Implantable neural microsensors have significantly advanced neuroscience research, but the geometry of most probes is limited by the fabrication methods. Therefore, new methods are needed for batch-manufacturing with high reproducibility. Herein, a novel method is developed using two-photon nanolithography followed by pyrolysis for fabrication of free-standing microelectrodes with a carbon electroactive surface. 3D-printed spherical and conical electrodes were characterized with slow scan cyclic voltammetry (CV). With fast-scan CV, the electrodes showed low dopamine LODs of 11±1 nm (sphere) and 10±2 nm (cone), high sensitivity to multiple neurochemicals, and high reproducibility. Spherical microelectrodes were used to detect dopamine in a brain slice and in vivo, demonstrating they are robust enough for tissue implantation. This work is the first demonstration of 3D-printing of free-standing carbon electrodes; and the method is promising for batch fabrication of customized, implantable neural sensors.