Aegae, the first capital of the Macedonians, in Northern Greece, is being excavated since 1938. The most impressive finds come from the unlooted tombs of the Great Tumulus, where the grave of Philip II, father of Alexander the Great, was discovered. Not far from the Great Tumulus, in the “Tumuli cemetery”, the most ancient part of the graveyard (1000-700 B.C.), recent excavations brought to light three looted graves dated in the mid-fourth century B.C., with very interesting finds such as weapons, gilded wreaths, pieces of jewelry, remains of decoration of wooden furniture, ceramic vases broken in small pieces and wall paintings. This paper describes studies carried out on the binding and the painting materials used for the decoration of the above wall paintings and ceramic vases. The characterization was performed through Optical Microscopy, Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Microscopy (SEM-EDS). It was found that the fresco technique was used, while all the pigments were identified. The results are discussed and related with other findings in that period in the Greek area