Self-Aligned Inkjet Printing of Resistors and Low- Pass RC Filters on Roll-To-Roll Imprinted Plastics with Resistances Ranging from 10 to 106 Ω

IOP Publishing Journal Title Journal XX (XXXX) XXXXXX https://doi.org/XXXX/XXXX

Self-Aligned Inkjet Printing of Resistors and Low- Pass RC Filters on Roll-to-Roll Imprinted Plastics with Resistances Ranging from 10 to 106 Ω

Motao Cao, Krystopher Jochem, Woo Jin Hyun, Lorraine F. Francis and

C. Daniel Frisbie

Department of Chemical Engineering and Materials Science, University of Minnesota, 421 Washington Avenue S.E., Minneapolis, Minnesota 55455, United States

E-mail: [email protected], [email protected]

Received xxxxxx Accepted for publication xxxxxx Published xxxxxx

Abstract

Resistors are essential and ubiquitous building blocks in electronic circuits. Fabrication of printed resistors in a manner compatible with roll-to-roll printing is important for realizing low-cost and high-throughput production of electronic devices. Here we present fully printed resistors fabricated via a novel self-aligned printing method termed SCALE (Self-aligned Capillarity Assisted Lithography for Electronics). Flexible substrates with imprinted features such as reservoirs and capillary channels were prepared by roll-to-roll processing. Functional inks were then delivered sequentially into the reservoirs by inkjet printing and the ink flowed spontaneously into the adjoining channels driven by capillarity. Poly(3,4-ethylene dioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) was used as the resistive material, and silver was used for the electrodes. Using SCALE, we achieved fully inkjet-printed, self-aligned resistors with resistance values ranging over five orders of magnitude while keeping the overall dimensions of the devices constant. We then employed SCALE to build low- pass RC (resistor-capacitor) filters with cutoff frequency from 0.4 - 27 kHz and excellent operational stability. Overall, this work expands the potential of self-aligned inkjet printing for producing fully printed electronic circuits.

Keywords: resistors, inkjet printing, PEDOT:PSS, RC filter, flexible electronics

contact operation, materials compatibility, minimal material 1. Introduction waste, and widespread commercial acceptance [8-22]. However, its application in high-throughput roll-to-roll The use of printing strategies for production of flexible processing of multilayered microelectronic circuits is limited circuits on plastic or paper substrates is attractive for several currently by poor resolution and materials registration reasons including the compatibility of printing with challenges. continuous, roll-to-roll processing, scalability to large areas at To solve this problem, a novel inkjet-based printing method lower cost, and reduced materials waste by eliminating called self-aligned capillarity-assisted lithography for subtractive etching steps [1]. Printed and flexible circuits have electronics (SCALE) has been developed [23]. The SCALE potential applications in large area sensor arrays [2], wearable process starts with imprinting a multi-level network of open electronics [3], displays [4], smart labels [5], and medical reservoirs, capillaries, and device cavities in a UV curable diagnostics [6, 7]. Among printing techniques, inkjet printing coating on a flexible substrate. Subsequent materials has been widely used for printed electronics demonstrations deposition and layer-to-layer alignment is achieved by due to its numerous advantages including digital control, non- xxxx-xxxx/xx/xxxxxx 1 © xxxx IOP Publishing Ltd

Journal XX (XXXX) XXXXXX Author et al inkjetting electronic inks sequentially into the easy-to-hit PEDOT:PSS ink formulation to adjust resistivity, as just reservoirs, followed by spontaneous capillary flow of the inks described. We achieved resistors on plastic substrates with via open channels into cavities shaping discrete electronic resistances varying from 10-106 Ω. The resistors were robust components. The SCALE process thus combines imprint to bending strains of up to 1% and to thousands of repeated lithography with inkjet printing to enhance printed resolution electrical measurements. To test dynamic performance, we - linewidths of 1 μm are readily achievable - while printed low-pass RC (resistor-capacitor) filters. The simultaneously simplifying materials registration. An fabrication of RC filters by inkjet printing was first reported additional benefit of SCALE is that crisp, well-defined line by Varahramyan and colleagues [42-44]. Then, Castro, et al. edges characteristic of conventionally photopatterned demonstrated all-inkjet-printed low-pass filters with cutoff materials are readily obtainable, which is not typical of inkjet frequency from 82 Hz to 740 Hz by applying printed organic printing [24, 25]. thin-film transistors [45]. Here we demonstrate fully printed Already, successful fabrication of discrete circuit elements low-pass RC filters with cutoff frequencies over three orders including transistors, capacitors, and resistors on individual of magnitude by varying the resistance. Collectively, the plastic sheets has been demonstrated by SCALE [23, 26-30]. results demonstrate that the SCALE process has excellent However, the use of SCALE and roll-to-roll processing to potential for self-aligned printing of resistors and RC filters create resistors with resistances over many orders of necessary for building more advanced electronic systems on magnitude has not been demonstrated. As resistors are flexible substrates. ubiquitous electronic building blocks, this is a crucial challenge for the ultimate goal of roll-to-roll printing of 2. Experimental Section complete circuits. Indeed, printed resistors have been realized utilizing screen printing [31-34], stencil printing [35], aerosol 2.1 Silicon master template fabrication jet printing [36] and inkjet printing [24, 37-39], but these The silicon master template was fabricated by two rounds fabrication procedures were not completely compatible with of traditional photolithography. (a) Patterning the recessed self-alignment and/or roll-to-roll processing. Thus, in this reservoirs and channels for electrodes: A 4-in silicon wafer paper we focus on demonstrating SCALE-based, roll-to-roll was heated at 115 ºC for 1 min to remove the water molecules approaches to creating resistors with resistances spanning on the top surface. Then the wafer was treated in a many orders of magnitude. hexamethyldisilazane (HMDS) atmosphere for 4 min. A layer Key to this effort is the choice of printable resistive of photoresist (Microposit S1813, Dow) was spin-coated onto materials. Poly(3,4-ethylene dioxythiophene):poly(styrene the silicon wafer at 3000 rpm for 30 s. The wafer was soft- sulfonate) (PEDOT:PSS), which has been widely used as both baked at 115 ºC for 1 min and then exposed to UV light for 5 a conductive and a resistive material in printed electronics, is s under a photomask designed for the electrodes. The wafer an ideal material due to its adjustable resistivity and good was developed in a mixture of Microposit 351 (Dow) and printability. It has been reported that the resistivity of deionized water (1:5 v/v) for 30 s. The exposed area of the PEDOT:PSS films deposited from the commercial PH1000 wafer was dry etched down to a depth of 7 μm in a deep trench ink (Heraeus) can be decreased by adding a small amount of etcher (SLR 770). The photoresist was then washed off by high boiling point solvents such as dimethyl sulfoxide acetone and the wafer was immersed in Piranha solution (DMSO) and ethylene glycol (EG) [40, 41]. Jung, et al. (H2SO4 and H2O2, 1:1) for 20 min at 120 ºC to clean the reported inkjet-printed resistors using PEDOT:PSS PH1000 residual photoresist. (b) Patterning the raised ink receivers: inks [24]. They modified the film resistivity by varying the SU-8 2010 photoresist (MicroChem) was spin-coated onto the concentration of DMSO added into the solution. Also, Ali et same silicon wafer at 500 rpm for 5 s and then at 2000 rpm for al. increased the resistivity of PEDOT:PSS films from 48 to 30 s, followed by baking at 65 ºC for 3 min and 95 ºC for 7 210 mΩ·cm by blending poly(methyl methacrylate)(PMMA) min. The photoresist was then exposed to UV light for 24 s into PH1000 PEDOT:PSS ink [25]. Though not explored through the photomask designed for the raised walls. The here, carbon based inks can also be used to print the resistive exposed wafer was heated at 65 ºC for 1 min and 95 ºC for 7 layer. Chang, et al. blended high (Dupont 5036) and low min. The wafer was immersed in 1-methoxy-2-propanyl (Dupont 7082) resistivity carbon materials and achieved a acetate for 5 min to develop the photoresist and then rinsed resistance range from 3.3 kΩ/□ to 800 kΩ/□ using screen with isopropyl alcohol. Lastly, the wafer was baked at 180 ºC printing [32]. for 10 min. In order to make resistors having resistance ranging over orders of magnitude, but with the same spatial footprint, which 2.2 PDMS Stamp Fabrication is important for circuit layout considerations, we employed a two-pronged strategy in which the distance between printed The silicon master template was first silane-treated in a electrodes was changed in concert with alterations of the vacuum chamber overnight with trichloro(1H,1H,2H,2H- perfluorooctyl)silane (Aldrich). A curing agent and PDMS

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Journal XX (XXXX) XXXXXX Author et al roll processing. Future work will focus on shrinking the size [13] Sirringhaus H, Kawase T, Friend R H, Shimoda T, of the reservoirs to further reduce the footprint and integrating Inbasekaran M, Wu W and Woo E P 2000 Science 290 the resistors into flexible circuits. 2123-6 [14] Ng T N, Wong W S, Chabinyc M L, Sambandan S and Acknowledgements Street R A 2008 Appl. Phys. Lett. 92 213303 [15] Kawase T, Sirringhaus H, Friend R H and Shimoda T The authors thank two undergraduate students Yuheng 2001 Adv. Mater. 13 1601-5 Miao and Alayna Erickson for their help in completing this [16] Ng T N, Mei P, Schwartz D E, Kor S, Krusor B, Veres J, project. This work was supported by the Multi-University Bröms P, Eriksson T, Wang Y, Hagel O and Karlsson C Research Initiative (MURI) program sponsored by the Office 2015 SPIE Organic Photonics + Electronics 9569 6 of Naval Research (MURI Award N00014-11-1-0690). [17] Tobjörk D, Kaihovirta N J, Mäkelä T, Pettersson F S and Additional support was provided by the National Science Österbacka R 2008 Org. Electron. 9 931-5 Foundation (NSF) under grant number CMMI-1634263 and [18] Khan Y, Pavinatto F J, Lin M C, Liao A, Swisher S L, Mann K, Subramanian V, Maharbiz M M and Arias A C the Xerox Research Centre of Canada. Krystopher Jochem 2016 Adv. Funct. Mater. 26 1004-13 further acknowledges support from the National Science [19] Whiting G L and Arias A C 2009 Appl. Phys. Lett. 95 Foundation Graduate Research Fellowship Program under 253302 Grant No. 00039202. The authors thank Prof. Jennifer Lewis [20] Lessing J, Glavan A C, Walker S B, Keplinger C, Lewis J (Harvard University) and Dr. Brett Walker (Electroninks, A and Whitesides G M 2014 Adv. Mater. 26 4677-82 Inc.) for providing silver ink and for collaboration on the use [21] Zirkl M, Sawatdee A, Helbig U, Krause M, Scheipl G, of the ink in SCALE. Parts of this work were carried out at the Kraker E, Ersman P A, Nilsson D, Platt D, Bodö P, Bauer Characterization Facility, University of Minnesota, which S, Domann G and Stadlober B 2011 Adv. Mater. 23 2069- receives partial support from NSF through the MRSEC 74 program. Portions of this work were conducted in the [22] Homenick C M, James R, Lopinski G P, Dunford J, Sun Minnesota Nano Center, which is supported by the National J, Park H, Jung Y, Cho G and Malenfant P R L 2016 ACS Science Foundation through the National Nano Coordinated Appl. Mater. Interfaces 8 27900-10 Infrastructure Network (NNCI) under Award Number ECCS- [23] Mahajan A, Hyun W J, Walker S B, Rojas G A, Choi J H, Lewis J A, Francis L F and Frisbie C D 2015 Adv. 1542202. Electron. Mater. 1 References [24] Jung S, Sou A, Gili E and Sirringhaus H 2013 Org. Electron. 14 699-702 [1] Ivanova O, Williams C and Campbell T 2013 Rapid [25] Ali S, Bae J and Lee C H 2015 Appl. Phys. A 119 1499- Prototyping. J. 19 353-64 506 [2] Yao S and Zhu Y 2014 Nanoscale 6 2345-52 [26] Hyun W J, Bidoky F Z, Walker S B, Lewis J A, Francis L [3] Wataru H, Shingo H, Takayuki A, Seiji A and Kuniharu T F and Frisbie C D 2016 Adv. Electron. Mater. 2 2014 Adv. Funct. Mater. 24 3299-304 [27] Hyun W J, Secor E B, Kim C H, Hersam M C, Francis L [4] Street R A, Wong W S, Ready S E, Chabinyc M L, Arias F and Frisbie C D 2017 Adv. Energy Mater. A C, Limb S, Salleo A and Lujan R 2006 Mater. Today 9 [28] Mahajan A, Hyun W J, Walker S B, Lewis J A, Francis L 32-7 F and Frisbie C D 2015 ACS Appl. Mater. Interfaces 7 [5] Street R A, Ng T N, Schwartz D E, Whiting G L, Lu J P, 1841-7 Bringans R D and Veres J 2015 Proc. IEEE 103 607-18 [29] Song D, Bidoky F Z, Hyun W J, Walker S B, Lewis J A [6] Yeo W H, Kim Y S, Lee J, Ameen A, Shi L, Li M, Wang and Frisbie C D 2018 ACS Appl. Mater. Interfaces 10 S, Ma R, Jin S H, Kang Z, Huang Y and Rogers J A 2013 15926-32 Adv. Mater. 25 2773-8 [30] Woo Jin H, Ethan B S, Fazel Zare B, Walker S B, Jennifer [7] Corea J R, Lechene P B, Lustig M and Arias A C 2017 A L, Mark C H, Lorraine F F and Frisbie C D 2018 Magn. Reson. Med. 78 775-83 Flexible and Printed Electronics 3 035004 [8] Calvert P 2001 Chem. Mater. 13 3299-305 [31] Numakura D 2008 2008 3rd International Microsystems, [9] Gans B J D, Duineveld P C and Schubert U S 2004 Adv. Packaging, Assembly & Circuits Technology Conference Mater. 16 203-13 205-8 [10] Scheideler W J, Kumar R, Zeumault A R and [32] Chang J, Zhang X, Ge T and Zhou J 2014 Org. Electron. Subramanian V 2017 Adv. Funct. Mater. 27 1606062 15 701-10 [11] Ng T N, Schwartz D E, Mei P, Kor S, Veres J, Bröms P [33] Słoma M, Jakubowska M, Kolek A, Mleczko K, Ptak P, and Karlsson C 2015 Flexible and Printed Electronics 1 Stadler A W, Zawiślak Z and Młożniak A 2011 Journal of 015002 Materials Science: Materials in Electronics 22 1321-9 [12] Bucella S G, Salazar‐Rios J M, Derenskyi V, Fritsch M, [34] Ostfeld A E, Deckman I, Gaikwad A M, Lochner C M and Scherf U, Loi M A and Caironi M 2016 Adv. Electron. Arias A C 2015 Sci. Rep. 5 15959 Mater. 2 1600094

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