Porous
silicon nanoparticles (pSiNPs) are of increased interest
for use in drug delivery systems, as catalysts, and as biomedical
imaging agents. The most common synthesis of pSiNPs involves electrochemical
anodization of a silicon wafer, followed by ultrasonic fracture of
the resulting mesoporous film to form well-defined nanoparticles.
A major source of loss in this process is the ultrasonic fracture
step. This work presents a method of synthesizing gram-scale quantities
of pSiNPs with high yield and high reproducibility using an ultrasonic
bath equipped with a sample rotation stage and a refrigerator (4 °C)
and a higher ultrasound frequency with power delivered in a pulsed
modality compared with the static ultrasound “cleaning baths”
commonly used for this purpose. The optimal processing conditions
are determined by adjusting the pSi film mass, solvent volume, and
iteration number of on/off cycles used in sonication. The approach
provides pSiNPs with a narrow size distribution (∼170 nm, PDI
= 0.149), higher yields (59%), and an approximately 12-fold reduction
in the total processing time, allowing the preparation of gram-scale
quantities of pSiNPs from single-crystal silicon wafers with high
reproducibility in a single 24 h process. The performance of the produced
pSiNPs is validated in a drug delivery application in which loading
and release of the anthracycline drug doxorubicin are compared with
pSiNPs prepared in a conventional cleaning bath ultrasonicator.