In situ monitoring of latex film formation by small-angle neutron scattering: Evolving distributions of hydrophilic stabilizers in drying colloidal films

The distribution of hydrophilic species, such as surfactants, in latex films is of critical importance for the performance of adhesives, coatings and inks, among others. However, the evolution of this distribution during the film formation process and in the resulting dried films remains insufficiently elucidated. Here, we present in situ (wet) and ex situ (dry) SANS experiments that follow the film formation of two types of latex particles, which differ in their stabilizer: either a covalently bonded poly(methacrylic acid) (PMAA) segment or a physically adsorbed surfactant (sodium dodecyl sulfate, SDS). By fitting the experimental SANS data and combining with gravimetry experiments, we have ascertained the hydrophilic species distribution within the drying film and followed its evolution by correlating the size and shape of stabilizer clusters with the drying time. The evolution of the SDS distribution over drying time is being driven by a reduction in the interfacial free energy. However, the PMAA-based stabilizer macromolecules are restricted by their covalent bonding to core polymer chains and hence form high surface-area disc-like phases at the common boundary between particles and PMAA micelles. Contrary to an idealized view of film formation, the PMAA does not remain in the walls of a continuous honeycomb structure. The results presented here shed new light on the nanoscale distribution of hydrophilic species in drying and ageing latex films. We provide valuable insights into the influence of the stabilizer mobility on the final structure of latex films

Influence of cooling rate on the precipitation kinetics of nanoscale isothermal omega-phase in metastable beta-Ti alloy, Ti-5Al-5Mo-5V-3Cr

In metastable β-Ti alloys, nanoscale isothermal ω-phase (ωiso) precipitates are regarded as the nucleation sites for the α strengthening phase. Here we investigate the precipitation kinetics of the ωiso precipitates as a function of cooling rate (air cooling and water quenching) after β-solutionising. A combined in situ small-angle neutron scattering (SANS) and electrical resistivity measurement approach was used during ageing of Ti–5Al–5Mo–5V–3Cr wt% (Ti-5553) alloy at 300 °C and 325 °C up to 8 h. The SANS modelling was consistent with ellipsoid shaped particles for the ωiso precipitates, for both air-cooled and water-quenched samples. The precipitates attained a maximum size (equatorial diameter) of ∼21 nm and ∼17 nm after 2 h and 4 h of ageing the water-quenched and air-cooled samples respectively. Although the air-cooled samples showed delayed nucleation in comparison to water-quenched sample, the volume fraction became approximately the same (∼11%) after ageing for 8 h. The average value of the activation energy for ωiso nucleation from the β-phase matrix was determined as 122 kJ mol−1 from electrical resistivity data using a modified Johnson-Mehl-Avrami-Kolmogorov (JMAK) model. The hardness increased with ageing time, with water quenching leading to a higher final value of hardness than air cooling