Micron size particles of poly(ether ether ketone) (PEEK) were prepared by self-made pan-type milling equipment operated at ambient temperature. The changes of particle morphology, crystalline properties, thermal behavior, and viscosity-average molecular mass during milling were studied by SEM, WAXD, DSC, TGA, and viscosimetry analyses, respectively. SEM analysis indicated that pan-milling firstly destroyed the original structure of PEEK through squeezing in-between mill pans, then to produce fine powder undergoing the processes of deforming and size reduction. The average particle size of PEEK was reduced to 100 lm only after 5 cycles of pan-milling and reached less than 50 lm after 50 cycles. DSC analysis showed that crystallinity of PEEK decreased with the panmilling cycles, agreed with WAXD data. The crystallinity of PEEK decreased from 46.2 to 39.9% of 50 pan-milling cycles was offered. The glass transition temperature increased slightly along with pan-milling cycles. Mechanochemical effects caused by pan-milling were also studied. Viscometer test exhibited that molecular weight dropped quickly at earlier pan-milling stage then decreased slightly during later pan-milling. Pan-milling technique is an efficient, clean, and environmental friendly method for preparing fine PEEK powder.