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2012 International Conference on Biobase Material Science and Engineering (BMSE)

Effects of Thermal Treatment on Surface Color,


Dimensional Stability and Mechanical Properties of
Bamboo-based Fiber Composites

Yamei Zhang, Wenji Yu


Research Institute of Wood Industry
Chinese Academy of Forestry
Beijing, China

Corresponding author: Tel.: +86 10 62889427; Fax: +86 10 62889427. E-mail address: yuwenji@caf.ac.cn

AbstractBamboo fibrous veneers were fabricated using a new 2], and increases the dimension stability [3, 4], but it reduces
technology and heat-treated in a vacuum by steaming at pressure the strength properties and lowers the surface wettability [5, 6,
of 0.40 MPa (151) for 170 min. Bamboo-based fiber composites 7].
(BFC) were made from bamboo fibrous veneers that were before A new technology for making BFC was developed at the
and after thermal-treated using a compression molding method. Chinese Research Institute of Wood Industry. This technology
The results pointed out that, chemical degradation occurred in treats the entire bamboo culm as a manufacturing unit and
bamboo fibrous veneers, mainly in relation to hemicelluloses, and
overcomes the bonding problems for outer and inner bamboo
its reduction reached 59.15%. The pH value decreased
significantly, whereas acid buffering capacity increased culms. It improves bamboo use efficiency, allowing it to
compared with control samples. The color of thermal-treated exceed 90% [8]. However, due to bamboos hygroscopic nature,
BFC was darkened; dimensional stability was significantly the species has some undesirable properties such as swelling
improved by reducing thickness swelling and wideness swelling. and shrinkage caused by water absorption and desorption,
The mechanical properties were affected with reduction in which limit applications.
Modulus of Rupture (MOR) and Horizontal Shear strength (HS), Compared with wood thermal treatment, there is no need to
but Modulus of Elasticity (MOE) was affected slightly. Thus it is consider bamboo fibrous veneers deformation and crack, so
shown that the surface color and dimensional stability of BFC treatment duration is much shorter than that of wood. Besides,
can be changed and improved by thermal treatment. thermal treatment increases dimension stability, and makes the
Keywords-Bamboo-based fiber composites; chemical material more suitable to be applied to the interior material if
compositions; surface color; dimensional stability; mechanical the strength requirement is not high. Much research has been
properties done with BFC [9, 10, 11], but research of thermal treatment
on it was not found. In this paper, Phyllostachys pubescen
I. INTRODUCTION bamboo was made into fibrous veneers using the new
technology. The bamboo fibrous veneers were heat-treated at
Bamboo has been developing rapidly in China since the 0.40MPa steam pressure for duration of 170min and then were
1990s as an important forest resource alternative for wood. made for BFC. The effects of thermal treatment on the surface
Along with the development of the bamboo-based panel color, dimensional stability, and mechanical properties of BFC
industry, bamboo glued-laminated timber and bamboo were investigated. In order to better understand the change
scrimber have elicited considerable attention as sustainable and reasons, the chemical properties of bamboo fibrous veneers
renewable materials for furniture and flooring. Flooring and were also studied.
furniture made from bamboo can be divided into natural and
carbonized colors based on surface color. Generally, bamboo II. MATERIAL AND METHODS
slabs are placed at 0.40 MPa to 0.50 MPa steam pressure and
heated for 1 h to 2 h in the process to obtain darker color A. Material
(commonly called carbonization). Lots of heat-treated bamboo Phyllostachys pubescen bamboo, aged 4 years was obtained
products have been produced for peoples needs in different from Anhui province. The bamboo was sawn into a bamboo
color. tube 2500 mm in length, which was longitudinally split into
Heat treatment has been investigated since the middle of two semicircular bamboo tubes. After the inner nodes were
last century for the purpose of avoiding the toxic effects of removed, the semicircular bamboo tube was pushed into the
chemical treatment which involves the chemical substances. designed fluffer along the grain direction, and then bamboo
Now, thermal treatment has been wildly used in wood industry. fibrous veneers were fabricated.
Heat treatment can make the material surface color darker [1,

978-1-4673-2383-3/12/$31.00 2012 IEEE 132 Changsha, China


B. Thermal treatment of bamboo fibrous veneers and dried at 105 to a constant mass. Two sets for each
The bamboo fibrous veneer specimens at 9% to 11% sample were prepared, and the error rate of calculation of the
moisture content were immersed in carbonation equipment - a two measurements was less than 0.40%. The result was the
horizontal carbonization furnace (THL1200X4300, made in average of the two sets. Bamboo is not wood material; the
China) set at steam pressure of 0.4MPa (151) for duration of content of ash specification should thus be subtracted in the
170min. After thermal treatment, the bamboo fibrous veneers calculation. However, for relative comparison, this was not
were reconditioned to reach equilibrium. followed.
c) Content of cold water extractives measurement
C. Manufacture of BFC
Approximately 2g (0.1mg) of bamboo flour was weighed
The bamboo fibrous veneers were the material for BFC. using 500-mL beakers. A total of 300 mL distilled water was
Commercial Phenol resin was provided by Beijing Dynea added to each sample, and let stand for 48h at 232. The
chemical industry limited company. The bamboo fibrous
solution was then filtered with a tared sintered glass crucible
veneers were immersed into PF resin for attaining 8% solid
before it was washed with distilled water. Then, the solution
resin based on bamboo-dry weight. When dried at 5% to 8%
was dried at 1052until a constant mass was obtained. The
moisture content, the bamboo fibrous veneers with PF resin
crucible was weighed again to the nearest 0.1 mg. The
were formed on steel caul-plates with 300mm170mm and
extractive was calculated as the percent of the extracted, oven-
then kept pressed under 4.5 MPa for 20min at 145 for a dry weight of the sample. Each sample was analyzed twice.
target thickness of 20 mm. The target panel density was 1100
kg m-3. d) Content of hot water extractives measurement
D. Measurements of property Approximately 2g (0.1mg) of bamboo flour was weighed
using 300-mL beakers. A total of 200mL of hot distilled water
1) Bamboo flour preparation
For chemical analysis, the bamboo fibrous veneers were (95 to 100) was added to each, and kept standing for 3h in
sawn into small pieces and milled. Powdered samples were boiling water, fitted in a reflux condensing tube. The solution
sieved into three fractions and the middle fraction (0.25- was then filtered with a tared sintered glass crucible before
0.42mm) was used for chemical determinations. being washed with distilled water. Next, the solution was dried
at 1052 until a constant mass was obtained. The crucible
2) Measurements of bamboo fibrous veneers chemical was weighed again to the nearest 0.1 mg. The extractive was
properties calculated as the percent of the extracted, oven-dry weight of
a) Content of Holocellulose measurement the sample. Each sample was analyzed twice.
Firstly, 2g (accurate to 0.0001g) of powder was bounded
with cotton after being wrapped by qualitative filter paper and e) PH value and buffering capacity measurement
extracted by benzene-ethanol. The treated bamboo powders The bamboo powders (approximately 3g, 0.1mg) were
were then placed in a 250-mL conical flask containing 65mL placed in 50-mL beakers. A total of 30mL of distilled water
distilled water, then heated at 75. Acetic acid (0.5 mL) and that was boiled and cooled down to room temperature was
sodium chlorite (0.6g) were added into the solution each hour added to the powders. The mixture was let stand for 15min
until the powder turned white. The mixture was shaken after being stirred for 5min, and then stirred again for 5min
constantly. The mixture was then filtered and washed with before it was let stand for another 5min. The acidity of UB-10
distilled water until the filtrate was no longer acidic, washed was used to determine the pH values. Prior to each titration, the
with acetone three times, and dried at 105 to a constant mass. pH meter was calibrated with standardized buffer solution to a
Two sets for each sample were prepared, and the error rate of pH of 4.
calculation of the two measurements was less than 0.40%. The The aqueous extract for pH value of reflux extraction liquid
result was the average of the two sets. Bamboo is not wood and buffering capacity measurement was prepared by refluxing
material; the content of ash specification should thus be 25g of dry bamboo powders in 200-mL of distilled water for
subtracted in the calculation. However, for relative comparison, 20min. Two sets for each sample were prepared. After
this was not followed. refluxing, the mixture was filtered through filter paper. After
calibration, exactly 50 mL of bamboo extract solution was
b) Content of -cellulose measurement pipetted into a 150-mL breaker. The pH of the extract solution
The holocellulose (separated according to the description was measured, and then titrated to a pH of 3(for alkaline
above) was placed in a 150-mL breaker and infused with buffering capacity) or 11(for acid buffering capacity) with
17.5% NaOH (30mL). The beaker was then placed in the water 0.0125 mol/L H2SO4 or 0.025mol/L NaOH solutions. The pH
bath (20) for 45min. A total of 30mL distilled water was of the constantly stirred solutions was measured after each
then added. Next, the mixture was filtrated and washed with incremental addition of acid or alkali. All pH and buffering
9.5% NaOH (25mL) three times and washed again with capacity measurements were conducted by using an acidity of
distilled water (400mL). Acetic acid was then added into the UB-10. Prior to each titration, the pH meter was calibrated with
residue and was held for 5min. The residue was washed with a standardized buffer solution to a pH of either 4 or 9,
distilled water until the filtrate solution was no longer acidic, depending on the buffering capacity measurement to be made.

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3) BFC property measurements radiata wood at 160 to 210, and found that the total
a) Color Measurement hemicelluloses content was reduced by about 35-69 %.
The BFC color was measured with a spectrophotometer The -cellulose content decreased only by 11.8% compared
(Mercury 2000) under a D65 light source and an observer angle with control samples due to its crystalline structure [13]. The
of 10. The sensor head of the spectrophotometer was 8mm in thermal degradation of cellulose requires higher temperature.
diameter. Color was expressed according to the CIEL*a*b* 2) Changes in water extractives, pH values and buffering
system. The difference in L*, a*, and b*and the total color capacity
change (E*) were calculated with the following formulas: Table.2 indicates that the contents of cold and hot water
L*= L*-L*0 extractives after heat treatment increased significantly,
a*=a*- a*0 approximately 3.2 and 2.9 times respectively as much as that of
control samples. In generally, in addition to containing the
b*= b*- b*0 cold-water extractives, the hot water extractives also include
starch and pectin [14]. The increase in water extractives shows
E (L ) 2 (a ) 2 (b ) 2
(1) that thermal treatment results in many more small soluble
*
where L represents lightness with values varying from 0 molecules due to the degradation of hemicelluloses and
(black) to 100(white). The parameters a* and b* parameter cellulose.
describe the chromatic coordinates on green-red (a*) and blue- TABLE II. CHANGES IN WATER EXTRACTIVES, PH AND BUFFERING
yellow (b*) axes. L0*, a0* and b0*are the reference values CAPACITY
obtained as the average of 20 control specimens. Color was 1 2
CW HW pH Buffering AA RA
measured for each group at 20 points near the outer bamboo (%) (%) pH of capacity (mmol l-1) (mmol l-
culms. The results were then averaged. REL (mmol l-1) 1
)
AL AC
b) Dimensional stability and mechanical strength
measurements Control 5.7 7.18 5.2 5.0 0.4 0.8 0.4 2.1
Treated 17.8 20.7 3.9 3.8 0.4 3.3 2.9 8.6
Swelling measurement on the samples were conducted to 1
Absolute acid buffering capacity=Acid buffer capacity-alkali buffer capacity
0.01mm accuracy at marked position before and after 2
Relative acid buffering capacity=Acid buffer capacityalkali buffer capacity
immersion in 632water for 24h. Thickness swelling (TS) (CW represents Cold water extractives; HW represents Hot water extractives;
and wideness swelling (WS) were determined using ISO 4859- pH of REL represents pH of reflux extraction liquid; AL represents alkali
buffer capacity; AC represents Acid buffer capacity;1AArepresents 1Absolute
1982. Dimensional stability was measured for six specimens acid buffering capacity; 2RA represents 2Relative acid buffering capacity)
each group, the results were then averaged.
Modulus of rupture (MOR), modulus of elasticity (MOE) The pH value reduced significantly after thermal treatment
and horizontal shear strength (HS) were carried out for heat- and reached the reduction of 25.5% compared with control
treated and control samples, based on ASTM D 1037-99. Six samples. According to the research of Windeisen et al. [15], the
specimens were obtained for each group to evaluate MOR, degradation of acetyl in hemicelluloses component can
MOE and HS. generate acetic acid. Sundqvist et al. [16] found that, the birch
would produce acid and formaldehyde when heated at 160 to
III. RESULTS AND DISCUSSION 200, which can promote the degradation of carbohydrate as
catalysts later. So, the increase in the water extractives may be
A. Analysis in chemical properties of bamboo fibrous one of the reasons for the decrease in pH values.
veneers The pH values of reflux extraction liquid were lower than
1) Change in the content of chemical components that of water extractives because of high temperature, which
resulted in more dissolved acid. During the hot pressing of
TABLE I. CHANGES IN THE CONTENT OF CHEMICAL COMPONENTS bamboo-based panels, the slabs were in high temperature that
Holocellulose -cellulose Hemicelluloses was above 100, the pH value of reflux extraction liquid was
(A) (B) (A-B) more useful.
Treatment (%) (%) (%)
After thermal treatment, the acid buffering capacity
Control 68.3 45.4 22.8 increased significantly compared with control samples, while
Treated 49.4 40.1 9.3 the alkaline buffer capacity did not change much. From the
definition, absolute acid capacity or relative acid capacity
Table.1 indicates that the holocellulose content decreased should stand for the final [H+] in the solution. The higher the
by 27.6% after thermal treatment compared with control absolute or relative acid buffering capacity is, the higher the
samples. The most significant change was for hemicelluloses [H+] is in the solution.
content, which decreased by approximately 59.2%. This
finding is in agreement with that of Dubey et al. [12], who B. The measurement results of BFC properties
studied the chemical composition of oil heat-treated Pinus
1) Color change of BFC

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TABLE III. CHANGES IN SURFACE COLOR OF BFC bamboo and degrade first (between 160 and 260) since
Color in CIE Color difference their low molecular weight, and their branching structures
system facilitate a faster degradation compared with other components
*
L a* b* L *
a* b* E* present in wood [13].The organic components of bamboo are
Control 69.3 7.0 30.9 similar to that of wood. According to the wood research, the
Treated 43.6 8.95 17.8 25.7 1.8 13.1 28.9 decrease in swelling of heat-treated wood is mainly due to the
reduction in hydroxyl group content of wood [18, 19] or due to
The result from measurement show a clear influence of the formation of cross-linking during thermal treatment [3]. A
thermal treatment on color coordinates L* a* b*, as shown in crosslinking increment makes the molecules less elastic and
Table.3. The color of heat-treated samples was darkened. reduces the possibility to enlarge the cellulose microfibrils,
Lightness (L*) decreased by 37.1%, which indicating the color thus it reduces wood ability to absorb water.
changes to black tone direction. The b* had similar trend as L*,
3) Mechanical property measurement
the reduction of b* was 42.5%. Lower values show the surface
color is closed to the center axis direction of the yellow-blue As shown in Table.4, it can be observed that thermal
axis after thermal treatment. The changes in a* chromatic treatment resulted in a significant reduction in MOR, MOR
coordinates followed another pattern, its values increased by decreased by 27.3% compared with control samples. Whereas,
25.7% after thermal treatment. The coordinate a* shifts MOE was more resistant to thermal treatment, it decreased
positively indicating the color of BFC become more red. only by 7.6%.
The decrease in MOR can be explained by thermal
As shown in Table.3, the color change (E*) was
degradation. According to the research of Curling et al. [20],
significant compared with control samples. E* increased by
bending property losses are highly associated with the kind of
28.9 units after thermal treatment. According to results
carbohydrate that is being degraded: loss of MOR corresponds
obtained by Varga and Van Der Zee [1], the main factors of the
to decrease in hemicellulose, whereas dropping MOE
color change were the dissolution and oxidation of wood
corresponds to cellulose loss. Menezzi et al. [21] found that the
components and the decomposition of the extractives.
contents of galactan, arabinan and mannan were reduced as
Sundqvist et al. [16] found that, the birch heat-treated at 160
treatment became more severe, while the content of glucan
to 220 can produce acetic acid, the heat absorption remained almost unaffected. The degradation of sugar contents
coefficient of heated lignin increased in acidic condition; can explain the drop in MOR while the unchanged glucan
thereby it increased the degree of wood discoloration. The content explains the unaffected MOE. According to the
lignin heat-treated in acidic conditions increased more phenolic research of Sivonen et al. [22], the deterioration of the
hydroxyl groups, and new phenolic hydroxyl groups were hemicellulose starts at or below 180, which produced acetic
formed, so the color of the wood was deepened [17]. But acid helping to degrade the structure of the hemicellulose.
explanations for this phenomenon are lack in bamboo, so Cellulose and lignin deteriorate at higher temperatures and at
further research need to be done. slower rate than hemicellulose.
2) Dimensional stability measurement For evaluating the internal bond strength (IB) property of
The density and moisture content of BFC were 1100 kg/m3 BFC, Horizontal shear strength was investigated.
and 8%, respectively. The dimensional stability in thickness (T) Table.4 indicates that, HS decreased by 29.0% after thermal
and wideness (W) direction in the water immersion test (63, treatment compared with control samples. The decrease in HS
24h) is shown in Table.4. can be mainly due to the change in pH value and buffering
capacity. According to the wood research, either pH or
buffering capacity of water extractives has a strong correlation
TABLE IV. DIMENSIONAL STABILITY AND MECHANICAL PROPERTIES OF
BFC with gel time of wood flour [23, 24]. The knowledge of pH and
buffering capacity of wood is an important consideration to a
Dimensional stability Mechanical properties better understanding of the wood gluing processes [25, 26].
Lebow and Winandy[27] and Winandy and Lebow[28] found
TS WS MOR MOE HS
(MPa) (GPa)
that cumulative thermal effects on strength and chemical
% % MPa
composition were not only related to exposure duration but
Control 6.8 1.6 209 18.9 21.2
Treated 5.0 1.3 152 17.5 15.0
also to the pH of the environment in which the biomaterials
were exposed during processing and in service. Thus, any
TS and WS decreased by 26.5% and 22.8% respectively discussion of heat treatments of bio-composites must also
after thermal treatment compared with control specimens. This include consideration of the pH effect from urea-formaldehyde
implies that BFC become more stable after heat treated at high (UF), PF, polymeric diphenyl-methane diisocyanate (PMDI),
temperature. or binderless systems. Poblete and Roffael [29] found that
As seen from the analyses in chemical components, thermal treatment alone in particleboard hot-pressing led to
hemicelluloses content decreased significantly after thermal decreased wood pH values.
treatment. That may be the reason of improved dimensional The pH value was significantly lower after thermal
stability of samples treated in pressurized steam. treatment, indicating that acidity in bamboo is added. In the
Hemicelluloses are the largest hygroscopicity component in paper, the BFC were made by using Phenolic resin adhesive

135
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IV. CONCLUSIONS
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