Yu 2014
Yu 2014
ABSTRACT: Lignocellulosic materials can be used for the development of bio-based composites. This study explores the potential of
long bamboo fiber bundles extracted directly from bamboo stems using the novel mechanical method and bamboo-based fiber com-
posites (BFC) fabricated using long bamboo fiber bundles and phenolic resins via cold pressing and thermal cure process. The micro-
structure, mechanical properties, and durability of BFC were evaluated, results being compared with raw bamboo and other
commercialized bamboo fiber composites. The mechanical properties of BFC reinforced with 87% (w/w) long bamboo fiber bundles
increased more than 50% than those of raw bamboo and were significantly higher than those of other bamboo-based composites.
Lower water absorption and thickness swelling were obtained in the case where bamboo fiber bundles with the small fineness. Higher
tensile strength was obtained in the case where bamboo fiber bundles with large sizes of bamboo fiber bundles. V
C 2014 Wiley Periodicals,
Chemical constituents
Volume fraction of bamboo tissues (%) (%) Strength (MPa)
Bamboo species Fiber Metaxylem vessel Parenchyma cells Holocellulose Lignin Tensile Compression
Ci bamboo 45.0 5.5 49.5 73.55 24.35 227.55 70.49
Moso bamboo 32.0 8.9 59.1 68.25 23.65 188.77 69.92
Lv bamboo 30.0 8.7 54.3 68.74 23.46 199.10 54.36
Dan bamboo 40.5 8.8 52.7 62.40 23.35 185.89 62.45
Ma bamboo 32.5 6.4 62.1 69.61 22.77 182.20 59.59
interactions between polar hydroxyl groups of the phenolic resin semicircular bamboo tubes were pushed into the fluffer11 along
and the hydrophilic fibers. This represents an important advant- the grain direction. The bamboo tube was fluffed along the lon-
age of this resin compared to the hydrophobic matrix14–16 gitudinal fiber direction to form a series of dotted and/or
because the intensity of the intermolecular interactions through linear-shaped cracks along the fiber direction for five and seven
the interface controls various properties of the composites.17 times, as shown in Figure 1(a). Two types of fineness fiber bun-
Another advantage of using phenolic resins is their water solu- dles were formed, as shown in Figure 1(c,d), respectively, and
bility and low processing temperature, which is below the ther- then dried in an air-circulated stove at 85 C until the moisture
mal decomposition temperature of the lignocellulosic fibers.18 content was approximately 10%.
This article describes the benefit of the use of long fiber bundles To obtain a uniform glue spread, the solid content of phenolic
extracted from bamboo stems and water-soluble phenolic resins formaldehyde resin was adjusted to 15% (in weight percent).
in the fabrication of bamboo-based fiber composites (BFC) for Next, the BF bundles were immersed in the resin at a room
commercial and industrial purposes. First, the long BF bundles temperature (RT) for 6 min. Then, the BF bundles were taken
are extracted directly from bamboo stems using the novel out and placed vertically for several minutes until the mass frac-
mechanical method. Second, composites using two types of tion of resin was approximately 13%. The glued BF bundles
fineness BF bundles are fabricated with a novel cold pressing were dried in an air-circulated oven at 55 C until the moisture
and thermal cure process. Finally, their mechanical properties content was around 12%.
and durability after the fabrication are evaluated.
The glued BF bundles were weighed according to the designated
EXPERIMENTAL
density and uniformly laid in the mould. They were then
pressed at 82 MPa in the mould using a cold press machine
Materials
(Qingdao Guosen Machinery Co.). Once pressed to the position
The characteristic, composition, and performance of bamboo
of the pinhole, the mould was locked by the pin, as shown in
vary greatly according to the species.8 Table I lists the volume
Figure 1(b). The moulds with slabs were placed in the air-
fraction of bamboo tissues, chemical constituents, and tensile
circulated baking chamber at a temperature of 132 C and cured
strength of five commercial specials: Ci bamboo (Neosinocala-
for 10 h. Then, the moulds were taken out from the baking
mus affinins (Rendle) Keng f.), Moso bamboo (Phyllostachys
chamber, and the slabs were demoulded. Finally, the BFC with
pubescens), Lv bamboo (Dendrocalamopsis oldhami (Munro)
dimension of 2000 3 145 3 150 mm3 were obtained, which
Keng f.), Dan bamboo (Phyllostachys glauca McClure), and Ma
reinforced with type 1 fiber bundles fluffed five times and type
bamboo (Dendrocalamus latiflorus Munro), abundantly grown in
2 fiber bundles fluffed seven times as shown in Figure 1(e,f),
the southern China.19,20 It can be seen that Ci bamboo has a
respectively.
considerably high volume fraction of fiber, holocellulose, and
shows relatively higher mechanical properties compared to other Diameter of Bamboo Fiber Bundles Testing
bamboo species. Therefore, Ci bamboo obtained from Hongya The diameter of fiber bundles was measured by image analysis.
Forest Reserve, Sichuan Province, Southwest China was selected A cross-section of BF bundles was imaged by a CCD video cam-
as reinforcing material in this study. era, and the image data were transformed into a binary-
The matrix material used in this study was based on a commer- processed image. To avoid the error according to the irregularity
cially available low-molecular-weight phenol formaldehyde resin of bamboo bundles on cross-section, the width measurement of
(trade name: PF16L510) supplied by Beijing Dynea Chemical each fiber bundle was repeated at different position. The mean
Industry Co., whose parameters are as follows: 5.59% of solid of the four values was taken as the diameter. One hundred
content, 36 mPa•s of viscosity, and 10.45 of pH. observations were recorded.
Figure 1. Bamboo fiber bundles and bamboo-based fiber composites. (a) Long bamboo fiber bundles; (b) slabs with moulds; (c) longitudinal surface of
bamboo fiber bundles fluffed for five times (type 1 fiber bundles); (d) longitudinal surface of bamboo fiber bundles fluffed for seven times (type 2 fiber
bundles); (e) cross-section of bamboo-based fiber composites reinforced with type 1 fiber bundles fluffed for five times; (f) cross-section of bamboo-
based fiber composites reinforced with type 2 fiber bundles fluffed for seven times. [Color figure can be viewed in the online issue, which is available at
wileyonlinelibrary.com.]
1990 (Reapproved 2003). Specimens were tested to failure under 10 3 5 3 5 mm3 (length 3 width 3 thickness). Their surfaces
tension at crosshead speed of 2 mm s21 using a standard mate- were smoothed with a sliding microtome. The BF bundles were
rial testing system (MWD-W10, Jinan Shiguang test Instrument sawn into a bamboo splinter with lengths of 10 mm. The cross-
Co.). An extensometer was attached to the gauges section of the sections of bundles were cut smoothly with a sliding microtome
specimen for strain measurement. Twenty-five specimens from but not for the longitudinal sections. Then surfaces of all speci-
five separately manufactured composites reinforced with two mens were sputter-coated with gold prior to morphological
types of fiber bundles were tested. The tensile Young’s modulus examination. The scanning electron microscope (SEM) micro-
and strength were recorded. graphs were obtained under conversation secondary electron
imaging conditions with an acceleration voltage of 10 kV.
Compressive Testing. Cuboid-shaped specimens of BFC sam-
ples with dimensions of 81.6 3 25.0 3 20.0 mm3 were pro- RESULTS AND DISCUSSION
duced from the composite plates and then tested according to
Microstructures of Raw Bamboo
ASTM D3501-2005 using a crosshead speed of 1 mm min21.
Figure 2(a) shows a cross-section of raw bamboo. It can also be
An extensometer was attached to the gauges section of the spec-
observed that the ci bamboo column mainly consists of vascular
imen for strain measurement. Twenty-five specimens from five
bundles and parenchymatous ground tissues, where the inho-
separately manufactured composites reinforced with two types
mogeneous distribution of vascular bundles that are embedded
of fiber bundles were tested. The compressive Young’s modulus
in the PCs [Figure 2(b)], densely dispersed in the outer part
and strength were recorded.
and sparsely in the inner part of the culm wall; therefore, the
Environmental Aging higher amount of vascular bundles in the outer culm wall is a
Cuboid-shaped specimens of BFC samples with dimensions of perfect structural adaptation toward a high bending stiffness
50 3 50 3 20 mm3 were immersed in distilled water at RT and strength of the bamboo culm. The vascular bundles mainly
(23 C) and boiling temperature (BT) (100 C) for up to 240 h. consisting of hollow metaxylem vessel (MV) and sclerenchyma-
Mass and thickness change of the sample were recorded using tous fiber caps or sheaths are the fundamental structural com-
an electronic balance and micrometer at regular time intervals. ponents of a bamboo culm, and the caps or sheath of fibers
Twenty-five specimens from five separately manufactured com- consists of many longitudinal single BF, whose diameter is
posites reinforced with two types of fiber bundles were tested. approximately 7–23 lm each for an average of 13.63 lm, [Fig-
The water absorption and thickness swelling were calculated ure 2(c)]. The fibers, playing a decisive role in the physiological
according to ASTM D1037. growth and biomechanical function of bamboo, are the main
components that determine the mechanical properties of bam-
Scanning Electron Microscopy boo owing to their unidirectional arrangement in the tissue as
To study the microscopic structural variations during the manu- well as their unique cell wall structure.21
facturing process, the surfaces of raw bamboo, BF bundles, and
BFC specimens were examined using a scanning electron micro- Bamboo Fiber Bundle Characteristics
scope (JEOL JSM-5500 LV). The raw bamboo and BFC samples Figure 1(a) shows the long BF bundles, wherein a series of dot-
were sawn with cuboid-shaped specimens with dimensions of ted and/or linear-shaped cracks are formed on the cylinder wall
Figure 2. SEM image of Ci bamboo (a) cross-section of raw bamboo; (b) parenchyma cells; (c) bamboo fiber.
Figure 3. SEM image of bamboo fiber bundles (a) cross-section of bamboo fiber bundles; (b) parenchyma cells and metaxylem vessel on longitudinal
direction; (c) bamboo fiber on longitudinal direction.
Table II. Morphology of Bamboo Fiber Bundles surfaces of fibers [Figure 3(c)]. Therefore, the resin impregna-
tion path and the effective bonding area of bamboo are
Diameter (lm) increased due to fluffing processing.
Fluffed Length
Fiber type times (mm) Range Average Figure 1(c,d) shows the BF bundles fluffed for five and seven
times. It can be observed that, with increasing the times of the
Type 1 5 2000 113–262 183 (35)
fluffed treatment, the more dotted and/or linear-shaped cracks
Type 2 7 2000 88–145 107 (25)
are formed in the culm wall. As shown in Table II, the diameter
of BF bundles decreases with the increase in fluffing times. This
of a semicircular bamboo tube. The epidermis on the outer increases the specific surface area of BF bundles, which makes it
layer of bamboo and the pith tissue on the inner layer of bam- more efficient to distribute PF resin on the surface of fiber bun-
boo have been removed. Figure 3 shows the SEM images of BF dles during the impregnation process and may potentially
bundles in different directions. During fluffing processing, a improve bonding performance. However, the increase of fluffing
series of cracks are formed along the PCs and MVs between process might lead to the further broking of fiber, and then the
fibers [see arrows in Figure 3(a)]. However, the fibers are not tensile strength of BF bundles may decrease.
destroyed. It can be observed that the bundles are not separated
into single fiber, and a large amount of PCs remain on the sur- Microstructures of BFC
face of the bundles, which can be seen in the SEM images of Figure 4 shows the SEM micrograph of BFC reinforced with BF
bundles in a longitudinal direction [Figure 3(b,c)]. The fibers bundles. It can also be observed from the micrographs that the
with good performance are exposed to the surface with high honeycomb structures of the MVs and PCs of BFC [Figure
rates of fibrillation and fragmentation [Figure 3(b)]. Fine voids 4(a)] become denser comparing to those of raw bamboo [see
are present in the wall of the PC and MV, which are around the Figure 1(a)] according to the high pressure and heating
Figure 4. SEM image of bamboo-based fiber composites. (a) Cross-section of BFC; (b) cross-section of dense parenchyma cells of BFC; (c) longitudinal
direction of BFC.
temperature during the moulding and curing process. This is playing a decisive role in the mechanical property of compo-
also reflected in the increase of BFC specific gravity (1.16 and sites, maintain the orientation of framework structure without
1.15 g/cm3 shown in Table III) compared with that of raw bam- severe rupture after fluttering treatment and loading process.
boo (0.72 g/cm3).19 In addition, it is possible to observe the Therefore, the BFs maintain their high mechanical performance.
presence of the adhesive inside or between the collapsed MVs However, the honeycomb ground tissues such as the MV and
and PCs [see arrows in Figure 4(b)]), where the dilute phenolic PCs are broken by fluttering treatment and condensed by high
resins can penetrate through the subtle cracks of thin-walled pressure. It can be obtained by image analysis that the volume
structure during the immersing process. The collapsed and fraction of fiber in BFC is approximately 57%, which signifi-
thin-walled tissue could lead to more intimate contacts and cantly increased compared with that of raw bamboo (45%). The
therefore the better inter-fiber bonding and compacting due to strength (610 GPa) and Young’s modulus (46 GPa) of BF are 12
high pressure (82 MPa). It can be observed from the longitudi- and 23 times more than those of the PCs (50 MPa and 2 GPa),
nal surface that significant amounts of dense PCs are mingled respectively.7 Increasing the volume fraction of fiber would lead
with aligned BF. These PCs and MV are recovered with, and to enhanced mechanical properties.24
then adhered to the phenolic resin [Figure 4(c)]. This confirms
The tensile strength and compression strength of BFC rein-
that the dilute phenolic resin penetrates through the subtle
forced with Ci long BF bundles are overwhelmingly higher than
crack formed by the fluffed treatment of bamboo tube when it
those of other bamboo-based composites. The excellent
was immersed in the phenolic resin liquid during the impregna-
mechanical properties of BFC are due to the superior mechani-
tion process.
cal characteristics of Ci long BFs and good bonding
Figure 1(e,f) shows the BFC reinforced with type 1 fiber bun- performance.
dles fluffed five times and type 2 fiber bundles fluffed seven
The tensile strength and Young’s Modulus of BFC reinforced with
times. It can also be observed that, with increasing the times of
long BF bundles in this study are more than 10 times higher than
the fluffed treatment, the bonding interface of BFC between BF
those of composites reinforced with bamboo short fibers/PF or EP,
bundles become mistiness. Consequently, the material is more
and its compression strength is more than 5 times higher than
uniform.
that of composites reinforced with bamboo short fibers/PF. The
separation of short BFs destroys the original strength of bamboo.
Mechanical Property
The orientation of the natural BF is disrupted for short bamboo
The results of tensile and compressive properties tests, with
composites, which results in the damage of the basic performances
respect to the BFC of the phenolic resins without any additives
of bamboo and consequently the loss of mechanical strengths. For
or curing agents and reinforced with 87% (w/w) BF bundles,
long BF composites, the tensile strength of BFC/PF composites is
are presented in Table III. The results of BFC are compared
more than 1.6 times higher than that of long BF/EP composites,
with those of other bamboo composites prepared by different
while its compression strength is slightly higher than that of long
bamboo bundles, and different additives published are also ref-
BF/EP composites. This indicates the important advantage of phe-
erenced to investigate the influence of long BF bundles and phe-
nolic resins compared to the hydrophobic thermoplastic matrix.
nolic resin on mechanical properties.22 Other bamboo
Their characteristic of water solubility brings about the good pene-
engineered products, such as bamboo laminated lumber and
trability of matrix in to reinforcement and then enhances the
bamboo scrimber, were used as controls for comparison.23
intensity of the intermolecular interactions. Another advantage of
In comparison with the raw bamboo (see Table I), it can be using phenolic resins is their low processing temperature, which is
seen that the tensile and compression strength of both BFC below the thermal decomposition temperature of the lignocellulo-
reinforced with BF bundles are increased by 44%–56% and sic fibers.18 The higher processing temperature (180 C) of long
83%–104%, respectively. Figures 3 and 4 display that the BFs, BF/EP results in the decomposition of BF, which decreases the
Figure 5. Durability of bamboo-based fiber composites. (a) Water absorption treated at RT; (b) water absorption treated at BT; (c) thickness swelling
rate treated at RT; (d) thickness swelling rate treated at BT. [Color figure can be viewed in the online issue, which is available at wileyonlinelibrary.com.]
mechanical properties. In addition, investigation of the mechani- distribute the stress along the fiber bundles during loading of
cal properties of BFC comparing with those of commercial bam- pressing process. Thus, the mechanical properties of BFC compos-
boo scrimber and laminated bamboo lumber was carried out. For ite are improved. However, the resin is generally distributed in the
tensile strength, BFC reinforced with both type fiber bundles surface of the units of bamboo strip, or bamboo bundle for bam-
shows more than 2.8 times higher than those of bamboo lami- boo laminated lumber and bamboo scrimber, which makes it diffi-
nated lumber and bamboo scrimber. The compression strength of cult to improve the properties of honeycomb foams.
BFC is more than 2.5 times higher compared to that of bamboo
The results also show that the compression strength and Young’s
laminated lumber and more than 1.6 times higher compared to
modulus of the BFC reinforced with type -1 fiber bundles fluffed
that of bamboo scrimber. Bamboo laminated lumber and bamboo
five times are lower than that of BFC reinforced with type 2 fiber
scrimber are mainly commercialized bamboo-based composites.
bundles fluffed seven times. As for polymer–matrix composites,
Bamboo laminated lumber, similar to the laminated veneer lum-
the compression strength depends on the interaction between the
ber, is made from parallel bamboo strip. Bamboo scrimber, similar
reinforcement and the matrix more than the reinforcement
to the scrimber developed in Australia, is a novel, engineered com-
posite made from parallel bamboo bundles. Compared with other alone.25 With decreasing fineness of fiber bundles, the phenolic
bamboo composites, bamboo scrimber has comparatively higher resin distribution is more uniform. Consequently, the bonding per-
raw material utilization rate because it has relatively more raw formance between BF bundles and resin is improved, which leads
material sources, which include small-sized bamboo culm.23 The to higher compression strength. However, it can be observed that
BF is the reinforcement, and the phenolic resin represents the the tensile strengths show the opposite results. The tensile strength
matrix during the system of bamboo-based composites. The inter- of BFC reinforced with type 1 fiber bundles is higher than that of
action between BFs and resins are strongly dependent on the con- BFC reinforced with type 2 fiber bundles. The tensile strength
tact surface. In other words, the phenolic resin distributes more mainly depends on the strength of the reinforcement for polymer–
uniformly with the increasing fineness of BF bundles. The cracks matrix composites.26 As for BFC composites system, long BF bun-
in thin-walled tissue could lead to increase of fineness of BF bun- dles represent the reinforcement. Increase of fluffing treatment
dles and better contacts between bamboo cells and PF resin, and time leads to form more short bamboo bundles and reduce the
hence the excellent inter-fiber compacting and bonding [see length and amount of long BF bundles. Therefore, the tensile
arrows in Figure 4(b)]. The excellent bonding is able to efficiently strength declines with the fluffing treatment times increasing.
It is clear that BFC reinforced with 87% (w/w) BF bundles have BF embedded in ground tissue is difficult to extract from bam-
excellent water resistance compared with those of raw bamboo,8 boo club. Hence, processes have been adopted to extract short
SFC reinforced with bamboo short fibers/PF22 and bamboo BFs for reinforcement of thermosetting and thermoplastic
scrimber.27 The low molecular weight phenol resin, penetrated matrix composites; however, most short BF composites suffer
into the intercellular space of bamboo and lumens of thin- from a lack of mechanical and dimensional properties, and only
walled cells through cracks during the immersed process, and a few applications have been realized. In addition, the polar and
adhesive inside the collapsed, thin-walled tissues, formed an nonpolar characteristics of BFs and many polymeric resins
excellent three-dimensional network of thin protecting water- could result in composites without appropriate properties,
resistant film on the surface of BF bundles. The phenol resin mainly owing to lack of adhesion at the interface.
film can effectively prevent the hydroxyl groups of BFs from If long BF bundles are used as reinforcement and phenolic type
interacting with water molecules. The mutually penetrated and resins are used as matrix, as in this study, these problems can
interlocked structures of dense, thin-walled cells and phenol be considerably minimized due to the interaction between polar
resin decrease the impregnation path of water. The effect of groups present in their chemical structure and the phenolic
fiber size and temperature on water absorption can be clearly resin. This is able to efficiently distribute the stress along the
seen. The weight gain percentage at the moisture saturation fiber bundles and protect BF erosion by water molecules.
point for BFC with type 1 and type 2 fiber bundles is 7.98%
and 3.98% at RT and 13.14% and 9.01% at BT, respectively. In addition, for the first time, the long BF bundles were
Both initial rate of water absorption and moisture saturation extracted by mechanical methods without any chemical altera-
point decrease as the diameter of BF bundles decreases. Com- tion or special alteration of the epidermis and pith tissue of the
pared with large fiber bundles, the resin is well distributed to bamboo. The remained fragments of PCs can act as effective
form a continuous firm film, and the voids are obviously reinforcing elements for composite manufacturing, and the PCs
reduced in small fiber bundles. do not need to be separated to provide good reinforcing capa-
bility. The phenol thermoset resin was reinforced by BF (87%
If the temperature of immersion increases, the moisture satura- w/w) using a novel cold pressing and thermal cure process,
tion time shortens greatly. And the rate of approach to equilib- owing to their excellent mechanical and dimensional properties.
rium is clearly more rapid. The water uptake process is linear in The mechanical properties of BFC increased more than 50%
the beginning and then decreases and approaches saturation than those of raw bamboo and were significantly higher than
after a prolonged time. The higher and faster weight gain upon those of other bamboo-based composites. Two different sizes of
exposure to boiling water may be attributed to the different dif- BF bundles are used: type 1, the diameter of the fibers bundles
fusivity of water into the materials, leading to moisture-induced ranges from 113–262 lm; type 2, the diameter of the fibers
interfacial cracks at an accelerated rate as a result of degradation bundles ranges from 88 to 145 lm. Type 2 displays the better
in the fiber resin interface region, as well as the state of water adhesion between the resin and the BFs, along with excellent
molecules existing in the BFC. Other studies have also reported compression strength, Young’s modulus, water absorption, and
a similar trend for aging of polymer composites at elevated thickness swelling, whereas type 2 displays the lower tensile
temperature.26,28 strength due to the fiber broken down further by the process.
These results are promising and demonstrate that BFC can be
prepared using high proportions of materials obtained from BF
Thickness Swelling. The evaluation of the dimensional stability bundles.
of the materials is especially important for the application of
bio-based composites. Hence, the thickness swelling of BFC ACKNOWLEDGMENTS
composites was carried out. Figure 5(c,d) present the thickness This study is partially supported by a grant from national forestry
swelling curves of phenolic BFC reinforced with 87% (w/w) BF public welfare industry research project (201304503).
bundles (type 1 and type 2) immersed in water at RT and at
BT. It is shown that BFC reinforced with 87% (w/w) BF bundles
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