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The morphology and properties of particulate films formed upon evaporation of colloidal suspensions have various important technological applications in optical, electrical and medical fields1,2,3,4. Interestingly these dried colloidal films very often accompany spatially periodic cracks which can be of different morphologies1. Different evaporation techniques such as sessile drop evaporation5,6,7, drying under confinement8,9, vertical deposition10,11,12,13, etc, have been used to tailor and achieve different types of particulate films. Moreover, different model systems have been studied to understand the crack nucleation and their propagation during drying8,14,15,16. Allian and Limat8 studied the crack patterns by preparing colloidal films using directional drying of the suspension (confined between two glass plates) and found that crack spacing varies non linearly with the film height8. Sessile drop evaporation of suspension of spherical particles dried under isotropic drying conditions, mostly form particulate films with radial cracks. During the evaporation of sessile drop, the dispersed particles accumulate at the drop edge due to outward radial flow17. During this process, the stress develops in both radial (in the drying front direction) and perpendicular to radial direction (tangential direction to the sessile drop circumference). Finally, when the accumulated stress exceeds the critical value (σc) along a particular direction, the cracks appear perpendicular to that direction. It is commonly accepted that drying of a colloidal suspension leads to an increase in stress within the film and the moment it exceeds σc, the excess stress is released by virtue of crack formation. In isotropic evaporation, the dependence of crack morphologies on salinity of suspension14, size of the particle15, relative humidity16 and effect of substrate18 is well studied. Several analytical8,19 and computational models20,21,22 have been proposed to explain different crack morphologies as a function of film height and ordering of spherical particles in the film. However it is shown that these cracks can be suppressed by adding polymers thereby inducing depletion interaction23. But, the dependence of particle shape on the crack morphology is not addressed yet. The growing importance of particulate films consisting of shape anisotropic particles which often accompany cracks9,11 motivates us to investigate the correlation between particle shape and crack morphology.
In the present work, we study the morphology of the particle deposits and the resulting crack patterns by considering evaporation of sessile drops consisting of charged spherical (silica) and ellipsoidal (hematite) particles. Upon the evaporation of sessile drop on a solid substrate, ring like patterns similar to coffee ring is observed17. In such coffee-ring like particulate deposits, cracks are invariably formed. In case of suspension of spherical particles, cracks along the radial direction are observed in line with reported results and the crack morphology is attributed to the packing and ordering of particles24. For dispersions containing ellipsoid particles, we observed cracks in the form of concentric circles. In this report, we show the dependence of crack morphology on particle shape anisotropy apart from the particle ordering and their arrangements25. The direction of crack propagation is dictated not only by the direction of propagation of drying fronts but also by the particle self-assembly and the cracks propagate through a least resistance path26. The effects of particle concentrations and aspect ratios on crack morphologies are also studied.
In order to understand and investigate the effect of self-assembly/particle ordering on crack patterns, we have recorded scanning electron micrographs of the area near cracks, as shown in Fig. 3B. From SEM micrograph it is clear that, ellipsoidal particles are arranged in a closed packed structure with major axis of the particle parallel to the crack direction. A similar ordered arrangement of ellipsoidal particles in particulate films fabricated via convective and vertical deposition have been reported9,11. We have recently shown that the ordering and hence the particle arrangement in the film is dictated by particle surface charge11. The particle self assembly near the edge depends on the ratio of particle diffusivity length scale to the hydrodynamic length scale6. If this ratio is lower than one, the radial velocity of fluid is sufficiently low and particles reaching the contact line have enough time to arrange into ordered structures. Otherwise, the radial flow velocity is sufficiently high and the particles do not have enough time to reassemble and this leads to disorder arrangement near the edge. Marin et al. observed an order to disorder transition with spherical particles within the ring and the ordering increased with decreasing particle size6. In case of nano size ellipsoidal particles, the hydrodynamic torque exerted on the one end of a particle due to the radial fluid flow turns the particles parallel to the contact line27. It is evident from the SEM image that particles major axes are parallel to each other and their alignment is parallel to the crack direction. The optical microscopy and SEM images for dried droplets of colloidal dispersions hematite ellipsoids with aspect ratio 2.69, 3.73 and 6.3 are included in the supporting information.
During the final stage of drying, the tensile stress builds up within the film due to the compression of particle assembly as a result of capillary pressure. When the stress exceeds its critical value σc, the excess stress is released via the nucleation of cracks at the film surface. It is known that, for brittle materials, crack propagation occurs by breaking of bonds between the atoms29. Similarly, for particulate films the crack propagation can be considered as detachment of colloidal particles or breaking of the contact between the particles. An ordered array of spherical particles having isotropic packing density will not have any preferred fracture direction. In contrast for an ordered assembly of anisotropic particles the crack propagation will have a preferred direction depending on the particle ordering. Our experimental observations unambiguously reveal the well ordered and closed pack arrangement of ellipsoids in the dried ring. Two possible scenarios that lead to circular cracks (Fig. 5A) and cracks along radial direction (Fig. 5B) in a dried drop of dispersions of ellipsoids are shown schematically. The crack path in Fig. 5A is rather straight whereas the path in Fig. 5B is tortuous. That is, the energy required to activate cracks along the straight path is certainly lower than the tortuous path. Hence straight cracks always form first to release excess stress in the ordered film of ellipsoidal particles. The crack direction observed in our experiments (SEM image shown in Fig. 3) is parallel to the major axis of ellipsoid which is similar to Fig. 5A. It is also evident from our experiments that the ordering of ellipsoids dictates the crack orientation. Similar experimental observations are reported for composite materials earlier26. In the past, several models are proposed where the cracks patterns are explained using bead-spring model in dense particulate films. Richardi et al. have shown through both simulation and experiments that ordering of particles leads to formation of ordered cracks30. 350c69d7ab