EXAFS Study on Irradiated ODS Ferritic Steel

5
EXAFS Study on Irradiated ODS Ferritic Steel Manuel A. Pouchon 1,a , Jiachao Chen 1,b , Claude Degueldre 1,c , Annick Froideval 1,d , Hermann Emerich 2,e and Wouter Van Beek 2,f 1 Energy and Safety Dep., Paul Scherrer Institute, CH-5232 Villigen PSI, Switzerland 2 SNBL/ESRF, BP220, F-38043 Grenoble Cedex, France a [email protected], b [email protected], c [email protected], d [email protected], e [email protected], f [email protected] Keywords: ferritic ODS, EXAFS, Radiation Damage, Dispersoids, Yttria, Fe-Cr Matrix Abstract. The commercial material PM2000 is investigated as a representative for the material class of Oxide Dispersion Strengthened (ODS) steels. ODS steels are envisaged as substance of structural components in Very High Temperature Reactors (VHTR). The VHTR concept is considered by the Generation IV International Forum, an initiative researching the next generation of nuclear power plants. The chosen ODS is mainly used for non-nuclear applications. In order to justify the applicability of this material within a neutron irradiative environment, the evolution of radiation damage must be investigated. PM2000 samples are therefore exposed to 4 He 2+ irradiation at different temperatures. The potential structural change is measured as a function of the radiation parameters, using Extended X-Ray Absorption Fine Structure (EXAFS) spectroscopy on the yttrium K-edge and on the iron K-edge. A degradation of the dispersoids or the steel matrix would show the limitation of this material candidate. Introduction The VHTR is a gas cooled reactor concept, where some of the structural materials are potentially exposed to nearly 1000 ºC, and maybe even higher temperatures under accidental conditions. High gas temperatures are desirable for an increase of the energy conversion efficiency in general, and also for direct heat applications. ODS steels are attractive material candidates for high temperature applications, where creep of conventional steels becomes an issue. The dispersoids are oxide particles, which are embedded in the steel matrix. These particles serve as pinning points for dislocations. Earlier EXAFS studies [1] have shown, that the structure of the dispersoids does not correspond to the one found under normal conditions, but that it is rather a mixture with the high pressure phases and/or phases including aluminum [2]. Even tough PM2000 is much less sophisticated than some especially for nuclear applications developed ODS steels (for example a Japanese candidate [3]), its investigation has several interesting aspects. It is important to see, how such a commercial grade, and therefore comparatively cheap material performs. With its large grain-size, in many studies, one is looking to a single crystal, which makes the material interesting for some basic studies. The irradiation behavior is investigated by exposing samples to a He-ion beam, and by characterizing the potential structural change with the EXAFS technique. Material The investigated ODS steel is the commercial product PM2000 from Plansee [4]. It is produced on a powder metallurgical way. The powder is refined by high energy milling, resulting in an extremely small grained structure, in which the dispersion particles and the alloying elements themselves are distributed very homogeneously. The material then reaches its final state after an extrusion, a hot and cold rolling process, and a final heat treatment [4]. It has very large grains, which are in the order of Materials Science Forum Vols. 561-565 (2007) pp 1761-1764 Online available since 2007/Oct/02 at www.scientific.net © (2007) Trans Tech Publications, Switzerland doi:10.4028/www.scientific.net/MSF.561-565.1761 All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP, www.ttp.net. (ID: 141.213.236.110, University of Michigan Library, Media Union Library, Ann Arbor, United States of America-01/03/13,14:05:41)

Transcript of EXAFS Study on Irradiated ODS Ferritic Steel

Page 1: EXAFS Study on Irradiated ODS Ferritic Steel

EXAFS Study on Irradiated ODS Ferritic Steel

Manuel A Pouchon1a Jiachao Chen1b Claude Degueldre1c

Annick Froideval1d Hermann Emerich2e and Wouter Van Beek 2f 1 Energy and Safety Dep Paul Scherrer Institute CH-5232 Villigen PSI Switzerland

2 SNBLESRF BP220 F-38043 Grenoble Cedex France

amanuelpouchonpsich

bjiachaochenpsich

cclaudedegueldrepsich

dannickfroidevalpsich

eermanoesrffr

fwouteresrffr

Keywords ferritic ODS EXAFS Radiation Damage Dispersoids Yttria Fe-Cr Matrix

Abstract The commercial material PM2000 is investigated as a representative for the material class of Oxide Dispersion Strengthened (ODS) steels ODS steels are envisaged as substance of structural components in Very High Temperature Reactors (VHTR) The VHTR concept is considered by the Generation IV International Forum an initiative researching the next generation of nuclear power plants The chosen ODS is mainly used for non-nuclear applications In order to justify the applicability of this material within a neutron irradiative environment the evolution of radiation damage must be investigated PM2000 samples are therefore exposed to 4He2+ irradiation at different temperatures The potential structural change is measured as a function of the radiation parameters using Extended X-Ray Absorption Fine Structure (EXAFS) spectroscopy on the yttrium K-edge and on the iron K-edge A degradation of the dispersoids or the steel matrix would show the limitation of this material candidate

Introduction

The VHTR is a gas cooled reactor concept where some of the structural materials are potentially exposed to nearly 1000 ordmC and maybe even higher temperatures under accidental conditions High gas temperatures are desirable for an increase of the energy conversion efficiency in general and also for direct heat applications

ODS steels are attractive material candidates for high temperature applications where creep of conventional steels becomes an issue The dispersoids are oxide particles which are embedded in the steel matrix These particles serve as pinning points for dislocations Earlier EXAFS studies [1] have shown that the structure of the dispersoids does not correspond to the one found under normal conditions but that it is rather a mixture with the high pressure phases andor phases including aluminum [2] Even tough PM2000 is much less sophisticated than some especially for nuclear applications developed ODS steels (for example a Japanese candidate [3]) its investigation has several interesting aspects It is important to see how such a commercial grade and therefore comparatively cheap material performs With its large grain-size in many studies one is looking to a single crystal which makes the material interesting for some basic studies

The irradiation behavior is investigated by exposing samples to a He-ion beam and by characterizing the potential structural change with the EXAFS technique

Material

The investigated ODS steel is the commercial product PM2000 from Plansee [4] It is produced on a powder metallurgical way The powder is refined by high energy milling resulting in an extremely small grained structure in which the dispersion particles and the alloying elements themselves are distributed very homogeneously The material then reaches its final state after an extrusion a hot and cold rolling process and a final heat treatment [4] It has very large grains which are in the order of

Materials Science Forum Vols 561-565 (2007) pp 1761-1764Online available since 2007Oct02 at wwwscientificnetcopy (2007) Trans Tech Publications Switzerlanddoi104028wwwscientificnetMSF561-5651761

All rights reserved No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTPwwwttpnet (ID 141213236110 University of Michigan Library Media Union Library Ann Arbor United States of America-010313140541)

cm in size and the dispersoids which are yttria particles are in the range of 40-70 nm The composition is 735 wt Fe 20 wt Cr 55 wt Al 05 wt Ti and 05 wt Y2O3

Experimental

In this paper two different experiments are compared One based on samples irradiated with low energy He ions at ambient temperature using a tandem accelerator and another experiment based on a high energy He ion irradiation at 571 K with a cyclotron The experiments are described in the following subsections and are also summarized in Table 1 Low energy irradiation and EXAFS Samples of the dimension 6 x 6 x 1 mm3 are cut in a long transverse direction One surface is then grinded with SiC papers down to a P-Grading of 4000 A polishing with a 6 and 3 microm diamond suspension is performed The polishing is finalized with OPS for 2rsquo Using the tandem accelerator at the ETH Zuumlrich (Switzerland) the polished surface is exposed to 15 MeV 4He2+ ions at room temperature and under multiple incidence angles (0-66ordm) The reached average displacement damage is roughly 06 dpa [5] Irradiated samples are then investigated at the 10ID (MRCAT) beamline at the Advanced Photon Source (APS) Argonne National Laboratory EXAFS measurements are performed on the yttria edge with a synchrotron radiation incidence angle of 20ordm with the detector placed perpendicular to the incoming beam For a further description and a scheme of the He irradiation profile combined with the region sensed by the EXAFS signal see [6] High energy irradiation and EXAFS Dog-bone shaped creep samples of 300 microm thickness are cut by spark erosion perpendicular to the rolling direction The samples are mechanically polished on both sides to 100 microm with a P-Grading paper of 2400 The final samples have an overall size of 28 mm in length 8 mm in width and 01 mm in thickness with a gauge volume of 10 x 2 x 01 mm3 Using the Compact Cyclotron of Forschungszentrum Juelich (Germany) the samples are exposed to an in-situ creep experiment with 4He2+ ions of 0-24 MeV at 300 ordmC The reached average displacement damage is 07 dpa [7] After the experiment small fractions are extracted from the gauge region and measured together with non-irradiated reference samples at the Swiss-Norwegian beamline BM1B at the ESRF in Grenoble (France) [8] The EXAFS measurements are performed at the yttria and at the iron edge All spectra are taken at 50 K using a He cryostat The incidence angle of the beam is 30ordm with the detector placed perpendicular to the incoming beam EXAFS evaluation For evaluating the EXAFS results and for the formation of the Fourier transforms the open source software ATHENA [9] is used For the Y-edge a sine window from k= [213]Aring-1 is used In case of the Fe edge the sine window is chosen in the interval k= [214]Aring-1

Sample He implantation EXAFS experiment

Absorp Edge [Boolean] Ref Dimensions

[mm3] Energy [MeV]

Inc angle [ordm]

Temp [K]

Ref Y Fe

Temp [K]

Inc angle [ordm]

Plates 60 x 60 x 10

15 0-66 300 [5] yes [6] no [-] 300 20

Dogbone gauge 100 x 20 x 01

0-24 0 571 [7] yes [-] yes [-] 50 30

Table 1 Summarized irradiation and EXAFS experiments presented in this paper The average

displacement dose is for both irradiations similar being 06 and 07 dpa for the low and the high energy implantation respectively For further information see text under the subsections low and high energy irradiation and EXAFS

1762 PRICM 6

Results and Discussion

This paper presents the experimental results The radiation and temperature depending behavior of the EXAFS spectra and its Fourier transform already represent by themselves an important proposition EXAFS is a technique which probes the coordination environment of a selected absorbing atom With this information the structure containing the absorbing atom can be reconstructed If no change is found in the spectra the investigated structure remained stable Otherwise a change was induced This change can be due to a phase transformation due to point defects and clusters or due to bubble formation and the resulting stress fields For a detailed analysis all the possibilities must be simulated using an ab initio multiple scattering calculations of the EXAFS spectra Y-edge By looking at the yttrium-edge EXAFS is sensing the structure of the dispersoids As mentioned before these very fine particles are the basis of the enhanced creep behavior of ODS materials and their integrity is important to guarantee the long term properties of the composite If the EXAFS signal changes as a function of the exposure (temperature irradiation and mechanical load) the change must be understood in order to judge its influence to the changed material performance The samples irradiated with the tandem accelerator at room temperature does not show changes in the EXAFS signal which would indicate a change in the dispersoid structure (see Fig 1a in the lower graph) The reference spectra has been taken at low temperature and therefore shows different peak intensities nevertheless the peak locations and shapes compare very well for the reference and the irradiated samples [6] It can therefore be concluded that under the given irradiation conditions the

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Figure 1 Fourier transforms of the EXAFS results In each graph the distribution function of the

reference samples is represented by the upper curve with its ordinate on the right side The irradiated samples are represented by the lower curve with the ordinate to the left a) Y-edge the lower graph shows the Fourier transform of the samples being irradiated at room temperature with 15 MeV ions (see also [6]) The reference here derives from [1] The upper graph shows the Fourier transform of the EXAFS taken from the 0-24 MeV irradiation at 571 K Here a box emphasizes the most interesting change in the distribution function b) Fe-edge Fourier transforms taken for a reference and a sample implanted with 0-24 MeV He ions A box emphasizes the most interesting change in the distribution function

Materials Science Forum Vols 561-565 1763

dispersoids remain stable In the actual experiment the samples are trough irradiated at 571 K The corresponding spectrum together with the reference is shown in Fig 1a in the upper graph Both spectra have been taken at the same beamline (ESRF) under the same conditions Therefore any change must be due to a change in the dispersoid structure The graph especially shows in the second shell a significant change in the spectra The structural change by itself must still be understood and is subject of future work Fe-edge By looking at the iron-edge EXAFS is sensing the bulk structure This experiment is only performed for the samples being irradiated with the Juumllich cyclotron at 571 K and for its reference Both spectra are again taken at one beamline (ESRF) under the same conditions (Table 1) Again a clear difference is visible in the distribution function In the second shell a doubling of the peak can be identified after irradiation Whether this change can be associated with point defects must be shown by ab initio multiple scattering calculations of the EXAFS spectra

Summary

Samples irradiated under two different environmental conditions are investigated by EXAFS addressing both the dispersoids and the matrix of the ODS composite When looking at the dispersoids a clear difference can be identified between the samples being irradiated at room temperature and at 571 K The dispersoids remain stable at room temperature whereas at 571 K a clear change in their structure can be identified When looking at the matrix the irradiation at 571 K also shows a clear effect on the structure For a further understanding of the damage mechanism more work towards the spectra modelling must and will be preformed

Acknowledgements

Two of the authors (MA Pouchon and J Chen) acknowledge the partial support of the work by the European FP6 projects RAPHAEL and EXTREMAT

References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

[2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) p 277-287

[3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

[4] Dispersion-Strengthened High-Temperature Materials Material properties and applications Prospectus from Plansee 2003 706 DE0403(1000)RWF

[5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

[6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3) (2007) p 253-258

[7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press doi101016jjnucmat200704051

[8] BM1B Main Page Last retrieved Mai 31st 2007 from lthttpwwwesrfeuexp_facilitiesBM1AindexBhtmgt

[9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

1764 PRICM 6

PRICM 6 104028wwwscientificnetMSF561-565 EXAFS Study on Irradiated ODS Ferritic Steel 104028wwwscientificnetMSF561-5651761

DOI References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) 277-

287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater ol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719 [1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Mslang and JA Schrder Powder Metall B Vol 48 (3) (2005) p 277-287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Dbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719

Page 2: EXAFS Study on Irradiated ODS Ferritic Steel

cm in size and the dispersoids which are yttria particles are in the range of 40-70 nm The composition is 735 wt Fe 20 wt Cr 55 wt Al 05 wt Ti and 05 wt Y2O3

Experimental

In this paper two different experiments are compared One based on samples irradiated with low energy He ions at ambient temperature using a tandem accelerator and another experiment based on a high energy He ion irradiation at 571 K with a cyclotron The experiments are described in the following subsections and are also summarized in Table 1 Low energy irradiation and EXAFS Samples of the dimension 6 x 6 x 1 mm3 are cut in a long transverse direction One surface is then grinded with SiC papers down to a P-Grading of 4000 A polishing with a 6 and 3 microm diamond suspension is performed The polishing is finalized with OPS for 2rsquo Using the tandem accelerator at the ETH Zuumlrich (Switzerland) the polished surface is exposed to 15 MeV 4He2+ ions at room temperature and under multiple incidence angles (0-66ordm) The reached average displacement damage is roughly 06 dpa [5] Irradiated samples are then investigated at the 10ID (MRCAT) beamline at the Advanced Photon Source (APS) Argonne National Laboratory EXAFS measurements are performed on the yttria edge with a synchrotron radiation incidence angle of 20ordm with the detector placed perpendicular to the incoming beam For a further description and a scheme of the He irradiation profile combined with the region sensed by the EXAFS signal see [6] High energy irradiation and EXAFS Dog-bone shaped creep samples of 300 microm thickness are cut by spark erosion perpendicular to the rolling direction The samples are mechanically polished on both sides to 100 microm with a P-Grading paper of 2400 The final samples have an overall size of 28 mm in length 8 mm in width and 01 mm in thickness with a gauge volume of 10 x 2 x 01 mm3 Using the Compact Cyclotron of Forschungszentrum Juelich (Germany) the samples are exposed to an in-situ creep experiment with 4He2+ ions of 0-24 MeV at 300 ordmC The reached average displacement damage is 07 dpa [7] After the experiment small fractions are extracted from the gauge region and measured together with non-irradiated reference samples at the Swiss-Norwegian beamline BM1B at the ESRF in Grenoble (France) [8] The EXAFS measurements are performed at the yttria and at the iron edge All spectra are taken at 50 K using a He cryostat The incidence angle of the beam is 30ordm with the detector placed perpendicular to the incoming beam EXAFS evaluation For evaluating the EXAFS results and for the formation of the Fourier transforms the open source software ATHENA [9] is used For the Y-edge a sine window from k= [213]Aring-1 is used In case of the Fe edge the sine window is chosen in the interval k= [214]Aring-1

Sample He implantation EXAFS experiment

Absorp Edge [Boolean] Ref Dimensions

[mm3] Energy [MeV]

Inc angle [ordm]

Temp [K]

Ref Y Fe

Temp [K]

Inc angle [ordm]

Plates 60 x 60 x 10

15 0-66 300 [5] yes [6] no [-] 300 20

Dogbone gauge 100 x 20 x 01

0-24 0 571 [7] yes [-] yes [-] 50 30

Table 1 Summarized irradiation and EXAFS experiments presented in this paper The average

displacement dose is for both irradiations similar being 06 and 07 dpa for the low and the high energy implantation respectively For further information see text under the subsections low and high energy irradiation and EXAFS

1762 PRICM 6

Results and Discussion

This paper presents the experimental results The radiation and temperature depending behavior of the EXAFS spectra and its Fourier transform already represent by themselves an important proposition EXAFS is a technique which probes the coordination environment of a selected absorbing atom With this information the structure containing the absorbing atom can be reconstructed If no change is found in the spectra the investigated structure remained stable Otherwise a change was induced This change can be due to a phase transformation due to point defects and clusters or due to bubble formation and the resulting stress fields For a detailed analysis all the possibilities must be simulated using an ab initio multiple scattering calculations of the EXAFS spectra Y-edge By looking at the yttrium-edge EXAFS is sensing the structure of the dispersoids As mentioned before these very fine particles are the basis of the enhanced creep behavior of ODS materials and their integrity is important to guarantee the long term properties of the composite If the EXAFS signal changes as a function of the exposure (temperature irradiation and mechanical load) the change must be understood in order to judge its influence to the changed material performance The samples irradiated with the tandem accelerator at room temperature does not show changes in the EXAFS signal which would indicate a change in the dispersoid structure (see Fig 1a in the lower graph) The reference spectra has been taken at low temperature and therefore shows different peak intensities nevertheless the peak locations and shapes compare very well for the reference and the irradiated samples [6] It can therefore be concluded that under the given irradiation conditions the

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Fe

Y

a)b)

Figure 1 Fourier transforms of the EXAFS results In each graph the distribution function of the

reference samples is represented by the upper curve with its ordinate on the right side The irradiated samples are represented by the lower curve with the ordinate to the left a) Y-edge the lower graph shows the Fourier transform of the samples being irradiated at room temperature with 15 MeV ions (see also [6]) The reference here derives from [1] The upper graph shows the Fourier transform of the EXAFS taken from the 0-24 MeV irradiation at 571 K Here a box emphasizes the most interesting change in the distribution function b) Fe-edge Fourier transforms taken for a reference and a sample implanted with 0-24 MeV He ions A box emphasizes the most interesting change in the distribution function

Materials Science Forum Vols 561-565 1763

dispersoids remain stable In the actual experiment the samples are trough irradiated at 571 K The corresponding spectrum together with the reference is shown in Fig 1a in the upper graph Both spectra have been taken at the same beamline (ESRF) under the same conditions Therefore any change must be due to a change in the dispersoid structure The graph especially shows in the second shell a significant change in the spectra The structural change by itself must still be understood and is subject of future work Fe-edge By looking at the iron-edge EXAFS is sensing the bulk structure This experiment is only performed for the samples being irradiated with the Juumllich cyclotron at 571 K and for its reference Both spectra are again taken at one beamline (ESRF) under the same conditions (Table 1) Again a clear difference is visible in the distribution function In the second shell a doubling of the peak can be identified after irradiation Whether this change can be associated with point defects must be shown by ab initio multiple scattering calculations of the EXAFS spectra

Summary

Samples irradiated under two different environmental conditions are investigated by EXAFS addressing both the dispersoids and the matrix of the ODS composite When looking at the dispersoids a clear difference can be identified between the samples being irradiated at room temperature and at 571 K The dispersoids remain stable at room temperature whereas at 571 K a clear change in their structure can be identified When looking at the matrix the irradiation at 571 K also shows a clear effect on the structure For a further understanding of the damage mechanism more work towards the spectra modelling must and will be preformed

Acknowledgements

Two of the authors (MA Pouchon and J Chen) acknowledge the partial support of the work by the European FP6 projects RAPHAEL and EXTREMAT

References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

[2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) p 277-287

[3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

[4] Dispersion-Strengthened High-Temperature Materials Material properties and applications Prospectus from Plansee 2003 706 DE0403(1000)RWF

[5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

[6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3) (2007) p 253-258

[7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press doi101016jjnucmat200704051

[8] BM1B Main Page Last retrieved Mai 31st 2007 from lthttpwwwesrfeuexp_facilitiesBM1AindexBhtmgt

[9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

1764 PRICM 6

PRICM 6 104028wwwscientificnetMSF561-565 EXAFS Study on Irradiated ODS Ferritic Steel 104028wwwscientificnetMSF561-5651761

DOI References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) 277-

287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater ol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719 [1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Mslang and JA Schrder Powder Metall B Vol 48 (3) (2005) p 277-287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Dbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719

Page 3: EXAFS Study on Irradiated ODS Ferritic Steel

Results and Discussion

This paper presents the experimental results The radiation and temperature depending behavior of the EXAFS spectra and its Fourier transform already represent by themselves an important proposition EXAFS is a technique which probes the coordination environment of a selected absorbing atom With this information the structure containing the absorbing atom can be reconstructed If no change is found in the spectra the investigated structure remained stable Otherwise a change was induced This change can be due to a phase transformation due to point defects and clusters or due to bubble formation and the resulting stress fields For a detailed analysis all the possibilities must be simulated using an ab initio multiple scattering calculations of the EXAFS spectra Y-edge By looking at the yttrium-edge EXAFS is sensing the structure of the dispersoids As mentioned before these very fine particles are the basis of the enhanced creep behavior of ODS materials and their integrity is important to guarantee the long term properties of the composite If the EXAFS signal changes as a function of the exposure (temperature irradiation and mechanical load) the change must be understood in order to judge its influence to the changed material performance The samples irradiated with the tandem accelerator at room temperature does not show changes in the EXAFS signal which would indicate a change in the dispersoid structure (see Fig 1a in the lower graph) The reference spectra has been taken at low temperature and therefore shows different peak intensities nevertheless the peak locations and shapes compare very well for the reference and the irradiated samples [6] It can therefore be concluded that under the given irradiation conditions the

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6

Houmlnggerberg

Juumllichirradiated |F

(ω(k)χ(k)middotksup3)| [Aring-4

]

reference |F(ω

(k)χ(k)middotksup3)| [Aring-4]

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10R [Aring]

-5

0

5

10

15

20

25

irradiated |F

(ω(k)χ(k)middotksup3)| [Aring-4]

reference |F(ω

(k)χ(k)middotksup3)| [Aring-4]

Fe

Y

a)b)

Figure 1 Fourier transforms of the EXAFS results In each graph the distribution function of the

reference samples is represented by the upper curve with its ordinate on the right side The irradiated samples are represented by the lower curve with the ordinate to the left a) Y-edge the lower graph shows the Fourier transform of the samples being irradiated at room temperature with 15 MeV ions (see also [6]) The reference here derives from [1] The upper graph shows the Fourier transform of the EXAFS taken from the 0-24 MeV irradiation at 571 K Here a box emphasizes the most interesting change in the distribution function b) Fe-edge Fourier transforms taken for a reference and a sample implanted with 0-24 MeV He ions A box emphasizes the most interesting change in the distribution function

Materials Science Forum Vols 561-565 1763

dispersoids remain stable In the actual experiment the samples are trough irradiated at 571 K The corresponding spectrum together with the reference is shown in Fig 1a in the upper graph Both spectra have been taken at the same beamline (ESRF) under the same conditions Therefore any change must be due to a change in the dispersoid structure The graph especially shows in the second shell a significant change in the spectra The structural change by itself must still be understood and is subject of future work Fe-edge By looking at the iron-edge EXAFS is sensing the bulk structure This experiment is only performed for the samples being irradiated with the Juumllich cyclotron at 571 K and for its reference Both spectra are again taken at one beamline (ESRF) under the same conditions (Table 1) Again a clear difference is visible in the distribution function In the second shell a doubling of the peak can be identified after irradiation Whether this change can be associated with point defects must be shown by ab initio multiple scattering calculations of the EXAFS spectra

Summary

Samples irradiated under two different environmental conditions are investigated by EXAFS addressing both the dispersoids and the matrix of the ODS composite When looking at the dispersoids a clear difference can be identified between the samples being irradiated at room temperature and at 571 K The dispersoids remain stable at room temperature whereas at 571 K a clear change in their structure can be identified When looking at the matrix the irradiation at 571 K also shows a clear effect on the structure For a further understanding of the damage mechanism more work towards the spectra modelling must and will be preformed

Acknowledgements

Two of the authors (MA Pouchon and J Chen) acknowledge the partial support of the work by the European FP6 projects RAPHAEL and EXTREMAT

References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

[2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) p 277-287

[3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

[4] Dispersion-Strengthened High-Temperature Materials Material properties and applications Prospectus from Plansee 2003 706 DE0403(1000)RWF

[5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

[6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3) (2007) p 253-258

[7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press doi101016jjnucmat200704051

[8] BM1B Main Page Last retrieved Mai 31st 2007 from lthttpwwwesrfeuexp_facilitiesBM1AindexBhtmgt

[9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

1764 PRICM 6

PRICM 6 104028wwwscientificnetMSF561-565 EXAFS Study on Irradiated ODS Ferritic Steel 104028wwwscientificnetMSF561-5651761

DOI References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) 277-

287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater ol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719 [1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Mslang and JA Schrder Powder Metall B Vol 48 (3) (2005) p 277-287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Dbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719

Page 4: EXAFS Study on Irradiated ODS Ferritic Steel

dispersoids remain stable In the actual experiment the samples are trough irradiated at 571 K The corresponding spectrum together with the reference is shown in Fig 1a in the upper graph Both spectra have been taken at the same beamline (ESRF) under the same conditions Therefore any change must be due to a change in the dispersoid structure The graph especially shows in the second shell a significant change in the spectra The structural change by itself must still be understood and is subject of future work Fe-edge By looking at the iron-edge EXAFS is sensing the bulk structure This experiment is only performed for the samples being irradiated with the Juumllich cyclotron at 571 K and for its reference Both spectra are again taken at one beamline (ESRF) under the same conditions (Table 1) Again a clear difference is visible in the distribution function In the second shell a doubling of the peak can be identified after irradiation Whether this change can be associated with point defects must be shown by ab initio multiple scattering calculations of the EXAFS spectra

Summary

Samples irradiated under two different environmental conditions are investigated by EXAFS addressing both the dispersoids and the matrix of the ODS composite When looking at the dispersoids a clear difference can be identified between the samples being irradiated at room temperature and at 571 K The dispersoids remain stable at room temperature whereas at 571 K a clear change in their structure can be identified When looking at the matrix the irradiation at 571 K also shows a clear effect on the structure For a further understanding of the damage mechanism more work towards the spectra modelling must and will be preformed

Acknowledgements

Two of the authors (MA Pouchon and J Chen) acknowledge the partial support of the work by the European FP6 projects RAPHAEL and EXTREMAT

References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

[2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) p 277-287

[3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

[4] Dispersion-Strengthened High-Temperature Materials Material properties and applications Prospectus from Plansee 2003 706 DE0403(1000)RWF

[5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

[6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3) (2007) p 253-258

[7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press doi101016jjnucmat200704051

[8] BM1B Main Page Last retrieved Mai 31st 2007 from lthttpwwwesrfeuexp_facilitiesBM1AindexBhtmgt

[9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

1764 PRICM 6

PRICM 6 104028wwwscientificnetMSF561-565 EXAFS Study on Irradiated ODS Ferritic Steel 104028wwwscientificnetMSF561-5651761

DOI References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) 277-

287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater ol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719 [1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Mslang and JA Schrder Powder Metall B Vol 48 (3) (2005) p 277-287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Dbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719

Page 5: EXAFS Study on Irradiated ODS Ferritic Steel

PRICM 6 104028wwwscientificnetMSF561-565 EXAFS Study on Irradiated ODS Ferritic Steel 104028wwwscientificnetMSF561-5651761

DOI References

[1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Moumlslang and JA Schroumlder Powder Metall B Vol 48 (3) (2005) 277-

287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Doumlbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater ol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719 [1] C Degueldre S Conradson and W Hoffelner Comput Mater Sci 33 (2005) 3-12

doi101016jcommatsci200412019 [2] M Klimiankou R Lindau A Mslang and JA Schrder Powder Metall B Vol 48 (3) (2005) p 277-287

doi101179174329005X64171 [3] S Ukai M Fujiwara J Nucl Mater Vol 307-311 (2002) p 749-757

doi101016S0022-3115(02)01043-7 [5] MA Pouchon J Chen M Dbeli and W Hoffelner J Nucl Mater Vol 352(1-3) (2006) p 57-61

doi101016jjnucmat200602070 [6] MA Pouchon AJ Kropf A Froideval C Degueldre and W Hoffelner J Nucl Mater Vol 362(2-3)

(2007) p 253-258

doi101016jjnucmat200701123 [7] J Chen P Jung MA Pouchon T Rebac and W Hoffelner J Nucl Mat (2007) in press

doi101016jjnucmat200704051 [9] B Ravel M Newville J Synchrotron Rad Vol 12 (2005) p 537-541

doi101107S0909049505012719