Poor solubility of high protein milk powders can be an issue during the production of nutritional formulations, as well as for end-users. One possible way to improve powder solubility is through the creation of vacuoles and pores in the particle structure using high pressure gas injection during spray drying. The aim of this study was to determine whether changes in particle morphology effect physical properties, such as hydration, water sorption, structural strength, glass transition temperature, and α-relaxation temperatures. Four milk protein concentrate powders (MPC, 80%, w/w, protein) were produced, i.e., regular (R) and agglomerated (A) without nitrogen injection and regular (RN) and agglomerated (AN) with nitrogen injection. Electron microscopy confirmed that nitrogen injection increased powder particles’ sphericity and created fractured structures with pores in both regular and agglomerated systems. Environmental scanning electron microscopy (ESEM) showed that nitrogen injection enhanced the moisture uptake and solubility properties of RN and AN as compared with non-nitrogen-injected powders (R and A). In particular, at the final swelling at over 100% relative humidity (RH), R, A, AN, and RN powders showed an increase in particle size of 25, 20, 40, and 97% respectively. The injection of nitrogen gas (NI) did not influence calorimetric glass transition temperature (T_g), which could be expected as there was no change to the powder composition, however, the agglomeration of powders did effect T_g. Interestingly, the creation of porous powder particles by NI did alter the α-relaxation temperatures (up to ~16 °C difference between R and AN powders at 44% RH) and the structural strength (up to ~11 °C difference between R and AN powders at 44% RH). The results of this study provide an in-depth understanding of the changes in the morphology and physical-mechanical properties of nitrogen gas-injected MPC powders.

The rehydration properties of original whey protein isolate (WPI_C) powder and spray-dried WPI prepared from either unheated (WPI_UH) or nanoparticulated WPI solutions were investigated. Nanoparticulation of whey proteins was achieved by subjecting reconstituted WPI_C solutions (10% protein, w/w, pH 7.0) to heat treatment at 90 °C for 30 s with no added calcium (WPI_H) or with 2.5 mM added calcium (WPI_HCa). Powder surface nanostructure and elemental composition were investigated using atomic force microscopy and X-ray photoelectron spectroscopy, followed by dynamic visualisation of wetting and dissolution characteristics using environmental scanning electron microscopy. The surface of powder particles for both WPI_UH and WPI_C samples generally appeared smooth, while WPI_H and WPI_HCa displayed micro-wrinkles with more significant deposition of nitrogen and calcium elements. WPI_H and WPI_HCa exhibited lower wettability and solubility performance than WPI_UH and WPI_C during microscopic observation. This study demonstrated that heat-induced aggregation of whey proteins, in the presence or absence of added calcium, before drying increases aggregate size, alters the powder surface properties, consequently impairing their wetting characteristics. This study also developed a fundamental understanding of WPI powder obtained from nanoparticulated whey proteins, which could be applied for the development of functional whey-based ingredients in food formulations, such as nanospacers to modulate protein–protein interactions in dairy concentrates.