Materials Science & Technology Application of advanced and non - - PowerPoint PPT Presentation

▶
materials science amp technology application of advanced
SMART_READER_LITE
LIVE PREVIEW

Materials Science & Technology Application of advanced and non - - PowerPoint PPT Presentation

May 01, 2023 440 likes •695 views

Materials Science & Technology Application of advanced and non destructive testing in solid oxide fuel cells Peter Wyss, Erwin Hack Laboratory for Electronics/Metrology/Reliability Artur Braun, Lorenz Holzer, Christian Soltmann, Peter

slide-1
SLIDE 1

Materials Science & Technology

Application of advanced and non destructive testing in solid oxide fuel cells

Peter Wyss, Erwin Hack Laboratory for Electronics/Metrology/Reliability Artur Braun, Lorenz Holzer, Christian Soltmann, Peter Holtappels Laboratory for High Performance Ceramics Empa, Swiss Federal Laboratories for Materials Testing and Research Überlandstr 129 , CH-8600 Switzerland

slide-2
SLIDE 2

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 2

Innenringdichtung Radialdichtung Innenringdichtung Radialdichtung

Outline

Test items and techniques

Non-destructive testing

neutron tomography

x-ray radiography

thermography

Advanced destructive testing

FIB tomography

Outlook metallic components ceramic components

slide-3
SLIDE 3

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 3

SOFC features&scaling Electrocatalytic activity Nano/atomic scale Ionic conductivity Nano/atomic scale Electronic conductivity „Nano/atomic/micro scale“ (Open) porosity Microscale

SEM/OM/EDX Only 2-D imaging

Solid Oxide Fuel Cell

  • Principles
  • Fuel: CH4

/H2 O CO2 /H2 O Air: O2 /N2

anode support Metallic IC Cr-, Ni-Cr-Steels

N2

Ni/YSZ

e- e-

anode Ni/YSZ electrolyte

OO

x

YSZ

cathode

LSM, LSCF, LSF Metallic IC Cr-, Ni-Cr-Steels

3

  • D

s t r u c t u r e s

slide-4
SLIDE 4

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 4

Non-destructive Testing (NdT)

component state potential problem ndt test method

metallic machined part cracks, bad welds X-ray RT, CT, UT for interconn. metallic assembled in stack corrosion, contamination RT, CT X-rays, Neutrons ? ceramic green machined part porosity + homogenity, shrinkage cracks RT, µCT local mode, X-rays, TT ceramic assembled and fired to cell cracks + delaminations (thermal cycling) RT, µCT local mode, X-rays, TT ceramic cells mounted in the stack fatigue cracks (thermal cycling) RT, CT, Neutrons + contrast fluid ?

slide-5
SLIDE 5

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 5

RT system data (typical)

  • 1. NdT

methods and test items

source beam geometry resolution in µm field

  • f view

(FOV) in mm

  • typ. penetrable

ZrO2 in mm Neutrons almost parallel 100 300 > 200 X-ray Mini / Micro focus conical 10 400 20 X-ray Synchrotron parallel 1 10 2

X-ray direction Field

  • f view
slide-6
SLIDE 6

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 6

Neutron tomography

~ 20 cm permits „insight“ into submillimeter porosity

  • f SOFC stack
slide-7
SLIDE 7

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 7

  • 2. RT and local

µCT to Empa YSZ pellets

The RT / CT microscopy (macroscopy) system X-ray flat panel Hamamatsu 7942 CA-02 VISCOM TEP 9225 panorama tube head

  • r

TXD 9160 subµ tube head Sample on low runout rotation stage

slide-8
SLIDE 8

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 8

The crack detection limit in radiography α c w

crack detection is possible if: c > 0.01 w * sin α tube spot size * 0.5 X-ray direction

RT and local µCT to Empa YSZ pellets

slide-9
SLIDE 9

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 9

Visible light microscopy Radiographies

  • f a hidden

coarse grain

RT and local µCT to Empa YSZ pellets

FOV 5 x 5 mm, pixelsize 2.5 µm

slide-10
SLIDE 10

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 10

Visible light microscopy Radiographies

RT and local µCT to Empa YSZ pellets

  • f a shrinkage

crack FOV 5 x 5 mm, pixelsize 2.5 µm

slide-11
SLIDE 11

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 11

Local X-ray µCT of crack in pellet Ø 35 x 1 mm Slices parallel to main surface Field

  • f view

5 x 5 mm, voxelsize 5 µm

RT and local µCT to Empa YSZ pellets

slide-12
SLIDE 12

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 12

Local X-ray µCT of hidden coarse grain Slices parallel to main surface Field

  • f view

5 x 5 mm, voxelsize 5 µm

RT and local µCT to Empa YSZ pellets

slide-13
SLIDE 13

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 13

The thermography cam, heart

  • f the

TT system

TT, RT and local µCT to HTceramics cells

Camera Cedip JADE Camera type Array Resolution 240 x 320 pix Wavelength range 3-5 μm Frame rate Full: 170 Hz ROI: 9 kHz Lateral resolution 15 x 15 μm2 NETD 20 mK

  • Temp. range
  • 20 –

1300 °C Lock-In frequency < 5 kHz

slide-14
SLIDE 14

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 14

TT, RT and local µCT to HTceramics cells Thermography testing (TT), impulse method

bad bond spot flash hits surface diffusion wave propagates bad bond spot stops the heat diffusion wave and after some time a thermic contrast appears: positive at the impulse side, negative at the rear side time ≈ depth

2

lateral resolution ≈ 2 x depth

slide-15
SLIDE 15

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 15

Impulse thermography images

  • f a region

containing a spot

  • f high thermal conductivity

TT, RT and local µCT to HTceramics cells

Istantaneous after flash 20 msec later FOV 180 x 150 pixel

  • r

28 x 25 mm, Pixelsize 167 µm FOV for RT +µCT

slide-16
SLIDE 16

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 16

The same region (FOV 5 x 5 mm) imaged with: Radiographies, pixel size 2.5 µm Local tomography, voxel size 5 µm

TT, RT and local µCT to HTceramics cells

slide-17
SLIDE 17

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 17

Focussed Ion Beam (FIB) technique

DLR BekNi 275/3

Advanced preparation procedure Conventional preparation procedure

Hi2 2 H

slide-18
SLIDE 18

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 18

TEM: Imaging & elemental analysis

chemical map: Ni Zr

DLR BekNi 275/3

slide-19
SLIDE 19

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 19

DLR BekNi 275/3

Electrolyte stabilised zirconia Fuel electrode Ni-Cermet Air electrode perovskite

volume: 40 x 40 x 40 m3

FIB-Nanotomography: 3-D structure

  • f a FC
slide-20
SLIDE 20

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 20

Nanotomography: Informationsgewinn

3D Imaging Particulate und micro structure

6 µm

A

6 µm

B

Distinction Crystallite-Particulate aggregates

Use

  • f Information:

Modeling Understanding degradation e.g. sulphur poisoning

slide-21
SLIDE 21

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 21

access to large scale facilities

Advanced characterisation

cm / mm micro meter nano meter

Source: J.R. Wilson et al., Nature Materials 5 541-544, 2006

software sample preparation

slide-22
SLIDE 22

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 22

NdT methods and diagnostics strategy

Visual testing (VT), including visible light microscopy

will be done in any case

Ultrasonic testing (UT)

requires flat surfaces and low damping, 3D possibility

Eddy current testing (ET)

for electrical conductors

  • nly

Magnetic testing (MT)

for ferritic materials

  • nly

Thermography (TT)

best for close to surface items, 3D possibility

Radiographic testing (RT, CT, XTM)

No requirements to surfaces and damping, 3D possibility

Quality assurance

cell production

stacking

Life time / Durability

comparison

  • f pre

and post test state by NdT possible

failures affecting mechanical properties visible by NdT

Combination

  • f NdT

advantageous

identification

  • f points

for destructive analysis

3D imaging  real structures  validation

  • f 2D analysis

(e.g. SEM, OM)

slide-23
SLIDE 23

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 23

Acknowledgement

Defne Bayraktar, EMPA

Ulrich Vogt, EMPA

Thomas Graule, EMPA

Günter Schiller, DLR

SINQ, PSI

Josef Sfeir, Hexis

HTceramix

Hi2 2 H

slide-24
SLIDE 24

Empa, Peter Holtappels, FC Tools, Trondheim, 23.6.2009 24

  • 4. A possible

NdT procedure for cells Impulse thermography

  • verview

(FOV = 80 x 80 mm) Pixel size 0.33 mm, meas. time per cell ≈ 2 min Impulse thermography close up (FOV = 8 x 8 mm) Pixel size 33 µm , meas. time per cell ≈ 10 min (automated) Radiography

  • verview

(FOV = 80 x 80 mm) Pixel size 20 µm , meas. time per cell ≈ 5 min Radiography close up (FOV = 8 x 8 mm) Pixel size 4 µm (OVHM - Movie) , meas. time per item ≈ 10 min (auto) Local tomography (FOV = 8 x 8 mm) , meas. time per item ≈ 60 min voxel size 4 µm or calculation

  • f items

depth by evaluating the trajectories from OVHM -Movie