Standardisation in High Temperature Corrosion TestingCorrosion Testing
Review of Task 4 of the UK-US Collaboration
23rd Annual Conference on Fossil Energy MaterialsPittsburgh Airport Marriott
May 12-14 2009May 12 14, 2009
Tony Fry National Physical Laboratory, Teddington, UK
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Overview
• Introduction to Task 4• Data collection and storage• Standardisation• Standardisation• Inter-comparison
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
What was task 4d ith?concerned with?
• To identify critical differences between standards for measurement of high temperature materials properties
1902• To identify where further standardisation for measurement of high temperature materials properties is required
1902NPL Opens
• To develop a common format for data exchange
• To investigate the use of commercial To investigate the use of commercial database software for collecting and maintaining materials properties data and micrographs 1906
Metallurgical
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Metallurgical laboratory
The collaboration willgenerate a lot of data – how do
we manage and collect it?
• What data is being recorded?
• Can we agree on what should be • Can we agree on what should be reported?
What is the best method of capturing • What is the best method of capturing this data?
C• Can everyone use the selected method?
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Data collation in a database, which includes metadatawhich includes metadata
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
How can we be sure thed t i bl ?data is comparable?
International Organisation for Standardisation
European Committee for Standardisation(CEN)
British Standrds Institure American National Standards Institure Deutsches Institut fur Normung
International Organisation for Standardisation(ISO)
British Standrds Institure(BSI)
American Society for Testing of Materials(ASTM)
American National Standards Institure(ANSI)
Deutsches Institut fur Normung(DIN)
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
How do the UK and USt d d ?standards compare?
Mechanical Tests
• Hardness
Corrosion Testing
• Laboratory exposures in steam and i d (i l di d it )• Tensile
• Creep• Low Cycle Fatigue (LCF)
High Cycle Fatigue (HCF)
mixed gases (including deposits)• Post-exposure evaluation of
environmental attack• Steam Loop exposures• High Cycle Fatigue (HCF)
Physical Testing
Steam Loop exposures• Coating Thickness• Burner rig testing• Thermal Cycling/Cyclic Oxidation
• Thermal Diffusivity• Dilatometry• Surface Area Measurement
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Findings of the review –h i l t timechanical testing
Test Addressed by Standards Further work needed
Knoop Brinell Hardness ISO - TC164 Knoop, Brinell, Vickers, Rockwell No
Tensile ISO - TC164Ambient Temp.
High TempNo
High Temp.Creep ISO Uniaxial No
Standards exist for LCF ASTM, CEN, BSI strain controlled,
TMF.Not at this point
HCF Yes Ambient Temp. Yes, HT HCF
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
p ,
Findings of the review –h i l t tiphysical testing
Test Addressed by Standards Further work needed
Thermal Diffusivity ASTM Laser flash NoThermal Diffusivity ASTM Laser flash NoDilatometry Yes
Surface Area M t ISO Gas adsorption or
bilit NoMeasurement ISO permeability No
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Findings of the review –i t ticorrosion testing
Corrosion Testing
• Laboratory exposures in steam and • Laboratory exposures in steam and mixed gases (including deposits)
• Post-exposure evaluation of environmental attack
At the time of the review there were no international US or Europeanenvironmental attack
• Steam Loop exposures• Coating Thickness
international, US or European standards existing for high temperature
corrosion of metallic materials.• Burner rig testing• Thermal Cycling/Cyclic Oxidation
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
But…
this area is being actively pursued by ISO TC156 WG13 and standards for:
• Test Method for Isothermal Exposure Testing under High Temperature • Test Method for Isothermal Exposure Testing under High Temperature Corrosion Conditions
• Method for Metallographic Examination of Samples after Exposure to High Temperature Corrosive EnvironmentsTemperature Corrosive Environments
• Thermal Cycling Exposure Testing Under High Temperature Corrosion Conditions
are in preparation.
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
No standards, so what…I t iInter-comparison
Seam Oxidation
• 3 materials (T92, 347HFG, IN740)
Boiler Corrosion
• 2 materials (T22 and P92)( , , )• Same material stock• Same temperatures
( )• Same material stock• Gas composition set
– 0.3% SO2 , 6.0% O2 , 14.6% CO2 , 74.2% H2
• Lab could prepare samples in their standard manner
• Tests conducted using their own
• Ash composition set– Na2SO4/K2SO4/Fe2O3 (1.5/1.5/1 on a molar basis)
• Temperatures setpreferred method
• Data analysed in their own preferred technique
• Lab left to prepare samples and expose using their preferred method
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
600°C
P92, 1000 h exposure
ALSD, H2O, 1 bar
ANSA, H20, I bar
CESI, H2O, 1 bar
600°C650°C
FZJ, Ar50%H2O, 1 bar
FZJ, H2O, 240 bar
INTA, Ar50%H2O, 1 bar
static steam
INTA, H2O, 1 bar
KEMA, H2O, 60 bar
NPL, H2O, 1 bar
0 100 200 300
SPGG, H2O, 1 bar
Willemshafen, 250 bar
static steam
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
0 100 200 300
oxide scale thickness, μm
Steam Oxidationi t l texperimental setup
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Steam oxidationi t lexperimental
• Sample geometry– 10 x 10 x 3mm– 20 x 10 x 2mm
• Exposure procedure– Duplicate samples exposed for a set
time duration (no cycling)20 x 10 x 2mm– Semicircular section
• Surface Preparation
– Sample all exposed at the same time, thermal cycles introduced to remove samples
• Surface Preparation– Samples from bulk– Samples retained original surface
Surfaces prepared 600 grit SiC
– Ambient pressure & 17 bar
– Surfaces prepared 600-grit SiC
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Steam oxidationlt T92 t 600 ºCresultsT92 at 600 ºC
25
-2
20
ge, m
gcm
-
10
15
ss C
hang
5
peci
fic M
as
NPL
Cranfield
00 1000 2000 3000 4000 5000 6000
Sp ORNL
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Steam oxidationlt T92 t 600 ºCresults T92 at 600 ºC
30
-2
20
25
e, m
gcm
-
15
20
ss C
hang
5
10
peci
fic M
as
NPL
Cranfield
00 1000 2000 3000 4000 5000 6000
Sp ORNL
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Steam oxidationlt T92 t 650 ºCresults T92 at 650 ºC
20
-2
141618
ge, m
gcm
-
81012
ass
Cha
ng
246
peci
fic M
a
NPL
Cranfield02
0 500 1000 1500 2000 2500 3000
Ti h
Sp
C a e d
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Steam oxidationT92 t t d dT92 temperature dependency
12
14
16
mgc
m -2
4
6
8
10
12
fic M
ass
Cha
nge,
m
NPL 600°C
0
2
4
0 500 1000 1500 2000 2500 3000Time, h
Spec
if 600 CNPL 650°C
101214161820
hang
e, m
gcm
-2
02468
10
Spe
cific
Mas
s C
Cranfield 600°CCranfield 650°C
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
00 500 1000 1500 2000 2500 3000
Time, h
Steam oxidationlt 347HFG t 650 ºCresults 347HFG at 650 ºC
6
2
3
45
mg,
cm
-2
01
2
s C
hang
e,
3
-2-1
0
ecifi
c M
ass
347HFG ORNL
347HFG NPL
34 HFG C fi ld
-4-3
0 1000 2000 3000 4000 5000
Spe 347HFG Cranfield
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Steam oxidationlt 347HFG t 700 ºCresults 347HFG at 700 ºC
5
3
4
mg,
cm
-2
1
2
s C
hang
e, m
-1
0
ecifi
c M
ass
347HFG NPL
-2
1
0 1000 2000 3000 4000 5000
Spe
347HFG Cranfield
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Steam oxidationlt IN740 t 750 ºCresults IN740 at 750 ºC
1.40
m -
2 IN740 ORNL
1.00
1.20
ge, m
g, c
m IN740 NPL
IN740 Cranfield
0.60
0.80
ass
Cha
ng
0.20
0.40
Spe
cific
Ma
0.000 1000 2000 3000 4000 5000
Time h
S
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
What could be causingth diff ?the differences?
• Specimen Geometry
• Thermal Cyclingy g
• Orientation of grains
• Spallation
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Seam Oxidation
• 3 materials (T92, 347HFG, IN740)
Boiler Corrosion
• 2 materials (T22 and P92)( , , )• Same material stock• Same temperatures
( )• Same material stock• Gas composition set
– 0.3% SO2 , 6.0% O2 , 14.6% CO2 , 74.2% H2
• Lab could prepare samples in their standard manner
• Tests conducted using their own
• Ash composition set– Na2SO4/K2SO4/Fe2O3 (1.5/1.5/1 on a molar basis)
• Temperatures setpreferred method
• Data analysed in their own preferred technique
• Lab left to prepare samples and expose using their preferred method
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
What about boiler corrosion, that’s OK isn’t?that s OK…isn t?
T22 at 425 ºC
50
60
30
40
oss,
mic
rons
10
20
Met
al L
o
NPL
Doosan
0
10
0 200 400 600 800 1000 1200
Doosan
NETL
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
P92 at 675 ºC
1800
1200
1400
1600
ons
800
1000
1200
Loss
, mic
ro
200
400
600
Met
al
NPL
Doosan
0
200
0 100 200 300 400 500 600 700 800 900 1000 1100
Time h
NETL
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Time, h
Why the differences?
• Specimen manufacture• Measurement accuracy• Fundamental differences in the apparatus• ?
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
What does all this mean?
No one is wrong the results are just differentNo one is wrong, the results are just different
• Results are self consistent with a laboratory
• Measurements are precise but there is scatter due to material effects (i.e. spalling)
• Ideally we would like high precision and good repeatability
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Where do we go f h ?from here?
• Standard test methods for corrosion testing which address specimen manufacture and preparation as well as the actual test procedure and analysis.procedure and analysis.
• Need to addressS i t– Specimen geometry
– Surface preparation– Testing procedures
Measurement accuracy & uncertainty– Measurement accuracy & uncertainty
Phase 2 will be addressing some of these issues
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials
Thank you for your attention
Any questions?y q
Pittsburgh – 14th May 2009 UK-US Collaboration on Fossil Energy R&D - Advanced Materials