Multi-walled carbon nanotubes (MWCNTs) synthesized by thermal chemical vapor deposition (Thermal CVD) have been successfully purified by high efficient microwave digestion purification method. In this paper, microwave digestion method was introduced to purify carbon nanotubes, because that acid can absorb microwave energy rapidly and dissolve metal efficiently in this method. MWCNTs were placed in 100 ml TFM (thennally resistant form of Teflon) vessels with 50 ml 5 M nitric acid. First, the temperature ramped up to 210 degrees C in 30 min and then kept for 10, 20, 30 to 120 min to digest the catalyst. The efficiency of this method was analyzed by thermogravimetric analysis (TGA) and the results showed that the catalyst content dropped from 10.39% to 1.75% only in 10-min digestion and 1.03% for 120 min treatment. Raman spectroscopy and high-resolution transmission electron microscopy (HRTEM) were applied to analyze the property and structure of raw and purified MWCNTs. This study presents a highly efficient and non-destructive purification method for high purity MWCNTs which can be provided in many applications or intrinsic property studies. (c) 2005 Elsevier B.V All rights reserved.