the influences of the chemica and absorption capacity of cell-fibers from the fibrous vascular system of loofah (Luffa cylindrical). Tex
treatment parameters on the structure of Luffa fibres. The treatment should enhanc Res J 2004;74(3):241–7. [15] Tserki V, Zafeiropoulos NE, Simon F, Panayiotou C. A study of the effect
the crystalline structure of fibres with the elimination of amorphous materials. SEMof acetylation and propionylation surface treatments on natural fibres. Compos Part A Appl Sci Manuf
2005;36(8):1110–8.
micrographs and XRD patterns show the change of the fibre structure after alka
and mixed treatment. The crystallinity index of many treated and untreated sample
63 L. Ghali et al. / Materials Letters 63 (2009) 61–63