Gold (Au) nanoparticles-decorated poly(o-phenylenediamine) (PoPD@Au) hollow microspheres were successfully synthesized by a simple two-step process without any other templates or additives. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, and ultraviolet–visible absorption spectra were performed to characterize the resulting samples. The results confirmed that the obtained PoPD@Au microspheres had a perfect hollow structure and revealed that there is an interaction between PoPD hollow microspheres and Au nanoparticles. Plausible explanation for the formation of PoPD@Au hollow microspheres has been elaborated. Furthermore, PoPD@Au hollow microspheres were immobilized onto the surface of a glassy carbon electrode and applied to construct a sensor. Cyclic voltammogram experiments indicated that the proposed sensor method had good sensitivity, stability, and repeatability.
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