Fine Particle Forum August 15, 2013, A. Lloyd Spetz New approaches to airborne particle monitoring...

Fine Particle Forum August 15, 2013, A. Lloyd Spetz

New approaches to airborne

particle monitoring

A. 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-581 83 Linköping, Sweden,

2Microelectronics and Material Physics Laboratories, University of OuluFIN 900 14 Oulu, Finland

3Laboratory for Measurement Technology, Saarland University, Campus A5 1D-66123 Saarbrücken, Germany

New approaches to airborne particle monitoring

• SiC-FET improved sensor devices New design, improved functionApplications

• Monitoring of particles byImpedance spectroscopyHeating and detection of emissionsFuture technology


SiC-FET sensors, wafer and mounting

SiC-FET sensor system

4” SiC wafer, ~2000 chip

Processing on 4” SiC wafers using standard methods


SiC-FET transistor as gas sensor

I/V characteristics SiC-FET: presence of gas –

a shift in the I/V-curve

Mike Andersson


O O H HSi OSi O

H H H

SiC/Si

Si O

Three phase boundary: gas - metal - oxide

Porous film

Pt, Ir, Pd, …

Metal

Insulator

SemiconductorSiO2

Strong OH dipoles charge the gate

H2C3H6

H2OO2

CO2

NH3

Control of primary and secondary air by• 2 SiC-FET gas sensors

(different operation temperatures)• 1 temperature sensor

Increased efficiency

and lower emissions

Temperature sensor

Gas sensors

Mike Andersson

Silicon Carbide Sensors Combustion control in small power plants

http://www.nibe.se/

http://www.nibe.se/

0200040006000800010000

020406080100

0,00,51,01,52,02,5

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121620

HC emissions

Sensor @ 325oC

O2

co

nc

[%

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Sensor @ 225oC

CO emissions

Em

iss

ion

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ns

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sig

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[V

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0102030405060

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.u.]

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O2

co

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%] CO emissions

HC emissions

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pm

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Emissions from controlled combustion

Emissions, uncontrolled combustion

SenSiC AB: Silicon Carbide SensorsCombustion control in small power plants

Mike Andersson

The sensors measure the ratio between CO and oxygen in the flue gases

SenSiC AB: SiC-FET sensor system combustion control in

small and medium sized power plants

www.sensic.se

New application: Control of urea injection when using SCR by ammonia sensors in power plants and stationary diesel engines


Control of urea injection in power plants

SNCR – Selective Non-Catalytic Reduction of NO/ NO2 by NH3 through urea injection in the flue gas

SCR-Selectiv Catalytic Reduction of NO/NO2 in a catalytic converter by NH3

Control of urea injection by an NH3 sensor


Portable nanoparticle sensor• Nanoparticles show adverse health effect

according to – Size– Shape– Content– Concentration

• Nanoparticles damage cells– Toxic effect on cells

CHEMPACK project (2011-2014) FiDiPro positionUniversity 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).


IMCS 2012, A. Lloyd Spetz EuNetAir

Soot sensor based on Thermophoresis

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

Soot sensor surface

Thermos

Soot measurement in diesel engine

Exhaust pipe

Robert Bjorklund, Linköing University and Ann Grant, Volvo Technology

SPIE Baltimore, April 29 2013, A. Lloyd Spetz

Soot sensor


Soot measurements during 6 World Harmonized Transient Cycles

0,1

1

10

100

1000

0 1475 2950 4425t(min)

MW

, °C

0 100 200 300

30 min/cycle, 18 min response time, 1370 mg/cycle, 40 mg/kWh)

Robert Bjorklund and Ann Grant

Heater on, 600°C

Exhaust gas 200°C

Sensor 160°C

Particle generator

Joni HuotariPeter MöllerMike AnderssonRobert Bjorklund

• 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


Impedance spectroscopy of particles

Airborne steel plant particles

Deposited CNT particles

CNT (8.9 µg/ml) CNT (89 µg/ml)

SEM:

Optical spectra

Impedance spectra, potential for size, concentration and kind of particles and possible for on-line measurements

Joni Houtari

SEM


Detection of particle content

Flow controller 1100ml/min

Flow controller 2100ml/min

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



Christian Bur

Ammonia containing fly ashParticles heated to 430°C. Detection by SiC-FETs and

environmental mass spectrometer. Gas flow: 25ml/ min

Mass spectrometer signal

SiC-FET signal. Pt gate, T=220oC, IS-G = 55 µA


Future: Envisaged packaging ideas

One alternative co-fired LTCC modules

Maciej SoboskinskiMike Anderson

Jari Juuti

Detection of emitted gases by sensor array


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


AcknowledgementsApplied Sensor Science at

Linköping UniversityProf. Anita Lloyd SpetzDr. Mike AnderssonDr. Robert BjorklundDr. Jens Eriksson, post docZhafira Darmastuti, PhD studentChristian Bur, PhD student Hossein Fashandi, PhD studentPeter Möller, research engineer

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

Microelectronics and Material Science Laboratories, University of OuluProf. Heli JantunenProf. Jyrki LappalainenProf. Anita Lloyd SpetzAss. Prof. Jari JuutiDr Mike AnderssonJoni Huotari, PhD studentMaciej Soboskinskij, PhD student

Laboratory for Measurement Technology, Saarland UniversityProf. Andreas SchützeChristian Bur, PhD student

COST Action EuNetAir TD 1105

European Network on Air Pollution Control

Sources of emissions: e.g. industry, vehicles, volcanous and candles (soot)

Swedish Lucia performance (1963)

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


SiC-FET transducer platform for gas sensors

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

Absence of gas

Presence of gas

Cross section of depletion SiC-FETGate sensing layer: porous catalytic metal, Pt, Ir

Mike Andersson


Impedance spectra of particles from steel plant and CNTs

Steel plant particles CNT

Optical image, airborne particles from steel plant

Impedance spectra, potential for on-line measurements

SEM: CNTs deposited on IDEs

Joni Huotari


Sensor signal set to alarm level of 15-20ppm ammonia.

Detection of NH3 in low oxygen and high CO concentration functions

NH3 detection using new SiC-FET sensor design

0 5000 10000 15000 200000

1

2

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sor si

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Time [s]

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200

300

400

500U

nburn

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atte

r [p

pm

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0510152025303540

Am

monia

[ppm

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NH3 CO

Mike Andersson


Inauguration A. Lloyd Spetz 2012-09-11

Impedance spectra of particles from steel plant and CNTs

Impedance spectra for detection of concentration, size, content with potential for on-line measurements

Joni Huotari

CNTsSteel plant particles

7.0

0.02

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

From 2015: 0.4g/kW-hr for NOx, 0.02 g/kW-hr for PM


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Sensor @ 225oCSensor @ 325C

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Silicon Carbide Sensors Combustion control in small power plants

Mike Andersson

SCR, Selective Catalytic Reduction, system

4NO +4NH3 + O2 4N2 + 6H2O

2NO2 +4NH3 + O2 3N2 + 6H2O

NH2CONH2 + H2O 2 NH3 + CO2

Engine

Catalyst

NH3 NOx

Ureainjection

ControlAlgorithms

UreaTank

Enginemodel

Catalystmodel

NH3 sensor requirements:

• Operation T > 400C(700C short periods of time)

• Detection limit <10 ppm

SCR now in trucks by both Volvo and Scania

OBD (On Board Diagnostics) expected

NH3 Lab measurements

4

4.1

4.2

4.3

4020 10 5 ppm

Vol

t

4

4.1

4.2

4.3

4020 10 5 ppm

Vol

t

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4.2

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4020 10 5 ppm

Vol

t

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4.1

4.2

4.3

4020 10 5 ppm

Vol

t

0 20 40 Tid (min) 60 80

SiC-FET sensor signal to ammonia for two SiC FETs. Detection limit < 5 ppm in 10% O2 / N2.

Mike Andersson


Particles spread by volcanos

The eruption plume of St. Helen volcano, in 1980 courtesy of NASA.

Volcanic iron oxide rich soil in Rwanda(courtesy Biomed Central.)

Podoconiosis

Aggressive African-endemic Kaposi’s

sarcoma of the foot

Buzea et al. Biointerphases, 2, 4 (2007) MR17-MR71


The SiC-FET ammonia sensor

Diesel engine measurement

SCR system Two MISiCFET

sensors and optical reference instrument

H. Svenningstorp, H. Wingbrant


31

Nano-ID™ NPS500 based on DMA (Differential Mobility Analyzer) technology, portable particle measurement device (5-500nm)

Present commercial particle detectors

DEKATI ELPI (Electrical Low Pressure Impactor (6 nm – 10 µm)


NH3 sensor mounting for urea control in boilers

Värmeforsk projects:A08-828 and P08-823Partners: SenSiC AB, Alstom Sweden AB, Tekniska Verken, Vattenfall

Two position sensor mounting ~ 40 cm apart

Robert Bjorklund


Gobi desert dust storm spread

Ten major sources of dust in the world

Bacteria, hitch hiking by African dust, was found in North America.

Hitchhiker in Luxemburg, 1977



Healthy particles

Sea spray from ocean waves (courtesy NASA).

Pale blue swirls in Lake Michigan, probably caused bycalcium carbonate chalk from the lake’s limestone floor (credit: NASA/GSFC)

TEM image of mineral dust mixture with sea salt collected from the marine troposphere



Fires produce (nano)particles

Distribution of active fires detected by Terra’s MODIS sensor across the planet on 10-19 July 2006



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.


Workplace and Indoor Aerosol conference in Lund:

Detection of Pd in particles by the catalytic CO conversion efficiency Christian Bur


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

PCB

MEMS

DIE

PARTLY TRANSPARENT SEALING

Piezoelectric layerfor sensing

50 TRANSMISSION LINE

{

THERMAL VIASAND GROUND

CAPACITOR

COUPLER

GRDSIGPOWGRDSIGSIGSIGGRDPOW

MICROWAVEFILTER

Ferroelectric layerfor electrical tuning

Ferromagnetic layerfor radiation protectionor electrical shortening

RESISTOR Deposited layers

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


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.


Tailoring of SiC based field effect sensors for O2 monitoring

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.

No response to hydrogen containing gases

Response to oxygen


Sensor system for control of small and medium sized power plants

www.sensic.se

Mike Andersson and Magnus Palm: installation of a sensor system for control of a domestic boiler) at Ariterm Sweden AB (key partner)


• NANOSIGHT- optical method to measure size- laser light source - typical range 10 nm - 1000 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

NANOSIGHT LM10KANOMAX MODEL 3800

AIRMODUS

LIGHTHOUSE HANDHELD 2016

42

Present commercial particle detectors


Envisaged packaging ideas

Material combinations and process development to enable wafer level integration of functional packages by cost effective means.


Fine Particle Forum August 15, 2013, A. Lloyd Spetz New approaches to airborne particle monitoring...

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