Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...

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Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Microstructural deterioration assessment of
ex-service power plant steel using concentric
 backscatter imaging

 Presented By: Melody van Rooyen, Supervisor: Prof TH Becker
In collaboration with: CHRTEM, NMU (Dr. J Westraadt and Dr. G Marx)
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Background – Power stations and creep
 350

 Max. operating hours
 Exceed design life Design life 300

 Life exhaustion ratio
 250

 Life exhaustion ratio OL/DL (%)
 200

 150

 100

 50

 0

 High temperature
 (> 550 °C), high
 Creep
 steam pressures
 (>15 MPa)
 iosrjournals.org

MSSA Conference, Langebaan, 4 December 2019 1
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Background – Material assessment
 Microcracks
 1.0
 Oriented
 cavities
 Isolated
 
 cavities
 Relative strain,

 No
 damage

 Macrocracks

 0.0
 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
 
 Life fraction,
 Damage state Cavities/mm2

 12 % Cr steel:
 New Ideally none
 X20CrMo12-1 Low 60-90
 (X20 for short) Ex-
 Medium ≈200
 service
 EPPEI
 X20 High >220-690
MSSA Conference, Langebaan, 4 December 2019 2
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Background – Microstructural analysis

 Micro-grain boundary

 Block Laths of
 boundary two
 variants
 Packet
 boundary Packet
 Cr23C6 / Laves phase (Fe2Mo)
 Lath MX
 Prior austenite grain boundary Mobile dislocations
 Dipole dislocations

MSSA Conference, Langebaan, 4 December 2019 3
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description - Materials

 Virgin Low Medium High Damage
 Material (New) Damage Damage
 Type:
 X20 CrMoV12-1

 Cavity density
 measured from
 250
 BSE-SEM
 (cavity/mm2)
 Operating
 - 545 545 543
 temperature (°C)
 Operating steam
 - 17.0 19.4 18.1
 pressure (MPa)
 Operating life
 - 130 000 130 000 156 000
 (hours)
MSSA Conference, Langebaan, 4 December 2019 4
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description – Creep testing
 (a) (b) Disc sampling locations in gauge region
 x=0x=5
 Longitudinal
 centreline
 5 mm
 Specimen
 extraction Disc sampling
 Gauge location in grip
 region
 Loading direction

 (c) Cameras (d) Specimen
 (d)
DIC: Digital
 Image
Correlation
 Water-cooled grips

 White LED Gleeble vacuum chamber

MSSA Conference, Langebaan, 4 December 2019 5
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description – Creep testing (cont.)

MSSA Conference, Langebaan, 4 December 2019 6
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description – Creep testing (cont.)

MSSA Conference, Langebaan, 4 December 2019 7
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description – Microstructure

CBS-SEM: Concentric Backscatter-
 CBS detector Specimen
 Scanning Electron Microscopy
 settings preparation
 • FIB-SEM • Twin-jet
 • 5 kV electropolishin
 • 0.20 nA g
 • 4 mm WD • 5 % HClO4
 • Total of 4 solution
 images per • 21-30 V
 site (680 μm2) • -20 °C

 FEI

MSSA Conference, Langebaan, 4 December 2019 8
Microstructural deterioration assessment of ex-service power plant steel using concentric backscatter imaging - Presented By: Melody van Rooyen ...
Experimental description – Micro. (cont.)

 Micro-grains

 5 μm

 Precipitates

 Diameter

 Interparticle
 Cr23C6 spacing
 Laves w
 phase Number
 density
 2.5 μm

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Results - Qualitative
 Low - Grip High - Grip

 Medium - Grip High – Fracture (gauge)

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Results – Quantitative (micro-grains)

 25 0.8
 Low
 EXL - Grip

 m)
 EXH - Grip 0.75
 20 High
 EXL - Grip lognormal fit
 Low
 EXH - Grip lognormal fit 0.7
 15 High

 Micro-grain short width (
Frequency (%)

 0.65
 10
 0.6

 5
 0.55

 0 0.5
 0 1 2 3 4 Low Med. High
 Subgrain short width ( m)

 Similar Larger
 sized grains
 grains

 MSSA Conference, Langebaan, 4 December 2019 11
Results – Quantitative (Precipitates)

 Particle Inter-particle Volume number density
 size spacing
Size or inter-particle spacing (nm)

 Volume number density (μm-3)
 :Gauge Cr23C6
 :Grip

 Low Medium High

 MSSA Conference, Langebaan, 4 December 2019 12
Results – Quantitative (Precipitates)

 Particle Inter-particle Volume number density
 size spacing
Size or inter-particle spacing (nm)

 Size or inter-particle spacing (nm)

 Volume number density (μm-3)
 Volume number density (μm-3)
 :Gauge Cr23C6 Laves
 :Grip

 Low Medium High
 Low Medium High

 Dense carbide Smaller micro-
 Higher Laves
 distribution grains
 phase distribution
 MSSA Conference, Langebaan, 4 December 2019 13
Results – Hardness

 Medium: high
 hardness

 Low
 Medium
 High

 Longitudinal distance from central gauge location

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Mechanical response

 High
 0.1
 600 °C

 0.08

 Low Med.
 0.06
 Creep strain

 0.04

 0.02

 0 New
 0 1 2 3 4 5
 Time (hours)

MSSA Conference, Langebaan, 4 December 2019 15
Mechanical response
 Confirms CBS results: high Cr23C6
 density enhances creep resistance
 despite cavity density
 Faster creep rates for
 High low compared to
 0.1 medium
 600 °C
 -3 °C
 0.08 10 600

 Low Med. -4
 0.06

 )
 10

 -1
 Creep strain

 Low Med.

 Creep rate (s
 0.04 -5
 10

 0.02 -6
 10

 0 New -7
 10
 0 1 2 3 4 5 0 1 2 3 4 5
 Time (hours) Time (hours)

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Conclusion

 • CBS is a convenient microstructural method for micro-grain and large
 particle characterisation of ex-service material
 • Highly damage material has large polygonal micro-grains, low density
 of carbides and high fraction of Laves phase especially near voids.
 • Low damage has less Laves phase but had a lower density of carbides
 than medium
 • Medium displays relatively smaller grains due to dense carbide
 distribution. Medium and low damage display similar creep rates
 despite differences in void distributions
 • Using CBS allows faster damage assessment through a single
 microstructural analysis stream – faster maintenance decisions

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Conclusion

 “No SINGLE measurement is sufficiently
 comprehensive to describe the [damage state
 of] the steel with all requisite completeness”
 ~ Bhadesia et al. (1998)

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Acknowledgements and questions
 Thank you to the following:

 Supervision:
 Prof Thorsten Becker and Materials Engineering Research Group at SU
 CBS-SEM imaging:
 NMU CHRTEM team, Dr J Westraadt and Dr G Marx
 Gleeble testing/specimen preparation facilities:
 Prof Rob Knutsen and S. von Willingh at CME
 Stakeholder guidance and material provision:
 EPPEI staff and fellow students
 Funding:
 NRF (THRIP) and THUTHUKA, Frank Wilhelm Bursary Fund

 MATENG group
 www0.sun.ac.za/mateng

 ResearchGate

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