“…Here, we want to note that our larger CS microgels seemed to be under the effect of gravitational settling during the DLS measurements, which could be the reason for their higher polydispersities (or overestimation of polydispersity) compared to the smaller microgels. Although the commonly quoted upper size limit for DLS is around 10 μm, it often is only achievable by increasing the viscosity of the continuous phase or by using capillary DLS [ 25 , 26 ]. In this study, however, we do not further discuss the matter and report the D h values as recorded and used for the calculation of δ.…”
Micron-sized hard core-soft shell hybrid microgels are promising model systems for studies of soft matter as they enable in-situ optical investigations and their structures/morphologies can be engineered with a great variety. Yet, protocols that yield micron-sized core-shell microgels with a tailorable shell-to-core size ratio are rarely available. In this work, we report on the one-pot synthesis protocol for micron-sized silica-poly(N-isopropylacrylamide) core-shell microgels that has excellent control over the shell-to-core ratio. Small-angle light scattering and microscopy of 2- and 3-dimensional assemblies of the synthesized microgels confirm that the produced microgels are monodisperse and suitable for optical investigation even at high packing fractions.
“…Here, we want to note that our larger CS microgels seemed to be under the effect of gravitational settling during the DLS measurements, which could be the reason for their higher polydispersities (or overestimation of polydispersity) compared to the smaller microgels. Although the commonly quoted upper size limit for DLS is around 10 μm, it often is only achievable by increasing the viscosity of the continuous phase or by using capillary DLS [ 25 , 26 ]. In this study, however, we do not further discuss the matter and report the D h values as recorded and used for the calculation of δ.…”
Micron-sized hard core-soft shell hybrid microgels are promising model systems for studies of soft matter as they enable in-situ optical investigations and their structures/morphologies can be engineered with a great variety. Yet, protocols that yield micron-sized core-shell microgels with a tailorable shell-to-core size ratio are rarely available. In this work, we report on the one-pot synthesis protocol for micron-sized silica-poly(N-isopropylacrylamide) core-shell microgels that has excellent control over the shell-to-core ratio. Small-angle light scattering and microscopy of 2- and 3-dimensional assemblies of the synthesized microgels confirm that the produced microgels are monodisperse and suitable for optical investigation even at high packing fractions.
“…The rate at which the particles diffuse is exquisitely sensitive to forms of particle motion other than diffusion, such as gravitational settling and bulk thermodynamic fluid flow in the thermally controlled cuvette. A careful analysis of the different relaxation times in the time-correlated data [1], failed to reproduce the timescales typically associated with gravitational settling, the uncertainty long assumed to be the limiting factor for the upper size limit of DLS measurements. Convective motion within the capillary cell was carefully modelled using ANSYS and the timescales associated with convective motion were identified in the correlogram.…”
Section: Methods Detailsmentioning
confidence: 99%
“…Capillary DLS seeks to suppress the convective motion within the sample, whilst maintaining excellent thermal control of the sample by conduction, with good thermal contact between a metal capillary holder and capillary outer surface, over the length of the capillary. It was discovered that 1.00 mm × 1.00 mm was an optimum size for the square capillary internal cross section [1] as a balance between the need to suppress the convective motion and reduce the sample volume, with the need to be able to reproducibly mount and align the capillary with the optical path within the instrument. The capillaries used in this work are 50 mm in length making them easy to handle, however, the 1.0 mm × 1.0 mm aperture means that care is needed in loading the sample into the capillary bore.…”
Nanomaterials are used in a wide range of applications bringing completely new properties to a material or considerable improving pristine material property. In the medical domain where they are named nanomedicines, their usefulness was found to resolve drug delivery challenges and to improve performances of imaging-based diagnostic methods. Some carry activity on their own giving birth to new types of medicines. Whatever the application of the nanomaterial is for, a quality assessment is needed to ensure the repeatability and efficiency of industrial processes and in turn activity and safety of the product. This chapter was aimed to discuss the characterization of physicochemical parameters that can be used to define a nanomaterial. It gives basis in metrology and explains how it can be used to develop validated procedures for the characterization of the main physicochemical parameters that define NMs including their transfer to be used in many laboratories. Examples discussed in the chapter include the measurement of the size of NMs, the evaluation of the size distribution and of the zeta potential. The development of validated procedures for the characterization of NM is in its infant ages facing challenges that are discussed in this chapter.
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