This study analyses the formation of polypyrrole/multi-walled carbon nanotube (PPy/MWCNT) composite materials using chemical oxidation with varying amounts of MWCNTs added. The samples are characterized by scanning electron microscopy, Fourier transform infrared emission spectroscopy, a four-probe method, and infrared thermal imaging using electromagnetic parameters. According to the test results, it is seen that the formation of PPy with the addition of MWCNTs can affect the material’s infrared properties and increase the material’s microwave return losses (up to −19dB). This production procedure can also make the peak frequency of the microwave return losses adjustable, and the composite’s infrared and microwave performance becomes compatible and adjustable.