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Journal of Thermoplastic 

Composite Materials 

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Thermal and Mechanical Properties of Wood Flour/Talc-filled Polylactic 

Acid Composites: Effect of Filler Content and Coupling Treatment 

Sun-Young Lee, In-Aeh Kang, Geum-Hyun Doh, Ho-Gyu Yoon, Byung-Dae Park and 

Qinglin Wu 

Journal of Thermoplastic Composite Materials 

2008; 21; 209 

DOI: 10.1177/0892705708089473 

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Thermal and Mechanical Properties 

of Wood Flour/Talc-filled Polylactic 

Acid Composites: Effect of Filler 

Content and Coupling Treatment 

SUN-YOUNG LEE, 1, *IN-AEH KANG, 1 GEUM-HYUN DOH, 1 

HO-GYU YOON, 2 BYUNG-DAE PARK 3 AND QINGLIN WU 4 

1 Division of Environmental Material Engineering 

Department of Forest Products, Korea Forest Research Institute 

Hoegi-Ro 57, Dongdaemun-Gu, Seoul 130-712, Korea 

2 Department of Material Science and Engineering 

Korea University, Anam-Dong, Seongbuk-Gu, Seoul 136-701, Korea 

3 Department of Forest Products, Kyungpook National University 

1370 Sankyuk-Dong, Buk-Gu, Daegu 702-701, Korea 

4 School of Renewable Natural Resources, Louisiana State University 

Agricultural Center, Baton Rouge, LA 70803, USA 

ABSTRACT: Wood flour (WF) and talc-filled polylactic acid (PLA) composites are 

prepared by melt compounding and injection molding. The effects of filler loading 

and silane treatment, the thermal and mechanical properties of the composites are 

studied. Loading of WF and WF/talc mixture into neat PLA results in a small 

decrease in the glass transition and crystalline temperatures of the composites. The 

use of WF, talc and silane in the composites causes successively larger decreased in 

the composite crystallinity. The addition of talc and silane to PLA/WF composites 

improved the tensile modulus. The tensile strength of the composites decreases 

slightly with the addition of talc, but it considerably improves with the use of 1 wt% 

silane. Morphological analysis shows improved interfacial bonding with silane 

treatment for the composites. 

KEY WORDS: polymer composites, coupling, PLA, talc, wood flour. 

*Author to whom correspondence should be addressed. E-mail: nararawood@forest.go.kr 

Journal of THERMOPLASTIC COMPOSITE MATERIALS, Vol. 21—May 2008 209 

0892-7057/08/03 0209–15 $10.00/0 DOI: 10.1177/0892705708089473 

ß SAGE Publications 2008 

Los Angeles, London, New Delhi and Singapore 



210 S.-Y. LEE ET AL. 

INTRODUCTION 

THE USE OF lignocellulosic materials and polymers from renewable 

resources has recently attracted increasing attention, predominantly due 

to environmental concerns and the depletion of petroleum resources [1–3]. 

In general, polymers from renewable resources can be categorized into 

natural polymers such as starch [4–6], protein and cellulose [7–9], and 

synthetic polymers [10–12]. The development of synthetic polymers using 

monomers from natural resources provides a new direction for the 

development of biodegradable polymers. 

The most common biodegradable synthetic polymers are aliphatic 

polyesters such as polylactic acid (PLA), polyglycolic acids (PGA), 

polycaprolactone (PCL), and polyhydroxybutyrate (PHB). Among these 

biopolymers, PLA as biodegradable aliphatic polyester is of increasing 

commercial interest, because of its desired mechanical strength, thermal 

plasticity, and biocompatibility [13,14]. PLA has been used for many 

applications including grocery and composting bags, automobile panels, 

textiles, and bio-absorbable medical materials [15,16]. PLA is generally more 

expensive than many petroleum-derived commodity polyolefins such as 

polypropylene (PP) and polyethylene (PE). However, its price has been 

falling recently as more biopolymer production comes on-line [17]. 

The compounding of fillers obtained from various sources into polymer 

matrices has been a well-accepted process to enhance mechanical and thermal 

properties of materials [1,2,18]. Wood flour (WF) and talc are two commonly 

used fillers for wood plastic composites (WPCs) [19,20]. The use of WF can 

reduce material costs and provide specific properties such as low density, high 

specific stiffness, and biodegradability [21–24]. In particular, WPCs with 

50 wt% or less plastic by weight, have been accepted by the construction 

industry and homeowners, largely for decking, fencing, roofing, window 

profile, and automotives [21]. Talc (up to 30% by weight) can have a positive 

influence on modulus, strength, processing efficiency, creep and elastic recovery 

performance of WPCs [25]. A combination of organic (e.g., wood) and 

inorganic (e.g., talc) fillers in PLA may lead to interesting composite properties. 

In the intricate structure and morphology of polymer reinforced by 

organic and/or inorganic fillers, there is a problem related to the character 

and extent of interaction at the polymer-filler interfaces [21]. The established 

procedure for improving the interfacial adhesion of polymer and wood fiber 

is the use of coupling agent, resulting in a good chemical and/or physical 

bonding between polymer matrix and particle surfaces [26]. For example, 

various types of silanes have been developed to promote the interfacial 

adhesion. Organo-functional silanes are used to couple organic polymers 

with inorganic materials such as talc, silica, and mica [27]. 



Thermal and Mechanical Properties of WF/Talc-filled PLA Composites 211 

Most of the polymer composites are generally subjected to a thermal 

degradation at elevated temperatures. It is important to understand the 

effects of the processing temperature on the thermal degradation process, 

since there is constant thermal stress during the manufacturing of filler 

reinforced composites. Fundamental information regarding the thermal 

stability of natural fiber reinforced composites has been obtained from 

thermogravimetric analysis (TGA) and differential scanning calorimetry 

(DSC) [28]. Additional information on the thermal and mechanical properties 

can shed more light on the manufacture of the composite materials. 

The objective of this study was to investigate the effects of WF and talc 

loading and silane treatment on thermal, mechanical and morphological 

properties of the PLA-based composites. TGA, DSC, scanning electron 

microscopy (SEM), and stress–strain behavior were used to evaluate the 

thermal degradation, thermal transition, morphological, and mechanical 

properties of the composites. 

Materials 

MATERIALS AND METHODS 

Polylactic acid (2100D, M w ¼ 180,000–210,000 g/mol and MI ¼ 5–15 g/ 

10 min) was obtained from the Natureworks Õ Co. (Minnetonka, U.S). Wood 

flour (Lignocel C120, particle size of 100–120 mesh per 2.54 cm 2 ) was supplied 

by J. Retenmaier & Sohne Co. (Rosenberg, Germany) and manufactured 

from European softwood. Talc powder supplied from Seobu Enterprise 

Co. (Goyang-City, Republic of Korea) has a chemical structure of 

Mg 3 Si 4 O 10 (OH) 2 and melting point of 900 10008C. Average particle size 

and density of talc were 2 mm and 2.5–2.8 g/cm 3 , respectively. Organo-silane 

(S-6020, H 2 N(CH 2 ) 2 NH 2 (CH 2 ) 3 Si(OCH 3 ) 3 ) was purchased from the Dow 

Corning Co. (Midland, Michigan, U.S.A.). The molecular weight and a 

density of the silane at 258C are 222 g/mol and 1.03 g/cm 3 , respectively. 

Melt Compounding 

A 19 mm co-rotating twin-screw extruder with 40 L/D ratio (Bautek Co., 

Uijungbu-City, Korea) a pelletizer (Bautek Co., Uijungbu-city, Korea) was 

used to compound the blends. Table 1 shows blend formulations of the 

composites used in this study. Silane was simply integral-blended with 

other components without any additional treatment. The compounding 

temperature was 1808C with screw speeds in the range of 100–150 rpm. The 

extrudated strands were air-cooled and pelletized with a pelletizer 

(Uijungbu-city, Bautek Co., Korea). The hybrid pellets were dried at 908C 




Table 1. Material formulations of the hybrids. 

PLA (wt%) WF (wt%) Talc (wt%) Silane (wt%) 

100 0 – – 

90 10 – – 

80 20 – – 

70 30 – – 

60 40 – – 

80 10 10 – 

70 20 10 – 

60 30 10 – 

50 40 10 – 

79 and 77 10 10 1 and 3 

69 and 67 20 10 1 and 3 

59 and 57 30 10 1 and 3 

49 and 47 40 10 1 and 3 

for 24 h in a vacuum oven to remove the absorbed moisture and cooled to 

room temperature, and then injection-molded at 1908C to form test samples. 

Thermal Analysis 

The thermal decomposition behavior of the composites was measured 

with a SDT Q600 Thermogravimetric analyzer (TA Instrument Inc., USA). 

Tests were done under nitrogen at a heating rate of 108C/min over a 

temperature range of 30–6008C. A sample of 5–10 mg was used for each run. 

The weight change was recorded as a function of heating temperature. 

Differential peak temperature (DT p ) was defined as the temperature of the 

maximum derivative of the weight change over time. DSC experiments were 

performed in a Q10 differential scanning calorimeter (TA Instrument Inc., 

USA). Each sample was heated and cooled at a heating rate of 108C/min 

under nitrogen atmosphere. Each test sample of 5–10 mg was placed in an 

aluminum pan and heated from 30 to 2008C and then cooled down to 308C 

after keeping at 2008C for 3 min. The glass transition temperature (T g ), 

melting temperature (T m ), melting enthalpy (H m ), and crystallinity (X c ) 

were determined from the first heating scan, while the crystallization 

temperature (T c ) and crystallization enthalpy (H c ) were obtained from the 

first cooling scan. T m is defined as the maximum of the endothermic melting 

peak and T g as the deflection of the baseline temperature from the first 

heating scan. The X c was obtained by the following expression: 

X c ð%Þ ¼ 

H m 

H mðcrysÞ 

100 

ð1Þ 




where H m is the enthalpy of the sample and H m(crys) is the enthalpy of 

100% crystalline PLA taken as 93.7 J/g [5]. The H m , H c , and X c were 

converted by the mass fraction of the pure PLA in the composites. 

Mechanical Properties 

The tensile test for the composites was performed according to ASTM 

D638 using a Zwick an Universal Testing Machine (Zwick Testing Machine 

Ltd., Leomister, United Kingdom). Test specimens were molded to a size of 

3.18 mm (width) 9.53 mm (length) 3.00 mm (thickness) with a gauge 

length of 12.5 mm. For each treatment level, five replicates were tested and 

the results were presented as the average of the tested samples. Tensile 

deformation was determined using an extensometer at a crosshead speed of 

10 mm/min. 

Morphological Properties 

Morphology of the fractured composites after tensile testing was observed 

using a scanning electron microscope (SEM) (JEOL-6700F) with a field 

emission gun and an accelerating voltage of 5 kV. A gold layer of a few 

nanometers in thickness was coated onto the fracture surfaces. The samples 

were scanned perpendicular to the fractured surface. SEM micrographs were 

taken at the magnification level of 200. 

RESULTS AND DISCUSSION 

Thermal Properties 

TGA DATA 

TGA results of PLA, WF, and their composites are shown in Figure 1(a). 

As the WF content increased, the decomposition temperature of the PLA/WF 

composites decreased slightly. This may be due to the decomposition of wood 

components in a temperature range between 200 and 3808C. Cellulose and 

hemicellulose components of WF are two major contributors to the 

decomposition between 2008C and 3808C, whereas lignin is responsible for 

the char formation over 3808C [29]. The lower decomposition temperatures of 

PLA/WF composites indicated that the composites were less thermally stable 

than the neat PLA matrix. Poor interfacial adhesion between the PLA matrix 

and WF due to incompatibility of hydrophobic PLA with hydrophilic WF 

might contribute to this behavior. Tar and ash content after thermal 

degradation over 3808C increased with an increase in the WF loading level. 

The differential peak temperatures (DT p ), as a function of WF loading for 

various systems are shown in Figure 1(b). The DT p of neat PLA was 




(a) 

100 

80 

Weight change (%) 

60 

40 

PLA 

PLA90/WF10 

20 

PLA80/WF20 

PLA70/WF30 

PLA60/WF40 

WF 

0 

200 300 400 500 600 

(b) 

DT p (˚C) 

370 

350 

330 

Temperature (°C) 

PLA/WF 

PLA/WF/Talc10% 

PLA/WF/Talc10%/Silane1% 


310 

0 10 20 30 40 

Wood flour (%) 

Figure 1. Thermogravimetric properties of the composites: (a) TGA thermograms of 

PLA/wood flour composites; and (b) Differential peak temperature of PLA/wood flour/talc/ 

silane composites. 

358.28C, and the DT p of the PLA/WF composites ranged from 8 to 248C 

lower than that of neat PLA. The addition of talc to PLA/WF composites 

showed no significant effect on the thermal decomposition process. The 

loading of talc at 10 wt% level caused a slight shift of TGA curves. The DT p 

values of composites with talc ranged from 0 to 7.58C lower than those of 

composites without talc. For example, the DT p values of PLA80/WF20 




composite and PLA70/WF20/talc10 composite were 348.0 and 340.58C, 

respectively. The thermal decomposition temperatures of PLA/WF/talc 

composites with 1 wt% silane were higher, compared to those of the 

composites with 3 wt% silane. 

At higher levels of WF, the DT p values of the composites with 1 wt% 

silane were 2–48C higher than those with 3 wt% silane. The incorporation of 

silane to PLA/WF/talc decreased the DT p by 27–398C compared to that of 

neat PLA. 

3.1.2. DSC DATA 

The glass transition temperature, T g as function of WF loading for 

various systems are shown in Figure 2(a). The T g of neat PLA was 63.48C. 

As the WF loading increased, double peaks were observed in DSC 

thermograms, and the T g decreased slightly (Figure 2(a)). For example, 

the T g of the composite with WF (40 wt%) to PLA (60 wt%) decreased 

about 2.58C from that of pure PLA. The use of talc (10 wt%) in PLA50%/ 

WF40% composites largely lowered the T g of the hybrids (4.08C), compared 

to that of PLA60%/WF40% hybrid. At the WF loading of 10, 20, and 

30 wt%, the addition of 1 wt% silane to the PLA/WF/talc combinations led 

to higher T g values than those of the combinations with 3 wt% silane. 

Similar to DT p data, higher T g of the composites with 1 wt% silane could be 

ascribed to an improved interfacial adhesion between two materials (i.e., 

polymer matrix and fillers). This result also indicated that the T g depends on 

molecular characteristics, composition, and compatibility of the components 

in the amorphous matrix [19]. The melting temperature, T m , as a function 

of WF loading is shown in Figure 2(b). The T m of the PLA was 164.58C. 

The loading of WF (10–40 wt%) to the PLA decreased the T m by 1.5–1.78C. 

A decrease in the melting temperature might be due to the presence of voids 

in the composites. 

The enthalpy H m of the PLA was 41.7 J/g (Figure 3(a)). The H m 

values for composites with increased WF loading from 10 to 40 wt% 

significantly decreased (as low as 11.4 J/g), indicating that less energy was 

required to melt the composites (Figure 3(a)). This phenomenon implies that 

thermal degradation of the polymer became easier upon the hybridization 

with WF. The addition of talc (10 wt%) and silane (1 and 3 wt%) to 

PLA/WF composites showed no significant effect on the T m and H m of 

composites. This result suggested that the addition of talc had resulted in 

tertiary interfaces in the composites and the added silane acted as a 

dispersing agent in the interfaces. 

Figure 3(b) shows the T c , representing an exothermic peak due to 

the crystallization of the polymer matrix. The T c of neat PLA was 113.18C, 

and the incorporation of WF to the neat PLA slightly decreased the T c by 




(a) 

Glass transition temp. (T g , °C) 

70 

65 

60 

55 

PLA/WF 




50 

0 10 20 30 40 


(b) 

170 

Melting temp. (˚C) 

168 

166 

164 

162 

160 

158 

156 

154 

152 

PLA/WF 




150 

0 10 20 30 40 


Figure 2. Differential scanning calorimetric properties of the composites (I): (a) Glass 

transition temperature of PLA/wood flour/talc/silane composites; and (b) Melting temperature 

of PLA/wood flour/talc/silane composites. 

about 2.0–4.28C for the resultant composites. However, the loading 

of 10 wt% talc to the PLA/WF composites had no significant effect on 

the T c . The addition of silane (1 and 3 wt%) to the PLA/WF/talc composites 

gave slightly lower T c values than those of other composites without silane. 




(a) 

50 

Melting enthalpy ( H m , J/g) 

40 

30 

20 

10 

PLA/WF 




0 

0 10 20 30 40 

Wood flour(%) 

(b) 

120 

Crystallization temp. (T c , °C) 

118 

116 

114 

112 

110 

108 

106 

104 

PLA/WF 




102 

100 

0 10 20 30 40 


Figure 3. Differential scanning calorimetric properties of the composites (II): (a) Melting 

enthalpy of PLA/wood flour/talc/silane composites; and (b) Crystallization temperature of 

PLA/wood flour/talc/silane composites. 

This result could be due to the presence of either WF or talc in the 

polymer matrix, which interfered the crystallization process of the PLA. 

The loading of 1 wt% silane to the PLA/WF/talc composites resulted 

in a similar or higher T c values than those of 3 wt% silane (Figure 3(b)). 




This result could be due to an improved interfacial adhesion between the 

polymer matrix and fillers. 

Neat PLA had the highest H c (34.1 J/g) and X c (44.5%) values 

compared to PLA/WF composites. The H c decreased as the loading 

level of WF increased (Figure 4(a)). Obviously, this result could be 

attributed to the amount of PLA in the composites as the WF content 

increased. The application of 10 wt% talc to PLA/WF composites further 

decreased the H c . The large decrease in the X c of the composites with the 

addition of WF, talc and silane was observed in Figure 4(b). This may be 

caused by the partial inhibition effect of WF, talc and silane on polymer 

crystal formation. 

Mechanical Properties 

The tensile modulus of neat PLA was 1,346 MPa (Figure 5(a)). As WF 

levels increased, the tensile modulus was enhanced. With the WF loading 

levels increased from 10 to 40 wt%, the tensile modulus increased from 62.5 to 

169.5%. The tensile strength of neat PLA was 63 MPa (Figure 5(b)). For 

PLA/WF composites, the tensile strength increased 13.7, and 16.7, and 13.9% 

at the loading levels of 10, 20, and 30 wt% WF, respectively. At 40 wt% WF 

loading, PLA/WF composite had a similar tensile strength as the neat PLA. 

As shown in Figure 5(a), the addition of talc (10 wt%) to PLA/WF 

composites improved the tensile modulus by about 18.3 to 50.2%. 

In addition, the use of 1 and 3 wt% silane led to the higher tensile modulus 

of composites, compared to neat PLA and PLA/WF composites without 

silane treatment. As shown in Figure 5(b), the addition of talc (10 wt%) to 

PLA/WF composites resulted in a slightly lower tensile strength than neat 

PLA. At 10 wt% talc loading, the tensile strength slightly decreased as the 

WF level increased. The PLA50%/WF40%/talc10% composite showed an 

8.6% lower tensile strength than the PLA80%/WF10%/talc10% composite. 

In addition, PLA50%/WF40%/talc10% composite had a 10.7% lower 

tensile strength than neat PLA. The addition of 1 wt% silane to PLA/WF/ 

talc composites improved the tensile strength considerably, which indicates 

that silane facilitates the chemical bonding between WF and PLA, and 

between inorganic filler and PLA. The tensile strength of PLA/WF/talc 

composites with 1 wt% silane was significantly greater than that of PLA/ 

WF/talc composites with 3 wt% silane. As discussed earlier, the addition of 

1 wt% silane was more effective to improve interfacial adhesion than the 

addition of 3 wt% silane. An improved interfacial adhesion could be 

explained by a mechanism shown in the following three steps; 

1st step: the formation of silanol (Si-OH) by hydrolysis, or R-Si- 

(OH) 3 þ MeOH. 




(a) 

Crystallization enthalpy (∆H c , J/g) 

40 

35 

30 

25 

20 

15 

10 

5 

PLA/WF 




0 

0 10 20 30 40 


(b) 

50 

Crystallinity (%) 

45 

40 

35 

30 

25 

20 

15 

10 

5 

PLA/WF 




0 

0 10 20 30 40 


Figure 4. Differential scanning calorimetric properties of the composites (III): (a) crystalline 

enthalpy of PLA/wood flour/talc/silane composites; and (b) crystallinity of PLA/wood flour/ 

talc/silane composites. 

2nd step: the reaction of silanol with OH-groups on the surface of talc, or 

R-Si-O-talc þ H 2 O 

3rd step: R-Si-O-talc þ PLA, then finally PLA-Si-O-talc þ WF þ R-Si- 

(OH) 3 þ H 2 O can be formed. 




(a) 

Tensile modulus (MPa) 

2200 

1900 

1600 

1300 

PLA/WF 




1000 

0 10 20 30 40 


(b) 

90 

80 

70 

Tensile strength (MPa) 

60 

50 

40 

30 

PLA/WF 

20 



10 


0 

0 10 20 30 40 


Figure 5. Tensile properties of the composites: (a) tensile modulus; and (b) tensile strength. 

From the 3rd step, the main chemical component is PLA-Si-O-talc. 

In terms of tensile strength, remaining R-Si-(OH) 3 and R-Si-(OMe) 3 have 

an interaction with PLA and WF, interfering the bonding potential of PLA- 

Si-O-talc. Therefore, the tensile strength at 3 wt% silane was significantly 

lower than that at 1 wt% silane level. 




(a) 

(b) 

(c) 

(d) 

Figure 6. SEM images of the composites: (a) PLA60%/WF40%; (b) PLA80%/WF20%; 

(c) PP60%/WF30%/Talc10%; (d) PLA59%/WF30%/Talc10%/silane1% composites. 

Morphological Properties 

The SEM photomicrographs of the composites with PLA (80% and 

60 wt%), WF (20 and 40 wt%), talc(10 wt%), and silane(1 wt%) prepared by 

the compounding are shown in Figure 6. The compounding method led to a 

uniform distribution of WF in the PLA matrix. The system without silane 

treatment showed a poor compatibility between the PLA matrix and WF. 

The surface of WF particle was believed to be delaminated from the PLA 

matrix, and micro-size voids were formed during tensile testing. The use of 

silane treatment significantly improved the compatibility, leading to less 

filler-matrix debonding. 

CONCLUSIONS 

This work examined the effects of WF, talc, and silane on thermal 

and mechanical properties of PLA/WF/talc composites. The thermal 

decomposition temperature of the PLA/WF composites decreased as the 




content of WF increased. The DT p of hybrids with talc was 5–88C lower than 

that of hybrids without talc. The loading of 1 wt% silane to PLA/WF/talc 

composites led to a higher thermal decomposition temperature than that of 

3 wt% silane. As WF loading into the PLA increased, the T g of the 

composites. The addition of talc to PLA/WF hybrids also lowered the T g . The 

addition of WF/talc to neat PLA decreased the T c slightly. The addition of 

1 wt% silane to PLA/WF/talc showed a similar or higher T c compared to that 

of 3 wt% silane. The application of WF, talc, and silane to PLA decreased the 

X c of composites. The tensile modulus of PLA/WF composites was similar or 

lower than that of neat PLA. The loading of talc and 1 wt% silane to 

PLA/WF composites improved the tensile modulus. The tensile strength of 

the composites decreased slightly with the addition of talc (compared to neat 

PLA strength), but it was considerably improved with the use of 1 wt% silane. 

ACKNOWLEDGMENTS 

The authors would like to especially thank Jin-Seong Kim of the Korea 

University and thank Dr Jong-Bae Lee of the Korea Research Institute of 

Chemical Technology for their help with DSC and SEM analysis. 

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