Heat treatment appears to induce a slight increase in ethanol extractives from 1.3% to 2.0%, a trend observed in other wood species such as heat-treated Paulownia [
22],
Eucalyptus globulus [
23], and
Pinus pinaster [
24]. This increase in ethanol extractives is likely due to the thermal degradation of hemicelluloses and the subsequent formation of low-molecular-weight compounds, which are more soluble in ethanol. However, this trend is not universal. For instance, in thermally modified tropical hardwoods like Afrormosia (
Pericopsis elata) and Duka (
Tapirira guianensis), no significant increase in ethanol extractives was observed. This discrepancy may be attributed to the already higher ethanol extractives content in the untreated wood of these species, which reduces the potential for further increase during heat treatment since several of the original compounds are degraded [
25]. The changes in extractive content during heat treatment play a critical role in determining the wood's physical and chemical properties, including its resistance to decay, dimensional stability, and overall durability. Understanding these variations helps optimize heat treatment processes for specific wood species and applications.
A slight reduction in dichloromethane extractives and no change in water extractives were also observed. Nevertheless, it is expected that the composition of heat-treated wood extractives differs from untreated wood.
Physical and Mechanical Properties
The main objective of heat-treatment is to improve the dimensional stability of wood.
Figure 2 compares dimensional changes (radial, tangential, and axial) over multiple cycles (three cycles) for untreated and heat-treated wood.
In the tangential direction, untreated wood experiences significant swelling, with values like 8.48%, 7.65%, and 7.16% in cycles 1, 2, and 3. This highlights the natural tendency of untreated wood to expand tangentially due to moisture. Heat-treated wood, however, has much lower tangential changes, with values like 5.38%, 5.37%, and 5.42%, indicating reduced swelling and improved stability. No significant differences were observed between cycles for both untreated and heat-treated wood showing that the improvements still remain after three wet and dry cycles.
For the radial direction, untreated wood has also higher swellings with values such as 3.73%, 3.72%, and 3.98% in cycles 1, 2, and 3, indicating instability. In contrast, heat-treated wood has lower values, such as 2.67%, 2.78%, and 3.26%, with smaller swellings, showing greater stability.
In the axial direction, untreated wood shows moderate instability, with values fluctuating between 2.57% and 1.76%. Heat-treated wood, on the other hand, has lower axial changes, such as 1.30%, 1.28%, and 0.66%, showing some improvement in stability. Overall, untreated wood exhibits larger dimensional changes, especially in the tangential direction, where it is most affected by moisture. The lower values and reduced fluctuations confirm that heat treatment reduces moisture absorption and minimizes swelling and shrinking, particularly in the tangential direction.
In order to best evaluate the improvements in dimensional stability, the ASE was determined to show how well the treatment reduces dimensional changes (radial, tangential, and axial) over different cycles,
Figure 3.
In the radial direction, ASE starts at 28.53% in the first cycle and slightly decreases to 25.23% in the second cycle. By the third cycle, it drops further to 18.15%, indicating a gradual decline in the treatment's effectiveness in reducing radial swelling over time. Similarly, for the tangential direction, ASE begins at 36.51% in the first cycle, decreases to 29.90% in the second cycle, and drops further to 24.34% in the third cycle. In the axial direction, ASE ranged from 49.42% to 43.37% but it has to be taken into account that in this direction the swelling is minimal. Even though there is a reduction on ASE along the wet and dry cycles heat-treated wood still performs significantly better than untreated wood. Yang et al [
30] determined the ASE for heat-treated Cryptomeria wood at temperatures ranging from 170 to 210 °C but without using a shielding gas. ASE ranged from 20% to 54%. The higher ASE observed for 210 °C during 4h (54%) is obtained with 18% mass loss which is much higher than the commonly accepted 3% for heat-treatments due to the higher degradation of wood. Heat treatment of Rubberwood and Silver Oak was studied by Srinivas and Pandey[
31] that reported a volumetric ASE of 20% and 12% for wood treated at 210 °C for 4h. To compare with the results presented here the volumetric ASE was determined for the first cycle to be 34%, which is significantly better than the reported before.
The water absorption data for untreated and heat-treated Cryptomeria japonica wood across three cycles is presented on
Table 2. Results show that there is a significant difference in the behavior of untreated and heat-treated wood in response to moisture exposure. These results highlight the impact of heat treatment on the wood's ability to absorb water, an important factor in its dimensional stability and durability.
In the first cycle, untreated wood exhibited an average water absorption of 160%. This significant variability indicates that untreated wood is highly susceptible to water uptake, likely due to its porous structure and hydrophilic nature. In contrast, heat-treated wood absorbed only 130%. This reduction in water absorption can be attributed to the heat treatment process, which typically causes the wood’s cell wall structure to undergo chemical and physical changes. In the second cycle, untreated wood showed a similar water absorption of 160%. Heat-treated wood's absorption decreased further to 113%, highlighting the lasting benefits of heat treatment in water absorption. In the last cycle heat-treated wood absorbed 125% maintaining its water absorption in the same levels.
The results from the three cycles demonstrate the significant impact of heat treatment on the water absorption behavior of
Cryptomeria japonica wood. These findings align with previous research, which has demonstrated that heat treatment reduces the water absorption of wood. Results presented before for fast growing hardwoods showed that heat treatment decreased water absorption in jabon, sengon, and mangium wood samples. The control samples of jabon, sengon, and mangium had average water absorption rates of 43%, 40%, and 15%, respectively. Following heat treatment, water absorption decreased by 34% in jabon, 30% in sengon, and 49% in mangium [
32]. The same happened for radiata pine, a known softwood [
33]. Nevertheless, results presented before show that heat treatment not always decreases water absorption. For example heat treatment affected differently the water absorption of Scots pine and Norway spruce [
34]. Pine sapwood absorbed water more quickly than heartwood, and heat treatment increased water absorption in pine sapwood. However, heat treatment reduced water absorption in pine heartwood and spruce, with the reduction being proportional to the treatment temperature.
Wood density can vary significantly depending on the geographic location, climate, and species. Trees grown in regions with favorable conditions, such as consistent rainfall and moderate temperatures, often exhibit higher wood density due to slower, more uniform growth. In contrast, wood from harsher environments, such as arid or cold regions, may have lower density as a result of faster or irregular growth patterns. This variation in density directly influences the mechanical properties of wood, such as strength, stiffness, and durability. Higher-density wood typically possesses greater mechanical strength and resistance to stress, making it more suitable for structural applications, while lower-density wood may be lighter but less robust, limiting its use in load-bearing scenarios. Untreated cryptomeria wood used in the tests presented a oven-dry density around 0.27 g/cm
3 which is slightly smaller than the 0.33 g/cm
3 presented by logs obtained from Ibaraki Prefecture in Japan [
35]. Density increased for heat treated wood from 0.27 g/cm
3 to 0.33g/cm
3 and, even though it was a small increase it might have protected wood from a higher decrease on mechanical properties.
Mechanical strength is known to decrease due to heat-treatment, specially bending strength [
36,
37]. The MOE is often observed to increase at the beginning of treatment, followed by a decrease in more severe treatments.
Table 3 shows the mechanical properties of untreated and treated wood, where the bending strength dropped from 52.6 MPa to 42.3 MPa, representing a 19.6% reduction compared to untreated wood, while the MOE increased from 7268 MPa to 10836 MPa. MOE is known to increase and then decrease for higher intensity treatments and tests made with cryptomeria wood treated at 210 °C for 2h without shielding gas lead to a 26% decrease on MOE and a 42% decrease on bending strength [
30]. The greater degradation of wood's mechanical properties observed by these authors could hinder the use of treated wood in various applications.
The main changes observed on the surface of heat-treated wood were the color that became darker as can be seen by the L* decrease from 67.5 to 46.6 in heat-treated wood. There has been a significant decrease in a* and b* corresponding to the reddening and yellowing of the samples,
Table 4. The changes in color due to heat-treatment have been reported to be dependent on the initial wood color. For instance, a* increased for black locust, linden and willow, but decreased for wild pear and alder while a decrease in b* followed by an increase was reported for black locust and linden, while for wild pear and alder a decrease with the intensity of the treatment was observed and in the case of willow, there was an initial increase in b* followed by a decrease [
38]. ΔL was 20.9 similar to the reported before for wood treated at 210ºC and 2h but without shielding gas [
30].