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New approaches to airborne particle monitoring

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1 New approaches to airborne particle monitoring
Lloyd Spetz,1,2 J. Huotari2, C. Bur1,3, M. Sobocinski2 R. Bjorklund1, J. Juuti2, J. Lappalainen2, H. Jantunen2, A. Schütze3, M. Andersson1 1Div Applied Sensor Science, Dept. Physics, Chemistry and Biology, Linköping University, SE Linköping, Sweden, 2Microelectronics and Material Physics Laboratories, University of Oulu FIN Oulu, Finland 3Laboratory for Measurement Technology, Saarland University, Campus A5 1 D Saarbrücken, Germany Fine Particle Forum August 15, 2013, A. Lloyd Spetz

2 New approaches to airborne particle monitoring
SiC-FET improved sensor devices New design, improved function Applications Monitoring of particles by Impedance spectroscopy Heating and detection of emissions Future technology Fine Particle Forum August 15, 2013, A. Lloyd Spetz

3 SiC-FET sensors, wafer and mounting
sensor system 4” SiC wafer, ~2000 chip Processing on 4” SiC wafers using standard methods Fine Particle Forum August 15, 2013, A. Lloyd Spetz

4 SiC-FET transistor as gas sensor
Strong OH dipoles charge the gate Three phase boundary: gas - metal - oxide H2 C3H6 H2O O2 CO2 NH3 O O H H Metal Insulator Semiconductor H H H Si O Si O Si O Porous film Pt, Ir, Pd, … SiO2 SiC/Si I/V characteristics SiC-FET: presence of gas – a shift in the I/V-curve Mike Andersson Fine Particle Forum August 15, 2013, A. Lloyd Spetz

5 Silicon Carbide Sensors Combustion control in small power plants
Gas sensors Control of primary and secondary air by 2 SiC-FET gas sensors (different operation temperatures) 1 temperature sensor Increased efficiency and lower emissions                    In a project with NIBE industry, one temperature sensor and one or two SiC-FET sensors are used to control the combustion in the boiler (villavärmepanna) and reduce the emissions. The intake of primary and secondary air is controlled. Mike Andersson Temperature sensor

6 SenSiC AB: Silicon Carbide Sensors Combustion control in small power plants
Emissions, uncontrolled combustion Emissions from controlled combustion The sensors measure the ratio between CO and oxygen in the flue gases Mike Andersson

7 Fine Particle Forum August 15, 2013, A. Lloyd Spetz
SenSiC AB: SiC-FET sensor system combustion control in small and medium sized power plants New application: Control of urea injection when using SCR by ammonia sensors in power plants and stationary diesel engines Fine Particle Forum August 15, 2013, A. Lloyd Spetz

8 Control of urea injection in power plants
SNCR – Selective Non-Catalytic Reduction of NO/ NO2 by NH3 through urea injection in the flue gas Control of urea injection by an NH3 sensor SCR-Selectiv Catalytic Reduction of NO/NO2 in a catalytic converter by NH3 Fine Particle Forum August 15, 2013, A. Lloyd Spetz

9 Portable nanoparticle sensor
Nanoparticles show adverse health effect according to Size Shape Content Concentration Nanoparticles damage cells Toxic effect on cells CHEMPACK project ( ) FiDiPro position University of Oulu i Finland Welding nanoparticles (courtesy of Pam Drake, National Institute for Occupational Safety and Health NIOSH). Asbestos fibers (courtesy of the US Geological Survey). Fine Particle Forum August 15, 2013, A. Lloyd Spetz

10 Soot sensor based on Thermophoresis
Soot sensor surface Thermos Thermophoresis: A force acting on particles in a temperature gradient → Soot is deposited on the coldest surface Thermos packaging to decrease temperature on the sensor surface IMCS 2012, A. Lloyd Spetz EuNetAir

11 Soot measurement in diesel engine
Exhaust pipe Soot sensor Robert Bjorklund, Linköing University and Ann Grant, Volvo Technology SPIE Baltimore, April , A. Lloyd Spetz

12 Soot measurements during 6 World Harmonized Transient Cycles
Heater on, 600°C t(min) MW, °C Exhaust gas 200°C Sensor 160°C 30 min/cycle, 18 min response time, 1370 mg/cycle, 40 mg/kWh) Robert Bjorklund and Ann Grant IMCS 2012, A. Lloyd Spetz EuNetAir

13 Fine Particle Forum August 15, 2013, A. Lloyd Spetz
Particle generator PALAS RGB 1000 dry particle generator Pegasor nanoparticle sensor as reference Flow through chamber for testing of sensors (SiC-FETs) A measurement chamber with probe connections will be built for measurements from DC to GHz range Joni Huotari Peter Möller Mike Andersson Robert Bjorklund Fine Particle Forum August 15, 2013, A. Lloyd Spetz

14 Impedance spectroscopy of particles
Airborne steel plant particles Optical spectra Deposited CNT particles SEM SEM: CNT (8.9 µg/ml) CNT (89 µg/ml) Joni Houtari Impedance spectra, potential for size, concentration and kind of particles and possible for on-line measurements Fine Particle Forum August 15, 2013, A. Lloyd Spetz

15 SiC- FET sensor Detection of particle content
Flow controller 1 100ml/min Flow controller 2 Heater with particles Sensor chamber Electronics Data acquisition LabView Gas mixing program T-control Const. I control N2 O2 Waste Heating of particles and detection of emissions with gas sensors Christian Bur Fine Particle Forum August 15, 2013, A. Lloyd Spetz SiC- FET sensor

16 Detection of particle content
Mass spectrometer signal SiC-FET signal. Pt gate, T=220oC, IS-G = 55 µA Ammonia containing fly ash Particles heated to 430°C. Detection by SiC-FETs and environmental mass spectrometer. Gas flow: 25ml/ min Christian Bur Fine Particle Forum August 15, 2013, A. Lloyd Spetz

17 Future: Envisaged packaging ideas
Detection of emitted gases by sensor array Maciej Soboskinski Mike Anderson Jari Juuti One alternative co-fired LTCC modules Fine Particle Forum August 15, 2013, A. Lloyd Spetz

18 SPIE Baltimore, April 29 2013, A. Lloyd Spetz
Conclusions Toxic gases and airborne nanoparticles need to be monitored for environmental control The new generation SiC-FETs provide a powerful sensor platform for detection of gases (and eventually particles) The content of nanoparticles is important to measure: Impedance spectroscopy or heating particles and subsequent detection of the emissions by gas sensors SPIE Baltimore, April , A. Lloyd Spetz

19 Acknowledgements Applied Sensor Science at Linköping University
Prof. Anita Lloyd Spetz Dr. Mike Andersson Dr. Robert Bjorklund Dr. Jens Eriksson, post doc Zhafira Darmastuti, PhD student Christian Bur, PhD student Hossein Fashandi, PhD student Peter Möller, research engineer Microelectronics and Material Science Laboratories, University of Oulu Prof. Heli Jantunen Prof. Jyrki Lappalainen Prof. Anita Lloyd Spetz Ass. Prof. Jari Juuti Dr Mike Andersson Joni Huotari, PhD student Maciej Soboskinskij, PhD student Laboratory for Measurement Technology, Saarland University Prof. Andreas Schütze Christian Bur, PhD student Grant support is acknowledged from: The VINN Excellence Center in Research & Innovation on Functional Nanostructured Materials (FunMat) The Swedish Agency for Innovation Systems (VINNOVA), The Swedish Research Council and TEKES in Finland COST Action EuNetAir TD 1105 European Network on Air Pollution Control

20 Clean environment through air quality control by sensor systems
A clean environment should belong to human rights. Sensor systems are needed for emission monitoring and control. Toxic substances include: NOx, SO2, CO, O3, PAH, PM10, PM2.5, PM1 The vulcano St. Helena Swedish Lucia performance (1963) Sources of emissions: e.g. industry, vehicles, volcanous and candles (soot) Fine Particle Forum August 15, 2013, A. Lloyd Spetz

21 SiC-FET transducer platform for gas sensors
Presence of gas Absence of gas Cross section of depletion SiC-FET Gate sensing layer: porous catalytic metal, Pt, Ir I/V characteristics SiC-FET: presence (red dashed line) of a gas - internal voltage drop at the gate metal/ insulator interface – a shift in the I/V-curve Mike Andersson Fine Particle Forum August 15, 2013, A. Lloyd Spetz

22 Impedance spectra of particles from steel plant and CNTs
Impedance spectra, potential for on-line measurements CNT Steel plant particles SEM: CNTs deposited on IDEs Joni Huotari Optical image, airborne particles from steel plant SPIE Baltimore, April , A. Lloyd Spetz

23 NH3 detection using new SiC-FET sensor design
CO Sensor signal set to alarm level of ppm ammonia. Detection of NH3 in low oxygen and high CO concentration functions Mike Andersson Fine Particle Forum August 15, 2013, A. Lloyd Spetz

24 Impedance spectra of particles from steel plant and CNTs
Steel plant particles Joni Huotari Impedance spectra for detection of concentration, size, content with potential for on-line measurements Inauguration A. Lloyd Spetz

25 Market legislations for heavy duty trucks
On Road US On Road EU On Road Japan 2.0 3.5 5.0 0.15 0.10 NOx (g/kWh) PM (g/kWh) 0.05 US’04 US’10 US’07 EU-II 95/96 EU-III 00/01 EU-VI 13/14 ~ Japan NLT 05 EU-V 08/09 EU-IV 05/06 0.02 7.0 From 2015: 0.4g/kW-hr for NOx, 0.02 g/kW-hr for PM Fine Particle Forum August 15, 2013, A. Lloyd Spetz

26 Silicon Carbide Sensors Combustion control in small power plants
Mike Andersson

27 SCR, Selective Catalytic Reduction, system
4NO +4NH3 + O2 4N2 + 6H2O 2NO2 +4NH3 + O2 3N2 + 6H2O NH2CONH2 + H2O  2 NH3 + CO2 Engine Catalyst NH 3 NOx Urea injection Control Algorithms Tank model NH3 sensor requirements: Operation T > 400C (700C short periods of time) Detection limit <10 ppm In the SCR system urea, (NH2)2CO, is injected in the exhausts system and reacts with H2O and forms two NH3 molecules and CO2 at elevated temperature. NH3 reacts with nitrogen oxides e.g. according to the reactions in the Figure and harmless N2 and H2O is formed. This is a very efficient way to reduce the nitrogen oxides in diesel exhausts but also in e.g. flue gases (rök gaser). The SCR process may be controlled by eíther a NOx sensor or an NH3 sensor. The NOx sensor which will be used for this control was described in the MOS lecture. SCR now in trucks by both Volvo and Scania OBD (On Board Diagnostics) expected

28 Fine Particle Forum August 15, 2013, A. Lloyd Spetz
NH3 Lab measurements Mike Andersson SiC-FET sensor signal to ammonia for two SiC FETs. Detection limit < 5 ppm in 10% O2 / N2. Fine Particle Forum August 15, 2013, A. Lloyd Spetz

29 Particles spread by volcanos
The eruption plume of St. Helen volcano, in 1980 courtesy of NASA. Aggressive African-endemic Kaposi’s sarcoma of the foot Podoconiosis Volcanic iron oxide rich soil in Rwanda (courtesy Biomed Central.) Buzea et al. Biointerphases, 2, 4 (2007) MR17-MR71 SPIE Baltimore, April , A. Lloyd Spetz

30 The SiC-FET ammonia sensor
Diesel engine measurement SCR system Two MISiCFET sensors and optical reference instrument According to the gas response characteristics of the SiC-FET sensor in Figur 15, a sensing layer of Ir operated at 300C is chosen as an ammonia sensor to control the SCR. This picture shows two SiC-FET sensors that are mounted in the exhaust system of a diesel engine, which is equipped with a SCR system. An optical reference system shows the ammonia concentration. The sensors give a good response for only 10 ppm of ammonia. This was the requirement from industry, that is, for this application concept is proven. H. Svenningstorp, H. Wingbrant Fine Particle Forum August 15, 2013, A. Lloyd Spetz

31 Present commercial particle detectors
31 Present commercial particle detectors DEKATI ELPI (Electrical Low Pressure Impactor (6 nm – 10 µm) Nano-ID™ NPS500 based on DMA (Differential Mobility Analyzer) technology, portable particle measurement device (5-500nm) Fine Particle Forum August 15, 2013, A. Lloyd Spetz 31

32 NH3 sensor mounting for urea control in boilers
Värmeforsk projects: A and P08-823 Partners: SenSiC AB, Alstom Sweden AB, Tekniska Verken, Vattenfall Two position sensor mounting ~ 40 cm apart Robert Bjorklund Fine Particle Forum August 15, 2013, A. Lloyd Spetz

33 Gobi desert dust storm spread
Buzea et al. Biointerphases, 2, 4 (2007) MR17-MR71 Ten major sources of dust in the world Hitchhiker in Luxemburg, 1977 Bacteria, hitch hiking by African dust, was found in North America. SPIE Baltimore, April , A. Lloyd Spetz

34 SPIE Baltimore, April 29 2013, A. Lloyd Spetz
Healthy particles Pale blue swirls in Lake Michigan, probably caused by calcium carbonate chalk from the lake’s limestone floor (credit: NASA/GSFC) Sea spray from ocean waves (courtesy NASA). TEM image of mineral dust mixture with sea salt collected from the marine troposphere Buzea et al. Biointerphases, 2, 4 (2007) MR17-MR71 SPIE Baltimore, April , A. Lloyd Spetz

35 Fires produce (nano)particles
Distribution of active fires detected by Terra’s MODIS sensor across the planet on July 2006 Buzea et al. Biointerphases, 2, 4 (2007) MR17-MR71 SPIE Baltimore, April , A. Lloyd Spetz

36 Detection of particle content
Workplace and Indoor Aerosol conference in Lund: Detection of Pd in particles by the catalytic CO conversion efficiency Christian Bur First results, detection of ammonia containing fly ash particles. Particles are heated repeatedly to ~ 800°C. A small gas flow brings emissions from heater to SiC-FET sensors. SPIE Baltimore, April , A. Lloyd Spetz

37 IMCS 2012, A. Lloyd Spetz EuNetAir

38 SPIE Baltimore, April 29 2013, A. Lloyd Spetz
Future development Particles are charged, SiC- FET device a possibility Source and drain contacts need protection by over glass, but also bond wires must be protected Additional functionality by smart packaging, LTCC packaging (Docent Jari Juuti): Collection of particles by thermophoresis (cold sensor surface), applied voltage, magnetic field Detection of content of particles by heating at a hot spot and detection of emissions by a sensor array, smart operation and data evaluation SPIE Baltimore, April , A. Lloyd Spetz

39 Tailoring of SiC based field effect sensors for CO2 monitoring
SiC based CO2 sensor Li2CO3-BaCO3 sensing layer MgO prevents response to hydrogen containing gases H. Inoue, M. Andersson, M. Yuasa, T. Kida, A. Lloyd Spetz, and K. Shimanoe: CO2 sensor combining an MISiC capacitor and a binary carbonate, Electrochemical and Solid-State Letters, 14 (1) (2011) J4-J7. SPIE Baltimore, April , A. Lloyd Spetz

40 Tailoring of SiC based field effect sensors for O2 monitoring
Response to oxygen No response to hydrogen containing gases M. Andersson, A. Lloyd Spetz, Tailoring of SiC based field effect gas sensors for improved selectivity to non-hydrogen containing species, IMCS13, Perth, Australia, July 12-14, 2010, 369. SPIE Baltimore, April , A. Lloyd Spetz

41 Sensor system for control of small and medium sized power plants
Mike Andersson and Magnus Palm: installation of a sensor system for control of a domestic boiler) at Ariterm Sweden AB (key partner) SPIE Baltimore, April , A. Lloyd Spetz

42 Present commercial particle detectors
42 Present commercial particle detectors NANOSIGHT - optical method to measure size laser light source typical range 10 nm nm BECKMAN COULTER particle size of fluid with nanoparticles laser light - for size analysis: electrophoretic light scattering (ELS) LIGHTHOUSE WORLDWIDE SOLUTIONS - handheld and portable particle counters - minimum sensitivity: 200 nm AIRMODUS - condensation to grow 1 nm diameter nanoparticles to optically detectable sizes KANOMAX condensation to grow 15 nm diameter nanoparticles to optically detectable sizes PEGASOR Portable real time measuring instrument Detection of total surface area, mass, number of particles BECKMAN COULTER AIRMODUS NANOSIGHT LM10 KANOMAX MODEL 3800 LIGHTHOUSE HANDHELD 2016 SPIE Baltimore, April , A. Lloyd Spetz 42

43 Envisaged packaging ideas
Material combinations and process development to enable wafer level integration of functional packages by cost effective means. SPIE Baltimore, April , A. Lloyd Spetz


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