Abstract: The objective of this work was to form a hydrophobic surface in a highly porous wood by coating and incorporating TiO2 micro/nano structures through the microwave-assisted solvotermal method, without need any pre- or post-modification of the wood substrate, using low temperatures and short times. The behavior and morphology of the TiO2-treated surfaces was characterized using scanning electron microscopy (SEM), while the elemental composition was determined via energy-dispersive X-ray spectroscopy and X-ray diffraction analysis. The results indicated that the crystallization of the TiO2 anatase phase was efficient and fully coated the wood surface during the solvothermal process. The treated wood contained TiO2 particles agglomerate with an average diameter of 200 nm that also allowed to coat an abundant fraction of tracheids cell walls. When investigated through X-ray spectroscopy-mapping, the element titanium appeared abundantly throughout the wood. After TiO2 growth in wood through the microwave-assisted solvotermal method, a roughness at the micro/nano scales structures was created on the wood surface, originating an increase in the contact angle up to 137°, which characterizes the appearance of a hydrophobic surface. The TiO2-treated wood demonstrated 85% of water absorption after 400 h of immersion, while untreated wood reached 160%, suggesting that the microwave-assisted solvotermal process promotes a delay in the progression of water absorption. This feature can improve the dimensional stability of wood, contributing to the increase of its durability and applications.

RESUMO A madeira é um material formado basicamente por polímeros, os quais são pouco resistentes a altas temperaturas e suscetíveis ao fogo. Em aplicações é desejável que esta madeira tenha um melhor desempenho quanto à ignição e perda de resistência mecânica devido à degradação térmica de seus componentes. O aumento de desempenho pode ser obtido pela modificação das propriedades térmicas madeira através de seu tratamento. Assim, utilizou-se o processo solvotermal assistido por micro-ondas para a modificação da superfície e do interior da madeira de Pinus elliotttii com TiO2 visando o aumento da resistência à inflamabilidade e à degradação térmica pelo retardamento da carbonização. Para isso, foi preparada uma solução precursora alcoólica com isopropóxido de titânio. Com temperatura de 140°C, por 60 minutos, foram cristalizadas, na superfície interna e externa da madeira, nanopartículas de TiO2 na fase anatase. Utilizando a Microscopia Eletrônica de Varredura foi possível demostrar o recobrimento uniforme e homogêneo. Através do espectro no infravermelho por Transformada de Fourier verificaram-se indícios de ligação por ponte de hidrogênio entre os dois materiais. A formação de uma camada protetora com as partículas proporcionou maior estabilidade e resistência térmica devido ao caráter cerâmico das nanopartículas de TiO2. A partir das análises termogravimétricas foi determinada uma perda de massa de 70% aos 380°C e 11% de resíduos aos 700°C, diferentemente da madeira modificada que nestas temperaturas atingiram percentagens de 45% e 46%, respectivamente. Em adição, verificou-se pelos testes de chama, retardo em cerca de 7 vezes o tempo para a ignição da madeira modificada, quando comparada com o controle. Desse modo, pode-se afirmar que a modificação da madeira pelo processo solvotermal assistido por micro-ondas foi efetiva na redução de sua inflamabilidade bem como de sua degradação com o aumento da temperatura. Cita-se ainda, que o método se apresenta com grande potencial para o aumento da qualidade da madeira e consequentemente de suas aplicações.

ABSTRACT Wood is composed by polymeric materials, with fire susceptibility. For applications, wood with better ignition resistance and lower fire stenght reduction is desirable. Enhancing of wood thermal properties can be achieved by means of right modification of wood by treatment. Thus, the microwave-assisted solvotermal process was implemented to modify the surface of the Pinus elliotttii wood with TiO2 in order to increase the resistance to flammability and thermal degradation through the retardation of carbonization. An alcoholic precursor solution with titanium isopropoxide was prepared and nanoparticles of TiO2 were crystallized to anatase on wood surface and interior at 140°C, for 60 minutes. Using Scanning Electron Microscopy, it was possible to demonstrate the uniform and homogeneous coating, and by Fourier transform infrared spectroscopy, it was possible to indicate presence of hydrogen bonds between the two materials. The formation of protective particle layer afforded greater stability and thermal resistance due to the ceramic character of TiO2. From the thermogravimetric analysis, 70% of weigh loss at 380°C and 11% of residual content at 700°C was verified, differently from the modified wood that at these temperatures reached 45% and 46%, respectively. Corroborating with these results, it was evident from the flame tests that wood with the presence of particles delayed about 7 times the moment of ignition. Thus, the microwave-assisted solvotermal process has great potential to transform wood and other porous materials into a less flammable material, maintaining its entire structure for a longer time when exposed to adverse conditions

Abstract: This study aimed to synthesize titanium dioxide nanoparticles by microwave-assisted hydrothermal method to incorporate them to the structure of Pinus elliottii wood. The color changes and the decay resistance of impregnated wood was investigated. The titanium dioxide nanoparticles were impregnated into Pinus elliottii wood by vacuum-pressure and simple immersion methods. Furthermore, Pinus elliottii wood was treated with chromated copper borate solution tocompare their effectiveness to the titanium dioxide treated wood. The titanium dioxide nanoparticles impregnated by vacuum-pressure were presented especially on the wood surface, forming a homogeneous coating. The titanium dioxide nanoparticles did not change the natural color of wood and, at the same time, decreased the degree of the white rot fungus (Ganoderma applanatum) colonization in the wood structure and the wood decay, compared to the untreated one. The titanium dioxide treated wood samples provided similar protection against decay in comparison to wood treated with chromated copper borate. The impegnation with titanium dioxide nanoparticles can be a good alternative to decrease/avoid the fungi proliferation, providing to Pinus elliottii wood a self-cleaning mechanism.