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Abstract:
The increasing demand of oil and gas has led to exploit oil fields and gas reservoirs with an increased content of
contaminants. Reserves of natural gas are abundant, but about 40% of the fields contain high concentration of hydrogen
sulfide, carbon dioxide and chlorides. This makes such fields difficult to exploit and need a complex system for refining
with a significant associated cost. Such fields are referred as Sour and are found in many areas of the world but the
Middle East and Central Asia hold the largest volumes.
Design of equipment for such harsh environments, especially high pressure centrifugal compressor needs a deep
knowledge of equation of state of gas mixture, material science and manufacturing technologies.
Material selection is performed taking into account several parameters like minimum design temperature, wet and dry
conditions of different compressor stages, partial pressure of hydrogen sulfide, carbon dioxide and the amount of other
contaminants like halides, elemental sulphur, mercury, etc…
This paper describes the design approach and the material selection for centrifugal compressors operating in extreme
sour service. Particular attention will be dedicated to the influence of chlorides on material stress corrosion cracking
resistance.
Secondly a description of GE Oil&Gas manufacturing technologies experience is provided by reporting standard special
processes and new trends in manufacturing technologies.
1
1 – INTRODUCTION
The increasing demand for oil and gas has led to exploit oil fields and gas reservoirs with an increased content of
contaminants. Reserves of natural gas are abundant, but about 40% of the fields contain high concentration of hydrogen
sulfide, carbon dioxide and chlorides. This makes such fields difficult to exploit and, as a consequence, it needs a
complex system for refining with significant associated costs. Such fields are referred to as “Sour” and are found in many
areas of the world. Middle East and Central Asia are presently some of the places of preeminent interest to the
International Oil Company due the large volumes, in spite of the high concentration of contaminants found in the oil
fields.
In order to maximize the exploitation of these oil reservoirs, it is necessary to safely handle the associated gases
containing high percentage of aggressive components which cannot be dispersed in the atmosphere.
The design of equipment for such harsh environments, especially high pressure centrifugal compressor, requires deep
knowledge of thermodynamics of gas mixture, material science and manufacturing technologies.
Material selection is performed taking into account several parameters such as minimum design temperature, wet and
dry conditions at the different compressor stages, partial pressure of hydrogen sulfide & carbon dioxide and the amount
of other contaminants such as halides, elemental sulphur, mercury, etc…
GE Oil & Gas is the company that has gained more experience in reinjection of sour gas at the pressures required by
Middle East and Central Asia wells.
This paper describes the design approach, the material selection and the manufacturing technologies for centrifugal
compressors operating in extreme sour service. Particular attention will be dedicated to the influence of halides on
material stress corrosion cracking resistance.
2
2 – DESIGN
Operating in extreme sour and acid environment requires specific attention from design standpoint. To make a proper
design and material selection, one has to precisely understand the steady and transient operating surrounding
environment as well as the stress load acting on each one of the components.
The compressor components that deserve a specific attention are the ones in contact with the process gas. In short, it
corresponds to (figure 1):
- Pressure containing components, such as casing and covers
- Rotating components, such as shaft, impellers, balance drum and spacers
- Internal static components, such as inner casing and diaphragms
- Sealing components, such as Dry Gas Seals (DGS) and gaskets
From a general standpoint, the basis of design criteria for material selection is to follow NACE guidelines. Risk of failure
is a combination of several factors: aggressiveness of the gas, wetness & stress distribution.
3
From a thermodynamics standpoint, the pressure rise across the compression stages leads to a temperature rise, which
contributes to move away from the dew curve. In other words, the operating margin vs. dew curve (figure 2) at each
compression stage increases while moving from suction to discharge area of the compressor.
Obviously, such analysis shall not be restricted to stabilized operations, but it should also look to the complete expected
operating envelope of the machine, from surge to choke area. Thanks to the high compression happening on surge side,
this area is generally the most favorable, whereas the choke area is the one which is traditionally the design case.
Stress Distribution
Finally, the stress distribution of the different components is also a key factor for the material selection. As a general
guideline, static components (which usually operate at no more than 200MPa) are less sensitive compared to rotating
components (where impellers typically operate above 400-500MPa). Regarding Stress Corrosion Cracking, the tensile
component of the stress is the critical one, which drives the failure mechanism by opening up the crack. This tensile
stress can be locally amplified by geometrical singularities, like stress concentration factors coming from pitting, for
example. Among other possible examples, one can consider the removal of keys at the bore diameter of the impeller in
order to avoid their resulting stress concentration factor.
When selecting Corrosion-Resistant Alloys, one shall make sure that the stress load of the component will not exceed
the threshold stress of the material in the given environment. For a given application with specific aggressiveness, in
case it is not already covered by field references operating at similar stress level & in environment of at least equivalent
aggressiveness, and if the threshold stress of the material is not known in that environment, then specific laboratory
testing might be required to properly qualify a material selection.
It is understood that the detailed determination of all these key parameters (aggressiveness of the gas, wetness & stress
distribution) across the whole life of the plant (including transients) is not an easy task. Considering the risk linked to a
release of such lethal gas to the surrounding atmosphere, in case the gas conditions with contaminants, in steady state
and in upset conditions, cannot be formally guaranteed by the process equipment of the end user, it could be
recommended not to select CRA material (Corrosion Resistance Alloys) for pressure-containing parts in such harsh
environment, in view of their susceptibility to rapid cracking when used out of their design envelope. In such cases,
other solutions, such as bulk carbon steel protected by a surface overlay, may be preferable to minimize uncertainties
on namely casing and cover.
In a similar way, the sealing between covers and casing is an area of significant interest. Potential leakages shall be
directed to a safe area (flare, typically) and a pressurized barrier based on Nitrogen is advisable to remove any (or at
least greatly dilute) any kind of leakage towards atmosphere.
4
3 – MATERIAL APPROACH
The purpose of this section is to cover the fundamentals aspects of material selection for compressors operating in the
natural gas refining. Natural gas is formed primarily of methane, but it can also include ethane, propane, butane and
pentane plus other contaminants as shown in the table 1, that outlines the typical makeup of natural gas before it is
refined. Natural gas processing consists of separating all of the various hydrocarbons and fluids from the pure methane,
thus generating different blend of gas.
For the purpose of this paper and to select material it is useful to classify the process gas service according to the
following rules :
- Sweet service
- Sour service
- Acid gas
Among the several rules for material selection for centrifugal compressors, corrosion is particular important for service
in harsh environment.
There are several corrosion phenomena, but for the sake of simplicity and for the subject of this paper, the following
types are the most relevant:
- General corrosion – an even attack of the surface of the material
- Pitting corrosion – an uneven localized attack
- Stress corrosion cracking (SCC and CSCC)
It must be highlighted that corrosion phenomena listed above can only take place if condensed water is present, that
acts as electrolyte for electrochemical process. For this reason, from now on and if not differently specified, the material
selection criteria and consideration given, are done assuming wet gas conditions. Another important condition that must
be addressed is represented by pressurized stops (SOP). In this case temperature drops and pressure in the different
stages become the same. This is normally one of the most severe conditions for material selection since it implies a wet
gas at high partial pressure of harsh gases. SOP are transient conditions limited in time and therefore can be addressed
with a different approach (time dependent) and be solved with different solution like coatings.
Sweet Gas
Sweet Service refers to a gas containing hydrocarbon with wet carbon dioxide (CO2), in sweet service, the failure risk is
due to CO2, the condensed water is acidified by carbonic acid that promotes the surface metal loss by general corrosion.
Carbon or low alloy steels can be used if corrosion rate is below acceptable limit. The rate of corrosion depends on
partial pressure of CO2 and service temperature.
If general corrosion rate of material is unacceptable, then stainless steels have to be selected for this service.
5
There are several types of stainless steels:
- Austenitic
- Ferritic
- Martensitic
- Duplex or Superduplex
Martensitic Stainless steels are the most important category of material used in centrifugal compressor for rotor and
stator parts. Martensitic stainless steels are characterized by a good corrosion behavior and outstanding mechanical
properties.
The following material types are normally used depending on design and environment requirements:
- 12 % Chromium steel like AISI 410 (UNS S41000)
- Low Carbon Chromium Nickel Steel like ASTM A182 F6NM (UNS S41500)
- Precipitation Hardening like 17-4 PH (UNS S17400) or 15-5 PH (UNS S15500)
Sour Gas
The sour service is characterized by hydrocarbons with wet hydrogen sulphide (H2S) where the pH2S is higher than
0.0030 bar. This value is valid for carbon and low alloy steels. NACE MR0175/ISO 15156-1 doesn’t define a minimum
pH2S limit for corrosion resistant alloys (CRAs), because this limit is a function also of acidity of the solution (pH) and the
values can be lower than the one defined for carbon and low alloy steels.
Two main mechanisms of metal cracking are considered with wet H2S:
Sulphide Stress Cracking (SSC)
Hydrogen Induced Cracking (HIC)
In general the mechanism involves the diffusion in the metal of hydrogen atoms generated by corrosion. SSC can occur
only if the following three conditions are verified [1]:
• Tensile stress (residual and/or applied)
• H2S + condensed water
• Material prone to SSC damage
Contaminants such as halides, arsenic (As), antimony and cyanides (CN-) act as catalyst, increasing the concentration of
hydrogen atoms on surface and by preventing their recombination in hydrogen molecules making SSC more severe [2].
The HIC is generated by the following conditions:
• Atomic hydrogen source (i.e. H2S) and condensed water
• Material prone to HIC damage
HIC occurs when atomic hydrogen generated by the corrosion reaction diffuses through the steel and then accumulates
as molecular hydrogen in correspondence of non-metallic inclusion, particularly when these inclusions have been
flattened by rolling operations, or at bands of segregation or perlite. The local H2 pressure generates cracks and blisters
6
on the material. If only H2S is present forged carbon or low alloy steels with a controlled cleanliness (low level of non
metallic inclusion), are suitable for service. The maximum SSC susceptibility occurs around ambient temperature [3].
Acid Gas
Gas containing hydrocarbon, CO2 and H2S represents a complex environment for material selection. The presence of
contaminants to this system such as chlorides, makes the material selection a very important design phase in order to
guarantee reliability and sustainability of products.
The material selection is therefore based on a three dimensional space governed by partial pressure of H2S (p(H2S)), pH
(mainly function of CO2), and chlorides (and/or other halides) content, as schematically represented in figure 3.
To approach the material selection in this three dimensional space is useful to define boundaries for the different class
of materials. In addition to the environmental criteria, the material selection must take into consideration the
manufacturability, the availability on market of the raw material and last but not least, the cost.
Due to the higher mechanical and corrosion properties, superduplex find application in turbomachinery environments,
allowing the production of both stator and rotating component in a design space ranging from -100°C to 200°C. Within
these limitations, and when the wet environment becomes critical (normally at 0÷90°C in Centrifugal compressor), the
superduplex offers the higher performances in Chlorides rich environments superseding most of the other stainless
steel classes.
Moreover, as reported in international standard NACE MR0175, duplex and superduplex materials can withstand in Sour
environment a maximum hydrogen sulfide partial pressure of respectively 0,1 bar and 0,2 bar (any pH and chloride
concentration up to 232°C). In general duplex stainless steels should not be used at temperature above 250-325°C.
7
Particular care is needed in the production and machining of duplex class materials due to embrittlement caused by
precipitation of detrimental phases during slow cooling (i.e. thick section of parts). High alloyed duplex and superduplex
are more susceptible to these phenomena, due to high content of second-phase forming elements, and requires
additional care.
GE O&G has extensively produced centrifugal pump components (casings and impellers) using duplex/superduplex
stainless steel. As said, because of their ferritic-austenitic microstructure, this class of alloy shows significant issues in
obtaining the required machining tolerances in terms of planarity, concentricity and dimension. Residual stresses
released during machining, non “linear” elastic behavior of material, hardening during cutting operations requires
specific machining methods with multiple part setting during raw and finishing operations. Typical machining
parameters are in the range of 100÷150 m/min for the cutting speed and of 0.2÷0.25 mm/rev for the feed rate using
carbide tools.
The face centered cubic structure (fcc) of austenite is characterized by a low diffusivity and high solubility of hydrogen.
The fcc structure acts as a trap for hydrogen, improving the resistance of the material to SCC.
The volume fraction of reverted austenite depends, as said previously by chemistry and heat treatment sequence. These
are not the only parameters since the volume fraction strongly depends on presence of retained austenite in the ingot
or bar, prior forging. It is therefore extremely important to control the steel production method in order to minimize the
presence of retained austenite and delta ferrite as result of the material segregation. It is also very important the
morphology of the reverted austenite. This aspect has been extensively studied by several authors [9-17]. The reverted
austenite can be as thin islands between martensite lath or as globular grains at prior austenite grains or within
martensite needles.
The influence of volume fraction of reverted austenite and its morphology has been extensively studied in GE Oil & Gas
in order to maximize material performance in terms of corrosion, stress corrosion and mechanical properties.
X4CrNi16-4 represents the best stainless steel inside the GE Oil & Gas portfolio.
95% AYS tests were passed standard NACE TM0177 – method A tests with 1 bar H2S up to 1 g/l NaCl. Several high
pressure tests was also performed demonstrating the suitability of X4CrNi16-4 up to 10 bar H2S (100 ppm chlorides) and
4 bar H2S (600 ppm chlorides).
As a term of comparison GE Oil & Gas performed an extensive characterization of F6NM (UNS S41500) resulting in
limiting the use of this material at pH2S at 0.1 bar or even lower depending on chlorides content.
9
X4CrNi16-4 shows a threshold stress in solution A method A according to TM-0177 higher than AISI 410 and 17-4 PH.
Many GE Oil & Gas compressors for sour gas service are equipped and are successfully running with stator and rotor
parts made of X4CrNi16-4 and it is validate by field experience as shown in figure 4.
The high strength of IN 718 and IN 625M makes this material a perfect solution for rotating components like impellers,
that are preferably manufactured in a single piece construction to avoid any kind of joint (welding or brazing) that could
reduce the rotating speed capability. GE has developed and applied several methods to manufacture single piece
impellers, one of each optimized for a certain range of dimension and shape.
Bi-dimensional impellers are characterized by low flow coefficients resulting in narrow gas passages that are created by
die sink EDM (Electro Discharge Machining). A set of graphite tools is generally used to access the impeller from inducer
(gas inlet side) and exducer (gas outlet side) performing rough and finishing operations. The EDM technology to
manufacture single piece impellers has started in 2004 and since then 5000+ EDM manufactured impellers made by low
alloy and stainless steel have been put in operation with zero recorded failure. In an average year, about 700 impellers
are produced using this technology. More than 50 Inconel 718 impellers have been manufactured by EDM since 2006.
The EDM material removal rate is largely independent by the kind of alloy machined, so that Inconel 718 and martensitic
stainless steels have comparable machining cycle time. After the optimization of EDM process parameters, the recast
layer generated by this process is generally less than 25µm; it is completely removed at the end of the vane generation
by an abrasive flow process that has also the benefit to improve the surface roughness. When very low levels of gas path
roughness are required, a more sophisticated super-finish process is used.
In GE O&G the EDM impeller shop has been implemented following a Lean Manufacturing concept that includes all pre
and post vane operations in a single flow line limiting the amount of unnecessary operations.
10
Tri-dimensional impellers have a more complex gas path that makes the manufacturing of those impellers in a single
piece a big challenge in terms of accessibility to the vane. GE O&G has patented several years ago a 5 axis milling process
that has guaranteed the production of high quality impellers for many different fields of application.
The low variation of mechanical properties from room to high temperature, is one of the most desirable characteristics
of Inconel alloys. Unfortunately, this is a disadvantage when it comes to cut them for machining purposes. These alloys,
in fact, tend to work harden during the cut and the relevant heat generated is preferably transferred to the tool than to
the piece, due to low thermal conductivity of nickel alloys. The result is that the cutter is typical subject to high thermal
shocks that drastically reduces its life. Further phenomena that limit the effectiveness of the process are the flank wear,
chipping, Build Up Edge (BUE) and catastrophic failure. Those alter the cutting mechanisms, cause tool rejection and
affect the surface integrity when cutting nickel based super-alloys [19].
Under so challenging machining conditions, the capability to obtain good final surfaces without affecting base material
properties can be obtained only through a rigorous tool and technological parameters selection. The nickel based alloys
turning machinability has been assessed by an engineering approach based on a wide FEM simulation campaign, where
several option of cutting parameters and inserts have been scouted. The best candidates have been selected and finally
validated in our Metal Working Laboratory under real machining conditions before their final release to the production
line. This resulted in a complete set of standard tools and cutting parameters that includes ceramic insert for rough
machining and solid carbides for finishing operations (figure 5).
Finishing turning operations of Inconel 625M and 718 (used for impellers) is performed using solid carbide inserts
(multilayer PVD coated). The relevant cutting depth, as usual for nickel based alloys, ranges from 0.7 mm to 0.1 mm
approaching the final dimension. The use of carbide inserts doesn’t allow cutting speed higher than 50 m/min because
of the poor thermochemical stability of this kind of material.
Rough turning operations (figure 6), especially during the first passes of Inconel 625 clad, is a tremendous challenge for
the cutter life as the welding asperities and discontinuities generate an interrupted cut. Some of the most advanced
ceramic inserts made of Alumina (Al2O3) mechanically reinforced with Silicon Carbides whiskers (in 50%-50% proportion)
is used here. The whiskers assure a fracture toughness doubled when comparing to a simple Alumina cutter.
Furthermore, the high thermal conductivity and the low thermal expansion coefficient of the whiskers guarantee an
improved durability to thermal shocks. A depth of cut of 3 mm, a feed rate of 0.25 mm/rev and a cutting speed limited
to 250 m/min resulted in a 4x extended life versus traditional ceramic inserts. Cutting speed can be pushed up to 400
m/min if the cut is continuous.
While turning is a well explored and tested “arena” for Nickel Super-alloys, the 5 axis milling of cavities, like that of a
single piece closed impeller, is still an area of development and potential optimization. Generally carbide tools are used
as the cutting speed capability of a milling machine at the tool diameter doesn’t permit to get the required cutting speed
for the use of ceramics.
The approach is both theoretical and experimental and it is made by a comprehensive effort of FEM simulations to
optimize cutting parameters and tool geometry. The tool life is maximized by the measurement of real cutting forces on
the workpiece for a dynamic characterization of the parameters to avoid chattering and other vibrations on the cut
surface. Two milling methods were specifically developed: deep drilling for rough machining and slot milling. In both
cases standard solid carbide tools were used.
Inconel Super-alloys rough milling productivity for impellers can be further improved by the use of the Blu ArcTM
Technology. This is a modified EDM process, for which GE owns several patents (general concept, tool shape, wear
compensation method, etc.), that improves drastically the material rate removal with the use of higher current
11
amperage. This equipment is designed to be installed on a 5 axis machine so that both rough and finish operations can
be performed in a single setting of the impeller.
This technology, after a period of development and validation, has been released for use in production in 2007 for low
alloy and martensitic stainless steel. The validation has been extended to Inconel 718 in 2008. The material removal rate
of Blu ArcTM for Inconel 718 can be up to 3 times higher than the most optimized five axis milling machining process. The
recast layer is completely removed during the 5 axis milling finishing operation.
Hybrid methods, combining the benefits of milling and EDM for finishing operations, are also used for impellers of
particularly complex vane shape.
The alloy development has been performed by a comprehensive metallurgical design approach. The first step was a
thermodynamics and kinetics modeling activity aimed to identify possible analytical variants starting from base
compositions.
Each chemical variation was made taking into account a set of critical requirements, related to material performance
(i.e. corrosion resistance and mechanical properties) or associated with production of alloys (raw material and post
processing). Through an array of calculations involving tens of variants, the final compositional ranges were down
selected and the experimental casts were made. The first attempt consisted of two variants for the new steel and two
for the new nickel base alloy.
After the cast process, a thermo-mechanical process, hot deformation plus heat treatment has been set-up taking into
account the theoretical data obtained by simulation and the literature data of similar materials.
In figure 8 and 9 the ingot after casting and a forging process step are shown. The casting and forging process have been
performed without any manufacturability problems (have proven to be successful). The experimental heats will be
characterized by mechanical and corrosion means. Based on results a further tuning of the chemistry and post
processing could be necessary in order to make the final pilot production prior the industrialization of the new alloys.
On Going Developments
A set of unconventional and transformative technologies to manufacture impellers and other stator components are
presently under development at O&G. The most promising one is based on powder metallurgy. Centrifugal pump casing
and two Inconel 625M net shape impellers were produced and tested using powder metallurgy and hipping process. The
process is actually capable to achieve a very complex final flow path shape drastically cutting the overall lead time, as no
forging procurement is necessary. Powder metallurgy and Additive Manufacturing technologies are key enablers for new
concepts in material science (i.e. functionally graded materials, composite structure, new strengthening mechanisms,...).
Additive manufacturing machine is already available in GE O&G to produce prototype parts. This program, started in
2011, will lead to install “3D printed” components in our prototype turbines and compressors by 2015.
13
4 – CONCLUSIONS
Exploitation of oil fields and gas reservoirs with an increased content of contaminants is a driver for research in the field
of materials, design equipment and manufacturing technologies.
GE Oil & Gas is pushing over the state-of-art of material technology with big efforts and investment in research.
Development of new materials is focused on the improvement of their properties and performances in order to increase
reliability and availability of equipment without affecting significantly capital expenditure.
Continuous improvement of manufacturing technology made possible to produce centrifugal compressors with nickel
based super-alloys reducing significantly machining cycle time.
New manufacturing technologies aim to reduce the waste of material and machining operation. The most promising
one is powder metallurgy that is capable to produce net shape parts with limited final machining operation. Efforts are
also in progress to further optimize cladding and coating technologies.
GE Oil & Gas has a large field experience in all sour services and is leading edge in reinjection of high pressure sour gas
fields. This successful experience has been gained with a solid partnership and co-engineering with EPCs, oil companies
and end users.
14
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Appendix
17
Figure 2 : operating margin vs. dew curve at each compression stage
18
Figure 4 : X4 Cr Ni 16-4 field application as function of pH2S
Figure 5 : FE macro-mechanical approach to investigate the machinability of Inconel718 when using Carbide and Ceramic
cutting tools.
19
Figure 6 : The Inconel 718 impeller under rough turning operation and a view of the metal working laboratory
20
Figure 8: the experimental alloy cast ingot
21