Assessment of Creep Damage in Fe-Ni-Cr Alloys: Frans Sorsh
Assessment of Creep Damage in Fe-Ni-Cr Alloys: Frans Sorsh
AVANCERAD NIVÅ, 30 HP
STOCKHOLM, SVERIGE 2019
Assessment of creep
damage in Fe-Ni-Cr alloys
FRANS SORSH
KTH
SKOLAN FÖR INDUSTRIELL TEKNIK OCH MANAGEMENT
www.kth.se
Abstract
It is only a matter of time before components working in high temperature environments fail due to
creep. Design for creep is therefore of vital importance to maximize the lifetime of components and
reduce costs that may arise from maintenance and replacement of components. This thesis aims to use
metallographical methods and finite element modeling to assess creep damage in a hydrogen reformer.
The decommissioned reformer, made of Fe-Ni-Cr alloys, was investigated thoroughly via replica
testing, hardness measurements as well as finite element modeling of the welds. An extended literature
review was performed to gain a better understanding of creep in Fe-Ni-Cr alloys, welds and the
modeling of creep generally. The microstructures of samples from the reformer were analyzed and
mapped out in terms of creep damage which were then compared to a creep analysis of the welds with
a simulation time of 100 000 h. The FE results yielded high stresses and creep strains with a maximum
of 0.95% in the boundaries of the welds which gave realistic representations of strain distributions
when compared to the metallographical results. Hardness measurement indicated that a relatively
narrow zone with altered mechanical properties is present along the weld boundaries. This area, called
the heat affected zone, was found to be most affected by creep with microcracks reaching maximum
lengths of 2 mm. The creep strains obtained from simulation did not fall in line with the observed
creep damage, it was thus concluded that a material model that considers tertiary creep would yield a
more realistic representation in FEM for Fe-Ni-Cr alloys.
Bedömning av krypskador i Fe-Ni-Cr legeringar
Sammanfattning
Det är bara en tidsfråga innan komponenter som arbetar i högtemperaturförhållanden misslyckas pga
kryp. Att designa med avseende på kryp är därmed viktigt för att maximera livslängden och reducera
kostnader som kan komma från underhåll och från utbyte av komponenter. I detta examensarbete
används metallografiska metoder och finita element modellering för att bedöma krypskador i en
vätgasreformer. Vätgasreformern, som är tillverkad i Fe-Ni-Cr legeringar, togs ur drift och
undersöktes metallografiskt med hjälp av replikprovning och hårdhetsprovning samt med finita
element modellering av svetsar. En djupgående litteraturstudie utfördes för att öka förståelsen av kryp,
specifikt i Fe-Ni-Cr legeringar och även modellering av kryp generellt. Mikrostrukturen från utvalda
provbitar undersöktes och krypskador kartläggdes för att sedan jämföra med en krypanalys av
svetsarna där 100 000 timmars kryp simulerades. Krypanalysen resulterade i höga spänningar och
kryptöjningar upp till maximalt 0.95% i svetsgränserna vilket gav realistiska representationer av
töjningsdistributionen jämfört med metallografiska resultaten. Hårdhetsmätningar indikerade att ett
smalt område med förändrade mekaniska egenskaper fanns utmed svetsgränserna. Detta område, den
värmepåverkade zonen, var mest utsatt för krypskador med mikrosprickor uppemåt 2 mm i längd.
Kryptöjningar som erhölls från simuleringen gav inte en tillräckligt bra uppskattning av
kryptöjningarna – de krypskador som observerades motsvarar lokalt högre töjning. Slutsatsen är att en
materialmodell som tar hänsyn till tertiärkryp skulle i det här fallet ge en mer realistisk representation i
FEM för Fe-Ni-Cr legeringar.
Contents
1 Introduction .......................................................................................................................................... 1
1.1 Hydrogen reforming ...................................................................................................................... 2
2 Literature review .................................................................................................................................. 3
2.1 Creep ............................................................................................................................................. 3
2.1.1 Creep deformation mechanisms ............................................................................................. 4
2.1.2 Creep damage ......................................................................................................................... 5
2.1.3 Cavity nucleation .................................................................................................................... 5
2.1.4 Cavity growth ......................................................................................................................... 6
2.1.5 Replica testing ........................................................................................................................ 7
2.2 Modeling of creep ......................................................................................................................... 9
2.3 Materials in the reformer ............................................................................................................. 12
2.3.1 Base materials....................................................................................................................... 12
2.3.2 Welds .................................................................................................................................... 13
3 Method ............................................................................................................................................... 19
3.1 Metallography ............................................................................................................................. 19
3.1.1 Sample preparation ............................................................................................................... 19
3.1.2 Microscopy ........................................................................................................................... 21
3.1.3 Hardness test......................................................................................................................... 21
3.2 FEM methodology....................................................................................................................... 23
3.2.1 Assumptions, limitations and geometry ............................................................................... 23
3.2.2 Loads .................................................................................................................................... 24
3.2.3 Material models .................................................................................................................... 24
3.2.4 Boundary conditions and contacts ........................................................................................ 25
3.2.5 Mesh ..................................................................................................................................... 26
4 Results ................................................................................................................................................ 29
4.1 Metallography ............................................................................................................................. 29
4.1.1 Hardness test......................................................................................................................... 34
4.2 FEM ............................................................................................................................................. 36
5 Discussion and conclusions ................................................................................................................ 42
5.1 Metallography ............................................................................................................................. 42
5.1.2 Hardness measurement ......................................................................................................... 43
5.2 FEM ............................................................................................................................................. 44
5.3 Conclusions ................................................................................................................................. 45
6 Future work ........................................................................................................................................ 46
References ............................................................................................................................................. 47
Appendix A: Material and creep data .................................................................................................... 49
Alloy 800H ........................................................................................................................................ 49
20Cr32NiNb ...................................................................................................................................... 54
Alloy 617 ....................................................................................................................................... 54
2133 Mn ............................................................................................................................................ 55
Weldments ......................................................................................................................................... 56
Appendix B ........................................................................................................................................... 59
Alloy 800H .................................................................................................................................... 59
Alloy 617 ....................................................................................................................................... 60
2133 Mn ........................................................................................................................................ 60
1 Introduction
Significant creep damage was detected in high temperature components in a hydrogen reformer after 5
years, less than half of its design life. The damage was detected by use of non-destructive replica
testing at critical components with respect to creep. The degree of creep damage was considered to be
unacceptable for a further service period of 4 years. The level of the creep damage, microcracks, was
significantly higher than expected after 5 years in service. The recommended re-inspection interval for
microcracks is one year. Further service to the next revision in 4 years, could therefore not be
recommended.
More specifically the creep damage was detected on the surface of welds that connect pigtails to a
manifold and at the welds of the manifold itself. A typical design of the reformer is displayed in
Figure 1. The figure illustrates how the furnace tubes, catalyst tubes, are connected to collectors,
manifolds, by tubes called pigtails. These components were replaced with new versions with the same
design as the original ones. In both cases the components were fabricated by the materials Alloy
800H/HT and 20Cr32NiNb which are austenitic stainless steels with a high Chromium and Nickel
content.
The development of creep damage, in the form of creep cavitation to creep cracks, has not been
studied as much in the current alloys, as for ferritic steels. Particularly, work on the behavior of welds
is scarce. Furthermore, classification of creep damage and the recommendations of re-inspection
intervals that are associated with the damage classes are based on research on ferritic steels. Thus, a
better understanding of the creep behavior of welds of the Fe-Ni-Cr alloys is needed.
A thorough investigation of the unexpected detection of creep damage after only 5 years was
suggested as a master thesis project by Kiwa Inspecta in cooperation with Nynas AB. The purpose of
the present work is to analyze and assess creep damage on the damaged components. The goal is to
gain a better understanding of the development of creep damage in welds of Fe-Ni-Cr alloys and to be
able to assess different levels of creep damage in terms of re-inspection intervals. This will be
accomplished with metallographic methods via replica testing on the weld joints, examining the
microstructure at the surface as well as at cross sections, study the damage distribution and classify
different stages of creep damage. Selected components including welds will be modeled by the finite
element method and creep analyses will be performed in order to predict the creep behavior where the
results can be verified by the metallographical work. The available creep data for Alloy 800H,
1
20Cr32NiNb, weldments and the heat affected zone (HAZ) are reviewed and presented in this
document for use in the creep analysis. Different models for creep are also reviewed to find the most
suitable model for use in the finite element analysis.
Syngas can be further processed with water to produce more hydrogen gas in a second stage reaction.
This is done by cooling the gas to around 360 °C where an exothermic reaction occurs as
𝐶𝑂 + 𝐻2 𝑂 → 𝐶𝑂2 + 𝐻2 . (2)
Lastly the hydrogen gas is purified from ca 80% to 99.9% with pressure swing adsorption (PSA).
Challenges for service at high temperatures in reformers are often caused by catalyst tube failure or
failure of components in the outlet manifold system which includes the pigtails. The internal pressure
can vary between 2000-3500 kPa and the operation temperature ranges from 800 to 900 °C [1].
The combination of high temperature and pressure in piping makes creep the most important damage
mechanism to consider and design for. Excellent creep and rupture properties are therefore vital to the
lifetime of the reformer and reduces the likelihood of unplanned shutdowns, further reducing costs of
maintenance, replacement of components and cost of lost production.
2
2 Literature review
2.1 Creep
Creep can be defined as a time-dependent and continuous plastic deformation of materials over
extended periods under constant stress. The temperature range for creep to occur is for most materials
over 0.4𝑇𝑀 , where 𝑇𝑀 is the melting temperature. When a certain temperature and stress threshold has
been reached it only becomes a matter of time before it fails. Components in high temperature
environments are therefore designed to withstand creep for a certain period, typically 100 000 hours.
The time to failure from load initiation is termed rupture life.
The creep rate depends on temperature and stress. Increasing the temperature will lead to higher creep
rate and the same applies for an increase in stress. The creep rate for a certain material can be obtained
via creep testing to form a creep curve where creep strain is expressed as a function of time. Creep
tests are often conducted at constant tensile load and constant temperature. The creep curve is usually
characterized by three stages, a schematic creep curve is illustrated in Figure 2.
Creep starts with an instantaneous strain, 𝜀0 , on loading which typically only contains elastic strain.
The first stage is the primary creep which is associated with decreasing strain rate where the material
experiences strain (dislocation) hardening as the amount of free dislocations decrease and become less
mobile.
The secondary stage, also called steady state creep is for many applications the most important creep
parameter because it is most often the longest of the three stages and the easiest to model. Thermally
assisted recovery leads to annihilation of dislocations thereby lowering dislocation density and internal
energy of the material. New dislocations still form during this process because of the strain hardening
which leads to a balance between the two processes. The balance is more or less pronounced
depending on material, load and temperature. Therefore, the minimum creep rate is often used as a
constitutive parameter for the second stage. However, a constant creep rate is achieved in this stage for
long term applications.
3
The tertiary stage is the last stage which culminates in fracture. Voids nucleate, grow and coalesce in
the microstructure. This weakens the material and further increases creep rates. The voids along grain
boundaries form microcracks which grow and link together to form a macro crack. Finally, the creep
crack grows until rupture.
There are four creep deformation mechanisms, see Figure 3, which can be divided into two categories,
diffusion creep and dislocation creep. A higher temperature will increase the diffusion rate in the
material, further assisting Coble & Nabarro diffusion mechanisms. When stresses exceed the yield
stress, dislocation glide without the aid of diffusion takes over the role of plastic deformation. For a
given mechanism, actual creep rates are dependent on material composition, microstructure and grain
size. The largest grain size dependence is observed in the diffusional flow region with an increase in
grain size resulting in a decrease in creep rate.
Diffusional creep has been described by Nabarro-Herring and Coble. Nabarro-Herring creep occurs at
very high temperatures and low stresses. While Coble creep is suggested at (T < 0.7TM ) for low to
intermediate stresses. For both models, transport of vacancies is described. Atoms flow from regions
4
of local compressive stress to regions of local tensile stress while excess vacancies diffuse in the
opposite direction. This leads to the elongation of grains in the direction of the diffusional flow. This
process takes place either through the grains or along the grain boundaries [4].
Dislocation creep is more relevant for engineering applications and generally occur at temperatures
above 0.4TM for materials exposed to intermediate to high stresses. The mechanisms here are high
temperature and low temperature power-law creep. Deformation is controlled by motion of
dislocations through the crystal lattice and is accompanied by vacancy diffusion. Dislocations that
have been stopped in their path by a particle or point defect can overcome the obstacle with dislocation
climb. The dislocation climb is assisted by vacancy diffusion that can cause dislocations to climb out
of its glide plane and thus move around the obstructions.
5
Figure 5: Cavity nucleation mechanisms: a) cavitation at ledges due to sliding, b) nucleation from vacancy
concentration, c) nucleation due to dislocation pile-up, d) cavity nucleation from particle in conjunction with
mechanisms (a-c) [7].
6
controlled by the deformation rate of the surrounding material. If the surrounding material is relatively
soft, the rate of cavity growth would be controlled by diffusion. The zone ahead of the cavity is
elongating locally with diffusional growth and may disperse the load from the diffusion zone. The
uncavitated areas may thus constrain the areas that are elongating under additional influence of
cavitation [4,9]. This process is called constrained cavity growth, see Figure 6. Under these conditions,
the growth of voids can be linked to deformation which means that creep deformation can be used as a
parameter to estimate creep damage. In practice, most materials used in power plant and in
petrochemical applications operate under constrained cavity growth [10].
Figure 6: Uniform cavitation to the left and heterogeneous cavitation to the right [4].
7
Table 1: Creep damage class system.
Class 3, oriented cavitation of type K refers to cases with little damage outside the main lines of
damage. This is common in coarse grained microstructures such as the coarse grained HAZ. Type C
refers to cases with more diffusely oriented cavity formations, typically found in fine grained and
intercritical HAZ microstructures. gb stands for grain boundary, Lcmax is the total summed maximum
length of continuous cavity lines and Lmax is the maximum length of cracks. If there are two cracks,
they are counted as one if the distance between them is less than the length of the shorter crack.
8
2.2 Modeling of creep
It requires costly long-term creep testing to obtain results that can be used for constitutive equations
for the creep properties that are present at service conditions. This limits the available data for design
and life assessment. The test data available are even more scarce for welded joints that are usually the
weakest links of creep exposed structures. It is therefore of great interest to reliably predict and
extrapolate long term creep behavior from small sets of creep data.
The minimum creep rate based models do not take the primary and tertiary creep stages into account
and therefore predict lower strains. This prediction can give considerably lower strains if larger parts
of the creep strain occurs in the primary or tertiary stages of the material. Advanced models which
models the primary and tertiary stage need large creep data sets and creep curves to determine many of
the required material parameters.
In general, specific model equations are better at representing creep strain accumulation for a given
material in either the primary/secondary or the secondary/tertiary stages, although some models can be
applied for the entire creep process [11].
Norton’s law
One of the most commonly used functions is Norton’s law which describes secondary creep. The
steady state creep crate is
𝜀̇𝑠 = 𝐴𝜎 𝑛 , (3)
where 𝜎 is the tensile stress, 𝐴 the creep rate coefficient and n is the creep exponent which depends on
the deformation mechanism. The value of n is typically between 3-5 when power-law creep dominates
although higher values may be measured in practice for high stresses. For diffusional flow n=1. The
rate coefficient is a temperature dependent variable and can be determined from
𝑄𝑐
𝐴 = 𝐵 𝑒𝑥𝑝 (− ), (4)
𝑅𝑇
where 𝑄𝑐 is the activation energy for creep, R is the ideal gas constant, T the absolute temperature and
B is a constant. The reason for the popularity of this law is its simplicity in application to stress
analysis [10].
Larson-Miller parameter
The Larson-Miller parameter (LMP) is a widely used creep model and can be used for design of high
temperature components by extrapolating creep-stress rupture data.
The LMP is derived from Norton’s law and assumes constant stress over a variable temperature range.
By assuming that the secondary creep rate is inversely proportional to the rupture time, 𝑡𝑟 , a time-
temperature parameter is derived as
𝑃𝐿𝑀 = 𝑇(𝐶 + 𝑙𝑜𝑔 𝑡𝑟 ) , (5)
where T is temperature in Kelvin and C is a constant which varies from one alloy to another and is
related to the activation energy for creep. The LMP indicates that longer times at lower temperatures
are equivalent to shorter times at higher temperatures and makes it possible to plot all stress rupture
data on to a single master curve.
This method can lead to an overestimation of the rupture life because the apparent activation energy
𝑄𝑐 decreases when moving from short-term test data to long-term data [12,13].
9
Monkman-Grant relationship
Monkman and Grant (MG) found that for many metals and alloys, the relation between the secondary
creep rate 𝜀̇𝑠 and time to rupture 𝑡𝑟 can be expressed by the relation
𝜀̇𝑠𝑚 𝑡𝑟 = 𝐶𝑀𝐺 , (6)
where 𝐶𝑀𝐺 and m are constants that can be found from plotting rupture time versus secondary creep.
The exponent m is typically in the range 0,8–1,2 and can sometimes be set as m=1 so that
𝜀̇𝑠 𝑡𝑟 = 𝐶𝑀𝐺 . (7)
The MG equation can be used together with Norton’s law for extrapolation by obtaining the secondary
creep rate from the MG plot for a given rupture life. The creep rate can then be used to determine the
corresponding stress from a Norton equation plot [12].
The Wilshire equation
Wilshire’s equation is a modification of the power law equation, that aims to model the whole creep
curve. It is expressed as
𝜎 𝑄𝑐∗ 𝑢
𝑙𝑛 ( ) = −𝑘 [𝑡𝑟 𝑒𝑥𝑝 (− )] . (8)
𝜎𝑇𝑆 𝑅𝑇
The stress 𝜎 has been normalized by the materials ultimate tensile stress 𝜎𝑇𝑆 for the specific
temperature T. The constants k and u are obtained by fitting to the creep rupture data, 𝑡𝑟 is time to
rupture and 𝑄𝑐∗ is the apparent activation energy. The minimum creep rate 𝜀̇𝑚 and time to given strain
𝑡𝜀 can be obtained from the Wilshire equation by substituting 𝑡𝑟 in equation (8) along with the
constants k and u as follows
𝜎 𝑄𝑐∗ 𝑣
𝑙𝑛 ( ) = −𝑘1 [𝜀̇𝑚 𝑒𝑥𝑝 (− )] , (9)
𝜎𝑇𝑆 𝑅𝑇
𝜎 𝑄𝑐∗ 𝑤
𝑙𝑛 ( ) = −𝑘2 [𝑡𝜀 𝑒𝑥𝑝 (− )] . (10)
𝜎𝑇𝑆 𝑅𝑇
The application of this model has shown good agreements for a variety of pure metals and alloys. A
benefit is that data scatter is reduced by the normalization performed in the model. The scatter is
related to differences in creep properties due to alloying, heat treatments and product forms for the
tested material heats. The equation also gives rupture times that go towards zero when approaching the
ultimate tensile strength and times that go towards infinity when the stress approaches zero. It should
be noted that application of this model requires both creep rupture data and tensile test data [14].
Logistic Creep Strain Prediction (LCSP)
A relatively new creep strain model, the logistic creep strain prediction (LCSP) was developed to
avoid creep strain models with too many fitting constants. The LCSP model assumes that the full
creep strain curves at specified temperature and stress can be obtained from knowing only the time to
rupture and two material specific shape functions p(σ,T) and 𝑥0 (σ,T). The model is expressed as
𝑙𝑜𝑔(𝑡𝑟 ) + 𝐶
𝑙𝑜𝑔 𝑡𝜀 = 𝑝 −𝐶,
𝑙𝑜𝑔(𝜀 𝑐 ) (11)
1+( )
𝑥0
where 𝑥0 , C and p are fitting factors. The LCSP can be used for rupture predictions as the MG
equation, except that it is not limited to predictions using the minimum strain rate. The LCSP model is
robust and simple mainly because of relatively low number of constants to be fitted, and no complex
10
numerical operations are needed for fitting. The model has been shown to provide accurate predictions
at 10 000 and 100 000 h [15].
Kachanov-Rabotnov
The Kachanov-Rabotnov (K-R) model is the most widely used model to describe continuum creep
damage. It is relatively robust and is useful in modeling the tertiary stage of creep deformation and
damage.
The damage factor as outlined by Kachanov-Rabotnov is described as
𝐴
𝜔 =1− , (12)
𝐴0
where 𝜔 varies from 0 (no initial damage) to 1 (failure) [10]. The conventional K-R equations for
uniaxial creep are expressed as
𝐵𝜎 𝑛
𝜀̇ = , (13)
(1 − 𝜔)𝑣
𝐵𝜎 𝜒
𝜔̇ = , (14)
(1 − 𝜔)𝜙
where 𝜀̇ is the secondary creep rate, 𝜔̇ is the damage rate, B, n, v, 𝜒 and 𝜙 are material dependent
constants. The modified multiaxial K-R constitutive equations are as follows
𝑐 3 𝜎𝑒 𝑛 𝑠𝑖𝑗 𝑚
𝜀̇𝑖𝑗 = 𝐵[ ] 𝑡 , (15)
2 1 − 𝜔 𝜎𝑒
𝑀[𝛼𝜎1 + (1 − 𝛼)𝜎𝑒 ] 𝜒 𝑚
𝜔̇ = 𝑡 . (16)
(𝜙 + 1)(1 − 𝜔)𝜙
𝑐
Here 𝜀̇𝑖𝑗 is the creep strain, 𝑠𝑖𝑗 the stress deviator, 𝜎1 the maximum principal stress and 𝜎𝑒 the
effective stress. Variable 𝛼 is the tri-axial stress state parameter which value ranges from 0 to 1, 𝜔 is
the damage variable, B, M, n, m, 𝜒 and 𝜙 are material constants relating the minimum creep strain rate
to rupture behavior [16]. These equations can be implemented into finite element software such as
ABAQUS.
A downside to the K-R equations is that it contains many material dependent constants which need to
be determined. More constants may lead to higher potential of errors. The constants can be determined
by fitting of uniaxial creep test data [17]. This model has had limited application in industry because
of the high cost of acquiring the creep rupture data and the costs in terms of computer simulation time.
11
2.3 Materials in the reformer
2.3.1 Base materials
Alloy 800H
Alloy 800H was used to manufacture the pigtails and weldolets of the reformer. Alloy 800 was first
developed in the 1950’s and through further research and refinement of the chemical composition, the
alloys 800H and 800HT were developed which had better creep rupture properties. One of the
improvements made was coarser grains which increased the creep rupture strength, an ASTM grain
size of 5 or coarser is required. The limiting chemical compositions of the 800 series are displayed in
Table 2 [18].
Table 2: Limiting chemical composition of the Alloy 800 series.
Alloy 800H is widely used in high temperature environments in power plants or oil refineries in
components such as boilers, reformers and pyrolysis tubes. It is characterized by its high temperature
strength, good creep properties, resistance to different types of high-temperature corrosion and
metallurgical stability for long-term service at elevated temperatures.
It derives its strength mainly from gamma prime (𝛾′), an intermetallic compound. Precipitation of 𝛾′
contributes to the high-temperature strength and creep resistance of the material, with increasing
strength as the volume fraction of 𝛾′ increases. The oxidation resistance of alloy 800H is attributed to
high nickel and chromium content with the nickel contributing to good adhesion of the chromium
scale. Titanium is also added to act as a carbide- and nitride-former which encourages precipitation of
titanium nitrides and titanium carbides. Formation of titanium carbides takes carbon out of the solution
that could otherwise react with chromium to form chromium carbides. This prevents the process called
sensitization, which would make the steel susceptible to intergranular corrosion [19].
An extensive literature review has been performed to find mechanical, tensile and creep data on Alloy
800H for the relevant temperatures (800-900°C). A selection of the material data found is presented in
Appendix A.
12
20Cr32NiNb
The tee-piece, cone and manifold of the reformer are manufactured by the alloy 20Cr32NiNb which is
essentially the centrifugally cast equivalent of Alloy 800, with a few differences in chemical
composition. Titanium and aluminum are not included in its composition and it is instead alloyed with
approximately 1% of niobium, see Table 3. The niobium is added to form and stabilize carbides, hence
improving the creep properties of the material [1,20]. The material properties of this alloy are
presented in Appendix A.
Table 3: Chemical composition of 20Cr32NiNb.
Parameter 20Cr32NiNb
Carbon 0.10
Silicon 1.50
Manganese 1.50
Chromium 20.00
Nickel 32.00
Niobium 1.00
Iron Balance
2.3.2 Welds
Welds in the alloy 800-series
Components joined by welding must be heated to its melting point and cooled again rapidly under
conditions of restraint imposed by the geometry of the joint. This thermal cycle may therefore change
the original microstructure and properties of the metal in a region close to the weld. This region is
referred to as the heat-affected zone (HAZ).
Welded joints are more susceptible to creep because of stress concentrations at the joints and
differences in creep properties between the weld metal, HAZ and base metal. Different coefficients of
thermal expansion and heat conductivity introduce thermal stresses. In addition, system stresses may
be present due to the effects of thermal expansion, dead weight and internal pressure.
It has been recognized that Alloy 800H is susceptible to HAZ relaxation cracking (reheat cracking) in
the temperature range 500-760°C. This problem is related to residual stresses and the precipitation of
carbides in HAZ in that temperature range. A way to avoid reheat cracking is to apply a post weld heat
treatment for components that operate in the range 500-760°C. In this project, the residual stresses
from welding is not a problem because the operation temperature is much higher (around 860°C),
therefore the residual stress will relax naturally. Neither is carbide precipitation a problem since this
predominantly occurs in the temperature range 650-760°C [21].
Welding often gives rise to microstructural changes in the HAZ of austenitic alloys. One of these
changes may be grain growth although the growth is usually restricted in most cases and generally
much more restricted compared to ferritic steels. Precipitation of carbides and nitrides along the grain
boundary is a common metallurgical change for austenitic stainless steels. Melting along the grain
boundaries can also occur which can lead to segregation of impurity elements [22].
The microstructural changes in the alloy 800-series during welding may depend on heat input and the
weld metal used. It has been shown that grain growth occurs, and grain boundary thickening can be
seen due to precipitation of titanium [23].
Welds in investigated manifold and pigtails
Replica testing has previously been carried out on the reformer by investigating the surface of
components to detect creep damage. One of the tests was for reference where the components had only
13
been in service for one year. Another test was made after five years of service which showed signs of
creep voids and microcracks.
The replica tests were performed on welds at different locations on the reformer which can be seen in
Figure 6. The manifold tube connects to the pigtails via a weldolet, which means that each connection
of pigtail-manifold has two welds where one is weldolet to manifold and the other weldolet to pigtail.
The following welds were analyzed in both inspections:
Figure 6: A schematic side view of the hydrogen reformer, with positions of tested welds [1].
14
Figure 7: Microstructure at position S1, base metal, unetched. First inspection.
Figure 8: Microstructure at position S1, unetched. The fusion line with the HAZ to the left and weld metal to the
right. First inspection.
15
Figure 9: Microstructure at position S4. Base material, unetched. First inspection.
Figure 10: Microstructure at weld S4, unetched. Fusion line with weld metal at the top and HAZ at the bottom.
First inspection.
16
Figure 11: Microcrack along the HAZ at weld S4. Second inspection.
Figure 12: Microcracks across the fusion line between base metal and weld metal, at weld S3. Second
inspection.
17
Figure 13: Microcracks and cavities in the HAZ of weld S7. Second inspection.
18
3 Method
3.1 Metallography
Specimens were cut out from the decommissioned hydrogen reformer for metallographical
investigations. Welds that had been replica tested previously were chosen for examination: S3, S4, S5,
S6 and S7 (Figure 6) had been in service for a total of 6 years. Two earlier investigations have been
carried out on these welds at different operation times. The first was to establish a reference where no
creep had occurred at approximately one year of service. The second was after almost five years of
service which detected creep damages in the form of microcracks. This made the welds S3-S7 a
reasonable choice for further investigation of the progression of creep.
Ideally, four positions of the weld are used to map out the creep damage in the material. The received
cut-out samples of weld S3 included no indications of the positions used in the previous studies.
Therefore, only one random S3 sample was examined which corresponded to one cross-section and
the outer surface of the weld.
The welds corresponding to samples S4-S5 were not included in the FE-analysis because of limitations
in the model, therefore S4-S5 were also excluded from the metallographic investigation.
The pieces were then cut in the middle of the weldolet to separately prepare each sample, see Figure
15.
19
Figure 15: Separated samples of welds S6 and S7.
The specimens were prepared by grinding and polishing to create a flat and defect-free surface thus
making the microstructure observable for examination under a microscope. The grinding procedure
involves several stages with increasingly finer silicon carbide paper for each stage. The specimen is
then washed with water to prevent contamination, followed by alcohol. The samples were polished
using polishing discs covered with soft cloth and abrasive diamond particles. Surfaces that are
polished mechanically are susceptible to leftover debris or underlying plastic deformation. Etching or
electropolishing were used to remove such material and leave a defect-free surface.
An etchant was used to selectively visualize constituents of the microstructure such as grain
boundaries and precipitations. It creates contrast between different phases and grains depending on
grain orientation and composition. Additionally, grain boundaries became more visible for identifying
creep cavities. The etchant, 10% oxalic acid, was applied on the sample surface with a cotton bud, in
combination with an electrical current to accelerate the chemical process.
Electropolishing was in some samples used in addition to conventional mechanical polishing. It is an
electrolytical process which removes material from the sample surface and reduces surface roughness,
see Figure 16. Electrolyte A2 containing perchloric acid was used for the electropolishing step.
Figure 16: High current density along with electrolyte remove peaks from the surface being electropolished [25]
20
3.1.2 Microscopy
After sample preparation, a plastic film was placed on the sample surface which created a negative
image of the microstructure. The replicas were used to observe the microstructure in an optical
microscope. The samples were also observed directly, although it was found to be more challenging to
distinguish creep damage from grain boundaries, debris or other defects with certainty by the direct
examination. A useful feature of the replica image is that cavities and cracks are more easily
identifiable by small protrusions where pits in the sample surface become protrusions in the replica.
The samples were methodically examined at magnifications ranging from 25x to 400x to find and
identify microcracks and cavitation. Each sample surface was divided into five areas:
1. Base material adjacent to the weld (BM1)
2. Heat affected zone adjacent to the fusion boundary (HAZ1)
3. Weld material at the center of the weld (WM)
4. Heat affected zone adjacent to the fusion boundary (HAZ2)
5. Base material adjacent to the weld (BM2)
Two base materials were present in weld S6, 20Cr32NiNb in areas 1-2 and alloy 800H in areas 4-5.
The samples of weld S6 were also mapped in terms of how damage varies in the depth of the cross-
section.
The observed creep damage was classified according to Nordtest TR 302 [5], see Table 1. The
progression of creep in the reformer is mapped out by comparing the findings of this work with the
two earlier inspections. The first inspection had, as expected after less than one year in service, no
signs of creep damage. The results from the second inspection after nearly five years in service are
displayed in Table 4.
Table 4: Creep damage found in the second inspection.
N 1 1 1
S3 S 1 1 2a 1
W 1 2a 1 4b/2b 1
N 1 2a 1 1 1
S6
S 1 1 1 1 1
N 1 3b/4a 2a 1 1 Cavity chains and 0.3 mm microcracks
S7
S 1 1 1 1 1
21
Figure 17: The indentation and its measured diagonals.
The average diagonal length, d, is used to calculate the Vickers hardness, HV, according to equation
(17).
𝐹 𝑁
𝐻𝑉 = 0.1891 ⋅ ( 2
)[ ]. (17)
𝑑 𝑚𝑚2
Hardness was measured along two lines at two thicknesses in the cross-section of the weld, see Figure
18. Each indentation was made in a minimum of 25 micrometer intervals close to the fusion
boundaries and increased up to a maximum of 200 micrometer intervals across the center of the weld
metal region to reduce the amount of indentations. The force, F, used on the indenter was 4.9 N (0.5
kilogram force).
22
3.2 FEM methodology
A FE-analysis of the problem was performed in ANSYS Workbench 19.2. A creep analysis was
performed in the static structural module to estimate creep life and compare with the results of the
metallographic investigation. The analysis was carried out in two steps where all the loads were
applied in the first step. Creep was simulated in the second step for 100 000 hours.
The welds and pigtails of the middle group were prioritized over the two outer groups. Only the 10
innermost weldolets were modeled.
23
3.2.2 Loads
The load case considered is the operation conditions specified for the reformer. The operation
temperature of all components included in the model are specified as 860 °C and the operation
pressure is 2.48 MPa. The pressure was applied to the inside surface of the piping components.
Standard earth gravity was applied in the model to account for dead weight. Thermal expansion was
accounted for by increasing the temperature of all components from 22 °C to 860 °C.
where 𝐶3 =0 is used due to the constant temperature, thereby removing the need of a temperature
dependence parameter. Determination of the creep parameters are outlined in Appendix B.
Table 5: Material and creep parameters of the four material models.
Alloy 800H and 20Cr32NiNb with disabled creep parameters were implemented on components
where creep was not concerned to reduce simulation time, such as the outer pigtails, cone, liner and
manifold. Material assignments are displayed in Figure 20.
24
3.2.4 Boundary conditions and contacts
The gas that is transported into the reformer passes through the catalyst tubes connected to the top of
the pigtails. The catalyst tubes connection to the pigtails are situated in the ceiling which separates the
upper inlet system from the lower hot manifold system, see A of Figure 21. The upper connections of
the pigtails are therefore considered rigid and fixed.
Two variable springs are used to support the structure, each located at the midpoint between the
middle and the two outer groups of pigtails. They were implemented as spring contacts with a pre-load
of 4800 N and a spring coefficient of 22236 N/m, see B in Figure 21.
Rod supports are situated at either end of the manifold pipe, restraining them in the vertical direction,
see C of Figure 21.
Counterweights were used to decrease the load on the pigtails. Two counterweight stacks are
connected to a beam via rope and each beam supports 10 pigtails each. There is one supporting beam
for each contact surface, one for position A and one for position B, see Figure 22. The counterweight
supports are assumed to be a constant load that is divided equally among all pigtails. According to
drawings, the beam weighs 𝑚𝑏𝑒𝑎𝑚 = 38 𝑘𝑔 and each counterweight stack weighs 𝑚𝑐𝑤 = 181 𝑘𝑔.
The force acting on each contact surface of a pigtail is therefore calculated as
𝑔(2𝑚𝑐𝑤 − 𝑚𝑏𝑒𝑎𝑚 )
𝐹𝑝𝑖𝑔𝑡𝑎𝑖𝑙 = = 318 [N] .
10
25
Figure 22: Model of one pigtail and the location of applied counterweight forces.
Because the transfer line was excluded an assumption of the boundary conditions of the cone and liner
connecting to it was made. The cone and liner are assumed to be constrained in the vertical direction,
see D and E in Figure 21.
Contacts were implemented between manifold shells to manifold solids, liner shell to the cone and
pigtail beams to solids with the MPC (Multi-Point Constraint) formulation. This creates constraint
equations between the contacting surfaces which binds the bodies together.
3.2.5 Mesh
All pigtails were modeled with beam elements except for the regions closest to the weldolets. The
manifold was modeled with shell elements and transitioned to solid elements as it approached the tee
piece and the tee welds S1 and S3. The liner was also modeled with shell elements. The tee piece,
cone and welds were modeled with solid elements, see Figure 23.
26
Figure 23: Model of the reformer, where blue are modeled as solids, grey as shells and green as beam elements.
The mesh was refined to evaluate the welds and the areas close to the welds with respect to stresses
and creep strain. Element sizes were increased further away from the welds. The pipes were modelled
using hexahedral elements, with element sizings listed in Table 6.
Table 6: Element sizes of components.
A mesh convergence study was performed on a sub model of one weldolet. The local circumferential
stresses along a line with a length of 4 mm on the upper surface of the weldolet was retrieved. Element
sizes ranging from 1 mm to 4 mm were evaluated and plotted, see Figure 24. The jumps in stresses
between points are transitions between elements. Figure 24 indicates that an element size of 3 mm
may be satisfactory. Element size 4 mm has a difference of at most 5 MPa (16%) compared to the
other element sizes which is significant. The mesh study indicates that the element sizes used in Table
6 are not completely accurate, but a trade-off is made for shorter simulation time at the expense of
accuracy.
27
Circumferential stress
30
28
26
Stress [MPa]
24
1 mm
2 mm
22
3 mm
4 mm
20
18
16
0 0,5 1 1,5 2 2,5 3 3,5
Distance [mm]
Figure 24: Mesh convergence study of circumferential stresses along the surface of a weldolet.
28
4 Results
4.1 Metallography
Microcracks were observed in the cross-sections of S3, S6 and S7. Most of them were found in the
HAZ of the welds. The complete results are presented in Tables 7-8.
Table 7: Results from metallographical investigation, surface.
*High angle in the transition between weld and base material on the surface made polishing of HAZ1 difficult. Replica tests
in this position yielded no usable results.
Three microcracks with varying lengths between 0.35 mm to 0.49 mm were found in the cross-section
of weld S3, all located in HAZ2. The microcracks were found throughout the depth of the cross-
section and were found near both the outer layer and the inner layer. Chains of cavities were observed
in WM of the cross-section and outer surface. The BM1 and BM2 areas showed less signs of creep
damage with very few cavities sighted.
Microcracks were observed in HAZ2 in positions South and West of weld S6. Creep damage was
more prominent in Alloy 800H (HAZ2, BM2) compared to 20Cr32NiNb (HAZ1, BM1). Cavities were
located along the fusion boundary lines, resulting in damage classifications of 3a. No cavities were
observed in BM1, and few cavities were observed in BM2, although not enough to classify it above
damage class 1.
Weld S7 showed signs of isolated cavitation in areas HAZ1 and HAZ2 of the weld. One microcrack
was found in S7-N at HAZ1. Few cavities were observed in BM1 and BM2 but not enough to warrant
a damage class of 2a.
A selection of micrographs with observed creep damage is presented in Figures 25-33.
29
Figure 25: Microcrack in HAZ of S3, cross-section. WM to left and BM to right of fusion boundary line.
Damage class 4b.
Figure 26: Cavity chain in HAZ of S3, surface. Damage class 3b.
30
Figure 27: Cavity chain in WM of S3, surface. Damage class 3a.
Figure 28: Microcrack in WM of S6-W. Damage class 4b, close to a class 5 classification.
31
Figure 29: Microcrack in HAZ2 of S6-S. Damage class 4b.
32
Figure 31: Microcrack in HAZ1 of S7-N. Damage class 4b.
33
The creep damage in the cross-sections of weld S6 were mapped out with respect to depth of the pipe.
Microcracks were mostly located in the layer closest to the outer surface (blue), except for one
microcrack identified in one of the middle layers (green). The damage is relatively spread across the
thickness where cavity chains (damage class 3) were observed in all layers of the HAZ.
Figure 33: A cross-section of S6, etched to make fusion boundaries visible. Four layers of depths where the
highest damage identified at that depth is displayed as well as the most prevalent damage. The damage is
compiled from all four S6 cross-sections. Locations of microcracks are also marked.
34
450
400
350
Vickers Hardness
300
Upper
250
Lower
200
150
100
-550 -450 -350 -250 -150 -50 50 150 250 350 450 550
Distance [µm]
Figure 34: Vickers hardness measurements across weld S5-S. The x-axis shows distance from the middle of the
weld.
35
4.2 FEM
The maximum stress (697 MPa) occurred in one of the weldolets as seen in Figure 35. The maximum
creep strain found was 0.95%, see Figure 36. The stress and creep strain distributions are similar in all
weldolets.
Figure 35: Von mises stress distribution of the tee piece and welds, first load case. Stress is given in Pa.
Figure 36: Equivalent creep strain distribution of tee piece and welds after 100 000 h creep simulation.
36
The von Mises stresses for two cases are presented, the linear-elastic load case before creep and the
creep case where 100 000 hours has been simulated. In the linear-elastic case higher stresses are
present in the boundaries of the welds incurred by the difference in thermal expansion coefficients.
This also contributes to creep strains being higher in and around the weld boundaries.
Stresses and creep strains at the tee weld and weldolet corresponding to welds S3, S6 and S7 were
analyzed and are shown in Figures 37-41. In weld S6, the maximum stress was 674 MPa on the inside
surface of the weld with a maximum creep strain of 0.67%. The highest stress in weld S7 was 677
MPa and the maximum creep strain 0.9%, both of which were found in the northern part of the weld
boundary between weld material and base material of the weldolet. High stresses were found in the
weld materials with the highest occurring in the inside and outside surfaces.
Figure 37: Von Mises stress at welds S6-S7, before (left) and after (right) creep simulation. Observe that the
stress scales change depending on load case. Stress is given in Pa.
Figure 38: Von Mises stress with top-down view of cross-section of S6 and S7, before and after creep
simulation. Stress is given in Pa.
37
Figure 39: Equivalent creep strain, welds S6-S7.
In the tee piece and weld S3 specifically, creep strains were found to be significantly lower with a
maximum creep strain of 0.37%. Maximum stresses were found on the inside surface of the tee for
both load cases.
Figure 40: Von Mises stress at weld S3, before and after creep simulation. Stress is given in Pa.
38
Figure 41: Equivalent creep strain, cross-section of weld S3.
The effect of thermal expansion can clearly be seen in Figures 42-43 for circumferential and axial
stresses where distinct boundaries between welds have formed with stresses in opposite directions.
Figure 42: Circumferential stresses, cross-section of welds S6-S7. Before and after creep simulation. Stress is
given in Pa.
39
Figure 43: Axial stresses, cross-section of welds S6-S7. Before and after creep simulation. Stress is given in Pa.
The areas with the highest stresses were relaxed significantly in the first 1000 hours of creep
simulation and leveled out towards a steady-state. Creep showed similar behavior in high stress areas
where high creep strains were observed in the beginning and reached a steady-state of constant creep
rate when stresses relaxed. Von Mises stresses in the steady-state settled around 3-8 MPa in pigtails
and weldolets. Steady-state stresses in the tee piece and tee welds settled at significantly higher values
of around 7-13 MPa. Plots in Figures 44-45 illustrate relaxation for a node located in S7-N.
75
Maximum von Mises stress
70
65
60
55
50
Stress [MPa]
45
40
35
30
25
20
15
10
5
0
0 10000 20000 30000 40000 50000 60000 70000 80000 90000 100000
Time [h]
Figure 44: Maximum von Mises stress of a node in S7-N plotted versus simulation time.
40
0,0011
Maximum equivalent creep strain
0,001
0,0009
0,0008
Creep strain [1]
0,0007
0,0006
0,0005
0,0004
0,0003
0 10000 20000 30000 40000 50000 60000 70000 80000 90000 100000
Time [h]
Figure 45: Creep strain of a node in S7-N plotted versus the simulation time.
41
5 Discussion and conclusions
5.1 Metallography
Results show conclusively that the HAZ exhibits the most creep damage in form of cracks and cavity
chains compared to other areas. The weld materials also show signs of extensive creep damage while
the base material experience little to no creep damage.
The results in section 4.1 compared to results from previous reports in Table 4 show that creep damage
has progressed significantly in one year. This can be expected where creep in the tertiary stage has
shown to have significantly higher creep rates compared to the secondary creep stage. However,
knowing from the earlier report that microcracks had been found one can assume that creep had
already entered the tertiary stage at those positions.
The further exposure of the welds for one more year after the inspection clearly shows the progression
of creep damage. One year in the tertiary creep stage significantly increases the number of cavities and
cavity chains found. The microcracks were on average longer and more numerous. The only direct
comparison that could be made between inspections is the surface results of weld S3, see Table 9. The
cross-section of S3 compared to surface results show that the damage is spread in a similar fashion,
except for the three microcracks that were found in the cross-section sample.
Table 9: Creep damage progression in one year, surface of weld S3.
The second inspection showed asymmetrical distribution of damage in the welds where some positions
did not show any signs of advanced creep. It can be seen from the metallographic investigation that
this damage has propagated to be more evenly spread in the different positions of the weld. The
mapping of creep damage of weld S6 in Figure 33 showed that the creep damage was relatively evenly
spread with respect to the depth of the weld, with slightly higher degree of damage found in the layer
closest to the surface. It could therefore be concluded that creep damage found on the surface is a good
indication of the general state also of the inside of the material.
There was a difference in damage found between HAZ1 (20Cr32NiNb) and HAZ2 (Alloy 800H) in
weld S6 which may be due to the different base metals present at each end of the weld, see Table 10.
This affirms the findings of the literature review that alloy 20Cr32NiNb has higher creep strength
properties compared to Alloy 800H.
Table 10: Metallographical results of HAZ1 and HAZ2 of weld S6.
42
Weld S7 showed less creep damage overall compared to S3 and S6 where damage was only located in
the HAZ in the form of isolated cavitation. The damage distribution was largely symmetric except for
the microcrack found in the northern cross-section which coincides with the higher stresses that were
found in the northern part of the weld in the FEM-results.
Figure 46: Microstructural comparison between pigtail base metal (left) and weldolet base metal (right).
43
5.2 FEM
The highest creep strains were found in and around weld boundaries which validates the fact that the
welds are more susceptible to creep due to the local differences in material properties. This is also
confirmed by the metallographical results where most creep damage was found along fusion
boundaries.
The creep strains in weld S3 do not compare well with the creep damages that were found. A
maximum creep strain of 0.37% is relatively low for a material that exhibits significant creep damage.
Possible explanations for this discrepancy may be the approximated creep parameters in the material
model of alloy 2133 Mn leading to overestimation of its creep strength. Another explanation may be
the use of incorrect thermal expansion coefficient due to unavailable data.
The thermal expansion coefficient was proven to have a great effect, giving rise to sharply varying
stresses between weld and base metal, as could be seen in the stress plots. This was confirmed to be an
effect from the differing thermal expansion coefficients of the material models, by simulating an
identical load case with the same thermal coefficients on both weld and base metal, stress differences
across boundaries were greatly reduced. Having an incorrect thermal expansion coefficient can
therefore greatly affect the results of the creep simulation.
The highest creep strains found in welds S6 and S7 was 0.67% and 0.9% respectively. This is partly
due to the difference in thermal expansion coefficients between Alloy 800H and Alloy 617. Stresses
from deadweight simulation (the load case where only gravity was considered) showed higher stresses
in the weldolets compared to the tee-piece which also explain the higher stresses and strains found in
weldolets.
The outer and inner surfaces of welds S6-S7 showed the higher stresses which partly coincided with
the metallographical findings, where the layers closest to the outer surface of the weld were slightly
more affected by creep compared to the innermost layers. The maximum stress and strain at the
northern part of weld S7 compares well to the metallographical result where the northern cross-section
(S7-N) was found to have the highest creep damage of the four cross-sections investigated.
The results from the FE-analysis show relatively low creep strains considering the level of creep
damage found in the specimens. A maximum creep strain of 0.95% is not near a level that would be
expected from a material that exhibits microcracks. The data presented in Appendix B show that the
secondary stage for Alloy 800H exhibit creep strains around 0.5-1.5% and strains can easily exceed
5% when tertiary creep is accounted for. The tertiary stage onset occurs approximately 30-50% into
the total lifetime of the specimen indicating that the tertiary stage is a large part of Alloy 800H creep
life [28,29]. It can be concluded that the Norton creep model is insufficient in fully representing the
creep strains for Fe-Ni-Cr materials and a model including tertiary creep would make for a better
representation.
44
5.3 Conclusions
A summary of the conclusions that can be drawn from this thesis work:
• The HAZ of the welds was most affected by creep while base metals were least affected.
• The HAZ is relatively small for Fe-Ni-Cr alloys, approximately 50µm according to hardness tests.
• Creep damage was found throughout the cross-section of all welds.
• Replica testing the surface gives a representative view of the creep damage in the rest of the
material.
• Creep damage propagated and microcracks became more numerous in only one year. This
indicates that creep had entered tertiary stage.
• Alloy 800H has lower creep strength properties compared to 20Cr32NiNb. This could be
confirmed by the observed creep damage distributions.
• Higher stresses in weldolets due to larger differences in thermal expansion coefficients between
base and weld metal in comparison to the tee-piece welds
• Higher creep strains in welds because of relaxation of high thermal stresses.
• Modelling the welds by including the weld metal creep properties yielded a better representation
of creep strain distribution compared to modelling the base metal only.
• Creep model using Norton’s law obtained a maximum of 0.95% creep strain after 100 000 h creep
simulation. This estimate does not fully fall in line with the observed creep damage, which points
to significantly higher creep strains locally.
• A material model that considers tertiary creep would yield a more realistic representation in FEM
for Fe-Ni-Cr alloys.
45
6 Future work
From the results of the present Master Thesis the following future work can be suggested:
• Further metallographical investigation of the other welds in the reformer such as S1, S2, S4 and
S5.
• Creep testing of 20Cr32NiNb, weld metals that suit to Alloy 800H and 20Cr32NiNb and possibly
the HAZ to obtain needed creep data for the material models.
• Creep simulation using a material model that considers tertiary creep.
46
References
[1] Anon. Materials, Fabrication, and Repair Considerations for Hydrogen Reformer Furnace Outlet Pigtails
and Manifolds. API Technical Report 942-A – 1st edition, 2014.
[2] Northwood, D.O. and Shi, L. Recent Progress in the Modeling of High-Temperature Creep and Its
Application to Alloy Development. Journal of Materials Engineering and Performance, 1995 196. Vol. 4(2), p.
196-211.
[3] Abe, F. Creep-resistant steels. Cambridge, England: Woodhead Publishing Limited, 2008. ISBN: 1-84569-
401-5.
[4] Kassner, M. E. Fundamentals of creep in metals and alloys – 3rd edition. Waltham, Massachusetts:
Butterworth-Heinemann, 2015. ISBN: 0-08-099432-6
[5] Auerkari, P., Borggreen, K. and Salonen, J. Guidelines for evaluating in-service creep damage. VTT
Manufacturing Technology, 1995. NT Technical Report 302.
[6] Hevner, K. Effective integrity management programs for steam reformers. Inspecteering Journal, 2014. Vol.
20, Issue 6.
[7] Kassner, M.E. and Hayes, T.A. Creep cavitation in metals. International Journal of Plasticity, Pergamon,
2003. Vol. 19, p. 1715–1748.
[8] Cocks, A. C. F. and Ashby, M. F. On creep fracture by void growth. Progress in Materials Science, 1982,
Vol. 27, p. 189-244.
[9] Riedel, H. Fracture at high temperatures – 1st edition. Springer-Verlag Berlin Heidelberg, 1987. ISBN: 978-
3-642-82961-1.
[10] Mariott D. L. and Penny, R. K. Design for creep – 2th edition. London: Chapman & Hall, 1995. ISBN 94-
011-0561-8.
[11] Holdsworth, S.R., Askins, M., Baker, A., Gariboldi, E., Holmström, S., Klenk, A., Ringel, M.,
Merckling, G., Sandström, R., Schwienheer, M. and Spigarelli, S. Factors influencing creep model equation
selection. International Journal of Pressure Vessels and Piping, 2008. Vol. 85, p. 80–88.
[12] Ennis, P. J. and Zyrska-filemonowicz, A. Recent advances in creep-resistant steels for power plant
applications. Sadhana, 2003, Vol. 28, p. 709-730.
[13] Holmström, S. Engineering Tools for Robust Creep Modeling, VTT Publications 728, 2010. ISBN: 978-
951-38-7378-3.
[14] Williams, S. J., Bache, M. R. and Wilshire, B. Recent developments in analysis of high temperature creep
and creep fracture behaviour. Materials Science and Technology, 2010, Vol. 26. p. 1332-1337.
[15] Auerkari P. and Holmström, S. Robust prediction of full creep curves from minimal data and time to
rupture model. Energy Materials, Materials Science & Engineering for Energy Systems, 2006. Vol. 1, p. 249–
255.
[16] Tu, S., Segle, P. and Gong, J. Creep damage and fracture of weldments at high temperature. International
Journal of Pressure Vessels and Piping, 2004. Vol. 81, p. 199–209.
[17] Hyde, T. H., Becker, A.A., Song, Y. and Sun, W. Failure estimation of TIG butt-welded Inco718 sheets at
620C under creep and plasticity conditions. Computational Materials Science, 2006. Vol. 35, p. 35–41.
[18] Anon. INCOLOY alloy 800H & 800HT. Publication Number SMC-047, Special Metals Corporation, 2004.
[19] Anand, K., Arun Kumar, S., Tamilmannan, K., Sathiya, P. and Arivazhagan, B. Metallurgical
characterizations and mechanical properties on friction welding of Incoloy 800H joints. Journal of Materials
Research, 2016. Vol. 31, p. 2173-2185.
[20] Anon. Centralloy G 4859, Material data sheet. Schmidt + Clemens, 2009.
47
[21] Farrar, J.C.M. and Marshall, A.W. Matching consumables for type 800 alloys – Development history,
metallurgy and performance.
[22] Lippold, J.C. Welding metallurgy and weldability of stainless steels, 2005. ISBN: 1-61583-614-4.
[23] Lippold J.C. Investigation of heat affected zone hot cracking in Alloy 800. Supplement to the Welding
Journal, January 1983.
[24] Storesund, J. Personal communication, October 2018.
[25] Fuchs, J. Electropolishing. Clean Technologies Group, 2014. Retrieved 2019-03-01 from
https://techblog.ctgclean.com/2014/01/electropolishing/
[26] MatNavi, NIMS Creep Data Sheet. Data sheets on the elevated-temperature properties of iron based
21Cr-32Ni-Ti-Al Alloy for heat exchanger seamless tubes. National research institute for metals, Japan.
[27] Eto M., Muto Y., Nishi H. and Tachibana K. Creep Characteristics of Alloy 800H. Japan Atomic Energy
Research Institute, 1998.
[28] SS-EN 10302 Creep resisting steels, nickel and cobalt alloys. Swedish Standards Institute, 2008.
[29] Holdsworth, S.R. and Robertson, D.G. European Creep Collaborative Committee (ECCC) data sheets
2005.
[30] Centrifugally cast tubes. Coils and catalyst tubes for petrochemical applications. Engemasa, Edition:
November 2011.
[31] Anon. INCONEL alloy 617. Publication Number SMC-029, Special Metals Corporation, 2005.
[32] Ekaputra, I.M.W., Kim, W.G, Kim, M.H., Kim, Y.W. and Park. J.Y. Analysis of Creep Behavior of
Alloy 617 for Use of VHTR System. Procedia Materials Science, 2014. Vol. 3, p. 1285-1290.
[33] Nafari, M. and Salemi Golezani, A. Heat affected zone creep characterization of INCOLOY 800H by
means of small punch test. Engineering Failure Analysis, 2018. Vol. 94, p. 407-411.
48
Appendix A: Material and creep data
Alloy 800H
The Special Metals Corporation has provided a brochure for the Alloy 800 series, including
mechanical properties, physical properties and creep rupture curves. The elastic modulus, shear
modulus and poisson’s ratio for elevated temperatures are presented in Table A1. The data does not
cover up to 900°C. This will be complemented with another source which can be used to extrapolate
the elastic modulus at 860°C, the operational temperature of the hydrogen reformer.
Table A1: Mechanical properties at elevated temperatures for Alloy 800H [18].
Temperature [°C] Elastic Modulus [GPa] Shear Modulus [GPa] Poisson’s Ratio
700 150.1 54.3 0.381
800 141.3 50.7 0.394
Values of dynamic modulus of elasticity and creep rupture data were obtained for Alloy 800H from
the Swedish Standards Institute (SIS) and the data for the relevant temperatures is displayed in Table
A2-A3.
Table A2: Elastic modulus at elevated temperatures for Alloy 800H [28].
Table A3: Creep rupture data for Alloy 800H at various temperatures [28].
In 1991 many industrial and research companies from different countries in Europe founded the
European Creep Collaborative Committee (ECCC). The ECCC is an independent group of high
temperature plant manufacturers, plant operators and alloy producers formed to co-ordinate creep data
49
development activities throughout Europe. A creep data sheet of Alloy 800H from the ECCC has been
provided in Figure A1.
Figure A1: Creep data sheet for Alloy 800H from the ECCC [29].
A series of creep tests were carried out on Alloy 800H under constant load conditions by Eto et. al
[18]. The data is presented in Figures A2-A3 and a creep curve with the similar test conditions to the
load cases in this thesis is presented in Figure A4.
50
Figure A2: Creep data for Alloy 800H at various stresses and temperatures and prediction of minimum creep
strain rate [27].
Figure A3: Stress plotted against minimum creep strain rate for temperatures 700, 800, 850, 900 and 950°C
[27].
51
Figure A4: Creep curve for Alloy 800H, 38 MPa at 850 °C [27].
MatNavi has one of the largest-scaled materials databases in the world which is provided by the National
Institute for Materials Science (NIMS). The tests involve 6 different tube samples of Alloy 800H with differing
processing, grain sizes and reference codes fCA-fCF. NIMS creep data sheets are presented in Figures A5-A7.
Figure A5: Creep data for Alloy 800H tube samples fCA and fCB [26].
52
Figure A6: Creep data for Alloy 800H tube samples fCC and fCD [26].
Figure A7: Creep data for Alloy 800H tube samples fCE and fCF [26].
53
20Cr32NiNb
The elastic modulus and Poisson’s ratio of 20Cr32NiNb for elevated temperatures are presented in
Table A4 and the average creep rupture data is presented in Table A5.
Table A4: Mechanical properties at elevated temperatures for 20Cr32NiNb [22].
Alloy 617
The elastic modulus, shear modulus and Poisson’s ratio for Alloy 617 at elevated temperatures are
displayed in Table A6 and the stress dependence of minimum creep rate is shown in Figure A8.
Table A6: Mechanical properties at elevated temperatures for Alloy 617 [31].
Temperature [°C] Elastic modulus [GPa] Shear modulus [GPa] Poisson’s ratio
700 166 64 0.30
800 157 61 0.30
900 149 57 0.30
54
Figure A8: Minimum creep rate for Alloy 617 plotted against stress at 850, 900, 950 °C [32].
2133 Mn
This material has very little available mechanical data and creep properties at elevated temperatures.
However, it has an almost identical chemical composition to Alloy 800H. An assumption is made that
they have similar mechanical properties and it is assigned the same elastic modulus, Poisson’s ratio
and thermal expansion coefficient as Alloy 800H in the material model.
55
Weldments
A summary of the weld metals most commonly welded with alloy 800H can be viewed in Table A7
and their chemical compositions are displayed in Table A8 [1].
Table A7: Typical weld metals used in hydrogen reformers.
Weld
metal Ni C Mn Fe Si Co Cr Mo Nb+Ta
Inconel 59.0 0.1 max 5.0-9.5 10.0 1.0 max 0.12 13.0- - 1.0-2.5
182 min max max 17.0
IncoWeld 62.0 0.1 max 1.0-3.5 12.0 0.75 0.12 13.0- 0.5-2.5 0.5-3.0
A min max max max 17.0
Inconel 82 67.0 0.1 max 2.5-3.5 3.0 max 0.50 0.12 18.0- - 2.0-3.0
min max max 22.0
Inconel 55.0 0.1 max 0.1 max 7.0 max 0.75 0.12 20.0- 8.0-10.0 3.15-
112 min max max 23.0 4.15
Inconel 44.5 0.05- 1.0 max 3.0 max 1.0 max 10.0- 20.0- 8.0-10.0 -
617 0.15 15.0 24.0
Thermanit 33.0 0.20 2.3 ~41 0.20 - 22.0 - 1.7*
21/33
UTP A 33.0 0.12 4.5 ~40 0.30 - 21.0 - 1.2*
2133 Mn
*Nb only
Stress-rupture behavior of Alloy 800 weldments with the weld metals: Inconel 182, Inconel 112,
IncoWeld A and Inconel 82 were characterized. Most of these weldments experienced failure in the
56
weld metal rather than base metal or HAZ. Two cast alloys were included where the first is
20Cr32NiNb and the second cast alloy is the HT-modified which has the chemical composition
20Cr32Ni but with no niobium content and a higher carbon content of 0.34%. Additionally, the weld
metal Inconel 617 is evaluated because it is often recommended for welding Alloy 800H. The stress
rupture data for the weldments was extrapolated to 100 000 hours using the Larson-Miller parameter.
The stress-rupture plots for temperatures 816°C and 871°C are shown in Figures A9-A10 [1].
Figure A9: Stress-rupture comparison of weldments and alloys used in hydrogen reformers at 816°C [1].
57
Figure A10: Stress-rupture comparison of weldments and alloys used in hydrogen reformers at 871°C [1].
A relatively new method for testing creep can be performed with small punch tests. This is done by
using a puncher in the form of a ceramic ball and applying a load to the surface of the material for an
extended period in a heated furnace. The creep deflection is monitored, and a time-deflection curve is
obtained as can be seen in Figure A11. This study showed that the HAZ was the weakest part of the
weldment with a 20% reduction in life compared to base metal [33].
Figure A11: Small punch creep curves of a) base metal and b) HAZ at 700 °C for Alloy 800H.
58
Appendix B
Young’s modulus, thermal expansion coefficient and Poisson ratios for the materials were determined
by interpolating the value for temperature 860 °C, based on the given data in Appendix A.
The creep parameters were determined for Norton’s creep law expressed as
𝜀̇𝑐𝑟 = 𝐶1 𝜎 𝐶2 .
Parameters 𝐶1 and 𝐶2 are determined from two sets of creep data, where the creep strain, time and
stress are required. Integrating Norton’s creep law with with respect to time gives
𝜀 = 𝐶1 𝜎 𝐶2 𝑡 .
Alloy 800H
The stresses corresponding to a creep strain of 1% is retrieved for two periods 10 000 hours and
100 000 hours at the temperature 860 °C [28]. The two periods are expressed in seconds; 𝑡1 =
36 000 000 [s] and 𝑡2 = 360 000 000 [s]. This gives two equations
2𝐶
0.01 = 𝐶1 𝜎1%,10000 𝑡1 ,
𝐶
2
0.01 = 𝐶1 𝜎1%,100000 𝑡2 .
Dividing the two equations and making use of logarithm laws gives
log(10)
𝐶2 = = 3.49 ,
log(𝜎1%,10000 /𝜎1%,100000 )
where
𝜎1%,10000 = 17.6 𝑀𝑃𝑎 ,
20Cr32NiNb
The available data from Engemasa [30] only has creep rupture stresses. An approximation was made
to calculate the corresponding stresses for 1% creep strain due to the similar chemical composition to
Alloy 800H. The proportion between rupture stress (𝜎𝑟 ) and 1% creep stress (𝜎1% ) for alloy 800H is
𝜎1%,10000 𝜎1%,100000
= 1.28977 , = 1.37363
𝜎𝑟,10000 𝜎𝑟,100000
59
𝜎𝑟,10000 = 40.13 𝑀𝑃𝑎 ,
Alloy 617
Stresses corresponding to 1% creep strain data from Swedish standard institute [28] are retrieved,
where
𝜎1%,10000 = 27 𝑀𝑃𝑎 ,
𝜎1%,100000 = 16 𝑀𝑃𝑎 .
2133 Mn
Available creep data from a material with almost identical chemical composition, 800Nb weldments in
a 20Cr32NiNb alloy was used [21]. Stress-rupture data was extracted using the Larson-Miller
parameter, see Figure A12.
60
1133(17.9 + log 100000)
𝑃= = 25.95 ⟹ 𝜎𝑟,100000 ≈ 27 𝑀𝑃𝑎 .
1000
The approximation used for alloy 20Cr32NiNb is once again applied. The stresses for 1% creep strain
are
𝜎𝑟,10000
𝜎1%,10000 = = 29.07 𝑀𝑃𝑎 ,
1.28977
𝜎𝑟,100000
𝜎1%,100000 = = 19.66 𝑀𝑃𝑎 ,
1.37363
which gives the parameters
61