Low-Cost Flexible Printed Circuit Technology Based Microelectrode
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Sensors and Actuators A 169 (2011) 89–97 Contents lists available at ScienceDirect Sensors and Actuators A: Physical jo urnal homepage: www.elsevier.com/locate/sna Low-cost flexible printed circuit technology based microelectrode array for extracellular stimulation of the invertebrate locomotory system a,∗,1 b Alper Bozkurt , Amit Lal a North Carolina State University, Department of Electrical and Computer Engineering, Raleigh, NC 27695-7911, USA b Cornell University, School of Electrical and Computer Engineering, Ithaca, NY 14853, USA a r t i c l e i n f o a b s t r a c t Article history: The biobotic control of invertebrates through functional electrical stimulation of neural and neuromus- Received 6 October 2010 cular tissue is under active exploration. Implantable microelectrodes are often designed to be used in Received in revised form 30 March 2011 chronic long term applications in vertebrates and subjected to strict endurance and resolution require- Accepted 12 May 2011 ments. However, these constraints can be relaxed in invertebrate-related applications to allow low cost Available online 20 May 2011 production for high-volume markets. In this study, we propose flexible printed circuit board (flex-PCB) based electrodes for implantable neuromuscular stimulation, address related shortcomings, and suggest Keywords: 2 modifications in the fabrication process. We were able to obtain a charge storage capacity of 3.18 mC/cm Neural stimulation × Electrodes and 1 kHz impedance of 52 k with gold electroplated 100 m 100 m electrode sites on the flex-PCB Gold electrodes. The electrodeposition of iridium oxide and electrochemical polymerization of PEDOT with 2 Iridium oxide dopant PSS on microelectrodes enhanced the charge storage capacity to 38.9 and 124.3 mC/cm where Conductive polymers the 1 kHz impedance magnitude was 16 k and 3 k , respectively. This improvement in electrochemical PEDOT performance was also corroborated by current pulsed voltage excursion studies. The long term dip test Flexible electronics in saline solution supports the potential of flex-PCB electrodes for neural electrostimulation of insects, Invertebrate physiology while revealing potential instability in PEDOT-PSS coatings with continuous high current density pulsing. © 2011 Elsevier B.V. All rights reserved. 1. Introduction the cost of fabrication. The vertebrate implantable microelectrodes are often designed to be used in chronic long term applications. The functional electrical stimulation of the neuromuscular sys- Hence, the endurance of these devices is an important design cri- tem has been increasingly used as a clinical treatment option for terion during the implantation process and against the long term restoration, rehabilitation, and control of movement [1]. Recently, reactions from the biochemical agents that exist in biological tis- this technique has been under investigation as a means to con- sue. In addition, higher sensitivity and specificity are required trol and direct the locomotion of invertebrate organisms, insects to obtain a successful outcome from the sophisticated vertebrate in particular, for applications ranging from ecological monitor- motor control system. Therefore, implantable stimulating micro- ing to search-and-rescue missions in a disaster [2,3]. Such a electrodes are often produced following high-cost conventional “biobotic” control paradigm may benefit extensively from meta- thin-film processing technologies derived from semiconductor fab- morphic development to couple electrically active microelectrodes rication techniques [5]. On the other hand, immunoreaction is into the electrically responsive tissue of the insect to enable an less an issue for the invertebrates and the lifespan of the elec- automated mass production line [4]. The cost of microfabricating trodes in tissue is much less due to the shorter life-time of insects. the metamorphosis-implanted electrodes on this production line Moreover, depending on the electrical actuation and movement is an important concern, especially for the biobotic applications in control scheme, lower spatial resolution for site specificity can be which a larger number of insects would be employed. tolerated due to the relatively less intricate insect motor control Nevertheless, the design constraints of these invertebrate system of the insect. This difference allows the use of larger pads microelectrodes can be compromised to a greater extent with with more pitch sizes. All these features provide the opportunity respect to vertebrate microelectrodes, thus enabling a reduction in to fabricate implantable electrodes through highly standardized and commonly available flexible printed circuit board (flex-PCB) technologies where the production cost is optimized for high ∗ volume markets. Polyimide, the most common substrate for flex- Corresponding author. Tel.: +1 919 515 7349. PCB production, is a biocompatible material [6]. These substrates E-mail address: [email protected] (A. Bozkurt). 1 This work was performed while A.B. was at Cornell University. are often covered with copper as a conductive layer, which can 0924-4247/$ – see front matter © 2011 Elsevier B.V. All rights reserved. doi:10.1016/j.sna.2011.05.015 90 A. Bozkurt, A. Lal / Sensors and Actuators A 169 (2011) 89–97 Fig. 1. Cross-section diagram of the one-layer flexible circuit board electrode (*immersion gold, ** electroplated gold). Nickel–phosphorus layer is only for immersion plating (ENIG). easily be coated with gold for biocompatibility as a standard part The tissue growing through these orifices provides mechanical of the flex-PCB production line. In addition to these, the elec- anchoring in in vivo setups, but that is not in the scope of this trode size (50–100 m on each side) and density (50–100 m paper. pitch size) can be determined with conventional flex-PCB technolo- Laser drilling and milling have been widely used to define minia- gies, which can be successfully accommodated for insect-biobot ture structures on flex PCB substrates. Carbon rich debris has been applications. Using this manufacturing technology, the circuit known to occur as a result of photothermal and photochemical components for control and data handling can also be directly mechanisms leading to the ablation of the polymer [9]. To remove assembled on the microelectrode substrate, which is a beneficial the laser ablation debris, we cleaned the received probes ultrason- property in terms of the size, power, and noise performance of the ically by soaking them in acetone and then isopropyl alcohol (IPA) electronics. baths, each for 10 min. Acetone and IPA are known to affect the So far, the use of flex-PCB technology in neural engineering molecular orientation of the polyimide; meanwhile, the ultrasonic research has been limited to manufacturing flexible interconnects pulsing has the potential to irritate the deposited gold surface, so between silicon-based microelectrode arrays and control micro- we performed an electrochemical analysis to characterize the effect electronics [7]. This technology also has been incorporated in of the probe cleaning procedure. in vitro culture dishes to “record” the electrical activity of cultured cardiac-cells [8]. The fabrication and use of implantable in vivo flex- 2.2. Electrochemical deposition PCB “stimulation” electrodes, however, require further analysis and modification. To enhance the electrochemical properties of the flex-PCB In this study, we report on the improvement of electrical and electrodes, we electrodeposited iridium oxide and electropolymer- electrochemical behavior of flex-PCB probes that will be used as ized poly(3,4-ethylenedioxythiophene) poly(styrene-sulfonate) implantable insect tissue stimulation microelectrodes. We present (PEDOT-PSS) over the gold coated electrodes to facilitate extra the in vitro characterization of morphological, electrical, and elec- charge transfer across the interface. For the deposition of iridium trochemical properties of these surface modifications through oxide, we followed a recipe similar to [10]. Seventy-five milligrams scanning electron microscopy, cyclic voltammetry, electrochemi- of iridium (IV) chloride hydrate was dissolved in 50 ml of deionized cal impedance spectroscopy, and current pulsed voltage excursions water by stirring for 30 min at room temperature, which formed in phosphate buffered saline solutions. a black colored solution. Then, 0.5 ml of 30% hydrogen peroxide solution were added to the solution and stirred for 10 min, which 2. Methods and materials turned the color of the solution to yellow. Adding 250 mg of oxalic acid dihydrate turned the color of the solution blue, and that was 2.1. Flexible printed circuit board fabrication stirred for another 10 min. Small amounts of anhydrous potassium carbonate were added to the solution slowly, until a pH of 10.9 was The layouts of the stimulation electrodes were prepared using obtained. The solution was kept at room temperature for 2 days to Target3001 software (Ing.-Buero FRIEDRICH, Germany) and the reach equilibrium before the deposition. generated Gerber files were submitted to Hughes Circuits, Inc. (San PEDOT-PSS monomer solution was prepared by stirring Marcos, CA, USA) for production. For the substrate, 100 m (∼4 mil) 35 mg of 3,4-ethylenedioxythiophene (EDOT) with 250 mg ® TM thick Kapton polyimide film (AP8545, DuPont , DE, USA) was poly(styrenesulfonic acid sodium salt) in 25 ml of deionized water 2 used, which was laminated with 17 m (0.5 oz/ft ) thick copper for 2 h until all of the globules