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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

in the new martensitic creep resistant steels.
Einfluss der Z-Phase auf Introduction Thus, the Z-phase transformation is a main
die langfristige Kriechstabilität cause for the lack of success to develop strong
von 9 bis 12 % Cr-Stählen martensitic steels with 12 % Cr for improved
Because of their combination of high creep
oxidation resistance.
and fatigue strength and moderate cost, the
Die langfristige Kriechstabilität der neuesten
Generation martensitischer 9 bis 12 % kriech- martensitic 9 to 12 % Cr steels are vital mate- In the present paper the Z-phase transforma-
fester Stähle basiert auf dem bekannten Grade rials for further increases in steam parameters tion is described in detail, and its influence on
91, d. h. auf der Stärkung durch die feinen MN- of fossil-fired steam power plants. Recently, the long-term stability of 9 to 12 % Cr steels
Nitride (V und Nb). Langzeit-Hochtemperatur- new stronger steels like the 9 % CrW steel is discussed. Finally, a possible way to over-
tests zeigen den Ersatz der MN-Nitride durch
die thermodynamisch stabileren Z-Phasen
Grade 92 for thick section boiler components come present difficulties to combine high Cr
(Cr(V,Nb)N) mit einem Verlust an Kriechfestig- and steam lines, and the 9 % CrCoB steels content with long-term microstructure stabil-
keit. Cr-Gehalte >10,5 % beschleunigen die FB2 and CB2 for large forgings and castings, ity is outlined.
Ausscheidung der Z-Phasen. Dies beschränkte have been introduced in commercial power
Bemühungen, einen martensitischen, kriech-
plant projects. These steels have enabled the
festen Stahl mit hohem Cr-Gehalt zum Schutz Microstructure and Creep Strength
vor Oxidation zu entwickeln. 9-%-Cr-Stähle construction of power plants with supercritical
of 9 to 12 % Cr Steels
werden offensichtlich nicht durch die Z-Phase live steam parameters up to 600 °C/300 bar
negativ beeinflusst. [1, 2]. The improved efficiency of these new
Die Untersuchung der Z-Phasen-Ausschei- plants compared to earlier sub-critical steam C re e p a nd Stre ngthe ning M e chani sm
dung hat zur Entwicklung eines 12-%-Cr-mar- plants (540 °C/180 bar) corresponds to a re-
tensitischen Versuchsstahls geführt, dessen The 9 to 12 % Cr steels have mainly tempered
Kriechfestigkeit durch die Z-Phase gewährleis- duction of some 30 % in specific CO2 emis-
martensite microstructures formed during a
tet wird. Derartige Stähle erlauben die Kombi- sion [3].
final normalising and tempering heat treat-
nation hoher Festigkeit bei gleichzeitig guter
Oxidationsbeständigkeit. Damit wird der Weg In order to further increase the steam param- ment, although for some compositions con-
frei für die weitere Entwicklung warmfester eters of steel-based power plants up to a target siderable amounts of ∆-ferrite may form in
martensitischer Stähle. 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
Authors 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
PhD Hilmar K. Danielsen new steels, due to results obtained by Fujita in
DTU Mechanical Engineering, Post. Doc. the late 1970s [6]. However, recent research
Lyngby/Denmark has demonstrated that the MN nitrides, (V,Nb)
N, may be replaced by the thermodynamically
Affiliated Professor John Hald
more stable Z-phases, Cr(V,Nb)N, which pre-
DONG Energy/Vattenfall/ cipitate as coarse particles and dissolve the 0,5 µm
DTU Mechanical Engineering
Senior Engineer
fine nitrides [7, 8]. This phase transformation
Lyngby/Denmark has been found to be a main cause for ob- Figure 1. Steel grade 92.Tempered martensite
served long-term microstructure instabilities microstructure.

68 VGB PowerTech 5/2009

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
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 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


Driving force in kJ/mol

Temperature in °C


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

70 VGB PowerTech 5/2009

Influence of Z-phase on Long-term Creep Stability

If the MN nitrides disappear from the micro-

structure during creep it has a clear negative
effect on the strength. The P122 steel contains Z-phase
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- Z-phase
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 0.2 µm 50 nm
steels can be increased above the level of steel
P92 by optimisation of chemical composition Figure 4. Large (a) and small (b) Z-phase particles co-existing in a 10.5 % Cr steel
and heat treatment. Figure 3 shows the effect after 43,000 hours at 600 °C.
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
Driving force in kJ/mol

strength are clear also in the short-term tests, 2.5
but they only remain in the long-term tests if 2.0
the nitrides are maintained in the steels. The 1.5
BH and MARBN steels have low Cr content 1
and good long-term stability based on MN 0.5
nitrides. In the NF12 steel with 11.6 % Cr the P92 P122 NF12 Z650
MN nitrides are dissolved by Z-phase precipi-
tation [7], and consequently the strength drops
below the level of steel P92. 50 nm
It is clear from above that the MN nitrides
play a crucial role in the long-term micro- 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
structure stability of the 9 to 12 % Cr steels, heat treatment 650 °C/3,000 hours.
and that the removal of MN nitrides by
Z-phase precipitation leads to a clear drop in N Z-phase grows by dissolution of the MN new stronger steels with Cr contents above
strength. The Cr content in the steels controls precipitates, which provide V, Nb and N, and 10.5 % have all failed. Further developments
the Z-phase precipitation, which explains the by picking up Cr from the steel matrix. In of 9 % Cr steels with low C or optimised
lack of success for all attempts to develop spite of the fast growth, observations of long- B and N contents seem to be able to increase
martensitic creep resistant steels with Cr con- term exposed specimens always reveal both the long-term strength close to the target
tent higher than 10.5 % combined with high large and small Z-phase particles, F i g u r e 4 . level of 100 MPa for rupture after 105 hours at
long-term strength based on MN nitrides. This indicates that the nucleation of Z-phase 650 °C, ( 3). However, if such steels are to be
is slow and continuous, and thus the nuclea- used at service temperatures significantly
tion process should be regarded as rate higher than 600 °C it is necessary to apply
The Z-phase Precipitation Process controlling for the Z-phase transformation some sort of surface coating for oxidation
[24, 25]. The fact that Z-phase grows fast protection. This will lead to significantly in-
Even though the Cr(V,Nb)N Z-phase is ther- means that even in early stages of the trans- creased production cost and open a wealth of
modynamically the most stable nitride in 9 to formation large Z-phase particles can be ob- new possibilities for component failure and
12 % Cr steels alloyed with V, Nb and N served in the microstructure even though only risks for unexpected plant outages.
it seems quite difficult for it to nucleate. a very limited part of the MN population has Basically, the whole story about the detrimen-
Z-phase has never been observed in any of the been dissolved. Thus, an observation of a few tal effects of Z-phase has so far not left much
steels directly after tempering for a few hours large Z-phase particles in the steel microstruc- hope for success in the development of more
in the normal range 650 to 800 °C. Even in ture is not necessarily alarming for the creep efficient environmentally friendly power
the high Cr steels, where Z-phase forms most stability. Instead, attention should be focused plants based on improved high-temperature
rapidly, widespread Z-phase formation has on the rate of removal of the MN nitrides by steels. Consequently, recent developments
only been observed after quite long exposure measurements of their number density. like the European AD700 project [26, 27]
times of 1000 hours or more at 650 °C. Ex- have focused on a jump in steam temperature
perimental studies of Z-phase TTP diagrams up to 700 °C based on the use of very expen-
indicate that the fastest precipitation happens New Strategy for Alloy Development sive Nickel-based alloys like the 617, 625 and
at 650 °C [23]. 263 for steam lines, boiler components and
Once a Z-phase has nucleated it can grow fast, As mentioned, the studies of Z-phase precipi- turbines.
and large Z-phase particles can be observed tation in modern MN strengthened 9 to 12 % However, the developed understanding and
after relatively short exposures. The Cr(V,Nb) Cr steels explains why the attempts to develop modelling of Z-phase might open an entirely

VGB PowerTech 5/2009 71

Influence of Z-phase on Long-term Creep Stability

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.

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-
As tempered Nucleation Growth 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.
NbN 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
Figure 6. T
 he principle in accelerated Z-phase transformation is to avoid growth of Z-phase, process has led to the design of experimental
and thereby obtaining a stable fine distribution of nitrides which contributes to
creep strength. 12 % Cr martensitic steels strengthened by
Z-phase. Such steels may again enable the
new path for alloy development of high Cr steels. And at the same time the necessary combination of high strength and oxidation
martensitic steels based on the strategy: If you oxidation resistance would be obtained, which resistance in the same alloy. This opens a new
can’t beat them, join them. would again make it possible to combine pathway for further alloy development of the
strength and oxidation resistance in the same heat resistant martensitic steels.
alloy. If successful, the 12 % Cr martensitic steels
Z-phase Strengthened 12 % Cr Steels strengthened by Z-phase could enable the
Scrutinising the thermodynamic model sug-
construction of low cost USC power plants
gests that Z-phases based on CrNbN or CrTaN
As mentioned, calculations of the driving with steam parameters approaching 325 bar/
could possibly serve as strengthening agents,
force for Z-phase precipitation allows estima- 650 °C entirely based on steels.
as the driving force for their formation are
tions of the precipitation rate of the Z-phase. significantly higher compared to that of CrVN
The obvious strategy is then to minimise or Cr(V,Nb)N. Finally, calculations of coars- Acknowledgments
the driving force in order to delay the harmful ening rates based on thermodynamic data
Z-phase precipitation to very long times (be- made as described in [14], indicate coarsening
yond 300,000 hours), where it would have no stabilities of the Z-phases similar to or better Financial support from the power utilities
influence on the long-term stability of the than the MN nitrides. DONG Energy and Vattenfall GN is kindly
steel in practical use. Unfortunately, as shown acknowledged. The described work is part
this leads to limitations on the Cr content, Ongoing work at the TU Denmark to study of the European COST 536 ACCEPT action
which prevent attaining the necessary oxida- possibilities to use the Z-phase as a strength- and the Swedish CROX project supported
tion resistance of the alloy. ening agent has included design and produc- by the SSF (Stiftelsen för Strategisk
tion of a number of experimental high Cr Forskning) and the VGB Research Foundation
However, if the Z-phase itself could be pro-
martensitic steels with high driving force for (Project no. 266).
voked to precipitate very quickly in a fine dis-
Z-phase precipitation, Figure 5 . So far the ex-
tribution, which could provide particle
perimental steels have demonstrated that it is
strengthening, then the steel could be expect- References
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edi­ti­on (In­fo­Ex­pert) and edu­ca­ti­on li­cen­se on re­quest Pos­tal Co­de Ci­ty Count­ry
(pho­ne: +49 201 8128-200).
* Plus VAT. Pho­ne/Fax
Annual update 1) Euro 150.–; 2) Euro 350.–
The update has to be ordered annually. Da­te 1st Sig­na­tu­re

Re­turn by fax or in business envelope with window to Can­cel­la­ti­on: This or­der may be can­cel­led wi­thin 14 days. A no­ti­ce must be
sent to to VGB Po­wer­Tech Ser­vice GmbH wi­thin this pe­ri­od. The deadline
VGB Po­wer­Tech Ser­vice GmbH will be observed by due mailing. I ag­ree to the terms with my 2nd sig­na­tu­re.
Fax No. +49 201 8128-329
In­fo­Ex­pert Da­te 2nd Sig­na­tu­re

DVD-VGB_2008-e.indd 1 25.11.2008 13:19:05

VGB Po­wer­Tech –
The generation of electricity and the disposal of heat is in all parts of the world a central
topic of technology, economy, politics and daily live. Experts are responsible for the
construction and operation of power plants, their development and monitoring as well
as for various tasks in connection with service and management.
The technical journal VGB PowerTech is a competent and internationally accepted
publication for power plant engineering. It appears with 11 bilingual issues
(German/English) annually. VGB PowerTech informs with technical/scientific papers and
up-to-date news on all important questions of electricity and heat generation.
VGB PowerTech appears with VGB PowerTech Service GmbH, publishing house of
technical-scientific publications.
VGB PowerTech e.V., the German and European technical association, is the publisher.

VGB PowerTech DVD 1990 to 2008:

Digitalised technical papers of VGB Kraftwerkstechnik and VGB PowerTech.
You find the competent technical know-how from 19 years on more than 10,000 pages
VGB Kraftwerkstechnik (German issues until 2000) and the international technical
journal VGB PowerTech (as of 2001) with:
– More than 2300 technical papers,
– All documents in PDF-format (up to the year 2000 for technical reasons as b/w scan),
– Convenient search function in all papers as full-text search and/or deliberate search
for authors and documents titles,
– Navigate quickly to the desired papers with a few mouse clicks.
The VGB PowerTech-DVD is available as single license or multi-user license for
companies, research institutions and authorities.
The single license can be ordered by form and by post/fax or use our online shop
A quotation for a multi-user license is made on demand.
You can bring up to date your DVD annually with the VGB PowerTech update.
The update has to be ordered annually.

Your contact at VGB PowerTech Service GmbH,

Jürgen Zimander, Phone: +49 201 8128-200, E-Mail:

VGB Po­wer­Tech Ser­vice GmbH

P.O. Box 10 39 32
45039 Es­sen


DVD-VGB_2008-e.indd 2 25.11.2008 13:19:05

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