Functional Dyes – Innovations in Medicine and Technology Functional Dyes for Organic Semiconductor Sensors Siemens AG Corporate Technology Erlangen, Germany Dr. Maria Sramek, Dr. Oliver Hayden, Sandro Tedde, Tobias Rauch Siemens AG, Corporate Technology CT T DE HW 3 Global Technology Field „Organic Electronics“ Günther-Scharowsky-Straße 1, D-91050 Erlangen Phone: +49 9131 7 32443 Email: maria.sramek@siemens.com Web: http://www.siemens.com/corporate-technology Copyright © Siemens AG 2012. All rights reserved. Page 1 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Motivation R&D Program „System Solutions“ Organic semiconductor Nanorods Quantum dots nanocrystals Fullerenes Carbon nanotubes „Working Nanotechnology“ From Materials to Business Concepts X-ray imaging Industrial sensors In-vitro diagnostics Open innovation Copyright © Siemens AG 2012. All rights reserved. Page 2 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Outline 1. Introduction 2. Processing 3. Applications for Visible and Infrared Range Copyright © Siemens AG 2012. All rights reserved. Page 3 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Outline 1. Introduction 1.a - Review 1.b - Organic Photodiodes 2. Processing 3. Applications for Visible and Infrared Range Copyright © Siemens AG 2012. All rights reserved. Page 4 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Aim: Integration to cut costs (CMOS paradigm) Roll-to-roll Molecules/Polymers 12‘‘/30 cm Workhorse - wafer Crystalline and impurityfree substrates „Silicon is Gods Material“ and What About Organics? Organic electronics – which way to go: - Low-cost processing vs. efficiency - Performance vs. material costs/purity - Large footprint vs. integrated solutions - Lifetime vs. Flexibility - Premium vs. low-cost products Copyright © Siemens AG 2012. All rights reserved. Page 5 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd „Nobel History“ of Conductive Organics 2000 1996 Fullerenes („Buckyballs“) Conductive Polymers „Replace silicon“ and „organics beyond silicon bandgap limit“ Copyright © Siemens AG 2012. All rights reserved. Page 6 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Properties of Small Molecules & Polymers Small molecules Amorphous to highly crystalline, designed for the target application OLED - OFET High mobility possible Cheap purification (sublimation, re-crystallization) Ready for deposition – minor batch dependence Vacuum deposition Polymers Amorphous to crystalline domains, designed for the target application (any) Low to medium mobility Expensive purification (chromatography, re-precipitation) Most are only soluble in chlorinated & aromatic solvents Specific deposition formulation necessary – major batch dependence Solution deposition (no vacuum deposition processes) The performance requirements of the application influences the choice of materials and the setup of equipment Copyright © Siemens AG 2012. All rights reserved. Page 7 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Device Fabrication Silicon Organics Copyright © Siemens AG 2012. All rights reserved. Page 8 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Revolution to Evolution Example of OLED Display Developments Uni Bayreuth 1994 Sony 11-inch OLED 2008 Samsung 2009 Philips, Passiv Matrix 1999 BenQ/Siemens Activ Matrix 2006 Sanyo-Kodak 2000 Mitsubishi 155-inch OLED 2009 The Holy Grail – Flexible TV Copyright © Siemens AG 2012. All rights reserved. Page 9 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Pros and Cons Pros: Technology is compatible with Large area processes (low cost) Low temperature processing (low cost) Molecules and polymers can be tailored for specific electronic or optical properties Compatible with inorganic semiconductors Cons: Low carrier mobility Electronic and optical stability of the materials Processing is incompatible with classical processing in semiconductor industry Copyright © Siemens AG 2012. All rights reserved. Page 10 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Outline 1. Introduction 1.a - Review 1.b - Organic Photodiodes 2. Processing 3. Applications for Visible and Infrared Range Copyright © Siemens AG 2012. All rights reserved. Page 11 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Organic Diode Solid state: PN-junction Organic: „Bulk heterojunction“ O Fullerene OM e 4+ O O + OM e O p-type n-type - OM e 4+ O C O 2- C OM e O - C OM e - C O - C OM e 3- C O OM e O - C OM e O - - O C OM e C 3- C 3- O OM e C OM e 2- C Depletion region 2- C 3- - C C 2- 4- O C 3- C OM e C Anode Cathode Semiconducting polymer Anode Cathode • Bulk heterojunction = blend of electron donor/acceptor (eg. polythiophene/fullerene) • No distinct pn-junction as in solid-state devices • High absorption coefficient of the semiconducting polymers (~105 cm-1 ) Copyright © Siemens AG 2012. All rights reserved. Page 12 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Layer Stack of Organic Photodiodes (OPDs) Encapsulation Cathode Bulk heterojunction (P3HT/PCBM/quantum dots) Interlayer ITO (Anode) ITO (Anode) Substrate Copyright © Siemens AG 2012. All rights reserved. Page 13 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd VIS to NIR Spectral Sensitivity Organic absorber up to ~1 µm Inorganic absorber >1 µm 1,0 80 0,8 70 50 EQE (%) EQE (normalized) 60 0,6 40 30 20 10 0 0,4 -10 400 500 600 700 800 900 1000 1100 Wavelength (nm) 0,2 0,0 400 Standard P3HT/PCBM (cf. plastic solar cells) 500 600 Low bandgap absorber 700 800 900 1000 Wavelength (nm) Copyright © Siemens AG 2012. All rights reserved. Page 14 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd 0 10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 10 -7 10 -8 10 -9 -4 1x10 AM 1.5 (solar) 2 10 Statistics over 100 devices Current density (mA/cm ) 10 1 532 nm @ 780 µW/cm2 Dark currents -4 1x10 -5 8x10 -5 6x10 -5 4x10 -5 2x10 0 5V.dark Dark current Photocurrents 2 OPD active area 1 cm² -5 -4 1V.dark 0,35 Current density (mA/cm ) Current Density (mA/cm²) Current/Voltage Characteristics -3 -2 -1 Voltage (V) 0 1 2 0,30 0,25 0,20 0,15 5V.light 1V.light Forward bias Reverse bias Copyright © Siemens AG 2012. All rights reserved. Page 15 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Outline 1. Introduction 2. Processing 3. Applications for Visible and Infrared Range Copyright © Siemens AG 2012. All rights reserved. Page 16 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Coating Techniques Comparison: Spin coating / Doctor blading / Spray coating PEDOT:PSS Spin coating Doctor blading Spray coating Copyright © Siemens AG 2012. All rights reserved. Page 17 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Spray Coating as Fabrication Process for OPDs OPD fabrication with spray coating in ambient conditions: Substrate independence Adjustable layer thickness Multiple spray-coated layers Flexibility using solvents Layer roughness is not a limitation Low/high throughput technique Scalable technology Movie „Spray coating of OPDs“ S. Tedde et al., Fully Spray Coated Organic Photodiodes, Nano Letters 9 (3), 980 (2009) Copyright © Siemens AG 2012. All rights reserved. Page 18 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Outline 1. Introduction 2. Processing 3. Applications for Visible and Infrared Range Copyright © Siemens AG 2012. All rights reserved. Page 19 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Application in the Visible Range: Organic Matrix X-Ray Detector Backplane Pixels Processed panel X-Ray image of hand phantom: Copyright © Siemens AG 2012. All rights reserved. Page 20 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Application in the NIR Range: Small Bandgap Polymer NIR OPDs – Fabrication Parameters Acknowledgements: Substrate size: 50x50 mm² Number of OPDs on each substrate: 16 Single OPD active area : 71.4 mm² poly[2,6-(4,4-bis-(2-ethylhexyl)-4H-cyclopenta[2,1-b;3,4b ]dithiophene)-alt-4,7-(2,1,3-benzothiadiazole)] (PCPDTBT) Semiconductor: blend of PCBM / PCPDTBT PCPDTBT Eg: 1.46 eV Easy and fast production processes Large area (cm² range) Thin (< 1mm) Semitransparent Copyright © Siemens AG 2012. All rights reserved. Page 21 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Signal (20*log(U/U0)) [dB] Dynamic Response and f-3dB 0 -2 -4 f-3bB= 130 KHz -6 Signal [dB] -3dB -8 -10 10 100 1k 10k 100k Frequency [Hz] Active area: 0.7 cm2 Light source: - 1 KingBright SMD Chip LED KPL-3015SRC-PRV ( peak ~660 nm) super bright red light - Light intensity ~ 130 µW/cm² Copyright © Siemens AG 2012. All rights reserved. Page 22 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Application in the NIR Range: Light Barrier with OPDs Motivation Demonstrate potential of organic photodiodes for new multidimensional light barrier applications Show that OPDs can substitute „silicon“ @ NIR Optic-free light barrier for variable emitter/detector distance High flexibility with respect to active area (mm²-cm²) Quadrant functionality: - Self-alignment of emitter/detector - Determination of direction/angle, and speed Specification Copyright © Siemens AG 2012. All rights reserved. Page 23 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Organic Quadrant Sensor (~4 cm² Active Area) Resolution Limit ~1 µm 1,0 0,0 Distance (µm) -1,0 Y-axis -2,0 -3,0 -4,0 -5,0 -6,0 -7,0 40 1.5 µm steps @ 15° 42 44 46 48 Time (s) 50 (B D ) ( A C ) A B C D X-axis X 52 ( A B ) (C D ) Y A B C D 54 4 organic photodiodes (A, B, C, D) giving X/Y positioning results for a light spot Absolute X/Y position is calculated according to formula Copyright © Siemens AG 2012. All rights reserved. Page 24 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Application in the NIR Range: PSD/Light Barrier @ 660 nm Demonstrator 4 Quadrant OPD Light Barrier Conveyor belt Implementation Copyright © Siemens AG 2012. All rights reserved. Page 25 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd NIR OPDs with a Small Molecule Absorber: Squaraine (SQ+PCBM = Polymer-Free BHJ) EQE 0 V -1V -2V -3V -4V -5V -6V -7V EQE [%] 80 60 40 20 0 400 600 800 1000 Wavelength [nm] -2 100 IV-characteristic Current Density [mA cm ] External quantum efficiency 10 2 10 1 10 0 -1 10 -2 10 -3 10 -4 532 nm Solar 870 nm Dark 10 -5 10 -6 10 -5 -4 -3 -2 -1 0 Voltage [V] 1 2 NIR peak sensitivity ~800 nm (tunable); low absorption in visible spectrum Dynamic response: -3 dB @ ~150 kHz (~1 cm² active area) Synthesis yield >90% (effortless up-scaling) Key advantage: Low cost absorber; no extensive polymer purification needed Copyright © Siemens AG 2012. All rights reserved. Page 26 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd sprayed Signal (20*log(U/U0)) [dB] Small Molecule Absorber Squaraine: Dynamic Response and f-3dB 0 f-3dB= 100 KHz -2 -4 OPD response f-3dB -6 doctorbladed 10 100 1k 10k 100k 1M Frequency [Hz] Reverse bias: -2V applied Copyright © Siemens AG 2012. All rights reserved. Page 27 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Application in the SWIR Range: www.omega.com Visible Application: Photography Si Bandgap QD range Pushing The Limits of OPDs with Quantum Dots NIR Imaging (0.7-2.5 µm): - Active night vision systems (NIR source) - Security applications (machine vision) - Tomography (Tissue scanning) MIR Imaging (3-5 µm): - Thermal Imaging - Passive night vision systems Copyright © Siemens AG 2012. All rights reserved. Page 28 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Hybrid Organic/Colloidal Photodiodes Photosensitive layer: Bulk heterojunction (P3HT:PCBM) with embedded PbS QD absorber Imager: 256x256 pixels with 154 µm pixel pitch Schematic layout of an a-Si active matrix TFT panel with OPDs T. Rauch et al., Near-infrared imaging with quantum dot sensitized organic photodiodes, Nature Photonics, 3, 332-336 (2009) Copyright © Siemens AG 2012. All rights reserved. Page 29 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Tunable Spectral Response with High EQE EQE of an organic photodiode sensitized with PbS-QDs of 4.6 nm diameter Peak sensitivity at 1290 nm with 18.4% EQE EQE ~ Electrons (%) Photon Tunable NIR sensitivity with increasing QD diameter Cut-off wavelength: 1350 nm to 1850 nm Copyright © Siemens AG 2012. All rights reserved. Page 30 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Current/Voltage Characteristic and Lifetime I-V characteristics High photoresponse for polychromatic light >870 nm Stable diode rectification ratio up to 8000 @ +/-2V Lifetime of more than one year! Accelerated lifetime conditions of 38°C and 90% rel. Humidity Stability for both, dark and light currents in the visibile and NIR region Copyright © Siemens AG 2012. All rights reserved. Page 31 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Energy Band Diagram QD can act as sensitizer and as traps PbS Conduction via QDs is unlikely due to long oleic acid ligands and the conductivity is orders of magnitudes lower compared to the bulkheterojunction material P3HT/PCBM No energy barrier for electron transfer between QD and PCBM; applied bias assists charge carrier transfer Staggered band alignment between P3HT and the PbS QD Almost flat band condition between the LUMO of PCBM and energy level of the PbS QD (first excitonic transition) Hole transfer might be possible from QDs to P3HT and/or to PEDOT Copyright © Siemens AG 2012. All rights reserved. Page 32 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd SWIR-Imaging Images @ 1310 nm Movies @ 1310 nm Si works only up to 1100 nm! Shadow cast of a slide (flat fielding) Original slide showing a monarch butterlfly 256x256 a-Si AM TFT panel (154 µm pixel pitch) Video shows 2 woodlice (young woodlouse on the back/adult woodlouse cleans its antennae with a foreleg) Copyright © Siemens AG 2012. All rights reserved. Page 33 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Conclusion Motivation: Replace silicon @ NIR for large active areas Solution-processable semiconductors beyond silicon bandgap limit Industrial fabrication process for OPD Spray coating Excellent statistics of IV-characteristics NIR sensors applying the dominant design of bulk heterojunctions Tunable absorber (polymer-free system) Industrial sensor prototypes (multifunctional light-barrier up to 900 nm) Low-cost imager for SWIR Quantum dots as absorber Imaging and videos >1100 nm with hybrid organic photodiode matrix Copyright © Siemens AG 2012. All rights reserved. Page 34 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Acknowledgements Dr. Oliver Hayden Sandro Tedde Tobias Rauch Regina Pflaum Dr. Joachim Wecker Prof. C. Brabec (ex-Konarka) Prof. W. Heiss (Uni Linz) Prof. Moungi Bawendi (MIT) Thank you for your attention! Copyright © Siemens AG 2012. All rights reserved. Page 35 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd Wishes and Hopes of Organic Electronics … CMOS Organic Electronics Copyright © Siemens AG 2012. All rights reserved. Page 36 May 2012 Dr. M. Sramek CT T DE HW 3/ Erlangen Süd