Digitally Printed Dewetting Patterns for Self‐Organized

© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim7708 wileyonlinelibrary.com

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Microelectronics

Ralph Eckstein , * Milan Alt , Tobias Rödlmeier , Philip Scharfer , Uli Lemmer , and Gerardo Hernandez-Sosa *

R. Eckstein, Dr. M. Alt, T. Rödlmeier, Prof. U. Lemmer, Dr. G. Hernandez-Sosa Karlsruhe Institute of Technology Light Technology Institute Engesser Str. 13, 76131 Karlsruhe , Germany E-mail: [email protected]; [email protected] R. Eckstein, Dr. M. Alt, T. Rödlmeier, Dr. P. Scharfer, Prof. U. Lemmer, Dr. G. Hernandez-Sosa InnovationLab Speyererstr. 4, 69115 Heidelberg , Germany Dr. P. Scharfer Karlsruhe Institute of Technology Institute of Thermal Process Engineering Thin Film Technology Kaiserstr. 12, 76131 Karlsruhe , Germany Prof. U. Lemmer Institute of Microstructure Technology Karlsruhe Institute of Technology Hermann-von-Helmholtz-Platz 1 76344 Eggenstein-Leopoldshafen , Germany

DOI: 10.1002/adma.201602082

a large variety of functional inks in a continuous process and therefore contributing to the envisioned high-throughput low-cost fabrication of future electronics.

Herein, we present the self-alignment of multilayer opto-electronic devices induced by highly dewetting, directly printed patterns and discuss the working mechanism in terms of fl uid and substrate interactions. To demonstrate this process via-bility, we utilize a digitally printed low-surface-energy UV-cur-able epoxy resin formulation for patterning a nanoparticular (NP) Ag ink on commonly used fl exible substrates in the fi eld of printed electronics, such as polyethylene terephthalate (PET). We used contact-free and additive printing techniques such as aerosol-jet printing (AJP) and inkjet printing (IJP) for the fabrication of the epoxy pattern and the local deposition of the functional ink, respectively. AJP was chosen due to its dig-ital prototyping and small feature-size capabilities on the order of tens of micrometers. Furthermore, the AJP work principle allows for larger aspect ratios of the printed SU-8 patterns compared to IJP. Detailed information about the AJP process can be found in refs. [ 27 ] and [ 39 ] . Finally, we demonstrate the advantages of the process in terms of registration accuracy and reproducibility in the fabrication of multilayer organic photo-detectors (OPD), organic fi eld-effect transistors (OFETs), and integrated unipolar ring oscillators with state-of-the-art per-formance. The all-printed OPDs with a size of (45 × 175 µm 2 ) exhibited high On–Off ratios of approximately fi ve orders of magnitudes with low dark currents of ≈10 −4 mA cm −2 at −1 V reverse bias. The n-type OFETs, with channel lengths defi ned by the line width of the AJP epoxy resin, showed threshold volt-ages of ≈1 V. The high reproducibility of the OFET processing enables the fabrication of ring oscillators showing working fre-quencies up to 400 Hz.

A schematic diagram of the simple two-step patterning pro-cess is shown in Figure 1 a. It involves the initial printing of the cross-linkable epoxy resin (SU-8) by AJP onto the substrate at ambient conditions. After UV and thermal cross-linking of the SU-8 patterns, the NP Ag ink was locally deposited by IJP, brushing, spray coating, or blade coating onto the substrate. Finally, after the self-organization of the Ag ink took place, the wet Ag fi lm was vacuum dried and thermally annealed. Figure 1 b presents an optical micrograph of a dewetted Ag stripe which was IJP over an AJP SU-8 pattern on PET. The ≈11 µm wide SU-8 line completely disrupts the continuity of the conductive Ag line. The image sequence over time from wet ink deposition to the completed alignment of the ink into the target pattern is illustrated in Figure 1 c. The images show the assembly of fi nger structures with feature sizes in the order of ≈100 µm after simply brushing the Ag ink with a swab. Videos of the process and additional experiments with spray and blade

The current research on printed electronic devices, such as organic solar cells and photodiodes, [ 1,2 ] light-emitting diodes, [ 3–6 ] thin-fi lm transistors, [ 7–10 ] sensors, [ 11 ] and batteries, [ 12,13 ] enables an exceptional variety of electronic applications. The mating of those electronic components in integrated circuits (ICs) for smart packaging, [ 14–18 ] remote sensing, [ 19,20 ] inexpensive medical diagnostics, or consumer electronics [ 21–23 ] fabricated by printing techniques can potentially constitute a keystone technology for the development of the Internet of Things. [ 24,25 ] Nevertheless, the future success of printed electronics and the development of wide-spread high-performing applications still depend on overcoming the current technological hurdles, such as the lack of both reproducible feature-sizes and registration accuracy of microscale multilayer devices, especially for methods compat-ible to high-throughput industrial requirements. On the one hand, printing and deposition techniques have undergone impressive improvements concerning direct printing of high resolution features. [ 7,26–30 ] On the other hand, surface modifi -cation processes involving hydrophobic self-assembled mono-layer (SAM) treatments, [ 31 ] electron-beam direct writing, [ 32 ] or physical processes such as nanoimprinting, [ 33 ] have been devel-oped as pretreatment strategies to obtain micrometer scale fea-tures by tuning the wettability of the substrate. Complementary approaches exploit the effect of wetting and capillarity driven self-alignment guided by either hot-embossed microfl uidic channels or microcontact stamping. [ 34–38 ] However, combining the advantages of high-resolution direct printing with local-ized dewetting would enable micrometer-scaled patterning for

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coating of the functional ink can be found in Video S1 and S2 (Supporting Information).

Figure 2 shows optical micrographs, 3D surface profi les, and topographical profi les of digitally micropatterned struc-tures with various geometries. The square pattern illustrates the assembly of the Ag ink in differently large areas, while the ring and spiral patterns illustrate the possibility of fabri-cating complex, conformable, or stretchable patterns with fea-ture sizes below 20 µm. The SU-8 line height in each of these

examples was ≈1.5 µm; however, it can be adjusted depending on the target application. In other words, the SU-8 aspect ratio would also defi ne device architecture parameters such as the maximum achievable fi lm thickness or the spacing between functional patterns (e.g., OFET channel length, OPD pixel size, etc.). Figure S1 (Supporting Information) shows the tunability of the line heights by varying the AJP printing parameters. The presence and shape of the convex profi le cross-section of the resulting metal layers between the SU-8 wall edges was found

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Figure 1. a) Schematic drawing of the patterning process starting with AJP of the epoxy followed by the deposition, drying, and annealing of the func-tional ink. b) IJP Ag stripe deposited onto an AJP SU-8 patterned PET substrate. The wet Ag ink forms an ≈11 µm gap predefi ned by the SU-8 structure. c) Time-lapsed sequence of the self-organization of brushed Ag ink and a magnifi cation of the structured microelectrodes after the annealing step.

Figure 2. a) Light microscopy images of self-organized Ag microstructures by AJP SU-8 patters. Bright and dark areas denote Ag and SU-8, respectively. b) 3D images of the corresponding structures recorded with a confocal microscope and c) cross-sectional height profi les extracted from the 3D images at the indicated white lines.

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to be strongly infl uenced by the drying conditions of the Ag ink as observed in Figure S2 (Supporting Information). However, a more detailed investigation of this issue will be addressed to future work.

In order to gain further insight into the self-organizing pat-terning process, we investigated its correlation to the surface tensions ( σ ) of common solvents used in printed electronics. First, a cleaned PET substrate was partially blade coated with SU-8 to form a step edge of ≈3–5 µm, as schematically shown in Figure 3 a. Subsequently, solvent droplets (≈2 µL) were depos-ited at the step edge and visually observed to determine if the solvent repels from the epoxy or not. Figure 3 b exemplifi es

the repelling effect with a droplet of the Ag ink, where the fl uid repeals from the SU-8 within seconds. This experiment was performed with all solvents listed in Table 1 which shows the solvent properties and whether or not complete dewet-ting from the SU-8 surface took place. Furthermore, a series of methanol:water (MeOH:H 2 O) mixtures with varying MeOH fractions ( χ MeOH ) was used to systematically probe the impact on the SU-8 surface repulsion to subtle changes of the polar ( σ P ), dispersive ( σ D ), and total ( σ total ) surface tension of the fl uid (see Figure 3 c). The correlation between the repulsion of a solvent or solvent mixture from the SU-8 surface and the σ P and σ D is depicted in Figure 3 d. The plotted circles indicate

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Figure 3. a) Schematic drawing of the SU-8/PET step edge with a deposited droplet before (I) and after (II) dewetting from the SU-8. b) Temporal sequence of the dewetting of a Ag-ink droplet (2 µL) deposited on the step edge. c) Polar, dispersive, and total surface tension of MeOH:H 2 O mixtures with different MeOH fractions ( χ MeOH ). d) Wetting envelopes and surface free energies (squares) of PET and SU-8. Polar and dispersive surface ten-sions of dewetting (circles) and not/insuffi ciently dewetting (triangles) test fl uids. MeOH:H 2 O mixtures are shown in green while pure solvents are shown in blue.

Table 1. Summary of surface tensions including polar and dispersive part, vapor pressures, boiling points, and viscosities of different solvents.

Solvent Surface tension/energy [mN m −1 ] Vapor pressure [kPa] Boiling point [°C]

Viscosity [cP] SU-8 dewetting [yes/no]

Total Polar Dispersive (@20 °C) (@20 °C)

Water (H 2 O) 72.6 50.8 21.8 2.4 100 0.98 N

Ethylene glycol (EG) 47.5 18.2 29.3 0.5 198.0 26 N

Methanol (MeOH) 24.0 5.1 18.9 13.0 64.7 0.55 Y

Ethanol (EtOH) 24.6 6.4 16.2 5.95 78.0 1.2 Y

Dimethylsulfoxide 44.0 8.0 36 0.055 189.0 2.14 Y

Toluene 28.4 2.3 26.1 5.4 110.0 0.59 Y

o -Xylene 29.3 3.0 26.3 0.7 144.5 0.76 Y

Ag ink a) 35.5 6.8 28.7 – – 10–18 Y

Substrates

SU-8 27.4 3.1 24.3 n.a. n.a. n.a. n.a.

PET b) 45.1 12.2 32.9 n.a. n.a. n.a. n.a.

a) Silverjet DGP-40LT-15C; b) Hostaphan GN-4600.


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a repulsion of the fl uid, while triangles represent that no or insuffi cient repulsion (i.e., no solvent motion) of the droplet took place. It was observed that the fl uids with σ P and σ D between the wetting envelopes of SU-8 and PET show clear dewetting. In contrast, the inks with σ located outside both wetting envelopes show no dewetting since both surfaces are similarly unfavorable. We observed that fl uids with σ P and σ D slightly inside the wetting envelope of SU-8 still tend to repeal from the epoxy instead of wetting both structures, which could be attributed to higher attraction between the fl uid and the PET. Increasing the wetting envelope of PET, by plasma treatment (with argon or oxygen), was observed to cause dewetting on the SU-8 structures for all test fl uids by increasing its affi nity to the PET surface (Figure S4, Supporting Information). However, the outcome of the self-organization process will also depend on dynamic interactions between the different surfaces and the fl uid during solvent evaporation. Therefore, it has to be ensured that the dewetting process is not hindered by the gradual evolu-tion of the surface tension and viscosity during drying. This can be optimized by the appropriate choice of solvents in terms of boiling point and vapor pressure.

The equilibrium contact angles (CA) of Ag ink on PET (≈20°) and SU-8 (≈43°) are shown in Figure 4 a. The relation between the CA and the σ is typically described via Young’s equa-tion when assuming a perfectly fl at surface. [ 40 ] However, sur-face roughness in the macro-, micro-, and nanoscopic regime and chemical heterogeneity of the surface can affect the CA, as described by the Wenzel (Equation ( 1) ) and Cassie-Baxter models. [ 41–43 ] The effective roughness emerging from the ratio

between the actual and projected area is represented by r , as shown in Equation ( 2) and schematically illustrated for the pro-truding SU-8 structures in Figure 4 b. In this work, we took into account the increase of surface area due to the size of the struc-ture. The structure topography in the micro and nanoscale is expected to further infl uence the wetting; however, a more detailed investigation of the correlation of the SU-8 surface roughness and the printing process is still to be performed in future work. The rms surface roughness of a typical AJP SU-8 structure used in this work was determined to be 0.4 nm from the atomic force microscope measurement showed in Figure S3 (Supporting Information)

rcos cos*θ θ= ⋅ ( 1)

rA

Aact

proj

= ( 2)

The Young–Dupré equation (Equation ( 3) ) describes how much work, W A , needs to be expended to separate a liquid from a solid phase [ 44 ]

W 1 cosA lσ θ( )= + ( 3)

where σ l represents the total surface tension of the liquid phase. In the present case, the fl ow of the Ag Ink toward PET can be explained by the lower W A required to separate the ink from the SU-8 (60.6 J m −2 ) than on PET (67.9 J m −2 ).

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Figure 4. a) Contact angles of Ag ink on PET and SU-8. b) Schematic drawing of the projected ( A proj ) and actual area ( A act ) of the SU-8 structures. c) Inverted split-ring resonators and slot antennas processed on a 5 µm thick PI foil. d) Self-organized Ag structures on a PCB (FR-4 glass epoxy). e,f) Ring structures printed on 1.4 and 175 µm thick PET foil for THz applications.


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The versatility of the process is demonstrated in Figure 4 c–f, which shows Ag patterned by SU-8 structures with feature sizes of <20 µm on (c) polyimide (PI), (d) con-ventional printed circuit boards (PCB, FR-4 glass epoxy), and (e) 1.4 µm and (f) 175 µm PET foil. The total surface ener-gies including the polar and dispersive contributions of the different substrates can be found in Figure S4 (Supporting Information). In all cases the SU-8 reveals the lowest σ com-pared to the examined substrates. Consequently, it can be assumed that the difference in σ between SU-8 and the sub-strate strongly correlates with the success of the self-organi-zation of a specifi c fl uid.

To demonstrate the viability of the presented patterning process for printed electronic devices, we fabricated organic photodiodes, as shown in the scheme in Figure 5 a. These opto-electronic devices embody the requirements needed for micro-electronic applications, especially precise layer deposition. The reservoir formed by the protruding SU-8 structures facilitates the deposition of thick layers, reducing the dark current den-sity and the probability of shortcuts. [ 1 ] Moreover, this reservoir ensures an excellent registration accuracy of any subsequent deposited layers. The aqueous solution of poly(3,4-ethylene-dioxythiophene): polystyrene sulfonate (PEDOT:PSS) did not show any repulsion from the SU-8 in combination with active material, allowing for an electrical connection between the top electrodes and the corresponding Ag contact pad. Figure 5 b presents microscope images of the patterned Ag back-elec-trode, the completed OPD devices, and a magnifi cation of a single OPD pixel with an active area of 0.0079 mm 2 (45 µm × 175 µm) showing dark current densities of ≈10 −4 mA cm −2 , a photo current density of ≈10 mA cm −2 at −1 V reverse bias resulting in an On–Off ratio of almost 10 5 . The linearity of the OPDs response as a function of light intensity is shown

in Figure 5 d for −1 and −2 V bias voltage under white light excitation.

As a second example, n-type OFETs were fabricated using AJP SU-8 patterns to defi ne the source–drain electrodes and channel lengths. Figure 6 a illustrates the transistor architec-ture comprising the n-type semiconductor N2200 (Polyera [ 45 ] ), parylene C as the dielectric, SAM treated Ag source–drain contacts separated by the SU-8 line, and an inkjet-printed Ag gate electrode. It is to be noted that no dewetting of the semiconductor layer on the SU-8 surface occurred due to the fast drying of the solvent during the spin-coating process. The output and transfer characteristics of a typical device are plotted in Figure 6 b,c. More information concerning the devi-ation of the device characteristics of multiple OFETs is shown in Figure S5 (Supporting Information). The low threshold voltage of ≈1 V can be ascribed to the low injection barrier of the Ag electrodes to the semiconductor as a result of the SAM treatment. [ 46 ] Furthermore, we fabricated ring oscillators in order to emphasize the device reproducibility and the applica-bility of the process to patterning over larger areas. A generic single inverter stage of the three-stage oscillator is presented in Figure 6 d. Figure 6 e shows a photograph of the oscillator and its circuit diagram. The ring oscillator contains three inverter steps each with a load ( L 1–3 ) and a drive transistor ( D 1–3 ), followed by an additional output buffer stage (BS). Due to the complex and entangled dependency of an integrated circuit’s electrical behavior to the single OFET performance, gate-leakage currents, overlap capacities, and contact resist-ances, we opted for a Simulation Program with Integrated Circuit Emphasis (SPICE) simulation prior to fabrication of the SU8 structures. The device geometries of respective drive and load OFET were adjusted accordingly. In this simulation, we used an equivalent circuit designed to model the nonideal

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Figure 5. a) Schematic drawing of the fully printed organic photodetector comprising structured Ag back-electrodes on PET foil. b) Microscope images of the patterned Ag electrodes, the fi nalized printed device, and a magnifi cation of one pixel (bottom image) with a 45 × 175 µm 2 active area. c) Dark current density (dashed line) and current density–voltage ( J – V ) characteristics under white light illumination at intensities from 0.1 to 100 mW cm −2 . d) J and responsivity R as a function of light intensity at −1 and −2 V reverse bias.


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behavior of OFET specifi cally. [ 47 ] A more detailed description of the simulation model and the SU-8 tool path can be found in Figure S5 (Supporting Information). The actual channel length of the load and drive transistors of each inverter step was defi ned by a curved SU-8 line surface of ≈30 µm. The load OFET comprised a channel width of 400 µm, while the drive transistor was designed to be 100 times wider (40 mm). The channel width of the BS load transistor ( L BS ) was dimen-sioned to have twice the size of the load transistors for the inverter stages ( L 1–3 ) to 800 µm. The AC output voltage of the fabricated ring oscillator at V dd 100 V DC supply voltage oscil-lates with a stable frequency of up to 400 Hz highlighting the consistent performance of all subdevices.

In summary, we presented a method to fabricate micro-patterns using self-organizing solution processable functional materials. It was found that AJP process addresses the current needs of printed electronics in terms of reliability, reproduc-ibility, accuracy, and simplicity, which could be emphasized by the fabrication of electronic devices, such as OPDs, OFETs, and integrated circuits in form of ring oscillators with state-of-the-art performances. A broad variety of solvents and substrates com-monly used in printed electronics were investigated and the requirements for the fl uid and substrate were explored. Patterns with feature sizes of ≈10 µm were fabricated on PET, with proof of principle tests presented on PI, glass, and commercially PCB. Owing to the use of digital techniques the presented method is expected to be useful for the addition of microfabricated opto-electronic devices in integrated systems. Moreover, it has the potential to be transferred to or combined with other printing techniques for its application in other fi elds of functional printing.

Experimental Section PET from Hostaphan (GN4600, Mitsubishi Plastics Inc.) was used as a substrate for all measurements and presented devices. The PET was cleaned with acetone and isopropanol for 10 min before use. The SU-8 (2025, MicroChem) was diluted with γ-butyrolactone (GBL) and 3-heptanone in a ratio of 1:1:1 resulting in a formulation with 24% solid content. The SU-8 from experiments in Figure 3 was blade coated on PET resulting in 3–5 µm step edge using the same ink formulation as for the AJP. All SU-8 patterns were printed with an aerosol jet printer (AJ-300, Optomec), using an ultrasonic atomizer section and a ceramic nozzle with a 100 µm diameter. The AJ printing parameters, such as sheath and atomizer gas fl ows, atomizer ultrasonic power, as well as printing speed and distance between nozzle and substrate were properly adjusted for an optimized printing outcome for the respective application. The parameters for tube temperature were fi xed to 75 °C and the substrate temperature were fi xed to 25 °C for all experiments. The printed patterns were exposed to UV light (365 nm) for 5 min and afterward thermally soft baked at 120 °C for 15 min on a hotplate. The Ag ink (Silverjet DGP-40LT-15C, Sigma-Aldrich) was brushed with a clean room swab (Figure 1 c) or inkjet printed (Figure 1 b) with a Dimatix DMP-2831 and a Fujifi lm Dimatix 10 pL cartridge. The stage temperature of the inkjet printer was set to 25 °C. The wet Ag pattern was then vacuum dried at 15 mbar for 20 min and fi nally annealed at 120 °C for at least 10 min on a hotplate.

OPD Fabrication : Ag patterns were fabricated as described with brushed Ag ink. Subsequently, aluminum doped zinc-oxide (AZO) NP (N-21 X, Nanograde) diluted with GBL and 3-heptanone in a ratio of 1:2:0.5 was AJ printed to obtain a 20–30 nm AZO layer. The fi lm was annealed at 100 °C for 5 min on a hotplate. A 1 µm thick layer of poly({4,8-bis[(2-ethylhexyl)oxy]benzo[1,2-b:4,5-b′]dithiophene-2,6-diyl}{3-fluoro-2-[(2-ethylhexyl)carbonyl]thieno[3,4-b]thiophenediyl}) commonly known as PTB7 (1-material) blended with [6,6]-phenyl-C71-butyric acid methyl ester or PC70BM (Solenne) in a ratio of 1:1.5 (10 g L −1 ) dissolved in 1,2-dichlorobenzene with 3 vol% of diiodooctane was AJ printed on top of the Ag/AZO cathode. The fi lm was then dried

Figure 6. Ring oscillator based on OFETs comprising digital SU-8 micropatterned source–drain electrodes. a) Schematic drawing of an OFET with a channel length defi ned by the SU-8 line width. b) Output and c) transfer characteristics of an OFET with 40 mm channel width ( w ) and ≈30 µm channel length. d) Microscope images of a load (top) with w = 0.4 mm and a drive (bottom) transistor with w = 40 mm channel width. e) Photograph of a substrate comprising two three-step ring oscillators (top). Circuit diagram of ring oscillator including an additional buffer stage (bottom). f) Output voltage at 100 V DC supply voltage showing an oscillation frequency of ≈400 Hz.


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was AJ printed using a diluted PEDOT:PSS dispersion (IJ 1005, Orgacon) comprising 1 vol% zonyl and fi nally dried in vacuum (15 mbar) in an antechamber and then transferred into the glovebox for encapsulation with a moisture and oxygen barrier foil (3M).

OFET and Ring Oscillator Fabrication : Ag patterns were printed as described via IJP and dried in vacuum. However, the annealing step was done a 135 °C on a hotplate inside a nitrogen fi lled glovebox. Subsequently, the SAM forming molecule bisjulolidyldisulfi de (9,9′-disulfanediylbis(2,3,6,7-tetrahydro-1H,5H-pyrido[3,2,1-ij]quinoline)) was deposited by a 1 min immersion in a 0.75 × 10 −3 M ethanol solution. The semiconductor (N2200, Polyera [ 45 ] ) was spun with a nominal 80 nm layer from 8 mg mL −1 CB solution inside a N 2 glovebox. As dielectric a chemical vapor deposited (CVD) 250 nm ParyleneC layer was deposited with a coating system (PDS2010, Specialty Coating Systems, IN, USA) to ensure a homogeneous coverage of the entire structured surface. As the fi nal step, the gate layer was IJP to complete the devices, followed by a vacuum drying step (15 mbar) and then thermal annealing at 120 °C for 10 min also under vacuum.

Characterization : CA of the MeOH:H 2 O mixtures were measured using a Krüss DSA-100 contact angle measurement setup. Additionally, surface free energies of the substrates and SU-8 surface were measured using H 2 O, EG, diiodomethane, and glycerine as test fl uids and calculated using the Young’s equation. Microscope images were captured with a Nikon Eclipse 80i. Topography measurements were performed using a Dektak profi lometer (Veeco, Dektak 150) and a Sensofar Plu Neox 3D profi lometer with a confocal 50x lens (Aperture 0.95). J – V characteristics of the OPDs were measured using a 400 W solar simulator (LOT-QuantumDesign), calibrated with a dedicated Si photodiode (LOT-QuantumDesign), and a Keithley 2636 source measurement unit. Light intensity was varied using a neutral density fi lter set. Dark currents and transistor measurements were carried out using an Agilent 4155C Semiconductor Parameter Analyzer (Agilent Technologies, CA, USA) and a shielded probe station.

Supporting Information Supporting Information is available from the Wiley Online Library or from the author.

Acknowledgements The authors gratefully acknowledge Anthony J. Morfa and Jerzy Kowalewski for their support and helpful contributions. Nanograde is acknowledged for providing the metal-oxide nanoparticle dispersions. 3M is acknowledged for providing the adhesive barrier foil for device encapsulation. Special acknowledgements are given to the Karlsruhe School of Optics and Photonics for their support. This work was funded by The German Federal Ministry of Education and Research (BMBF) through grant FKZ: 13N13691.

Received: April 19, 2016 Revised: May 25, 2016

Published online: June 27, 2016

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