pwi meeting, 4-6 nov. warsaw (poland) 1 of 26 slides program of the efda materials topical group...

PWI meeting, 4-6 Nov. Warsaw (Poland)1

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Program of the EFDA Materials Program of the EFDA Materials Topical Group (FMTG)Topical Group (FMTG)

Sehila M. Gonzalez de VicenteMaterial Responsible Officer

EFDA Close Support Unit - Garching


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FUSION MATERIALS TOPICAL GROUPFUSION MATERIALS TOPICAL GROUP

• MAT-REMEV: MAT-REMEV: Radiation Effects Modelling and Radiation Effects Modelling and Experimental ValidationExperimental Validation

-Phase Stability and He & dpa Accumulation Trigger in-service Properties of Materials in DEMO: Magnetic Cluster Expansion: a g phase transition points in Fe, and Rate Theory: He-desorption from pre-implanted Fe-C alloys.

• MAT-ODSFS: MAT-ODSFS: Nano-structured ODS Ferritic Steel Nano-structured ODS Ferritic Steel DevelopmentDevelopment

- Improve the present generation of nano-structured ODS RAF steels- Improve the present generation of nano-structured ODS RAF steels- Start the industrial fabrication of the present generation of nano-structured - Start the industrial fabrication of the present generation of nano-structured ODS RAF steelsODS RAF steels- Develop an optimised generation of nano-structured and nano-grained ODS - Develop an optimised generation of nano-structured and nano-grained ODS RAF steelsRAF steels- Investigate the stability of present and optimised generation of nano-- Investigate the stability of present and optimised generation of nano-structured ODS RAF steels under creep and irradiationstructured ODS RAF steels under creep and irradiation


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FUSION MATERIALS TOPICAL GROUPFUSION MATERIALS TOPICAL GROUP

•MAT-W&WALLOYS: MAT-W&WALLOYS: Tungsten and Tungsten Alloys Tungsten and Tungsten Alloys DevelopmentDevelopment

- Development of Structural Tungsten Materials - Development of Structural Tungsten Materials - Optimization of Tungsten Armour Materials - Optimization of Tungsten Armour Materials - Manufacturing Parts of Tungsten Materials- Manufacturing Parts of Tungsten Materials- Materials Science and ModelingMaterials Science and Modeling

The long-term objective of the EFDA fusion materials programme is to develop The long-term objective of the EFDA fusion materials programme is to develop structural as well as armour materials in combination with the necessary structural as well as armour materials in combination with the necessary production and fabrication technologies for future divertor conceptsproduction and fabrication technologies for future divertor concepts

• MAT-SiC/SiC: SiCf/SiC Composite for Structural MAT-SiC/SiC: SiCf/SiC Composite for Structural Application in Fusion ReactorApplication in Fusion Reactor

- - Processing techniques for manufacturing SiCf/SiCProcessing techniques for manufacturing SiCf/SiC-Increase in thermal conductivityIncrease in thermal conductivity


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MAT-REMEVMAT-REMEVRadiation Effects Modelling and Radiation Effects Modelling and

Experimental ValidationExperimental Validation


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Phase Stability and He & dpa Accumulation Trigger in-service Properties of Materials in DEMO:

• Magnetic Cluster Expansion: phase transition points in Fe.

• Rate Theory: He-desorption from pre-implanted Fe-C alloys.


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Magnetism Stabilises bccMagnetism Stabilises bccFe at low TemperatureFe at low Temperature

DFT data

FM bcc

AF fcc10mRy~1600 K

At 0K the lowest Energy:

Ferro-Magnetic (FM) bcc FeMagnetic Cluster Expansion (MCE)

Fitted on DFT data at 0K

Atomic Configuration Energy with Explicit Magnetism

Contribution

Allows Calculating Free Energy & Phase Stability at

any Finite Temperature


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Magnetic Cluster DynamicsMagnetic Cluster Dynamics

0 400 800 1200 1600-40

-20

0

20

40

60

80

100

120

140 E(fcc)-E(bcc) -T(S

fcc-S

bcc)

Fmag

(fcc)-Fmag

(bcc)

E (

me

V/a

tom

)

T (K)

1000 1200 1400 1600 1800-5

0

5

10

15

20

Tm

TC

Ffcc

-Fbcc

TT

F (

me

V/a

tom

)

T (K)

Monte Carlo Simulation of the Free Energy:

Configuration Entropy

Magnetic Excitation Entropy

Not sufficient to Stabilise the fcc () at High Temperature

Adding

Phonons entropy based on

experimental data (Neutron

Diffraction & Elastic Constants

Monte Carlo Simulation of the Free Energy:

Configuration Entropy

Magnetic Excitation Entropy

Experimental Phonons entropy

For the First Time the high T “domain” of iron

is predicted based on DFT and Atomistic Modelling & Experimental data


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He-desorption from Fe-C: Rate Theory ModellingHe-desorption from Fe-C: Rate Theory Modelling (i) DFT Energetics of He, Vacancies and Carbon in (i) DFT Energetics of He, Vacancies and Carbon in -Fe-Fe

VC VC2 VC3 V CbE 0.52 eV VC C

bE 0.89 eV 2VC CbE 0.12 eV

V + He HeV

Eb = 2.3 eVVC + He HeVC

Eb = 2.09 eV

VC2 + He HeVC2

Eb = 0.94 eV

Carbon reduces the He-V binding energy

Hen-1Vm + Heint → HenVm

He Binding Energy to Hen-1Vm C Binding Energy to VCm-1

VCm-1 + C → VCm

He Binding Energy to Hen-1CVm


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-Fe with 50 appm Carbon

He-desorption from Fe-C: Rate Theory Modelling He-desorption from Fe-C: Rate Theory Modelling (ii) DFT based Rate Theory Modelling as function of C content(ii) DFT based Rate Theory Modelling as function of C content

10-1 10 103

10-3

10-2

10-1

Des

orb

ed f

ract

ion

Annealing Time (s)

559 K 577 K 667 K Model

Pure -Fe

• C-V Binding Energiesand

• He-V Binding Energy Reductions

Favour He –Desorption

Submitted Phys. Rev. B

-Fe with 88 appm Carbon


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MAT-ODSFSMAT-ODSFSNano-structured ODS Ferritic Nano-structured ODS Ferritic

Steel DevelopmentSteel Development


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The 2008-2009 work programme of the European The 2008-2009 work programme of the European research project on nano-structured ODS RAF research project on nano-structured ODS RAF steels is being organized along four steels is being organized along four programmatic lines:programmatic lines:

• Improve the present generation of nano-structured ODS Improve the present generation of nano-structured ODS RAF steelsRAF steels

• Start the industrial fabrication of the present generation Start the industrial fabrication of the present generation of nano-structured ODS RAF steelsof nano-structured ODS RAF steels

• Develop an optimised generation of nano-structured and Develop an optimised generation of nano-structured and nano-grained ODS RAF steelsnano-grained ODS RAF steels

• Investigate the stability of present and optimised Investigate the stability of present and optimised generation of nano-structured ODS RAF steels under generation of nano-structured ODS RAF steels under creep and irradiationcreep and irradiation


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Manufacturing route:• Mechanical alloying - elemental or pre-alloyed powders• Canning and degassing of the milled powders• Compaction of the powders by HIPping• Thermal-mechanical treatments– Hot pressing– Hot rolling– High speed hot extrusion

Z. Oksiuta et al., MAT-ODSFSEFDA Monitoring Meeting,Garching, January 2009

Materials:Fe-(12-13-14)Cr-(1-2)W-(0.3-0.5)Ti-0.3Y2O3 (in wt.%)

Improve the present generation of nano-structured ODS RAF steels:


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• Refinement of the grain size using equal channelangular pressing (ECAP) or high-speed hot extrusion:• Successful trials on the EUROFER RAFM steel• Experiments will be performed on ODS steel variants

M.A. Auger et al., MAT-ODSFSEFDA Monitoring Meeting,

Stockholm, July 2009

T = 550°Cα = 105°C8 passes

Develop an optimised generation of nano-structured and nano-grained ODS RAF steels:


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Investigate the stability of present and optimised generation of nanostructured ODS RAF steels under creep and irradiation

Specimens of the MA957 ODS ferritic steel in the hot extruded and cold worked condition have been irradiated in the SINQ facility (Swiss Spallation Neutron Source):

– Doses = 5-20 dpa– T = 115-360°C– 50 appm He/dpa– 450 apm H/dpa

Tensile tests: The irradiated MA957 ODS ferritic steel retained a significant ductility at both 25°C and 250°C testing temperatures

J. Henry et al.EFDA Monitoring

Meeting,July 2009


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MAT-W&WALLOYSMAT-W&WALLOYSTungsten and Tungsten Alloys Tungsten and Tungsten Alloys

DevelopmentDevelopment


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Goals & RoadmapGoals & Roadmap

20082008

Structural Material DevelopmentStructural Material Development

20092009 20102010 20112011 20122012 20132013 ……

Armour Material OptimisationArmour Material Optimisation

Fabrication Process DevelopmentFabrication Process Development

……

……

……

Materials Science & ModelingMaterials Science & Modeling ……


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• Development of Structural Tungsten Materials – Can the DBTT be significantly decreased?– Is it possible to reach a compromise between strength, ductility, and heat

conductivity?– Can we live with a pronounced anisotropic micro-structure or is it necessary to

produce isotropic structured materials?

• Optimization of Tungsten Armour Materials – What is the optimized microstructure for fusion relevant thermo-mechanical load

conditions?– Is it possible to increase the crack resistivity?– What are possible solutions for the oxidation problem?

• Manufacturing Parts of Tungsten Materials– How to avoid micro-cracks? – What alternative fabrication process could be suitable? – Are there applicable reduced activation brazing materials for W-W and W-steel

joints? – Can mass/series production processes be applied to tungsten parts?

• Materials Science and Modeling– What makes tungsten so brittle?– Is ductilization possible besides Re addition?– What is the influence of impurities and microstructure on the material behavior?– How does tungsten behave under high neutron doses and after significant He/H

load?


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Structural Tungsten Materials: Microstructure of Structural Tungsten Materials: Microstructure of Commercial AlloysCommercial Alloys

Ø20 mm

93%

Swaging Ø20 mm

93%

Swaging Ø10 mm

81% Rolling Ø7 mm

91% Sw+Rol

W-1%Ta

Ø6,9 mm

91% Rolling

R. Pippan, ÖAWR. Pippan, ÖAW

Forging Direction

Forging Direction


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Structural Tungsten Materials: DevelopmentStructural Tungsten Materials: Development

Fabrication by Mechanical Alloying and Hot Isostatic PressingFabrication by Mechanical Alloying and Hot Isostatic Pressing

200 µm200 µm

20 µm20 µm

W-1La2O3

W-4VAlloysAlloys Hardness Hardness

(GPa)(GPa)W-1La2O3 1.43

W-4V-1La2O3 4.0

W-4V 3.40

W-2V 3.16

W 2.67

W-0.5Y2O3 2.34

W-4Ti 4.47

W-4%Ti-0.5Y2O3 6.36

A. Muñoz, M.A. Auger, T. Leguey, A. Muñoz, M.A. Auger, T. Leguey, M.A. Monge, R. Pareja, CIEMAT/M.A. Monge, R. Pareja, CIEMAT/UC3M/UPMUC3M/UPM


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Oxidation Resistant Tungsten Armor MaterialsOxidation Resistant Tungsten Armor Materials

W-Si-Cr Protection Bulk MaterialsW-Si-Cr Protection Bulk Materials Self Passivating Thin FilmsSelf Passivating Thin Films

C. García-Rosales, P. López, C. García-Rosales, P. López, N. OrdásN. Ordás, CEIT, CEIT

F. Koch, C. Lenser, F. Koch, C. Lenser, M. Rasinski*,M. Rasinski*,M. Balden, Ch. LinsmeierM. Balden, Ch. Linsmeier, IPP, IPP

0.25 h0.25 h 0.5 h0.5 h

1 h1 h

0.75 h0.75 h

2 µmµm

quarternary alloys quarternary alloys WSi3Cr10Zr5 WSi3Cr10Zr5SEM of cross section, oxidized at 1000°C at SEM of cross section, oxidized at 1000°C at different timesdifferent times

1 µmµm

W10Si10Cr after 1400 °CW10Si10Cr after 1400 °C

MA: W/CrSiMA: W/CrSi22

MA: WSiMA: WSi22/W/Cr/W/Cr


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Manufacturing Parts of Tungsten MaterialsManufacturing Parts of Tungsten Materials

Functional Gradient Material, Mass Production, EC Layer DepositionFunctional Gradient Material, Mass Production, EC Layer Deposition

Thimble by Press RollingThimble by Press Rolling

J. Reiser,J. Reiser, FZK FZK

S. S. Antusch,Antusch, FZK FZK

Tile by Powder Injection MoldingTile by Powder Injection Molding

J. v.d. Laan,J. v.d. Laan, NRG NRG

5 µmµm 5 µmµm

WC

W/WCW/WC

WC/FeWC/Fe

EuroferEurofer

W or W alloy

W –Fe –C (1200°C) W –Fe –C (1200°C)

Gradient by Powder MetallurgyGradient by Powder Metallurgy

J.M. Missiaen, J. Schlosser, Grenoble-INP & CEAJ.M. Missiaen, J. Schlosser, Grenoble-INP & CEA

Ni on WNi on W

Electro-Chemical Layer DepositionElectro-Chemical Layer Deposition

constantthickness on edges

EuroferEurofer

WW

W. Krauss, N. Holstein, J. Konys, J. LorenzW. Krauss, N. Holstein, J. Konys, J. Lorenz,, FZK FZK


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Materials Science and ModelingMaterials Science and Modeling

Experiments at JANNUS etc.Experiments at JANNUS etc. Theory/Computation/ValidationTheory/Computation/Validation

TEM (extended defects investigations)TEM (extended defects investigations)

Dual and triple beam irradiation: Dual and triple beam irradiation: high dpa levelshigh dpa levelssimultaneously with He implantationsimultaneously with He implantationH / He co-implantation synergyH / He co-implantation synergy

Positron Annihilation Spectroscopy (PAS)Positron Annihilation Spectroscopy (PAS)Doppler broadeningDoppler broadeningPositron Lifetime SpectroscopyPositron Lifetime Spectroscopy

SurfaceSurface

300 nm~ 750 nm~ 750 nm

M.-F. Barthe, P.-E. Lhuillier, T. Sauvage, P. M.-F. Barthe, P.-E. Lhuillier, T. Sauvage, P. Desgardin,Desgardin, CEMHTI, CNRS Orléans, CEMHTI, CNRS Orléans,

R. Schäublin, EPFL, CRPPR. Schäublin, EPFL, CRPP P. Trocellier, CEAP. Trocellier, CEA

Object Kinetic Monte Carlo (LAKIMOCA)Object Kinetic Monte Carlo (LAKIMOCA) C.S. Becquart, C. Domain, U. Sarkar, C.S. Becquart, C. Domain, U. Sarkar,

M. Hou, LMPGM Villeneuve d´Ascq, EDF M. Hou, LMPGM Villeneuve d´Ascq, EDF Moret sur Loing, Université Libre de Moret sur Loing, Université Libre de BruxellesBruxelles

DFT Calculations: He & Vacancies near DFT Calculations: He & Vacancies near Surfaces (SIESTA)Surfaces (SIESTA) C.-C. Fu, CEAC.-C. Fu, CEA

Ab InitioAb Initio Dislocation Modeling Dislocation Modeling L. Ventelon, F. Willaime, M.-C. Marinica, L. Ventelon, F. Willaime, M.-C. Marinica,

CEACEA L. Romaner, ÖAWL. Romaner, ÖAW

MicromechanicsMicromechanics R. Pippan, ÖAWR. Pippan, ÖAW

10 µm10 µm


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MAT-SiC/SiCMAT-SiC/SiC SiCf/SiC Composite for SiCf/SiC Composite for

Structural Application in Fusion Structural Application in Fusion ReactorReactor


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SiCSiC/SiC /SiC CompositesComposites for structural application for structural application

High residual porosity for the most developed processing route (CVI)

SiC fibres sensitive at high T processing

Sintering additive are needed for densification

Porosity and oxide impurities lower the

-SiC transforms to -SiC at high temperatures

ISSUES MAIN REQUIREMENTS

Non-porous (gas impermeability) …………….

High mechanical strength and reliability……

Low netron activation ……………………..

High thermal conductivity ……………………….

No (low) swelling …………………………………..

Elimination / lowering porosity alternative processing technique

Increase in thermal conductivity lower porosity + incorporation of

materials with higher e.g. metal)

OBJECTIVES


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Processing techniques for manufacturing SiCf/SiC

CVI - Chemical vapor infiltration open porosity, ..

PIP - Preceramic polymer infiltration and pyrolysis open porosity, ..

NITE - Nano-powder infiltration and transient eutectoide Ceramic processing: SiO2-Al2O3-Y2O3 high sintering T & p, Al, ..?.

SiTE* - Slip-Infiltration (EPI) + Transient Eutectoide

Hybrid SITE# - Slip infiltration (EPI) + PIP

1. E-field driven powder infiltration

2. Vacuum infiltration with precursor* SiO2-MeO-P2O5 (Me=Al, Mg) /# preceramic polymer

3. *Sintering at T< 1500 °C / #pyrolysis+crystallisationIncrease in thermal conductivity

Porosity reduction: electrophoretic infiltration to increase “green” density

W-wires incorporation: feasibility study reactivity?!

CNT-coating on SiC-fibres: feasibility study W-wire

SiC-matrix (SITE)

?


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CNT-interphase layer on SiC CNT-interphase layer on SiC fibersfibers

Proposed effects of CNT interphase layer on SiC fibers:

• increase in toughness and reliability

by crack deflection (energy dissipation)

• Increase in thermal conductivity

(CNT-SiC)f/SiCCNT = > 2000 W/mK

K. König, S. Novak, et al, Fabrication of CNT-SiC/SiC composites by electrophoretic deposition, JECS, xxx (2009)

Tyrano SA

CNT

CNT-coated SiC-fiberCNT-coated SiC-fiber

Increase in thermal conductivity

(W,SiC)f/SiCW-wire

SiC-matrix (SITE)

?w ~ 170 W/mK

pwi meeting, 4-6 nov. warsaw (poland) 1 of 26 slides program of the efda materials topical group...

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