Supplementary Information. High-Performance, Transparent and Stretchable Electrodes using. Graphene-Metal Nanowire Hybrid Structures
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1 Supplementary Information High-Performance, Transparent and Stretchable Electrodes using Graphene-Metal Nanowire Hybrid Structures Mi-Sun Lee, Kyongsoo Lee, So-Yun Kim, Heejoo Lee, Jihun Park, Kwang-Hyuk Choi, Han-Ki Kim, Dae-Gon Kim, Dae- Young Lee, SungWoo Nam, Jang-Ung Park *, School of Nano-Bioscience and Chemical Engineering, School of Mechanical and Advanced Materials Engineering, Low- Dimensional Carbon Materials Center, Ulsan National Institute of Science and Technology (UNIST), Ulsan, , Republic of Korea Department of Advanced Materials Engineering for Information and Electronics, Kyung Hee University, Yongin-si, , Republic of Korea Samsung Techwin R&D Center, Seongnam-si, , Republic of Korea Display Research Center, Samsung Display, Yongin-city, , Republic of Korea Department of Mechanical Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois This PDF file includes: Methods Supporting Figures S1-S8 Supporting Table S1 Captions of Supporting Movies Supporting References 1
2 Methods CVD synthesis and transfer of graphene. After loading a Cu foil (Alfa Aesar, item No.: 13382) onto the center of a quartz CVD chamber under vacuum (100 mtorr), the furnace was heated up to 1000 o C under the flow of Ar (200 sccm) and H 2 (500 sccm). CVD growth was carried out under the flow of CH 4 (12 sccm) and H 2 (500 sccm) for 5 minutes, and then the chamber was cooled to room temperature under the flow of Ar (500 sccm) over ca. 30 min. A 200 nm-thick poly(methyl methacrylate) (MicroChem Corp. 950 PMMA) supporting layer was spun on the synthesized graphene sample. The foil was dissolved in a diluted etching solution of FeCl 3 : HCl: H 2 O (1:1:20 vol.%) with the PMMA-coated graphene layer floating on the solution surface. Subsequently the sample was transferred onto substrates, and the PMMA supporting layer was removed with acetone. Figure S1a shows the typical Raman spectrum obtained from the transferred graphene with exhibiting three characteristic bands of graphene (D: centred at ~ 1,350 cm -1, G: ~ 1,590 cm -1, 2D: ~ 2,680 cm -1 ). This spectrum presents (i) the G-to-2D peak intensity ratio of ~ 0.5, (ii) the FWHM value of ~30 cm -1 for the 2D band, and (iii) the D-to-G peak intensity ratio below 0.1, which indicates a monolayer graphene sheet with a relatively low defect density 1-3. As shown in Figure S1b, the transmittance of the graphene sheet is 97.7 % at 550 nm in wavelength and almost flat in the range of nm. Preparation of Ag nanowire films. AgNWs with average length of 30 m ( 7 m) and average diameter of 20 nm ( 5 nm) (Figure S2a) dispersed in isopropyl alcohol (0.3 wt%) were purchased from Nanopyxis Co., Ltd. (Product name: AgNW ink (LOT No.: B 424-1)). The nanowires are single crystalline (face-centered cubic lattice), as shown in the high-resolution transmission electron microscope (HRTEM) image and electron diffraction pattern (Figure S6). 2
3 This solution was stored at 5 o C, and then stirred at room temperature for 10 minutes using a magnetic stir bar before spin-coating. For the results in Figure 1, the solution was spun for 30 sec with different spin rates. For all results in Figures 2-5, the spin-coating condition of AgNWs was 500 rpm for 30 sec, in order to yield the lowest sheet resistance in our experiments. After spinning the AgNW suspension on substrates (with or without graphene top-layers), samples were dried at 150 o C for 90 sec to evaporate the solvent completely. Formation of Graphene-AgNW hybrid nanostructures. We have employed two approaches to assemble the hybrid structures: (i) AgNWs on graphene, or (ii) graphene on AgNWs. (i) After CVD synthesis of graphene layer, graphene was transferred onto a desired substrate. Spinning the AgNW suspension onto the graphene surface and then drying at 150 o C for 90 sec completed the formation of the hybrid. (ii) AgNW network films were prepared, as described above. After graphene synthesis using CVD, the graphene layer was transferred onto the AgNW networks using PMMA. Subsequently the PMMA supporting layer was removed with acetone. Also, the spun AgNW sample can be dried at room temperature for 10 min without the heating step (150 o C for 90 sec). R s values of the graphene-agnw hybrid films were not changed by this heating step, as shown in figure S7. When we performed the adhesion test using 3 M scotch tape, all heated or unheated samples were peeled off from the substrate (PET), which indicates that this heating process does not improve the adhesion significantly. Patterning and transfer of Hybrid Electrodes. Graphene-AgNW hybrid electrodes can be photolithographically patterned using the etch-back process. The hybrid films were dry-etched first using oxygen reactive ion etching plasma (50W, 60 sccm, 160 sec) to remove carbon. Figure S3 presents the SEM image and electrical conductance of the AgNWs remained after this 3
4 Oxygen plasma etching. The exposed areas became electrically non-conductive because residues of the NWs were oxidized and chopped. Subsequently, these AgNW residues were completely dissolved in an etching solution of H 3 PO 4 : C 2 H 4 O 2 : C 6 H 4 NO 5 SNa: H 2 O (55:1:4:40 vol.%). For figure 5, the hybrid electrodes were patterned only using the plasma exposure without the wetetching step, because the IGZO layer was damaged by the wet etchant. For the transfer process, the hybrid film was formed on a Cu foil where graphene was presynthesized using CVD. Then a 200 nm-thick PMMA (MicroChem Corp. 950 PMMA) supporting layer was spun on the hybrid surface, and the foil was dissolved. Subsequently, the floating layer (with PMMA) was transferred onto a target substrate, and the PMMA supporting layer was removed with acetone. Adhesion test. Adhesion properties of AgNW networks and the hybrid to a substrate (PET) were compared. All samples were easily peeled off from a PET substrate using a 3 M scotch tape. Instead of this scotch tape method, we also immersed our samples inside 1-methyl-2-pyrrolidone (NMP, a typical photoresist stripper), DI water, or tetramethylammonium hydroxide (TMAH)- based photoresist developer (AZ 300 MIF), for 5 minutes. R s of AgNWs significantly increased after the immersion test while R s values of the hybrid samples changed negligibly (figure S8), which suggests that the hybrid shows better adhesion to the substrate (PET) than the AgNW alone. Although the adhesion against peeling-off of the hybrid on a PET is similar to that of AgNW alone (scotch tape testing), the adhesion of hybrid on a PET against organic solvents showed that our hybrid film is suitable for conventional photolithography. Preparation of 2 m-thick polyimide substrate. After spinning the 200 nm-thick PMMA sacrificial layer on a bare Si wafer, a polyimide precursor (Poly(pyromellitic dianhydride-co- 4
5 4,4 oxydianiline), Aldrich) was subsequently coated at 3000 rpm for 30 sec. Thermal curing was carried out at 250 o C for 6 hours. After forming graphene-agnw hybrid electrodes on the polyimide surface, this 2 m-thick polyimide film together with the hybrid electrodes could be delaminated from the Si wafer by dissolving the PMMA using acetone. Electrical characterization. The four-point probe method was used for the R s measurement using a probe station with a Keithley 4200-SCS semiconductor parametric analyzer. And the two-point probe method was used for the resistance measurements and breakdown experiments with a Keithley 2425 source meter. In figure 2b, sheet resistances were calculated from the measured resistances by considering the aspect ratio of patterns ( R s film width R ). film length Optical characterization. The Raman spectra were recorded with a WITec CRM200 Raman system with a 532 nm laser as excitation source. Optical transmittance of films was measured using UV-vis-NIR spectroscopy (Cary 5000 UV-Vis-NIR, Agilent). Transmittance of substrates was excluded. Rabbit experiment. All in vivo studies were performed according to the guidelines of the National Institutes of Health for care and use of laboratory animals, and with the approval of the Institute of Animal Care and Use Committee of UNIST (UNISTIACUC A). And the preparation of the contact lens sample for this in vivo rabbit eye test was carried out in the same way as the mannequin experiment. 5
6 Supporting Figures Figure S1. (a) Raman spectrum and (b) transmittance of monolayer graphene transferred on a glass slide. 6
7 Figure S2. (a) AFM image of AgNWs coated on a glass slide at 500 rpm for 30 sec. Scale bar, 5 μm. (b) Optical transmittance of graphene, AgNW networks, and the hybrid films at the wavelength of 550 nm. (c) Sheet resistance of the hybrid nanostructure (black squares) and the parallel resistor model (red circles). (d) Relative difference in the sheet resistances of these two cases as a function of NW density. 7
8 Figure S3. (a) SEM image of AgNWs exposed by oxygen plasma. Scale bar, 500 nm. (b) Change in electrical conductance of the AgNWs by the oxygen plasma. 8
9 Figure S4. Dependence of resistance of AgNW networks on the length of patterns. 9
10 Figure S5. EDS and XRD measurements of AgNW film (a, c) before and (b, d) after the thermal oxidation stability test. 10
11 Figure S6. (a) High-resolution transmission electron microscope (HRTEM) image and (b) electron diffraction pattern of AgNWs. Scale bar; 2 nm. 11
12 Figure S7. Sheet resistances of graphene-agnw hybrid films with and without heat treatment step (150 o C for 90 sec). 12
13 Figure S8. Changes in the sheet resistances of AgNW networks and the hybrid after the immersion test. 13
14 Table S1. Densities of AgNWs coated with different spin rates. 14
15 Captions of Supporting Movies Supporting Movie 1. Video of light emitting from the contact lens device on a mannequin eye with a supplying bias of 4V. Supporting Movie 2. Video of the rabbit movement after wearing the contact lens device on a rabbit eye. 15
16 Supplementary References 1. Li, X.; Cai, W.; An, J.; Kim, S.; Nah, J.; Yang, D.; Piner, R.; Velamakanni, A.; Jung, I.; Tutuc, E.; et al. Large-Area Synthesis of High-Quality and Uniform Graphene Films on Copper Foils. Science 2009, 324, Li, X. S.; Zhu, Y. W.; Cai. W. W.; Borysiak, M.; Han, B. Y.; Chen, D.; Piner, R. D.; Colombo, L.; Ruoff, R. S. Nano Lett. 2009, 9, Dresselhaus, M. S.; Jorio, A.; Hofmann, M.; Dresselhaus, G.; Saito, R. Nano Lett. 2010, 10,
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