A simple but effective in situ polymerization method has been developed to prepare phenolic resin-based nanocomposites with pristine or carboxylated multi-walled carbon nanotubes (MWNTs) as fillers. As revealed by scanning electron microscopy, the nanotubes are well-dispersed in and strongly adhered to the phenolic resin. The resultant nanocomposites have thus obtained the improved thermostabilities. As compared to pristine MWNT-filled nanocomposite, the carboxylated MWNT-filled one has shown more improved thermostability, resulting from the higher dispersion quality of functionalized nanotubes. The related mechanisms have been analyzed qualitatively. To achieve the similar effects, however, more mixing energy should be deposited on the melt mixture in the melt-mixing process. These indicate that phenolic resin-MWNT nanocomposites with high performance may be realized by adoption of pertinent preparation method and moderate functionalized nanotubes.KEY WORDS: Phenolic Resin / MWNT / In situ Polymerization / Nanocomposite / Dispersion Behavior / Thermal Properties / Due to their excellent mechanical property and high aspect ratio, carbon nanotubes (CNTs) are increasingly considered to be unique reinforcement fillers for making polymer-based nanocomposites. [1][2][3][4][5][6] In order to achieve strength enhancement as high as possible, homogeneous dispersion of CNTs and strong interaction between CNT and surrounding matrix are generally required.7 However, the pristine nanotubes are usually bundled due to strong van de Waals interactions, thus making their dispersibility in most of polymer matrices rather poor. Otherwise, intrinsically smooth surface and chemical inertness of the nanotubes lead to their weak adhesion to polymer matrix. As a result, the nanocomposites based on simple polymer-pristine nanotube blends prepared by highspeed mixing and/or ultrasonication have shown limited strength enhancement as compared with conventional composites, and their mechanical properties are noticeably below the highly anticipated potential. [7][8][9] To resolve these problems, there is growing research effort in understanding the interface between CNT and matrix. Functionalization of CNTs, which permits directly tailoring of the chemical and physical properties of nanotubes according to their specific applications, is envisaged as an ideal cut-in point and has therefore been extensively investigated.10-15 Strength enhancement of the functionalized nanotube-filled nanocomposites was generally achieved. However, these functionalization techniques more or less rely on wet chemistry. Toxicity of chemicals and damage to nanotubes are issues which must be addressed. Comparatively, it may be easier and more direct as well as environment friendly for a given polymer matrix to prepare its nanocomposites by adopting a pertinent preparation method. At least, as having been proven, it is feasible for certain polymer matrix. 8,[16][17][18][19][20] In this work, taking phenolic resin as a matrix example, we have also addressed this iss...