Influence of Z-phase on Long-term Creep Stability
Influence of Z-phase on Long-term Creep Stability
of Martensitic 9 to 12 % Cr Steels
Hilmar K. Danielsen and John Hald
Kurzfassung
Einfluss der Z-Phase auf
die langfristige Kriechstabilität
von 9 bis 12 % Cr-Stählen
Die langfristige Kriechstabilität der neuesten
Generation martensitischer 9 bis 12 % kriech-
fester Stähle basiert auf dem bekannten Grade
91, d. h. auf der Stärkung durch die feinen MN-
Nitride (V und Nb). Langzeit-Hochtemperatur-
tests zeigen den Ersatz der MN-Nitride durch
die thermodynamisch stabileren Z-Phasen
(Cr(V,Nb)N) mit einem Verlust an Kriechfestig-
keit. Cr-Gehalte >10,5 % beschleunigen die
Ausscheidung der Z-Phasen. Dies beschränkte
Bemühungen, einen martensitischen, kriech-
festen Stahl mit hohem Cr-Gehalt zum Schutz
vor Oxidation zu entwickeln. 9-%-Cr-Stähle
werden offensichtlich nicht durch die Z-Phase
negativ beeinflusst.
Die Untersuchung der Z-Phasen-Ausschei-
dung hat zur Entwicklung eines 12-%-Cr-mar-
tensitischen Versuchsstahls geführt, dessen
Kriechfestigkeit durch die Z-Phase gewährleis-
tet wird. Derartige Stähle erlauben die Kombi-
nation hoher Festigkeit bei gleichzeitig guter
Oxidationsbeständigkeit. Damit wird der Weg
frei für die weitere Entwicklung warmfester
martensitischer Stähle.
Authors
PhD Hilmar K. Danielsen
DTU Mechanical Engineering, Post. Doc.
Lyngby/Denmark
Affiliated Professor John Hald
DONG Energy/Vattenfall/
DTU Mechanical Engineering
Senior Engineer
Lyngby/Denmark
68 VGB PowerTech 5/2009
in the new martensitic creep resistant steels.
Introduction Thus, the Z-phase transformation is a main
cause for the lack of success to develop strong
martensitic steels with 12 % Cr for improved
Because of their combination of high creep
oxidation resistance.
and fatigue strength and moderate cost, the
martensitic 9 to 12 % Cr steels are vital mate- In the present paper the Z-phase transforma-
rials for further increases in steam parameters tion is described in detail, and its influence on
of fossil-fired steam power plants. Recently, the long-term stability of 9 to 12 % Cr steels
new stronger steels like the 9 % CrW steel is discussed. Finally, a possible way to over-
Grade 92 for thick section boiler components come present difficulties to combine high Cr
and steam lines, and the 9 % CrCoB steels content with long-term microstructure stabil-
FB2 and CB2 for large forgings and castings, ity is outlined.
have been introduced in commercial power
plant projects. These steels have enabled the
Microstructure and Creep Strength
construction of power plants with supercritical
of 9 to 12 % Cr Steels
live steam parameters up to 600 °C/300 bar
[1, 2]. The improved efficiency of these new
plants compared to earlier sub-critical steam C re e p a nd Stre ngthe ning M e chani sm
plants (540 °C/180 bar) corresponds to a re-
The 9 to 12 % Cr steels have mainly tempered
duction of some 30 % in specific CO2 emis-
martensite microstructures formed during a
sion [3].
final normalising and tempering heat treat-
In order to further increase the steam param- ment, although for some compositions con-
eters of steel-based power plants up to a target siderable amounts of ∆-ferrite may form in
value of 650 °C/325 bar it is necessary to the microstructure. The tempered martensite
double the creep strength compared with consists of prior austenite grains separated by
Grade 92, and at the same time the resistance high angle grain boundaries. These grains are
against steam oxidation must be improved. If subdivided by high angle boundaries into
the oxidation protection is to be achieved blocks of martensite laths [9]. After tempering
through alloy additions instead of surface the blocks consist of sub-grains with an aver-
coatings, it is necessary to increase the Chro- age width of 0.3 to 0.5 μm separated by low
mium content in the steels from 9 % to 12 % angle boundaries. The dislocation density of
[4]. However, so far all such attempts to make the tempered martensite is high (in the order
stronger 12 % Cr steels have failed because of 1014 m–2), F i g u r e 1 .
the high chromium content introduced severe
The technically interesting stress and temper-
microstructure instabilities in the tested steels,
ature ranges for creep testing and service ex-
which led to breakdowns in long-term creep
strength [5].
Since the well-known steel Grade 91, the
long-term creep strength of the new genera-
tion of martensitic creep resistant steels relies
strongly on particle strengthening by fine
MN nitrides based on V and Nb. Additions of
about 0.15 to 0.25 % V, 0.04 to 0.08 % Nb and
0.02 to 0.07 % N are common to all of the
new steels, due to results obtained by Fujita in
the late 1970s [6]. However, recent research
has demonstrated that the MN nitrides, (V,Nb)
N, may be replaced by the thermodynamically
more stable Z-phases, Cr(V,Nb)N, which pre-
cipitate as coarse particles and dissolve the 0,5 µm
fine nitrides [7, 8]. This phase transformation
has been found to be a main cause for ob- Figure 1. Steel grade 92.Tempered martensite
served long-term microstructure instabilities microstructure.
 Influence of Z-phase on Long-term Creep Stability

Table 1. C
 r content of steels compared to experimentally found Z-phase contents. Recently, the authors made systematic studies
Steels are ranked according to Z-phase content. of Z-phase content in a number of 9 to 12 %
Cr steels, which rely on MN strengthening
Steel type Cr content, wt % Exposure Observed Z-phase quantity
[7]. Both commercial and experimental grades
P91 8.30 8,000 h / 650 °C Very low were investigated after exposure to creep, and
E911 8.61 10,000 h / 650 °C Low a clear correlation between the Cr content of
P92 8.96 31,000 h / 650 °C Low
the steels and the observed Z-phase quantity
was found, T a b l e 1 . Comparisons with
P122 11.0 10,000 h / 650 °C Medium creep testing on a number of the investigated
AXM 10.48 43,000 h / 600 °C Medium steels show that for Cr contents above 10.5 %
FN5 11.20 8,000 h / 650 °C Medium the strongly accelerated Z-phase precipitation
leads to a breakdown in long-term creep
HCM12 12.20 85.000 h / 585 °C Medium
strength. In steels with Cr contents below 9 %
VM12 11.61 16,000 h / 625 °C High Z-phase precipitation is so slow that they are
TB12M 11.33 10,000 h / 650 °C High largely unaffected up to very long testing
times at 600 to 650 °C [7].
T122 12.20 12,000 h / 660 °C High
NF12 11.60 17,000 h / 650 °C High Results from detailed studies of the mentioned
steels were used to develop a thermodynamic
equilibrium model of the Z-phase [18]. This
Table 2. C
 hemical composition and heat treatment of 9 to 12 % Cr steels discussed. model has demonstrated that Z-phase Cr(V,
Wt % bal. Fe. [19 to 22]. Nb)N is thermodynamically the most stable
nitride in all 9 to 12 % Cr steels containing V,
9Cr3W3Co 9Cr3W3CoB P92 P122 BH Steel NF12 MARBN
Nb and N ( F i g u r e 2 ). This means that
C 0.078 0.077 0.11 0.12 0.03 0.085 0.078 Z-phase should eventually form in all of the
Si 0.31 0.29 0.10 0.24 0.36 0.25 0.31 new generation 9 to 12 % Cr steels with po-
Mn 0.50 0.51 0.45 0.63 0.49 0.44 0.49 tentially detrimental effects on their creep
strength. However, as seen from Table 1, large
Cr 8.94 8.95 8.82 10.73 9.12 11.60 8.88 differences in Z-phase precipitation rate has
Mo – – 0.47 0.38 0.15 0.14 – been found, which seem to correlate well with
W 2.94 2.93 1.87 1.97 2.40 2.68 2.85 similarly observed large differences in the rate
of breakdown in creep strength.
Ni – – 0.17 0.36 0.01 0.17 –
Co 3.03 3.03 – – 1.8 2.48 3.00 The thermodynamic equilibrium model can
be used to estimate Z-phase precipitation rates
Cu – – – 0.97 – – – by calculations of the thermodynamic driving
V 0.19 0.19 0.19 0.22 0.20 0.20 0.20 force for the Z-phase precipitation. This driv-
Nb 0.050 0.050 0.06 0.056 0.05 0.08 0.051 ing force is the difference in free energy be-
tween the steel with all MN nitrides present
N 0.002 0.001 0.047 0.072 0.050 0.045 0.0079
and the steel with only Z-phase present, and it
B – 0.0048 0.0020 0.0039 0.0060 0.0026 0.0135 can give indications of the influence of chem-
Norm 1050 °C 1050 °C 1070°C 1050 °C 1050 °C 1100 °C 1150 °C ical composition on the Z-phase precipitation
rate. Such calculations clearly demonstrate
Temp 790 °C 790 °C 780 °C 770 °C 780 °C 760 °C 770 °C
that Cr is the most influential element for the
Z-phase driving force, Figure 2. Further it is
posure of the 9 to 12 % Cr steels are 250 MPa termetallic Laves phases Fe2(Mo,W) and the
found that elements like C or Co, which are
to 20 MPa at 500 °C to 700 °C. In these rang- MN nitrides (V,Nb)N. The MN nitrides pre-
not included in the Z-phase, also affect its
es the main creep mechanism in the steels is cipitate in high number densities as very fine
driving force. C forms as M23C6, which ties
dislocation creep. This leads to glide of free particles, which are much more stable against
up Cr and thus effectively lowers its content,
dislocations and migration of sub-grain coarsening than the other precipitates [14]. As
while Co reduces the Cr affinity in the matrix,
boundaries during creep, resulting in a reduc- such they contribute significantly to long-
thus encouraging it to form as Z-phase. Re-
tion of the dislocation density and growth of term precipitation hardening in the steels. Bo-
sults by Strang and Vodarek indicated a strong
sub-grains [10, 11]. These deformation proc- ron addition to the steels may stabilise the
accelerating effect of Ni content on Z-phase
esses can be delayed by precipitate particles, M23C6 carbides, especially near the prior
precipitation [8]. However, the model studies
which pin dislocations and sub-grain bounda- austenite grain boundaries. [15, 16].
provide no support to any effect of Ni content
ries.
on the precipitation rate of the Z-phase.
B e h av i o u r a n d T h e r m o d y n a m i c
A number of different precipitates can be
Modelling of Z-phase in 9 to 12 % E ff e c t o f M N a n d Z - p h a s e
found in the 9 to 12 % Cr steels. Depending
Cr Steels on Long-term Creep Strength
on their particle hardening effect and stability
against coarsening or dissolution during long- Z-phase Cr(V,Nb)N was first found in a mar- The quantitative effect of MN precipitates on
term exposure the precipitates determine the tensitic 11 % Cr steel by Schnabel et.al. in long-term creep strength of modern 9 to 12 %
microstructure stability of the steels. Precipi- 1987 [17]. In 1996 Vodarek and Strang Cr steels can be demonstrated by comparisons
tate hardening should be regarded as the most realised that Z-phase precipitation could ex- of selected steels, which all have fully tem-
significant creep strengthening mechanism to plain observed sigmoidal creep behaviour in pered martensite microstructures free of
obtain high long-term creep strength in the older 12CrMoVNb steels, since the Z-phase ∆-ferrite. The chemical composition and heat
9 to 12 % Cr steels [12, 13]. The most useful precipitates as coarse particles and dissolves treatment of the discussed steels are shown in
precipitates are the Cr carbides M23C6, the in- fine MN nitride particles [8]. Ta b l e 2 and results of creep rupture tests at

VGB PowerTech 5/2009 69

Influence of Z-phase on Long-term Creep Stability

1400 2.7
Ferrite

1200
2.4
Ferrite

Driving force in kJ/mol

Austenite+MX
+MX
1000
Temperature in °C

2.1
Ferrite+Z+M2X
800

1.8
600 Ferrite+Z

400 1.5
0 4 8 12 16 20 8 9 10 11 12 13
Cr (wt%) wt% chromium

2.7 2.7

2.4 2.4
Driving force in kJ/mol

Driving force in kJ/mol

2.1 2.1

1.8 1.8

1.5 1.5
0.00 0.05 0.10 0.15 0.20 0.0 0.5 1.0 1.5 2.0 2.5 3.0
wt% carbon wt% cobalt

Figure 2. a) Thermodynamic stability of Z-phase in 0.06Nb-0.21V-0.06N steels.

b-d) Driving force for Z-phase precipitation in 0.10C-0.06Nb-0.21V-0.06N steel at 650 °C. (All in wt %, bal. Fe.)

300 300
9Cr3W3Co P92
9Cr3W3CoB NF12
P122 MARBN
200 P92 200 BH steel
BH cont.
Stress in MPa

Stress in MPa

100 100
90 90
80 80
70 70
60 60

50 50
10 100 1000 10000 100000 10 100 1000 10000 100000
Time to rupture in h Time to rupture in h

Figure 3. Creep rupture tests at 650 °C of the 9 to 12 % Cr steels discussed [19 to 22].

650 °C are shown in F i g u r e 3 . The 9Cr3W-
3CoVNb and 9Cr3W3CoVNbB steels have
very low Nitrogen content and consequently
they contain only M23C6 carbides and inter-
metallic Fe2W Laves phase, but no MN ni-
trides. The 9Cr3W3CoVNbB steel is stabi-
lised by Boron addition. As such these two
steels represent baseline strength levels of the
modern 9 % Cr steels without nitrides. The rupture strength. Above 2,000 hours the Bo-
P92 steel contains fine (V,Nb)N MN nitrides ron addition in steels 9Cr3W3CoVNbB and
in addition to M23C6 carbides, Fe2W Laves P92 is effective, and above 10,000 hours the
phases and Boron stabilisation. Because of MN nitrides in steel P92 are effective to stabi-
the low Cr content the nitrides in steel P92 are lise the microstructure and increase the
stable against Z-phase precipitation up to strength. All three steels have similar heat
long-term creep exposures. In short-term tests treatment.
up to 2,000 hours the three steels have similar

70 VGB PowerTech 5/2009


If the MN nitrides disappear from the micro-
structure during creep it has a clear negative
effect on the strength. The P122 steel contains
MN nitrides, M23C6 carbides, Fe2W Laves
phases and Boron similar to the P92 steel, but
due to the high Cr-content of 10.7 %, strong
precipitation of Cr(V,Nb)N Z-phase occurs
above 10,000 hours and this dissolves the MN
nitrides [7]. Consequently, the strength of the
P122 steel stays at the level of the 9Cr3W-
3CoVNbB steel, which is without nitrogen,
but has a similar Boron content as P122
(Figure 3).
The creep rupture strength of the 9 to 12 % Cr
steels can be increased above the level of steel
P92 by optimisation of chemical composition
and heat treatment. Figure 3 shows the effect
on high W steels of a) lowering the carbon
content (steel BH); b) increasing the normal-
ising temperature (steel NF12) and c) increas-
ing normalising temperature together with an
optimisation of the Boron and Nitrogen con-
tents (steel MARBN). Here, the effects on
strength are clear also in the short-term tests,
but they only remain in the long-term tests if
the nitrides are maintained in the steels. The
BH and MARBN steels have low Cr content
and good long-term stability based on MN
nitrides. In the NF12 steel with 11.6 % Cr the
MN nitrides are dissolved by Z-phase precipi-
tation [7], and consequently the strength drops
below the level of steel P92.
It is clear from above that the MN nitrides
play a crucial role in the long-term micro-
structure stability of the 9 to 12 % Cr steels,
and that the removal of MN nitrides by
Z-phase precipitation leads to a clear drop in
strength. The Cr content in the steels controls
the Z-phase precipitation, which explains the
lack of success for all attempts to develop
martensitic creep resistant steels with Cr con-
tent higher than 10.5 % combined with high
long-term strength based on MN nitrides.
The Z-phase Precipitation Process
Even though the Cr(V,Nb)N Z-phase is ther-
modynamically the most stable nitride in 9 to
12 % Cr steels alloyed with V, Nb and N
it seems quite difficult for it to nucleate.
Z-phase has never been observed in any of the
steels directly after tempering for a few hours
in the normal range 650 to 800 °C. Even in
the high Cr steels, where Z-phase forms most
rapidly, widespread Z-phase formation has
only been observed after quite long exposure
times of 1000 hours or more at 650 °C. Ex-
perimental studies of Z-phase TTP diagrams
indicate that the fastest precipitation happens
at 650 °C [23].
Once a Z-phase has nucleated it can grow fast,
and large Z-phase particles can be observed
after relatively short exposures. The Cr(V,Nb)
VGB PowerTech 5/2009 71
Z-phase
0.2 µm
Figure 4. Large (a) and small (b) Z-phase particles co-existing in a 10.5 % Cr steel
after 43,000 hours at 600 °C.
4.0
3.5
Driving force in kJ/mol
3.0
2.5
2.0
1.5
1
0.5
0
P92 P122 NF12
Figure 5. a) Driving force for Z-phase precipitation in 9 to 12 % Cr steels. Z650 is an
experimental 12 % Cr steel. b) Very fine Z-phase particles in steel Z650 after
heat treatment 650 °C/3,000 hours.
N Z-phase grows by dissolution of the MN
precipitates, which provide V, Nb and N, and
by picking up Cr from the steel matrix. In
spite of the fast growth, observations of long-
term exposed specimens always reveal both
large and small Z-phase particles, F i g u r e 4 .
This indicates that the nucleation of Z-phase
is slow and continuous, and thus the nuclea-
tion process should be regarded as rate
controlling for the Z-phase transformation
[24, 25]. The fact that Z-phase grows fast
means that even in early stages of the trans-
formation large Z-phase particles can be ob-
served in the microstructure even though only
a very limited part of the MN population has
been dissolved. Thus, an observation of a few
large Z-phase particles in the steel microstruc-
ture is not necessarily alarming for the creep
stability. Instead, attention should be focused
on the rate of removal of the MN nitrides by
measurements of their number density.
New Strategy for Alloy Development
As mentioned, the studies of Z-phase precipi-
tation in modern MN strengthened 9 to 12 %
Cr steels explains why the attempts to develop
Influence of Z-phase on Long-term Creep Stability
Z-phase
Z-phase
Z-phase
50 nm
Z650
50 nm
new stronger steels with Cr contents above
10.5 % have all failed. Further developments
of 9 % Cr steels with low C or optimised
B and N contents seem to be able to increase
the long-term strength close to the target
level of 100 MPa for rupture after 105 hours at
650 °C, ( 3). However, if such steels are to be
used at service temperatures significantly
higher than 600 °C it is necessary to apply
some sort of surface coating for oxidation
protection. This will lead to significantly in-
creased production cost and open a wealth of
new possibilities for component failure and
risks for unexpected plant outages.
Basically, the whole story about the detrimen-
tal effects of Z-phase has so far not left much
hope for success in the development of more
efficient environmentally friendly power
plants based on improved high-temperature
steels. Consequently, recent developments
like the European AD700 project [26, 27]
have focused on a jump in steam temperature
up to 700 °C based on the use of very expen-
sive Nickel-based alloys like the 617, 625 and
263 for steam lines, boiler components and
turbines.
However, the developed understanding and
modelling of Z-phase might open an entirely
Influence of Z-phase on Long-term Creep Stability
VN
As tempered Nucleation
NbN
Figure 6. T
 he principle in accelerated Z-phase transformation is to avoid growth of Z-phase,
and thereby obtaining a stable fine distribution of nitrides which contributes to
creep strength.
new path for alloy development of high Cr
martensitic steels based on the strategy: If you
can’t beat them, join them.
Z-phase Strengthened 12 % Cr Steels
As mentioned, calculations of the driving
force for Z-phase precipitation allows estima-
tions of the precipitation rate of the Z-phase.
The obvious strategy is then to minimise
the driving force in order to delay the harmful
Z-phase precipitation to very long times (be-
yond 300,000 hours), where it would have no
influence on the long-term stability of the
steel in practical use. Unfortunately, as shown
this leads to limitations on the Cr content,
which prevent attaining the necessary oxida-
tion resistance of the alloy.
However, if the Z-phase itself could be pro-
voked to precipitate very quickly in a fine dis-
tribution, which could provide particle
strengthening, then the steel could be expect-
ed to be immune to dissolution of its strength-
ening nitrides. Inspections of the developed
thermodynamic model show that the neces-
sary steps to accelerate Z-phase precipitation
involve an increase of the Cr-content to the
highest possible level. Further, the Carbon
content should be low in order to accelerate
the Z-phase formation together with additions
of Cobalt, which would also limit delta ferrite.
The high Cr content would then be turned
from being the main cause of instability into
being a necessary beneficial element to secure
the long-term microstructure stability of the
72 VGB PowerTech 5/2009
CrVN
Growth
CrNbN
steels. And at the same time the necessary
oxidation resistance would be obtained, which
would again make it possible to combine
strength and oxidation resistance in the same
alloy.
Scrutinising the thermodynamic model sug-
gests that Z-phases based on CrNbN or CrTaN
could possibly serve as strengthening agents,
as the driving force for their formation are
significantly higher compared to that of CrVN
or Cr(V,Nb)N. Finally, calculations of coars-
ening rates based on thermodynamic data
made as described in [14], indicate coarsening
stabilities of the Z-phases similar to or better
than the MN nitrides.
Ongoing work at the TU Denmark to study
possibilities to use the Z-phase as a strength-
ening agent has included design and produc-
tion of a number of experimental high Cr
martensitic steels with high driving force for
Z-phase precipitation, Figure 5 . So far the ex-
perimental steels have demonstrated that it is
indeed possible to produce a stable distribu-
tion of fine Z-phase particles in 12 % Cr mar-
tensitic steels.
Fine NbN or TaN nitrides, which are precipi-
tated during tempering, transform to a fine
distribution of Z-phase in relatively short time
at 650 °C. The strong acceleration of the
Z-phase transformation means that each indi-
vidual MN nitride transforms quickly into one
Z-phase. Thereby the detrimental Z-phase
growth process involving MN dissolution is
effectively suppressed. The result is a fine dis-
tribution of Z-phase particles, ( F i g u r e 6 ),
which seem to be very stable against coarsen-
ing. Ongoing creep tests will clarify if the
high targets of a doubling of creep strength
compared to steel Grade 92 can be achieved.
Summary
The long-term creep strength of the new gen-
eration of martensitic creep resistant 9 to
12 % Cr steels since the well-known steel
Grade 91 relies strongly on particle strength-
ening by fine MN nitrides based on V and Nb.
The MN nitrides may be replaced by the ther-
modynamically more stable Z-phases,
Cr(V,Nb)N causing a breakdown in long-term
creep strength.
Thermodynamic modelling show that Cr
contents above 10.5 % strongly accelerates
Z-phase precipitation and the breakdown in
creep strength. This explains the lack of suc-
cess for all attempts to develop martensitic
creep resistant steels with high Cr content for
oxidation protection.
Careful control of the Z-phase precipitation
process has led to the design of experimental
12 % Cr martensitic steels strengthened by
Z-phase. Such steels may again enable the
combination of high strength and oxidation
resistance in the same alloy. This opens a new
pathway for further alloy development of the
heat resistant martensitic steels.
If successful, the 12 % Cr martensitic steels
strengthened by Z-phase could enable the
construction of low cost USC power plants
with steam parameters approaching 325 bar/
650 °C entirely based on steels.
Acknowledgments
Financial support from the power utilities
DONG Energy and Vattenfall GN is kindly
acknowledged. The described work is part
of the European COST 536 ACCEPT action
and the Swedish CROX project supported
by the SSF (Stiftelsen för Strategisk
Forskning) and the VGB Research Foundation
(Project no. 266).
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[24] H. K. Danielsen: “Z-phase in 9-12%Cr steels”
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Forschungszentrum Jülich. h
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 VGB Po­wer­Tech – www.vgb.org
The generation of electricity and the disposal of heat is in all parts of the world a central
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