We present the creation of a unique nanostructured amorphous/crystalline hybrid silicon material that exhibits surface enhanced Raman scattering (SERS) activity. This nanomaterial is an interconnected network of amorphous/crystalline nanospheroids which form a nanoweb structure; to our knowledge this material has not been previously observed nor has it been applied for use as a SERS sensing material. This material is formed using a femtosecond synthesis technique which facilitates a laser plume ion condensation formation mechanism. By fine-tuning the laser plume temperature and ion interaction mechanisms within the plume, we are able to precisely program the relative proportion of crystalline Si to amorphous Si content in the nanospheroids as well as the size distribution of individual nanospheroids and the size of Raman hotspot nanogaps. With the use of Rhodamine 6G (R6G) and Crystal Violet (CV) chemical dyes, we have been able to observe a maximum enhancement factor of 5.38 × 106 and 3.72 × 106 respectively, for the hybrid nanomaterial compared to a bulk Si wafer substrate. With the creation of a silicon-based nanomaterial capable of SERS detection of analytes, this work demonstrates a redefinition of the role of nanostructured Si from an inactive to SERS active role in nano-Raman sensing applications.
Currently, the quantum-scale surface-enhanced Raman scattering (SERS) properties of Si materials have yet to be discovered for universal biosensing applications. In this study, a potential universal biosensing probe is generated by activating the SERS functionality of Si nanostructures through near quantum-scale (nQS) engineering. We introduce herein 3D nonplasmonic Si nanomesh structure with nQS defects for SERS biosensing applications. Through ionization of a single-crystal defect-free Si wafer, highly defect-rich Si subnano-orbs (sNOs) are fabricated and self-assemble as connective 3D Si nanomesh structures with enhanced SERS biosensing activity. By amending the laser ionization and ion-ion interactions, we observe the controlled synthesis of engineered nQS defects in the form of nQS-grain boundary disorder or surface nQS voids within the interconnected Si sNOs. To our knowledge, it is shown here for the first time that defect-rich Si nanomesh structures exhibit enhanced Raman activity, with the nQS morphological and crystallographic defects acting as the prime SERS contributors without a plasmonic contribution. The SERS biosensing sensitivity with the synthesized defect-rich Si nanomesh structures without an additional plasmonic material was evaluated using of a tripeptide biomarker l-glutathione (GSH); we observe an enhancement factor value of ∼10 for the GSH biomolecules with 10 M sensitivity, a phenomena to our knowledge that has yet to be reported. Additionally, the SERS detection of multiple disease-signaling biomolecules (cysteine, tryptophan, and methionine) is achieved at very low analyte concentration (10 M). These results indicate a potential new dimension to universal SERS biosensing applications with these unique nonplasmonic defect-rich 3D nQS-Si nanostructures.
Ceramic carbon electrodes were prepared via polymerization of silane materials containing sulfonic acid groups in the presence of Pt/Vulcan XC72. Cyclic voltammetry and electrochemical impedance spectroscopy were used to investigate the effects of sulfonic acid functionalities on platinum utilization and proton conductivity, as well as CCE microstructure. It has been determined that incorporation of small amounts of sulfonated silane to the CCE structure can lead to a profound enhancement of proton conductivity despite decreases in BET surface area. Retention of surface area was achieved through combination of sulfonated and unsulfonated organosilane precursors. These composite samples show improved performance during fuel cell testing than for CCEs prepared using unsulfonated precursors.
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