The size and dispersity of nanoparticles (NPs) determine the properties that such particles display. In this study, synthesis of silver nanoparticles in a coaxial flow reactor (CFR) was investigated by confining the reaction and subsequent nucleation to an interface away from the channel wall. Silver NPs were formed at room temperature by reducing silver nitrate with sodium borohydride in the presence of sodium hydroxide, while trisodium citrate was used as the surfactant. The main parameters investigated were flow rate of reagents through the CFR and concentrations of trisodium citrate and silver nitrate.Decreasing the total flow rate resulted in the NP size and dispersity reducing from 5.4 AE 3.4 nm to 3.1 AE 1.6 nm. Increasing surfactant concentration reduced size and dispersity from 8.5 AE 6.9 nm to 4.1 AE 1.1 nm. By tuning the precursor concentration the size and dispersity could be reduced from 9.3 AE 3 nm to 3.7 AE 0.8 nm.
In this work we present a detailed study of flow technology approaches that could open up new possibilities for nanoparticle synthesis. The synthesis of gold and silver nanoparticles (NPs) in a flow device based on a coaxial flow reactor (CFR) was investigated. The CFR comprised of an outer glass tube of 2 mm inner diameter (I.D.) and an inner glass tube whose I.D. varied between 0.142 and 0.798 mm. A split and recombine (SAR) mixer and coiled flow inverter (CFI) were further employed to alter the mixing conditions after the CFR. The 'Turkevich' method was used to synthesize gold NPs, with a CFR followed by a CFI. This assembly allows control over nucleation and growth through variation of residence time. Increasing the total flow rate from 0.25 ml min to 3 ml min resulted initially in a constant Au NP size, and beyond 1 ml min to a size increase of Au NPs from 17.9 ± 2.1 nm to 23.9 ± 4.7 nm. The temperature was varied between 60-100 °C and a minimum Au NP size of 17.9 ± 2.1 nm was observed at 80 °C. Silver NPs were synthesized in a CFR followed by a SAR mixer, using sodium borohydride to reduce silver nitrate in the presence of trisodium citrate. The SAR mixer provided an enhancement of the well-controlled laminar mixing in the CFR. Increasing silver nitrate concentration resulted in a decrease in Ag NP size from 5.5 ± 2.4 nm to 3.4 ± 1.4 nm. Different hydrodynamic conditions were studied in the CFR operated in isolation for silver NP synthesis. Increasing the Reynolds number from 132 to 530 in the inner tube created a vortex flow resulting in Ag NPs in the size range between 5.9 ± 1.5 nm to 7.7 ± 3.4 nm. Decreasing the inner tube I.D. from 0.798 mm to 0.142 mm resulted in a decrease in Ag NP size from 10.5 ± 4.0 nm to 4.7 ± 1.4 nm. Thus, changing the thickness of the inner stream enabled control over size of the Ag NPs.
Synthesis of silver nanoparticles (NPs) in an impinging jet reactor (IJR) was investigated due to its unique properties of efficient mixing and lack of channel walls which avoid fouling. Silver NPs were formed at room temperature by reducing silver nitrate with sodium borohydride in the presence of sodium hydroxide. Two types of ligand were used to stabilize the NPs, trisodium citrate, and polyvinyl alcohol (PVA). Weber number, the ratio between inertial forces and surface tension forces, is used to characterize flow in impinging jets. Flow regimes were investigated for Weber numbers in the range of 13-176. A liquid sheet/chain regime was identified at lower Weber numbers (<90), and an unstable rim structure was identified at higher Weber numbers (>90). Mixing time was found to be in the range 1-7 ms, using the Villermaux-Dushman reaction system and interaction by exchange with the mean mixing (IEM) model. Fastest mixing occurred at Weber number ca. 90. Using trisodium citrate as a ligand, NP size decreased from 7.9 ± 5.8 nm to 3.4 ± 1.4 nm when flow rate was increased from 32 mL/min to 72 mL/min using 0.5 mm jets, and from 6.4 ± 3.4 nm to 5.1 ± 4.6 nm when flow rate was increased from 20 mL/min to 32 mL/min using 0.25 mm jets. Using PVA as a ligand, NP size decreased from 5.4 ± 1.6 nm to 4.2 ± 1.1 nm using 0.5 mm jets and stayed relatively constant between 4.3 ± 1 nm and 4.7 ± 1.3 nm using 0.25 mm jets. In general, the size of the NPs decreased when mixing was faster.
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