Featured Application: A unique set-up for real-time monitoring of the size of nanoparticles during bottom-up liquid phase synthesis is presented in this article. The analysis method applied to study the size of dispersed nanoparticles during synthesis is dynamic light scattering (DLS). In contrast to conventional DLS, the DLS set-up presented in this article comprises a modulated 3D cross correlation geometry, and therefore allows accurate measurements of particle size in flow at flow rates of at least up to 17 mL·min −1 . This is essential for obtaining real-time information on the size of the dispersed nanoparticles. The DLS system could be connected to reactors of various sizes using the analysis loop presented in this article, which is coupled to a flow cell in the DLS set-up. Thus, the DLS set-up presented here is suited to study the nucleation and growth of nanoparticles in dispersion, facilitates a rational scale-up, and allows intervention in the production process of nanoparticle dispersions to minimize the number of off-spec batches.Abstract: To tailor the properties of nanoparticles and nanocomposites, precise control over particle size is of vital importance. Real-time monitoring of particle size during bottom-up synthesis in liquids would allow a detailed study of particle nucleation and growth, which provides valuable insights in the mechanism of formation of the nanoparticles. Furthermore, it facilitates a rational scale-up, and would enable adequate intervention in the production process of nanoparticle dispersions to minimize the number of off-spec batches. Since real-time monitoring requires particle size measurements on dispersions in flow, conventional dynamic light scattering (DLS) techniques are not suited: they rely on single scattering and measure the Brownian motion of particles dispersed in a liquid. Here, we present a set-up that allows accurate measurements in real-time on flowing dispersions using a DLS technique based on modulated 3D cross-correlation. This technique uses two simultaneous light scattering experiments performed at the same scattering vector on the same sample volume in order to extract only the single scattering information common to both. We connected the reactor to a flow-cell in the DLS equipment using a tailor-made analysis loop, and successfully demonstrated the complete set-up through monitoring of the size of spherical silica nanoparticles during Stöber synthesis in a water-alcohol mixture starting from the molecular precursor tetraethyl orthosilicate.
Here, we report a continuous flow synthesis of nano LDH, comprising a continuous precipitation process using static mixers and followed by an immediate cleaning process via a semi-continuous centrifuge to obtain the final product in one-go. Via this synthesis setup, it is possible to independently vary the concentrations of the reactants during precipitation and at the same time ensure constant reaction conditions and an immediate “quenching” of the precipitate due to “on the flow”-washing. We found that this paves the way to adjust the synthesis parameters in a way that the final morphology of the nano-LDH particles can be controlled to be either round or platelet-like
This paper describes experimental measurement results for photonic crystal sensor devices which have been functionalized for gas sensing applications. The sensor consists of a two dimensional photonic crystal etched into a slab waveguide having a refractive index of 1.7-1.9. Test devices were fabricated from SiON material on silicon / silicon dioxide platform, and also in polymer materials on silicon platform. The inorganic photonic crystals were made using direct write electron-beam lithography and reactive ion etching. The polymeric devices were made by nano-imprint lithography using the SiON structure as the imprint master. The high refractive index polymer was composed of a TiO 2 -UV resin nanocomposite having a nanoparticle fraction between 50 and 60 wt%. This resulted in a tunable refractive index between 1.7 and 1.85. Devices were functionalized for gas sensing applications by coating the surface with a chemical receptor. This responsive layer reacts with the target gas and changes its refractive index. This change causes the angle of out-coupling to change slightly. In this paper we report successful detection of formaldehyde in air at sub ppm levels, and discuss details of chemical functionalization of the PC sensor.
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