Skin-Like Disposable Tattoo on Elastic Rubber Adhesive with Silver

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Skin-Like Disposable Tattoo on Elastic Rubber Adhesive with Silver Particles Penetrated Electrode for Multi-Purpose Applications Seoungwoong Park, Mingyeong Kim, dain kwak, GaHyeon Im, and Jong-Jin Park ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b03057 • Publication Date (Web): 10 May 2018 Downloaded from http://pubs.acs.org on May 10, 2018

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ACS Applied Materials & Interfaces

Skin-Like Disposable Tattoo on Elastic Rubber Adhesive with Silver Particles Penetrated Electrode for Multi-Purpose Applications

Seoungwoong Park, Mingyeong Kim, Dain Kwak, GaHyeon Im, and Jong-Jin Park*

School of Polymer Science & Engineering, Chonnam National University, Gwangju 61186, Republic of Korea *Corresponding authors: [email protected]

Keywords: nanoconfinement effect, Ag penetrated electrode, confined-area reduction, free-standing transfer printing, attachable electrode

Abstract We propose a silver precursor with in-situ reduction under an adhesive substrate with a silver precursor penetration effect. It shows a high durability under mechanical deformation resulting from the composite form of the Ag-penetrated electrode adhesive. This stretchable electrode in which the silver particles are tightly penetrated into the adhesive with a confining effect can be used for various purposes since it offers water-proof properties and a high mechanical stability up to 70% strain, radius of curvature 0.5 mm (R / R0< 1.5), and electrical resistance of 0.58 ± 0.063 kΩ□-1 by adhering to the multi-purpose application.

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Recently, the fabrication of flexible electronics has attracted much attention from researchers focusing on the various methods to form electrodes. These fabrication methods generally disallow using brittle substrates and require a highly durability against deformed states due to compression, concave, folding and so on with pliable substrates and multi-dimensional (nD) materials. 1D electrodes to fabricate soft electrodes with a high conductivity are based on the fundamental percolation effect. In previous reports, the representative of 1D based materials, such as silver nanowire (AgNW),1-5 copper nanowire (CuNW)6, 7 and carbon nanotube (CNT)8-10 have been applied as soft electronics and have gained a great deal of interest due to their potential in applications with flexible and/or stretchable touch screens11, 12, energy harvesting devices,3, 8 human monitoring sensor,1, 9, 13-15 and electronic skins (e-skins).16, 17 In particular, the John A. Rogers group has announced multiple devices for e-skin using a gold circuit on the skin, and many research groups have also published results for e-skin.18 - 20 However, among these, applications using various substances have serious weaknesses, including a high cost, low adhesive property on hydrophobic pliable layer, difficultly in dispersion, to avoid conductive materials cracking from the existing protecting layers on the conductive electrode.4, 5, 9 The intrinsic electrode is brittle against external deformations when just fixed to the housing material with an embedded effect.1, 5, 21 Therefore, obscure flexible conductive pathway materials must be pressed using a composite form consisting of organic and metal materials.1, 5, 21, 22 There has been research to overcome the disadvantage of this housing needed, and one of these are the nanofibers that are confined to the Ag nanoparticles on or inside the fiber by electrospinning and using surface-embedded Ag nanoparticles with poly(styrene-b-butadiene-bstyrene) (SBS)as a stretchable rubber, which showed good stretchable conductivity and 3D adhesion.21, 23 ZhenanBao, Chung and colleagues demonstrated a highly-stretchable semiconductor polymer with an elastomer through a nanoconfinement effect over a substrate for a highly stretchable polymer.21 In our study, we suggest a skin-like disposable tattoo with Ag particles penetrating the electrode. The material should be made robust by using a highly-durable adhesive substrate via noble confined-area reduction between the elastic rubber adhesive substrate dissolved in a solvent-based silver precursor and a reducing agent. This method comprises a facile, one-step reduction process with silver nanoparticles due to the penetration of Ag particles into the rubber adhesive without the need for a high thermal energy to reduce the silver nanoparticles. The penetrated silver salt exhibits a confinement effect via drop-casting with a reducing agent with a confined-area reduction, and the method results in absorbing the propagation energy against a deformation force by surrounding the rubber and Ag particles penetrated into an elastic adhesive (Ag-PEA) layer due to the confinement effect of the silver that is tightly penetrated into the elastic adhesive. Furthermore, we can fabricate various wearable devices, such as adhesive heaters, that are tightly transferred on the textile strain sensor as well as attachable electrodes on paper. Figure 1a shows a schematic of the confined-area dissolving of the adhesive elastic layer from a silver precursor with an optimized condition of electro-hydrodynamic narrow-nozzle-to-substrate distance printing (e-NDP).24 The elastomeric adhesive rubber was coated on an eco-flex (adhesive / eco-flex) with a bar-coater (Figure S1). When patterning on the adhesive substrate, we can produce the patterning on a tunable line width obtained from a pre-penetrated silver salt electrode with a controlled pattern speed and nozzle-to-substrate distance (Figure 1b), (Figure S2).25 The pre-patterned infiltrated silver salt was reduced from the drop-casting method with diluted hydrazine monodehydrate in ethyl alcohol (20 wt%). At that time, the hydrazine monodehydrate was dissolved in a dilute aqueous solution, which should be possible with the confined-area reduction by e-NDP. As a result, silver nanoparticles confined in the adhesive layer can be made, and the hydrazine can be completely removed via vacuum exhaustion to produce a harmless electrode on the skin (Figure 1b, Figure S3). Figure 1c shows that the additional stretching with the penetrated effect can reach 0% to 70%. These characteristics are suitable for creating tattoo-type electronic devices applicable to the human body (step 1).Afterward, all of the residue solvent evaporation (at 65 °C for 30 min) formed an electrode attached on the eco-flex (6:4). These can be transferred onto the eco-flex (6:4) substrate with a difference in the


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interfacial adhesive energy (first transferred electrode). The first transferred electrode attached to the skin or textile substrate for the second transfer printing to fabricate the stretchable sensors (Figure 1d, e), (step 2).25 Figure 1f shows second transferred electrode on the back of the one`s hand with compressed state of electrode as shown in Figure 1g with ensuring a tight sealing on the human skin (Figure S4).

Figure 1. Schematic illustration of the method to manufacture a free-standing Ag-PEA penetrated patch type electrode. a) Silver precursor micro-pattern array on the adhesive/substrate. b) Drop casted reduction ink on a silver pre-penetrated electrode with a confined-area reduction. c) Pattern on adhesive / eco-flex stretchable electrode (step 1). d) First transfer printing on Ecoflex (3:2) used as a receiver for the second transfer printing. e) Attached on any substrate with second transfer printing. f) Attached on the back of the one`s hand Ag-PEA disposable tattoo electrode g) Compressed Ag-PEA disposable tattoo electrode.

Figure 2a, b shows the Ag-PEA tattoo FE-SEM cross-sectional image. This silver penetrated electrode has silver particles with a confined effect with an organic solvent penetrated with silver salt at the inner section of the adhesive elastic layer (Figure S5). Also, there is a microthickness, spontaneous formation of a robust electrode resulting from the continuous phase of the elastic adhesive incorporated with rubber properties (Figure S6), like a buffer,against external deformation forces. The silver particles that penetrated the electrode have a damping layer with rubber, with which the patterned electrode formed an inner silver nanoparticle percolation network. Figure 2c shows the Ag-PEA grasping the pre-patterned infiltrated silver salt and reduced silver nanoparticles. FT-IR was used to observe the pristine adhesive substrate and pre-patterned silver salt. After all of residue solvent has dried, the Ag-PEA penetrated electrode still has the two absorbance features for C-F stretching at 1,150 cm-1 and 1,216 cm-1. Therefore, these two peaks indicate that the reduced silver nanoparticle penetrated into the adhesive elastic active layer with an adhesive rubber peak (C=C) as a result of showing the confinement effect.26 This Ag-PEA has a high silver binding energy compared to a pattern on a polyethylene terephthalate (PET) substrate. Figure 2d shows the relationship of the silver precursor penetration effect and the binding energy of the inter-particle percolation network, we performed X-ray photoelectron spectroscopy (XPS). The process to form the electrode patterns has a different value for the binding energy according to the silver penetrated effect as a result of the formation of nanoparticles in the elastic adhesive layer. The pattern on the PET substrate observed under XPS shows two peaks at 369 eV and 375 eV. When using the penetrated electrode in the elastic adhesive layer, the XPS results for the



Ag-PEA tattoo show a somewhat increased binding energy in 3 and 3 (1 eV).24 Therefore, using this as a buffer for the patterned adhesive substrate has a confining effect of the Ag particle percolation network with elastic properties. Figure 2e shows a penetrated phenomenon affecting the electrode roughness measured using a non-contact 3 dimensional optical compiler (3D-OP). The pattern on the Ag-PEA surface roughness (Ra = 45 nm) is lower than the pattern on the PET substrate (570 nm). In the case of the pattern and reduction on the PET substrate, there is an irregular reduction at a low processing temperature. On the other hand, a wellordered coated elastic adhesive rubber is at the top of the housing materials when the silver penetrated into the elastic adhesive rubber. There is a good surface roughness without a high temperature during sintering. Figure 2f shows the Ag-PEA tattoo sheet resistance value (Ω□-1) followed over the patterning cycles (1, 3, 5) and patterning speed (3, 5, 10 mm s-1).When the e-NDP process is applied on the adhesive substrate, there can be a controllable sheet resistance with a fixed flow rate of 3.0 µl min-1. Therefore, we can fabricate the tunable conductive electrodewith the over printing of silver precursor, the amount of silver salt to be spread over a unit area will also be increased by an accumulation thereon; this leads to an additional formation of a percolation network after the reduction. When there is an over printing over 6 times, only the pattern width will be increasing, and this eventually degrades the resolution thereof without further increasing electrical conductivity.This electrode resistance has 3 mm s-1/ 0.58 ± 0.063 kΩ□-1, 5 mm s1

/1.18 ± 0.12 kΩ□-1 and 10 mm s-1/5.463 ± 0.048 kΩ□-1 with a 1-cycle patterning. When patterning on the adhesive substrate, the silver

precursor penetrates into the adhesive active layer and dissolves 3.0 wt% with the optical transmittance (> 80 %) (FigureS7a).

Figure 2. Characteristic analysis of the patterned electrode. a), b) Cross-section FE-SEM image of silver penetrated patch type electrode; FETEM image energy-dispersive X-ray spectroscopy (EDS), silver and carbon of Ag-PEA mapping image (inset). c) Fourier-transform infrared spectroscopy(FTIR) analysis of the processing step for fabricating Ag-PEA penetrated electrode.(The C-F stretching of the pre-infiltrated silver salt electrode at 1,132 cm-1 and 1,185 cm-1 shows two strong peaks at the pre-patterned material penetrating into the adhesive elastic rubber).d) XPS analysis of pattern on PET and adhesive substrate, there are different binding energies plotted with the penetrated effect. e)


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PET and penetrated electrode roughness average value (Ra) via non-contact 3D-OP. f) Tunable resistance printing with over printing cycles and printing velocity.

Therefore, we can fabricate a flexible and stretchable electrode using step 1 (included substrate) or step 2 (free-standing skin-like electrode). Using step 1, the fabricated electrode has robust properties with radius of curvature Rc is 0.5 mm, R / R0< 1.5 against a flexible state deformation on the adhesive/PET structural electrode as shown in Figure S7.The durability of the electrode shows a somewhat increasing resistance ratio arising from the silver-penetrated electrode with a silver particle confinement surrounded by rubber. Figure3a presents the step 1-patterned electrode with a stretched state (30%) for wearable electronics. The top part of the Ag-PEA absorbed the energy of the deformation propagation, which ripped at the stretched state. However, the Ag electrode has not been damaged in terms of its electrical resistance due to the inner Ag penetrated percolation network. Also, the undamaged part of the electrode can undergo stretching under the thickness of the elastic adhesive rubber with silver particles that are slightly rising to the top of the electrode. Thus, it was possible to produce a stretchable tattoo with a superior repeatability, as shown in Figure 3b, c in the FE-SEM image and photo image (Figure S8). Figure 3d shows the Ag-PEA stretching test deformation rates (30%, 50%, 70%, respectively) for 1000 measurement cycles. After, all measurement test R/R ratio valueswere under 1.2. As such, the tattoo can be applied on an elastic substrate. Figure 3e shows the step 2 process on the textile substrate. Also, the Ag penetration effect produces a chemical stability with sonicating treatment (used as a basic cleaning solvent) such as with water, ethanol and iso-propyl alcohol (IPA) at 25°C for 15 mins with 10 repeated cycles (Figure 3f).27 In addition, we conducted patterning on paper substrates that are widely used for low-cost disposable devices through a crumping test (100 times), and the Ag-PEA showed a high durability of 1.15 at the R/R value ratio change. We fabricated the step 2 process based on a stickertype LED to a peacock-shaped origami structure using its excellent adhesive properties (Figure 3g, h, detail explain Figure S9).The dimensions of the LED used were 3.20 mm (L) x 1.60 mm (W)x 1.10 mm (H). It was of forward bias and can be activated with a 3V battery. Our conductor of the LED, the electrode (3 Ω □-1), capable of 5 consecutive printings at a printing speed of 3 mm/s, was used without any issue related to heating.



Figure3. Schematic illustration of Ag-PEA penetrated electrode stretched state. a) Stretched electrode has somewhat torn in upper layer, but in fixed electrical resistance inner percolation network. b), c) As shown FE-SEM image of stretched state Ag-PEA penetrated electrode. d) Stretching fatigue test with (30 % to 70%). e) Printed on textile (step 1. process). f) Sonication test with washing solvent for proving water proof and chemical stability. g), h) Using (step 2. process) for applying paper origami structure on attachable LED, inset, scale bar, 0.5 cm and toughness property against crumping test.

Figure 4a shows a photograph of the Ag-PEA sticker on the textile substrate. It is tightly attached to polyurethane-based textiles and does not need a glue solution for use with e-skin electronics.17, 28 Figure 4b shows the Ag-PEA / textile hand and elbow bending strain sensor. This sensor is very stable with its stretchable properties which is adaptive for our e-skin (R/R0 is > 1.5). However, the stretched state of the Ag-PEA is obtained by tearing up the upper percolation network. The distance of the silver particles to each other increases, so the electrical resistance (R / R0) value rapidly increases. When the Ag-PEA is let loose into the pristine shape of the electrode, the silver particle-to-particle distance decreases and, at the same time, the electrical resistance of the Ag-PEA returns to its original state. We also measured the human walking motion as the interval walking time. This function can analyze the human gait interval for a long time periodically or irregularly. If the user has an irregular walking impairment, it indicates it is “too fast” to send the wireless arduino signal to a mobile phone and so identify early signs of dementia.29 (irregular walking time) (Figure 4c). Figure 4d shows a slow and/or fast gait measurement value. The initial state for slow walking has a long time interval with a left inserted image (in this case: normal walking). When fast walking has a short interval time (right inserted image) with highly sensitive repeatable strain sensors (in this case: Too fast). Average values of the walking interval sensor (R/R0) were 1.8 at the slow gate and 2.1 at the fast gate; the standard deviation of the 100 values of walking was less than 0.22 and it was reliable (Figure S10)


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Figure 4e shows a photograph of an attachable curved shape of Ag-PEA / PET heater including an infrared thermal image. The conductor for Joule heater, the electrode (1 kΩ □-1) of a single printing at a printing speed of 3 mm/s, was easily heated due to the low electrical conductivity.This type of heater is easy to attach onto any substrate with a preheating feature containing water (step 1.). In particular, the attachable heater operates at 3.7 V (mobile phone output voltage) at 45.3 °C for a wearable heater or heats water. Figure 4f shows that the heating range can be controlled over the temperature of the applied voltage through patterning cycles (Figure S11).

Figure4.Attachable electrode applications for human motion sensing and as a Joule heater. a) Photograph of Ag-PEA transferred (Step 2.) on a textile FE-SEM image, b) Ag-PEA transferred on a textile strain sensor with finger and elbow motion (R / R0). c) Walking interval analysis transferred via a Bluetooth Arduino module. d) Slow and fast walking interval value (R / R0), in case of fast walking, the mobile phone display prints “Too fast” and under normal walking prints “Normal” (inset). e) Attachable heater with a curved shape of the Ag-PEA (Step 2.) pattern, which can be patterned and attached on a water-filled PET bottle for heat insulation water. e) Attached to the textile heater with a tunable heating range through patterning cycles, f) Tunable range of the heating temperature following the applied voltage (V).

In summary, we can fabricate stretchable electrodes with the silver-penetrated confinement effect derived from the Ag penetration effects on all substrates, including elastic rubber, polymer films, paper, and textile substrates via e-NDP. This pattern printing method allows for controllable results from the printing conditions, which included an adjustable sheet resistance of 3 mm s-1/ 0.58 ± 0.063 kΩ□-1, 5 mm s1

/1.18 ± 0.12 kΩ□-1 and 10 mm s-1/5.463 ± 0.048 kΩ□-1 at 1-cycle patterning. Increasing the patterning cycle increase the electrical

conductivity depending on the application. The Ag-PEA exists in the composite form of the confinement effect, and the elastic adhesive layer absorbs the propagation energy in the flexible state. The stretched state of the Ag-PEA also absorbs the propagation energy to the ripped top of the silver particle percolation network. We demonstrated that the silver-penetrated adhesive electrode was suitable for use as a dementia sensor, human motion, strain sensor, and adhesive wearable heater.



ASSOCIATED CONTENT Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI: am-2018-030572. Experimental details, measurement method of electrical conductivity of Ag-PEA. Bar-coated elastic adhesive layer (Figure S1). Characterization of e-NDP (Figure S2), determined reduction process (Figure S3). Over view of optical images of Ag-PEA (Figure S4). Penetrated silver particles (Figure S5). Optimization of thickness of elastic adhesive layer (Figure S6, Table S1).Detail explain ofAg-PEA flexibility (Figure S7), stretchable Ag-PEA (Figure S8). Attachable LEDs (Figure S9), walking interval sensor stability (Figure S10), attachable heater infrared thermal image (Figure S11).

AUTHOR INFORMATION Corresponding Author [email protected] ORCID SeoungwoongPark : 0000-0002-5958-4050 MingyeongKim : 0000-0002-0946-9046 Dain Kwak : 0000-0001-9642-4227 Ga Hyun Im : 0000-0002-5958-7614 Jong-JinPark : 0000-0002-7196-9789

Notes The authors declare no competing financial interest.

ACKNOWLEDGEMENTS This research was financially supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education (NRF-2015R1D1A1A01057245) and additional support was provided by the Ministry of Trade, Industry & Energy (MOTIE, Korea) under the Industrial Technology Innovation Program. No.10067151, smart device connected and textilebased smart function mounted outdoor garment for smart life with ergonomic design.This research was also supported by the Energy Efficiency & Resourcesof the Korea Insitute of Energy Technology Evaluation and Planning(KETEP) grant funded by the Korea government Ministry of Knowledge Economy (No. 20172020109240).

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Skin-Like Disposable Tattoo on Elastic Rubber Adhesive with Silver

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