Texture development during rolling of α + β dual phase ZrNb alloys

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1 Texture development during rolling of α + β dual phase ZrNb alloys Christopher S. Daniel 1, Peter D. Honniball 2, Luke Bradley 2, Michael Preuss 1, João Quinta da Fonseca 1 1 The University of Manchester, Manchester, UK 2 Rolls-Royce plc, Derby, UK

2 Industrial Relevance Zr alloys: Structural Components, Cladding, Pressure Tubing. α - hcp β - bcc 20μm Pressurised Water Reactor (PWR) schematic; nuclear fuel assembly; α + β dual phase ZrNb alloy microstructure. α + β dual phase ZrNb alloys offer higher strength and fracture toughness, with improved corrosion properties compared to single phase α Zr alloys. 2

$α + β dual phase ZrNb alloys offer higher strength and fracture toughness, with improved$

3 Industrial Relevance Zr alloys: Structural Components, Cladding, Pressure Tubing. α - hcp β - bcc 20μm High temperature rolling ZrNb alloy at Manchester; nuclear fuel assembly; α + β dual phase ZrNb alloy microstructure. α + β dual phase ZrNb alloys offer higher strength and fracture toughness, with improved corrosion properties compared to single phase α Zr alloys. 3

In-Reactor Texture Effects Texture Distribution of crystallographic orientations. Fuel assembly buckling.

1 In-reactor texture determines 2 Yield and creep strength, SCC, Irradiation growth, Hydride precipitate cracks.

3 Require better understanding, to predict effect of processing parameters manufactured texture in ZrNb alloys. [1] Mahmood, S. T.

4 In-Reactor Texture Effects Texture Distribution of crystallographic orientations. Fuel assembly buckling. Basal pole orientation in cladding and pressure tubing. 1 In-reactor texture determines 2 Yield and creep strength, SCC, Irradiation growth, Hydride precipitate cracks. Hydrides in Zr alloy tube. 3 Require better understanding, to predict effect of processing parameters manufactured texture in ZrNb alloys. [1] Mahmood, S. T. Mechanical Testing of Zirconium Alloys. in ZIRAT18 Semin (ANT International, 2014). [2] Banerjee, S. in Encycl. Mater. Sci. Technol. (Cahn, K. H. et al.) (Elsevier Science Ltd., 2001). doi: /b / [3] Adamson, R. B. et al. Mechanical Testing of Zirconium Alloys - Hydrides (Volume: 1, Section: 11). in ZIRAT18 Semin (ANT International, 2014). 4

Texture Development Rolling / Pilgering / Extrusion Microstructure reorientation via Slip, Twinning,

1 Body-centred cubic (bcc) slip systems {110} β 0001 α and < 111 > β < 1120 > α Burger s relationship for

4 Texture evolution of α + β dual phase ZrNb alloys depend on plastic strain (rate) partitioning. [1] Mahmood, S. T. Mechanical Testing of Zirconium Alloys.

5 Texture Development Rolling / Pilgering / Extrusion Microstructure reorientation via Slip, Twinning, Recrystallisation. τ = F A cosϕcosλ. Slip planes of the hexagonal close-packed (hcp) lattice. 1 Body-centred cubic (bcc) slip systems {110} β 0001 α and < 111 > β < 1120 > α Burger s relationship for crystallographic α β and β α phase transformation. 4 Texture evolution of α + β dual phase ZrNb alloys depend on plastic strain (rate) partitioning. [1] Mahmood, S. T. Mechanical Testing of Zirconium Alloys. in ZIRAT18 Semin (ANT International, 2014). [4] Daymond, M. R. et al. Texture inheritance and variant selection through an hcp bcc hcp phase transformation. Acta Mater. 58, (2010). 5

6 Dual Phase α Texture Development {0002} {1120} ND Single phase α texture Dual phase α texture {0002} {1120} Rolling schematic Pole figure comparison for CW single phase α Zr and hot-rolled dual phase α + β ZrNb alloy. Rolling tests to decouple Deformation mode activation, 5 α - β phase interaction, 6 Phase transformation during heating / cooling, 7 Effect of annealing. Using ex-situ EBSD measurement. [5] Honniball, P. D. et al. Grain Breakup During Elevated Temperature Deformation of an HCP Metal. Metall. Mater. Trans. A 46, (2015). [6] Saibaba, N. et al. in Zircon. Nucl. Ind. 17th Vol (ASTM International, 2015). doi: /stp [7] Gey, N. et al. Modeling the transformation texture of Ti-64 sheets after rolling in the β-field. Mater. Sci. Eng. A 230, (1997). 6

$5%Nb and +7%Nb alloys, showing difference in α grain size and retained β fraction.$

7 Materials Zircaloy %Nb and +7%Nb. Temperature 800ºC Reduction 50% (2:1) and 75% (4:1) Heat-Treatment (HT) 2 hours at 750ºC Rolling at 800ºC Images of cast Zircaloy %Nb and +7%Nb alloys, showing difference in α grain size and retained β fraction.* +2.5%Nb +7%Nb 100μm *DIC optical micrographs taken with Zeiss Axio Scope.A1 7

$5%Nb and +7%Nb alloys, +2.5%Nb showing variation in β volume fraction with temperature.*,8 50% 50% HT 75% 75% HT *Results from Electro-Thermal Mechanical Tester (ETMT). [8] Fan, Z.$

8 Rolling at 800ºC Materials Zircaloy %Nb and +7%Nb. Temperature 800ºC Reduction 50% (2:1) and 75% (4:1) Heat-Treatment (HT) 2 hours at 750ºC β transus curves for Zircaloy %Nb and +7%Nb alloys, +2.5%Nb showing variation in β volume fraction with temperature.*,8 50% 50% HT 75% 75% HT *Results from Electro-Thermal Mechanical Tester (ETMT). [8] Fan, Z. A New Approach to the Electrical Resistivity of Two-Phase Composites. Acta Metall. Mater. 43, (1995). 8

9 Optical Microscopy 50% HT 50% HT 75% HT α β +2.5%Nb ND 100μm 20μm 50% β matrix 50% HT 75% HT 100μm Secondary α +7%Nb ND 100μm 100μm 20μm *DIC optical micrographs taken with Zeiss Axio Scope.A1 9

10 +2.5%Nb {0002} {1010} {1120} 50% 50% HT 75% 6mud 75% HT *Using FEI Sirion FEG-SEM and CamScan MX2000 SEM, with Channel 5 software analysis < 1010 > component 10

11 +2.5%Nb {0002} {1010} {1120} +7%Nb {0002} {1010} {1120} 50% 50% HT 75% 6mud 10mud 75% HT *Using FEI Sirion FEG-SEM and CamScan MX2000 SEM, with Channel 5 software analysis. 11

12 50% +2.5%Nb {0002} {1010} {1120} 75% HT +7%Nb Secondary α 50% HT ND 20μm 75% 6mud 10mud 75% HT *Using FEI Sirion FEG-SEM and CamScan MX2000 SEM, with Channel 5 software analysis. 12

13 +2.5%Nb +7%Nb Secondary α +2.5%Nb rolling texture results summary. +7%Nb rolling texture results summary. *Using FEI Sirion FEG-SEM and CamScan MX2000 SEM, with Channel 5 software analysis. 13

14 50% +2.5%Nb α Orientation 0002 aligned in rolling plane {0002} {1120} ND 1mm but lamellae not fully aligned. *Using FEI Sirion FEG-SEM, with Channel 5 software analysis. 14

15 +2.5%Nb α Orientation 50% 75% ND 1mm High temperature β reconstruction software. {110} β 0001 α and < 111 > β < 1120 > α 2º, 3º *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 15

+2.5%Nb α Orientation and β Reconstruction 75% 50% 50% ND β Reconstruction 75% 1000μm β Reconstruction 1mm *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, 2009.

16 +2.5%Nb α Orientation and β Reconstruction 75% 50% 50% ND β Reconstruction 75% 1000μm β Reconstruction 1mm *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 16

+2.5%Nb α Orientation and β Reconstruction {0002} {1120} 75% 1.

ND *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, 2009.

17 +2.5%Nb α Orientation and β Reconstruction {0002} {1120} 75% Phase transformation {110} {111} 75% β Reconstruction 1. ND *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 1mm 17

18 +2.5%Nb α Orientation and β Reconstruction 75% {0002} {1120} 2. 75% β Reconstruction β Reconstruction 1000μm 2. Variant selection {110} {111} 2. ND *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 1mm 18

+2.5%Nb α Orientation and β Reconstruction 75% {0002} {1120} 3.

19 +2.5%Nb α Orientation and β Reconstruction 75% {0002} {1120} Prismatic slip 75% β Reconstruction β Reconstruction 1000μm {110} {111} 3. ND *Using FEI Sirion FEG-SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 1mm 19

+2.5%Nb β Deformation Components α-fibre <110> {001}<110> to {111}<110> BCC Steel 11 γ-fibre {111} ND {111}<110> to {111}<112> +2.5%Nb α-fibre γ-fibre 50%, HT max. 5.3 75%, HT max.

20 +2.5%Nb β Deformation Components α-fibre <110> {001}<110> to {111}<110> BCC Steel 11 γ-fibre {111} ND {111}<110> to {111}<112> +2.5%Nb α-fibre γ-fibre 50%, HT max %, HT max. 9.9 [11] Kestens, L. & Jacobs, S. Texture Control During the Manufacturing of Nonoriented Electrical Steels. Texture, Stress. Microstruct. 1 9 (2008). 20

5.3 {0002} {1120} 75%, HT Measured α texture max. 9.9 6mud [12] Stanford, N.

21 +2.5%Nb Variant Selection α-fibre γ-fibre <110> {001}<110> to {111}<110> {111} ND {111}<110> to {111}<112> +2.5%Nb {0002} {1120} 50%, HT Transformed α variants 12 max. 5.3 {0002} {1120} 75%, HT Measured α texture max mud [12] Stanford, N. & Bate, P. S. Crystallographic variant selection in Ti 6Al 4V. Acta Mater. 52, (2004). 21

22 +7%Nb β Deformation Components Rotated cube Goss {001}<110> {110}<001> +2.5%Nb +7%Nb 50%, HT 75%, HT max. 5.3 max max. 9.9 max ND Rotated cube Goss 22

+7%Nb α Orientation and β Reconstruction 50%, HT {0002} {1120} 1.

ND 1mm *Using CamScan MX2000 SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, 2009.

23 +7%Nb α Orientation and β Reconstruction 50%, HT {0002} {1120} Phase transformation 50% β Reconstruction {110} {111} 1. ND 1mm *Using CamScan MX2000 SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 23

24 +7%Nb α Orientation and β Reconstruction 50%, HT {0002} {1120} 2. 50% β Reconstruction 2. Variant selection {110} {111} 2. ND 1mm *Using CamScan MX2000 SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 24

25 +7%Nb α Orientation and β Reconstruction 50%, HT 75%, HT 50% β Reconstruction 75% β Reconstruction ND 1mm *Using CamScan MX2000 SEM, with Channel 5 and β reconstruction software analysis. [9] P. S. Davies, University of Sheffield, [10] Glavicic, M. G. et al. Automated method to determine the orientation of the high-temperature beta phase from measured EBSD data Mater. Sci. Eng. A 351, (2003). 25

26 +7%Nb α Orientation and β Reconstruction {0002} {1120} 75%, HT Measured α Texture 75% β Reconstruction {0002} {1120} Transformed α Variants 12 1mm [12] Stanford, N. & Bate, P. S. Crystallographic variant selection in Ti 6Al 4V. Acta Mater. 52, (2004). 26

27 +7%Nb α Orientation and β Reconstruction Non- Reconstructed α (Primary) {0002} {1120} 75%, HT {0002} {1120} Reconstructed α (Secondary) 75% β Reconstruction Transformed α Variants 12 {0002} {1120} 1mm [12] Stanford, N. & Bate, P. S. Crystallographic variant selection in Ti 6Al 4V. Acta Mater. 52, (2004). 27

28 +7%Nb α Orientation and β Reconstruction Non- Reconstructed α (Primary) {0002} {1120} 75%, HT {0002} {1120} 75% 75% β Reconstruction Transformed α Variants 12 {0002} {1120} 1mm [12] Stanford, N. & Bate, P. S. Crystallographic variant selection in Ti 6Al 4V. Acta Mater. 52, (2004). 28

$In-Situ Neutron Diffraction d hkl = Neutron h 2sinθ B m(l 1 +L 2 ) t hkl Load partitioning. Large gauge vol. High temp. compression. Slow acquisition ~6 mins.$

29 In-Situ Neutron Diffraction d hkl = Neutron h 2sinθ B m(l 1 +L 2 ) t hkl Load partitioning. Large gauge vol. High temp. compression. Slow acquisition ~6 mins. RT α β 550ºC α β Load partitioning at RT and 550ºC. ISIS neutron spallation source and Engin-X facility. 13 ISIS, Engin-X facility with high temp. compression rig set-up. 13 [13] Santisteban, J. R., Daymond, M. R., James, J. a. & Edwards, L. ENGIN-X: a third-generation neutron strain scanner. J. Appl. Crystallogr. 39, (2006). 29

$In-Situ Neutron and Synchrotron Diffraction d hkl = Neutron h 2sinθ B m(l 1 +L 2 ) t hkl Load partitioning. Large gauge vol. High temp. compression. Slow acquisition ~6 mins.$ ISIS neutron spallation source and Engin-X facility. 13 Diamond synchrotron schematic. ETMT load test. [13] Santisteban, J. R., Daymond, M. R., James, J. a. & Edwards, L.

ISIS neutron spallation source and Engin-X facility. 13 Diamond synchrotron schematic. ETMT load test. [13] Santisteban, J. R., Daymond, M. R., James, J. a. & Edwards, L.

30 In-Situ Neutron and Synchrotron Diffraction d hkl = Neutron h 2sinθ B m(l 1 +L 2 ) t hkl Load partitioning. Large gauge vol. High temp. compression. Slow acquisition ~6 mins. Synchrotron 2d hkl sinθ B = nλ Load partitioning and texture analysis. 14 Small gauge vol. High temp. tensile. Fast acquisition ~10Hz. ISIS neutron spallation source and Engin-X facility. 13 Diamond synchrotron schematic. ETMT load test. [13] Santisteban, J. R., Daymond, M. R., James, J. a. & Edwards, L. ENGIN-X: a third-generation neutron strain scanner. J. Appl. Crystallogr. 39, (2006). [14] Romero, J., et al. Texture memory and variant selection during phase transformation of a zirconium alloy. Acta Mater. 57, (2009). 30

31 Aim to decouple; Results Summary Slip mode activation; α - β phase interaction; phase transformation; annealing. +2.5%Nb alloy; Higher α volume fraction, consistent with prismatic slip, Homogeneous β deformation (α and γ fibre components), Variant selection dependant on prior-β orientation, Texture strengthening during annealing. +7%Nb alloy; Lower α shear band formation in β (Goss component), Variant selection via anisotropic grain breakup, Secondary α growth strengthen 0002 / weaken prismatic. Limitations; Prior-β grain size, single temperature, load partitioning behaviour. Future Work; In-situ neutron/synchrotron diffraction, rolling matrix, CPFEM, 31

32 References [1] Mahmood, S. T. Mechanical Testing of Zirconium Alloys. in ZIRAT18 Semin (ANT International, 2014). [2] Banerjee, S. in Encycl. Mater. Sci. Technol. (Cahn, K. H. et al.) (Elsevier Science Ltd., 2001). doi: /b / [3] Adamson, R. B., Rudling, P. & Mahmood, S. T. Mechanical Testing of Zirconium Alloys - Hydrides (Volume: 1, Section: 11). in ZIRAT18 Semin (ANT International, 2014). [4] Daymond, M. R., Holt, R. A., Cai, S., Mosbrucker, P. & Vogel, S. C. Texture inheritance and variant selection through an hcp bcc hcp phase transformation. Acta Mater. 58, (2010). [5] Honniball, P. D., Preuss, M., Rugg, D. & Quinta da Fonseca, J. Grain Breakup During Elevated Temperature Deformation of an HCP Metal. Metall. Mater. Trans. A 46, (2015). [6] Saibaba, N. et al. in Zircon. Nucl. Ind. 17th Vol (ASTM International, 2015). doi: /stp [7] Gey, N., Humbert, M., Philippe, M. J. & Combres, Y. Modeling the transformation texture of Ti-64 sheets after rolling in the β-field. Mater. Sci. Eng. A 230, (1997). [8] Fan, Z. A new approach to the electrical resistivity of two-phase composites. Acta Metall. Mater. 43, (1995). [9] P. S. Davies, Investigation of Microstructure and Texture Evolution in the Near-α Titanium Alloy Timetal 834, University of Sheffield, [10] Glavicic, M. G., Kobryn, P. A., Bieler, T. R. & Semiatin, S. L. An automated method to determine the orientation of the high-temperature beta phase from measured EBSD data for the low-temperature alpha-phase in Ti 6Al 4V. Mater. Sci. Eng. A 351, (2003). [11] Kestens, L. & Jacobs, S. Texture Control During the Manufacturing of Nonoriented Electrical Steels. Texture, Stress. Microstruct. 1 9 (2008). [12] Stanford, N. & Bate, P. S. Crystallographic variant selection in Ti 6Al 4V. Acta Mater. 52, (2004). [13] Santisteban, J. R., Daymond, M. R., James, J. a. & Edwards, L. ENGIN-X: a third-generation neutron strain scanner. J. Appl. Crystallogr. 39, (2006). [14] Romero, J., Preuss, M. & Quinta da Fonseca, J. Texture memory and variant selection during phase transformation of a zirconium alloy. Acta Mater. 57, (2009). [15] Stark, A. et al. In Situ High-Energy X-ray Diffraction during Hot-Forming of a Multiphase TiAl Alloy. Metals (Basel). 5, (2015). 32

33 Acknowledgements The University of Manchester. Peter Honniball, Luke Bradley, Michael Preuss, João Quinta da Fonseca Profile: 33

19/03/2014. Research In Focus. Microstructural Control for Optimized Formability

19/03/2014. Research In Focus. Microstructural Control for Optimized Formability Conquering low formability for optimized microstructures Dr João Fonseca Conquering Low Formability for optimized microstructures Key Objectives AIM: Advance understanding and predictive modelling to enable