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MÁRIO RICARDO GÓNGORA MÁRIO RICARDO GÓNGORA - - RUBIO, RUBIO, Instituto de Pesquisas Tecnológicas do Estado de São Paulo Instituto de Pesquisas Tecnológicas do Estado de São Paulo IPT, SÃO PAULO, BRAZIL IPT, SÃO PAULO, BRAZIL

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Page 1: MÁRIO RICARDO GÓNGORA-RUBIO, Instituto de Pesquisas ... · MÁRIO RICARDO GÓNGORA-RUBIO, Instituto de Pesquisas Tecnológicas do Estado de São Paulo . IPT, SÃO PAULO, BRAZIL

MÁRIO RICARDO GÓNGORAMÁRIO RICARDO GÓNGORA--RUBIO,RUBIO,Instituto de Pesquisas Tecnológicas do Estado de São Paulo Instituto de Pesquisas Tecnológicas do Estado de São Paulo

IPT, SÃO PAULO, BRAZILIPT, SÃO PAULO, BRAZIL

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THIS IS A COLLABORATIVE EFFORT WITHTHIS IS A COLLABORATIVE EFFORT WITH

•• UNIVERSITY OF SÃO PAULOUNIVERSITY OF SÃO PAULO--LSILSI--DMIDMI

•• AUTONOMOUS UNIVERSITY OF BARCELONA AUTONOMOUS UNIVERSITY OF BARCELONA – SENSORS AND BIOSENSORS GROUP

•• UNIVERSITY OF PENNSYLVANIAUNIVERSITY OF PENNSYLVANIA

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PRESENTATION OUTLINE PRESENTATION OUTLINE

1.1. Introduction to LTCC TechnologyIntroduction to LTCC Technology2.2. LTCC ProcessingLTCC Processing3.3. Modular System Interfaces Modular System Interfaces 4.4. LTCC Devices for MEMS/MSTLTCC Devices for MEMS/MST5.5. Meso Systems ApplicationsMeso Systems Applications6. Conclusions6. Conclusions

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WHAT IS LTCC ?WHAT IS LTCC ?–LTCC was originally developed by Hughes and DuPont for Military Systems.

– The (LTCC) technology can be defined as a way to produce multilayer circuits with the help of single tapes, which are to be used to apply conductive, dielectric and / or resistive pastes on.

–These single sheets have to be laminated together and fired in one step all.

Multi Chip Module Bluetooth Interface (National)

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CERAMIC INTERCONNECT TECHNOLOGYCERAMIC INTERCONNECT TECHNOLOGYSource: Green Tape Application Group

PI-LTCC

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TECHNOLOGY VISIONTECHNOLOGY VISION

Meso Meso

SystemSystem

ModuleModule

ActuatorMicro

Fluidics

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2.2. LTCC PROCESSINGLTCC PROCESSING

–– MaterialsMaterials––Processing stepsProcessing steps––LaminationLamination–– SinteringSintering––Tape MachiningTape Machining

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LOW TEMPERATURE COLOW TEMPERATURE CO--FIRED CERAMICS (LTCC)FIRED CERAMICS (LTCC)

• Glass-ceramic composite materials

• The ceramic filler is usually alumina, Al2O3

• The usual composition also includes a glass frit and an organic binder (plasticizerand anti-flocculant)

• Called green tape before firing and sintering

LTCC-951 Composition

40%

45%

15%

Alumina

Glasses (Silicates)

Other Organics

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LTCC PROCESSING SCHEDULE LTCC PROCESSING SCHEDULE

Source:Thales Microsonics

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LTCC MANUFACTURING PROCESS (1)LTCC MANUFACTURING PROCESS (1)•• Materials PreparationMaterials Preparation

–LTCC Ceramic tape materials are prepared by milling precise amounts of raw materials into a homogeneous slurry.

–This mixture is principally of ceramic/glass powders with controlled particle sizes with fluxes and small amounts of organic binders and solvents.

–This slurry is poured onto a carrier and then passed under a blade to produce a uniform strip of specific thickness.

–When dried, this strip becomes a ceramic-filled “Green ceramic tape” which is easily handled in rolls or sheets for unfired processing.

Ceramic Slurry

Doctor BladeHot Air

Mylar coil Green Ceramic coil

Base

Coil Movement System

DuPont

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LTCC MANUFACTURING PROCESS (2)LTCC MANUFACTURING PROCESS (2)•• Tape PreparationTape Preparation

–Cutting tape –Pre-Conditioning in the furnace –Punching or burning registration holes –Removing Mylar-tape

•• BlankingBlanking–A blanking die is used to create orientation marks and the final working dimension of the green sheets.

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LTCC MANUFACTURING PROCESS (3)LTCC MANUFACTURING PROCESS (3)

•• Via FillingVia Filling–Performed using an thick film screen printer with a stencil metal mask.

–Registration is performed using a vision system.

•• Via MachiningVia Machining–Using high-speed mechanical punching with a matrix tool, Laser System, CNC or JVE.

Via HoleMetal

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MECHANICAL MACHINING OF CERAMIC TAPESMECHANICAL MACHINING OF CERAMIC TAPES

PUNCHINGPUNCHINGCircular or square shapeSmallest size 0.004”(~100microns)Machining of curved features is difficultPartial depth machining cannot be done

CNC MILLINGCNC MILLINGSmallest size (~150 microns)Machining of curved features is easy Partial depth penetration facilitating shallow channels and thin membranesVacuum chuck holder or wet tape is used to fix tape

Punched curve

MilledPunched

CNC milling

Machined SamplesMachined Samples

CNC milled curve

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LTCC HOT EMBOSSINGLTCC HOT EMBOSSING•• Small features can be transferred to LTCC layers using Hot Small features can be transferred to LTCC layers using Hot

Embossing TechniqueEmbossing Technique•• Several Molds for complex structures have been constructedSeveral Molds for complex structures have been constructed•• Development of the technique is on goingDevelopment of the technique is on going

Hot Embossing Mold for Pre-Concentrator

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LTCC MANUFACTURING PROCESS (4)LTCC MANUFACTURING PROCESS (4)

•• Paste PrintingPaste Printing–Resistor, conductor and dielectrics deposits are performed using an automatic thick film screen printer with mesh screens.

•• CollatingCollating–All layers will be collated and stacked with a special tool and will be fixed together to avoid misalignment.

–Can be performed using a vision system for alignment.

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LTCC MANUFACTURING PROCESS (5)LTCC MANUFACTURING PROCESS (5)

•• LaminatingLaminating–Accomplished using uniaxial or isostatic lamination in a specially designed thermal press

–Temperature for lamination 100 oC–Laminating pressure is 3000 PSI –Typical cycle time is 10 minutes.

•• PrePre--CuttingCutting–Laminates are pre-cut with a hot blade, meeting the panel drawing specifications.

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LAMINATION PROCESSLAMINATION PROCESSThermocompressionThermocompression Cold Low Pressure Cold Low Pressure

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LTCC MANUFACTURING PROCESS (6)LTCC MANUFACTURING PROCESS (6)glass

Alumina

glass

Alumina

Sintering Model•• CoCo--FiringFiring–Made in a belt or special furnace at a peak temperature of 850°C and a dwell time of 30 minutes.

–The typical cycle time is 3 hours.

Sintering Furnace

850

350

Temperature (oC)

Time (min)

45 min

30 min

Ramp = 10oC/min

LTCC Temperature profile

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LTCC MANUFACTURING PROCESS (7)LTCC MANUFACTURING PROCESS (7)•• Dimensional Measurements Dimensional Measurements

/Electrical Test:/Electrical Test:–Panel and circuit size can be checked with automatic measurement vision system. Electrical resistance test is performed with an automatic system with probe card.

•• Final Inspection:Final Inspection:–Optical, Laser and acoustic inspection techniques are performed on completed parts in accordance with the applicable standards.

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PROCESSING DIFFICULTIES IN MST APPLICATIONS: PROCESSING DIFFICULTIES IN MST APPLICATIONS: LAMINATIONSLAMINATIONS

An often encountered problem in MST applications is the lamination at low uniaxial or hydrostatic pressures, as to avoid the collapse of internal voids, channels and cavities in the green. Several possibilities are available, the two that we have pursued in recent times are: cold low pressure lamination (Erlanger’s CLPL method) and Lamination using organic fluids.

Cavity deformation after thermo-compression lamination

Three layer lamination using organics

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PROCESSING DIFFICULTIES IN MST APPLICATIONS : PROCESSING DIFFICULTIES IN MST APPLICATIONS : LAMINATIONLAMINATION

High viscosity polysaccarides (sugars) used as laminating vehicles for LTCC tapes

Thermo-gravimetric studies of the different laminating vehicles “burn-off” compared to a typical 951 series LTCC tapes sintering cycle.

Ceramic Green Tape

Lamination

Sintering

Organic Fluid Deposition

Ceramic Green Tape

Lamination

Sintering

Organic Fluid Deposition

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PROCESSING DIFFICULTIES IN MST APPLICATIONS: PROCESSING DIFFICULTIES IN MST APPLICATIONS: LAMINATIONLAMINATION

••AdvantagesAdvantages ofof lamination using organic fluidslamination using organic fluids ::–Excellent gluing function and easy tapes alignment in room temperature due to their high viscosity;–Low pressure and temperature process;–No pressure gradients in laminate;–Easy method of deposition, allowing lamination of complex shapes and non-uniform surfaces;–Sintering temperature profile with high heating rate compared with CLPL method;–Organic fluid deposition can be realized by dipping, screen printing or dispensing techniques;–-Inexpensive and readily available.

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PROCESSING DIFFICULTIES IN MST APPLICATIONS : PROCESSING DIFFICULTIES IN MST APPLICATIONS : SAGGINGSAGGING

The sagging, or the collapsing of the top and bottom (mostly top, due to body forces)of internal voids or channels in LTCC tapes is a common problem for MST and Microfluidic applications.

The inexpensive solution is to mix graphite or carbon black powder with an organic vehicle of high viscosity. This mixture is easy oxidized during the sintering cycle ( a fugitive or sacrificial phase).

Here is a SEM micrograph of the same size channel sintered with and without the fugitive phase.

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PROCESSING DIFFICULTIES IN MST APPLICATIONS: PROCESSING DIFFICULTIES IN MST APPLICATIONS: CONSTRAINT LAMINATIONCONSTRAINT LAMINATION

•• Before firing the green tapes are laminated to a rigid substrateBefore firing the green tapes are laminated to a rigid substrate..zz--shrinkage must be considered during the device design.shrinkage must be considered during the device design.

0%5%

10%15%20%25%30%35%40%45%50%

0 1 2 3 4 5

Layer #

z Sh

rinka

ge %

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LTCC STRUCTURES FOR MICROFILTERINGLTCC STRUCTURES FOR MICROFILTERING

•• NeedNeed to to integrate integrate a a Microfiltering stage into Microfiltering stage into LTCC MicrofluidicLTCC Microfluidicsystemsystem

•• Possibility Possibility of of create create structures structures for for CatalyticCatalyticmaterial material deposition deposition for for Fuel CellsFuel Cells

•• Possibility Possibility of of creating creating high area high area for for biological biological seedsseeds.

LTCC

LTCC

LTCC

Ceramic Porous Membranes

.

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POROUS LTCC POROUS LTCC

200 µm

150 µm

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3. MODULAR SYSTEM INTERFACES3. MODULAR SYSTEM INTERFACES

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MODULAR SYSTEM INTERFACES MODULAR SYSTEM INTERFACES Source: Fraunhofer Institute

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LTCCLTCC--TBTB--BGA (TOPBGA (TOP--BOTTOMBOTTOM-- BGA)BGA)

Source: Fraunhofer Institute

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ASSEMBLY OF A LTCC CARRIERASSEMBLY OF A LTCC CARRIER

Source: Fraunhofer Institute

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OPTICAL & FLUIDIC INTERFACESOPTICAL & FLUIDIC INTERFACES

Source: Fraunhofer Institute

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SOME 3D LTCC MODULES SOME 3D LTCC MODULES •• 16 Bits 16 Bits Microcontroller FlowMicrocontroller Flow SensorSensor

Source: Fraunhofer Institute

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4. LTCC DEVICES FOR 4. LTCC DEVICES FOR MEMS/MSTMEMS/MST

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MANUFACTURING OF MESO SCALE SYSTEMS MANUFACTURING OF MESO SCALE SYSTEMS USING LTCC USING LTCC

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SENSORS USING GREEN CERAMIC TAPESSENSORS USING GREEN CERAMIC TAPES•• Basic MicroBasic Micro--Fluidic DevicesFluidic Devices

– Micro-channels– Critical orifices – Micromixers– Hot Plates – Micropumps

•• Thermal Flow Sensor Thermal Flow Sensor – Flow sensor using thermal loss

measurement

•• Chemical SensorsChemical Sensors– SNO2 Gas Sensor– PH Sensor– Electrochemical Electrodes

•• Displacement and attitude Displacement and attitude sensorssensors– LVDT type displacement

sensor– Attitude sensor using

ferrofluids– Eddy current proximity

sensor

•• Pressure SensorsPressure Sensors– Load Cells – Differential pressure sensors – High temperature pressure

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PRESSURE SENSORSPRESSURE SENSORS•• Pressure sensors Pressure sensors for for applicationsapplications, , like like media media isolated isolated

devicesdevices,, were developed using were developed using LTCC LTCC technologytechnology

Technical University of Darmstadt

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CONDUCTIVITY SENSORSCONDUCTIVITY SENSORS

INTERDIGITAL ELECTRODES FABRICATED DEVICES

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THERMAL FLOW SENSOR WITH LTCCTHERMAL FLOW SENSOR WITH LTCC

•• Thermal methods display some advantages for Thermal methods display some advantages for implementing flow sensors as:implementing flow sensors as:

–Thermal isolation between structure and support;–Low thermal capacity improving response times;–Small dimension devices;–Integration in a micro-system or MEMS scheme.

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LTCC FLOW SENSORSLTCC FLOW SENSORS

A-A

Layer

Layer 2 Layer 3

Layer 4 Layer 5 Cross-section A-A

L1

L2

L3

L4

L5

Layer 1

Fabricated Device

0 1 2 3 420

25

30

35

40

45

50

Dissipation factor Vs. Flow velocity k = 18,79 + 31,03 * e(-vf / 1,66) for exponential regression

Diss

ipat

ion

Fact

or (W

att/K

elvin

)

Flow Velocity (SLM)

Experimental Set-Up

Device Lay-out

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Oxygen SensorsOxygen Sensors•• The dissolved oxygenThe dissolved oxygen (DO) (DO)

sensor issensor is oneone ofof the most the most important sensorsimportant sensors forforenvironmental monitoringenvironmental monitoring..

•• A ClarkA Clark--typetype DO sensorDO sensorusing using (LTCC)(LTCC) targetedtargeted forforcontinuous monitoring continuous monitoring applicationsapplications waswas implementedimplemented..

0 20 40 60 80 1000

100

200

300

400

500

-I(nA

)

dissolved oxygen (%)

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HotHot--LayerLayer--ElectrochemistryElectrochemistry sensor sensor usingusing LTCCLTCC•• Chemical applicationChemical application to determine to determine temperature coefficientstemperature coefficients of of

redoxredox--couplescouples•• SampledSampled linearlinear sweepsweep curves for 5 mM K4[curves for 5 mM K4[FeFe(CN)6] in 0.1 M (CN)6] in 0.1 M

NaSONaSO44 atat different Temperaturesdifferent Temperatures

Technical University of Ilmenau

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ACTUATORS WITH LTCCACTUATORS WITH LTCC

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HOT PLATESHOT PLATES•• With few layers it is possible With few layers it is possible

to get a simple hot plate. •• Surface heating VsSurface heating Vs. . currentcurrent in in

hot hot plateplateto get a simple hot plate.

-15 -10 -5 0 5 10 1520

30

40

50

60

70

80

90

100

110

120

130

140Temperatura na superficieda bobina para diversas correntes de excitação

50mA 100mA 150mA

Tem

pera

tura

na

supe

rfici

e (C

)

Distância do centro da Bobina (mm)

Layer1

Layer2

Layer 3

Layer 4

Layer 5

Base

Layer 6

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•• High current coils can be High current coils can be fabricatedfabricated in LTCC in LTCC usingusing a CNCa CNC low relief low relief techniquetechnique

Test Structure Test Structure CNC CNC Machined Coil Printed and Fired coilMachined Coil Printed and Fired coil

Screen printing in a low relief structure

POWER LTCC COILSPOWER LTCC COILS

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SOME RESULTSSOME RESULTS

•• Coil depth can be defined between 50 to 150 Coil depth can be defined between 50 to 150 µµm, with 150 m, with 150 µµm m pitch, coils can be done with 5 to 20 number of turns per layer pitch, coils can be done with 5 to 20 number of turns per layer and and working layers are: 1 to 6.working layers are: 1 to 6.

•• We have found coil layer resistance ranging from 0,1 to 0,4 We have found coil layer resistance ranging from 0,1 to 0,4 ΩΩ. .

BOBINA 6 (1 camada)

0.0 G

5.0 G

10.0 G

15.0 G

20.0 G

25.0 G

30.0 G

35.0 G

40.0 G

0 mA 200 mA 400 mA 600 mA 800 mA 1000 mA 1200 mA 1400 mA

h=0 mm

h=1 mm

h=2 mm

h=3 mm

h=4 mm

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LIQUID COOLING SYSTEMSLIQUID COOLING SYSTEMS

•• Thermal management is an Thermal management is an important problem in important problem in electronic packaging.electronic packaging.

•• LTCC thermal LTCC thermal viasvias and and microchannels microchannels can deliver can deliver liquid cooling systems with liquid cooling systems with thermal dissipation of up to thermal dissipation of up to 50 W/cm50 W/cm2

Technical University of Dresden

2

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-150 -100 -50 0 50 100 150-250

-200

-150

-100

-50

0

50

100

150

200

250Deslocamento do diaf ragma Vs corrente no atuadorpara v arias distâncias imã-bobina

2mm 2.25mm 2.5mm

Corre

nte no

atua

dor (

mA)

Deslocamento da membrana ( µ m)Coil Current (mA)

Dia

phra

gm D

ispl

acem

entµ

m)

Displacement Vs. Coil Current in Microvalve

Flexible DiaphragmMagnet

Fluidiclayers

Multilayer Coil

Input

OutputSpacerSpacer

Fabricated Microvalve

Fluidic Layers

In: Gongora-Rubio M.R., Santiago-Aviles J.J. et al., SPIE (1.999), v.3877. p.230 - 239

LTCC HYBRID ACTUATORS (MICROVALVE)LTCC HYBRID ACTUATORS (MICROVALVE)

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MESOMESO--SCALE PLASMA GENERATORSCALE PLASMA GENERATOR

Characteristics of Meso-Scale Plasmas:- suitable for operation at high pressure (10-760 Torr).- sofisticated vacuum system is not required.- high plasma density (1013 - 1015 cm-3)

Advantages of LTCC:- easy to construct 3D structures.- resistant to high temperature.- low cost.

Applications of Meso-Scale Plasmas:- surface treatments / coatings.- etching of materials.

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DEVICE DIMENSIONS & PARAMETERSDEVICE DIMENSIONS & PARAMETERSDimensions:

- Inter-electrode spacing: 500 µm.- Area: 10 x 10 mm2.- Green tape thickness: 250 µm (before firing)

220 µm (after firing)- Microchannel cross-section: 500 µm x 500 µm- Gas inlet tube diameter: 2.5 mm.- Gas distributor hole diameter: 500 µm.- Electrode width: 500 µm.- Electrode thickness: 5 µm.

Operation parameters:- RF frequency: 13.56 MHz.- RF power: 10 - 30 W- Pressure: 10 - 20 Torr- Gas flow-rate: 1 - 10 sccm.

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GENERATOR OPERATIONGENERATOR OPERATION

gas inletgas outlet

plasmainterdigitated

electrode(silver)

microchannel

substrate

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DEVICE LAYOUTDEVICE LAYOUT

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FABRICATED DEVICESFABRICATED DEVICES

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BASIC MICROFLUIDIC DEVICESBASIC MICROFLUIDIC DEVICES

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MICROMICRO--CHANNELS IN LTCCCHANNELS IN LTCC

A A

Corte A-A

A A

A A

•• PoiseuillePoiseuille equation relates equation relates linearly pressure drop with linearly pressure drop with flow in reduced geometry flow in reduced geometry channels.channels.

•• LTCC can be easily used for LTCC can be easily used for implementing channels.implementing channels.

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NEW MICROCHANNEL FORMING TECHNIQUENEW MICROCHANNEL FORMING TECHNIQUE

•• Sacrificial Sacrificial volume volume technique technique is is used used to to create microchannels create microchannels during lamination by deformation during lamination by deformation of of the unfired the unfired tape. tape.

Sandia Labs

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MICROCHANNELS FOR MIXINGMICROCHANNELS FOR MIXING

1

X

Y

Z

0

22.74245.484

68.22690.968

113.71136.452

159.194181.936

204.678

MAR 31 200316:04:23

VECTOR

STEP=1SUB =1VNODE=66MIN=0MAX=204.678

Channel width = 150 µm

•• In In Microchannels Microchannels of minute of minute dimensions result in very low dimensions result in very low Reynolds Number, making Reynolds Number, making difficult liquid mixing.difficult liquid mixing.

•• MicrochannelMicrochannel corners can be corners can be used as chaotic advection used as chaotic advection generators for mixersgenerators for mixers

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PASSIVE MIXING PASSIVE MIXING CHAOTIC ADVECTION BY CHANNEL EDGES CHAOTIC ADVECTION BY CHANNEL EDGES

risin

g m

ixin

gra

te

Serpentine channel

Square channel

Straight channel

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PASSIVE MIXING PASSIVE MIXING CHAOTIC ADVECTION BY CHANNEL EDGESCHAOTIC ADVECTION BY CHANNEL EDGES

↑↑ ratemixingnedge _~

↑∆↑ pnedge ~

Spiral channel

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3D MICRO MIXERS IN LTCC3D MICRO MIXERS IN LTCC

•• 3D 3D Serpentine Serpentine Micromixers can be Micromixers can be used used for for chemical chemical Microreactors Microreactors in in orderorder to to fabricatefabricateemulsionsemulsions, , particle particle packaging and packaging and nanomaterial nanomaterial fabrication

10 mm

fabrication

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LTCC MANIFOLDS FOR MICROFLUIDICSLTCC MANIFOLDS FOR MICROFLUIDICS

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Technical University of Dresden

LTCC LTCC ApplicationsApplications onon MICROFLUIDICS MICROFLUIDICS

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Heat ConductivityHeat Conductivity

•• DetectionDetection ofof heat heat conductivityconductivity,, fluid flow fluid flow resistanceresistance,,

•• Membrane withMembrane with 40µ40µ--thicknessthickness, 16mm, 16mm diameter diameter andand 15µ15µ--thicknessthickness..

Swiss Federal Institute of Technology, Lausanne)

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5. MESO SYSTEMS APPLICATIONS5. MESO SYSTEMS APPLICATIONS

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MST APPLICATIONS: GUSTATORY PROBEMST APPLICATIONS: GUSTATORY PROBE•• ThisThis is is an applicationan application inin the fieldthe field

ofof Physiological PsychologyPhysiological Psychology. . •• The proposed systemThe proposed system isis designeddesigned

toto extractextract asas much information much information about the chemical and about the chemical and neurological responsesneurological responses ofof the the taste buds withintaste buds within aa given papillagiven papillaasas possiblepossible. .

•• The systemThe system is tois to measure the measure the physiologicalphysiological ((electrochemicalelectrochemical))responseresponse to ato a flavor stimulusflavor stimulus ininthe tongue andthe tongue and toto see howsee how ititcorrelates with the persons correlates with the persons perceived senseperceived sense ofof tastetaste..

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MST APPLICATIONS:MST APPLICATIONS:PCR IN CONTINUOUS FLOWPCR IN CONTINUOUS FLOW

•• IntegratedIntegrated microfluidicmicrofluidic devicesdevices for PCRfor PCR amplification amplification and detectionand detection ofof biological samples that employ closedbiological samples that employ closed--loop temperature monitoring and control have been loop temperature monitoring and control have been demonstrated withindemonstrated within a multilayera multilayer low temperaturelow temperature coco--fired ceramicsfired ceramics (LTCC)(LTCC) platformplatform. .

Motorola Labs

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MST APPLICATIONS: MST APPLICATIONS: FUEL CELLS FOR PORTABLE ELECTRONICSFUEL CELLS FOR PORTABLE ELECTRONICS

Motorola Labs

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MST APPLICATIONS:MST APPLICATIONS:LAB ON A CREDIT CARDLAB ON A CREDIT CARD

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POLLUTANTS CONTROLPOLLUTANTS CONTROL•• Mobile devices for monitorazing the eutrophication process Mobile devices for monitorazing the eutrophication process (nitrites, ammonium & phosphorous species ), dissolved oxygen (nitrites, ammonium & phosphorous species ), dissolved oxygen and heavy metal contamination in lakes.and heavy metal contamination in lakes.

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FLOW INJECTION ANALYSIS (FIA) FOR WATER CONTAMINATION FLOW INJECTION ANALYSIS (FIA) FOR WATER CONTAMINATION STUDIESSTUDIES

•• Sensitivity and selectivity of the sensor can be optimizedSensitivity and selectivity of the sensor can be optimized•• Time for analysis is minimizedTime for analysis is minimized•• Waste and sample size are minimizedWaste and sample size are minimized

Control Unit

SampleSample

Carriersolution

DetectionDetectionsystemsystem

PeristalticPeristalticpumppump

InjectionInjectionvalvevalve

wwReaction Reaction

coilcoil

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LTCC MANIFOLD FOR HEAVY METAL DETECTIONLTCC MANIFOLD FOR HEAVY METAL DETECTION•• Here one can seeHere one can see aa laboratory the sizelaboratory the size of aof a creditcredit cardcard realizedrealized in LTCC. It is in LTCC. It is

aa systemsystem forfor the electrochemical detectionthe electrochemical detection ofof heavy metalsheavy metals inin river watersriver waters. . •• A manifold for various tasks was designed, we include the possibA manifold for various tasks was designed, we include the possibility of ility of

mixing two fluids (if a reagent is needed) and implement a spiramixing two fluids (if a reagent is needed) and implement a spiral coil used as l coil used as a mixing/reaction chamber. a mixing/reaction chamber.

•• DuPontDuPont 951 LTCC tapes with layer thickness of 250 951 LTCC tapes with layer thickness of 250 µµm were used to m were used to fabricate 500 micron width micro channelsfabricate 500 micron width micro channels..

Fluid Merging Passive Mixer Measuring Cavity

Sensor Array

Nozzle

Fluid Outlet

Inlets

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ELECTRODE DESIGNELECTRODE DESIGN•• A multiA multi--electrode sensor array for electroelectrode sensor array for electro--chemical measurement was chemical measurement was

fabricated using thick film screenfabricated using thick film screen--printing deposition of gold paste. printing deposition of gold paste. •• The sensor array is composed of a silver/silver chloride referenThe sensor array is composed of a silver/silver chloride reference electrode, ce electrode,

a gold counter electrode and two gold detection electrodes (L=30a gold counter electrode and two gold detection electrodes (L=3000µµm, m, W=2mm)W=2mm)

Electrical outputs

Detection ElectrodeAg/AgCl ElectrodeDetection Electrode

Counter Electrode

Fluid Outlet

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MANIFOLD RESPONSEMANIFOLD RESPONSE

•• SquareSquare--wave stripping wave stripping responses for increasing responses for increasing concentrations of Copper and concentrations of Copper and Mercury (10 a 115 µg LMercury (10 a 115 µg L--11).).

•• PrePre--concentration time: 60 sconcentration time: 60 s

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SPECTROPHOTOMETRICAL DETECTION OF NITRITESSPECTROPHOTOMETRICAL DETECTION OF NITRITES

•• Nitrite ion was determined by its reaction Nitrite ion was determined by its reaction with sulphanilamidewith sulphanilamide toto form the diazonium form the diazonium salt which was coupled withsalt which was coupled with NN-- (1(1--naphthylnaphthyl))ethylene diamineethylene diamine toto yield anyield an azoazo dye whose dye whose absorbance was measuredabsorbance was measured at 540nmat 540nm

Spectrophotometer

Peristaltic pump

Waste

Solenoid valves

H2O Reagent NO2-

V1 V2 V3

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AMMONIA ION DETECTIONAMMONIA ION DETECTION•• InvolvedInvolved inin the eutrophication processthe eutrophication process•• FoundFound as NHas NH44

++

•• RelatedRelated toto the presencethe presence ofof other ionsother ions,, suchsuch as NOas NO33-- andand NONO22

-- ((nitrogen cyclenitrogen cycle))•• Potentiometric detectionPotentiometric detection:: Ion Selective ElectrodeIon Selective Electrode (ESI)(ESI)

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DEVICES WITH PVDF MEMBRANEDEVICES WITH PVDF MEMBRANE

Spiral mixer provides a good interaction betweenreagents.

A Gas-diffusion membrane is used so that a better sensibilityand selectivity can be achieved.

PVC

PVC

PVDF

NH4+ + OH-

NH3

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Anion exchanger needed topreconcentrate analyte in order toincrease detection limits.

Metallic meshes are needed to keepthe resin inside the cavity.

•• InvolvedInvolved inin the eutrophication processthe eutrophication process•• Mainly foundMainly found as HPOas HPO4 4

22-- andand HH22PO PO 44--

•• Potentiometric detectionPotentiometric detection: : –Ion Selective Electrode (ESI)

PHOSPHATES DETECTIONPHOSPHATES DETECTION

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6. CONCLUSIONS6. CONCLUSIONS

• The brief description given here demonstrates how LTCC technology is a suitable material for the fabrication of Meso systems.

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Thanks for your Thanks for your attention !attention !