Composites: Part A 40 (2009) 20132019

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Inuence of moisture absorption on the interfacial strength of bamboo/vinyl ester composites

Hongyan Chen a,b, Menghe Miao a,*, Xin Ding b
a b

CSIRO Materials Science & Engineering, PO Box 21, Belmont, Victoria 3216, Australia College of Textiles, Donghua University, Shanghai 201620, China

a r t i c l e

i n f o

a b s t r a c t
Moisture absorption is a major concern for natural bers used as reinforcement in structural composites. This paper reports a detailed study on the moisture sorption characteristics of bamboo strips and their inuence on the interfacial shear strength (IFSS) of bamboo/vinyl ester composite. The IFSS determined by pull-out test decreased dramatically as the fabrication humidity increased. The bamboo strips provide a reservoir of moisture which diffuses into the interfacial region and inhibits the hardening of vinyl ester matrix. The interface of the bamboo/vinyl ester composite can also be damaged due to moisture exposure after fabrication. Post-fabrication exposure of composites to moisture was found to be less damaging than the moisture exposure during the composite fabrication. The IFSS of the composite decreased by nearly 40% in the rst 9 d of water immersion. Further immersion up to 100 d did not cause any further reduction in interfacial shear strength. Crown Copyright 2009 Published by Elsevier Ltd. All rights reserved.

Article history: Received 12 June 2009 Received in revised form 30 July 2009 Accepted 6 September 2009

Keywords: A. Bamboo A. Polymermatrix composites (PMCs) B. Interface E. Cure

1. Introduction Natural bamboo itself is a unidirectional ber reinforced composite consisting of long and parallel cellulose bers (vascular bundles) embedded in a ligneous matrix (ground tissues). The bers have a specic density of 1.16 g/cm3 while the ground tissues, which are honeycomb foams, have a much lower density of 0.67 g/cm3 [1]. The density distribution of bamboo bers in the bamboo plant varies according to the radial position in the crosssection and along the length of the plant. The ber density is much higher in the outer skin region than in the inner region [2], and for this reason bamboo is often referred to as a functionally gradient material [3]. The compressive strength of bamboo is closely related to the mean ber density in the section [4]. Bamboo can be used as reinforcement in different forms, including whole bamboo [5], sections of bamboo [6], bamboo strips [7,8] and bamboo bers [9,10]. This study focused on bamboo strips, which can be produced by manual or machine splitting of the bamboo culm. Bamboo strip reinforced polymeric composites have been studied by various research groups. Shin et al. [11] found that the tensile strength of bamboo strip reinforced epoxy composites was superior to that of glass ber reinforced epoxy composites. The bamboo composite was found to be more durable than the bamboo itself [12]. Bashar et al. [13] observed improvement of mechanical
* Corresponding author. Tel.: +61 3 5246 4000; fax: +61 3 5246 4057. E-mail address: menghe.miao@csiro.au (M. Miao).

properties when the bamboo strips were made into composites with poly(methyl methacrylate) in the presence of additives. Das et al. [8] studied the effect of mercerization of bamboo strips on the mechanical properties of unidirectional bamboo strip reinforced novolac composites. Because of its structure and composition, bamboo absorbs moisture when it is exposed to humid conditions or immersed in water. The mechanical properties of bamboo may change signicantly due to moisture absorption depending on the bamboo species and treatment conditions. Chung and Yu [14] investigated the inuence of moisture on the mechanical properties of two species of bamboo, Kao Jue (Bambusa pervaribilis) and Mao Jue (that is Moso, Phyllostachys pubescens). When Kao Jue absorbed 20% moisture (by soaking in water), its bending strength was reduced by nearly a half and its bending modulus was reduced by about one-third. On the other hand, when moso absorbed 30% moisture, the bending strength did not change signicantly, but its bending modulus was reduced by about one-third. Godbole and Lakkad [15], soaked a bamboo of unspecied species in distilled water for 144 h, which allowed the bamboo to absorb 81.2% moisture by its dry weight. Consequently, the tensile strength of the bamboo was reduced by 37% and the tensile modulus was reduced by nearly a half. The transverse dimension of the bamboo swelled up to 6% due to the soaking. The mechanical properties of natural ber (such as ax, hemp and sisal.) reinforced composites can decrease considerably when they are exposed to moisture [1625]. Besides affecting the properties of the polymer matrix and the natural bers themselves,

1359-835X/$ - see front matter Crown Copyright 2009 Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.compositesa.2009.09.003

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moisture can seriously damage the bermatrix interface, leading to poor stress transfer efciencies from matrix to reinforcement [26,27]. The degradation process starts with the swelling of cellulose bers that develops stress at the interface and causes microcracking of the matrix around the swollen bers [19,28]. The cracks exacerbate water absorption and its attack on the interface. The absorbed water starts to establish intermolecular hydrogen bonding with the bers and thereby reduces the interfacial adhesion between the ber and the matrix, and water soluble substances start leaching from the bers. These eventually lead to the ultimate debonding between the ber and the matrix. For long periods of water exposure, biological activities (growth of fungi) can play an important role in the degradation of the natural bers. The damaging effects of moisture on the natural berresin interface could be reduced to some extent by different ber treatments [2934]. Compared to polymeric composites reinforced with glass bers and carbon bers, the natural ber composites generally have low interfacial strength. A major cause of the poor interface is the incompatibility between the hydrophilic natural bers and the hydrophobic polymer matrix. The moisture present during manufacture can further exacerbate this problem, leading to poor processability and low mechanical performance of composite [17]. For example, when methyl ethyl ketone peroxide (MEKP) is used as the catalyst, vinyl ester resin cures poorly or does not cure under excessive moisture conditions. Although the problem is known to the industry [35,36], quantitative relationship between the moisture exposure in manufacture and the interfacial bonding strength of nal composites has not been found in scientic literature. In this study, bamboo strips and vinyl ester resin were used to investigate the inuence of moisture on interfacial shear strength (IFSS). The large size and regular sectional shape make the bamboo strips a material particularly convenient for pull-out testing. The study was aimed to clarify how pre-fabrication moisture exposure affects the matrix hardening process and to establish the relative importance between pre-fabrication moisture exposure and postfabrication moisture exposure. 2. Materials The middle section of a mature moso bamboo plant (P. pubescens) grown near Jinhua, Zhejiang Province, China, was used in this investigation. The bamboo section was manually split into strips by a bamboo craftsman. All the strips used in this investigation were from the second and third layers below the epidermis to minimize variability in material properties. The strips used in pull-out specimens were 0.71.0 mm thick (radial direction in the plant), 2.0 3.0 mm wide and approximately 130 mm long. Longer strips (approximately 250 mm) were used for tensile testing. The matrix used in this study was a commercial vinyl ester resin SPV 6017 supplied by Nuplex Industries (Australia) Pty Ltd. (viscosity of 120230 MPas, tensile strength of 7085 MPa and elongation at break of 35%). A Norox 925H methyl ethyl ketone peroxide (MEKP) hardener was used for curing. Vinyl ester is commonly used with glass bers in the marine industry due to its good corrosion resistance and ability to withstand water degradation [35]. The resin is also known for its sensitivity to ambient conditions during manufacturing, especially when used together with MEKP. 3. Experimental 3.1. Moisture content and dimensional expansion The bamboo strips were dried in a vacuum oven dryer at 105 C for 5 h followed by cooling in a desiccator, as recommended in ASTM D2495-07. The dry weight (W0) was measured using an elec-

tronic balance to the accuracy of 0.0001 g. The predried sample was then conditioned in a humidity chamber set to a chosen relative humidity at the constant temperature of 20 0.1 C. The moisture content of the sample at any given time (Mt) was calculated from:

Mt

Wt W0 100% W0

The dimensional changes of the bamboo strips in width, thickness and length at each humidity condition were determined by using a digital micrometer that applies a standard compression force during measurement. 3.2. Tensile test of bamboo strips An Instron 5567 testing machine was used to determine the tensile properties of the bamboo strips according to ASTM D3039. The length of the tensile test samples was 250 mm. The bamboo strip specimens were predried in the vacuum oven and then conditioned to moisture equilibrium at the relative humidity level chosen to investigate. Again, the temperature was kept to a constant (20 0.1 C) in all humidity treatments. To minimize loss of moisture, the specimens were taken out from the conditioning chamber immediately before the tensile testing. The cross sectional dimension of each bamboo strip was measured by using the digital micrometer mentioned earlier. The tensile tests were conducted at a gauge length of 150 mm and a cross-head speed of 5 mm/min. 3.3. Pull-out test of bamboo strips embedded in vinyl ester resin The regular shape and large cross-sectional size of the bamboo strips are ideal for pull-out testing. Vinyl ester resin containing 1.5% MEKP hardener was lled into a cylindrical mold of 20 mm in diameter while a bamboo strip was kept in an upright position by a bracket. The embedded length of the strip was kept to 10 mm or less to ensure that the bamboo strips could be pulled out from the resin block instead of breaking. Predried bamboo strips were rst conditioned in the humidity chamber to reach their moisture equilibrium at the chosen relative humidity levels (the temperature was kept constant at 20 0.1 C in all cases). After the resin was lled into the pull-out test mold, the mold was immediately placed in the humidity chamber to cure under the chosen relative humidity. The cured specimens were stored in the humidity chamber under the same humidity and temperature conditions. To maintain the moisture content of the specimens, the specimens taken out from the humidity chamber were kept in a sealed plastic bag during transport to the pull-out testing room, and they were taken out from the sealed bag immediately before the pull-out test. The bamboo strip pull-out tests were also carried out on the Instron 5567 tensile tester. The resin block was placed on top of the upper clamp that was kept open and the exposed bamboo strip was gripped by the lower clamp. The gauge length was set to 20 mm, which gave a 50 mm distance between the resin surface and the gripping point. The pull-out test was carried out at a cross-head speed of 2 mm/min. The average interfacial shear strength (IFSS) of each specimen was calculated using the Kelly Tyson equation [37]:

Fm SL

where Fm is the maximum load recorded when debonding occurs, S is the perimeter of the cross section of bamboo strip, and L is the embedded length of the bamboo strip in the matrix. Twenty speci-

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mens were used for each evaluation, and the average value and standard deviation were reported. 4. Results and discussion
Moisture Content (%)

30

100

-----25

Moisture Content Relative Humidity 80

4.1. Moisture sorption behavior of bamboo strips When cellulose bers are exposed to moisture, the rst water molecules are absorbed directly onto the hydrophilic groups of the ber material and after that, the other water molecules are attracted either to other hydrophilic groups or they may form further layers on top of the water molecules already absorbed [38,39]. At high humidity levels, liquid water may be held by the forces of surface tension in capillary spaces available in the material. To obtain the moisture absorptiondesorption curve, the bamboo samples were subjected to a step-by-step moisture cycle while the temperature was kept to a constant 20 0.1 C. Due to the limitation of the conditioning chamber, the cycle started from 40% RH and increased in 10% steps up to 90% RH, then decreased stepwise down to 40% RH. Sample weight at each step was measured at a series of time intervals until the moisture absorption reached its equilibrium level (Me). Moisture equilibrium was considered to be reached when the instantaneous weight Wt of the sample varied less than 0.01% within 1 h, as recommended in ASTM D2495-07. The instantaneous moisture absorption by bamboo strips at each RH level initially increased with the square root of time and then slowed down as the moisture content approached equilibrium (Fig. 1a). This is similar to the behavior of other natural bers [12,34] and natural ber composites [13]. The equilibrium moisture contents for different relative humidity levels increased approximately in proportion to the relative humidity up till about 60% RH (Fig. 1b). The equilibrium moisture content then took off sharply at 70% relative humidity, and it nearly doubled as the relative humidity increased from 80% to 90%. This trend is very similar to that demonstrated by other cellulose bers, such as cotton [39]. In bamboo, the ground tissues that surround the cellulose bers occupy a large proportion of the volume in the bamboo strip (refer to the microphotographs in Fig. 7). These ground tissues are of a honeycomb structure [1] with numerous capillary spaces that are ideal sites for holding liquid water. As shown in Fig. 1b, the experimental relationship between relative humidity and equilibrium moisture content in bamboo strips tted quite well with the model proposed by Peirce [39]. Fig. 2 shows the change of equilibrium moisture content of the bamboo strips when the relative humidity was varied in a stepwise manner as indicated by the dotted lines. This equilibrium absorp-

20

absorption

desorption
60

15 40 10 20

0 0 200 400 600

0 800

Time (Hour)
Fig. 2. Moisture hysteresis of bamboo strips: change of equilibrium moisture content of bamboo strips in a cycle of absorption and desorption.

tiondesorption cycling curve demonstrated distinctive characteristics of hysteresis. In other words, the equilibrium moisture content is determined not only by the storage environment (relative humidity and temperature) but also by the previous humidity history of the material.
10 9 Width Thickness Length

Dimensional Expansion (%)

8 7 6 5 4 3 2 1 0 0 20 40 60

80

100

Relative Humidity (%)

Fig. 3. Dimensional expansion of bamboo strips in a cycle of absorption and desorption.

25

Equilibrium Moisture Content (%)

(a)
Moisture content (%)

30

RH 90%

(b)

30 25 20 15 10 5 0 Fit to Peirce's model

20 15 10 5 0 0 2 4 6 8
1/2

RH 80% RH 70% RH 60% RH 50% RH 40%

10

12

20

40

60

80

100

Square root of time (Hour )

Relative Humidity (%)

Fig. 1. Moisture absorption curves from oven dry to equilibrium at different levels of relative humidity (temperature was kept at 20 C): (a) absorption curves at different relative humidity levels and (b) relationship between relative humidity and equilibrium moisture content.

Relative Humidity (%)

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Bamboo strips undergo an anisotropic dimensional expansion as they absorb moisture. This is shown in Fig. 3. The expansion in the width direction (i.e., along the circumference of the bamboo plant) was the largest, followed by the expansion in the thickness direction. The dimensional expansion along the length direction was 100 times smaller than that along the width. Like moisture content, the dimensional expansion of bamboo strips demonstrated hysteresis as the samples went through a moisture absorptiondesorption cycle. 4.2. Effect of moisture absorption on tensile properties of bamboo strips Moisture absorption has a softening effect on the bamboo strip as indicated by the consistent increase in breaking strain (Fig. 4a) and decrease in elastic modulus (Fig. 4b). Moisture absorption also caused a small increase to the tensile strength of the bamboo strips, as shown in Fig. 4b. These are in broad agreement with the bending test results on moso bamboo by Chung and Yu [14]. They found that the moisture absorption had no effect on extural strength. It should be noted that their bending test was conducted on bamboo trunks while our tensile test was done on bamboo strips taken from the high ber density region of the bamboo trunk. Improved tensile strength of cellulose bers due to humidication has been reported by other workers. For example, Stamboulis et al. [22] reported that after being humidied at 90% RH, green ax bers increased their tensile strength by about 20%. They suggested that the availability of some free water molecules had a

plasticizing effect which was advantageous to the strength of cellulose bers. 4.3. Interfacial shear strength (IFSS) of bamboo/vinyl ester composites Fig. 5 shows two loaddisplacement curves obtained from the bamboo strip pull-out tests. Fig. 5a is a typical curve of specimens manufactured at dry and low RH conditions, and Fig. 5b is a typical curve of specimens manufactured at high RH conditions (>80% RH). For the specimens produced at lower RH, the loaddisplacement curves exhibited typical linear-elastic behavior up until it reached its maximum load, followed by a precipitous load drop when the interface failed completely and then frictional pull-out. The pullout force of samples produced at high RH conditions was of much lower magnitude, coupled with high frequency uctuations. In this case, the maximum load spike in the loaddisplacement curve was used to calculate the IFSS. The force uctuations appeared to be the result of a high frequency stick-slip frictional force between two surfaces sliding apart. There was no sudden load drop after the maximum load point, indicating a gradual transition from debonding to pull-out, which continued until the total embedded length of the bamboo strip was extracted. This behavior is typical of a poor interfacial bonding between ber and matrix [40]. Fig. 6a shows how the interfacial shear strength of the bamboo/ vinyl ester composite was affected by the humidity condition during manufacture. The IFSS decreased steadily with the increase of relative humidity at manufacture. As compared with the composites manufactured at dry condition, the IFSS value was reduced

(a)
Breaking strain (%)

1.6 1.4

(b)
Tensile Strength (MPa)

400

Tensile Strength Tensile Modulus

50000

1.2 1 0.8 0.6 0.4 0.2 0 0 10 20 30 40 50 60 70 80 90 100

40000 300 30000 200 20000 100

10000

Relative humidity (%)

10

20

30

40

50

60

70

80

90

0 100

Relative Humidity (%)

Fig. 4. Effect of humidity on the tensile properties of bamboo strips: (a) breaking strain and (b) tensile strength and modulus.

(a)

600 500

(b)

3 400

Load (N)

Load (N)

300 200

1 100 0 0.0 0 0.0

0.5

1.0

1.5

2.0

2.5

3.0

0.5

1.0

1.5

2.0

Displacement (mm)

Displacement (mm)

Fig. 5. Typical loaddisplacement curves from pull-out tests of bamboo strip/vinyl ester composites: (a) low RH and (b) high RH (>80%).

Tensile Modulus (MPa)

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(a)
IFSS (MPa)

12 10

(b)
IFSS (MPa)

12 10 8 6 4 2 0 0 5 10 15 20 Bamboo moisture content (%) 25 30

8 6 4 2 0 0 20 40 60 80 100

Relative humidity (%) during manufacture

Fig. 6. Inuence of relative humidity (a) and moisture content (b) during manufacture on interfacial shear strength of resultant composites.

by over a half as RH increased to 70%, by more than 90% at 80% RH, and to almost zero value at 90% RH. This drop of IFSS was mainly attributed to the poor interfacial bonding formed at the high relative humidity conditions. The bamboo dimensional expansion due to moisture absorption had little to do with the IFSS deterioration. To illustrate this, one set of specimens manufactured at dry condition were conditioned to moisture equilibrium at 80% RH and then tested for IFSS. Despite the swelling of bamboo strips inside the resin block, which should increase the mechanical locking between the bamboo strip and the matrix, the average IFSS suffered a small loss, from 10.82 MPa to 9.58 MPa. Damage caused by post-fabrication moisture exposure will be discussed in Section 4.4. Another set of specimens manufactured at 80% RH were dried in a desiccator for 48 h before subjecting to pull-out test. The drying of the composite caused a reduction of IFSS, from 0.8 MPa to 0.25 MPa. The relationship between IFSS and the equilibrium moisture content of bamboo strip in composite manufacture is plotted in Fig. 6b. The IFSS decreased almost linearly with the increase of bamboo moisture content from 0% to about 12%. The rate of decrease suddenly accelerated after this point. A further increase of 2% in bamboo moisture content caused a reduction of more than 80% in IFSS. The inuence of moisture during manufacture on the quality of interface formed between the bamboo strip and the vinyl ester matrix may be further demonstrated by the optical microphotographs in Fig. 7. Small bamboo/vinyl ester composite samples were prepared and cured at dry condition (0% RH) and at 80% RH, respectively. After being conditioned in the laboratory (20 C and 65% RH), the composite samples were sectioned by using an ultra-

microtome and then observed under an optical microscope. The specimen produced at dry condition showed no visible void at the interface between the bamboo and the matrix (Fig. 7a) while the sample produced at 80% RH exhibited thin void lines along the brous region and wide void spaces along the ground matrix regions (Fig. 7b). The capillary water accumulated in the honeycomb cells in the ground tissue regions became a physical barrier between the bamboo and the vinyl ester matrix, leading to the formation of these wide voids in the nal composite. 4.4. Inuence of water immersion on composite interface The bamboo strips were dried at 105 C for 5 h followed by cooling in the desiccator. To further eliminate the effect of moisture absorption, the impregnated specimens were placed in the desiccator for curing. The cured specimens were then immersed in 2 L beakers of tap water at room temperature (20 C) for different time intervals. Ten specimens were taken out from the water beakers at the end of each predetermined time interval. Immediately before subjecting the specimens to pull-out test, surface water was removed from the specimens using absorbent tissue papers. The interfacial shear strength is plotted with water immersion time in Fig. 8. The IFSS of the specimens increased slightly after being immersed for one day. In the following 8 d, the interfacial strength decreased linearly with immersion time. The accumulated loss of interfacial strength on the ninth day amounted to about 38%. Thereafter, the interfacial shear strength remained very stable as the immersion time extended up to 100 d. Kim and Seo [28] subjected sisal ber in vinyl ester and epoxy matrix composites to cy-

Thin void line

Wide void space

Wide void space

(a)

(b)

Fig. 7. Optical microphotographs of sectioned bamboo vinyl ester composites prepared at dry condition (a) and 80% RH (b).

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5. Conclusions Bamboo is a hydrophilic material that absorbs a signicant amount of moisture at standard humidity conditions. Bamboo strips demonstrate moisture sorption hysteresis similar to other natural bers such as ax and hemp. They also experience anisotropic expansion with the absorption of moisture. The largest expansion took place along the circumference of the bamboo culm and this was twice as much as that in the radial direction. The longitudinal expansion was negligibly small. Moisture absorption softened the bamboo strips, causing an increase in extensibility and a reduction in elastic modulus while the tensile strength was not signicantly affected. The inuence of moisture absorption on the interfacial shear strength (IFSS) of bamboo/vinyl ester composite was studied using the pull-out test. The relative humidity in composite manufacture had a severe impact on the IFSS of the resulting composites. The IFSS achieved at normal room conditions (20 C, 60% RH) was only a half of what is achieved in the dry condition. Composites produced at high relative humidity conditions (80% and 90%) had negligible interfacial strength. Exposure of the bamboo/vinyl ester composite to water caused signicant damage to the interfacial shear strength. The damage took place in the rst 9 d, causing a 38% reduction in IFSS. Prolonged water immersion up until 100 d did not result in further reduction in IFSS. Therefore, exposure to high humidity during material storage and composite manufacture can be much more damaging to the interfacial strength of the nal composites than post-fabrication moisture exposure. Acknowledgements The authors would like to acknowledge the China Scholarship Council for granting a scholarship that enabled Honyan Chen to pursue this work at CSIRO and the Cooperative Research Centre for Advanced Composite Structures Limited (CRCACS) for its support of their work, which has been carried out as part of the CRC ACS research program. The assistance of Margret Pate on microscopy is highly appreciated. References
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Residual IFSS (MPa)

12 10 8 6 4 2 0 0 20 40 60 80 100 120

Time immersed in water (day)

Fig. 8. Residual interfacial shear strength of bamboo strip/vinyl ester composite after water immersion.

cles of wetting and drying (each cycle consisted of 9 d of wetting at 21 C and one day of drying at 50 C) and tested for change of mechanical properties. They found a similar decreasing pattern of breaking stress of the composites, i.e., the breaking stress suffered a signicant decrease after one cycle and then maintained its value up until ve cycles of wetting and drying. There are three possible scenarios for the reduction of the IFSS of bamboo/vinyl ester composite caused by water immersion: water damage on the bamboo strip, on the vinyl ester matrix, or on the interfacial bonding. The weakest of the three elements (bamboo, matrix and interface) determines the actual composite failure mechanism. Vinyl ester matrix is known for its good water resistance [35]. The exural strength of cured neat vinyl ester resin was not signicantly affected after being immersed in water for 1300 h (i.e., 54 d) [41]. We tested the tensile strength of the bamboo strips without water immersion, after immersion in water for 50 d and 100 d. As shown in Fig. 9, the bamboo strips maintained their tensile strength up until 50 d of immersion and the tensile strength started to deteriorate sometime between 50 d and 100 d. At 100 d, the bamboo strips lost 46% of their tensile strength. This change of bamboo strip strength was not reected in the IFSS results in Fig. 8. The reduction of IFSS in the initial nine-day period can thus be attributed to water damage on the interface. The hydroxyl groups in the bamboo structure allow a large number of hydrogen bonds to be formed between the macromolecules of the cellulose and polymer. With the absorption of water, hydrogen bonds between water molecules and the cellulose bers are formed, causing loss of compatibilization between the cellulose bers and the matrix, which results in debonding and weakening of the interface adhesion [23].
350 300

Tensile strength (MPa)

250 200 150 100 50 0 0 20 40 60 80 100 120

Time immersed in water(day)

Fig. 9. Effect of water immersion time on the tensile strength of bamboo strips.

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