Wood Sci Technol (2011) 45:399404 DOI 10.

1007/s00226-010-0343-5 ORIGINAL

Study on the effect of nano-silver impregnation on mechanical properties of heat-treated Populus nigra
Hamid Reza Taghiyari

Received: 4 August 2009 / Published online: 22 May 2010 Springer-Verlag 2010

Abstract The present study is aimed at investigating the effect of heat treatment of nano-silver-impregnated Populus nigra on weight loss, modulus of rupture (MOR), modulus of elasticity (MOE), and compression parallel to grain. Specimens were impregnated with 200 PPM water-based solution of nano-silver particles at 2.5 bar in a pressure vessel. For heat treatment, both nano-silver-impregnated and simple specimens were kept for 24 h at 45C and then further for 24 h at 145C and nally for 4 h at 185C. MOR decreased from 529 to 461 kg/cm2 in heat-treated specimens; MOE and compression parallel to grain were though improved. Also, comparison between heat-treated and nano-silver-impregnated heat-treated specimens showed that there was a decrease in MOR and MOE in nano-silver-impregnated heat-treated specimens. This shows that nano-silver impregnation facilitates transfer of heat in wood and it may increase the process of degradation and pyrolysis of wood structures in deeper parts of specimens.

Introduction Of all the various wood modication processes that have been studied, thermal modication is by far the most commercially advanced one. Thermal modication of wood has long been recognized as a potentially useful method to improve the dimensional stabilization of wood and to increase its decay resistance (Hill 2006). Tiemann (1915) was one of the rst workers to report on the effect of hightemperature treatment upon the physical properties of wood. He heated air-dry wood in superheated steam at 150C for 4 h, which reduced the subsequent moisture sorption by 1025%, with relatively low reductions in strength found in most cases.
H. R. Taghiyari (&) Wood Industries Department, Faculty of Civil Engineering, Shahid Rajaee Teacher Training University, Tehran, Iran e-mail: htaghiyari@srttu.edu

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At around 270C, there is a signicant change in the reaction kinetics due to the onset of an exothermic reaction. Less certain are the exact points at which the different reactions become dominant (Stamm et al. 1946). Thermal modication is invariably performed at temperatures between 180 and 260C; temperatures lower than 140C resulting in only slight changes in material properties and higher temperatures resulting in unacceptable degradation of the substrate. Studies of the thermal treatment of wood above 300C are of limited value due to severe degradation of the material. There is also evidence to show that there is an abrupt change in the degradation kinetics close to this temperature (Elder 1991). Modern thermal modication processes are limited to temperatures no higher than 260C. Temperature ranges from 150 to 230C are generally used, because hydrolysis is very slow at lower temperatures, whereas cellulose degradation begins to occur in the region of 210220C. Cellulose degradation becomes predominant at 270C. A sharp increase in the free-radical content of the wood was also found when the wood was heated at temperatures above 200C (Garrote et al. 1999). Upon review of the above-mentioned literature and taking into account the fact that nano-silver particles have the potential of increasing heat transfer from the surface of wood, as a non-heat-conductive material, to its deeper parts, it was decided not to increase the temperature above 185C.

Materials and methods Specimen procurement Three poplar (Populus nigra) trees were cut and harvested from Shahid Rajaee University Campus. From each tree, 60 specimens were cut for MOR and MOE tests and 60 for compression parallel to grain. Specimens were free from any checks, knots, rots, and blue stains. They were separated randomly into three groups; control samples, heat-treatment specimens, and nano-silver-impregnated specimens. All compression parallel to grain specimens were weighed by a digital scale having 0.0001 gr. precision before any further steps were taken to measure weight loss. Nano-silver impregnation Specimens for nano-silver impregnation were rst impregnated with 200 PPM water-based solution of nano-silver particles at 2.5 bar in a pressure vessel. Nanosilver solution was purchased from Nano-Pooshesh Felez Company (Iranian registration No. 12695). Rueping (empty cell) process was used. After impregnation process, some control samples, which were put in the pressure vessel, were cut, and it was observed that nano-silver solution had penetrated to the deepest part of the specimens. Before heat treatment, nano-silver-impregnated specimens were kept for 1.5 months in room conditions (30C and 4550% relative humidity) so that they lose their free water and much of their bound water.

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Heat treatment Both nano-silver-impregnated specimens along with heat-treatment specimens were then arranged randomly in an oven for the heat-treatment process. In order to make sure that both nano-silver-impregnated and heat-treatment specimens had the same moisture content, they were rst kept at 45C for 24 h. Then, temperature was increased to 145C for 24 h. After that, temperature was increased to 185C. Once it had reached 185C, the temperature was kept constant for 4 h. The oven was then turned off and left alone until next day without opening the door of the oven. Specimens were taken out of the oven and kept in room conditions (30C and 4550% RH) for 2 weeks. All compression parallel to grain specimens were again weighed to measure the amount of weight loss. Mechanical tests All mechanical tests were done in accordance with terms and conditions of ASTM D 143-94 (Reapproved 2000). Statistical analysis Statistical analysis was conducted using SAS software program, version 9.1. Twoway analysis of variance (ANOVA) was performed to conclude signicant difference at 99% condence level.

Results Weight loss Results show a slightly extra decrease in weight in nano-silver-impregnated heattreated specimens although not signicantly different from heat-treated specimens. Weight loss in heat-treated specimens was about 4.98%, while in nano-silverimpregnated heat-treated specimens it was 5.11% (Fig. 1). Modulus of rupture (MOR) Modulus of rupture (MOR) in control samples was 529.4 kg/cm2, while in heattreated ones it was 460.7 kg/cm2. MOR values in nano-silver-impregnated heattreated specimens were the lowest and measured to be 406.8 kg/cm2 (Fig. 2). Modulus of elasticity (MOE) Results show that modulus of elasticity is more in heat-treated specimens (75587.4 kg/cm2) in comparison with control samples (73375.3 kg/cm2). MOE

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Weigth Loss Based on the Initial Weight (%)

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8 7 6 5 4 3 2 1 0

Weight Loss (%)

% weight Loss (HeatTreated)

% weight Loss (Nano-silver Impregnated HeatTreated)

Fig. 1 Weight loss in heat-treated and nano-silver-impregnated heat-treated specimens (%)

Modulus of Rupture (MOR)

700 600 500 400 300 200 100 0 Control Heat-Treated Nano-silver Impregnated Heat-Treated

Fig. 2 Modulus of rupture (MOR) values in control, heat-treated, and nano-silver-impregnated heattreated specimens (kg/cm2)

Kg/Sq.cm

100000 90000 80000 70000 60000 50000 40000 30000 20000

Modulus of Elasticity (MOE)

Kg/Sq.cm

Control

Heat-Treated

Nano-silver Impregnated Heat-Treated

Fig. 3 Modulus of elasticity values for control, heat-treated, and nano-silver-impregnated heat-treated specimens (mega Pascal)

values in nano-silver-impregnated heat-treated specimens (73737.9 kg/cm2) are less than those in heat-treated specimens, although slightly more than those in control samples (Fig. 3).

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Compression Parallel to Grain

700 600

Kg/Sq.cm

500 400 300 200 100 0

Control

Heat-Treated

Nano-silver Impregnated Heat-Treated

Fig. 4 Compression parallel to grain values for control, heat-treated, and nano-silver-impregnated heattreated specimens (kg/cm2)

Compression parallel to the grain Heat-treated specimens have higher compression parallel to grain values than control samples (580.6 kg/cm2 in comparison to 489.8). Although not signicantly different, values of nano-silver-impregnated heat-treated specimens were slightly higher than the values of heat-treated specimens (588.8 kg/cm2) (Fig. 4). Appearance and color change of the specimens After 24 h at 145C, no obvious color change was observed for the heat-treatment specimens; but a slight color change (light brownish yellow) was observed for the nano-silver-impregnated specimens. Color change was more obvious at both crossends of the specimens. After 4 h at 185C, one side of some of the specimens near the top right corner of the oven turned to coal so that mechanical tests could not be done on them. This showed that only in this part of the oven chamber (top right corner), accumulation of heat occurred. These specimens were omitted from further measurement to prevent any errors.

Discussion and conclusion Considering the amount of weight loss, it may be concluded that degradation and pyrolysis occur to the same extent in heat-treated and nano-silver-impregnated heattreated specimens. It may be true from the point of view of the amount of material decreased in the specimens, but from the viewpoint of the location of the material lost, other factors should also be taken into account, such as MOR. Considering MOR values, an obvious decrease can be seen; this decrease can imply that the processes of degradation and pyrolysis were not supercial and have penetrated to the inner parts of the material. That is, in heat-treated specimens, heat was accumulated on the surface layer of the specimens because wood is a non-heat-

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conductive material, while in nano-silver-impregnated specimens, heat could penetrate to the inner parts as to the heat-conductive properties of nano-silver particles. Although the same amount of heat was exposed to both kinds of specimens (heat-treated and nano-silver-impregnated heat-treated specimens) as to the fact that the area of both were the same, the process of penetration of heat was improved in nano-silver-impregnated specimens. The transfer of heat in heat-treated specimens to the inner parts could be done mainly by convection and airdisplacement through vessels and pits of wood as a non-heat-conductive porous material, while in nano-silver-impregnated heat-treated specimens, it could be transferred more rapidly through nano-silver particles that covered all surface area of cell wall, vessels, and pits. Many studies have shown that there is a slight increase in MOE and compression parallel to grain when wood is thermally treated for short time periods. A reduction in MOE then occurs (Hill 2006). Considering Figs. 3 and 4, the increase in MOE and compression parallel to grain values of heat-treated specimens can clearly be seen. Still, the decrease in nano-silver-impregnated heat-treated specimens for MOE values may imply that nano-silver impregnation of wood has accelerated the process of heat transfer and it can be considered as an increase in heating periods of wood. Therefore, further studies should be done at lower temperature, as low as about 140C, to observe and analyze whether maximum MOE increase can be achieved at these temperatures when wood is impregnated with nano-silver particles. The amount of weight loss can be considered equal in heat-treated and nanosilver-impregnated heat-treated specimens; still it was not studied whether their weight-loss gradients are the same. Easy transfer of heat in nano-silver-impregnated heat-treated specimens might have resulted in a more even density gradient in the specimen. Furthermore, as to the fact that nano-silver particles accelerate heat transfer in wood as a porous material, the amount of weight loss should also be studied at lower temperatures.
Acknowledgments The author is grateful to Dr. Mohammad Layeghi (associate professor at faculty of natural resources, The University of Tehran) for preparing nano-silver solution for the present study. Also, I would like to deeply thank Mr. Hossein Afshar, managing director of Afshar Wood-Machinery Manufacturing Co., for being instrumental in nano-silver impregnation treatment in pressure vessels.

References
Elder T (1991) The pyrolysis of wood. In: Hon DNS, Shiraishi N (eds) Wood and cellulosic chemistry. Marcel Dekker, New York, pp 66699 Garrote G, Dominguez H, Parajo JC (1999) Hydrothermal processing of lignocellulosic materials. Holz Roh- Werkst 57(3):191202 Hill C (2006) Wood modication chemical, thermal and other processes. John Wiley & Sons, Ltd., ISBN: 0-470-02172-1. p 239 Stamm AJ, Burr HK, Kline AA (1946) Staybwood. Heat stabilized wood. Ind Eng Chem Res 38(6):630 634 Tiemann HD (1915) The effect of different methods of drying on the strength of wood. Lumber World Rev 28(7):1920

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