Bonding as an assembly technique in upgrades to aLIGO and detectors like ET and KAGRA R. Douglas1, A. A. van Veggel1, K. Haughian1, D. Chen2, L. Cunningham1, R. Glaser3, G. Hammond1, G. Hofmann3, J. Hough1, M. Masso Reid1, P. Murray1, R. Nawrodt3, M. Phelps1, S. Reid4, S. Rowan1, Y. Sakakibara2, T. Suzuki5, C. Schwarz3, K. Yamamoto2 1 SUPA, Institute for Gravitational Research, University of Glasgow, Glasgow, UK ICRR, University of Tokyo, Tokyo, Japan 3 Friedrich Schiller University, Jena, Germany 4 SUPA, University of the West of Scotland, Paisley, UK 5 High Energy Accelerator Research Organisation, Tokyo, Japan 2 Amaldi Gwangju, June 2015 Introduction • GEO600, aLIGO, and advanced VIRGO use quasi-monolithic fused silica test mass suspensions with superior thermal noise performance at room temperature • Hydroxide catalysis bonding (HCB) is used in all to attach interface pieces to the mirrors, allowing attachment of the fibres (which are welded) Steel wires Penultimate mass Attachment or ‘ear’ Steel wire break-off prism Silica fibres Fibres Weld horns Ear End/input test mass Ear • We are considering upgrades to detectors at room temperature (A+ and ETHF) and various cryogenic temperatures (Voyager, ET-LF, KAGRA) LIGO-G1500838 2 Chemistry This method can create strong, durable bonds. Chemistry of bonding between silica surfaces: Hydration and Etching Dehydration Polymerisation - OH ions from the bonding solution OH ions form weak fill any open bonds bonds with surface Si on the surface atoms Bonding Bonding solution solution with OH OH OH OH lots with- of anfree OH ions excess of SiO Si Si free OH ions Si O Bonds between the Si Bulk Silica atoms and the bulk weaken due to the extra OH ions bonding to the Si atom O O Silicate molecule breaking away from being released from the bulk into and into the the Bonding solution with bonding solution lots of free OH ions Si(OH)-5 H2O H2O H2O OH OH OH OH OH SiO2 Si OH H O SiO2 OH Si OH H O Si OH H O Si OH H Si O OHOH Si i OH OH OH OH H Si O O O Bulk Silica LIGO-G1500838 H H Bond 3 Feasibility study: how? • Can we bond sapphire and silicon using HCB? Yes, we can Silicon surfaces must be oxidised to facilitate reliable bonding Chemistry is different for sapphire: aluminate chains • Are there other jointing techniques that may be suitable? Indium bonding but only under compression and if suspension is not baked out • What is the strength of bonds in conditions consistent with those of cryogenic suspension, assembly and operation? LIGO-G1500838 4 Bond Strength Two types of strength tests carried out: 4 point bend tester to measure tensile strength and a torsional shear strength tester. Load, F 4 contact Bonded sample points d L Bond l 3F ( L l ) tensile 2 2bd Where b is the breadth of the sample max_shear T 2 0.208ab Where T is the torque, a is the length and b is the width of the cross-section of the sample LIGO-G1500838 5 Cryogenic strength of HCBs between sapphire Load, F • • • 40x10x5 mm samples, 10x5 mm M-to-M-plane bond in the centre Results published Douglas et al., CQG, 2014 4 line contacts Bonde d sampl e d L [MPa] strength [MPa] Shearstrength Tensile 100 120 Room temperature pH 12 Pristine samples M-to-M 80 60 40 20 0 Sodium aluminate Bon d l 100 [MPa] strength [MPa] Shearstrength Tensile 120 Sodium hydroxide Potassium hydroxide Sodium silicate Bonding solution LIGO-G1500838 80 60 40 20 0 R.T. 77 K Temperature 6 Bond strength: sapphire, curing time Load, F •Curing time for bonds between silica has been found to be ~4 weeks. 4 line contacts Bonded sample d Bonded sapphire sample 5x5x40 mm. C-C plane. 5x5 mm bonding surface L Bon d l •All C-C samples broke clean across the bond. •Strength within error the same for the 3 different curing times. •Curing time of sapphire doesn’t appear to be longer than 4 weeks. Investigations are ongoing. •Strength for A-A, M-M and CC within error the same. LIGO-G1500838 7 Bond strength: silicon, thermal cycling •Check the effect of thermal cycling on the strength of line bonds as suspended silicon masses are likely to go 4contacts through multiple thermal cycles in their lifetime. •40 bonds tested in set 1, 28 bonds tested in set 2. •Thermal cycling done in Jena ~4 K – ~293 K, 2 hours per cycle. Load, F Bonde d sampl e d L l Bon d Oxidised silicon sample 10x5x20 mm Boron doped P-type <100> ~150 nm dry thermal oxide Observations: • Overall average strength doesn’t change • Two strength groups (thought to be linked to bond quality). LIGO-G1500838 8 Bond strength: questions remaining? Silicon • What is the minimum oxide layer thickness for ion-beam sputtered coatings? • What is causing difference in strength between different sets of bonds: bond quality? • How can we best to assess this? • Can strength/mechanical loss be improved through heat/vacuum treatment? • What is the curing time? Sapphire • Influence of thermal expansion differences between different crystal orientations on bond strength when bonding e.g. c-a plane or c-m plane? • Influence of polishing process/surface damage on strength. • Literature study suggests surface reactivity higher for mechanically polished surfaces as opposed to pristine surfaces • Can strength/mechanical loss be improved through heat/vacuum treatment? • Bond strength of sapphire notLIGO-G1500838 polished or cut on specific crystal plane? 9 Thermal conductivity • Thermal conductivity has now been measured of: Heater and temperature sensor used to thermally stabilise the clamp 1. Silicon-silicon HCB bonded cylinders (25 mm x 76 mm) down to 30 K (Lorenzini, ET Clamped silicon sample T2 ΔL T1 Heater used to induce heat flow meeting Jena, 2010) 2. Silicon-silicon HCB bonded samples (5x5x40 mm) down to 8K 3. Sapphire-sapphire HCB bonded samples (Poster C. Schwarz, D. Chen, ET meeting 2014, Lyon). 4. Sapphire-sapphire indium bonded sample Results suggest drop in thermal conductivity is very small. LIGO-G1500838 10 Summary • HCB between silicon and sapphire have been extensively demonstrated to be strong enough for typical gravitational wave detector suspensions • Thermal cycling of HCB bonded silicon does not negatively impact strength of bonds but more work is needed to be able to assess bond quality • Thermal conductivity measurements of HCB and indium bonds appear to be high enough for suspension attachments. • Aim: Understand better the influence of cross-sectional size on thermal conductivity • For more information see Marielle van Veggel’s recent GWADW talk (LIGO-G15008) which includes details on loss measurements. LIGO-G1500838 11 Thank you for your attention Thank you for your attention Any questions? LIGO-G1500838 12 LIGO-G1500838 Bond strength: what do we know? Silicon • In Glasgow we bond with sodium silicate solution. (Potassium hydroxide is also possible, see Dari et al., CQG, 2010) • Using a wet thermal oxide layer, we need 50 nm oxide layer to get reliably strong bonds (Beveridge et al., CQG, 2011) • Strengths tested at R.T. and at 77 K • Ion beam sputtered oxide layer is an excellent and probably more practical alternative (Beveridge et al., CQG, 2013) • Average strength values are 20–40 MPa (depending on type of material, crystal orientation, temperature of test. • Strength at 77 K higher than at R.T. • Recent thermal cycling tests (3,10 and 20 times down to ~8 K) of <100>-<100> silicon (2 sets tested), suggest that the average stays constant. We are developing techniques to assess the quality of bonds during the bonding procedure to ensure only high quality bonds are accepted. LIGO-G1500838 14 Silica Silicon 0 Cumulative dL/L [-] 1.0E-04 5.0E-05 0.0E+00 -5.0E-05 -1.0E-04 -1.5E-04 -2.0E-04 -2.5E-04 -3.0E-04 -3.5E-04 100 200 Temperature [K] 300 Silica Silicon dL/L difference 300 Perpendicular to C-axis 7.0E-06 6.0E-06 5.0E-06 4.0E-06 3.0E-06 2.0E-06 1.0E-06 0.0E+00 Coefficient of linear thermal expansion [1/K] 3.0E-06 2.5E-06 2.0E-06 1.5E-06 1.0E-06 5.0E-07 0.0E+00 -5.0E-07 -1.0E-06 -1.5E-06 200 100 Temperature [K] Parallel to C-axis 0 Cumulative dL/L [-] Coefficient of linear thermal expansion [1/K] Stress due to thermal expansion differences 1.0E-04 -5.0E-19 -1.0E-04 -2.0E-04 -3.0E-04 -4.0E-04 -5.0E-04 -6.0E-04 -7.0E-04 -8.0E-04 0 LIGO-G1500838 100 200 Temperature [K] 300 parallel to c-axis perpendicular to c-axis Difference between planes 300 200 100 Temperature(K) 0 15 Bond mechanical loss, overview • Silica-silica HCB bond made with sodium silicate solution @ RT Bond loss: 0.11 ± 0.02 (Cunningham, CQG, 2010) • Silica-silica HCB bond (same as above) after 3 years and after heat treatment 150 C for 48 hours. Bond loss: 0.06 ± 0.01 (Haughian, thesis, 2012) • Silicon-silicon HCB bond made with sodium silicate solution @ RT. Not an ideal bond (offset). Bond loss: 0.27-0.52 (Haughian, thesis, 2012) • Sapphire-sapphire HCB made with sodium silicate solution @ RT temperature • Bond loss @ R.T. 0.03± 0.01 • Bond loss @ 20 K (3 - 7)x10-4 ± 1x10-4 • Sapphire-sapphire indium bond • Bond loss @ 20 K (2 – 3)x10-3 (Talk K. Yamamoto, ET meeting 2014, Lyon). LIGO-G1500838 16 Thermal noise associated with HCBs in aLIGO • In aLIGO thermal noise arising from bonds was to be 10% of the total thermal noise budget @ 100 Hz • Thermal noise budget @ 100 Hz is 2.510-24 /Hz Bond thermal noise budget per test mass 710−22 m/√Hz, (T01007501,2009) • Calculated: 5.4 10−22 m/√Hz ) assuming bond loss of 0.11 at 293 K Hild, S., CQG. 29 (2012) 124006 Assumptions for calculations following: • bond thermal noise budget < 10% of overall thermal noise budget @ 100 Hz • Ear size (where unknown): same ratios and average shear stress (0.17 MPa) as aLIGO. LIGO-G1500838 17 Thermal noise from bonds for cryogenic detectors Name detector A+2 ET-LF1 (option 1) ET-LF1 (option 2) TM material Silica silicon sapphire Temperature TM [K] 293 10 10 Bond area 1 ear [mm x mm] 39x118 45x136 45x136 Assumed bond thermal noise requirement [m/Hz] 310-22 210-22 210-22 Bond loss [-] *1.110-1 **1.110-1 *710-4 Calculated expected thermal noise (±15%) [m/Hz] 5.310-22 1.410-22 1.210-23 * Measured value ** Assumed value (bond loss) silica-silica bond @ R.T LIGO-G1500838 18