One dimensional carbon structure (carbyne) was tried to be synthesized through electrochemical defluorinationof polytetrafluoroethylene (PTFE) in nonaqueous electrolytes. When tetrahydrofuran (THF) solution containingtetrabutylammonium perchlorate (TBAP) was used as electrolyte, the electrochemical defluorination of PTFEproceeded sufficiently with the potentiostatic reduction at 0 V vs. Li/Li+. According to the results with Raman analysis, it was found that polyacetylene structure were contained in the defluorination products. The FTIR spectrum suggestedthe existence of triple bond of carbon atoms in the defluorination products. On the other hand, the electrochemical defluorination did not so proceed in THF solution containing lithium perchlorate (LiClO4) at OV vs. Li/Li+. Moreover, triple bond of carbon atoms was not found when LiClO4/THF was used. Considering the stability against electrochemicalreduction of these two electrolytes, it can be concluded that decomposed species of TBAP promote the defluorinationof PTFE.