Experimental study on tensioned‐web slot coating

Tensioned‐web slot coating (TWSC) technology was developed in the early 1980s and was considered an efficient method for thin liquid film coating. An experimental study was carried out to investigate the effects of several key parameters on the minimum wet thickness of TWSC. The experiment was performed on a pilot coater with dilute Newtonian poly(vinyl) alcohol (PVA) solutions as test fluids coating on polyethylene‐terephthalate (PET) substrates. It was found that the minimum wet thickness for TWSC was between 0.5 and 1.5 μm, which is much lower than that obtained using conventional slot die coating. The minimum wet thickness was proportional to the tension number T_N, which is defined as the ratio of fluid viscous force over web tension. Furthermore, on the basis of the experimental data, two additional dimensionless groups: dimensionless pressure P_N and dimensionless surface tension L_N were found to be relevant to the performance of TWSC. A universal correlation involving these dimensionless groups as well as the die geometry was used to predict the minimum wet thickness of TWSC. POLYM. ENG. SCI., 47:841–851, 2007. © 2007 Society of Plastics Engineers     

A macroscopic mathematical model for tensioned‐web slot coating

A mathematical model was developed to predict the performance of tensioned‐web slot coating (TWSC), in particular, the minimum wet thickness. The model was based on the lubrication approximation for the coating solution flow and a simplified membrane theory for the moving web. The theoretical predictions compared reasonably well with available experimental data. The effects of fluid viscosity, web tension, coating speed, and wrapping angle on the performance of TWSC were evaluated. An example was presented to illustrate how die lip design could be varied to improve its performance. POLYM. ENG. SCI., 2008. © 2007 Society of Plastics Engineers     

Process limits in two-layer reverse roll transfer

Reverse roll coating in which a thin single layer of liquid is applied onto a substrate has been used in industry for decades and has been extensively analyzed in the literature. Modern coatings, however, are often composed of more than one layer to improve the product performance and to reduce the manufacturing cost. Premetered methods such as slot, slide, and curtain coatings are typically used to produce such multilayer coatings. If the caliper of the substrate to be coated is not constant, then the coating gap and consequently the final film thickness deposited on the web will also be nonuniform. In this study, we focused on the use of reverse roll technique with slot die liquid delivery system to produce a uniform thin two-layer coating. The use of this coating technique to produce such a coating has not been previously explored. The liquid film surface as it is transferred from a rigid steel roll to a deformable urethane-covered roll was visualized to find out how the uniformity of the two-layer coating is affected by the speed ratio between two rolls, layers’ wet thicknesses, and liquid viscosities. The effect of these parameters on the ribbing frequency and amplitude was also investigated. The results show that in the two-layer coating, as in the single layer reverse transfer, there is a critical web speed above which ribbing occurs. The critical speed is determined by the bottom layer viscosity.     

Minimum wet thickness for double‐layer slide‐slot coating of poly(vinyl‐alcohol) solutions

A combined slide‐slot coating die, with the slide coating on top, was designed and built to investigate the double‐layer coating of poly(vinyl‐alcohol) solutions. The operating coating windows were examined as a function of flow rates and viscosities of the two coating layers. The top coating layer could be made much thinner as compared to the double‐layer coating so long as a stable thin film could be formed on the slide. A minimum wet thickness of the top layer was found to be as thin as 5 μm or less. A large viscosity ratio of the two layer solutions appears to be helpful in expanding the coating windows. Addition of a small quantity of polymer, such as carboxymethyl cellulose, can further enhance the coating speed and reduce the top layer thickness. A flow visualization technique was employed to observe the coating bead region. It was found to be easier to change the flow direction in the slide‐slot coating die than the double‐layer slot die, resulting in a more stable coating flow and much thinner top layer. POLYM. ENG. SCI., 45:1590–1599, 2005. © 2005 Society of Plastics Engineers.     

Comparison of vertical and horizontal slot die coatings

Comparison of vertical and horizontal slot coatings was carried out experimentally using aqueous glycerin solutions with varying viscosity on a laboratory‐scale slot coater. The maximum coating speeds achieved in vertical slot coating were found to be higher than those of horizontal slot coating for low‐viscosity solutions. The coating defects observed below the minimum wet thickness changed from ribbing to air entrainment at a critical solution viscosity of around μ = 75 mPa s. Above this critical viscosity, a lower minimum wet thickness was obtained for the horizontal coating but not for vertical coating. The difference between vertical and horizontal coating was mainly the length of the coating bead. The dimensionless minimum wet thickness was correlated as a function of Reynolds number. There existed three regions of minimum wet thickness depending on Reynolds number. Initially, the dimensionless wet thickness increased in the low Reynolds number region (Region I), then reached a plateau in the intermediate Re region (Region II), finally dropped off sharply in the high Re region (Region III). The boundaries of these three regions were identified by two critical Reynolds numbers, i.e., Re = 1 and 20. Only Regions I and II of the wet thickness could be found for horizontal coating, while mainly Regions II and III were obtained for vertical coating, depending on the viscosity of the coating solution. POLYM. ENG. SCI., 47:1927–1936, 2007. © 2007 Society of Plastics Engineers     

Knurl roll design for stable rotogravure coating

When a thin film of fluid is coated on a web by any type roll or spreader coater such that the fluid splits while in a divergent channel the resulting fluid surface is not smooth but is made up of ridges, running in the direction of coating. At production speeds (50 m/min and higher) there is a natura frequency of this fluid ribbing effect which is independent of the type of coater and fluid rheology, and depends only on the depth of the wet coat of transferred liquid. A study has been made to determine how this natural ribbing frequency is related to coating stability on a rotogravure coater with ruling mill knurled coating roll. It has been observed that many knurl rolls deposit a metastable fluid pattern on the web when the resulting fluid sur matches the knurl pattern of the roll. Under some coating conditions this resulting surface becomes unstable and the fluid is transferred to a conditio fewer ridges per cm, resulting in a non-uniform coated surface. It was found that to enhance stable transfer from the knurl grooves it is necessary to the knurl roll surface to match the natural fluid ribbing frequency. The farther the knurl line frequency deviates from the natural fluid ribbing frequ the more often the coating surface will become unstable.     

Start‐up of slot die coating

A flow visualization technique was employed to observe the start‐up of slot die coating. The effects of five variables, i.e., prewetting on the die surface, fluid viscosity, slot gap, coating gap, and die lip length on the start‐up time were investigated. Prewetting on the die surface can effectively reduce the start‐up time. Any variable that enlarges the steady‐state coating bead would increase the start‐up time. Therefore, increasing the fluid viscosity, coating gap, slot gap and decreasing the die lip length can be helpful in reducing the start‐up time. It was found that there exist four distinct modes for the establishment of steady‐state coating bead. The four distinct modes can be distinguished by a Reynolds number, which is defined as the ratio of the inertial force of the coating solution impinging on the moving web to the viscous force needed to pull the coating solution on the web. Comparison of the experimental observation with the theoretical prediction based on the commercial package Flow3D was also performed; the four modes can be found in the numerical simulations, the start‐up time computed to reach steady state is shorter. POLYM. ENG. SCI., 2009. © 2009 Society of Plastics Engineers     

Simulation of particle migration in free‐surface flows

The migration of particles in free surface flows using the diffusive flux model was investigated. As the free‐surface flows, a planar jet flow and a slot coating flow were chosen. The suspension was assumed to be a Newtonian fluid with a particle concentration dependent viscosity. The governing equations were solved numerically by the finite volume method, and the free‐surface problem was handled by the volume of the fraction model. The result shows that even though the velocity profile is fully developed and becomes flat, the particle distribution never reaches the uniform distribution for both of the cases. It is also shown that the die swell of the free jet is reduced compared to the Newtonian fluid and when the particle loading is 0.5, die contraction is observed. The change in die swell characteristics is purely due to particle migration since the suspension model does not show normal stress differences. © 2010 American Institute of Chemical Engineers AIChE J, 2010     

Model for the outer cavity of a dual‐cavity die with parameters determined by two‐dimensional finite‐element analysis

A coating die forms liquid layers of uniform thickness for application to a substrate. In a dual‐cavity coating die an outer cavity and slot improves flow distribution from an inner cavity and slot. A model for axial flow in the outer cavity must consider the ever‐present cross flow. A 1‐D equation for the pressure gradient for a power‐law liquid is obtained as a small departure from a uniform flow distribution and no axial flow. The equation contains a shape factor dependent on cavity shape, Reynolds number, and power‐law index. The shape factor for five triangular cavity shapes is obtained by finite‐element analysis and correlated for application to die design up to the onset of flow recirculation which arises at the junction of the cavity and outer slot. The performance of the combined cavity and slot is considered and the most effective design determined. © 2017 American Institute of Chemical Engineers AIChE J, 64: 708–716, 2018     

Coupled fluid‐particle modeling of a slot die coating system

This work seeks to develop a fundamental understanding of particle motion in the slot die coating process through studying the interaction of forces between particles, with the die walls and the fluid phase. Coupled computational fluid dynamics and the discrete element method is employed for evaluating the motion of individual suspended particles near moving surfaces in a complex three‐dimensional flow field, motivated by the flow of particle laden fluid in a slot die coating system, including the presence of free surfaces. Overall, the particles follow the flow streamlines and their final position in the coating depends on the initial entry region of the particles. Particles experiencing adhesion with each other agglomerate in the low velocity regions of the coating gap, and have long residence times near the edge of the die at the end of the feed slot in the coating gap. © 2016 American Institute of Chemical Engineers AIChE J, 62: 1933–1939, 2016     

Slot coating flows of non‐colloidal particle suspensions

Slot coating is used in the manufacturing of functional films, which rely on specific particle microstructure to achieve the desired performance. Final structure on the coated film is strongly dependent on the suspension flow during the deposition of the coating liquid and on the subsequent drying process. Fundamental understanding on how particles are distributed in the coated layer enables optimization of the process and quality of the produced films. The complex coating flow leads to shear‐induced particle migration and non‐uniform particle distribution. We study slot coating flow of non‐colloidal suspensions by solving the mass and momentum conservation equations coupled with a particle transport equation using the Galerkin/Finite element method. The results show that particle distribution in the coating bead and in the coated layer is non‐uniform and is strongly dependent on the imposed flow rate (wet thickness). © 2016 American Institute of Chemical Engineers AIChE J, 63: 1122–1131, 2017     

Rheological properties of poly(trimethylene terephthalate) in capillary flow

The shear viscosity, extensional viscosity, and die swell of the PTT melt were investigated using a capillary rheometer. The results showed that the PTT melt was a typical pseudoplastic fluid exhibiting shear thinning and extensional thinning phenomena in capillary flow. There existed no melt fracture phenomenon in the PTT melt through a capillary die even though the shear rate was 20,000 s^?1. Increasing the shear rate would decrease the flow activation energy and decline the sensitivity of the shear viscosity to the melt temperature. The molecular weight had a significant influence on the flow curve. The flow behavior of the PTT melt approached that of Newtonian fluid even though the weight‐molecular weight was below 43,000 s^?1 at 260°C. The extensional viscosity decreased with the increase of the extensional stress, which became more obvious with increasing the molecular weight. The sensitiveness of the extensional viscosity to the melt temperature decreased promptly along with increasing the extensional strain rate. The die swell ratio and end effect would increase along with increasing the shear rate and with decreasing the temperature, which represented that the increase of the shear rate and the decrease of temperature would increase the extruding elasticity of the PTT melt in the capillary die. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 705–709, 2005     

The effects of polymer additives on the operating windows of slot coating

An experimental study was carried out to investigate the effects of polymer additives on the operating windows of slot coating. Two polymer additives—carboxylmethylcellolose (CMC) and polyacrylamide (PAA)—were added to Newtonian glycerin solutions as test fluids. The flow experiment was performed on a lab coater. A flow visualization technique was employed to observe the shapes of coating beads. It was found that three types of defects appear at the lower bound of the operating window, i.e., ribbing, air entrainment, and break lines coupled with dripping. Adding a small amount of polymer additives has little effect on the operating window if the defect is ribbing, but it will expand the air entrainment region. The coating speed can be increased significantly if the defect is break lines coupled with dripping. Polym. Eng. Sci. 44:1970–1976, 2004. © 2004 Society of Plastics Engineers.     

Numerical simulation and experimental validation of liquid‐film‐flow characteristics in dip coating for non‐Newtonian fluids

The film‐flow problem in dip coating is simulated numerically for non‐Newtonian fluids based on Carreau–Yasuda (CY) and Herschel–Bulkley (HB) constitutive equations, with particular focus on coating‐film‐thickening phenomena and on the evolution of free surface and flow field under different sets of conditions. Finite element method (FEM) is combined with remeshing technique using a commercial code (Polyflow). Numerical predictions of the final film thickness and free surface for HB and CY fluids are successfully compared with experiments under the given conditions. Results show that the combination of FEM‐remeshing technique could be useful for dip‐coating design and optimization. Effects of coating fluid properties and withdrawal speed on film thickening and free surface shape and location are also discussed. Flow fields under different conditions are presented to analyze the evolution of the entire flow field and flow characteristics in detail. POLYM. ENG. SCI. 56:1070–1078, 2016. © 2016 Society of Plastics Engineers     

Rheology of plastisol formulations for coating applications

A plastisol is a suspension of PVC particles and mineral fillers in a liquid phase composed of plasticizer and adjuvants. Plastisol formulations are commonly used in coating processes for flooring application. In the knife‐over‐roll process, they are subjected to a wide range of shear rates (0–10⁵ s^?1). They are adjusted in order to fulfil the target end‐use properties but their processability depends on their rheology. Plastisol based on three PVC resins with or without mineral filler have been investigated using a Couette device and a capillary rheometer. Results show a high impact of PVC particle content, particle sizes and distribution on rheology: a polydisperse formulation displays a shear‐thinning behavior in the whole shear rates range and exhibits yield stress; a monodisperse formulation shows a shear thinning behavior at low shear rate, followed by a Newtonian plateau, then a more or less pronounced dilatancy peak depending on plasticizer rate and finally another shear‐thinning behavior; a bidisperse resin stands in between. Filler content also impacts the rheology: shear thickening effects at intermediate shear rates decrease or even disappear; however, the viscosity increase is important for low shear rates and depends on the filler particle size and particle size distribution. POLYM. ENG. SCI., 57:982–988, 2017. © 2016 Society of Plastics Engineers     

Particle migration and alignment in slot coating flows of elongated particle suspensions

We analyze slot coating flows of elongated particle suspensions and investigate particle concentration and average orientation at the coated film. Shear‐induced particle migration is described by the Diffusive Flux Model, and particle orientation is given by the principal direction of the particle conformation tensor. The conformation evolution and the constitutive equation for the resulting complex liquid are adapted from classical models that describe the behavior of suspensions of cylinders and fibers and polymeric solutions of almost rigid rod‐like molecules. The proposed fully coupled model is applied to slot coating flows, and is solved using the DEVSS‐TG/SUPG finite element method. The results show that the wet coated film is highly nonuniform. Particle concentration and orientation vary along the film thickness and are a strong function of the operating parameters of the process, such as the film thickness‐to‐coating gap ratio and the capillary number of the flow. © 2017 American Institute of Chemical Engineers AIChE J, 63: 3187–3198, 2017     

Operability coating windows and frequency response in slot coating flows from a viscocapillary model

Slot coating, indispensable to the manufacturer of flat panel displays and long-life secondary batteries, can be susceptible to unexpected disturbances at high speeds, leading to many kinds of undesirable defects. Operability coating windows for both Newtonian and non-Newtonian (shear-thinning) liquids have been investigated using a simplified viscocapillary model in a slot coating bead flow regime. Stable coating windows, free from leaking (or dripping) and bead break-up, have been determined by the position of upstream meniscus. They quantitatively coincided with those from two-dimensional calculations by a CFD Fluent solver. The pressure range that allowed a stable bead widened as the viscosity of the coating liquid or the capillary number in downstream die region increased. Also, the sensitivity of the slot coating flow through frequency response method was tested by measuring the amplitude of final wet coating thickness with respect to ongoing sinusoidal disturbances at different frequencies imposed to web speed, flow rate, bead pressure and coating gap. The viscocapillary model was compared with a 2D model and was found to be a fast and efficient tool that could enhance the productivity and processability of coating systems.     

Rheological properties,flow visualization and extrudate swell of NR compound by rotating‐die rheometer

An experimental apparatus coupled with a rotating die system was especially designed and manufactured to study the rheological properties, flow patterns and swelling behavior of natural rubber (NR) compound for different shear rates and die rotating speeds at a test temperature of 110°C, the results being compared with those by the static capillary die. It was found that NR compound used exhibited psuedoplastic non‐Newtonian behavior. The rotation of the capillary die could reduce the extrusion load. The wall shear stress for any given shear rates increased with increasing die rotating speed. The fluctuation of the entrance pressure drop increased with increasing die rotating speed. The flow pattern development in the rotating‐die rheometer was different from that observed in the static die. The flow patterns in the rotating die were clearly unstable and contained two flow components which included axial flow along the barrel and circumferential flow at the die entrance. The size and shape of the axial and circumferential flows were more dependent on the piston displacement. It was found that the swelling ratio of the NR compound decreased with increasing die rotating speed. POLYM. ENG. SCI., 2008. © 2008 Society of Plastics Engineers.     

Viscoelastic behavior of AN‐g‐casein copolymer concentrated solution of sodium thiocyanate

The viscoelastic behavior of sodium thiocyanate concentrated solution of graft copolymer of acrylonitrile onto casein (AN‐g‐casein) was investigated in detail by nitrogen pressure capillary rheometer. The experimental results show that the concentrated solution of AN‐g‐casein is a non‐Newtonian fluid of shear thinning. The end correction increases with the increase of shear rate. In the course of practical spinning, the real shear stress only attributes about 35% to the apparent shear stress, which confirms the essentiality of end correction for the capillary extrusion of the concentrated solution of the graft copolymer. By using the Dewitt model, the Couette correction ξ and recoverable shear strain S_R were analyzed and separated. Quantitative function relation of ξ and S_R versus shear rate and temperature were deduced. It is a common equation within the range of experiment. In practical spinning process, the real viscoelastic parameters can be easily predicted by only a piece of flowing curve based on the common equation. Real elastic model G under any shear rate in the range of experiment was calculated. It was found that G increases with an increase of shear rate, which is opposite to the conclusion reported by Hayahara. The main reason for the error may be that Hayahara used the same Couette correction at a higher shear rate. Further, the die swell in the spinning process can be estimated efficiently. The theoretical base for the stability of AN‐g‐casein spinning technology was provided. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 1721–1728, 2002; DOI 10.1002/app.10554     

Operability limits of slide coating

Slide coating is one of the pre-metered methods used for high precision single and multilayer coatings. The thickness of each liquid layers is set by the flow rate and web speed only and it is independent of other process parameters. The uniformity of the deposited layer, however, is affected by the operating conditions. In the design of coating processes, it is crucial to know the set of conditions at which the deposited layer is adequately uniform, i.e. to define the operability window of the process. We developed a theoretical model of slide coating flow by solving the full two-dimensional Navier–Stokes equations and used it to uncover the mechanisms of coating bead breakdown at low vacuum, high vacuum, and low flow limits. With full understanding of the bead breakup processes, we then constructed a theoretical coating window as a function of coating thickness, web speed, and applied vacuum. A simple stability criterion was used to predict the onset of ribbing instability and deployed to add the onset of ribbing limit inside the coating window.