Herein,　we　fabricated　a　novel　NiO@CuxO　nanorods　(NRs)　composite　electrode　grown　in-situ　on　copper　foam　(CF),　designated　as　NiO@CuxO　NRs/CF.　This　electrode　demonstrates　excellent　performance　in　a　heterogeneous　electro-Fenton-like　system.　It　efficiently　activates　O2　to　generate　1O2　in-situ　without　the　addition　of　oxidant　precursors　and　effectively　degrades　chloroquine　phosphate　(CQ).　The　combination　of　NiO　and　CuxO　nanoarrays　created　multiple　synergistic　sites　for　molecular　oxygen　adsorption　and　activation.　The　addition　of　NiO　induced　the　formation　of　low-valence　Cu　species　and　effectively　optimized　oxygen　reduction　reaction　(ORR)　kinetics.　This　enhancement　led　to　an　increased　generation　of　key　intermediates　(center　dot　O2-　and　center　dot　OH),　which　further　promoted　the　efficient　production　of　1O2　through　the　chain　reaction　mediated　by　center　dot　O2-　and　center　dot　OH.　NiO@CuxO　NRs/CF　achieved　a　3.9-fold　increase　in　1O2　production　compared　to　the　CF　electrode.　NiO@CuxO　NRs/CF　electrodes　exhibited　exceptional　performance　in　degrading　CQ　across　a　wide　pH　range　(3-11).　Meanwhile,　it　also　displayed　remarkable　stability　and　anti-interference　capability,　highlighting　their　promising　potential　for　practical　applications.　The　study　provides　an　innovative　strategy　for　the　in-situ　production　of　1O2　through　molecular　oxygen　activation　with　a　bimetallic　composite　catalyst　to　efficiently　degrade　organic　pollutants.