The　water　monitoring　parameter　of　chemical　oxygen　demand　(COD)　is　a　universal　way　to　assess　organic　pollution　in　aqueous　systems.　Though　the　ways　for　the　detection　of　COD　have　been　developed　for　decades,　it　is　still　a　challenge　to　achieve　highly　sensitive　and　portable　COD　detectors.　In　this　work,　a　new　electrode　composite　of　Ni/ZnO/Cu　(CE-1)　was　prepared　for　the　electrochemical　tests　of　COD.　The　electrode　was　structural　characterized　by　using　scanning　electron　microscope　(SEM),　transmission　electron　microscope　(TEM),　and　X-ray　Diffractometer　(XRD),　which　showed　that　self-supported　Cu　microflowers　were　successfully　electrodeposited　on　the　ZnO　micro-prims　that　were　firstly　loaded　on　the　Ni　foils.　The　electrochemical　behaviors　were　investigated　with　the　comparison　of　CE-1　and　the　electrode　that　Cu　nanoparticles　were　directly　deposited　on　the　Ni　foil　(CE2).　It　shows　that　CE-1　possesses　much　superior　electrochemical　properties　than　CE-2,　which　indicates　that　the　introduction　of　ZnO　micro-rod　the　electrode　can　significantly　enhance　the　electrocatalysis　property.　CE-1　exhibited　a　linear　COD　detection　range　of　2.3603　to　577.8　mg/L　as　well　as　an　excellent　correlation　with　the　classic　dichromate　method　(R-2　=　0.99933).　Moreover,　low　detection　limit　of　0.6036　mg/L　(the　signal　blank/　slope=3)　and　high　sensitivity　of　2.403　x　10(-2)　mA　/　(mg.L-1)　can　be　simultaneously　achieved　by　using　CE-1,　which　is　hard　to　attain　for　its　counterparts　reported　in　literature.　CE-1　also　shows　good　concordance　with　the　classic　method　for　real　water　sample　detections.　Consequently,　the　environmentally　friendly　CE-1　is　supposed　as　a　promising　candidate　for　COD　detection　electrode.