Ferroelectric Zinc Oxide Nanowire Embedded Flexible. Sensor for Motion and Temperature Sensing

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1 Supporting information for: Ferroelectric Zinc Oxide Nanowire Embedded Flexible Sensor for Motion and Temperature Sensing Sung-Ho Shin 1, Dae Hoon Park 1, Joo-Yun Jung 2, Min Hyung Lee 3, Junghyo Nah 1,* 1 Department of Electrical Engineering, Chungnam National University, Yuseong-Gu, Daejeon 34134, Korea 2 Department of Nano Manufacturing Technology, Korea Institute of Machinery and Materials, Yuseong-Gu, Daejeon 34103, Korea 3 Department of Applied Chemistry, Kyung Hee University, Yongin, Gyeonggi 17104, Korea *Corresponding author: jnah@cnu.ac.kr S-1

2 Experimental details Synthesis of Li-doped ZnO NWs. The 50 mm of zinc nitrate (Zn(NO 3 ) 2 H 2 O, Sigma Aldrich) and 50 mm of hexamethylenetetramine (HMTA, Sigma Aldrich) were poured into a container filled with deionized (DI) water of 50 ml. As a lithium doping reagent, 50 mm of lithium nitrate (LiNO 3, Sigma Aldrich) was added in the solution and stirred on a hot plate at 60 C for 2 h. Next, for the hydrothermal growth of undoped and Li-doped ZnO NWs, the solutions were kept in oven at constant temperature of 95 C for 10 h. After the growth process, the solution was completely dried and remaining the NW powder was subsequently cleaned with DI water and ethanol. The container was then dried in oven at 200 C for 3 h and then the container was cooled down to room temperature. Lastly, the grown NWs were annealed in a furnace at 550 C for 1 h 30 m in oxygen ambient. Device fabrication. The sensor devices were fabricated as follows. First, a Si wafer was cleaned using acetone, IPA, deionized water, respectively, followed by N 2 blow dry. The precleaned wafer was then placed in a sealed container and coated with vaporized trichloro (1H,1H,2H,2H-perfluorooctyl) silane (FOTS) (97 %, Sigma Aldrich) at 95 C for 1 h in oven. Subsequently, AgNWs were spray-coated on a FOTS-treated Si wafer and polydimethylsiloxane (PDMS) (Sylgard, 184 Silicon elastomer) was poured on it, followed by curing on a hot plate at 80 C for 5 h. After the curing process, the AgNWs layer coated on the Si wafer was peeled off, forming the electrode layer capped under the PDMS layer. Lastly, Li-doped ZnO NWs-PDMS composite layer was sandwiched between top and bottom AgNWs implanted PDMS layer. As poling process, electric field of 100 kv/cm was applied between top and bottom electrodes at thermal condition of 75 C for 20 h. In this process, the S-2

3 PDMS polymer plays a role in preventing from electrical breakdown during the high E-field poling process. Characterization. The resistance and output voltage were measured using high precision digital multi meter (Agilent 34401A). The custom-built bending stage and push machine were used to adjust the horizontal travel distance, motion speed, frequency, and applied pressure, respectively. The scanning electron micrographs (SEMs) were achieved using Hitachi S A PL spectrometer (Horiba Jobin Yvon, Inc., LabRAM HR-800) was used to analyze the PL spectrums of undoped and Li-doped ZnO NWs. The PL measurement was carried out by using He-Cd laser (325 nm). Water contact angle (CA) analyzer Surface Electro Optics, Phoenix 300) was used to acquire CA of Si wafer surface and FOTS-coated Si wafer surface. S-3

4 Figure. S1 (a) Schematic illustration of spray-coated AgNWs transferring process on the PDMS surface by employing anti-adhesive FOTS coating. (b) Contact angle (θ) measurement of a water droplet on the FOTS coated Si wafer, showing hydrophobicity with CA (θ = 123 ), attributed to low surface energy of nonpolar ( CF 3 ) end groups in FOTS. 1 (c) (left) SEM of the AgNWs on FOTS-coated Si wafer before the transferring process. (right) SEM of Si wafer surface after transferred Ag NWs. After transferring process, it can be noticed that there is no remaining AgNWs on the Si surface. (d) Schematic illustration of the AgNW transfer process in the absence of FOTS coating. (e) Measured CA (θ = 75 ) on a pure Si wafer, showing hydrophilic property (0 < θ < 90 ). 2 (f) SEM of AgNWs on the Si surface (left) before and (right) after the transferring process. S-4

5 Figure. S2 Cross sectional SEMs of the piezoelectric Li-doped ZnO NWs and PDMS composite layer. The SEMs explicitly show that the NWs are well-distributed inside the composite layer. S-5

6 Figure. S3 Measured piezoelectric output voltages by varying the bending angle, stretching distance, applied pressure, speed, and frequency. (a d) Output voltages at the bending angles of (a) 30, (b) 60, (c) 70, (d) and 90. (e h) Output voltages at the stretch lengths of (e) 1 mm, (f) 2 mm, (g) 3 mm, (h) and 4 mm. (i l) Output voltages under the applied pressure of (i) 0.05 MPa, (j) 0.1 MPa, (k) 0.2 MPa, and (l) 0.3 MPa. During the measurements, the motion speed and frequency were varied as 65 mm/s or 1 Hz (black), 70 mm/s or 2 Hz (red), 75 mm/s or 3 Hz (blue), 80 mm/s or 4 Hz (pink), and 85 mm/s or 5 Hz (green). S-6

7 References (1) Oyola-Reynoso, S.; Wang, Z.; Chen, J.; Çınar, S.; Chang, B.; Thuo, M. Revisiting the Challenges in Fabricating Uniform Coatings with Polyfunctional Molecules on High Surface Energy Materials. Coatings 2015, 5, (2) Chua, Z.; Seeger, S. Superamphiphobic Surfaces. Chem. Soc. Rev. 2014, 43, S-7

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