Continuous synthesis of silver nanoparticles based on a polyol process was conducted using a microwave-assisted flow reactor installed in a cylindrical resonance cavity. Silver nitrate (AgNO(3)) and poly(N-vinylpyrrolidone) (PVP) dissolved in ethylene glycol were used respectively as a silver metal precursor and as a capping agent of nanoparticles. Ethylene glycol worked as the solvent and simultaneously as the reductant. Silver nanoparticles of narrow size distributions were synthesized steadily for 5 h, maintaining almost constant yield (>93%) and quality. The reaction was achieved within 2.8 s of residence time, although nanoparticles were not formed under this flow rate by conventional heating. A narrower particle size distribution was realized by the increased flow rate of the reaction solution. Nanoparticles of 9.8 nm average size with a standard deviation of 0.9 nm were synthesized at the rate of 100 ml h(-l).

We present a flow type single-mode microwave (MW) reactor that forms a uniform electromagnetic field along a tubular reactor (quartz glass, i.d. 1.5 mm × 100 mm) located in the center of a cylindrical MW cavity. The temperature of liquid flow in the reactor tube was controlled precisely by a resonance frequency autotracking function. This MW reactor system is useful for rapid heating of liquid flow at pressures up to 10 MPa. Continuous flows of polar solvents including water, ethylene glycol, and ethanol were heated instantaneously beyond their boiling points by application of pressure. Acceleration of the reaction was exemplified in continuous synthesis of Cu nanoparticles by elevation of the reaction temperature beyond the boiling point of solvent (ethylene glycol) at 2 MPa.

Continuous synthesis of Pd@Pt and Cu@Ag core-shell nanoparticles was performed using flow processes including microwave-assisted Pd (or Cu) core-nanoparticle formation followed by galvanic displacement with a Pt (or Ag) shell. The core-shell structure and the nanoparticle size were confirmed using high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) observation and EDS elemental mapping. The Pd@Pt nanoparticles with a particle size of 6.5 ± 0.6 nm and a Pt shell thickness of ca. 0.25 nm were synthesized with appreciably high Pd concentration (Pd 100 mM). This shell thickness corresponds to one atomic layer thickness of Pt encapsulating the Pd core metal. The particle size of core Pd was controlled by tuning the initial concentrations of Na2[PdCl4] and PVP. Core-shell Cu@Ag nanoparticles with a particle size of 90 ± 35 nm and an Ag shell thickness of ca. 3.5 nm were obtained using similar sequential reactions. Oxidation of the Cu core was suppressed by the coating of Cu nanoparticles with the Ag shell.

Continuous syntheses of carbon-supported Pd@Pt core–shell nanoparticles were performed using flow processes including microwave-assisted Pd core–nanoparticle formation.

Rapid and continuous synthesis of size-controlled platinum nanoparticles is achieved using a single-mode microwave flow reactor controlled with temperature feedback module. Platinum nanoparticles are synthesized within 2.8 s of residence time in glycerol and 1,3-propanediol having large dielectric dissipation factor and high solvent viscosity.