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Niobium superconduct or sheet rolling – Results of Preliminary Tests 2019. January

Niobium superconduct or sheet rolling – Results of Preliminary Tests 2019. January. University of Miskolc, Faculty of Material Science and Engineering Institute of Physical Metallurgy, Metalforming and Nanotechnology, Laboratory of Image and Structure Analysis (LISA) Hungary , 3DLab.

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Niobium superconduct or sheet rolling – Results of Preliminary Tests 2019. January

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  1. Niobium superconductor sheet rolling – Results of PreliminaryTests2019. January University of Miskolc,Faculty of Material Science and Engineering Institute of Physical Metallurgy, Metalforming and Nanotechnology, Laboratory of Image and Structure Analysis (LISA) Hungary, 3DLab University of Miskolc Miskolc-Egyetemvaros 3515, Hungary Prof. Valeria Mertinger, Head of Institute femvali@uni-miskolc.hu 36-30-20183699

  2. Participants

  3. Work schedule

  4. Sampleidentification „CERN ID #3” „CERN ID #2” „CERN ID #4” 2 Parallel rolling withoutcutting 4 Parallel rolling withcutting 6 Crossrolling withoutcutting 3 Crossrolling withcutting 5 1 1 W2 1 W1

  5. CERN characterisation „longest” „shortest”

  6. Cutting tests Laser cut- con: heat effect - no option Mechanical (CNC machining)- stiffness problem, fixing, geometrical limitation Water jet cut- satisfactory results- our chosen technology EDM- limited access- still option

  7. Characterisation and Mechanicaltests of thebasematerial Cutting of basematerial: …bya dense toothed saw blade ID 1 W1 and 1 W2 Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test Conventionalrolling of narrowsample No1 XRD, SEM, EDX Sixpieces of cylindrical specimen

  8. OpticalMicroscopy – Nb-Initialsheet Transversesection Longitudinalsection Basematerial

  9. Initialsample- samplesizesuitability (211) (200) (310)

  10. Initial- Polefigures – {110} W1 CrossrolledFe ConventionalrolledFe Tmax=2.55 Tmax=2.36 Tmax=6.41 Tmax=4.03 Tmax=2.79 Tmax=1.98 Shearcomponent University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  11. Initial- Polefigures – {200} W1 CrossrolledFe ConventionalrolledFe Tmax=11.21 Tmax=1.94 Tmax=4.30 Tmax=7.36 Tmax=2.48 Shearcomponent University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  12. Initial-Polefigures – {200} InitialPolefigures – {110} W1 W1-other side W1-other side W1 Tmax=24.51 Tmax=11.21 Tmax=6.41 Tmax=6.15 Thus, W1 sample is probably cross rolled, but rolling in one direction caused more deformation than in the other direction. Tmax=9.2 Tmax=7.36 Tmax=4.03 Tmax=4.31 Shearcomponent Shearcomponent

  13. Watts-Ford test (plainstraincompression test) Mechanicaltests of thebasematerialand rolledNb Conditions: Notations: s0 – initial thickness of specimen b – initial length of specimen w – width of dies F- force Toolsizes: Dies with different width Inserted die in holder • Cutting and Preparation of Nb • Watts- Ford test • Tensile Test • Hardness • Anisotropy test FE simulation of Nbconv. and crossrolling

  14. Multi - Step Compression Test of Nb cylindrical specimen: • ~ 0.5 mm reduction per step • Optical measurement of the minimum and maximum diameters after each step Mechanicaltests of thebasematerial • Cutting and Preparation of Nb • Watts- Ford test • Tensile Test • Hardness • Anisotropy test H

  15. Conclusions of theinitialsamples • Non-uniform grainsize • Anisotropy of initial material confirmed • As received material produced by cross rolling assumed • Texture shows different frictional conditions on two sides • Niobium exhibits good formability

  16. Rolling parameters: • Two High Rolling Mode • Roll diameter x length: 220 mm x 220 mm • Liquid lubricant: mineral oil based(PetroPal – commonly used for cold rolling of aluminium strip) • Rolling Speed: 30 m/min • Sample geometry: 50 x 50 x 4 (mm) • Using the same unloaded rolling gap for each paralell pass • Measured data: force and torque Rolling tests • Cutting and Preparation of Nb • Rolling test of AlMg3 samples • Comparative test of AlMg3 & Nb • First experimental rolling of parallel samples (ID „3”; ID „4”) • Second experimental rolling of parallel samples (ID „5”; ID „6”)

  17. Narrow sample rolling of Aluminium and Nb: • samples geometry are the same: 20 x 50 x 4 (mm) • to evaluate the rolling gap under the condition of cold rolling • Final thickness after 10 rolling passes • same unloaded rolling gap for both material Conventionalrolling of Niobium Nbsample ID „1” Cutting and Preparation of Nb Rolling test of AlMg3samples Comparative test of AlMg3 & Nb Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) Secondexperimentalrolling of parallel samples (ID „5”; ID „6”) • Microstructuralanalysis: • Texture • Optical • DSC

  18. Rolledsheet – Hardness Nb 1.10 – rolled

  19. Additional measurements are running (?Endo) DSC measurement 1_10 1_6 Victor Pantsyrny: 08.02.2019.: recryst 900-950°C

  20. OpticalMicroscopy – Nb 1.6 BeforeDSC 50x 100x 200x Coarse grain after recrystallization and grain growth AfterDSC University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  21. OpticalMicroscopy – Nb 1.10 BeforeDSC 50x 100x 200x Coarse grain after recrystallization and grain growth AfterDSC University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  22. Conventionalrolling, 1.6, 1.10 Polefigures – {200} Polefigures – {110} 1.10, phi=2.667 1.10, phi=2.667 • 1.6, phi=1.435 • 1.6, phi=1.435 Tmax=1.95 Tmax=2.49 Tmax=7.43 Tmax=4.5 Tmax=1.89 Tmax=3.23 Tmax=2.0 Tmax=4.68

  23. Roll bonding Rolling multilayer Cu+Nbfor adhesion test (Cladding test) There is room for improvement. Heat treatment tests.- 1_10 sample Protective atmosphere is needed!!!

  24. Cutting of basematerial: Conventional & Cross Rolling of Niobium Conventionalrolling withoutcutting 4 Conventionalrolling withcutting 6 …bya dense toothed saw blade Crossrolling withoutcutting 3 Crossrolling withcutting 5 • Cutting and Preparation of Nb • Rolling test of AlMg3samples • Comparative test of AlMg3 & Nb • Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) • Secondexperimentalrolling of parallel samples (ID „5”; ID „6”)

  25. Aluminiumsamplesrolling: • alloy: 5056 AA (DIN) or AlMg3) • approximately the force, the moment requirement • to evaluate the rolling gap under the condition of cold rolling • successfulcomparabilityexpected • flow stressesareclosetoeachother • samplesgeometryarethesame • Sixpassrolling Conventional & Cross Rolling of Niobium • Cutting and Preparation of Nb • Rolling test of AlMg3samples • Comparative test of AlMg3 & Nb • Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) • Secondexperimentalrolling of parallel samples (ID „5”; ID „6”) conv. rolled: crossrolled:

  26. Conventionalrolling of „3” sample Conventional & Cross Rolling of Niobium Analysis: • Microstructure • Mechanical • Texture Crossrolling of „4” sample • Cutting and Preparation of Nb • Rolling test of AlMg3samples • Comparative test of AlMg3 & Nb • Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) • Secondexperimentalrolling of parallel samples (ID „5”; ID „6”) Analysis: • Microstructure • Mechanical

  27. Conventionalrolling of „5” sample Conventional & Cross Rolling of Niobium Analysis: • Microstructure • Cutting and Preparation of Nb • Rolling test of AlMg3samples • Comparative test of AlMg3 & Nb • Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) • Secondexperimentalrolling of parallel samples (ID „5”; ID „6”) Crossrolling of „6” sample Analysis: • Microstructure

  28. Conventional & Cross Rolling of Niobium • Cutting and Preparation of Nb • Rolling test of AlMg3samples • Comparative test of AlMg3 & Nb • Firstexperimentalrolling of parallel samples (ID „3”; ID „4”) • Secondexperimentalrolling of parallel samples (ID „5”; ID „6”) http://www.uni-miskolc.hu/~femgabor/50x50_niobium_sheet_rolling.mp4

  29. Rolling - Images 3.6, 4.6 Nbsheetsafterthe 6th pass 3.8, 4.8 Nbsheets, finished

  30. Polefigures – {110} Conventionalrolling 5.4, phi=0.653 3.8, phi=1.656 • 5.2, phi=0.289 Tmax=1.83 Tmax=1.89 Tmax=1.67 Tmax=1.4 1 Tmax=1.72 Tmax=1.47 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  31. Polefigures – {200} Conventionalrolling 5.4, phi=0.653 3.8, phi=1.656 • 5.2, phi=0.289 Tmax=3.63 Tmax=6.11 Tmax=3.93 Tmax=2.82 Tmax=2.26 Tmax=1.96 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  32. Polefigures – {220} Conventionalrolling 5.4, phi=0.653 3.8, phi=1.656 • 5.2, phi=0.289 Tmax=2.98 Tmax=3.47 Tmax=3.20 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  33. Polefigures – {110} Crossrolling 6.4, phi=0.658 4.8, phi=1.559 • 6.2, phi=0.294 Tmax=1.75 Tmax=1.92 Tmax=3.05 Tmax=1.4 5 Tmax=1.28 Tmax=1.94 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  34. Polefigures – {200} Crossrolling 6.4, phi=0.658 4.8, phi=1.559 • 6.2, phi=0.294 Tmax=14.10 Tmax=3.24 Tmax=6.22 Tmax=1.88 Tmax=2.5 Tmax=3.36 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  35. Crossrolling Polefigures – {220} 6.4, phi=0.658 4.8, phi=1.559 • 6.2, phi=0.294 Tmax=3.07 Tmax=3.84 Tmax=6.34 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  36. X-raypenetrationdepths University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  37. ODF Nb 3.8 – 4.8 Conventionalrolling Crossrolling Nb 4.8 Nb 3.8 University of Miskolc,Institute of Physical Metallurgy, Metalforming and Nanotechnology, Hungary

  38. Cut-pattern – Images A2 Alsheet’scut-pattern 3.8, 4.8 Nbsheets, cut-pattern

  39. Mechanicaltests of thebasematerial and rolledNb Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test

  40. Mechanicaltests of thebasematerial and rolledNb Rolling direction Conventional Rolling: ID „3” Rolling direction Cross Rolling: ID „4” rotatearoundnormaldirection Rolling direction Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test Twopieces of flattensile test specimen per direction (0°; 22,5°; 45°; 67,5°; 90°)

  41. Mechanicaltests of thebasematerial and rolledNb Rolling direction Conventional Rolling: ID „3” Rolling direction Cross Rolling: ID „4” rotatearoundnormaldirection Rolling direction Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test Twopieces of flattensile test specimen per direction (0°; 22,5°; 45°; 67,5°; 90°)

  42. Tensile Test of rolled Nb: • Directional dependent mechanical properties • Measurement of longitudinal elongation by video extensometer • GOM analysis of longitudinal and transversal elongation Mechanicaltests of thebasematerial and rolledNb Geometry of flat specimen: • Cutting and Preparation of Nb • Watts- Ford test • Tensile Test • Hardness • Anisotropy test

  43. Conventionalrolled specimen - stressstraincurve Mechanicaltests of thebasematerial and rolledNb S3 Crossrolled specimen - stressstraincurve Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test

  44. AnisotropyTest ofrolledNb: • Onthebasis of Stress Ratio • Directiondependentmechanicalproperties Mechanicaltests of thebasematerial and rolledNb Cutting and Preparation of Nb Watts- Ford test Tensile Test Hardness Anisotropy test

  45. The three Niobium samples (100x50x4mm) sent by CERN were examined. 17/12/2018- 10/02/2019 • MU has performed DSC tests to obtain the recrystallization temperature of Niobium after rolling • or on the part of the deep drawn leftover component after receiving. • MU has not yet performed metallography + hardness profile on the samples sent, in order to assess homogeneity of deformation along the thickness (for both rolling directions) when cross rolling of Nb sheet. Clarification is needed. • Evaluation of the effect of cross rolling (comparison of effect of unidirectional and cross rolling) was performed. • CERN provided details on metallographic preparation procedure for Niobium. • Conventional and cross rolling experiment were carried out. Rolling parameters were experimentally determined based on aluminium alloys experiments. • XRD texture tests were performed on initial and rolled samples. Pole figure and ODF syntheses were obtained. • CERN will send a part of the leftover after deep drawing to MU for XRD testing. • Direction dependent tensile test specimens were obtained (water jet cutting) and anisotropy results were presented. • Conventional and cross rolling effects were compared. Summary and results

  46. Open issues and tests in progress • Tensile test with GOM • EBSD tests • Left over part investigation (after deep drawing) • DSC of rolled sheets for confirmation of recrystallization • OM (SEM) investigation • XRD LPA • Writtenreport

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