Orientation behavior of MWNTs (0.01-0.05%) in PMMA matrix has been studied using scanning electron microscopy, FT-IR spectroscopy and Raman spectroscopy. MWNT/PMMA nanocomposites have been synthesized by solution cast method. Dispersion of MWNT in PMMA matrix has been performed by ultrasonication. SEM images show surface morphology of MWNTs oriented in PMMA matrix. FT-IR spectra show interaction nature of MWNT with PMMA matrix. Shifted wavenumber shows the orientation characteristics and bonding nature. Increased Raman intensity for 0.01% MWNT in PMMA matrix shows orientation nature of MWNTs in PMMA matrix.