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Crack formation is a frequent result of residual stress release from colloidal films made by the evaporation of colloidal droplets containing nanoparticles. Crack prevention is a significant task in industrial applications such as painting and inkjet printing with colloidal nanoparticles. Here, we illustrate how colloidal drops evaporate and how crack generation is dependent on the particle size and initial volume fraction, through direct visualization of the individual colloids with confocal laser microscopy. To prevent crack formation, we suggest use of a versatile method to control the colloid-polymer interactions by mixing a nonadsorbing polymer with the colloidal suspension, which is known to drive gelation of the particles with short-range attraction. Gelation-driven crack prevention is a feasible and simple method to obtain crack-free, uniform coatings through drying-mediated assembly of colloidal nanoparticles.

Colloidal suspensions, where colloids or nanoparticles are uniformly suspended in a solvent, are widely used in industry. A drying process is usually adopted to deposit the colloids on a solid surface, allowing fabrication of thin colloidal films1. Drying-mediated assembly of colloidal nanoparticles2 is a cutting-edge technology. However, cracking of the dried colloidal films frequently takes place, particularly for those made from nanoparticle suspensions3,4,5,6,7,8,9,10,11,12, which can thus cause critical problems for application. Prevention of cracking is a significant task to improve the quality of colloidal films containing nanoparticles13,14, as well as to increase the applicability of large-area, highly ordered and crack-free colloidal films15.

A variety of feasible methods for crack prevention have been suggested to date. For example, avoidance of cracking had been achieved through use of subsequent depositions of thin crack-free nanoparticle layers13, addition of hydrogels to suspensions to reduce their capillary pressures16, variation of the pH17 or addition of inorganic particles18 to control suspension flocculation, addition of a sol-gel glue19 or a sol-gel precursor15, addition of emulsion droplets to modulate suspension viscosity14 and use of organic colloids20 to enhance the fracture resistance of sol-gel coatings. Some examples of polymer addition for prevention of cracks can also be found in ceramic materials (for review, see21): polymers are added as binders into clays to increase fracture resistance22, which is an industrial tradition23, while poly(vinylalchohol) was found to reduce cracking in colloidal alumina24 and a variety of soft components, including polymers, soft spheres and glycerol, were reported to increase fracture resistance in mixtures with colloids25. However, despite the many attempts which have been made to prevent cracking, a simple and highly versatile method that utilizes well-known and well-controlled physics, such as gelation, is still required to allow more effective elimination of cracking in various colloidal suspensions.

The three evaporation stages could clearly be identified through confocal laser microscopy and use of fluorescent-dyed colloidal particles, as demonstrated in Fig. 1c. In particular, each stage was distinguishable owing to differences in the fluorescence intensities among the air, solvent and colloids. Confocal microscopy has widely been used for the direct observation of real-space motions of individual colloids29. A confocal laser microscope is a laser scanning optical microscope that utilizes a fluorescent technique36. With this approach, we are able to directly investigate crack initiation and growth dynamics. A similar approach was used in recent reports for crack studies14,37. Confocal microscopy is also useful for studies on evaporation gradients38, as well as on evaporative lithography39.

In conclusion, we demonstrated that cracking is an intrinsic and inevitable phenomenon for colloidal films made with hard sphere-like small colloids or nanoparticles (with radii at the nanoscale). We directly visualized the generation of cracks during evaporation of colloidal droplets using confocal laser microscopy and standard colloidal suspensions, with fluorescent-dyed colloids. From direct tracking of the individual colloids via confocal microscopy, we confirmed the critical effects of the particle size and initial concentration on crack formation. For versatile crack prevention, we demonstrated the gelation-mediated crack prevention that enabled us to obtain uniform, crack-free coatings through drying-mediated assembly of colloidal nanoparticles. This crack prevention method would be useful to obtain crack-free uniform colloidal films for inkjet printing, paints, coatings and ceramics.

We demonstrate the positive feedback between charge heterogeneity and intergranular fracture in an NMC secondary particle. Four different constant-concentration boundary conditions in each quarter domain of the particle surface are prescribed to mimic the variation of Li access at different sites of the NMC secondary particle. These approximated boundary conditions naturally induce a global heterogeneity of SoC in the NMC secondary particle. This setting is a simplification of the electrochemical condition at the surface of the NMC secondary particle in contact with the liquid electrolyte, binders, and conductive matrix. The actual surface concentration can be determined by solving the Butler-Volmer equation with an appropriate overpotential profile on the particle surface. To capture the local charge heterogeneity facilitated by intergranular fracture, we couple the diffusion kinetics and damage evolution in the way that Li concentration at the newly formed crack surfaces are set to be the external Li concentration. This is a good replication of the experimental observation that the liquid electrolyte can quickly penetrate into the cracked surface of NMC particles and segregates along the grain boundaries30.

In this work, we present a direct visualization of the structural and chemical complexity throughout a single NMC811 secondary particle with the combination of nano-resolution X-ray probes in both soft and hard X-ray regimes correlatively. It is observed that the degree of the lattice reconstruction effect is inhomogeneous over the particle surface. More importantly, the regions with higher porosity are associated with more severe surface lattice reconstructions, which suggests a mutual modulation between the surface chemistry and the bulk microstructure. Our FEM results further shed some light on the underlying interplay among the charge heterogeneity, bulk fracture, and surface passivation at the single-particle level. This work presents a fundamental understanding of the coupling effect between the surface chemistry and the bulk microstructure. Such a surface-to-bulk correlation highlights that both crack mitigation and surface modification are key points that shall be considered in an integrated manner for the design of the next-generation cathode materials for LIBs industry. The herein developed correlative nano-resolution imaging method (with both hard and soft X-ray probes) not only paves a new way toward more comprehensive understanding of LIBs material, but also will have profound impacts on a broad range of scientific fields well beyond battery research. We also point out that the battery cathodes are composed of many particles. While the current study has a strong focus on the single-particle level structural and chemical complexity and the intercoupling, a follow-up study of many particles is highly desirable for the electrode level statistical significance. We also clarify that the presented experimental results are at a static state. While the chemical heterogeneity within NMC particles can persist even after long term relaxation of the material and can be utilized as fossil evidence for our investigation of the surface-to-bulk correlation4, we acknowledge the importance of utilizing in situ and/or operando methods for studying the dynamic aspect of the reaction experimentally31,32,33. Our study focuses on the surface-to-bulk correlation, which involves a complicated experimental procedure that sets a practical limitation in our experiment. Significant efforts will be needed in the follow-up research in this direction.

Fluid Catalytic Process, also introduced in 1942, offered an excellent integration of the cracking reactor and the catalyst regenerator that provides the highest thermal efficiency, as shown in Figure 7.7. In FCC, a fluidized-bed (or fluid-bed) of catalyst particles is brought into contact with the gas oil feed along with injected steam at the entrance (called the riser) of the reactor. The hot catalyst particles coming from the regenerator unit evaporate the feed gas oil upon contact in the riser, and the cracking starts as the gas oil vapors and the catalyst particles move upward in the reactor. The temperature of the catalyst particles drops as the evaporation of gas oil and endothermic cracking reactions proceed during the upward movement. Cracking reactions also deposit a significant amount of coke on the catalysts, leading to the deactivation of the catalyst. After removing the adsorbed hydrocarbons by steam stripping, the coked catalyst is sent to the regeneration unit to burn off the coke with air. Heat released from burning the coke deposit increases the temperature of the catalyst particles that are returned to the riser to complete the cycle. Burning off the rejected carbon (coke) in the regenerator provides the energy necessary for cracking without much loss, thus increasing the thermal efficiency of the process. The cracking products are sent to the fractionator for recovery after they are separated from the catalyst particles in the upper section of the reactor [3]. 2ff7e9595c