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Licensed Unlicensed Requires Authentication Published by De Gruyter June 29, 2020

Surface properties of thermally treated European beech wood studied by PeakForce Tapping atomic force microscopy and Fourier-transform infrared spectroscopy

Rastislav Lagaňa ORCID logo EMAIL logo , Csilla Csiha ORCID logo , Norbert Horváth , László Tolvaj , Tomáš Andor , Jozef Kúdela , Róbert Németh ORCID logo , František Kačík ORCID logo and Jaroslav Ďurkovič ORCID logo
From the journal Holzforschung


Natural constituents of wood cell-wall layers are affected in various ways by thermal treatment. This study investigated the effect of high-temperature treatment on the properties of cell-wall layers. The properties were studied using PeakForce quantitative nanomechanical mapping and Fourier-transform infrared spectroscopy (FTIR). European beech wood was thermally treated at 200 °C for 1, 3, and 5 h in an oxidizing atmosphere. Modulus of elasticity, adhesion force, and roughness of the secondary S2 layer and the compound middle lamella (CML) were determined using atomic force microscopy (AFM). Results showed that both the S2 layer and CML were affected by thermal treatment. Stiffening of the S2 layer was caused by increased crystallinity of the cellulose-dominated component, having peaked after 1 h of treatment. The degradation thereafter resulted in a decrease of the S2 as well as the CML stiffness. An increase of CML roughness after 3 h of treatment was associated with the effect of thermal degradation on CML integrity. The analysis suggested that the reduction in syringyl lignin is potentially associated with an increase in adhesion of cell-wall layers.

Correction notes

Correction added after online publication July 20, 2020: One of the supportive grants was mistakenly removed by the corresponding author during the last proof of the manuscript. The text “, the Slovak Scientific Grant Agency VEGA (grant no. 1/0450/19)” was inserted back to the Research funding statement.

Corresponding author: Rastislav Lagaňa, Department of Wood Science, Technical University in Zvolen, T. G. Masaryka 24, Zvolen, 96053, Slovakia, E-mail:

Award Identifier / Grant number: APVV-16-0177

Award Identifier / Grant number: APVV SK-HU-2013-0035

Funding source: Slovak Scientific Grant Agency VEGA

Award Identifier / Grant number: 1/0450/19

Funding source: National Research, Development and Innovation Fund of Hungary

Award Identifier / Grant number: TÉT_12_SK-1-2013-0035

  1. Author contribution: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This work was supported by the Slovak Research and Development Agency (grant nos. APVV-16-0177, APVV SK-HU-2013-0035), the Slovak Scientific Grant Agency VEGA (grant no. 1/0450/19) and the National Research, Development and Innovation Fund of Hungary (grant no. TÉT_12_SK-1-2013-0035)

  3. Employment or leadership: None declared.

  4. Honorarium: None declared.

  5. Conflict of interest statement: The authors declare that there is no conflict of interest regarding this study.


Alen, R., Kotilainen, R., and Zaman, A. (2002). Thermochemical behavior of Norway spruce (Picea abies) at 180 °C to 225 °C. Wood Sci. Technol. 36: 163–171, in Google Scholar

Allegretti, O., Brunetti, M., Cuccui, I., Ferrari, S., Nocetti, M., and Terziev, N. (2012). Thermo-vacuum modification of spruce (Picea abies Karst.) and fir (Abies alba Mill.) wood. BioResources 7: 3656–3669, in Google Scholar

Arnould, O., Siniscalco, D., Bourmaud, A., Le Duigoua, A., and Baleya, C. (2017). Better insight into the nano-mechanical properties of flax fibre cell walls. Ind. Crop. Prod. 97: 224–228, in Google Scholar

Bhuiyan, T.R., Hirai, N., and Sobue, N. (2000). Changes of crystallinity in wood cellulose by heat treatment under dried and moist conditions. J. Wood Sci. 46: 431–436, in Google Scholar

Blanchet, P., Kaboorani, A., and Bustos, C. (2016). Understanding effects of drying methods on wood mechanical properties at ultra and cellular levels. Wood Fiber Sci. 48: 117–128.Search in Google Scholar

Boonstra, M.J., Van Acker, J., Tjeerdsma, B.F., and Kegel, E.V. (2007). Strength properties of thermally modified softwoods and its relation to polymeric structural wood constituents. Ann. For. Sci. 64: 679–690, in Google Scholar

Casdorff, K., Kläusler, O., Gabriel, J., Amen, C., Lehringer, C., Burgert, I., and Keplinger, T. (2018a). About the influence of a water-based priming system on the interactions between wood and one-component polyurethane adhesive studied by atomic force microscopy and confocal Raman spectroscopy imaging. Int. J. Adhesion Adhes. 80: 52–59, in Google Scholar

Casdorff, K., Keplinger, T., and Burgert, I., (2018b). Nano-mechanical characterization of the wood cell wall by AFM studies: comparison between AC- and QI™ mode. Plant Methods 13: 60, in Google Scholar PubMed PubMed Central

Charrier, A.M., Lereu, A.L., Farahi, R.H., Davison, B.H., and Passian, A., (2018). Nanometrology of biomass for bioenergy: the role of atomic force microscopy and spectroscopy in plant cell characterization. Front. Energy Res. 6: 11, in Google Scholar

Chu, D., Mu, J., Avramidis, S., Rahimi, S., Lai, Z., and Ayanleye, S. (2020). Effect of heat treatment on bonding performance of poplar via an insight into dynamic wettability and surface strength transition from outer to inner layers. Holzforschung, online first, in Google Scholar

Csanady, E., Magoss, E., and Tolvaj, L. (2015). Quality of machined wood surfaces. Springer, Berlin, pp. 41–91, in Google Scholar

Derjaguin, B.V., Muller, V.M., and Toporov, Y.P. (1975). Effect of contact deformations on the adhesion of particles. J. Colloid Interface Sci. 53: 314–326, in Google Scholar

Ďurkovič, J., Čaňová, I., Javoříková, L., Kardošová, M., Lagaňa, R., Priwitzer, T., Longauer, R., and Krajňáková, J. (2016). The effects of propagation techniques on leaf vascular anatomy, modulus of elasticity, and photosynthetic traits in micropropagated and grafted plants of the Dutch elm hybrid ‘Dodoens’. J. Am. Soc. Hortic. Sci. 141: 351–362, in Google Scholar

Eriksson, M., Notley, S. M., and Wågberg, L. (2007). Cellulose thin films: degree of cellulose ordering and its influence on adhesion. Biomacromolecules 8: 912–919, in Google Scholar PubMed

Esteves, B., Velez Marques, A., Domingos, I., and Pereira, H. (2013). Chemical changes of heat treated pine and eucalypt wood monitored by FTIR. Maderas Cienc. Tecnol. 15: 245–258, in Google Scholar

Fergus, B.J. and Goring, D.A.I. (1970). The distribution of lignin in Birch wood as determined by ultraviolet microscopy. Holzforschung 24: 118–124, in Google Scholar

González-Peña, M.M., Curling, S.F., and Hale, M.D.C. (2009). On the effect of heat on the chemical composition and dimensions of thermally-modified wood. Polym. Degrad. Stabil. 94: 2184–2193, in Google Scholar

Gurdil, G.A.K., Selvi, K.C., Malatak, J, and Pinar, Y. (2009). Biomass utilization for thermal energy. Ama, Agric. Mech. Asia, Afr. Lat. Am. 40: 80–85.Search in Google Scholar

Hill, C.A.S. (2006). Wood modification: chemical, thermal, and other processes. Wiley, Chichester, p. 260.10.1002/0470021748Search in Google Scholar

Hill, C. (2014). Thermally modified wood – the role of hemicelluloses. In: Proceedings of the Final Cost Action FP0904 Conference “Recent Advances in the Field of TH and THM Wood Treatment”, May 19-21, 2014, Skellefteå, Sweden, pp. 1–2.Search in Google Scholar

ISO 13061-17 (2017). Physical and mechanical properties of wood -- test methods for small clear wood specimens. Part 17: Determination of ultimate stress in compression parallel to grain, p. 4.Search in Google Scholar

Jin, X. and Kasal, B. (2016). Adhesion force mapping on wood by atomic force microscopy: influence of surface roughness and tip geometry. R. Soc. Open Sci. 3: 160248, in Google Scholar PubMed PubMed Central

Kačíková, D., Kačík, F., Čabalová, I., and Ďurkovič, J. (2013). Effects of thermal treatment on chemical, mechanical, and colour traits in Norway spruce wood. Bioresour. Technol. 144: 669–674, in Google Scholar PubMed

Kong, L., Zhao, Z., He, Z., and Yi, S. (2017). Effects of steaming treatment on crystallinity and glass transition temperature of Eucalyptuses grandis × E. urophylla. Results Phys. 7: 914–919, in Google Scholar

Konnerth, J., Gierlinger, N., Keckes, J., and Gindl, W. (2009). Actual versus apparent within cell wall variability of nanoindentation results from wood cell walls related to cellulose microfibril angle. J. Mater. Sci. 44: 4399–4406, in Google Scholar PubMed PubMed Central

Kotilainen, R., Toivannen, T., and Alén, R. (2000). FTIR monitoring of chemical changes in softwood during heating. J. Wood Chem. Technol. 20: 307–320, in Google Scholar

Kruer-Zerhusen, N., Cantero-Tubilla, B., and Wilson, D.B. (2018). Characterization of cellulose crystallinity after enzymatic treatment using fourier transform infrared spectroscopy(FTIR). Cellulose 25: 37–48, in Google Scholar

Kučerová, V., Kačíková, D., and Kačík, F. (2011). Alterations of extractives and cellulose macromolecular characteristics after thermal degradation of spruce wood. Acta Fac. Xylologiae Zvolen 53: 77–83.Search in Google Scholar

Marti, O. (2001). Measurement of adhesion and pull-off forces with the AFM. In: Bhushan, B (Ed.). Chapter 17. Modern tribology handbook. CRC Press, Boca Raton, United States, p. 1760.10.1201/9780849377877.ch17Search in Google Scholar

Michell, A.J. and Higgins, G.H. (2002). Infrared spectroscopy in Australian forest products research. CSIRO Forestry and Forest Products, Melbourne, p. 35.Search in Google Scholar

Missio, A.L., Mattos, B.D., de Cademartori, P.H.G., Pertuzzatti, A, Conte, B, and Gatto, D.A. (2015). Thermochemical and physical properties of two fast-growing eucalypt woods subjected to two-step freeze heat treatments. Thermochim. Acta 615: 15–22, in Google Scholar

Missio, A.L., Mattos, B.D., de Cademartori, P.H.G., and Gatto, D.A. (2016). Effects of two-step freezing-heat treatments on japanese raisintree (Hovenia dulcis thunb.) wood properties. J. Wood Chem. Technol. 36: 16–26, in Google Scholar

Poletto, M., Zattera, A.J., Forte, M.M.C., and Santana, R.M.C. (2012). Thermal decomposition of wood: Influence of wood components and cellulose crystallite size. Bioresour. Technol. 109: 148–153, in Google Scholar PubMed

Sader, J.E., Chon, J.W.M., and Mulvaney, P. (1999). Calibration of rectangular atomic force microscope cantilevers. Rev. Sci. Instrum. 70: 3967–3969, in Google Scholar

Sakakibara, A. and Sano, Y. (2001). Chemistry of lignin. In: Hon, D.N.S. and Shiraishi, N. (Eds.). Wood and cellulosic chemistry, 2nd ed. Marcel Dekker, New York, NY, pp. 109–173.Search in Google Scholar

Seborg, M., Tarkow, H., and Stamm, A.J. (1953). Effect of heat upon the dimensional stabilization of wood. J. For. Prod. Res. Soc. 9: 1−9.Search in Google Scholar

Smolyakova, G., Pruvost, S., Cardoso, L., Alonso, D., Belamie, E., and Duchet-Rumeau, J. (2016). AFM PeakForce QNM mode: evidencing nanometre-scale mechanical properties of chitin-silica hybrid nanocomposites. Carbohydr. Polym. 151: 373–380, in Google Scholar PubMed

Tjeerdsma, B.F., and Militz, H. (2005). Chemical changes in hydrothermal treated wood: FTIR analysis of combined hydrothermal and dry heat-treated wood. Eur. J. Wood Wood Prod. 63: 102–111, in Google Scholar

Usov, I., Nyström, G., Adamcik, J., Handschin, S., Schütz, C., Fall, A., Bergström, L., and Mezzenga, R. (2015). Understanding nanocellulose chirality and structure–properties relationship at the single fibril level. Nat. Commun. 6: 7564, in Google Scholar PubMed PubMed Central

Výbohová, E., Kučerová, V., Andor, T., Balážová, Ž., and Veľková, V. (2018). The effect of heat treatment on the chemical composition of ash wood. BioResources 13: 8394–8408, in Google Scholar

Wimmer, R., Lucas, B.N., Tsui, T.Y., and Oliver, W.C. (1997). Longitudinal hardness and Young’s of spruce tracheid secondary walls nanoindentation technique. Wood Sci. Technol. 31: 131–141, in Google Scholar

Yildiz, S., Gezer, E.D., and Yildiz, U.C. (2006). Mechanical and chemical behavior of spruce wood modified by heat. Build. Environ. 41: 1762–1766, in Google Scholar

Yildiz, S. and Gumuskaya, E. (2007). The effects of thermal modification on crystalline structure of cellulose in soft and hardwood. Build. Environ. 42: 62–67, in Google Scholar

Zawadzki, J., Gawron, J., Antczak, A., Kłosińska, T., and Radomski, A. (2013). The influence of heat treatment on the physico-chemical properties of pinewood (Pinus sylvestris L.). Drewno 59: 49–57, in Google Scholar

Zeng, Y., Himmel, M.E., and Ding, S.Y. (2017). Visualizing chemical functionality in plant cell walls. Biotechnol. Biofuels 10: 263, in Google Scholar PubMed PubMed Central

Received: 2019-05-17
Accepted: 2020-03-24
Published Online: 2020-06-29
Published in Print: 2021-01-26

© 2020 Walter de Gruyter GmbH, Berlin/Boston

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