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1
2 Properties of Wood Treatment Technology and Thermo-
3 Vacuum Process Treated Birch (Betula pendula Roth)
4 Veneers
5
6 Anete Meija-Feldmane,a Ignazia Cuccui,b Ilze Irbe,c Andris Morozovs,a and
7 Uldis Spulle a
8
9 Thermal modifications of birch (Betula pendula Roth) veneers by wood
10 treatment technology (WTT) and thermo vacuum (TV) processes were
11 compared in this study. After modification of veneers in the range of
12 temperatures from 160 °C to 218 °C and times from 0.5 h to 3 h, color,
13 mass loss, density, tensile strength, hygroscopicity, and decay resistance
14 against brown rot fungus Coniophora puteana were determined. Treatment
15 regimes with the greatest mass loss were at 217°C for 3.0 hours in
16 TV(7.8%) and 160°C for 0.8 hours in the WTT (6.7%). As expected, wood
17 mass loss correlated well with moisture exclusion efficiency (MEE) in all
18 relative humidity (RH) environments (r = 0.95 to 0.99). Strength loss in the
19 WTT was considerable compared to the TV process (57% and 40%,
20 respectively). The resistance against brown rot fungus was moderate with
21 a mass loss of 12% to 33%. Among the investigated samples, the regime
22 217/3.0/TV showed the best resistance against brown rot fungus and
23 acceptable other properties.
24
25 Keywords: Birch; Thermal modification; Wood treatment technology; Thermo vacuum treatment; Decay
26 resistance
27
28 Contact information: a: Latvia University of Life Sciences and Technologies (LULST/LLU), Liela Street 2,
29 Jelgava, LV-3001, Latvia; b: BioEconomy Institute CNR-IBE, via Biasi, 75 - 38010 San Michele all'Adige
30 –(TN), Italy; c: Latvian State Institute of Wood Chemistry, Dzerbenes Street 27, Riga, LV-1006, Latvia;
31 *Corresponding author: a.meija.feldmane@gmail.com
32
33
34 INTRODUCTION
35
36 With an increasing awareness of global climate change and greenhouse gas
37 emissions, among which CO2 is the crucial one, the interest in wood materials that can
38 accumulate and store carbon dioxide also increases. The longer the wood material can be
39 used, the longer it stores carbon, therefore several techniques to prolong the life span of
40 wood materials have been developed (Hildebrandt et al. 2017).
41 Plywood is an engineered cross-glued wood material made from peeled veneers.
42 World production of plywood reached 107.4 million m3 in 2017 (Raute 2017). The
43 properties of plywood are mainly determined by the characteristics of veneers such as wood
44 species and technological features (Gilbert et al. 2017). Veneer swells in a humid
45 environment and shrinks when it is drying, which can provoke internal stresses in plywood
46 and also its delamination. izlaists
47 Wood thermal treatment at temperatures of 160 °C to 240 °C is the most acceptable
48 industrial method for wood modification. The wood thermal modification increases the
49 dimensional stability of veneer by increasing its hydrophobicity. Chemical changes in
50 wood due to the thermal modification depend on the duration of treatment and temperature.
114 where m0 is the mass of oven-dry untreated wood samples (kg) and mm is the mass of
115 oven-dry modified wood samples (kg).
116
117 Density
118 Density was determined according to ISO 13062-2 (2014). Standard deviation and
119 coefficient of variation were calculated for the analysis of the results.
120
121 Color
122 A MicroFlash 200D portable spectrophotometer (DataColor, Lawrenceville, NJ,
123 USA) suitable for direct determination of CIE L*a*b* color coordinates according to
124 ISO/CIE 11664-4 (2008) was used for measurement over an 18 mm diameter spot with a
125 standard light source D65 and an observer angle of 10°. Color was also measured with a
126 Minolta CM-2500d spectrophotometer with D65 light source and d/8 measuring geometry
127 and 10° standard observer (Konica Minolta, Tokyo, Japan). Each of the 30 samples was
128 measured 3 times at the same spot before and after the heat treatment.
129 Total color change ΔE between treated and untreated samples was calculated according to
130 Eq. 2,
143 where EMCNT (%) is EMC of untreated reference samples and EMCHT (%) is EMC of
144 treated samples.
145 The MEE value expressed the relative variation of EMC of treated wood
146 equilibrated at RH 30%, 65%, and 80% (MEE = 0% indicated no EMC variation; MEE =
147 100% indicated an EMC value of 0%).
148
149 Tensile strength
150 Tensile strength of veneers parallel to the grain was determined according to GOST
151 20800-75 (1976). Twenty random samples with the dimensions of: width 20 mm; length
152 (grain direction) 200 mm; thickness 1.5 mm were cut from both treated and untreated
153 veneers. To prevent the samples from slipping out of the clamps, pieces of plywood with
154 the dimensions 20 mm × 50 mm × 4.5 mm were glued on both sides of the veneers and on
155 both ends of samples using one-component polyurethane glue. Afterwards, the samples
156 were conditioned at 20 ± 3 °C and 65 ± 5% relative humidity. A tensile strength test was
157 conducted with the INSTRON 5500 device (Instron, Norwood, MA, USA) with a constant
158 speed of approximately 1 mm per minute to obtain a rupture of samples in 60 ± 30 s.
159
160 Decay resistance
161 Decay resistance was determined according to European Prestandard ENV 12038
162 (2002) using brown rot fungus Coniophora puteana BAM Ebw 15. The fungus was
163 cultivated on a medium which contained 5% malt extract concentrate and 2% Fluka agar.
164 10 samples of each regime with the dimensions of 50 mm × 25 mm × 1.5 mm were
165 aseptically placed on 3 mm steel supports in Petri dishes on fungal mycelium and incubated
166 at 22 ± 2 °C and 70 ± 5% RH for 6 weeks. After cultivation, the samples were removed
167 from the culture vessels, brushed free of mycelium, and oven dried at 103 ± 2 °C.
168 Percentage weight loss (WL) of the samples was the measure for the extent of fungal
169 degradation.
170
171 Microscopy
172 Light microscopy (LM) was performed on 10 samples from thermally modified and
173 unmodified birch veneers with the dimensions of 20 mm × 20 mm ×1.5 mm. Before
174 microscopy, the samples were soaked for 24 h in distilled water to soften the wood structure
175 and make it sliceable. Wood sample cuts (15 µm to 30 µm) were obtained with a razor
176 blade. Microscopy was made with a Leica DMLB light microscope (Leica Microsystems,
177 Mannheim, Germany) at 400× magnifications. The images were taken with a Leica
178 DFC490 video camera, using Image-Pro Plus 6.3 software for picture analysis (Media
179 Cybernetics, Inc., Silver Spring, MD, USA).
180
181 Statistics
182 To determine a statistically significant difference among groups of data, one-factor
183 ANOVA with a confidence level of 0.05 was considered.
184 The CORREL function in MS EXCEL was used to estimate how two or more variables
10
9
8
7
6
Mass loss,%
5
4
3
2
1
0
207
208 Fig. 1. Mass loss after thermal modification of birch veneer samples (STDEV error bars)
209
210 According to Grinins (2016) concerning the mass loss for birch veneers,
211 160/0.8/WTT was 6.3%, which are the same than observed with treated veneers at 6.7%.
212 If the mass and dimensions of the sample increase, for example for birch planks, mass loss
213 at the same regime 160/0.8/WTT becomes considerably greater 16% (Biziks et al. (2016)
214 and it is important for plywood production if thicker veneers are used. According to
215 Chaouch et al. (2013), mass loss occurs mainly due to deacetylation of strongly acetylated
216 glucuronxylan which causes liberation of acetic acid, which then catalyzes
217 depolymerization of less-ordered carbohydrates.
50
40
30
20
10
0
Unmodified 160/0.8/WTT 204/2.0/TV 214/2.0/TV 217/3.0/TV 218/0.5/TV
birch
246
12
a, units 10
0
Unmodified birch
160/0.8/WTT 204/2.0/TV 214/2.0/TV 217/3.0/TV 218/0.5/TV
247
30
25
20
b, units
15
10
0
Unmodified 160/0.8/WTT 204/2.0/TV 214/2.0/TV 217/3.0/TV 218/0.5/TV
birch
248
249
250 Fig. 2. Color coordinates L*, a*, and b* of untreated and treated wood samples at different
251 process conditions (STDEV error bars)
252
253 The total color changes (ΔE) depending of the mass loss can be seen in Fig. 3.
254 Visually visible changes were considered if ΔE was greater than 3.5 units (Mokrzycki and
255 Tatol 2011). Hemicellulose was the component that was damaged most during heat
256 treatment. Consequently, the relative content of lignin in heat-treated wood increased
257 accordingly, which might explain darker colors (Lovrič et al. 2014). Brischke et al. (2007)
258 described that the sum of lightness parameter and yellow-blue axis parameter (L*+b*)
259 correlate with treatment regime for beech wood (R2=0.951). The total colour change in this
260 research correlated (r = 0.98) well with mass loss, and the most severe was the regime
261 217/3.0/TV, followed by 160/0.8/WTT. As it is observed, color changes did not follow the
262 temperature increased changes, also treatment duration and treatment method were
263 substantial. The results can be seen in Fig. 3.
264
50
217/3.0/TV
218/0.5/TV
40
204/2.0/TV
ΔE
30
214/2.0/TV
20
y = 2.6204x + 24.255
10 R² = 0.9556
0
0 2 4 6 8 10
Mass loss, %
265
266 Fig. 3. Total color change (ΔE) correlation with mass loss during thermal modification
267
268 Total color changes in VT and WTT process treated veneers are considerably larger
269 than observed by Barcik et al. (2015) – in the Termowood® process. For birch treated at
270 160°C ΔE was 1.16 and at 210°C it was 2.56. Using birch thermal modification under
271 saturated 160°C and superheated 185°C steam, Torniainen et al. (2011) showed that L*
272 decreased from 80.92 to 52.72 and 55.48 accordingly, which coincides with the findings in
273 this research.
274
275 Equilibrium Moisture Content (EMC) and Moisture Exclusion Efficiency
276 (MEE)
277
278 As shown in Fig. 4, the treated wood had a lower EMC compared to wood that was not
279 treated. The veneers treated at 204/2.0/TV was the most hygroscopic at all RH. The least
280 hygroscopic materials were 160/0.8/WTT and 217/3.0/TV. It is commonly known that
281 hydrothermally-treated wood becomes less hygroscopic (Mirzaei et al. 2017). Water
282 uptake of wood is reduced by the heat-treatment process (Hyttinen et al. 2010), since
283 hemicellulose and cellulose are the main wood components responsible for decay and
284 hygroscopicity of wood (Li et al. 2017). The moisture content of heat-treated wood was
285 about half compared to that of untreated wood. Because of the loss of hygroscopic
286 hemicellulose sugars and their conversion to less hygroscopic furan-based polymers,
287 predominantly furfural and hydroxymethylfurfural, during heat treatment, the equilibrium
288 moisture content was reduced to about half the value of untreated wood (Jämsä et al. 2000;
289 Sandberg et al. 2013), which coincided with the results in Fig. 4.
290
16
14
12
EMC, %
10
0
30% 65% 80%
302
303 Tensile strength
304 The results of tensile strength properties along fibers are reported in Fig. 5. The
305 data had considerably high standard deviations, but the mean values of tensile strength
306 were compared to the values for untreated birch, and there was no remarkable difference,
307 such as 117 MPa in this research compared to 125.5 MPa according to Grinins (2016),
308 although this was over 20% higher than 75 MPa as shown in literature (Volynsky 2009).
309
120
100
τ, MPa
80
60
40
20
0
Untreated birch 204/2.0/TV 217/3.0/TV
160/0.8/WTT 214/2.0/TV 218/0.5/TV
310
311 Fig. 5. Tensile strength along fibers of untreated and treated birch veneer samples (STDEV error
312 bars)
313
314 The state of the wood cell wall directly affected the veneers` strength properties. As a result
315 of the degradation of hemicelluloses, the wood becomes brittle and rigid, which indicates
316 the important role that hemicelluloses have in imparting viscoelastic properties to wood
317 (Hill 2006). After the thermal modification of birch veneers in the TV process, the tensile
318 strength along the fibers decreased from 117 MPa to approximately 76 MPa apart from
319 treatment regime. In the WTT process, the tensile strength decreased to approximately 51
320 MPa. Strength loss in the WTT process was considerably greater than in the TV process.
321 The tensile strength fairly correlated with mass loss (r = 0.57), and for the TV-treated
322 samples it was notable (r = 0.86). As shown in Fig. 6, the WTT-treated veneers differed
323 from the TV-treated veneers.
324
120
218/0.5/TV
100
214/2.0/TV
80
204/2.0/TV
τ, MPa
60 217/3.0/TV
40 160/0.8/WTT
20
0
0 2 4 6 8 10
Mass loss, %
325
326 Fig. 6. Mass loss correlation with the tensile strength of treated birch veneer samples
327 (STDEV error bars)
328
329 Decay Resistance
330 Figure 7 showed that none of the veneers could be considered durable according to
35
7
30
25 6
5 214/2.0/TV
20
15 4 218/0.5/TV
10 3
5 2
- 204/2.0/TV
1
-
- 20 40 60
Weight loss Coniophora
341 puteana, %
342
343 Fig. 7. Weight loss after fungus Coniophora puteana and its correlation with a mass loss after
344 thermal treatment (STDEV error bars)
345
346 Microscopy
347 The color changes were observed to light brown in all TV regimes and dark brown
348 in WTT process in comparison with untreated light silver birch sample (Fig. 2). The treated
349 birch was the most affected by treatment processes 217/3.0/TV -cell walls became thinner
350 – red arrow and 160/0.8/WTT cell walls became fluffy or sharp less – orange arrow, as
351 shown in Fig. 8.
352
353 Untreated birch 204/2.0/TV
354
355
356
357
358
359 214/2.0/TV 217/3.0/TV
360
361
362 218/0.5/TV 160/0.8/WTT
363
364 Fig. 8. Cross-section before and after thermal treatment, LM, ×400. Bar = 100 µm.
365
366 The shrinkage of fiber cell walls was observed in both treatment regimes. The
367 thermally modified samples, especially for treatment regimes 217/3.0/TV and
368 160/0.8/WTT were more brittle than their untreated counterparts, which coincided with the
369 findings by Ahmed et al. (2013) and it makes influence to tensile strength (Fig. 5). During
370 thermal modification, middle lamella did not disappear because it consisted mainly of
371 lignin (70% to 90%), which was a more thermally stable wood component. Birch is diffuse-
372 porous wood and has sparse apotracheal parenchyma (Schoch et al. 2004). Besides, regime
373 160/0.8/WTT caused deformation of the vessels and fibers due to the increased pressure
374 and moist environment during modification. The cellulose framework shrank, and as a
375 result of that the fibers obtained an oval form in the cross-section (Biziks et al. 2013).
376
377
378 CONCLUSIONS
379
380 1. The TV thermal modification process was more suitable for birch (Betula pendula
381 Roth) veneer treatment than the WTT process both in terms of maintaining strength
382 properties and providing durability.
383 2. Among investigated samples, the regime 217/3.0/TV showed the best resistance
384 against brown rot and acceptable other physical - chemical properties and tensile
385 strength.