Heat-Resistant Steels for Energy
Generation Systems under Extreme
Enviroments
Carlos Capdevila
Centro Nacional de Investigaciones Metalúrgicas (CENIMCSIC)
Master in Materials Engineering. Seminar 20.02.2015
GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems and structural materials: present and future
needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
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Outline
1. Presentation
2. Steel: Material for the future
Seminar 1
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
Seminar 2
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
Seminar 3
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
Seminar 4
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
Seminar 5
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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GRUPO MATERALIA
Outline
1. Presentation
2. Steel: Material for the future
3. Properties of interest in HR steels for energy generation systems
4. HR steel families
5. Energy generation systems: present and future needs in power generation
6. Optimizing the microstructure I: Alloy design
7. Optimizing the microstructure II: processing technologies
8. Oxide Dispersion Strengthened (ODS) steels
9. Biomass: case study of a ODS FeCrAl steel
10. Steels for conventional power plants
11. Steels for nuclear applications: Fission
12. Steels for nuclear applications: Fusion
13. Other metals for high-temeprature applications
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A brief introduction
1. Presentation
GRUPO MATERALIA
Spanish National Research Council (CSIC)
CONSEJO SUPERIOR DE
INVESTIGACIONES CIENTIFICAS
CENTRO NACIONAL INVESTIGACIONES METALÚRGICAS (CENIM-CSIC)
Avda Gregorio del Amo, 8. E-28040 Madrid-Spain
The Spanish National Research Council
(CSIC) is the largest public institution
dedicated to research in Spain and the third
largest in Europe.
Its main objective is to develop and promote
research that will bring scientific and
technological progress.
CSIC is among the World’s Top 10 Research
Institutions (SCImago Institutions Ranking
World Report 2012).
The World’s Top 10 Research Institutions for 2012: CNRS (France), Chinese Academy of Sciences (China), Russian
Academy of Sciences (Russia), Harvard University (USA), Max Planck Gesellschaft (Germany), Tokyo University (Japan),
National Institutes of Health (USA), University of Toronto (Canada), CSIC (Spain), Tsinghua University (China).
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GRUPO MATERALIA
Spanish National Research Center for Metallurgy
(CENIM-CSIC)
Fundamental and applied scientific
research in metallic materials
Mission
Vision
Role
01/07/2016
Center focused on research and
knowledge transfer in metallic
materials with the aim that all the
knowledge generated at our
institution have an impact on both
the economy and the welfare of
our society.
 Thematic Centre of reference for the Spanish
steel industry.
 High visibility in Europe and Latin America.
 Experience in the training of young
researchers who have been the seed of other
centers of excellence.
 Our research activities span the entire value
chain of raw materials; from extraction, design,
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production and processing, and recycling to final
in-use properties in various industrial sectors.
Master in Materials Engineering. Seminar #1
GRUPO MATERALIA
Spanish National Research Center for Metallurgy
(CENIM-CSIC)
Permanent Staff
The staff of CENIM in 2013 was
composed by
Scientists
Technicians
Administration
Students
Source of Funding
49 Scientists,
58 Technicians and administrative
assistants and
32 Non-permanent staff (PhD students,
post-docs)
The total funding obtained during the last
four years was 8 M€ (50% from national
projects, 25% from international projects,
and 25% from industrial contracts).
The total number of publications in SCI
journals in the same period was 480. The
sum of times cited is 11,606 and CENIM
h-index is 42.
The total number of patents was 24.
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GRUPO MATERALIA
Spanish National Research Center for Metallurgy
(CENIM-CSIC)
Department of Surface
Engineering, Corrosion
and Durability
RESEARCH TOPICS
• Corrosion in natural environments and anticorrosive coatings.
• Degradation and durability of metallic biomaterials.
• Functionalisation of materials by means of surface treatments.
• Metallic corrosion and protection for construction and cultural heritage.
• Nanocomposite materials and tailored thin films.
• Joining Techniques and Mechanical Properties of Joined Materials
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GRUPO MATERALIA
Spanish National Research Center for Metallurgy
(CENIM-CSIC)
Department of Primary
Metallurgy and Materials
Recycling
RESEARCH TOPICS
• Processes, materials and energy in sustainable and ecological metallurgy
• Advanced and emerging technologies for clean production
• Characterization of raw materials and waste materials.
• Physical processes of separation and purification
• Waste Treatment. Hydrometallurgy and Pyrometallurgy
• Nanoaerosol Science and Technology
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GRUPO MATERALIA
Spanish National Research Center for Metallurgy
(CENIM-CSIC)
Physical Metallurgy
Department
RESEARCH TOPICS
• Nanostructured materials with improved mechanical properties
• Development of new light alloys: crystalline, nanocrystalline and amorphous
• Composites and nanocomposites
• Intermetallics and superalloys for high temperature applications
• Metallic materials for health care
• Recrystallization, precipitation and thermomechanical treatments
• Design and development of advanced steels.
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GRUPO MATERALIA
MATERALIA
Group
Solid-solid
Phase Transformation
(MATERALIA)
Major Research Field: Research and Development of Advanced Steels
Current Staff
1 Research Professor (Head)
2 Senior Scientists
2 Tenured Scientists
6 PhD Students
3 Technitians
RESEARCH TOPICS
•
•
•
•
•
Solid-solid phase transformation in steels
Modeling of phase transformations and properties
ReX processes
Superalloys for structural application
Advanced bainitic steels. High strength high toughness bainitic steels
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GRUPO MATERALIA
Solid-solid Phase Transformation (MATERALIA)
Developing New Generation of AHSS
Main Expertise: Design, processing and characterisation of advanced
high strength steels
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Microstructure characterisation of
advanced high strength steels
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Solid-solid Phase Transformation (MATERALIA)
Develeopment of novel Fe-base alloys for high-temperature
Air to gas turbine
applications
expander
Heat-exchanger
tube in-service at
1100 ºC
CIEMAT
CSIC
Univ. Carlos III
IMDEA Mater.
CEIT
Biomass power
plant Värnamo
(Sweden)
Convective banks
Air from GT compressor
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Tubo ODS Fe-Cr-Al
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Solid-solid Phase Transformation (MATERALIA)
Develeopment of novel Fe-base alloys for high-temperature
applications
Creep strength at 1100 ºC
111
100
110
Hoop Stress / MPa
100
10
MA 956
PM 2000 twisted
PM 2000
1
0.1
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1
10
100
Time to Rupture / h
1000
10000
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GRUPO MATERALIA
Solid-solid Phase Transformation (MATERALIA)
Ultra-high Strength Martensitic and Austenitic Metastable
Stainless Steels
High Energy X-ray micro-diffraction (Synchrotron radiation). Isothermal formation of martensite at 233 K (-40 ºC)
assisted by high magnetic fields in a metastable austenitic stainless steel: (a)-(b) 2D X-ray diffraction patterns.
Independent spots in these patterns correspond to single austenite grains; (c) Monitoring of the austenite to
martensite transformation (volume and strain) at single grain level. Collaboration : CENIM & TUDelft & ESRF &
University of Warwick.
a
Austenite to martensite transformation in a
metastable austenitic stainless steel during
isothermal holding at sub-zero temperatures
assisted by external applied magnetic field:
(a) Kinetics of the transformation at 233 K (40 ºC) for different magnetic fields; (b) TTT
diagram under a 20 T field. Collaboration:
CENIM & TUDelft & HFML.
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b
c
Achievement of sub-micrometer austenitic microstructures; (a-b) TEM images of Ni3(Ti,Al) precipitates and
sub-micrometer austenite grains; (c) Tensile behaviour of reaustenitized samples. Collaboration: CENIM &
National Taiwan Univ. & Philips.
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Facilities at CENIM-CSIC
 Electron
Microscopes:
SEM-FEG
HITACHI S-4800, SEM-FEG JEOL
J8M6500 with EBSD, TEM JEOL 2010
 X-Ray Diffractometers: Siemens D5000
and Bruker AXS D8
 X-ray
photoelectron
spectroscope
(XPS) and atomic force microscope
(AFM) for surface analysis and
characterization.
 Infrared, mass, atomic absorption and
X-Ray fluorescence spectrometers.
 Ultra micro indentation system.
 Full-equipped mechanical testing lab
(tension, compression, torsion, fatigue
and creep resistance testing machines).
 Latest generation dilatometer .
 DTA, TGA and DSC for thermal and
gravimetric analysis.
 Corrosion electrochemical systems
(LEIS, SECM, Kelvin probe).
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Access to other facilities
in Madrid, Spain, EU,
USA
 Other Scanning and Transmission
Electron Microscopes at Electron
Microscopy Centre – The Complutense
University of Madrid.
 Nano-indentation and Atomic Force
Microscopy at Materials Science
Institute of Madrid – CSIC.
 Atom probe tomography at Oak ridge
National Laboratory – US Department
of Energy
 ESFR
European
Synchrotron
Radiation Facility – Grenoble, France
 ALBA – 3 GeV Synchrotron – Barna,
Spain
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Steels
2. Steel: Material for the
future
GRUPO MATERALIA
Some figures ……
Sustainable
Steel:
Safe,
Life
cycle
innovative
A
Everywhere
key
thinking:
driver
steel:
and
At
in
ofNew
progressive
our
the solutions
core
world's
lives of the
economy
steel
forgreen
new times
economy







168 million tones of crude steel production in 2012
EU is the second steel producer in the world
Over 85% of steel used in automotive sector is less than 10-years old
Modern cars are built with new steels that are stronger but up to 25% lighter
Steel is the solely material that surround us from sunrise to dawn
There are more than 3,500 steel grades
Spain is the 4th steel producer in EU with 8% total crude production

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Some figures ……
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… and some applications
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… and some applications
Steel world in 1 minute
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… and breakthrough research
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… and breakthrough research
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What do we understand by “Extreme conditions”?
“ …..Extreme conditions involve low or high temperatures (> 1500 K),
high pressures (> 30 MPa), high strains or strain rates, high radiation
fluxes (> 100 dpa), and high electromagnetic fields (> 15T). Material
properties under extreme conditions can be extremely different from
those under normal conditions. Understanding material properties and
performance under extreme conditions, including their dynamic evolution
over time, plays an essential role in improving material properties and
developing novel materials with desired properties.” (sic)
Q. An, CALTECH, 2012
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What do we understand by “Extreme conditions”?
Our definition of “extreme conditions”:
 T > 800 ºC (normally T  1100 ºC)
 Corrosive / oxidating enviroment
 Nuclear: dpa > 100
 High-stress / high-strain conditions (variable f(T))
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Steels for energy generation
REQUIREMENTS




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Work at high-temepratures
Strength at high temperature
No catastrophic failure (ductility)
Surface protection is an add-on (self-healing)
Proper alloy system to stand irradiation
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Material Properties
3. Properties of interest in HR
steels for energy generation
systems
GRUPO MATERALIA
Materials properties of interest
The materials properties of interest for HR steels:
 Creep
 Oxidation / Corrosion and compatibility
 Irradiation resistance (nuclear)
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Fundamentals of creep
Creep of materials is classically associated with time-dependent plasticity under
a fixed stress at an elevated temperature, often greater than roughly 0.5 Tm,
where Tm is the absolute melting temperature.
Constant stress
Constant strain-rate
It can be observed three regions in these curves
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Fundamentals of creep
Stage I, or primary creep, which denotes
that portion where [in (a)] the creep-rate
(plastic strain-rate), 𝜀 = d/dt, is changing
with increasing plastic strain or time.
Stage II, secondary, or steady-state
creep is defined, in (b), under constant
strain-rate conditions, the metal hardens,
resulting in increasing flow stresses (as
seen in (a)).
The regime known as Stage III, or
tertiary creep, corresponds to the
cavitation and/or cracking, which increases
the apparent strain-rate (see (a)), or
decrease the flow stress as shown in (b)
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Fundamentals of creep
Effect of strain rate
Decreasing the testing strain-rate from a
regular value of 10-4 to, for example, 10-7 s-1,
the yield stress decreases significantly, as will
be shown is common for metals and alloys at
high temperatures.
To a “first approximation,” we might consider
the microstructure (created by dislocation
microstructure evolution with plasticity) at
just 0.002 plastic strain to be independent of
𝜀. We define the “constant structure” stresssensitivity exponent, N, defined by
𝑁=
𝜕 ln 𝜀
𝜕 ln 𝜎
𝑇,𝑠
M.E. Kassner, ‘Fundamentals of Creep in Metals and Alloys’, 2008
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Fundamentals of creep
Stress sensitivity exponent
Creep is important at
T > 0.5 Tm
Nickel
For certain applications, such as pressurized tubes, the strain-rate is a key factor
on determining the feasibility of a certain HR steel in the power-plant boiler design
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Mechanism of creep
There are two mechanisms of creep: dislocation creep (which gives powerlaw behaviour) and diffusional creep (which gives linear-viscous creep). The
rate of both is usually limited by diffusion, so both follow Arrhenius's Law.
Creep fracture, too, depends on diffusion. Diffusion becomes appreciable at
about 0.3Tm - that is why materials start to creep above this temperature.
(After Ashby & Jones, Engineering Materials, BH, 1998)
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Mechanism of creep
Dislocacion creep
The stress required to deform plastically is
that needed to make the dislocations in it
move. Their movement is resisted by (a)
the intrinsic lattice resistance and (b) the
obstructing effect of obstacles (e.g.
dissolved solute atoms, precipitates formed
with undissolved solute atoms, or other
dislocations).
Diffusion of atoms can 'unlock' dislocations
from obstacles in their path, and the
movement of these unlocked dislocations
under the applied stress is what leads to
dislocation creep.
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Mechanism of creep
Diffusional creep
As the stress is reduced, the rate of powerlaw creep falls quickly (dislocation creep).
But creep does not stop; instead, an
alternative mechanism takes over.
A polycrystal can extend in response to
the applied stress, u, by grain elongation;
here, u acts again as a mechanical driving
force but, this time atoms diffuse from one
set of the grain faces to the other, and
dislocations are not involved.
At high T / Tm, this diffusion takes place
through the crystal itself by bulk diffusion
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Creep maps
This competition between mechanisms is conveniently summarised on Deformation
Mechanism Diagrams. They show the range of stress and temperature or of strain-rate and
stress in which we expect to find each sort of creep.
Diagrams like these are available for many metals and ceramics, and are a useful summary of
creep behaviour, helpful in selecting a material for high-temperature applications.
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Creep maps
National Institute for Metal Science in Japan (NIMS)
Sometimes creep is desirable. Extrusion, hot rolling, hot pressing and forging are carried out at
temperatures at which power-law creep is the dominant mechanism of deformation. Then raising
the temperature reduces the pressures required for the operation.
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Oxidation / Corrosion
High-temperature material should resist
attack by gases at high temperatures and, in
particular, that it should resist oxidation.
Heat’exchanger tubes do oxidise in service,
and react with H2S, O2 and other combustion
products. Excessive attack of this sort is
obviously undesirable in such a highly
stressed component. Which materials
best resist oxidation, and how can the
resistance to gas attack be improved?
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Oxidation / Corrosion
This tendency of many materials to
react with oxygen can be quantified by
laboratory tests which measure the
energy needed for the reaction
Material + Oxygen + Energy 
Oxide of material
If this energy is positive, the material is
stable; if negative, it will oxidise.
(After Ashby & Jones, Engineering Materials, BH, 1998)
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Iron is not good from
oxidation resistance
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Oxidation / Corrosion
The important thing about the oxide film is that it acts as a barrier which keeps
the oxygen and iron atoms apart and cuts down the rate at which these atoms
react to form more iron oxide. Aluminium, and most other materials, form oxide
barrier layers in just the same sort of way - but the oxide layer on aluminium
is a much more effective barrier than the oxide film on iron is.
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Irradiation resistance
Types of radiation
Alpha, beta (‘particulate’, positive, negative charge), neutron (‘particulate’, no
charge); gamma; x-ray (electromagnetic, no charge); etc. (e.g., heavy-ions)
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Irradiation resistance
Effects of irradiation
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Irradiation resistance
Irradiation Produces Defect Microstructures
Irradiation Temperature (T/Tm)
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Irradiation resistance
(After M.Serrano, CIEMAT, 2010)
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Irradiation resistance
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Irradiation resistance
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Irradiation resistance
How can be improved irradiation resistance?
 Introduce features that act as sink for neutrons or
other particulate radiation (nanofeatures such as YTioxides, e.g., NFA steels)
 Select a proper alloy system (Fe-Cr) with optmised
microstructure (ferrite)
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Heat-Resistant Steels
4. HR steel families
GRUPO MATERALIA
Heat-Resistant steels
How many types of HR steels are?
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Heat-Resistant steels
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Heat-Resistant steels
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Heat-Resistant steels
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Heat-Resistant steels
Fe-9Cr-0.5Mo-1.8WVNb
(aged 104 h at 450 ºC)
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Heat-Resistant steels
(After Maruyama et al., ISIJ, 2010)
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Heat-Resistant steels
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Heat-Resistant steels
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Energy generation systems
and structural materials
5. Present and future needs in
power generation
GRUPO MATERALIA
Future needs in nuclear structural materials
o The need to reduce CO2 emissions coupled with the need to increase the
quantity of electricity supplied are driving to the development of new power
generation systems.
o Significant gains in efficiency for power generation systems can be made by
increasing the steam temperatures and pressures. This lead to an improvement
of the high-temperature properties of current heat resistant alloys.
o The low creep resistance at high temperatures of Fe-base alloys could be
mainly improved by different methods:
 One method consists on a combination of composition adjustments,

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guided by computational thermodynamics, and thermo-mechanical control
process (TMCP) optimization.
Second method is to strength the steel by oxide dispersion, and this line
led to work on ferritic oxide dispersion-strengthened (ODS) alloys. The
advantages of ODS alloys at high temperatures are clear: high strength
and high creep resistance.
Third method consists on compositional tunning to induce the formation of
nanoclusters and nanophases.
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GRUPO MATERALIA
Future needs in nuclear structural materials
 The Generation IV program aims to develop next-generation reactors that will be
more efficient, safer, longer lasting (60 years and beyond), proliferation-resistant, and
economically viable when compared to current nuclear reactors.
 Two reactor concepts, the SFR and the VHTR reactors are of the highest priority. The
heat produced will co-generate electricity and hydrogen.
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Future needs in nuclear structural materials
SFR
VHTR
 The demanding service conditions (higher neutron doses, exposure to higher
temperatures, and corrosive environments) that the structural components will
experience in these reactors would pose a significant challenge for structural material
selection
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Future needs in nuclear structural materials
There are extreme conditions!
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Our starting point
(After Charit and Murty, JOM, 2010)
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Candidate materials
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Candidate materials
WE are going to review those in this seminar series
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Questions
Thanks for your attention
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