Material for European XFEL Cavity Production

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Material for European XFEL Cavity Production X. Singer, W. Singer, Presented by Xenia Singer

Main issues 2 Requirement to cavity material for XFEL Qualification of Nb suppliers for XFEL Current status of the material contract for XFEL cavity

Technical Specification for High Purity Niobium for SC Cavities Concentration of impurities in wt.ppm Mechanical properties Ta* 500 H* 2 Yield strength**, σ 0,2 50<σ 0,2 <100 N/mm 2 (Mpa) W* 70 N* 10 Tensile strength** > 100 N/mm 2 Ti* 50 O* 10 Elongation at break** Fe* 30 C* 10 Vickers hardness** HV 10 Mo* 50 RRR* 300 Absence of foreign material inclusions* Ni* 30 Recrystal. degree. Grain size*,**? 50 μm Texture *, **? (Mpa) 30 % 60 * - relevant for performance ** - relevant for fabrication Proven by scanning

Fabrication schema of Nb sheets at Tokyo Denkai (courtesy of Tokyo Denkai) Mother material Forging Cutting Pressing Milling Annealing 1st EB melting Rolling Levering 2nd, 3rd etc. EB melting Separate from base plate In the final sheet the purity of niobium should be not inferior as in the ingot Polishing Rolling Chemical polishing Inspection L-He ICP-AES Gas Analysis RRR Grain size Hardness Tensile tests

HERAEUS Structure of Nb on different stages of sheet production Rolled Nb sheet before final annealing Examples of bad recrystallization. Ingot After forging Rolled rough plate Recrystallized niobium sheet Task: starting with cm size grain of ingot finish with ca. 50 µm uniform grain without contamination of Nb

The world's largest niobium deposit is located in Araxá, Brazil (CBMM). The mining of weathered ore, running between 2.5 and 3.0% Nb 2 O 5, is carried out by open pit mining. 85 to 90% of the niobium industry obtains its niobium ores.

PPR 2-2009 There are several companies, which can produce high purity Nb in larger quantities: Wah Chang (USA), W.C.Heraeus (Germany), Tokyo Denkai (Japan), Ningxia (China), CBMM (Brasil),, USA) Control room (Wah Chang) Electron beam melting furnace of CBMM (Brazil) EB melting after liquid-liquid extraction and ATR (aluminum thermal reduction WP-X, Speaker Name XFEL Project Progress Report (2-2009) 1 st & 2 nd Dec. 2009

Electron Beam Melting of Niobium 8 Electron Beam Gun Starting Ingot (Rotating) Focus & Aiming Coils lectron Beam Vacuum Water Cooled Crucible Ingot Molten Pool

9 The melting temperature is a compromise between the maximization of purification and minimization of the material losses by evaporation. RRR=300-500 are reachable currently

Independent from company QC and acceptance on company site are indispensable In House (DESY) RRR Scanning - Apparatus Interstitial impurity analysis (H,N,O, C) Metallic impurities analysis (another RM, Fe, Ni etc.) Metallography Tensile test Hardness, HV Surface roughness Thermal conductivity Scheme of QC of Nb sheets Outsource NAA Neutron Activation Analysis Radiation Fluorescence Analysis SEM, EDX SIMS, XPS, AUGER X-ray radiography Neutron radiography Texture analysis Bulging test

Qualification of Nb suppliers for XFEL Three qualification steps Step 1. Material testing (RRR, Microstructure, Eddy current scanning, Tensile test, HV, Impurity content, Surface conditions etc.). Step 2. Single cell cavity fabrication, treatment and RF tests at DESY. Step.3. 9-cell cavity fabrication at Industry, treatment at DESY and RF tests. 11 OTIC Ningxia Plansee XFEL Requirement XFEL Requirement RF test results of 9 cell cavities produced from material of Plansee (Austria) and Ningxia OTIC (China). Only this companies successfully passed all qualification steps. 5 qualified suppliers now.

RRR 1000 800 600 400 200 0 0 2 4 6 8 Blech Nr. RRR values of Nb produced at GIREDMET (Russia) Chemical analysis: Ta = 6 wt. ppm, N = 1 wt. ppm, O = 5 wt. ppm, W, Ti, Fe, Si, Mo, Ni < 5 wt. ppm all together The EB melting technique in combination with advanced Nb -Ta separation allows to reach very high RRR values (700-1000)

Status: Material for XFEL Cavities Material for 800 Cavities will be provided by DESY to RI and E.ZANON Mid 2011 Mid 2013 Contracted to companies: W.C. Heraeus (Germany) Tokyo Denkai (Japan) OTIC Ningxia (China) SE Plansee (Austria) >20 000 pieces of semifinished products (sheets, tubes, etc.)

Eddy current scanning Principle of eddy current measurement Equipment for eddy current scanning of ca. 16.000 XFEL niobium sheets at DESY

Foreign material inclusions in the cavity Temperature mapping: Cavity D6 with Eacc=13 MV/m shows excessive heating at a localized spot Positive print of a X-ray radiograph (X-Ray irradiation and imaging) showing the hot spot as a dark point (0.2 mm large Ta inclusion).

Local defects Iron signal distribution in one of the locations of the Nb sheet T17 measured Synchrotron Radiation Fluorescence Analysis (SURFA) and defects image. Iron particles, probably imbedded during rolling T17

PPR 2-2009 Status Niobium and NbTi material for XFEL Cavities 17 Equipment for tactile 3D dimension measurement Four previously qualified companies (Heraeus, Tokyo Denkai, Ningxia OTIC and Plansee) are contracted for cavity material supply Supervision of production at companies; incoming control, scanning, documentation and delivery to RI and EZ of cavity material is task of DESY. (status 3/2012). >70% of all niobium incl. sheets, tubes etc. delivered to cavities vendors Material for Option 80+160 cavities contracted. Equipment for sheets marking WP-X, Speaker Name XFEL Project Progress Report (2-2009) 1 st & 2 nd Dec. 2009

Material PED (Pressure Equipment Directive) activities The cavity and helium tank material has to be produced according PED/97/23/EC 18 PED Activities on Material for Cavities and Helium Tanks Qualification of cavity material Nb40, Nb300, NbTi, Ti1, Ti2 (creation the particular material appraisal (PMA) by notified body). Certification of QM system at the companies (producing cavity material). Tokyo Denkai and Ningxia OTIC certified by TUEV NORD. Certification of QM system at the company Skodock (producing bellows for helium tank) by TUEV NORD. Supervising of the semi finished material products procurement (traceability, marking, Acceptance of Nb sheets at Ningxia 3.1 test certificates). OTIC (courtesy of NOTIC)

Status of material shipment from DESY to RI and E.Zanon 19 Example of first shipment to E.Zanon/RI Mid July 2011 (55 boxes) Shipment status end of July 2012

R&D: Large Grain LG Cavity for European XFEL LG ingot and disc fabrication Cutting of the large grain Ingots by wire sawing at W.C.Heraeus Development of LG disc production was done within the framework of the XFEL R&D program of DESY and the W. C. HERAEUS.

R&D: Large Grain LG Cavity for XFEL. The R&D must be completed before TT starts BCP only XFEL Requirement 11nine-cell DESY cavities from LG Nb of Fa. HERAEUS are fabricated at Fa. RI Treatment: 100µm BCP, 800 C 2h, 20µm BCP, HPR and 125 C, 50 h baking.

Eacc up to 45 MV/m after add. EP World record 22 XFEL Requirement Encouraging results, but the time was not sufficient to finish R&D. One cryomodule with 8 LG Cavities will be produced for European XFEL

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