The preparation of nanocomposites through melt mixing was challenging as the nanofillers tend to form agglomeration. The silicon carbide nanowhiskers (SiCNWs) filled poly (methyl methacrylate) (PMMA) thin film in this study was prepared by means of solution casting. Acetone with low toxicity was used as solvent to dissolve the PMMA pellets. A coupling agent, silane was used to enhance the properties of composite films. Besides, the untreated and treated SiCNWs were filled into PMMA matrix, respectively with the filler loading varied from 0.2 to 0.8 wt%. The universal testing machine was used to investigate the tensile properties of composites. It was found out that the tensile strength of the PMMA was reduced in the presence of SiCNWs. However, the tensile strength had increased with the rise of filler loading. At 0.8 wt% of SiCNWs, the composites’ tensile strength was comparable to virgin PMMA. Meanwhile, the SiCNWs had reduced the elongation at break but increased the elastic modulus of PMMA/SiCNWs nanocomposite films. In addition, silane surface treatment on SiCNWs had improved the tensile strength and ductility but lowered the elastic modulus of the nanocomposites. The improvement was due to the enhancement of interfacial adhesion between SiCNWs and PMMA.