STATUS OF LHC COLLIMATOR MATERIAL RD Elena Quaranta

STATUS OF LHC COLLIMATOR MATERIAL R&D Elena Quaranta BE BEAM DEPARTMENT Working Group on Advanced Collimator Materials July 21 st 2014

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Materials for LHC collimators Type Material TCP/TCS § CFC (AC-150 -K) TCDI § R 4550 graphite TCLP § Copper OFE Already used in collimators active jaw TCT § Inermet 180 - § Molybdenum - § Glidcop Al-15 Already used for collimators, but not in the active jaw TCP/TCS § Silver-Diamond TCP/TCS/TCT § Molybdenum-Copper-Diamond TCP/TCS § Copper-Diamond R&D TCP/TCS/TCT § Molybdenum-Graphite TCT § Tungsten-Rhenium Ad. Col. Mat - 21/7/2014 Elena Quaranta 4

CFC AC-150 K • Developed by Tatsuno (Japan) Composition : • Graphite flakes • Carbon fibers Density: 1. 67 g/cm 3 Currently used as TCPs and TCSGs active jaw material Main limitations: Poor electrical conductivity (0. 18 MS/m) RF Impedance induced beam perturbations Limited Radiation Hardness Reduced Lifetime for LHC operations Need for replacing degraded Collimators Ad. Col. Mat - 21/7/2014 Elena Quaranta 5

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Collimator material R&D focused on Metal Matrix Composites combine the properties of Diamond and Graphite (high k, low CTE low r and) with those of Metals (σ Materials investigated are: el) • Silver-Diamond (Ag. CD) • Copper-Diamond (Cu. CD) • Molybdenum-Diamond (Mo. CD) • Molybdenum-Copper-Diamond (Mo. Cu. CD) • Molybdenum-Graphite (Mo. Gr). Ag. CD and Mo. CD are limited by, respectively, low melting temperature and difficulty to produce in large size and machine. Ag. CD Mo. Gr Mo. CD Cu. CD Ad. Col. Mat - 21/7/2014 Elena Quaranta 7

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Copper-Diamond composite • Developed by RHP-Technology (Austria) Composition : • 60%v diamonds (90% 100 µm, 10% 45 µm) • 39%v Cu powder (45 µm) • 1%v B powder (5 µm) • No diamond degradation • Thermal (~490 Wm-1 K-1) and electrical conductivity (~12. 6 MSm-1) • No direct interface between Cu and CD (lack of affinity). Partial bonding bridging assured by Boron Carbides limits mechanical strength (~120 MPa). n • Cu low melting point (1083 °C) tio Limita • CTE increases significantly with T due to high Cu content (from ~6 ppm. K-1 at RT up to ~12 -1 at 900 °C) ppm. K Ad. Col. Mat - 21/7/2014 Elena Quaranta r! to a m i l l for co BC “bridge” stuck on CD surface. No CD graphitization 9

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Molybdenum-Diamond composite • Mo. Cu. CD: co-developed by and (Italy) during 2010 -2011. Why adding Mo? Thermal stability (low CTE), mechanical strength, good affinity with C. Composition & main production parameters: • 40%v synthetic diamonds (45 µm) • 25%v Cu powder (45 µm) • 35%v Mo powder (5 µm) • Powders pre-cleaning under H 2 -N 2 atmosphere at 600°C • RHP: 30 min at 1200°C, 30 MPa applied pressure, reducing H 2 -N 2 atmosphere at 10 -4 mbar § Low melting phase (Cu) limiting operational temperature § Poor thermal properties (k=155 W/m. K) § Expensive raw materials and difficult sample machining Ad. Col. Mat - 21/7/2014 Elena Quaranta 11

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Molybdenum-Graphite composite • Mo. GR: co-developed by and (Italy) during 2011 -2012 Why switching to graphite? • • • Low CTE Low density High thermal conductivity High melting (degradation) point Lower cost (with respect to diamond) Use solid state reaction to obtain strong Mo 2 C-graphite interfaces: 2 Mo + C => Mo 2 C: stable, electrically conductive. The high content of Mo 2 C and the low strength of graphite however are limiting the material robustness … Ad. Col. Mat - 21/7/2014 Elena Quaranta 13

Molybdenum-Graphite composite • Mo. GRCF: co-developed by and 2012. • Addition of mesophase pitch-base carbon fibers • Liquid Phase Spark Plasma Sintering (>2500° C) (Italy) since Advantages of Carbon Fibers: • Mechanical strength • Thermal conductivity • Along with Mo. C 1 -x , catalyze graphitization process Ad. Col. Mat - 21/7/2014 Elena Quaranta 14

MG: composition and production Basic composition & main production parameters: • 40%v natural graphite flakes (Asbury) • 20%v short carbon fibers (300 µm, Cytek DKD) • 20%v long carbon fibers (3 mm, Granoc XN-100 -03 Z), blended • 20%v Mo powder (5 µm) • Powders pre-cleaning under H 2 -N 2 atmosphere at 600°C • RHP: complete melting of Mo 2 C at ~2600°C, 35 MPa applied pressure (in steps), reducing H 2 -N 2 atmosphere at 10 -4 mbar. Graphite and molybdenum powder Ad. Col. Mat - 21/7/2014 Elena Quaranta MG 5220 S plate 15

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Summary of the tests (1) Characterization AC-150 K Cu. CD MG 3110 P Thermo-physical properties Density LFA (cp, k, diffusivity) DIL (α) Emissivity Electrical properties Electrical conductivity (Sigma. Test v 2. 069) !! If interested, do not hesitate to ask for the values!! Ad. Col. Mat - 21/7/2014 Elena Quaranta 17

Main results of the tests Properties CFC Cu. CD Mo. Gr r [g/cm 3] 1. 67 5. 33 2. 65 ay, z(RT to 1200° C) [10 -6 K-1] -1. 32 7. 8 <1. 3 ax (RT to 1200° C) [10 -6 K-1] 9 - 7. 9 ky, z (RT) [W/m. K] 220 490 >770 kx (RT) [W/m. K] 55 - 85 sy, z (RT) [MS/m] 0. 18 12. 6 1. 1 sx (RT) [MS/m] 0. 04 - 0. 3 Ad. Col. Mat - 21/7/2014 Elena Quaranta 18

Summary of the tests (II) Characterization @Grindo. Sonic (Belgium) AC-150 K Cu. CD MG 3110 P Mechanical properties Elastic matrix constants Flexural strength (σfl) with Hopkinson Compressive strength * * * bar @Poli. To (Italy) Dynamic Outgassing Coating Ad. Col. Mat - 21/7/2014 On-going Elena Quaranta - Scheduled 19

Summary of the tests (III) Characterization AC-150 K Cu. CD MG-3110 P Irradiation 30 Me. V protons (KI, Russia) 26 Me. V C-ions (KI, Russia) 200 Me. V proton + spallation neutron (BNL, USA) On-going (on MG 5220 S) U-ions (GSI, Germany) Au-ions (GSI, Germany) Ad. Col. Mat - 21/7/2014 On-going Elena Quaranta 20

Au 24+ irradiation at GSI Eu. CARD 2 - WP 11: Collimator Materials for fast High Density Energy Deposition. Beam time: 13 th -23 rd July On-Line monitoring and Post. Mortem analysis on CFC, Cu. CD and MG 5220 S samples are ON-GOING to assess property degradation under Au ions irradiation. Many thanks to M. Tomut and GSI material research group Ad. Col. Mat - 21/7/2014 Elena Quaranta 21

Outline § Overview of present LHC collimator materials § Post LS 1 secondary collimator: material R&D ² Copper-Diamond composite ² Molybdenum-Graphite composite § Review of the tests § Summary

Summary ü Different materials investigated to replace CFC active jaw of secondary collimators for system upgrade ü Cu. CD and Mo. GRCF are the most performing materials so far ü Several tests (thermo-physical, mechanical, irradiation) performed/on going on present and possible future collimator materials Ad. Col. Mat - 21/7/2014 Elena Quaranta

Summary – what is still missing? § CFC: - Emissivity - Flexural test (with strain gauges) - Dynamic tests § Cu. CD: - Emissivity Flexural test (with strain gauges) Dynamic tests Elastic constants Compressive strength Outgassing § Mo. Gr: Ad. Col. Mat - 21/7/2014 Flexural test (with strain gauges) Dynamic tests Elastic constants Compressive strength Elena Quaranta

Thank you for your attention

Backup slides

Numero Placca ID Stampo %Vol %Vol Fibre Corte % Vol Fibre Lunghe Mo GR (CY) (GRA) 1 MG-1220 -A 70 x 55 mm 20 60 20 2 MG-1130 -A 70 x 55 mm 20 40 40 3 MG-1140 -A 70 x 55 mm 20 40 20 %Vol Altro T (C) t (s) 0 0 2200 1200 20 0 2200 1200 P Atmosphere (Mpa) Data Densita’ Compat. Teorica (g/cm 3) tazione (g/cm 3) Cond Elettrica (MS/m) 35 0. 1 mbar, 97%- Jun-12 N 2, 3% H 2 35 0. 1 mbar, 97%- Jul-12 N 2, 3% H 2 35 10 -3 mbar, 05/02/2013 vacuum 3. 9121 3. 68 94. 07% 0. 61 240 59 3. 9121 3. 65 93. 30% 0. 41 200 45 3. 9121 3. 65 93. 30% 0. 98 (centro) 315 53 3. 9121 3. 53 90. 23% 0. 3 200 37 3. 9121 3. 73 95. 35% 0. 42 205 77. 5 3. 8218 3. 66 95. 77% 0. 27 139 49 3. 8218 3. 68 96. 29% 0. 41 187 43 3. 9463 3. 73 94. 52% 0. 52 199 57 3. 9121 - - 3. 9121 3. 5186 89. 94% 0. 21 150 28. 4 3. 9121 3. 6935 94. 41% 1. 1 centro, 0. 5 lati 367 74. 5 4 MG-1350 -A 70 x 55 mm 20 20 30 30 0 2200 1200 4 -Bis MG-1360 -A 70 x 55 mm 20 20 30 30 Separata 0 2200 1200 5 MG-1411 -B ø 80 H 4 20 30 20 20 Separata 10% CD 3 µm 2200 1200 6 MG-1571 -B ø 80 H 4 20 50 0 20 Separata 10% CD 3 µm 2200 1200 7 MG-1280 -B ø 80 H 4 20 60 0 18 Separata (+2% Si) 0 2200 1200 8 MG-1270 -D ø 80 H 4 20 60 0 20 separata 0 2400 1200 35 9 MG-1690 -A ø 90 H 4 20 25 55 0 0 2200 10 MG-1110 -A ø 90 H 4 20 40 20 20 separata 0 2200 1200 35 0. 1 mbar, 97%- 09/03/2013 N 2, 3% H 2 10/1 MG-1110 -A ø 90 H 4 10/2 MG-1110 -A ø 90 H 4 10/3 MG-1110 -A ø 90 H 4 10/4 MG-1110 -A ø 90 H 4 10/5 MG-1110 -C ø 90 H 4 10/6 MG-1110 -D ø 40 H 4 10/7 MG-1110 -E ø 90 H 4 10/8 MG-1110 -E ø 90 H 4 10/9 MG-1110 -E ø 90 H 4 10/10 MG-2110 -F 60 mm-1 60 mm-2 - - … r a f o s d e c u ! od y r l p e u n ee niq b u e v m ha he t s y e f t i a t n pl e y d i n a o t M D I d r a Stand 20 40 20 20 separata 0 2200 1200 20 40 20 20 separata 0 2300 1200 20 40 20 20 separata 0 2420 20 40 20 20 separata ø 90 H 4 20 40 20 MG-1110 -G ø 60 H 22. 8 20 40 MG-1110 -H ø 60 H 22. 8 20 40 60 mm-3 MG-1110 -J ø 60 H 22. 1 20 60 mm-4 MG-1110 -K ø 60 H 22. 5 80 mm-5 MG-1110 -L 80 mm-6 MG-1110 -M Cond Termica Resistenza a Flessione (W/m. K) (MPa) 35 0. 1 mbar, 97%N 2, 3% H 2 26/03/2013 3. 9121 3. 69 94. 32% 0. 52 - - 26/03/2013 3. 9121 3. 73 95. 35% 0. 51 - - 26/03/2013 3. 9121 3. 7 94. 58% 0. 5 245 - 12/04/2013 3. 9121 3. 71 94. 83% 0. 48 - - 35 0. 1 mbar N 2 13/04/2013 3. 9121 3. 74 95. 60% 0. 88 centro, 0. 62 lati - - 1200 35 0. 1 mbar N 2 26/04/2013 3. 9121 3. 68 94. 07% 0. 99 centro, 0, 5 lati - - 2420 1200 35 0. 1 mbar N 2 26/04/2013 3. 9121 3. 68 94. 07% 0. 92 c, 0. 5 lati - - 0 2420 1200 35 0. 1 mbar N 2 26/04/2013 3. 9121 3. 66 93. 56% 0. 90 c, 0. 5 l - - 20 separata 0 2560 1200 35 0. 1 mbar N 2 26/04/2013 3. 9121 2. 78* 0. 95 720 73 20 20 separata 0 1692* 1200 35 0. 1 mbar N 2 06/10/2013 3. 9121 3. 72 Mo 2 C flow out - No compactio n available 95. 09% 0. 6 270 65 20 20 Separata 0 1735 * 1200 35 0. 1 mbar N 2 31/10/2013 3. 9121 3. 8 97. 13% 0. 7 40 20 20 Separata 0 1775* 1200 35 0. 1 mbar N 2 05/11/2013 3. 9121 3. 78 96. 62% 0. 7125 20 40 20 20 Separata 0 1805* 1200 35 0. 1 mbar N 2 13/11/2013 3. 9121 3. 73 95. 35% 0. 8 ø 80 H 17. 5 20 40 20 20 Separata 0 1920* 400 35 0. 1 mbar N 2 29/11/2013 3. 9121 3. 5257 90. 12% 1. 022 (parte fusa) - - ø 80 H 17. 5 20 40 20 20 Separata 0 35 0. 1 mbar N 2 05/12/2013 3. 9121 3. 6 92. 02% 1. 005/0. 95 180 85 ? mm-7 MG-1110 -N 35 0. 1 mbar N 3 90 mm-8 MG-1110 -P ø 90 H 5. 5 20 40 20 20 Separata 0 2000 600 35 0. 1 mbar N 4 03/02/2014 3. 72 3. 65 1. 16/0. 7 90 mm-9 MG-3110 -Q ø 90 H 5. 25 20 40 20 20 Separata 0 2005 350 35 0. 1 mbar N 5 05/02/2014 3. 72 2. 62 80 90 mm-10 MG-4110 -P ø 90 H 16. 5 20 40 20 20 Separata 0 35 0. 1 mbar N 5 07/02/2014 3. 5 2. 669 90 (from LFA @CERN) 85 Ad. Col. Mat - 21/7/2014 Elena Quaranta Mo 2 C 1. 00 flow out - (centro)/0. 92(periferi No a) compactio n available 1. 13(centro)/1. 12(m età)/0. 96(bordo) 27

Nomenclature Materi al Productio n cycle Composition MG # # A Molybdenum Graphite %v Mo or Mo 2 C (final) %v Gr %v CF %v other elements (A…Z) Info about: • Tcycle • tcycle • p • atmosphere # = 0… 9 => each digit corresponds to initial* component content in composite *first digit correspond to: %vin Mo if no melting %vfin Mo 2 C if melting with Mo 2 Cflow out Ad. Col. Mat - 21/7/2014 Elena Quaranta 28

Where to access the info… DFS folder: G: DepartmentsENProjectsMME_Mechanical. Engineering Elena. QuarantaMaterials New classification of MG plates: …Mo. GRCF_Summary_new. Name. xlsx Nomenclature legend: …MG_legend. xlsx Ad. Col. Mat - 21/7/2014 Elena Quaranta 29

Nomenclature: some example MG 1110 A Fully characterize d: outstanding electrical and thermal properties, low density! • 20%v Mo, 40% GR, 40% CF, 0% others • A=1200 s at 2200°C, 35 MPa, H 2 -N 2 at 10 -4 mbar • ρ=3. 7 g/cm 3 Mo 2 C melt and flowed out for the first time MG 2110 F • 7. 6%v Mo 2 C, 40% GR, 40% CF, 0% others • F=2560°C for 1200 s, 35 MPa, N 2 at 10 -4 mbar • ρ=2. 78 g/cm 3 MG 3110 Q • 6. 2%v Mo 2 C, 40% GR, 40% CF, 0% others • Q=2005°C (pyrometer) for 350 s, 35 MPa, N 2 at 10 -4 mb • ρ=2. 62 g/cm 3 MG 3110 P • 6%v Mo 2 C, 40% GR, 40% CF, 0% others • P=2000°C (pyrometer) for 600 s, 35 MPa, N 2 at 10 -4 mb • ρ=2. 67 g/cm 3 Ad. Col. Mat - 21/7/2014 Elena Quaranta 30

Last produced plate: 23/06/2014 MG 5220 S • Ø 90 mm x 24. 29 mm => THICK plate! • ≈4%v Mo 2 C, 96%v graphite + CF • T=2600°C (pyrometer) for 600 s, 35 MPa, N 2 at 10 -4 mbar • ρ=2. 65 g/cm 3 Ad. Col. Mat - 21/7/2014 Elena Quaranta 31

Irradiation campaign at BNL § ON-GOING irradiation and post-irradiation studies on Molybdenum, Glidcop, Cu. CD, Mo. GRCF 200 Me. V proton and spallation neutron (by ~120 Me. V protons) irradiation @BLIP C/C Graphit e Proton beam profile Energy deposited in target Ad. Col. Mat - 21/7/2014 Mo. Graphite Proton beam profile Spallation Neutron profile Elena Quaranta 32

Irradiation campaign at BNL 28 Me. V proton irradiation for very localized proton -induced damage @Tandem van de Graaff X-Ray Diffraction studies @ NSLS (100 -200 ke. V X-rays) Ad. Col. Mat - 21/7/2014 Elena Quaranta 33