Effects of trapped air bubbles on frequency responses of the piezo-driven inkjet printheads and visualization of the bubbles using synchrotron X-ray

The reliability of drop formation is one of the key factors for the successful commercialization of inkjet printing applications. However, when the air bubble is entrapped from the nozzle exit, it leads to stop jetting of the droplets immediately. It has been known that the trapped air bubbles inside the chamber prevent a printhead from stable jetting. In this study the synchrotron X-ray has been used to visualize the air bubbles in the flow field inside of the printhead undergoing the standard jetting with the firing frequency of 1–20 kHz. An air pocket of bubble was formed repeatedly and reproduced well through the tested printheads at a certain jetting condition. To see the effects of the bubbles on the dynamic characteristics of the piezoelectric printheads, the piezoelectric velocity on the top of the pressure chamber was measured with a laser vibrometer. When the bubble was trapped at the nozzle exit orifice, the piezo velocity signals showed significantly different frequency peaks appearing in the spectrum and the high frequency components were identified with the frequency response measurements.     

Pneumatic dispensing of nano- to picoliter droplets of liquid metal with the StarJet method for rapid prototyping of metal microstructures

This study presents a new, simple and robust, pneumatically actuated method for the generation of liquid metal micro droplets in the nano- to picoliter range. The so-called StarJet dispenser utilizes a star-shaped nozzle geometry that stabilizes liquid plugs in its center by means of capillary forces. Single droplets of the liquid metal can be pneumatically generated by the interaction of the sheathing gas flow in the outer grooves of the nozzle and the liquid metal. For experimental validation, a print head was build consisting of silicon chips with a star-shaped nozzle geometry and a heated actuator (up to 280°C). The silicon chips are fabricated by Deep Reactive Ion Etching (DRIE). Chip designs with different star-shaped geometries were able to generate droplets with diameters in the range of the corresponding nozzle diameters. The StarJet can be operated in two modes: Either continuous droplet dispensing mode or drop on demand (DoD) mode. The continuous droplet generation mode for a nozzle with 183?μm diameter shows tear-off frequencies between 25 and 120?Hz, while droplet diameters remain constant at 210?μm for each pressure level. Metal columns were printed with a thickness of 0.5–1.0?mm and 30?mm height (aspect ratio >30), to demonstrate the directional stability of droplet ejection and its potential as a suitable tool for direct prototyping of the metal microstructures.     

Three-dimensional valve-based controllable PDMS nozzle for dynamic modulation of droplet generation

In this work, we developed a shape-controllable nozzle inside a multilayer PDMS microchip. The nozzle was able to control the shape of the fluid channel in three dimensions. All the four walls of the fluid channel were comprised of pneumatic PDMS membrane valves, and their deformation was controlled by air pressure. As both the limitation of the fluid flux and the shape of the fluid channel were adjustable spatially in three dimensions, this valve-based nozzle generated droplets with less response time and in a more effectively controlled manner comparing to conventional droplet devices. It could also function as a microinjector to modulate the compositions of droplets precisely and continuously. In addition, the nozzle was able to form a specific shape to generate core–shell particles.     

A superposable double-gradient droplet array chip for preparation of PEGDA microspheres containing concentration-gradient drugs

This article describes a superposable double-concentration-gradient droplet array chip, which allows a variety of concentration combinations of two components to be formed simultaneously. The concentration gradients generated from two layers of the chip could be arbitrarily superimposed by adjusting the center angle between the two bonding layers. With the aqueous phase flow rate of 1.0 μL min^?1 and the oil phase flow rate of 30.0 μL min^?1, the droplets about 58 μm in diameter were produced, and the coefficients of variation were below 6.0% for single channel and 5.7% for all the channels. Using a dual-32-channel superposable gradient droplet array chip, poly(ethylene glycol) diacrylate (PEGDA) microspheres containing concentration-gradient combinations of rhodamine B and fluorescein were fabricated to demonstrate the capability of PEGDA for encapsulating hydrophilic and hydrophobic substances, as well as the proper concentration-gradient distribution. Furthermore, PEGDA microspheres loaded with two anticancer drugs, hydrophilic doxorubicin hydrochloride and hydrophobic paclitaxel, of 17 concentration combinations were simultaneously prepared. The drug-induced apoptosis of human uterine cervix cancer cells was investigated using the dual-drug-loaded PEGDA microspheres. The optimum synergistic concentration combination of the two drugs was 12.5 μg mL^?1 for doxorubicin hydrochloride and 43.75 μg mL^?1 for paclitaxel according to the preliminary screening. The superposable double-gradient droplet array generator was demonstrated to be a promising platform for screening multiple drug combination in microcarriers.     

“From microtiter plates to droplets” tools for micro-fluidic droplet processing

Droplet-based microfluidic allows high throughput experimentation in with low volume droplets. Essential fluidic process steps are on the one hand the proper control of the droplet composition and on the other hand the droplet processing, manipulation and storage. Beside integrated fluidic chips, standard PTFE-tubings and fluid connectors can be used in combination with appropriate pumps to realize almost all necessary fluidic processes. The segmented flow technique usually operates with droplets of about 100–500 nL volume. These droplets are embedded in an immiscible fluid and confined by channel walls. For the integration of segmented flow applications in established research workflows—which are usually base on microtiter plates—robotic interface tools for parallel/serial and serial/parallel transfer operations are necessary. Especially dose–response experiments are well suited for the segmented flow technique. We developed different transfer tools including an automated “gradient take-up tool” for the generation of segment sequences with gradually changing composition of the individual droplets. The general working principles are introduced and the fluidic characterizations are given. As exemplary application for a dose–response experiment the inhibitory effect of antibiotic tetracycline on Escherichia coli bacteria cultivated inside nanoliter droplets was investigated.     

Investigation to minimize heater burnout in thermal thin film print heads

A test system to improve the reliability of a printhead was developed and various printheads was tested. We developed a thermally driven monolithic inkjet printhead comprising dome-shaped ink chambers, thin film nozzle guides and omega-shaped heaters integrated on the top surface of each chamber. In a durability test of an inkjet printhead, the test system automatically detects a heater failure using a Wheatstone bridge circuit. Various models were designed and tested to develop a more reliable printhead. Three design parameters of the thickness of heat-transmission layer, reinforcement layer, and insulation layer were investigated in the test. Specially, the reinforcement layer was introduced to improve the lifetime of printhead. The thicker the heat-transmission layer as well as the insulation layer, the longer the life of the printhead. The lifetime of a heater with a reinforcement layer was longer than the lifetime of a heater without a reinforcement layer.     

Electro-thermal analysis of an embedded boron diffused microheater for thruster applications

One of the important design criteria of micropropulsion systems in particular VLM is the type of microheater, its layout and placement with a view to achieve uniform heating of propellant, fast heat transfer efficiency with minimum input power. Thrust produced by microthruster not only depends on the structural geometry of the thruster and propellant flow rate, but also on the chamber temperature to produce super saturated dry stream at the exit nozzle. Detailed design of microheater in thermal and electrical domains using co-solvers available in MEMS software tools along with material’s thermal property, temperature dependence of electrical resistivity and thermal conductivity have been considered in the present work to achieve precise modeling and experimental accuracy of heater operation. The chamber temperature was analytically calculated and subsequently the required resistance and power were estimated. The boron diffused microheaters of meanderline configuration in silicon substrate has been designed and its finite element based electro-thermal modeling was employed to predict the heater characteristics. The variation of microheater temperature with time, applied voltage and along chamber length has been determined from the modeling. Subsequently the designed microheater was realized on silicon wafer by lithography and boron diffusion process and its detailed testing was evaluated. It was found that boron diffused resistor of 820 Ω can generate 405 K temperature with applied input power 2.4 W. Finally the simulated results were validated by experimental data.     

Comparison of micro-dispensing performance between micro-valve and piezoelectric printhead

In micro-dispensing applications, printhead activation mechanism, its design and operating parameters are integrated together to affect the droplet generation process. These factors give each printhead advantages and limitations over the others in specific fabrication. Hence, multiple printheads on micro level fabrication are preferred to perform multi-material dispensing task. In this paper, the mechanisms of two commonly used micro printheads, solenoid actuated micro-valve and piezoelectric printhead are discussed. Comprehensive experiments are conducted to characterize their performance and the results are analyzed so as to explore optimal droplet formation condition. With regards to the operational parameters’ influence on droplet formation, micro-valve is investigated in terms of pressure, and operational on time, and piezoelectric printhead is investigated based on pulse amplitude, and width of driving pulse. Nozzle size, a key design parameter in the two printheads, is also studied according to its influence on dispensing capability. To facilitate dispenser selection, the two printheads are compared based on droplet size, droplet stability, droplet velocity, and dispensing viscosity of successful ejection. Other factors such as chemical compatibility, time consumption in determining optimal condition and reliability of dispensing process are also reported to play an essential role in this selection. Our investigation on the relationship between related parameters and dispensing performance will not only benefit dispenser selection in multi-material dispensing application, but also build a solid background to develop multiple printhead system for fabrication of bioengineering components.     

Study on the effect of heating plate thickness on the micro induction heater for thermal bubbles generation

This paper designed a micro planar induction heater for thermal bubbles generation. The micro heater which consists of a micro planar coil, a copper heating plate and a glass slide was fabricated with MEMS fabrication process. The relations between the heating performance and the thickness of heating plate were studied in the simulation with the software of COMSOL. The experimental system has been built and the experimental tests for thermal bubble generation have been also carried out with the prototype. The process of thermal bubbles generation was recorded by the video camera. The frequency of AC current applied in the experiment is 100 kHz and the heating time of 1 s. The experimental results indicated that the micro heater has the best heating performance with the heating plate thickness of 12–16 μm, and the minimum power for thermal bubbles generation was only 0.427 W. This micro heater can be applied to a variety of thermal bubble devices, such as micro actuator, micro ejector and micro pump.     

A high-resolution high-frequency monolithic top-shooting microinjector free of satellite drops - part I: concept, design, and model

Introduces an innovative microinjector design, featuring a bubble valve, which entails superior droplet ejection characteristics and monolithic fabrication, which allows handling of a wide range of liquids. This new microinjector uses asymmetric bubbles to reduce crosstalk, increase frequency response and eliminate satellite droplets. During a firing, i.e., droplet ejection, the "virtual valve" closes, by growing a thermal bubble in the microchannel, to isolate the microchamber from the liquid supply and neighboring chambers. Between firings, however, the virtual valve opens, by collapsing the bubble, to reduce flow restriction for fast refilling of the microchamber. The use of bubble valves brings about fast and reliable device operation without imposing the significant complication fabrication of physical microvalves would call for. In addition, through a special heater configuration and chamber designs, bubbles surrounding the nozzle cut off the tail of the droplets being ejected and completely eliminate satellite droplets. A simple one-dimensional model of the operation of the microinjector is used to estimate the bubble formation and liquid refilling.     

Microchannel geometry design for rapid and uniform reagent distribution

Rapid and uniform reagent distribution is critical to the performance of a high-throughput microfluidic system, and its geometric design of the microchannels dominates the accuracy and distribution uniformity of the daughter droplets. This research’s purpose is to optimize the geometry of the T-junction to achieve a uniform distribution of two daughter droplets from a single liquid droplet. Models of gas–liquid flow were realized in the transient numerical simulations to investigate the geometry-dependent pressure distributions and the flowing velocities inside the droplet during the splitting process that leads to an improved design of the T-junction that can increase the stability of the droplet splitting process. To validate that increasing the stability of the splitting process can help improve the distribution uniformity of the daughter droplets, microfluidic devices were manufactured on poly(methyl methacrylate) substrates with micromilling and thermal bonding for experiments. In the multiple experiments, 2 μl of reagent was loaded into the microfluidic device and a uniform pneumatic pressure was applied to push the droplet into the T-junction for splitting. The experimental results, after statistical analysis, show that the improved T-junction can achieve better distribution uniformity of the daughter droplets with a higher reliability and a less reagent loss during the splitting process.     

Research on a large power thermal bubble micro-ejector with induction heating

The present study investigates a large power thermal bubble micro-ejector with induction heating device. The traditional thermal-bubble ejectors adopted resistors as the heating resources, it can only work with lower power and convey liquid with lower flow rate. Induction heating devices are adopted to replace the resistor for heating liquid in this paper. With this heating method, there is no physical contact between the heating core and the external power supply circuit. The liquid in the chamber of micro-ejector is heated by the induction heating device and changes from liquid phase to gas phase, generating vapor bubbles in the micro chamber of the micro ejector. The bubble expands rapidly and ejects droplets through the nozzle. The prototype of the micro-ejector is fabricated and experiments are carried out. Continuous droplets are ejected out from the nozzle as the applied AC current is 0.6–0.65 A with the power frequency of 100 kHz. The total volume of the continuous droplets is ranging from 18.84 to 49.87 nL, and the corresponding flow rate is about 0.52–1.36 μL/min. Furthermore, this new micro-ejector can be adopted in conveying of micro-scale liquid, the injection of trace drugs and the 3D printing.     

Driving characteristics of the electrowetting-on-dielectric device using atomic-layer-deposited aluminum oxide as the dielectric

Electrowetting on dielectric (EWOD) is useful in manipulating droplets for digital (droplet-based) microfluidics, but its high driving voltage over several tens of volts has been a barrier to overcome. This article presents the characteristics of EWOD device with aluminum oxide (Al₂O₃, ε _r  ≈ 10) deposited by atomic layer deposition (ALD), for the first time as the high-k dielectric for lowering the EWOD driving voltage substantially. The EWOD device of the single-plate configuration was fabricated by several steps for the control electrode array of 1 mm × 1 mm squares with 50 μm space, the dielectric layer of 1,270 Å thick ALD Al₂O₃, the reference electrode of 20 μm wide line electrode, and the hydrophobic surface treatment by Teflon-AF coating, respectively. We observed the movement of a 2 μl water droplet in an air environment, applying a voltage between one of the control electrodes and the reference electrode in contact with the droplet. The droplet velocity exponentially depending on the applied voltage below 15 V was obtained. The measured threshold voltage to move the droplet was as low as 3 V which is the lowest voltage reported so far in the EWOD researches. This result opens a possibility of manipulating droplets, without any surfactant or oil treatment, at only a few volts by EWOD using ALD Al₂O₃ as the dielectric.     

Droplets coalescence and mixing with identical and distinct surface tension on a wettability gradient surface

The influence of identical and distinct surface tensions on the coalescence and mixing of droplets after a direct collision on a wettability gradient surface (made from a self-assembled monolayer, SAM technique) was investigated. The results indicate that their mixing is driven sequentially by interior convection and diffusion; the convection endures less than 100 ms but dominates more than 60 % of the mixing. If the stationary droplet has a large surface tension (73.28 mN × m^?1), whether the moving droplet has a large surface tension (73.28 mN × m^?1) or a small surface tension (38.63 mN × m^?1), the mushroom-shaped mixing pattern is generated within the coalesced droplet that enhances the convective mixing and also significantly enlarges the interface for mass diffusion. The mixing index of these two cases was greater than 0.8 at 120 s after the collision. For the cases in which the stationary droplet with a small surface tension collided by the moving droplet with a large surface tension, a mixing pattern with a round-head shape developed, which was insufficient to benefit the mixing. When the stationary and moving droplets both had small surface tension, the moving droplet was unable to merge with stationary droplet and had poor mixing quality due to the small surface Gibbs energy of both stationary and moving droplets. For the collision of droplets of identical surface tension, the surface tension affects the coalescence behavior; for the collision of droplets with distinct surface tension, the coalescence behavior and mixing quality depend on the colliding arrangement of stationary and moving droplets.     

High-aspect-ratio through-hole array microfabricated in a PMMA plate for monodisperse emulsion production

Microchannel (MC) emulsification is a promising technique for producing monodisperse emulsions consisting of highly uniform droplets. The authors developed a high-aspect-ratio microstructure (HARMST) made of poly(methyl methacrylate) (PMMA) as a new MC emulsification device. A PMMA straight-through MC array plate consisting of 31,250 through-holes with a 7.3 × 22.9-μm oblong section and a 200-μm depth was fabricated by a process of synchrotron radiation (SR) lithography and etching. Oblong MCs fabricated in a PMMA straight-through MC array were highly uniform with a coefficient of variation of less than 2%. The fabricated PMMA straight-through MC array plate was used to produce water-in-oil (W/O) emulsions. Monodisperse W/O emulsions with average droplet diameters of approximately 25 μm and a minimum coefficient of variation of 3.2% were produced via a hydrophobic PMMA straight-through MC array. The PMMA straight-through MC array plate also produced monodisperse W/O emulsions at droplet production rates of up to 1.7 × 10⁴/s. The PMMA straight-through MC array plates developed in this work are expected to expand the application field of emulsification using straight-through MC array plates, which have previously been made of single-crystal silicon.     

Precise droplet volume measurement and electrode-based volume metering in digital microfluidics

In this work, for the first time, we demonstrate nanoscale droplet generation from a continuous electrowetting microchannel using a simple and precise image-based droplet volume metering technique. One of the most popular ways of droplet generation in electrowetting devices is to split a droplet from a preloaded volume as a fluid reservoir. This method is effective, but lowers volume consistency after multiple droplets are generated. Impedance- and capacitance-based methods of volume metering have been successfully used in digital microfluidics, but require complex circuitry and feedback signal processing. In this work, we demonstrate nanoliter droplet generation from a continuous electrowetting channel used as a replenishable fluid reservoir which compensates for the loss of reservoir volume as droplets are sequentially split. This improves volume consistency especially for applications requiring multi-droplet generation. Based on the area of the electrode, the volume of each droplet split from the electrowetting channel can be obtained by a simple and precise image processing technique with no need for additional hardware and measurement errors of ±0.05 %. This simple technique can be used in a wide range of applications that require precise volume metering, such as immunoassay.     

Study of flow behaviors of droplet merging and splitting in microchannels using Micro-PIV measurement

Droplet merging and splitting are important droplet manipulations in droplet-based microfluidics. However, the fundamental flow behaviors of droplets were not systematically studied. Hence, we designed two different microstructures to achieve droplet merging and splitting respectively, and quantitatively compared different flow dynamics in different microstructures for droplet merging and splitting via micro-particle image velocimetry (micro-PIV) experiments. Some flow phenomena of droplets different from previous studies were observed during merging and splitting using a high-speed microscope. It was also found the obtained instantaneous velocity vector fields of droplets have significant influence on the droplets merging and splitting. For droplet merging, the probability of droplets coalescence (η) in a microgroove is higher (50% < η < 92%) than that in a T-junction microchannel (15% < η < 50%), and the highest coalescence efficiency (η = 92%) comes at the two-phase flow ratio e of 0.42 in the microgroove. Moreover, compared with a cylinder obstacle, Y-junction bifurcation can split droplets more effectively and the droplet flow during splitting is steadier. The results can provide better understanding of droplet behaviors and are useful for the design and applications of droplet-based microfluidics.     

Fluid dynamic behavior of dispensing small droplets through a thin liquid film

This paper presents a technology for dispensing droplets through thin liquid layers. The system consists of a free liquid film, which is suspended in a frame and positioned in front of a piezoelectric printhead. A droplet, generated by the printhead, merges with the film, but due to its momentum, passes through and forms a droplet that separates on the other side and continues its flight. The technology allows the dispensing, mixing and ejecting of picolitre liquid samples in a single step. This paper overviews the concept, potential applications, experiments, results and a numerical model. The experimental work includes studying the flight of ink droplets, which ejected from an inkjet print head, fly through a free ink film, suspended in a frame and positioned in front of the printhead. We experimentally observed that the minimum velocity required for the 80 pl droplets to fly through the 75 ± 24 μm thick ink film was of 6.6 m s^?1. We also present a numerical simulation of the passage of liquid droplets through a liquid film. The numerical results for different initial speeds of droplets and their shapes are taken into account. We observed that during the droplet–film interaction, the surface energy is partially converted to kinetic energy, and this, together with the impact time, helps the droplets penetrate the film. The model includes the Navier–Stokes equations with continuum-surface-tension force derived from the phase-field/Cahn–Hilliard equation. This system allows us to simulate the motion of a free surface in the presence of surface tension during merging, mixing and ejection of droplets. The influence of dispensing conditions was studied and it was found that the residual velocity of droplets after their passage through the thin liquid film well matches the measured velocity from the experiment.     

Droplet group production in an AC electro-flow-focusing microdevice

We report the production of droplet groups with a controlled number of drops in a microfluidic electro-flow-focusing device under the action of an AC electric field. This regime appears for moderate voltages (500–700 V peak-to-peak) and signal frequencies between 25 and 100 Hz, much smaller than the droplet production rate (\({\sim }\,{500}\) Hz). For this experimental condition the production frequency of a droplet package is twice the signal frequency. Since the continuous phase flow in the microchannel is a Hagen–Poiseuille flow, the smaller droplets of a group move faster than the bigger ones leading to droplet clustering downstream.     

Flow-induced particle migration in microchannels for improved microfiltration processes

Microchannels can be used to induce migration phenomena of micron sized particles in a fluid. Separation processes, like microfiltration, could benefit from particle migration phenomena. Currently, microfiltration is designed around maximum flux, resulting in accumulation of particles in and on the membrane. In this paper it is shown that starting the design at the particle level will result in a new microfiltration process. The behaviour of suspensions between 9 and 38 volume% was studied by confocal scanning laser microscopy; migration as a result of shear-induced diffusion was observed in a rectangular microchannel with nonporous walls. Particles segregated on size within the first 10 cm of the channel. To illustrate this, at 20 volume% of small (1.53 μm) and large (2.65 μm) particles each, the larger particles migrated to the middle of the channel, while the small particles had high concentrations near the walls. The small particles could then be collected from their position close to the permeable walls, e.g. membranes, where the pore size of the membrane is no longer the determining factor for separation. Guidelines for using this phenomenon in a microfiltration process were derived and the selectivity of the process was experimentally evaluated. The small droplets could be removed from the mixtures with a membrane having pores 3.7 times larger than the droplets, thereby minimizing accumulation of droplets in and on the membrane. As long as the process conditions are chosen appropriately, no droplet deposition takes place and high fluxes (1.7 × 10³ L h^?1 m^?² bar^?1) can be maintained.