Conversion of Polymer Surfaces into Nonwetting Substrates for Liquid Metal Applications.

Liquid metal-based applications are limited by the wetting nature of polymers toward surface-oxidized gallium-based liquid metals. This work demonstrates that a 120 s CF4/O2 plasma treatment of polymer surfaces-such as poly(dimethylsiloxane) (PDMS), SU8, S1813, and polyimide-converts these previously wetting surfaces to nonwetting surfaces for gallium-based liquid metals. Static and advancing contact angles of all plasma-treated surfaces are >150°, and receding contact angles are >140°, with contact angle hysteresis in the range of 8.2-10.7°, collectively indicating lyophobic behavior. This lyophobic behavior is attributed to the plasma simultaneously fluorinating the surface while creating sub-micron scale roughness. X-ray photoelectron spectroscopy (XPS) results show a large presence of fluorine at the surface, indicating fluorination of surface methyl groups, while atomic force microscopy (AFM) results show that plasma-treated surfaces have an order of magnitude greater surface roughness than pristine surfaces, indicating a Cassie-Baxter state, which suggests that surface roughness is the primary cause of the nonwetting property, with surface chemistry making a smaller contribution. Solid surface free energy values for all plasma-treated surfaces were found to be generally lower than the pristine surfaces, indicating that this process can be used to make similar classes of polymers nonwetting to gallium-based liquid metals.

Axially-Anisotropic Hierarchical Grating 2D Guided-Mode Resonance Strain-Sensor.

Guided-mode resonance strain sensors are planar binary gratings that have fixed resonance positions and quality factors decided by material properties and grating parameters. If one is restricted by material choices, the quality factor can only be improved by adjusting the grating parameters. We report a new method to improve quality factor by applying a slotting design rule to a grating design. We investigate this design rule by first providing a theoretical analysis on how it works and then applying it to a previously studied 2D solid-disc guided-mode resonance grating strain sensor design to create a new slotted-disc guided-mode resonance grating design. We then use finite element analysis to obtain reflection spectrum results that show the new design produces resonances with at least a 6-fold increase in quality factor over the original design and more axially-symmetric sensitivities. Lastly, we discuss the applicability of the slotting design rule to binary gratings in general as a means of improving grating performance while retaining both material and resonance position choices.

Fabrication of a microneedle/CNT hierarchical micro/nano surface electrochemical sensor and its in-vitro glucose sensing characterization.

We report fabrication of a microneedle-based three-electrode integrated electrochemical sensor and in-vitro characterization of this sensor for glucose sensing applications. A piece of silicon was sequentially dry and wet etched to form a 15 × 15 array of tall (approximately 380 µm) sharp silicon microneedles. Iron catalyst was deposited through a SU-8 shadow mask to form the working electrode and counter electrode. A multi-walled carbon nanotube forest was grown directly on the silicon microneedle array and platinum nano-particles were electrodeposited. Silver was deposited on the Si microneedle array through another shadow mask and chlorinated to form a Ag/AgCl reference electrode. The 3-electrode electrochemical sensor was tested for various glucose concentrations in the range of 3~20 mM in 0.01 M phosphate buffered saline (PBS) solution. The sensor's amperometric response to the glucose concentration is linear and its sensitivity was found to be 17.73 ± 3 µA/mM-cm2. This microneedle-based sensor has a potential to be used for painless diabetes testing applications.

Acoustic Wave-Driven Liquid Metal Expansion.

In this paper, we report a volume expansion phenomenon of a liquid metal droplet naturally oxidized in an ambient environment by applying an acoustic wave. An oxidized gallium-based liquid metal droplet was placed on a paper towel, and a piezo-actuator was attached underneath it. When a liquid metal droplet was excited by acoustic wave, the volume of liquid metal was expanded due to the inflow of air throughout the oxide crack. The liquid metal without the oxide layer cannot be expanded with an applied acoustic wave. To confirm the effect of the expansion of the oxidized liquid metal droplet, we measured an expansion ratio, which was calculated by comparing the expanded size in the x (horizontal), y (vertical) axis to the initial size of the liquid metal droplet, using a high-speed camera. For various volumes of the droplet, when we applied various voltages in the range of 5~8 Vrms with 18.5~24.5 kHz using the piezo-actuator, we obtained a maximum expansion ratio of 2.4 in the x axis and 3.8 in the y axis, respectively. In addition, we investigated that the time to reach the maximum expansion in proportion to the volume size of liquid metal differed by five times from 4 s to 20 s, and that the time to maintain the maximum expansion differed from 23 s to 2.5 s, which was inversely proportional to the volume size. We also investigated the expansion ratios depending on the exposure time to the atmosphere. Finally, a circuit containing LED, which can be turned on by expanded liquid metal droplet, was demonstrated.

Review of Electrothermal Micromirrors.

Electrothermal micromirrors have become an important type of micromirrors due to their large angular scanning range and large linear motion. Typically, electrothermal micromirrors do not have a torsional bar, so they can easily generate linear motion. In this paper, electrothermal micromirrors based on different thermal actuators are reviewed, and also the mechanisms of those actuators are analyzed, including U-shape, chevron, thermo-pneumatic, thermo-capillary and thermal bimorph-based actuation. Special attention is given to bimorph based-electrothermal micromirrors due to their versatility in tip-tilt-piston motion. The exemplified applications of each type of electrothermal micromirrors are also presented. Moreover, electrothermal micromirrors integrated with electromagnetic or electrostatic actuators are introduced.

Biofriendly bonding processes for nanoporous implantable SU-8 microcapsules for encapsulated cell therapy.

Mechanically robust, cell encapsulating microdevices fabricated using photolithographic methods can lead to more efficient immunoisolation in comparison to cell encapsulating hydrogels. There is a need to develop adhesive bonding methods which can seal such microdevices under physiologically friendly conditions. We report the bonding of SU-8 based substrates through (i) magnetic self assembly, (ii) using medical grade photocured adhesive and (iii) moisture and photochemical cured polymerization. Magnetic self-assembly, carried out in biofriendly aqueous buffers, provides weak bonding not suitable for long term applications. Moisture cured bonding of covalently modified SU-8 substrates, based on silanol condensation, resulted in weak and inconsistent bonding. Photocured bonding using a medical grade adhesive and of acrylate modified substrates provided stable bonding. Of the methods evaluated, photocured adhesion provided the strongest and most stable adhesion.

Biocompatibility of SU-8 and Its Biomedical Device Applications.

SU-8 is an epoxy-based, negative-tone photoresist that has been extensively utilized to fabricate myriads of devices including biomedical devices in the recent years. This paper first reviews the biocompatibility of SU-8 for in vitro and in vivo applications. Surface modification techniques as well as various biomedical applications based on SU-8 are also discussed. Although SU-8 might not be completely biocompatible, existing surface modification techniques, such as O2 plasma treatment or grafting of biocompatible polymers, might be sufficient to minimize biofouling caused by SU-8. As a result, a great deal of effort has been directed to the development of SU-8-based functional devices for biomedical applications. This review includes biomedical applications such as platforms for cell culture and cell encapsulation, immunosensing, neural probes, and implantable pressure sensors. Proper treatments of SU-8 and slight modification of surfaces have enabled the SU-8 as one of the unique choices of materials in the fabrication of biomedical devices. Due to the versatility of SU-8 and comparative advantages in terms of improved Young's modulus and yield strength, we believe that SU-8-based biomedical devices would gain wider proliferation among the biomedical community in the future.

Electric Field-Driven Liquid Metal Droplet Generation and Direction Manipulation.

A gallium-based liquid metal got high attention recently, due to the excellent material properties that are useful in various research areas. We report here on electric field-induced liquid metal droplet generation and falling direction manipulation. The well-analyzed electro-hydrodynamic method is a selectable way to control the liquid metal, as the liquid metal is conductive. The electric field-induced liquid metal manipulation can be affected by the flow rate (0.05~0.2 mL/min), voltage (0~7 kV), and distance (15 and 30 mm) between electrodes, which changes the volume of the electric field-induced generated liquid metal droplet and the number of the generated droplets. When the electric field intensity increases or the flow rate increases, the generated droplet volume decreases, and the number of droplets increases. With the highest voltage of 7 kV with 15 mm between electrodes at the 0.2 mL/min flow rate, the lowest volume and the largest number of the generated droplets for 10 s were ~10 nL and 541, respectively. Additionally, we controlled the direction of the generated droplet by changing the electric field. The direction of the liquid metal droplet was controlled with the maximum angle of ~12°. Moreover, we exhibited a short circuit demonstration by controlling the volume or falling direction of the generated liquid metal droplet with an applied electric field.

Pressure-tunable guided-mode resonance sensor for single-wavelength characterization.

A method of tuning a one-dimensional guided-mode resonance grating through the use of an air-pressure-responsive membrane is demonstrated here using finite-element method simulation. The device consists of a titanium dioxide (TiO(2)) grating structure embedded in a flexible polydimethylsiloxane membrane. This grating has a resonant response to TM-polarized light at a wavelength dependent upon the refractive index of the surrounding medium. By varying the pressure by 5500 Pa, lateral strain may be applied to the grating; this allows resonances to be produced for medium refractive indices ranging from 1.33 to 1.50 for a fixed-wavelength 850 nm light source.

Thermo-optically tunable silicon photonic crystal light modulator.

We designed, fabricated, and characterized a thermo-optically tunable compact (10 µm × 10 µm) silicon photonic crystal (PhC) light modulator that operates at around 1.55 µm for TE polarization. The operational principle of the device is the modulation of the cutoff frequency in a silicon-based line defect PhC. The cutoff frequency is shifted because of the thermo-optic tuning of the silicon refractive index, which is realized by localized heating on the PhC. The modulator is formed by a triangular lattice array of cylindrical air holes on a silicon-on-insulator wafer. Optical characterization was carried out, and the result clearly showed thermo-optic tuning of the cutoff frequency at around 1.55 µm.

An Implanted Magnetic Microfluidic Pump for In Vivo Bone Remodeling Applications.

Modulations of fluid flow inside the bone intramedullary cavity has been found to stimulate bone cellular activities and augment bone growth. However, study on the efficacy of the fluid modulation has been limited to external syringe pumps connected to the bone intramedullary cavity through the skin tubing. We report an implantable magnetic microfluidic pump which is suitable for in vivo studies in rodents. A compact microfluidic pump (22 mm diameter, 5 mm in thickness) with NdFeB magnets was fabricated in polydimethylsiloxane (PDMS) using a set of stainless-steel molds. An external actuator with a larger magnet was used to wirelessly actuate the magnetic microfluidic pump. The characterization of the static pressure of the microfluidic pump as a function of size of magnets was assessed. The dynamic pressure of the pump was also characterized to estimate the output of the pump. The magnetic microfluidic pump was implanted into the back of a Fischer-344 rat and connected to the intramedullary cavity of the femur using a tube. On-demand wireless magnetic operation using an actuator outside of the body was found to induce pressure modulation of up to 38 mmHg inside the femoral intramedullary cavity of the rat.

Editorial for the Special Issue on the ICAE 2019.

This special issue is a collection of 10 selected papers after presenting at the Fifth International Conference on Advanced Electromaterials (ICAE 2019), held in Jeju, South Korea on 5-8 November 2019 [...].

Cell encapsulation and oxygenation in nanoporous microcontainers.

With strides in stem cell biology, cell engineering and molecular therapy, the transplantation of cells to produce therapeutic molecules endogenously is an attractive and achievable alternative to the use of exogenous drugs. The encapsulation of such cell transplants in semi-permeable, nanoporous constructs is often required to protect them from immune attack and to prevent their proliferation in the host. However, effective graft immunoisolation has been mostly elusive owing to the absence of a high-throughput method to create precisely controlled, high-aspect-ratio nanopores. To address the clinical need for effective cell encapsulation and immunoisolation, we devised a biocompatible cell-encapsulating microcontainer and a method to create highly anisotropic nanopores in the microcontainer's surface. To evaluate the efficacy of these nanopores in oxygenating the encapsulated cells, we engineered 9L rat glioma cells to bioluminesce under hypoxic conditions. The methods described above should aid in evaluating the long term survival and efficacy of cellular grafts.

SU-8-based immunoisolative microcontainer with nanoslots defined by nanoimprint lithography.

Cells can secrete biotherapeutic molecules that can replace or restore host function. The transplantation of such cells is a promising therapeutic modality for the treatment of several diseases including type 1 diabetes mellitus. These cellular grafts are encapsulated in semipermeable and immunoisolative membranes to protect them from the host immune system, while allowing the transport of nutrients and small molecules that are required for cell survival and function. The authors report on SU-8-based biocompatible immunoisolative cuboid microcontainers for cell transplantation. Each microcontainer comprises a 300×300×250 or a 1100×1100×250 µm(3) SU-8 hollowed cuboid base that houses the cells and an optically transparent SU-8-based nanoporous lid that closes the device. The hollowed cuboid base was formed by conventional optical lithography to have 8 nl (200×200×200 µm(3)) encapsulation volume for cellular payload. The lid comprises a thick SU-8 slab with an array of cylindrical wells, whose bottom surface is sealed with a thin nanoporous SU-8 membrane. The nanoporous membrane was created from a 100 nm grating (width and spacing) initial silicon mold subjected to a repeated cycle of oxidation and wet etching to achieve a 20 nm wide and 200 nm pitch nano silicon grating. Nanoimprinting and oblique-angle metal deposition, followed by inductively coupled plasma etching were utilized to create 15 nm wide and 350-450 nm deep nanoslots in the thin SU-8 membrane. Isolated mouse islets were encapsulated in the hollowed cuboid base and the nanoporous lid was assembled on top. The penetration of large and small molecules into the microcontainer was observed with fluorescence.

Surface Modification with Gallium Coating as Nonwetting Surfaces for Gallium-Based Liquid Metal Droplet Manipulation.

We report gallium (Ga) coating as a simple approach to convert most common microfluidic substrates to nonwetting surfaces against surface-oxidized gallium-based liquid metal alloys. These alloys are readily oxidized in ambient air and adhere to almost all surfaces, which imposes significant challenges in mobilizing liquid metal droplets without leaving residue. Various flat substrates (e.g., PDMS, Si, SiO2, SU-8, glass, and parylene-C coated PDMS) were coated with thin film (75-200 nm in thickness) of gallium by evaporation and the coated gallium formed nanoscale uneven and rough surface through Ostwald ripening with its surface covered with oxide shell. Static and dynamic contact angles of the gallium-coated surfaces were found to be greater than 160°, while dynamic contact angle measurements showed contact angle hysteresis in the range of 6.5-24.4°. Surface-oxidized gallium-based liquid metal alloy droplets were shown to bounce off and roll on the gallium-coated surfaces without leaving any residue which confirms the nonwettability of the gallium-coated flat surfaces. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) showed the gallium-coated flat substrates consist of nanoscale hemispherical structures with average surface roughness of 33.8 nm. Pneumatic actuation of surface-oxidized liquid metal droplets in PDMS microfluidic channels coated with gallium was conducted to confirm the feasibility of utilizing gallium coating as an effective surface modification for surface-oxidized gallium-based liquid metal droplet manipulation.

Electromagnetic three dimensional liquid metal manipulation.

In this paper, we report three-dimensional (3-D) liquid metal manipulation using electromagnets, which can be applied to electrical switching applications. The liquid metal droplet was coated with iron (Fe) particles by chemical reaction with hydrochloric acid (HCl), and thus it became responsive to the magnetic field, becoming a magnetic liquid metal marble. Using electromagnets, the magnetic field was turned on and off on-demand. We investigated an average velocity and the maximum working distance of the horizontal and vertical electromagnetic field-driven manipulation of the magnetic liquid metal marble. Linear (1-D) and plane (2-D) manipulation of the marble was successfully demonstrated and 3-D manipulation was verified for electrical switching.

Cost-effective surface modification for Galinstan® lyophobicity.

In this paper we investigate the feasibility of using a cost-effective fabrication method based on sandblasting, chemical etching and spray coating processes, to render common surfaces to be non-wettable by Galinstan®. Although Galinstan® is a non-toxic liquid metal alternative to mercury, the viscoelastic and extremely wetting characteristics of Galinstan® have been the major bottleneck limiting the wide applicability of the gallium-based liquid metal. This paper tries to accomplish non-wettability to Galinstan® by combining surface texture and chemistry with the unique property of Galinstan®, that is, its high surface tension and yield strength that prevent the penetration of the liquid metal into surface asperities. Fabricated surfaces resemble traditional superhydrophobic (water-repellent) surfaces, and exhibit a superior non-wettability to Galinstan® as quantified by high static and dynamic contact angles, small hysteresis, as well as impact resistance. Reported fabrication method based on sandblasting, etching and spray coating is easily applicable to various surfaces ranging from metals, ceramics, to plastics and is scalable to large surfaces.

On-demand magnetic manipulation of liquid metal in microfluidic channels for electrical switching applications.

We report magnetic-field-driven on-demand manipulation of liquid metal in microfluidic channels filled with base or acid. The liquid metal was coated with iron (Fe) particles and treated with hydrochloric acid to have strong bonding strength with the Fe particles. The magnetic liquid metal slug inserted in the microchannel is manipulated, merged, and separated. In addition, corresponding to the repositioning of an external magnet, the liquid metal slug can be readily moved in microfluidic channels with different angles (>90°) and cross-linked channels in any direction. We demonstrated the functionality of the liquid metal in the microfluidic channel for electrical switching applications by manipulation of the liquid metal, resulting in the sequential turning on of light emitting diodes (LEDs).

Woven-Yarn Thermoelectric Textiles.

The fabrication and characterization of highly flexible textiles are reported. These textiles can harvest thermal energy from temperature gradients in the desirable through-thickness direction. The tiger yarns containing n- and p-type segments are woven to provide textiles containing n-p junctions. A high power output of up to 8.6 W m(-2) is obtained for a temperature difference of 200 °C.

PDMS based coplanar microfluidic channels for the surface reduction of oxidized Galinstan.

Galinstan has the potential to replace mercury - one of the most popular liquid metals. However, the easy oxidation of Galinstan restricts wide applicability of the material. In this paper, we report an effective reduction method for the oxidized Galinstan using gas permeable PDMS (polydimethlysiloxane)-based microfluidic channel. The complete study is divided into two parts - reduction of Galinstan oxide and behavior of reduced Galinstan oxide in a microfluidic channel. The reduction of Galinstan oxide is discussed on the basis of static as well as dynamic angles. The contact angle analyses help to find the extent of reduction by wetting characteristics of the oxide, to optimize PDMS thickness and to select suitable hydrochloric acid (HCl) concentration. The highest advancing angle of 155° and receding angle of 136° is achieved with 200 µm thick PDMS film and 37 wt% (weight percent) HCl solution. The behavior of reduced Galinstan oxide is analyzed in PDMS-based coplanar microfluidic channels fabricated using a simple micromolding technique. Galinstan in the microfluidic channel is surrounded by another coplanar channel filled with HCl solution. Due to the excellent permeability of PDMS, HCl permeates through the PDMS wall between the two channels (interchannel PDMS wall) and achieves a continuous chemical reaction with oxidized Galinstan. A Lab VIEW controlled syringe pump is used for observing the behavior of HCl treated Galinstan in the microfluidic channel. Further optimization of the microfluidic device has been conducted to minimize the reoxidation of reduced Galinstan oxide in the microfluidic channel.