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Beyond Conventional Patterns: New Electrochemical Lithography with High Precision for Patterned Film Materials and Wearable Sensors Xiaowei Zhang, Shaojun Guo, Yanchao Han, Jing Li, and Erkang Wang Anal. Chem., Just Accepted Manuscript • DOI: 10.1021/acs.analchem.6b04816 • Publication Date (Web): 23 Jan 2017 Downloaded from http://pubs.acs.org on January 28, 2017

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Analytical Chemistry

Beyond Conventional Patterns: New Electrochemical Lithography with High Precision for Patterned Film Materials and Wearable Sensors Xiaowei Zhang, a,b Shaojun Guo, c Yanchao Han, a,b Jing Li, a,b,* and Erkang Wang a,b,*

a. State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun, Jilin, 130022, China.

b. Graduate School of the Chinese Academy of Sciences, Beijing, 100039, P. R. China.

c. College of Engineering, Peking University, Beijing 100871, China.

*Corresponding author: Assoc. Prof. Jing Li and Prof. Erkang Wang, Tel: +86-431-85262003, Email: [email protected] and [email protected]

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ABSTRACT

We report a simple, low-cost, and brand-new electrochemical lithography technique for replicating the template pattern with high resolution at ~2 µm. The developed method is that the electroactive material is first deposited on the patterned conductive template by the electrochemical technique, and then peeled by an adhesive tape/material. The resulting film with the precise pattern shows excellent mechanical and electronic properties and promises high prospect in designing flexible electronics. This interesting approach can be performed at ambient condition and easily generalized to pattern various electroactive materials covering metal, alloy, nonmetal, salt, oxide and composite on different types of substrates in several seconds to a few minutes, making the mass production of flexible/rigid/stretchable patterned thin films quite possible.


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INTRODUCTION Patterning techniques are changing the world, and new patterning techniques for film materials have received intensive attention because of their great importance in designing flexible electronics.

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Traditionally, the most commonly adopted methods are directly depositing and patterning materials on the flexible substrate, but suffer from the specific substrate selection (e.g. polydimethylsiloxane (PDMS),

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paper, 2,17-21 textile, 22-25 and polyimide 26-29 to meet the stringent requirements of safety,

flexibility, and strength. The biggest limination for the existed methods is in the depositing and patterning processes, the high-energy deposition techniques (E-beam, sputter, and vapor deposition) and the micro-electromechanical systems (MEMS, e.g. photolithography technique) were generally adopted, 1-3,30,31

which involve in the complicated fabrication processes, expensive instruments, and the

requirement of cleanroom environment, seriously limiting the mass production and practical applications of the resulting devices (ca. 1 h~ for every chip). To well solve these problems, the screenprinting, ink jet printing and flexographic printing techniques were employed to coat and pattern the substrate simultaneously, but still hampered by the problems of limited resolution (1200 dpi) and few printable inks available.

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Moreover, these techniques can hardly print the pure substance

(additives in the ink), which may interfere with the performance of resulting chips in some cases. Recently, some interesting lithography approaches have been developed, which use hard or soft stamps for patterning various materials with high resolution at ambient condition. These methods usually undergo a phase transition around (in many cases are “inside“) the stamp or use the self-assemble strategy and thus are limiting by the long reaction time and available "inks".

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In this regard, the

development of a fast, cheap, universal and high-precision method for the mass production of different types of flexible, rigid, stretchable, and patterned film is highly desirable yet a great challenge to date. Electroplating is a highly developed and adopted technique in the coating industry. However, no reports have demonstrated on the use of electroplating as an ingenious method to replicate the surface pattern of the substrate. This may be owing to that the researchers often prefer a stable coating so that major studies have been focused on improving the mechanical stability of the coating.

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On the

contrary, we feel the low coating adhesion is precisely an advantage when the electroplating is used as a copying technique. Inspired by this, we propose a simple yet brand-new electrochemical lithography technique to prepare large scale, flexible/rigid/stretchable, and patterned material thin films with high ACS Paragon Plus Environment

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resolution for developing flexible devices. Compared with the traditional techniques, the key feature of our new strategy for flexible and high-precision patterning is much faster and cheaper, which needs only two simple steps: electrodeposition and peeling (termed EDP, Scheme 1). That is, electroactive material was first deposited on the patterned conductive template by the electrochemical technique, and then peeled by an adhesive tape/material. The resulting films with precise patterns show excellent mechanical and electronic properties and promise high prospect in designing flexible electronics. EXPERIMENTAL SECTION Chemicals and Materials All the chemicals (analytical reagent grade) were used as received without any further purification. Chlorauric acid, silver nitrate, copper sulfate, ferric chloride, and potassium ferricyanide were purchased from Beijing Chemical Reagent Company (Beijing, China). Ru(bpy)3Cl2·6H2O, tripropylamine (TPrA) were purchased from Sigma–Aldrich Chemical Co. (Milwaukee, WI). Graphite oxide (GO) was prepared from natural graphite by a modified Hummers’ method. The synthesized GO powder was exfoliated in 1:1 pure water and ethanol by ultrasonication for 30 min to form homogeneous GO dispersions with a concentration of 1.0 mg/mL. Indiumtin oxide (ITO) and fluorine-doped tin oxide (FTO) coated glass substrate (sheet resistance: ~ 6 Ω/square) was obtained from CSG Holding Co., ltd. (Shenzhen, China). Au/Ti coated glass was prepared by the physical vapor deposition. Standard transparent tape and polyethylene terephthalate (PET) double-sided tape were obtained from 3M Co., USA. Nickel conductive adhesives were purchased from Shenzhen, China. Al foil tape was obtained from the local grocery. Silver-epoxy conductive adhesive was purchased from Sigma-Aldrich Chemical Co. (Milwaukee, WI). All the stock and buffer solutions were prepared with deionized water (18 MΩ cm−1) purified by a Milli-Q system (Millipore, Bedford, MA). Fabrication of the Patterned Templates The standard photolithographic technique was employed to fabricate patterned ITO, FTO, and Au templates (simple electrode, bipolar system, or the high-precision interdigital electrodes) for the following EDP strategy. First, the photomasks with the designed patterns for the patterned template were fabricated by a laser printer (with line width ≥ 60 µm), and the high-precision ones (line width: 10, 8, 6, 4 and 2 µm) were bought commercially (Figure S1). Second, RZJ 390 photoresist was spin-coated ACS Paragon Plus Environment

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onto the clean ITO/FTO/Au substrate (3000 rpm for 20 s) and prebaked at 95 °C for 5 min. Then, the coated ITO/FTO/Au substrate was covered by the photomask and exposed to the UV irradiation (365 nm, 15 mJ/cm2) for 9 seconds. 0.1 M NaOH was employed to remove the exposed photoresist layer. Exposed ITO, FTO, and Au coatings could be easily etched by the HCl-FeCl3, Zn-HCl, and I2-KI solution, respectively. And the patterned ITO/FTO/Au template was finally obtained by removing the remained photoresist with ethanol. The as-prepared ITO, FTO, and Au templates were cleaned and stored for the following EDP strategy.

RESULT AND DISCUSSION

Versatility of the EDP Technique. To perform the EDP method, the conductive and patterned templates were prepared by the standard photolithographic technique (Details in Supporting Information). Then, an electrochemical technique (Table S1, included but not limited) was employed to deposit an electroactive material onto the pattern of the indium tin oxide (ITO) template, followed by the use of a transparent adhesive tape (T-A tape) to peel off the patterned electroactive materials. During the whole EDP process, no visible damage to the patterned template was observed (after 30 EDP cycles, Figure S3. It should be noted that more than 100 EDP cycles have been performed with a single simple ITO electrode, Figure 1I), enabling the repeatable use of a single template for fabricating versatile or large amount of patterned films. Thus, it is not hard to find that the cost of EDP strategy is very low. In addition, the EDP method is highly controllable and very benefits from the highly developed electroplating technique. Another exciting feature is that the present simple EDP technique can be generalized to prepare various films consisting of Au, Ag, Cu, and Prussian blue (PB) (Figure 1Ia-d) in several seconds to a few minutes. Furthermore, with the patterned Au template, the patterned MnO2 films (Figure 1Ie) can be quickly produced as well. The synthesis of MnO2 can be used in industrial catalyst or a dry cell depolarizer. Most interestingly, the high-precision and patterned reduced graphene oxide (rGO) film, which is highly urgent in the modern electronics, can also be prepared by using the patterned fluorine-doped tin oxide (FTO) template (Figure 1If & g). From all above results, we believe that the EDP strategy can be widely expanded to prepare various electroactive materials covering metal, alloy, nonmetal, salt, oxide and even composite.


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The peeling step is also flexible, besides the T-A tape (Figure 1IIa), the double-side adhesive tape (D-A tape) can be applied to peel the patterned materials. Then, the D-A tape with patterned materials can be transferred to a rigid substrate, which is a core part of the traditional lab-on-chip device (Figure 1IIb). To our surprise, the flexible and stretchable films can be fabricated by peeling the deposited film with PDMS through a curing process (Figure 1IIc). Therefore, it is reasonable to conclude that any adhesive tapes or materials with enough mechanical strength and adhesive strength can be adopted for peeling the patterned material from the template. From all above results, the key points for the EDP generalization are concluded: (i) electroactive materials can be electrodeposited on the patterned template; (ii) both the intermolecular forces of the materials and the adhesive strength of the adhesive tape/material are stronger than the interaction between the materials and templates. Resolution of the EDP Technique. The established EDP method has quite high resolution for flexible and patterned film materials. As shown in Figure 2, the patterns with 60 µm, 10 µm, 8 µm, 6 µm, 4 µm, and 2 µm line width can be easily fabricated in several seconds to a few minutes. By testing in 0.5 M H2SO4 (Figure S4) using the cyclic voltammetry, it is demonstrated that the copied pattern with micron-grade line width is electrically connected. The scanning electron microscope (SEM) was employed to test the resolution of the EDP strategy. From Figure 3, it was found that the peeled patterns were highly consistent with the Au deposited on the templates. In addition, the line edge roughness of these patterns was relatively low (Figure 3c and f, 4 µm pattern: ± 0.2 µm; 2 µm pattern: ± 0.3 µm). What important is that the EDP strategy with such high resolution can be achieved at ambient conditions in a short span of time. In the ideal situation, the electrodeposited film is evenly distributed on the depositing substrate, and patterned film with nano-scale thickness (resolution) may be reached by electroplating. Thus, the limitation of the EDP strategy is the precision of the conductive template. Based on these deductions, a higher resolution may be reached by the EDP method using conductive template with finer features. Flexibility, Extensibility, and Conductivity of the Resulting Film. The flexibility and conductivity of the prepared Au/T-A tape (deposition time: 80 cycles, Figure S7b) were evaluated through first folding Au/T-A films more than 270° (front and backwards, bending radius ≤ 1.5 mm) for 100 times, and then bending degrees fixed to 180° and -180°. In Figure 4a & Figure S5I, no matter which direction it was bended, the Au films exhibit quite good conductivity


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(resistance 2-3 Ω), and the resistance was quite stable and low during 400 bending cycles (Figure 4b), indicating that the patterned film was able to withstand repeated stress. When two pieces (or one cuts into two) of Au/T-A films were pasted face to face, the flexibility and conductivity of the resulting film is still very good (Figure 4a). This special property ensures the potential for fabricating the threedimensional (3D) device (e.g. planar coils) by the EDP strategy. Then, the extensibility of the Au/PDMS film by the EDP strategy was also tested. As depicted in Figure 4, the conductivity of the films was related to the stretched length. Even if it was stretched to 150%, the resistance of the film was only 324±83 Ω, Figure S5c), indicating the extensibility and conductivity of the Au/PDMS film by the EDP method. The cyclic strain tests, showed a good stability of the Au/PDMS film (at least 900 cycles), although there is still a weakening trend to the current flow. On the Au/T-A film, a flexible circuit with four LEDs was constructed (Figure 4e & f), showing that the circuit worked well even if it was folded 180° (bending radius≤ 2 mm). Finally, it should also be noted when the Au layer was too thin or constructed with separated Au particles (Figure 4g), its conductivity would be poor. However, such patterned film with numerous and uniform Au particles as the anchoring sites for some biomolecules is potentially suitable for combining with the 96-wells enzyme linked immunosorbent (ELISA) plate, the SERS-active substrate, and the paper-based chips for the point-of-care diagnosis. 42,43 Applications. The Au/T-A tape electrode is highly stable in 0.5 M sulfuric acid, as revealed by testing the cyclic voltammetry (CV) from -0.2 V to 1.8 V 200 cycles (Figure 5a). Therefore, it can be used as a stable electrochemical interface for the determination of Hg(II), which is one of the most prevalent heavy metal pollutants in soil and water. 44 Under the optimized conditions (analysis steps: preconcentration (0.2 V, 120 s) → determination (step increment: 4 mV; amplitude: 50 mV; pulse period: 0. 2 s; potential range: -0.2 to 0.8 V) → clean (0.9 V, 90 s)), the analysis of Hg(II) in HCl buffer solution was easily achieved with the flexible Au electrode. The peak current at 0.55 V was linearly related to the concentration of Hg(II) in the range of 1 to 150 µg/L with a detection limit of 1 µg/L (Figure 5b). This result is comparable to that obtained from the traditional Au disc electrodes. Moreover, the pretty cheap electrodes obtained from the EDP strategy avoided the relatively complicated clean process before using due to the electrodeposition fabrication process. ACS Paragon Plus Environment

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Besides the applications in environmental monitoring, the EDP strategy also exhibits broad potential in health care. By making minor modifications to the coated ITO template, a flexible bipolar system

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(lab on T-A tape, Figure 1IIa) can be fabricated with single electrodeposition process. A bare tape punched with holes as the sample cells was adhered to the other tape with BPE array to construct the socalled lab on T-A tape (Figure S6). This design can be used for the visual analysis [with electrochemiluminescence (ECL) technique] of H2O2, which is one of the most important intermediates in various biological processes. The flexible lab was fixed with a glass slide to facilitate the following experiments. All the cathodic cell (marked with -) were filled with ECL solution [10 mM TPrA + 1 mM Ru(bpy)32+], and all the anodic cell (marked with +) were filled with phosphate buffer solution (PBS, pH 7.4, 0.1 M). The driving voltage was set at 7 V. In this case, there were no visual ECL signals being observed from the BPE anodes. However, when the PBS in the third anodic cell (Figure 5e) was replaced with 10 mM H2O2 (in 0.1 M PBS, pH 7.4), an obvious ECL signal was observed from the anode of the third BPE. Finally, the four anodic cells were filled with 10 mM, 0.1 mM, 0.01 mM H2O2 and PBS (pH 7.4, 0.1 M), respectively. An obvious difference of the ECL signal from the BPE anodes was observed (Figure 5f), indicating that the flexible lab has similar functions to the hard ones.

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Owing to the ultra-low cost of the EDP strategy, the flexible lab developed here can be used disposably without the need of considering the poison of the Au electrodes by the TPrA. CONCLUSIONS In conclusion, we have developed a simple, low-cost, universal, and new electrochemical lithography technique to prepare large-scale, flexible/stretchable, and patterned material films with high precision (~2 µm) for the fabrication of flexible electronics. Compared with the traditional techniques, the EDP strategy with high resolution is much faster and cheaper. Using the EDP method, any electroactice materials (e.g. Au, Ag, Cu, PB, MnO2, rGO, and PB/Au) can be patterned on various substrates as long as both the intermolecular forces of the materials and the adhesive strength of the adhesive substrate were stronger than the interaction between the materials and selected template. The resulting flexible films are able to withstand repeated stress and show good electric conductivity, which are the critical concerns in flexible and stretchable electronics. We expect that the EDP strategy demonstrated here may open up a new way for designing flexible and stretchable electronics, disposable electrochemical interfaces and the wearable sensors. ACS Paragon Plus Environment

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ACKNOWLEDGMENT This work was supported by the National Natural Science Foundation of China (Grant No. 21427811), MOST, China (No. 2016YFA0203200 and 2016YFA0201300) and Youth Innovation Promotion Association CAS (No.2016208). ASSOCIATED CONTENT Supporting Information. Additional information about the device fabrication, characterization of the EDP methods and deposition parameters and conditions are available free of charge via the Internet at http://pubs.acs.org.


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(45) Zhang, X. W.; Li, J.; Jia, X. F.; Li, D. Y.; Wang, E. K. Anal. Chem. 2014, 86, 5595-5599.

(46) Zhang, X. W.; Chen, C. G.; Yin, J. Y.; Han, Y. C.; Li, J.; Wang, E. K. Anal. Chem. 2015, 87, 46124616.


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FIGURE CAPTIONS

Scheme 1. Schematic illustration on the EDP strategy for copying the pattern of the conductive template with electroactive materials (M) onto the adhesive tape/material.

Figure 1. Versatility of the EDP strategy. I. (a) Au; (b) Ag; (c) Cu; (d) PB; (e) MnO2; (f) rGO; (g) rGO pattern with 60 µm line width. Note: PB and MnO2 are nonconductors. II. (a) Flexible Au on T-A tape; (b) rigid Au on D-A tape and transferred to hard substrate; (c) stretchable Au on PDMS.

Figure 2. Resolution of the EDP strategy (magnification: 500 times). (a) 60 µm; (b) 10 µm; (c) 8 µm; (d) 6 µm; (e) 4 µm; (f) 2 µm. Au electrodeposition parameters: 30 CV cycles (-0.9 to 0.6 V, 1.5 V/s) in 20 mM HAuCl4 + 1 M LiCl. Figure 3. Pattern with 4 µm (a, b) and 2 µm (d, e) line width recorded using SEM under different magnifications and subatrates, and the average width of the Au line from 40 random locations (c and f). a and d was from Au/ITO (a: 6400x, d: 6900x); b and e from Au/T-A tape (b: 4400x, e: 5000x). Figure 4. Characterization of the flexibility, extensibility, and conductivity of the films obtained from the EDP strategy with different transfering substrates. (a, b). Au/T-A tape: (a) bending and cutting test; (b) cyclic bending tests; (c, d). Au/PDMS film: (c) tensile testing; (d)cyclic strain tests; flexible circuit integrated with 4 LEDs using Au/T-A tape before (e) and circuit after with the 180° bended and (g) pthotos nonconductive Au patterns for other applications. Figure 5. (a) The chemical and electrochemical stability of the flexible Au electrode from the EDP strategy. (b) The determination of Hg(II) with Au T-A tape electrode. The application of the so-called lab on adhesive tape in electrochemiluminesence imaging analysis with driving voltage of 7 V (c-f)). (c) Samples on the lab on adhesive tape. (d) All the anodic cells were filled with PBS. (e) The PBS of the third anodic cell was replaced with 10 mM H2O2. (f) 10 mM, 0.1 mM, 0.01 mM and PBS was added to the anodic cells respectively.


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Scheme 1.


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Figure 1.


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Figure 2.


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Figure 3.


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Figure 4.


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Figure 5.


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Beyond Conventional Patterns: New ... - ACS Publications

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