Fused filament fabrication (FFF) has emerged as a versatile additive manufacturing (AM) process for high-performance polymers, combining accessibility with the capability to process advanced materials such as polyether ether ketone (PEEK). This thesis focuses on process optimization of multi-material FFF using carbon fiber-reinforced PEEK (CF-PEEK) and laser direct structurable PEEK (LDS-PEEK) for CubeSat applications. CF-PEEK offers excellent stiffness and thermal resistance, while LDS-PEEK enables electronic integration; however, their simultaneous processing poses challenges due to differences in thermal expansion and solidification behavior. A two-phase experimental methodology was applied: baseline CF-PEEK panels were optimized through parameter screening, followed by dual-material CF-PEEK/LDS-PEEK printing to assess interfacial compatibility.