General Observations of Constant Flow Rate Filter Pressing

Consolidating powder compacts to a uniform and high particle packing density is a central aspect of ceramic processing. Experiments on the formation of powder compacts from slurries of differing properties and filter pressed under different conditions are presented. The influence of (1) piston velocity, (2) the solid content of the slurry, and (3) slurry viscosity are discussed. A simplified theory of nonuniform cake growth is developed. This theory is based on the assumption that the cake profile is time independent in a reference plane moving with the cake/slurry interface. Classical theory assumes uniform cake density, while more difficult finite element methods are required for calculating nonuniform cake growth conditions. This theory simplifies nonuniform cake consolidation mechanics and allows simple spread-sheet-type calculations on cake uniformity. Cake uniformity is an important goal in processing. Piston stress-displacement behavior can be reasonably simulated from the fundamental cake properties (permeability and yield curve). The inverse, estimating the fundamental cake properties from piston stress-displacement behavior, appears to provide only rough estimates of these characteristic parameters. The Kozeny-Carman equation appears to reasonably fit the permeability behavior of these filter cakes.     

A nonlinear control method for resin transfer molding

In performing permeability measurements on the fiber reinforced preforms typically used in the resin transfer molding (RTM) process, two types of fluid injection are commonly utilized: constant fluid pressure and constant fluid flow rate. The constant pressure condition is often enforced by placing the test fluid within a pressure pot and supplying a constant gas pressure, thereby forcing the fluid into the mold under a constant pressure. In the case of constant fluid flow rate, the fluid is often supplied by forcing a piston through a fluid-filled cylinder at a constant rate of displacement through the use of a press or Instron machine. This paper presents a nonlinear control method for providing constant flow rate RTM processes with a pressure pot solely through the use of a regulator. Computer simulations of the control examined the effect of various parameters on the ability to maintain constant flow rate. Rectilinear flow experiments were carried out to evaluate the theoretical development. Experimental results are in good agreement with the computer simulations. Both computer simulations and experiments show significant promise for the proposed control methodology.     

Experimental Evaluation of a New Flocculation-Filtration Model for Ceramic Shape Forming Processes

The effect of suspension rheology on the casting mechanics of 37 vol% aqueous silicon carbide slips was examined. Slip viscosities of 180, 120, 90, and 58 mPa.s were evaluated. The 58 mPa.s slip was considered to be fully deflocculated; the others were underdeflocculated to varying degrees. The fully deflocculated slip cast according to parabolic rate behavior, while the others cast at a faster than parabolic rate. Deviations from parabolic rate behavior were correlated with a nonuniform cake structure observed through ultrasound and mercury porosimetry measurements. The observed casting behavior was explained on the basis of a suspension flocculation-filtration model. From rheological measurements, it was found that flocculation of the SiC particles during casting in the underdeflocculated suspensions caused the local void volume within the forming cake to increase as a function of cake thickness. The fully deflocculated slip was rheologically stable, and therefore cast with a uniform microstructure.     

Consolidation Behavior of Flocculated Alumina Suspensions

The consolidation behavior of flocculated alumina suspensions has been analyzed as a function of the interparticle energy. Consolidation was performed by a centrifugal force field or by gravity, and both the time-dependent and equilibrium density profiles were measured by a gamma-ray absorption technique. The interparicle energy at contact was controlled by adsorbing fatty acids of varying molecular weight at the alumina/decalin interface. We found that strongly attractive interactions result in a particle network which resists consolidation and shows compressible behavior over a large stress range. The most weakly flocculated suspension showed an essentially incompressible, homogeneous density profile after consolidation at different centrifugal speeds. We also found a significant variation in the maximum volume fraction, φ_m, obtained, with φ_m∼ 0.54 for the most strongly flocculated suspension to φ_m∼ 0.63 for the most weakly flocculated suspension. The compresive yield stresses show a behavior which can be fitted to a modified power law. In this paper, we discuss possible correlations between the fitting parameters and physical properties of the flocculated suspensions.     

Application of a Two-Dimensional Computer Simulation to Cake Growth in Slip Casting with Complicated-Shape Gypsum Molds

A two-dimensional computer simulation method, developed by the authors using the method of finite differences, was applied to estimate the cake growth in slip casting of alumina with a triangular gypsum mold and a box-type gypsum mold with a convex bottom. The cake growth patterns, water penetration patterns, water flow rate distributions, and pressure distributions were simulated in the molds and/or cakes. The simulated cake growth patterns were in good agreement with those observed experimentally in both molds. Moreover, the cake growths could be well understood from the results of the water flow rate distributions in each case. The present method is applicable to cake growth simulation in slip casting with complicated-shape gypsum molds.     

Experimental Analysis and Modeling of Slip Casting

The filtration mechanics of slip casting is extended to account for the filtrate transporting the finer particles to the bottom of the cake. Scanning electron micrographs of alumina (Al₂O₃) green microstructures illustrate that a higher concentration of fine particles can accumulate at the bottom section of a cake. The rheological behavior of alumina suspensions with different solids loadings, particle-size distributions, and amounts of deflocculant is discussed. Slip-casting experiments demonstrate that the rheology of a suspension greatly affects the green density and growth rate of the cake.     

Gravitational drainage of compressible organic materials

A model was developed to simulate drainage of compressible particle suspensions, and study how cake compression and volumetric load influence the process. The input parameters were settling velocity, cake resistance and compressibility. These parameters were found using a new experimental method. Dextran‐MnO₂ particle suspensions were drained as these resemble organic waste slurries with respect to settling and compressibility. It was demonstrated that cake compressibility must be taken into account to obtain adequate simulations. This implies that pressurized filtration resistances cannot be used for drainage simulations. In the filtration step, a distinct increase of dry matter from top to bottom of the cake was observed. During the subsequent consolidation, the cake compressed and a uniform dry matter profile was found. The final dry matter content of the cake increased with feed concentration and volumetric load. The drainage time increased proportionally with feed concentration and, more importantly, proportionally with squared volumetric load. © 2010 American Institute of Chemical Engineers AIChE J, 2010     

Data Analysis and Modeling of Constant Pressure Batch Dewatering of Fine Particle Suspensions

The problems of data analysis and modeling of experimental constant pressure batch dewatering of materials forming compressible cakes are considered. Dewatering in these materials is typically completed in two stages, viz. cake formation and cake consolidation. A data representation method especially useful for determining the transition point between the filtration and consolidation stages, as well as for comparing accuracy of model predictions, is illustrated. It is shown that dewatering occurs via one of three qualitatively different pathways. A simplified model for engineering analysis of the process is presented. A time-invariant spatially uniform volume fraction of solids approximation is invoked in the cake formation stage. A time-dependent spatially uniform volume fraction of solids assumption is made in the cake consolidation stage. The two models contain four model parameters and have a common physical basis in Darcy's law. Interrelationships between key process parameters are determined and employed to predict the temporal evolution of dewatering in the cake consolidation stage as well as the end point of dewatering.     

Fluid Flow Model for Ceramic Tape Casting

The flow behavior of a ceramic slurry during tape casting is analyzed based on the principles of fluid dynamics. The fluid model yields explicit expressions for tape thickness as a function of viscosity, the pressure gradient, and the speed and geometry of the casting head. The theoretical predictions are verified by experiments using a perovskite slurry as the testing material. The results show that within the range of normal operating conditions a uniform tape thickness can be attained. Furthermore, it is feasible to maintain a high-speed casting operation without any deleterious effect on the tape quality.     

Rheology and pressure filtration of aqueous SiC suspensions of nanometer-sized bimodal particles

The consolidation behavior of mixed SiC particles (30 and 800 nm diameters) at pH 7 was examined using a developed pressure filtration apparatus at a constant crosshead speed of a piston. The addition of 30 nm SiC to 800 nm SiC changed the rheological properties of colloidal suspension from Newtonian to pseudoplastic flow through Bingham flow with increasing amount of 30 nm SiC. A phase transition from a well dispersed suspension to a flocculated suspension occurred when the applied pressure exceeded a critical pressure (ΔP_tc). The ΔP_tc value decreased with increasing amount of 30 nm SiC. The packing density of bimodal SiC particles was analyzed based on the partial molar volume of each powder. The larger particles were more densely packed than the smaller particles in the mixed powder compact.     

Investigations on the State of Water in a Flocculated Filter Cake

Abstract

The vacuum filtration of hematite slurries and flocculated hematite slurries with anionic, cationic, and nonionic polyacrylamides was investigated. Test results show that the flocculated filter cake generally contains higher residual water than the unflocculated cake. Measurements of flocculants adsorption on a hematite surface, zeta potential, and contact angle of the mineral surface were carried out; the filter cakes were analyzed with a microscope and image analyzer; and the structure of the filter cakes was studied from the viewpoint of fractal theory. The existence state of residual water in flocculated filter cake was discussed. It was pointed out why a flocculated filter cake generally has a higher residual moisture content.     

Processing defects and their relevance to strength in alumina ceramics made by slip casting

Al₂O₃ made by slip casting inherently contained the elongated and the spherical shaped defects. The pores of elongated shape were formed through the liquid flow during the casting process, since they were found in all slip cast specimens and not found in the spontaneously dried specimen where no rigorous flow of water happened. The formation of these defects was insensitive to the slurry properties. The origin of spherical pores was likely due to the entrapped air bubbles during de-airing procedure. Their removal by de-airing was easy for a dispersed slurry having a low viscosity, but difficult for a flocculated slurry of high viscosity. The Weibull's plots for the flexural strengths are essentially the same in the region of high strengths. Specimens made from the flocculated slurry contain a higher concentration of the spherical pores, and some of the resultant specimens have low strength. The lower strength of those ceramics has been ascribed to more detrimental defects, i.e. the spherical ones.     

Colloidal Processing of a Very Fine BaTiO3 Powder—Effect of Particle Interactions on the Suspension Properties, Consolidation, and Sintering Behavior

The relation between the suspension state and the rheological properties, the consolidation, and packing of a very fine (nanosized) BaTiO₃ powder has been investigated. The BaTiO₃ powder was suspended in a nonaqueous medium by adsorbing fatty acids and a polymeric dispersant, poly(12-hydroxy stearic acid), (PHS), at the BaTiO₃/decane interface. Calculated interparticle energies imply that the suspension with PHS adsorbed is colloidally stable, while the suspensions with oleic and octanoic acid can be characterized as weakly and strongly flocculated, respectively. Analysis of settling experiments and rheological measurements at high concentrations confirmed these characteristics. Pressure filtration resulted in nearly identical green body densities in spite of the differences in colloidal properties, but the preliminary sintering experiments and microstructural characterization showed that the strongly flocculated suspension displays a significantly retarded sinterability compared to the colloidally stable and the weakly flocculated suspensions. The absence of a correlation between green density and sintering behavior was explained by considering both the volume taken by the adsorbed fatty acids and the PHS polymer—which can be substantial for nanosized powders—and the state of the suspension. While a decrease in the thickness of adsorbed surfactant or polymer layer will enable a higher particle packing density, such a thin adsorbed layer results in a more strongly flocculated suspension which will resist dense packing. Hence, it is suggested that the green bodies of the colloidally stable and the weakly flocculated suspensions correspond to a relatively homogeneous, but loosely packed, green body microstructure. The strongly flocculated suspension results in a green body with a more inhomogeneous microstructure.     

Study of the filter cake formed due to the sedimentation of monodispersed and bidispersed particles using discrete element method–computational fluid dynamics simulations

This study aims to investigate the sedimentation and the consolidation of the packed bed/cake formed due to the monodispersed and bidispersed particles under different flow conditions. Mutual interactions between the bidispersed particles and the liquid are considered by using a polydispersed drag model. The attractive force is considered by using the JKR model. Sensitivity of the void fraction of a sedimented packed bed/cake due to particle–particle interaction parameters is studied. Furthermore, the effect of the fluid flow is analyzed by performing the simulations in two stages. In the first stage, packed bed/cake is formed by the sedimentation of the particles in the absence of the fluid forces and in the second stage flow through the packed bed/cake is simulated by using the CFD coupled with the discrete element method. Based on the simulations, correlations between the sedimented and the consolidated void fractions are developed. © 2019 American Institute of Chemical Engineers AIChE J, 65: 1294–1303, 2019     

Experimental analysis and numerical modeling of flow channel effects in resin transfer molding

Composite manufacturing by Liquid Composite Molding (LCM) processes such as Resin Transfer Molding involve the impregnation of a net‐shape fiber reinforcing perform a mold cavity by a polymeric resin. The success of the process and part manufacture depends on the complete impregnation of the dry fiber preform. Race tracking refers to the common phenomenon occurring near corners, bends, airgaps and other geometrical complexities involving sharp curvatures within a mold cavity creating fiber free and highly porous regions. These regions provide paths of low flow resistance to the resin filling the mold, and may drastically affect flow front advancement, injection and mold pressures. While racetracking has traditionally been viewed as an unwanted effect, pre‐determined racetracking due to flow channels can be used to enhance the mold filling process. Advantages obtained through controlled use of racetracking include, reduction of injection and mold pressures required to fill a mold, for constant flow rate injection, or shorter mold filling times for constant pressure injection. Flow channels may also allow for the resin to be channeled to areas of the mold that need to be filled early in the process. Modeling and integration of the flow channel effects in the available LCM flow simulations based on Darcian flow equations require the determination of equivalent permeabilities to define the resistance to flow through well‐defined flow channels. These permeabilities can then be applied directly within existing LCM flow simulations. The present work experimentally investigates mold filling during resin transfer molding in the presence of flow channels within a simple mold configuration. Experimental flow frot and pressure data measurements are employed to experimentally validate and demonstrate the positive effect of flow channels. Transient flow progression and pressure data obtained during the experiments are employed to investigate and validate the analytical predictions of equivalent permeability for a rectangular flow channel. Both experimental data and numerical simulations are presented to validate and characterize the equivalent permeability model and approach, while demonstrating the role of flow channels in reducing the injection and mold pressures and redistributing the flow.     

Influence of pressure on filtration of aqueous alumina suspensions

The dispersibility of colloidal alumina particles (median size 310 nm) was related to the surface potential, the solid concentration in a suspension and the pressure applied to the particles. The consolidation behavior of colloidal alumina particles with an isoelectric point pH 8.7 was examined using a developed pressure filtration apparatus at 1–10 MPa of applied pressure. The height of 7 or 20 vol% alumina suspensions at pH 3.0, 7.8 and 9.0 as a function of filtration time was fitted by a filtration model developed for a flocculated suspension rather than a traditional filtration model for a dispersed suspension. An increased pressure, a decrease of particle concentration and a porous microstructure of colloidal cake reduced the consolidation time of alumina suspension. The wet alumina compacts were significantly compressed during filtration but relaxed after the release of the applied pressure. However, the packing density of alumina compact after calcination at 700 °C was almost independent of the filtration pressure and controlled by the structure of network of alumina particles in a solution.     

One‐dimensional model of vacuum filtration of compressible flocculated suspensions

This work details the one‐dimensional modeling of the different processes that may occur during the vacuum filtration of compressible flocculated suspensions. Depending on the operating conditions of the applied pressure and the initial solids concentration relative to the material properties of the compressive yield stress and the effective capillary pressure at the air–liquid interface, the dewatering process undergoes a combination of cake formation, consolidation, and/or desaturation. Mathematical models for these processes based on the compressional rheology approach are presented and appropriate solution methods outlined. Results using customary material properties are given for different operating conditions to illustrate the three dewatering processes. This approach lays the theoretical basis for further work understanding two‐ and three‐dimensional effects during desaturation, such as cracking and wall detachment. © 2010 American Institute of Chemical Engineers AIChE J, 2010     

The Effect of Cook‐Off on the Bulk Permeability of a Plastic Bonded Explosive

Plastic bonded explosives when exposed to prolonged heating environments undergo a variety of changes that affect their bulk chemical, thermophysical, and mechanical properties. During slow heating conditions, referred to as cook‐off, the thermal behavior of the polymeric binder plays an important role in the transformations of these composite energetic materials. The recently introduced Darcian flow hypothesis for PBX‐9501 implies that, during preignition, temperature gradients will lead to pressure gradients which in turn will drive convection of decomposition gases throughout the explosive, thus affecting ignition time and location. Here, we focus on the cook‐off behavior of PBX‐9501 and investigate its effects on bulk permeability to gases produced as a result of thermal decomposition. The concept of Darcian convection through porous media is defined and illustrated in detail by the derivation of the governing equations for a permeameter. Based on a systematic analysis involving: 1) our current understanding about binder behavior as a function of temperature, 2) the physics of the gas permeameter apparatus, 3) the concept of liquid drainage by gas, and 4) the experimental record of four permeameter experiments with cooked PBX‐9501, we conclude that samples heated up to 186 °C were not permeable in the Darcy‐flow sense.     

Flow analysis of natural rubber in a capillary rheometer. 1: Rheological behavior and flow visualization in the barrel

Capillary rheometers have been widely used in the study of the rheological behavior of thermoplastics but their application to rubber has so far been limited. An investigation was therefore carried out to determine the effect of mastication and temperature on the rheological properties of natural rubber using a capillary rheometer. The flow of the rubber in the barrel of the capillary rheometer was observed at various test conditions such as die geometry, piston speed, and test temperature using layers of pigmented rubber compound, this involving the use of a split barrel system. It was found that the flow patterns in the barrel of the capillary rheometer used were very complex and were a function of piston displacement.     

Two-Dimensional Simulation of Cake Growth in Slip Casting

A two-dimensional computer simulation of cake growth was studied for the slip casting of alumina with a gypsum mold. Based on the Adcock and McDowall model, the method of finite differences was applied to the simulation, and numerical calculations were performed for the cake growth on the inside wall of a rectangular, box-type mold by using the cake-growth controlling parameters that were obtained experimentally. Good agreement was observed between the experimental and calculated cake growth in the vicinity of the boundary between the gypsum mold and the silicon rubber and at the rectangular corner of the gypsum mold. The present simulation method is expected to be useful for estimating cake growth on molds with complicated shapes in slip casting.