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This study presents an approach for targeted comminution of component mixtures within a wet-operated stirred media mill. In the first step, a general understanding of the interactions between individual components on the grinding result with mixtures could be gained with basic experiments and following our former research work. In particular, a protective effect of the coarser particles on the fines could be elucidated. These findings were used to develop a process for the production of a battery slurry containing fine ground silicon particles as well as dispersed carbon black and graphite particles. By a tailored sample preparation applying a combination of particle dissolution and separation, the particle size distributions of carbon black and graphite particles were analyzed separately within the produced battery slurries. Based on the selective particle size analysis, the slurry preparation could be transferred from a complex multistage batch process using a dissolver to a stirred media mill, which was finally operated in a continuous one-passage mode. The prepared slurries were subsequently further processed to silicon-rich anodes using a pilot scale coating and drying plant. Afterward, the produced anodes were electrochemically characterized in full cells. The cell results prove a comparable electrochemical behavior of anode coatings derived from a dissolver- or mill-based slurry production process. Therefore, we could demonstrate that it is possible to integrate the mixing process for the production of multicomponent slurries into the comminution process for the preparation of individual materials upstream. Even with nearly identical starting sizes of their feed materials, the targeted particle size distributions of the single components can be reached, taking into account the different material-dependent particle strengths and sequential addition of single components to the multicomponent comminution process.
Wet-operated stirred media mills are commonly used in the field of fine and ultra-fine grinding. Depending on the application, there are different mill geometries, sizes and mill equipment materials of which the grinding chamber lining and the stirrer are made. Increasing energy prices demand an energy-efficient mill operation for a desired product, which can be achieved with mechanistic stress models. Here, besides the mill geometry and volume, the process parameters and various energy-transfer-coefficients are of importance. In this work, the impact of different mill equipment materials affecting the mill-related-energy-transfer-coefficients on performance prediction and scale-up using the advanced stress model are investigated. It was found that the mill-related-energy-transfer-coefficients as well as the improved grinding-media-energy-transfer-coefficients have a significant effect on the prediction precision of the comminution times and specific energies for chosen target particle sizes.
The choice of stabilizers to prevent particle agglomeration during nanomilling is an elaborate process which is often based on empirical rules and experience. Usually, extensive screening studies are required to find an appropriate stabilizing additive. The present study shows how the selection of polymeric stabilizers can be narrowed down to a couple of additives based on Hansen solubility parameters. The stabilizing capability was found to be a function of the difference between solubility parameters of additive and particulate species. Solubility parameters of different additives and two particle species were determined by inverse gas chromatography and the stabilization performance was evaluated by nanomilling experiments conducted with a stirred media mill. It is shown that a certain difference of solubility parameters between particle and additive is necessary in order to provide colloidal stability of small particles after milling. On the one hand, the additive needs a certain affinity to the particle surface, while on the other hand it also has to be compatible with the solvent. Based on experimental data, a solubility parameter difference in the range of 7.5–10 MPa0.5 was identified as a good measure for a proper stabilizer selection. The approach was proved for two organic particle species and represents a promising tool for a more efficient formulation development of drug nanosuspensions.
Particle size characterization of heterogeneous mixtures is a challenging task, as it is not feasible to assign the measured signals to the individual components. Within this framework, the study proposes a method that applies the working principle of differential centrifugal sedimentation (DCS) in order to simultaneously separate and measure the denser component within a binary material mixture of submicron particles. The method was validated using a model system consisting of polyvinyl chloride (PVC) and diamond particles in a size range of 0.5 – 1.5 µm. The results proved that by applying a proper density gradient fluid, the diamond particles can be selectively analyzed by hindering the sedimentation of the lighter PVC component. Furthermore, a very promising application could be found with respect to wet fine grinding processes in stirred media mills. In fact, the approach was utilized to individually determine the particle size distribution of the grinding media wear within an ultrafine organic product. Despite the low quantity of wear particles, it was possible to separate them from the organic product under appropriate density conditions. The size distributions of both the wear and the product particles were validated with SEM images, confirming the feasibility of the method.
Wet-operated stirred media mills are commonly used in the field of fine and ultra-fine grinding. Depending on the application, there are different mill geometries and mill equipment materials of which the grinding chamber lining and the stirrer are made. Polyurethane and ceramics are frequently implemented materials. Besides the process-relevant effects such as cooling and wear prevention, an energy efficient mill operation is intended, which can be achieved, by using mechanistic stress models. Here, besides the mill geometry, the process parameters, various energy-transfer-coefficients are also determined. In this work, the effect of different mill equipment materials on the mill-related-energy-transfer-coefficient are investigated by experiments while operating different mills only with water and grinding media but without feed material. It was found that the mill equipment material has a significant effect on the power consumption and thus, the energy transfer within the mill as a result of friction between different materials.
This study presents a simple but effective process route for the production of transparent coatings on glass substrates from inorganic pigment goethite. For this purpose, coating suspensions were prepared by wet milling with a stirred media mill. A water/ethanol mixture was used as the liquid medium to take advantage of the resulting low surface tension for the coating process. In this manner, stable suspensions with particles of down to 50 nm in size were obtained, which already showed a significant increase in transparency. With regard to grinding characteristics, particularly low stress energies proved to be energetically reasonable. The coating step was performed by wet film deposition, achieving coating thicknesses in a range of 0.5–2.5 µm via dip coating. Highly transparent coatings were obtained by applying small particles of 50 nm, which exhibited a significantly lower scattering loss of light (≈3%) in comparison to particles of around 300 nm (70–80%). Additionally, the film color could be adjusted through a variation of the drying temperature due to a conversion of goethite to hematite by dehydration. Since transparency was not affected, this provides an easy-to-implement process adaptation for controlling coating colors.
Effects of axial grinding media distribution on the disc wear behavior of a stirred media mill
(2022)
Stirred media mills are commonly used process units for wet fine grinding and dispersing. During operation the grinding media and the feed material can cause wear to the process units of the stirred media mill. One typical representative of horizontal stirred media mills is the IsaMillTM, in which an internal classifier diverts the grinding media away from the discharge and implies a counteracting current force to the drag forces caused by the suspension flow. In this work, the disc wear of a pilot scale horizontal mill was investigated with regard to the axial grinding media distribution and other process parameters. In order to create quickly and well visible disc wear patterns, manufactured aluminum discs instead of the original polyurethane discs were specially used. For each set of operating parameters, a separate new pair of discs was installed. A radiometric densitometer was installed to measure the axial grinding media filling degree lengthwise to the M4 IsaMillTM. This method allows the determination of the local filling degree by correlation of the attenuation of gamma radiation from a Cs137 nuclide. The experiments showed that the disc wear per energy input increases with rising stress energy. With respect to the axial grinding media distribution, higher wear rates were observed in areas of increased grinding media filling ratios. As a result, it can be stated that the wear is a function of the local grinding media distribution and of the stress energy. In zones with a higher local grinding media filling degree, an increased disc wear is evident. Consequently, mills on a production scale could theoretically realize longer plant operating times and lower maintenance costs by securing a more homogeneous grinding media distribution.
The ancient inorganic pigment Egyptian Blue is a fluorophore with outstanding near-infrared (NIR) performance and is thus considered as an emerging optical material that meets the current demand for cheap, efficient, and nontoxic NIR nanofluorophores. Herein, we present a protocol for the quick mass production of Egyptian Blue (CaCuSi4O10) nanosheets (EBNSs) with lateral size down to ∼100 nm by applying state-of-the-art ball-milling techniques. A systematic decay of the NIR photoluminescence behavior with decreasing size of the EBNSs was found, which challenges the desired application of EBNSs as bioimaging markers and other nanoapplications. To pave the way to surface modifications of EBNSs, we deposited a thin layer of silica on the surface of the EBNSs. Taking advantage of this modification, we subsequently performed surface-initiated reversible addition–fragmentation chain transfer (RAFT) polymerization in order to grow both hydrophilic and hydrophobic polymer brushes from EBNSs, which enhanced dispersibility of the nanosheets and even delivered function. By matching the refractive index of the EBNS with its polymer shell, the quality of the NIR photoluminescence of the EBNS could significantly be improved, since disturbing light scattering at the interface could effectively be suppressed. Our results provide a clear picture of the advantages and limitations of EBNSs as optical nanomaterials for NIR fluorescence applications.
Lithium-ion batteries (LIBs) provide the largest source of electrical energy storage today. This paper covers the use of comminution processes and, thus, crushers and mills for particle breakage and dispersing, as well as classifiers for particle separation within the process chain, from the raw material to the final lithium battery cell and its recycling at end of life. First of all, the raw materials for the active material production have to be produced either by processing primary raw materials, or by recycling the spent lithium batteries. The end-of-life battery cells have to be shredded, the materials separated and then milled in order to achieve the so-called black mass, which provides a secondary material source with very valuable components. Using these materials for the synthesis of the cathode active materials, milling has to be applied in different stages. The natural graphite, increasingly used as anode material, has to be designed in mills and classifiers for achieving targeted properties. Nanosized silicon is produced by nanomilling using stirred media mills as a primary option. Conductive additives for LIBs, like carbon black, have to be dispersed in a solvent with machines like planetary mixers, extruders or stirred media mills. In the future, mechanochemical synthesis of solid electrolytes will especially require additional application of comminution processes.
A grinding technology should consider the physical properties of the material, i.e., size, shape, which have effects on the product specifications, i.e., quality, strength or overall process efficiency. In this respect, this study aimed at evaluating the variations in the shape of product size distribution of a stirred media mill as the attention on this technology has been growing in the recent years. Within the scope of the research, series of grinding tests were performed at different operating conditions, i.e. bead size, bead type, tip speed, feed rate and mill design, with a laboratory scale continuously operated horizontal stirred media mill. The investigations proved that the use of coarser and denser beads as well as adjusting higher tip speeds resulted in obtaining narrower product size distribution for the same mean size. For a better understanding of the process, the stress energy and mean residence time evaluations were also undertaken. It was found that the stress energy and its normalization with the mean residence time are directly proportional to the slope of the distributions. As a conclusion, the dry stirred media mill is able to adjust the shape of the distribution, which may be beneficial regarding to the mechanical properties of the end products (cement manufacturing) or efficiency of the mineral beneficiation processes.