Microelectronic Engineering 193 (2018) 91–97 Contents lists available at ScienceDirect Microelectronic Engineering journal homepage: www.elsevier.com/locate/mee Sintering process of inkjet-printed silver patterns using a heated inert gas Kwon-Yong Shin a, Nam Son Park b, Jun Young Hwang a, Kyungtae Kang a, Sang-Ho Lee a,⁎ a b Korea Institute of Industrial Technology, 14, Hanggaul-ro, Ansan 15588, Republic of Korea Jesagi Hankook Ltd., 17, MTV 25-ro, Siheung 15117, Republic of Korea a r t i c l e i n f o Article history: Received 26 September 2017 Received in revised form 3 February 2018 Accepted 17 February 2018 Available online 21 February 2018 Keywords: Inert gas Sintering Inkjet Silver Printing a b s t r a c t In this study, we introduce a thermal sintering process using a heated inert gas as a new sintering method. The heated gas flow is formed by passing nitrogen (N2) gas through a heating head of 300 to 700 °C, and the desired substrates are then exposed to the heated gas flow through a 400 mm long and 5 mm wide slit-nozzle. Sintering performance of Ag films was characterized by analyzing the electrical resistivity and metallographic structures according to the temperature change of the heating head. The temperature distribution of the heating region is analyzed by infrared (IR) thermal imaging and surface temperature measured by thermo-label tape. To test the feasibility of the proposed method for application to printed circuit board (PCB) manufacturing, we performed a reliability evaluation using the printed Ag patterns under the standard of the Institute for Interconnecting and Packaging Electronic Circuit (IPC), TM650. Various reliability test patterns were created by Ag inkjet-printing on both a rigid flame retardant 4 (FR4) substrate and a flexible polyimide (PI) film substrate. The reliability evaluation includes withstanding voltage, adhesive strength, thermal shock, pressure cooker, and bending tests. The surface wettability of the substrates was controlled to obtain high quality fine and uniform patterns by UV/O3 treatment after coating a fluoropolymer thin film. © 2018 Elsevier B.V. All rights reserved. 1. Introduction Printed electronics is a technology used to create electrical devices on various substrates using printing methods such as screen printing, flexography, gravure, offset lithography and inkjet-printing [1]. Recently, the scientific community has shown a growing interest of developing low-cost flexible electronics by printed electronics. This interest is driven by several factors: (1) the need for low-cost and mass-production processes; (2) numerous applications require shapeable and disposable devices; and (3) the demand for the quick realization of electronics [2,3]. Typical printed devices include printed strain sensors, temperature sensors, printed image sensors, printed humidity sensors, printed biosensors and RFID tag with light detection [2–5]. In the last decade, inkjet-printing has been attracting growing interest for the production of micro-patterns as an alternative to the conventional photolithography process. The inkjet-printing method has many advantages including low-cost manufacturing, a low-temperature process and patterning compatibility on a non-planar substrate or a flexible substrate due to the direct-writing feature. Furthermore, it is possible to produce micron-sized patterns in a drop-on-demand manner without predefined masking and etching [6–10]. Inkjet-printing technology has been steadily utilized as a fabrication process to demonstrate field-effect transistors [6,7], conductive electrodes [8,9], memory ⁎ Corresponding author. E-mail address: sholee7@kitech.re.kr (S.-H. Lee). https://doi.org/10.1016/j.mee.2018.02.016 0167-9317/© 2018 Elsevier B.V. All rights reserved. devices [11], sensors [3,5], light-emitting polymer displays [12,13] and organic solar cells [14,15]. Recent advances in 3D printing technology can provide electronic prototypes that can be rapidly fabricated in comparable time frames to those for traditional 2D bread-boarded prototypes by component placement and electrical interconnection on 3Dprinted thermoplastic dielectric structures [16,17]. Hybrid prototyping with 2D printed electronics and 3D printing is referred to as 3D structural electronics. 3D printing techniques such as stereo-lithography and fused deposition modeling have recently been explored in the context of 3D structural electronics [17]. Interest in 3D printed electronics has motivated the development of several new types of commercially available equipment. Nano Dimesion's DragonFly 2020 enables multilayer printing of conductive traces using an inkjet technique at a lateral resolution of ~30 μm. The Voxel 8 combines a conventional plastic filament extrusion nozzle with a syringe-based silver ink extruder. The lateral resolution of the traces that can be printed with the Voxel 8 is 250 μm with a recommended pitch of 2 mm, and the printer allows pausing of the printing to enable manual placement of circuit components [18]. Recently, demonstrated electronic devices include a 3D-printed spherical dipole antenna [19], a surface acoustic wave transponder [20], a 3Dprinted conditioning circuit [16], and a three-axis magnetic flux sensor system [17]. In inkjet printing of a conductive nanoparticles pattern, selection of the sintering method is a critical factor to obtain stable conductivity of the printed patterns because the electrical performance depends on the inter-connection of individual nanoparticles onto a substrate after 92 K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 deposition by inkjet printing [21]. Generally, Ag nanoparticle ink consists of nanoparticles and a solvent. Before sintering, there are no significant changes in the particle size and neck growth. However, when the ink is sintered, neck growth gradually takes place at the grain boundary surface and the pores are gradually reduced between the particles. A continuous conductive printed pattern is then created [22]. In recent years, many research results related to sintering technology such as laser sintering [23], thermal sintering [24,25], electrical sintering [26], microwave sintering [27], plasma sintering [22], and photonic sintering [28], for printed electronics applications have been reported. Also, several theoretical studies were introduced to understand the nanoparticle sintering process at the level of the nanoscale process [29–32]. In particular, a theoretical approach to understanding the electrical and thermal properties is extremely important for applications of nanostructured materials in microelectronics, thermoelectric, and thermal barrier coatings. Ertekin et al. proposed a generalized model to describe the thermal conductivity for nanostructured materials [30,31] and Kang et al. proposed a charge-transport model for a fundamental understanding of conducting polymers [32]. In this study, we introduce a thermal sintering process using a heated gas flow as a new sintering method and evaluate its feasibility for PCB manufacturing through a reliability characterization of inkjetprinted Ag patterns. The gas flow is heated by passing N2 gas through a heating head of 300 to 700 °C, and then the heated gas flow is jetted from a nozzle with a length of 400 mm and, a width of 5 mm onto the substrates. In order to control the sintering characteristics, we controlled the gas flow rate, heating head temperature and exposure time of the heated gas flow. Sintering performance on printed Ag patterns was characterized by analyzing the electrical resistivity and metallographic structures according to the temperature change of the heating head. A reliability evaluation was performed according to the standard of the IPC, TM650 commonly used in the PCB industry. The test patterns were fabricated by inkjet printing of an Ag nanoparticle ink on a FR4 rigid substrate and a PI flexible film, respectively. surface. We determined the surface energy through Wu's harmonic mean model using the average contact angles of DI water and formamide as input parameters. Rigid FR4 and flexible PI substrates were used to fabricate the specimens for the withstanding voltage, adhesive strength, thermal shock and pressure cooker tests. The dielectric withstanding voltage, thermal shock, and pressure cooker tests were conducted with a high-speed electric load (6330, CHROMA, Taiwan), high temperature tester (TSA41L, ECPEC, Japan), and, a pressure cooker tester (PCT-183CP, Lab Companion, Korea), respectively, and the American Society for Testing and Materials (ASTM) D3359 adhesive strength test rating system was used along with Scotch tape (610, 3M, Korea) to measure the adhesion of the Ag patterns. Flexible PI (DSF-600, Doosan Electronic Corp., Korea) films were used to fabricate the specimens for the bending test, which was carried out using a bending tester (MIT-SA, Toyoseiki, Japan). Fig. 1 show schematic images of the heated N2 gas flow-based sintering process and a picture of the sintering system (HBS-I, Jesagi Hankook Co., Korea) used in this study. The N2 gas flow was heated by passing N2 gas through a heating head of 300 to 700 °C. The heated gas flow was jetted through a nozzle with a length of 400 mm and a width of 5 mm. The gas feeding flow rate was 40 L/min and the gap distance between the nozzle and the substrate was 3 mm. The substrate was moved to the heated gas exposure region after loading the substrates onto the stage. 3. Results and discussion Fig. 2 shows the horizontal temperature distribution of the heated gas flow around the slit nozzle at various measuring positions with the head heating time. We measured the temperature at the gap area Slit nozzle Heated gas flow (Inert gas) 2. Experimental methods We used Ag ink (DGP 40LT-15C, Advanced Nano Products Co., Korea) in which ~50 nm Ag nanoparticles were dispersed in a triethylene glycol monomethyl ether solution. The ink contained Ag nanoparticles in an amount of 30.1 wt.%. A piezoelectric print-head system with a 19 μm nozzle diameter (DMP-2800, Dimatix, Fujifilm, USA) was used for printing the Ag ink. The printing system was composed of a print-head, a motorized X-Y stage, a heatable working table and an alignment system. Before printing the patterns, we first optimized the droplets ejected from the nozzle by controlling the voltage and the waveform of the piezo actuator drive to ensure stable single droplet deposition during all the experiments. FR4 and PI were used as the substrate material. The substrates were ultra-sonicated in acetone and 2-propanol alcohol for 10 min to remove surface contamination, rinsed with de-ionized water, and subsequently dried in a convection oven at 110 °C for 10 min. The cleaned substrate was coated with fluorocarbon (FC) solution to produce a hydrophobic surface. A hydrophobic FC thin film was spun onto the substrate at 2000 rpm for 1 min using a fluoropolymer solution: a mixture of FC 722 and FC 40 (Fluorad™, 3 M, Korea). The FC-coated substrate was then immediately loaded into a convection oven and baked at 110 °C for 10 min. In order to increase the hydrophilicity of the hydrophobic surface, UV/O3 treatment was performed using an UV/O3 cleaner (AH1700, Vision Semicon Co., Korea). The UV/O3 treatment was conducted for 6 min to control the surface wettability of the substrate. We measured the contact angles of the FC-coated and UV/O3 treated substrates using a contact angle measuring instrument (DSA 100, Krüss, Germany). Three test liquids were used for the contact angle measurement: DI water, diiodomethane and formamide. Contact angles were measured using the sessile drop method at five different locations on the Thin film Substrate Stage (a) Gas heating head Gas flow rate controller Stage speed controller Temperature controller (b) Fig. 1. Heated N2 gas flow-based sintering system: (a) a schematic image of the sintering process; (c) a picture of the sintering system. K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 Nozzle Measurement position 5 cm Front 93 Nozzle 5 cm Left 5cm Left 2.5cm Substrate Right 5cm Right 2.5cm Center (a) A a B b C c D d E (b) Fig. 2. Horizontal temperature distribution of the heated gas flow around the slit nozzle: (a) IR camera image of nozzle front side; (b) temperature change at various measuring positions with head heating time. between the nozzle and the substrate by an IR thermal image camera system (A40, FLIR, USA). The heated gas flow was generated through a slit nozzle of 400 mm length and 5 mm width. Fig. 2(a) shows an IR thermal image of the nozzle front side at a gap distance = 3 mm between the nozzle and the substrate. We measured the temperature at the center, 2.5 cm and 5 cm away from the center, respectively. The head temperature was held for 20 min at 300 °C, 400 °C, 500 °C, 600 °C, and 700 °C, respectively, at sections A, B, C, D, and E in Fig. 2 (b), and ramped up for 5 min from 300 °C to 400 °C, 400 °C to 500 °C, 500 °C to 600 °C, and 600 °C to 700 °C, respectively, at sections a, b, c, d Table 1 Evaluation results of colorimetric thermo-label sensors by hot plate heating and thermocouple sensor monitoring. Hot plate set temperature (°C) Measured temperature (°C) Thermo-label color change Measurement setup 200 202 210 210 230 234 250 254 94 K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 Nozzle (a) (b) (c) Thermo-label Stage Stage 5 cm 5 cm Fig. 3. Surface temperature analysis of a substrate during exposure of heated N2 gas flow using colorimetric thermo-label sensors: (a) scheme of surface temperature measurement; (b) before exposure; (c) after exposure. in Fig. 2(b). After the head temperature reached 600 °C, the temperature at the center region was above 250 °C. The temperature at the 5 cm-away left/right position was 40–42% lower than the center temperature (Fig. 2(b)). Before sintering the Ag patterns, we analyzed the surface temperature change of the substrate during exposure of the heated gas flow using colorimetric thermo-label sensors (5E, Nichiyu Giken Kogyo Co., Japan). The actual surface temperature can be measured by monitoring the color change of thermo-label tapes. First, we evaluated the accuracy of the thermo-label sensor using a hot plate and a thermocouple sensor monitor (GL240, Basecamp C&M Co., Ltd., Korea). After attaching the thermo-label sensor and the thermocouple on the hot plate, we monitored color changes by elevating the temperature as shown in the measurement set-up presented in Table 1. As soon as the temperature increased from 200 °C to 250 °C, the white dots of the thermo-label tapes started to change to black. In the results, five dots changed to black at 250 °C (Table 1). The target surface temperature is 250 °C, which is recommended for sintering of the Ag nanoparticle ink used in this study [24]. Next, we loaded quartz plate (40 cm × 40 cm) with ten attached thermos-label sensors into the heated gas flow-based sintering system (Fig. 3(a)). The quartz substrate was moved toward the heated gas exposure region at a stage velocity = 3.5 mm/s. The heating head temperature was 600 °C and the N2 flow rate was 40 L/min. The color of all five dots changed to black (Fig. 3(b)). This indicates that the heated N2 gas flow induced a surface temperature above 250 °C at a head temperature of 600 °C. The electrical resistivity of the Ag thin films was measured to investigate the thermal sintering performance of the heated N2 gas flowbased sintering system. The electrical resistivity is a key variable to characterize the sintered Ag patterns as a metal electrode after the sintering process. The electrical resistivity (ρ) of the fully sintered film was calculated by multiplying the sheet resistance by the film thickness [21]. We prepared an Ag ink-coated glass substrate and the thickness of the Ag film was about 330 nm. The sheet resistance decreased gradually from 1.6 Ω/□ to 0.12 Ω/□ when the head temperature increased from 300 °C to 600 °C. The Ag-coated glass substrate was exposed to the heated N2 gas flow for 10 min. The electrical resistivity of the Ag film reaches about 3.96 × 10−8 Ω·m after being sintered by the heated N2 gas flow at 600 °C (Fig. 4). The calculated electrical resistivity of the Ag film sintered by the heated N2 gas flow was approximately 2.5 times that of bulk Ag metal (1.6 × 10−8 Ω·m), but ~30% lower than that of the Ag film sintered in a convection oven at 250 °C for 60 min (5.8 × 10−8 Ω·m) [24]. Fig. 4 shows the change of the sheet resistance and electrical resistivity with the head temperature. We compared metallographic structures of the Ag films after sintering in a convection oven and a heated gas flow sintering system, respectively. Fig. 5 shows the sintering conditions and scanning electron microscope (SEM) images of the Ag film before and after sintering. For oven sintering, we observed the overall intra-microstructure of neck growth, grain growth, and pore growth (Figs. 5(c) and (d)). However, heated-gas sintering show a closely-packed microstructure with large grains of about 300 nm and very few pores were found (Figs. 5(e) and (f)). The SEM analytical results reveal why the electrical resistivity of the Ag film sintered by the heated N2 gas flow is ~30% lower than that of the Ag film sintered in a convection oven. It is presumed that the additional connections among the nanoparticles without pore growth led to a decrease in the electrical resistivity. To assess the feasibility of applying the proposed method to PCB manufacturing, we performed a reliability evaluation with the inkjetprinted Ag patterns under the standard of the IPC, TM650. Various test patterns were created by Ag inkjet-printing on both a rigid FR4 substrate and a flexible PI film substrate for the reliability analysis. In the inkjet-printing process, the ink wettability of the substrate is a critical factor to make fine patterns [8,33,34]. In this study, wettability is controlled by a FC thin film coating followed by UV/O3 treatment to print fine and uniform Ag patterns with the desired dimensions. UV/O3 treatment can increase the surface energy of a non-wettable FC thin film. To examine the influence of the UV/O3 treatment on the surface wettability of the FC thin film, the surface energy of the substrates was evaluated by measuring the contact angles of two polar liquids (D.I. water and formamide) and one nonpolar liquid (diiodomethane). Table 2 shows the contact angles of the three test liquids, the surface energies, and microscopic images of printed single dots and lines for each surface treatment condition. Straight lines could be ink-jet printed with a 50% overlap rate without a merging or bulging phenomenon after UV/O3 treatment for 4 min. The treatment time was increased from 4 min to 10 min at an interval of 2 min and the surface energy was increased from 15.4 mJ/m2 to 43.8 mJ/m2. This means that the UV/O3 treatment contributes to creating high wettability. Regarding the surface energy of the FC thin film, Fig. 4. Change of sheet resistance and electrical resistivity versus head temperature. K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 Sintering conditions 95 Oven sintering Heated gas flow sintering 250 C, 1 hr Head Temp. = 600 C, 10 min (a) (c) (e) (b) (d) (f) Before sintering Observation view Surface view ( 100,000) Cross sectional view ( 100,000) Fig. 5. Scanning electron microscope images of Ag film before and after sintering and sintering conditions. the diameter of the printed Ag dots increased gradually from ~40 μm to ~155 μm and the line width increased from ~ 50 μm to ~200 μm. In this study, we selected five different test items and conditions used in the conventional PCB industry according to the standard of the IPC, TM650. Table 3 presents a summary of the test conditions, substrate type, and evaluation results for the reliability test items including the withstanding voltage, adhesive strength, thermal shock, pressure cooker, and bending tests. Fig. 6 shows a photographic image of inkjet-printed test patterns for the reliability analysis items (Fig. 6(a)) and the schematic design and dimensions of each test pattern (Fig. 6 (b)). The withstanding voltage test was conducted by transmitting 5000 V DC, 1 mA for 60 s through both ends of a 5 cm line pattern and examining it for any evidence of spark discharge, short circuiting, or dielectric breakdown. The test patterns were printed with a line width and spacing of 100 μm and a thickness of ~1 μm, as shown in Fig. 6(b). The test patterns were printed with a line width and spacing of 100 μm and a thickness of ~1 μm, as shown in Fig. 6(b). Figs. 7(a) and (b) shows photographic images of the withstanding voltage test pattern with the inset showing magnified images. The Ag patterns on the FR4 substrate maintained its initial shape in the withstanding voltage test without damage due to spark discharge, short circuiting, or dielectric breakdown phenomena (Fig. 7(a)), but the Ag patterns on the PI substrate were seriously damaged by the withstanding voltage test and showed failure phenomena of peel-off and disconnection (Fig. 7(b)). The adhesive strength test was performed using the ASTM D3359 rating method for the cross-cut tape test. Square 5 mm × 5 mm patterns were printed with a thickness of ~1 μm for ASTM D3359. The ASTM D3359 rating method employs a scale from 0B to 5B and the rating is calculated by observing the ratio of the pattern test area removed by a strip of 3M 610 Scotch tape [35]. The ASTM D3359 adhesive strength rating achieved by the test patterns was 5B for FR4 and 3B for PI, as shown in Figs. 7(c) and (d). The thermal shock test was conducted by observing the change in the insulation resistance after 100 cycles of temperature variation from −55 °C to 125 °C for 30 min. The test pattern was a single line of 4 cm length, 100 μm width and ~1 μm thickness. The variation in the resistance after the thermal shock tests was found to be ±4.5% for FR4 and ±4.3% for PI, respectively, with no signs of spark discharge or short circuiting. The pressure cooker test was conducted by measuring the insulation resistance through both ends between two independent Ag lines at 121 °C, 2 atm, and 97% RH after 48 h. The pressure cooker Table 2 Contact angles of the three test liquids, surface energies, and printed Ag pattern images for UV/O3 treatment time of FC films. UV/O3 treatment time of FC film Surface energy (mJ/m2) Contact angle of probe liquids (degree) D.I. water Diiodomethane Formamide 4 min 87.7 84.2 25.4 15.4 6 min 85.1 72.0 15.9 21.8 8 min 55.3 53.9 60.1 30.4 10 min 68.5 34.9 50.4 43.8 Single dot (ϕ: diameter) Line (W: line width) 96 K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 Table 3 Reliability test items, conditions, substrates, and evaluation results (RH: Relative Humidity). Test items Conditions Substrates Evaluation results Withstanding voltage No spark discharge, short circuiting, or dielectric breakdown at 5000 V DC, 1 mA, 60 s Adhesive strength No peel off in 1 mm cross-cut tape test Thermal shock Variation of resistance within ±10% at −55 °C, 15 min and 125 °C, 15 min, 100 cycles Pressure cooker Insulation resistance above 100 MΩ at 121 °C, 2 atm, 97% RH; 48 h Bending Angle of rotation: 135°, velocity of rotation: 175 times/min above 10,000 times FR4 PI FR4 PI FR4 PI FR4 PI PI Pass Fail Pass Fail Pass Pass Pass Pass Pass test is a standard for determining the occurrence of leakage current. The pressure cooker test was conducted by measuring the insulation resistance through both ends between two independent Ag lines at 121 °C, 2 atm, and 97% RH after 48 h. Two lines of 4 cm length, 1 mm width, and ~1 μm thickness were printed with a spacing of 100 μm. In the pressure cooker test, the average insulation resistance values and standard deviation after 48 h were 7.3 × 106 ± 2.2 MΩ for FR4 and 7.9 × 106 ± 2.1 MΩ for PI, respectively. A remarkable difference in the resistance was not observed. The serpentine-shape patterns for the bending test were printed with a line-width and spacing of 1 mm and length of 130 mm and thickness of ~1 μm on the PI substrate. The bending test was conducted by measuring the rotation number of the printed Ag patterns that could be bent or folded over just before failure. The samples were folded through an angle of 135° from their initial position at a rotation velocity of 175 cycles/min. The inkjet-printed Ag patterns passed the test criterion of more than 10,000 times, showing a value of 11,878 ± 1888 times for three samples. No damage Spark discharge and short circuiting 0% peel off (5B) ~13% peel off (3B) ±4.5% ±4.3% 7.3 × 106 ± 2.2 MΩ 7.9 × 106 ± 2.2 MΩ 11,878 ± 1888 times/min conventional oven sintering, the observations of lower resistivity and a closely-packed metallographic structure supported that the heated inert gas sintering process is applicable to printing-based PCB production. However, for PI film-based flexible PCB production, the proposed sintering method is limited by poor adhesion of the printed Ag patterns to PI films. Further optimization of the proposed sintering method should be accompanied with a specific approach to find suitable substrate surface conditions and Ag nanoparticle-based ink formulation. Also, future studies will focus on investigating the compatibility of the 16 cm 16 cm 4. Conclusions Heated inert gas sintering was studied as a thermal sintering method of printed metal conductive patterns and the feasibility of its application to PCB manufacturing was evaluated by a reliability characterization of inkjet-printed Ag patterns sintered by the proposed approach. The inert gas flow was heated by passing N2 gas through a heating head of 300 to 700 °C and the heated N2 gas flow was jetted from a nozzle with a length of 400 mm, and a width of 5 mm onto the substrates. The IR thermal image analysis showed that the temperature at the center region of the heated N2 gas is above 250 °C and at a point 5 cm-away left/right is 40–42% lower after the head temperature reached 600 °C. It was further confirmed that the surface temperature is above 250 °C by temperature measurement using colorimetric thermo-label sensors. In particular, heated inert gas sintering showed better performance than the oven sintering method in the analysis of electrical resistivity and metallographic structures according to the temperature change of the heating head. The electrical resistivity of the heated N2 gas-sintered Ag film is ~30% lower than that of the Ag film sintered in a convection oven although its electrical resistivity is approximately 2.5 times greater than that of bulk Ag. Heated N2 gas sintering yield a closely-packed microstructure with a large grain growth of about 300 nm and few or no pores within the intra-microstructure overall. The surface wettability of the substrate was controlled by FC thin film coating followed by UV/O3 treatment to print fine and uniform Ag patterns. A reliability evaluation of the inkjet-printed Ag patterns for PCB application was performed under the standard of the IPC, TM650. Various test patterns were fabricated by Ag inkjet-printing on both a FR4 substrate and a PI film substrate. Ag patterns printed on the FR4 substrate passed all test items: withstanding voltage test, adhesive strength test, thermal shock test, and pressure cooker test, but Ag patterns printed on the PI substrate failed the withstanding voltage test and showed poor adhesion in the adhesive strength test. In conclusion, compared with (a) 5 mm 4 cm 5 mm Adhesion strength test pattern Thermal shock test pattern 4 cm 13 cm 1 mm 100 Pressure cooker test pattern Bending test pattern 5 cm L/S=100 /100 Withstanding voltage test pattern (b) Fig. 6. Standard test patterns for reliability analysis items: (a) a photograph of inkjetprinted test patterns on PI films; (b) schematic design and dimension of each test pattern. K.-Y. Shin et al. / Microelectronic Engineering 193 (2018) 91–97 97 100 m 100 m (a) (b) 1 mm 1 mm (c) (d) Fig. 7. Photographic and microscopic images: (a) FR4 substrate after withstanding voltage test; (b) PI substrate after withstanding voltage test; (c) FR4 substrate after adhesive strength test; and (d) PI substrate after adhesive strength test (the insets show magnified pattern images in Figs. 7(a) and (b)). heated gas sintering process with a roll-to-roll process for flexible electronic device production. [16] Acknowledgment [17] We would like to acknowledge the financial support from the Industrial Technology Innovation Program (Project grant No. 10063277) of the Ministry of Trade, Industry and Energy (MOTIE) of the Republic of Korea and the R&D Convergence Program (Project grant No. CAP-1504-KITECH) of the National Research Council of Science & Technology (NST) of the Republic of Korea. [18] [19] [20] [21] [22] [23] References [24] [1] P. Calvert, J. Chem. Mater. 13 (2001) 3299–3305. [2] B. Ando, S. Baglio, A.R. Bulsara, T. Emery, V. Marletta, A. Pistorio, Sensors 17 (2017) 748. [3] G. 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