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The brain is a complex network that accounts for only 5% of human mass but consumes 20% of our energy. Uncovering the mysteries of the brain’s functions in motion, memory, learning, behavior, and mental health remains a hot but challenging topic. Neurochemicals in the brain, such as neurotransmitters, neuromodulators, gliotransmitters, hormones, and metabolism substrates and products, play vital roles in mediating and modulating normal brain function, and their abnormal release or imbalanced concentrations can cause various diseases, such as epilepsy, Alzheimer’s disease, and Parkinson’s disease. A wide range of techniques have been used to probe the concentrations of neurochemicals under normal, stimulated, diseased, and drug-induced conditions in order to understand the neurochemistry of drug mechanisms and develop diagnostic tools or therapies. Recent advancements in detection methods, device fabrication, and new materials have resulted in the development of neurochemical sensors with improved performance. However, direct in vivo measurements require a robust sensor that is highly sensitive and selective with minimal fouling and reduced inflammatory foreign body responses. Here, we review recent advances in neurochemical sensor development for in vivo studies, with a focus on electrochemical and optical probes. Other alternative methods are also compared. We discuss in detail the in vivo challenges for these methods and provide an outlook for future directions. 

Abstract Neuromodulation technologies have gained considerable attention for their clinical potential in treating neurological disorders and advancing cognition research. However, traditional methods like electrical stimulation and optogenetics face technical and biological challenges that limit their therapeutic and research applications. A promising alternative, photoelectric neurostimulation, uses near‐infrared light to generate electrical pulses and thus enables stimulation of neuronal activity without genetic alterations. This study explores various design strategies to enhance photoelectric stimulation with minimally invasive, ultrasmall, untethered carbon electrodes. Employing a multiphoton laser as the near‐infrared (NIR) light source, benchtop experiments are conducted using a three‐electrode setup and chronopotentiometry to record photo‐stimulated voltage. In vivo evaluations utilize Thy1‐GCaMP6s mice with acutely implanted ultrasmall carbon electrodes. Results highlighted the beneficial effects of high duty‐cycle laser scanning and photovoltaic polymer interfaces on the photo‐stimulated voltages by the implanted electrode. Additionally, the promising potential of carbon‐based diamond electrodes are demonstrated for photoelectric stimulation and the application of photoelectric stimulation in precise chemical delivery by loading mesoporous silica nanoparticles (SNPs) co‐deposited with polyethylenedioxythiophene (PEDOT). Together, these findings on photoelectric stimulation utilizing ultrasmall carbon electrodes underscore its immense potential for advancing the next generation of neurostimulation technology.