The methodologies applied in this study to prepare material samples, consisting of solution casting, extrusion process and 3D printing, are discussed in this chapter. Besides, experimental characterisation, such as the measurements of dimensional accuracy and surface roughness, hardness, abrasion resistance, tensile, shape memory and compression tests, are covered in this chapter. Other characterisations like scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transmission infrared (FTIR) analysis, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), are also employed in order to conduct holistic evaluation. To undertake a comprehensive analysis, this study uses statistical design of experiments (DoEs) based on Taguchi method, as well as Pareto ANOVA, along with confirmation tests for parametric optimisation with warranted experimental reproducibility.