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This paper reports spatially arranged pyrolyzed polymer-gold probes to allow high-sensitivity monitoring of spatially distributed chemicals. Pyrolyzed polymer is a promising carbon material for applications of electrochemical sensors. Out-of-plane gold microelectrodes coated by polymer film (parylene-C) are transformed to conductive carbon-gold materials by annealing at 1000°C for 2h in a vacuum chamber. 3D probe technology using wire bonding makes it possible to provide the spatially arranged microelectrodes. This paper demonstrates pyrolyzed polymer-gold 3D probes have high sensitivity and wider electrochemical potential window than typical electrochemical electrode materials such as gold to realize spatial chemical sensing.