Directly Convert Carbonaceous Microspheres to Three-Dimensional Porous Carbon Microspheres with a Robust Self-Supporting Structure as a Metal-Free SERS Substrate for Online High-Throughput Analysis.

It is of great significance for practical applications to directly convert readily available biomass carbon into three-dimensional (3D) porous carbon microspheres with a self-supporting structure. Herein, we report the convenient conversion of biomass carbon microspheres to hierarchical porous carbon microspheres (HP-CMSs) with a robust self-supporting framework structure. A general SiO₂-induced etching mechanism is proposed for the formation of the HP-CMSs. Benefiting from this robust 3D self-supporting frame structure, these HP-CMSs have outstanding mechanical, chemical, and thermal stability. As a metal-free surface-enhanced Raman scattering (SERS) substrate with an ultrahigh specific surface area (4216 m² g^-1) and a high density of active sites, the HP-CMSs exhibit high sensitivity with a detection limit of 10^-10 M and a Raman enhancement factor of 3.5 × 10⁶. By integrating the enrichment and sensing functions of the HP-CMSs in a microfluidic channel, online high-throughput SERS detection of 20 samples within 5 min is achieved in a single channel, and the relative standard deviation of the signals between samples is only 5.1%. The current work develops a convenient preparation method that converts sustainable biomass carbon to 3D hierarchical porous carbon and provides a potential material for sensing, energy, catalysis, and other fields.