Cellulose

DOI 10.1007/s10570-016-1116-6

ORIGINAL PAPER

Effect of alkali treatment on microstructure and mechanical

properties of individual bamboo fibers
Hong Chen . Yan Yu . Tuhua Zhong . Yan Wu .
Yanjun Li . Zhihui Wu . Benhua Fei

Received: 10 July 2016 / Accepted: 27 October 2016

Ó Springer Science+Business Media Dordrecht 2016

Abstract The aim of this study was to study the resulted in more wrinkles and pores on the surface of
microstructure and mechanical properties of individ- bamboo fibers. Microfibril aggregates treated by 15
ual bamboo fibers after alkali treatment. The individ- and 25% NaOH solution changed from a randomly
ual bamboo fibers were treated by sodium hydroxide interwoven structure to a granular structure. Cellulose
(NaOH) solution with varying concentration (6, 8, 10, I was transformed to cellulose II after 15 and 25%
15 and 25%) followed by rinsing and freeze-drying NaOH solution treatment. The alkali treatment
treatments. The alkali treated individual bamboo fibers reduced the diameter, lumen and cross sectional area
were subsequently characterized by scanning electron of fiber, leading to the cracks in cell wall. The tensile
microscopy, atomic force microscopy, Fourier trans- strength and modulus of elasticity (MOE) of individ-
form infrared spectroscopy, X-ray diffraction, confo- ual bamboo fibers decreased with alkali treatment.
cal laser scanning microscopy and tensile strength NaOH concentration almost did not affect the tensile
tests. The results indicated that the alkali treatment strength but influenced the MOE significantly. The
elongation at break of treated individual fiber
increased significantly. When compared to untreated
H. Chen (&)
Y. Wu
Z. Wu individual fibers, the elongation at break of the fiber
College of Furnishings and Industrial Design, Nanjing was increased by 232 and 221% after 15 and 25%
Forestry Universtiy, Nanjing 210037, China
NaOH treatments, respectively. Besides, increasing
e-mail: [email protected]
alkali concentration caused the change of the fibers
H. Chen
Y. Yu
B. Fei (&) from brittleness to ductility, indicating that alkali
International Centre for Bamboo and Rattan, treated bamboo fibers have a promising application in
Beijing 100102, China
textile.
e-mail: [email protected]

T. Zhong Keywords Individual bamboo fiber
Alkali

Composite Materials and Engineering Center, Washington treatment
Microstructure
Mechanical properties
State University, Pullman, WA 99164, USA

Y. Li
College of Materials Science and Engineering, Nanjing
Forestry University, Nanjing 210037, China Introduction
Y. Li
School of Engineering, Zhejiang Agriculture and Forestry In recent decades, there has been an increasing effort
University, Linan 311300, China to exploit the renewable raw materials to produce

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sustainable products so as to reduce the use of fossil varied depending on different treatments such as
fuels, and to decrease the environmental pollution. NaOH (Das and Chakraborty 2008; Liu and Hu 2008;
The natural fibers as raw materials became a major Ray and Sarkar 2001), HNO3–KClO3 (Liu et al. 2012),
alternative to synthetic fibers since they are widely NaClO (Chen et al. 2011), benzoate (Amel et al.
abundant in nature. The natural fibers have great 2013). Alkali treatment has been considered as one of
potential applications in composites (Lee and Wang the most popular and cost-effective methods to obtain
2006; Okubo et al. 2004), pulp (Yang et al. 2008) and high-performance natural fibers (Liu et al. 2011).
textile (Liu et al. 2011; Nayak and Mishra 2016). Many studies reported that the alkali treatment is
There have been lots of researches studied on the important in determining the structure and properties
mechanical properties of natural fiber, e.g. wood of natural fibers, such as wood (Chen et al. 2015b;
(Burgert et al. 2002; Groom et al. 2002), jute (Saha Ishikura et al. 2010; Nakano 2010), abaca (Cai et al.
et al. 2010), kenaf and ramie (Wang et al. 2011). The 2015), hemp (Kabir et al. 2013; Liu et al. 2013; Ouajai
fibers derived from bamboo have attracted more and Shanks 2005), jute (Gassan and Bledzki 1999;
interests and attention due to their extraordinary Ray and Sarkar 2001; Saha et al. 2010; Sinha and Rout
mechanical performances (e.g. average tensile 2008), oil palm (Chowdhury et al. 2013), cotton
strength 1.43–1.69 GPa, and modulus 32–34.6 GPa, (Keshk 2015; Eronen et al. 2009), kenaf (Amel et al.
Yu et al. 2011) and plenty sources for the production 2013; Nitta et al. 2013) and Alfa (Borchani et al.
of bamboo fibers. Compared with other natural fibers, 2015).
such as kenaf (average tensile strength 0.98 GPa, However, there are a limited number of researches
modulus 19 GPa) and ramie (average tensile strength on the bamboo fibers with alkali treatment, especially
1 GPa, modulus 11 GPa), bamboo fibers have better on the individual bamboo fibers. Alkali treatments
tensile strength and modulus, but lower elongation at with different concentrations in bamboo strips and
break (bamboo 7.1%, kenaf 8.3%, remie 8.9%) bamboo dusts brought about changes in dimensions,
(Wang et al. 2011). In 2013, there are 1.88 billion morphology and mechanical properties (Chen et al.
bamboo culms consumed creating a total production 2016; Das and Chakraborty 2006, 2008). Bamboo
value of 27.4 billion US dollar in China (SFA 2014). fiber bundles treated by NaOH with different concen-
In Jiangxi province, China, the bamboo industry trations in different times have various structures (Liu
provides 0.86 million jobs linked to bamboo products and Hu 2008). To my knowledge, there is no report on
including pulp, textile, composites, furniture etc., the microstructure and mechanical properties of alkali
creating about 4.6 billion US dollar in 2014 reported treated individual bamboo fiber, because natural
by society of bamboo industry (http://blog.sina.com. individual bamboo fiber is very small (length is
cn/jxzcy09). However, the utilization rate of bamboo 1.49–2.28 mm, diameter is 12.24–17.32 lm) (Tian
material is still very low, only about 40% (Wang et al. 2015) and much harder than many plant fibers
2016). (average hardness is almost 0.5 GPa) (Yu et al.
At present, bamboo based textiles have not yet 2011). Therefore, it is difficult to characterize the
achieved their full potential. As reported, almost all microstructure and mechanical properties of individ-
available bamboo fabric in market is made using the ual bamboo fibers.
viscose process (Nayak and Mishra 2016). Conse- To expand the application of bamboo fibers in the
quently, most bamboo textiles in market are not textile, chemical modification bamboo fibers is of
natural fibers but come from a natural source (Liese great importance. In this research individual bam-
and Köhl 2015). It was reported that natural bamboo boo fibers (Neosinocalamus affinis) were isolated
fibers has antibacterial properties (Xing and Liu 2004). from bamboo strips. The individual fibers were
But the natural coarse and stiff quality of natural treated by NaOH solutions with varying concentra-
bamboo fibers restricted their applications in the field tions and were characterized by FE-SEM, AFM,
of textile, fine and soft fibers are highly desirable for FIIR, XRD, CLSM and micro tensile strength
the textile (Liu et al. 2011; Nayak and Mishra 2016). testing. The objective of this research is to inves-
Many techniques have been employed successfully for tigate the effects of NaOH concentrations on the
chemical modification of natural fibers. The microstructure and mechanical properties of indi-
microstructures and performances of natural fibers vidual bamboo fibers.

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Experimental selected and scanned, and untreated fiber specimen

was characterized as control.
Samples preparation
Fourier transform infrared spectroscopy (FTIR)
Raw materials were obtained from bamboo analysis
(Neosinocalamus affinis) grown in Chengdu, Sichuan
Province, China. Bamboo was taken from the culm The FTIR spectra of treated and untreated bamboo
where was 2 m high from the ground with an initial fibers were obtained in Nexus 670 spectrometer
moisture content of 8–12%. Bamboo was cut into (Thermo Nicolet, CA, USA) within the range of
small strips (30 mm longitudinally and 2 9 2 mm in 4000–500 cm-1, with a resolution of 4 cm-1 and 64
cross section). Individual bamboo fibers were isolated scans. The KBr pellet consisting of KBr and fibers
by immersing the small bamboo strips in a chemical selected randomly with a weight ratio of 100:1 was
solution (one part 30% hydrogen peroxide and one prepared prior to the measurement. The FTIR analysis
part glacial acetic acid) at 65 °C for 18.5 h (Wang for each sample was performed in triplicate.
et al. 2011). Individual bamboo fibers were washed
with deionized water to neutrality and then one part X-ray diffraction (XRD) analysis
was dipped in 6, 8, 10, 15 and 25% NaOH solution at
room temperature (23 ± 2 °C) for 2 h maintaining The crystal structure of the treated and untreated fibers
fiber weight to alkali volume ratio of 1:100 (Das and selected randomly was characterized using a Panalyt-
Chakraborty 2008; Zhang 2011). After the treatment, ical X-ray Diffractometer (Panalytical Corporation,
individual bamboo fibers were thoroughly washed Almelo, Netherlands). The X-ray diffraction patterns
using deionized water in order to remove NaOH from of the treated and untreated fibers were obtained in the
the fibers until the pH was 7. Both the untreated and diffractometer with a CuKa radiation source (X-ray
treated fiber suspension were frozen in liquid nitrogen wavelength k = 0.154178 nm) with a detector placed
followed by drying for 24 h in a freeze dryer. on a goniometer scanning the range from 5° to 45°.
The XRD analysis for each sample was performed in
triplicate.
Surface morphology
Confocal laser scanning microscopy (CLSM)
The morphology of the freeze-dried fibers was
analysis
selected randomly to observe with a field emission
scanning electron microscope (FE-SEM, XL30 ESEM
The areas of cross-section of bamboo cell wall were
FEG, FEI Company, OR, USA). The microfibrillated
observed with a confocal laser scanning microscopy
aggregates on the bamboo fiber surfaces were imaged
(CLSM; Zeiss, LSM 510 Meta, Germany). Prior to
by Icon atomic force microscope (AFM, Burker
CLSM observation, the fibers were dyed with acridine
Corporation, CA, USA). The specimens were scanned
orange solution. Axio vision software (Zeiss, Ger-
under tapping mode using sharp tapping mode probes
many) was used to calculate the fiber area (Yu et al.
with a tip radius 8 nm. The length of the cantilever was
2011; Wang et al. 2011). Fifteen specimens for each
125 lm, the spring constant was 42 N/M and the
treatment were tested.
resonant frequency was 320 kHz. The samples were
scanned at room temperature of 23 ± 2 °C and
ambient humidity of 35 ± 5%. Images were captured Mechanical properties test
as 512 9 512 pixel images. Real time scanning was
performed with scan rates 1.0 Hz, scan angle 0°, and Mechanical properties test of the individual bamboo
tapping frequencies ranging from 340–380 kHz. fibers was conducted in accordance with the procedure
Images were obtained in the phase mode, where the described in Chen et al. (2011). First, individual
phase lag was used to determine differences in bamboo fibers were selected with length more than
materials, as presented by Fahlén and Salmén 2 mm. Then fibers were glued on an organic, chan-
(2005). Ten specimens for each treatment were neled glass plate with one droplet of glue at each end,

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Fig. 1 SEM images of the surface morphology of individual bamboo fiber treated by NaOH solutions with different concentrations
(a untreated; b 6%; c 8%; d 10%; e 15%; f 25%)

and then placed in ambient condition (25 ± 2 °C, Results and discussion
35 ± 5% RH) for at least 24 h. The tensile strength
test of individual fibers was conducted at a high- Surface morphology
resolution commercial mechanical tester with the
measurement accuracy of 0.005 N (Microtester 5848, The surface morphologies of individual bamboo fibers
Instron, MA, USA). A constant strain rate of 48 lm/ treated by NaOH solutions with varying concentra-
min was set at 25 °C and 20% RH. The fibers were tions are presented in Figs. 1 and 2.
removed from the tensile apparatus immediately upon With increasing NaOH concentration, the diameter
failure and stored for subsequent CLSM imaging of of individual bamboo fiber decreased as shown in Fig. 1,
cross-sectional area for tensile modulus and strength the similar phenomenon was also reported for fruit fibers
calculations. Typical failures of individual fibers were (Boopathi et al. 2012). The average diameters (13
observed in FE-SEM and CLSM, respectively. Fifteen individual fibers measured for each type) were
specimens for each treatment were tested. 16.46 ± 4.47, 15.23 ± 1.33, 11.47 ± 3.55, 9.75 ±

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Fig. 2 Higher-magnification SEM images of the surface morphology of individual bamboo fiber treated by NaOH solutions with
different concentrations (a untreated; b 6%; c 8%; d 10%; e 15%; f 25%)

4.10, 7.42 ± 2.05, 8.02 ± 1.57 lm for individual Meanwhile the wrinkle on the surface was increas-
bamboo fibers treated by 0, 6, 8, 10, 15 and 25% alkali ingly apparent and the microfibril aggregates became
solution, respectively, while the average lengths (30 more distinguishing. The untreated fibers surface was
individual fibers measured for each type) were smooth. The orientation of cellulose microfibril aggre-
2.65 ± 0.64, 2.75 ± 0.55, 2.99 ± 0.64, 3.07 ± 0.65, gates was not obvious as shown in Figs. 1a and 2a but
2.37 ± 0.49, 2.59 ± 0.56 mm for individual bamboo can be observed distinctly in Figs. 1b–d and 2b–d.
fibers. The diameter decreased with increasing alkali Furthermore, the cellulose microfibril aggregates
concentration, while the length increase at low alkali not only can be seen clearly, but also some pores were
concentration and then decreased with high alkali observed between microfibril aggregates in Fig. 2e, f
concentration. For the dimension change of fiber, it at high magnification.
possibly resulted from the loss of matrix and microfibrils It indicated that matrix in the cell wall were
aggregations with alkali treatment. removed after alkali treatment. In our previous

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the diameter of fiber with the alkali treatment at higher

concentration.
It showed that alkali concentration is an important
factor affecting the surface morphology of bamboo
fibers. The higher concentration tended to cause more
cracks as shown in Figs. 1 and 2, leading to a rougher
surface of bamboo fibers. The similar phenomena were
also reported on other plant fibers after alkali treatment
(Liu et al. 2013; Saha et al. 2010; Sinha and Rout 2008).
The phase images, obtained by AFM, of individual
bamboo fiber treated with various NaOH concentra-
tions are shown in Figs. 4 and 5. It can be found that
cellulose microfibril aggregates in cell wall varied
depending on NaOH concentrations.
Fig. 3 FT-IR spectra of bamboo fibers treated by NaOH
The microfibril aggregates in surface of bamboo
solutions with different concentrations fiber treated by low concentration (6 and 8%) showed
a randomly interwoven structure in Figs. 4b, c and 5b,
research, the isolated method used in this paper can c, which is similar with the untreated ones in Figs. 4a
remove the lignin of bamboo fiber (Chen et al. 2013). and 5a.
In addition, FT-IR indicated the absence of the peaks However, the microfibril aggregates began to
at 1510 and 1423 cm-1 in Fig. 3 assigned to aromatic change when the NaOH concentration increased up
skeletal vibration and aromatic skeletal vibration to 10% as shown in Figs. 4d and 5d. In the case of 15
combined with C–H in plane deformations, respec- and 25% NaOH treatment, the randomly interwoven
tively (Qin et al. 2004; Tian 2015), suggesting lignin in structure of cellulose microfibril aggregates disap-
bamboo fibers have been removed during the isolation peared. Granular structure was observed, which might
process. There was no lignin in the isolated individual be due to the transformation of cellulose I to cellulose
fibers, either treated by alkali or untreated. II (Das and Chakraborty 2006; Liu and Hu 2008) or the
However, as shown in Fig. 3, there was peaks at damage of fine fiber structure as the alkali concentra-
1718 cm-1 in fiber untreated and treated by alkali with tion increased more than 10% (Cai et al. 2015).
concentration at 6 and 8%, respectively. The band at Microfibrils were swollen and more granular in
1718 cm-1 was attributed to C=O stretching vibration cellulose II than in cellulose I (Eronen et al. 2009).
in hemicellulose presenting in bamboo fibers (Das and In addition, the transformation of cellulose I into
Chakraborty 2006). There was still hemicellulose in cellulose II was irreversible at both the crystallo-
fiber treated by 6 and 8% NaOH solution. graphic level and the morphological level (Dinnad
As the concentration of alkali increased to 10, 15 et al. 2002).
and 25% respectively, the bands at 1718 cm-1 disap-
peared, which indicated hemicellulose in bamboo fiber X-ray diffraction
was almost removed. It is widely reported that alkali
treatment can remove hemicellulose at certain NaOH The XRD patterns of bamboo fibers treated with
concentrations (Ariawan et al. 2015; Ouajai and various NaOH concentrations are shown in Fig. 6.
Shanks 2005; Rajulu et al. 2003; Saha et al. 2010; In Fig. 6, two characteristic peaks in the XRD
Zuluaga et al. 2009). In our case, it seems the NaOH patten of untreated bamboo fiber were observed at
concentration at 10% is adequate to remove all the 2h = 16.01° and 22.25°, which correspond to typical
hemicellulose that exists in the individual bamboo cellulose I with crystallities having preferred orienta-
fibers. tion along the fiber axis (indicated by reduced tensity
In addition, microfibrils were prone to aggregate near 34.7°) (French 2014). The similar XRD patterns
easily when the cell wall lost lignin and hemicellulose, of the 6, 8 and 10% alkali treated fibers were observed
which might be partly responsible for the reduction in as the untreated one, showing the similar cellulose I

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Fig. 4 AFM images of the arrangement of microfibrils of bamboo fiber treated by NaOH solutions with different concentrations
(a untreated; b 6%; c 8%; d 10%; e 15%; f 25%)

structure. As reported by Sun et al. (2014), for poplar However, when the NaOH concentration increased
treated by Ca(OH)2 solution at low concentration, up to 15 and 25%, XRD patterns changed, the peaks at
there was no transition of cellulose I into II occurred 2h = 12.25°, 20.2° and 21.8° correspond to (1–10),
and the relative carbohydrate was not significantly (110) and (020) planes of typical cellulose II with
altered. preferred orientation of the crystallites along the fiber

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Fig. 5 Higher-resolution AFM images of the arrangement of microfibrils of bamboo fiber treated by NaOH solutions with different
concentrations (a untreated; b 6%; c 8%; d 10%; e 15%; f 25%)

axis (indicated by no peak near 34.7°), respectively was the major component in the fiber (El Oudiani et al.
(French 2014). This finding is consistent with the 2011). The chains in cellulose I organized in sheets
phenomenon reported by Das and Chakraborty (2006), packed in a ‘‘parallel-up’’ fashion (Nishiyama et al.
Eronen et al. (2009), and Liu and Hu (2008). Therefore, 2002, 2003), while cellulose II structure is antiparallel
when NaOH concentration exceeded 15%, cellulose II (Langan et al. 1999). In compact cell wall, microfibrils

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Table 1 Cross-sectional area of bamboo cell wall

Treatment Area (lm2) (CV)

A (untreated) 108.48 (0.26)

B (6%) 103.58 (0.27)
C (8%) 107.54 (0.26)
D (10%) 88.08 (0.29)
E (15%) 90.23 (0.32)
F (25%) 105.53 (0.27)

comparison with the untreated one. Furthermore, after

alkali treatment with 10% NaOH solution, the cross-
sectional area of individual bamboo fiber decreased to
be the minimum. While increasing NaOH concentra-
tion up to 15 and 25%, the cross-sectional areas
Fig. 6 XRD patterns of bamboo fiber treated by NaOH
solutions with different concentrations increased when compared with fibers with 10% NaOH
treatment. It might be attributed to transformation of
of opposite polarity co-existed side by side in native cellulose I to cellulose II.
cellulose system. In an alkali treatment, during the Lumens in cross sections of bamboo fibers treated
swelling process, neighboring cellulose chains belong- by both 6 and 8% NaOH solution were observed,
ing to microfibrils of opposite polarity would get close which was similar with the one untreated.
enough to meet each other. At washing and drying step, However, when NaOH concentration increased to 10,
the cellulose chains would recrystallize into antiparallel 15 and 25%, the lumens disappeared and a crack
form which is thermodynamically more stable (Dinnad appeared between different layers. Bamboo fiber has a
et al. 2002; Nishimura and Sarko 1987; Okano and polylamellate structure of alternating broad and narrow
Sarko 1985; Wang and Chen 1996). lamellae which is different from that in wood cell wall
The patterns of untreated fibers showed that there was (Liese and Köhl 2015). The removal of cementing
only cellulose I in bamboo fiber, the alkali treatment led materials during alkali treatment led to better packing of
to different lattice transformation when the concentra- cellulose microfibrils (Das and Chakraborty 2008). The
tion increased. Lattice transformation from cellulose I to aggregation of cellulose microfibrils may result in various
cellulose II have been reported occurring in many alkali stresses in different layers in bamboo cell wall and thus
treated plant fibers such as wood (Borysiak and created cracks between layers as shown in Fig. 6d–f.
Doczekalska 2005; Ishikura et al. 2010; Nakano and
Nakano 2014), ramie (Kobayashi et al. 2011), abaca Mechanical properties
(Cai et al. 2015), Alfa (Borchani et al. 2015).
In this study, it was found that mechanical properties
CLSM analysis were significantly affected by the alkali treatment due
to the change of fiber structure.
The cross-sectional area and cross sections of cell wall The typical stress–strain curves of untreated indi-
in individual bamboo fiber are shown in Table 1 and vidual bamboo fibers and fibers treated by NaOH with
Fig. 7, respectively. It indicated that different alkali various concentrations are shown in Fig. 8.
treatment significantly influenced the lumen and cross The stress–strain curves of individual bamboo
sectional area of cell wall of the fibers. fibers treated with 6 and 8% NaOH are similar to the
The cross-sectional area of all the treated individual untreated one. However, the stress–strain curves of 10,
bamboo fibers were smaller than that in untreated one 15 and 25% NaOH treated fibers appeared differently
that might be due to partial removal of amorphous in comparison of the untreated one.
materials in fiber as a result of alkali treatment. The tensile strength, the modulus of elasticity
The areas of individual bamboo fiber treated by 6 (MOE) and the elongation at break are summarized in
and 8% NaOH solution were slightly smaller in Table 2.

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Fig. 7 Typical CLSM images of the cross section of individual bamboo fibers treated by NaOH solutions with different concentrations
(a untreated; b 6%; c 8%; d 10%; e 15%; f 25%)

The tensile strength of all alkali treated individ- In the case of fibers treated by 6, 8 and 10%, the
ual bamboo fibers decreased as compared to removal of matrix materials was the main cause of the
untreated fiber as shown in Table 2. That might reduction in the modulus (Fahlén and Salmén 2005;
be attributed to the damage and the change in the Zhang 2011). For individual bamboo fibers treated by
structure of fine fiber. When concentrations were at 15 and 25%, the combined effects of the removal of
6, 8 and 10%, the alkali treatment removed hemicellulose and the transformation of cellulose I to
hemicellulose gradually. While increasing concen- II led to the bigger reduction in the MOE, because the
tration to 15 and 25%, the treatment not only MOE of cellulose I (around 140 GPa) is higher than
removed the hemicellulose, but also resulted in that of cellulose II (90 GPa) (Northolt et al. 2001).
cellulose transforming from I to II. The elongations at break of all treated individual
MOE of all treated individual bamboo fibers was bamboo fibers were higher than the untreated one.
lower than that of untreated fiber. With increasing While the NaOH concentration increased to 10%, the
NaOH concentration, MOE decreased significantly. elongation at break began to increase significantly.

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Once the concentration increased to 15 and 25%, the

elongation at break increased by 232 and 221%,
respectively when compared with untreated fiber. The
elongations at break of individual bamboo fibers
treated were much higher than that of bamboo fiber
bundles (2.61%) which can be used for making yarn
(Chen et al. 2015a). It indicated that bamboo fibers had
a potentiality to making soft and fine yarn for textile
with good quality.
As reported by Salmén (2004) that cellulose
microfibril aggregates were filled with the matrix
consisting of lignin and hemicellulose. The isolation
process and alkali treatment removed matrix in the cell
Fig. 8 Typical tensile stress–strain curves of individual bam- wall resulting in lots of interspace as shown in Fig. 9.
boo fibers treated by NaOH solutions with different When the fiber was pulled, the interspaces first
concentrations

Table 2 The data of tensile strength, modulus of elasticity and elongation at the break
Sample Tensile strength (GPa) (CV) Modulus of elasticity (GPa) (CV) Elongation at break (%) (CV)

A (untreated) 0.83 (0.57) 14.48 (0.49) 5.85 (0.15)

B (6%) 0.64 (0.40) 10.64 (0.40) 6.53 (0.22)
C (8%) 0.68 (0.63) 11.61 (0.56) 6.06 (0.17)
D (10%) 0.59 (0.31) 8.89 (0.39) 8.21 (0.25)
E (15%) 0.59 (0.39) 4.22 (0.50) 19.42 (0.21)
F (25%) 0.61 (0.19) 4.85 (0.44) 18.76 (0.30)

Fig. 9 The model of

individual bamboo fiber
under load after removing
the matrix

Interspace
Interspace

Microfibril
Microfibril

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Fig. 10 FE-SEM images of the fracture after the tensile testing of individual bamboo fiber treated by NaOH solutions with different
concentrations (a untreated; b 6%; c 8%; d 10%; e 15%; e 25%)

changed to be small, then loading on the microfibril reported by other researchers, the alkali treatment can
which led to much higher elongations at break of the soften the fibers dramatically (Gassan and Bledzki
alkali treated samples. The analysis of FT-IR indicated 1999; Liu et al. 2013).
that NaOH concentration at 10% is adequate to The typical fractures of individual bamboo fibers
remove all the hemicellulose in the individual bamboo during the tensile testing are shown in Fig. 10. For
fibers. While the elongations at break treated by 15 and alkali treated bamboo fibers, chemical and structural
25% NaOH solution were much higher than that changes resulted in the difference in the fracture. The
treated by 10% NaOH solution. When the concentra- fractures of individual bamboo fiber treated by 6 and
tion increased to 15 and 25%, not only removal of 8% were similar to that of untreated fibers presenting
hemicellulose happened but also transition of cellu- as a brush. This type of fracture resulted from the
lose happened. Both accounted for the increase of cutting alongside with the microfibril or the microfib-
elongation at break of individual bamboo fiber. As rils were pulled away from each other (Rowell 1984).

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Cellulose

It suggested that most of the fracture happened in the concentration because of cellulose lattice trans-
weak interface between microfibrils. The factures of formation and microfibril swollen.
fibers with 15 and 25% NaOH treatment were neat and 4. The tensile strength and MOE of individual
uniform which indicated the fracture mainly happened bamboo fibers decreased after treated by the
in microfibril instead of between the microfibrils as alkali. Alkali concentration almost did not affect
happened in the untreated fibers (Rowell 1984). This the tensile strength but influenced MOE signifi-
fracture form was called broken in pieces by Rowell. cantly. For NaOH treated fibers, the elongations at
In addition, the holes resulted from loss of lignin and break were higher than the untreated one. When
hemicellulose in the alkali treatment helped to form with strong alkali treatment (10, 15 and 25%), the
brittle facture surface. Microfibrils slippage probably elongation at break increased significantly, espe-
happened due to the decreasing bonding when losing cially at 15 and 25%, the elongation at break
the matrix in cell wall. While for 10% NaOH treated increased by 232 and 221% comparing with the
fibers, the fracture was between the ‘‘brush type’’ and untreated fiber, respectively. Alkali treatment
the ‘‘uniform type’’. caused individual bamboo fibers from brittle to
ductile with increasing NaOH concentrations.

Conclusions Acknowledgments This work was financed by National

Natural Science Foundation of China (31500474, 31370563,
The effect of alkali concentration on microstructure 31570552), Zhejiang Provincial Natural Science Foundation of
and mechanical properties of individual bamboo fibers China under Grant (LZ13C16003, LY16C160009), the project
(YH-NL-2014002B) and the Priority Academic Program
were investigated. The results obtained are as follows: Development of Jiangsu Higher Education Institutions
(PAPD), the authors are grateful to Dr. Shang Lili and Zhang
1. Alkali treatment changed the surface morphology Xuexia from International Centre for Bamboo and Rattan for
and the microfibril aggregates in cell wall. The FT-IR testing and Zhang Wenfu from Zhejiang Forestry
alkali treatment resulted in more wrinkles in the Academy for the fiber length testing.
surface of bamboo fibers when compared with the
untreated ones. The 15 and 25% NaOH treatment
caused the change of the microfibril aggregates
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