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COST 531 Meeting Vienna, Mai 2007

COST 531 Meeting Vienna, Mai 2007 Riccardo Ferro  a , Gabriella Borzone a , Gabriele Cacciamani a , Stefano Amore a,d , Nadia Parodi a , Gilda Zanicchi a , Jean-Pierre Bros b , Michèle Gambino b , Daniele Gozzi c , Vincenzo Piacente c ,

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COST 531 Meeting Vienna, Mai 2007

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  1. COST 531 Meeting Vienna, Mai 2007 • Riccardo Ferroa, Gabriella Borzonea, Gabriele Cacciamania, Stefano Amorea,d, Nadia Parodia, Gilda Zanicchia, • Jean-Pierre Brosb, Michèle Gambinob, • Daniele Gozzic, Vincenzo Piacentec, • Enrica Riccid, Rada Novakovicd, • Luca Moliternie, Virginia Cinellif, • Andy Watsong • a Dipartimento di Chimica e Chimica Industriale Università di Genova, Italy, • b Université Aix-Marseille I Ecole Polytechnique Universitaire de Marseille Mécanique et Energétique, Marseille, France • c Dipartimento di Chimica, Università di Roma "La Sapienza", Italy, • d National Research Council of Italy Institute of the Energetics and Interphases, Department of Genoa, Italy, • e Dept: Area Corsi Microsaldatura, Istituto Italiano della Saldatura, Genova, Italy • f OMODEO A&S Metalleghe SpA, Milano, Italy • g IMR/SPEME, University of Leeds, UK GP2 Contribution to the Constitutional Characterisation of Selected Groups of Lead-free Alloys as Soldering Material

  2. Structure of GP2 Coordinator R.Ferro, IT 2-1 IT 2-1 Università di Genova, Genova – I R.Ferro Alloy thermodynamics; phase diagrams: experimental and optimization UK 2-2 University of Leeds, Leeds – UK A.Watson Thermodynamics optimization and modelling; experimental thermodynamics FR 2-2 Université Aix-Marseille I , Marseille- F J.P.Bros Thermodynamics of liquid alloys; heat capacity IT 2-4 Università di Roma La Sapienza – Roma- I D.Gozzi Thermodynamic properties, tensimetry; kinetics of oxidation IT 2-5Consiglio Nazionale Ricerche , Genova- I E.Ricci Surface properties; wetting behaviour IT 2-6Istituto Italiano della Saldatura, Genova- I L.Moliterni Brazing tests IT 2-7 OMODEO A&S Metalleghe SpA, Milano- I V.Cinelli Preparation of alloys and wave soldering

  3. Acknowledgment Researchers Cooperation Funds • INSTM ((Italian Interuniversity Consortium on Materials Science and Technology)- PRISMA04 Final Meeting COST Action 531 Vienna 17-18 May 2007

  4. Contribution WG 1 -WG 2 Thermochemistry and Phase Diagrams – Optimized Phase Diagrams WG 3 – WG 4 Physical properties – Chemical Properties Final Meeting COST Action 531 Vienna 17-18 May 2007

  5. AIM… X-In-Sn systems Au-In-Sn and binary sub-systems Bi-In-Sn Pd-In Pd-Sn Pd-Zn and X-In-Sn-Zn (X=Ag, Cu) quaternary alloys In-Sn-Zn ternary Cu-In-Sn ternary Final Meeting COST Action 531 Vienna 17-18 May 2007

  6. AIM… Au-In-Sn system • To produce a thermodynamic description by: • Experimental studies of phase equilibria • Experimental studies of thermodynamic properties • Au4In3Sn3 ternary phase • Direct reaction calorimetry • Sn solution calorimetry • Enthalpies of mixing of liquid alloy • Thermodynamic Modeling by CALPHAD Method Final Meeting COST Action 531 Vienna 17-18 May 2007

  7. Au4In3Sn3 solid phase Enthalpy of formation - Experimental results DIRECT REACTION DROP CALORIMETER calorimeter working T = 653 K IT 2-1 University of Genova – I TIN SOLUTION CALORIMETRY SETARAM HT1500 calorimeter working T = 673 K UK 2-2 University of Leeds - UK Au4In3Sn3 Final Meeting COST Action 531 Vienna 17-18 May 2007

  8. Enthalpies of mixing of liquid Au-In-Sn alloys UK 2-2 University of Leeds – UK, A.Watson • Indium calibration • One tin sample drop to form In0.5Sn0.5 liquid alloy • Heat changes measured on dropping gold samples • T=882K Final Meeting COST Action 531 Vienna 17-18 May 2007

  9. Au-In-Sn. Enthalpy of mixing : experimental and calculation results Section at x(Sn)/(In)=1/3 Section at x(Sn)/(In)=1/1 Section at x(Sn)/(In)=3/1 Experimental points by A. Watson et al. Enthalpy of mixing in the liquid at 609°C (reference states for calculation are fcc Au and liquid In and Sn; reference states for experiment are fcc Au and liquid In-Sn alloy at the reported composition). Final Meeting COST Action 531 Vienna 17-18 May 2007

  10. Au-In-Sn. Isothermal section from literature Prince et al., assessment, 1990 at about 250°C for x(Au) > 0.3, at about 100°C for x(Au) < 0.3. The ternary phase Au4In3Sn3 was reported to melt congruently at about 430°C. No thermodynamic data are available in literature. Isothermal section calculated at about 25°C by Liu et al., 2003. According to this work, Au4In3Sn3 is stable between 80 and 428°C. Final Meeting COST Action 531 Vienna 17-18 May 2007

  11. Au-In-Sn isothermal section at 130°C. Phase equilibria established by metallographic analysis and DSC IT 2-1 University of Genova – I, N.Parodi and G.Borzone • the melting behaviour of the different alloys have been investigated • the results agree with the general feature of the isothermal section of the literature and the corresponding two and three phase equilibria • incongruent formation at 380°C of the Au4In3Sn3 phase • other invariant reactions were identified • E1 ternary Sn-rich eutectic at Au3.5In0.5Sn95.0 ,T = 204°C Final Meeting COST Action 531 Vienna 17-18 May 2007

  12. Au-In-Sn. Isothermal section at 130°C IT 2-1 University of Genova – I Prince et al., assessment, 1990 at about 250°C for x(Au) > 0.3, at about 100°C for x(Au) < 0.3. Experimental tie-lines and tie-triangles determined in this work are drawn in blue. Final Meeting COST Action 531 Vienna 17-18 May 2007

  13. Thermodynamic modeling of the Au-In-Sn system UK 2-2 University of Leeds – UK, A.Watson IT 2-1 University of Genova – I, G.Cacciamani section 1 Au-In-Sn > Liquidus surface section 2 Experimental points by G. Borzone et al. Final Meeting COST Action 531 Vienna 17-18 May 2007

  14. Au-In-Sn: Experimental and Calculation Results Experimental points determined in this work by DSC are reported in blue. Not all of them are exactly in the sections. Notice, here below, the incongruent melting of Au4In3Sn3. Vertical section at x(Au)=0.4 Vertical section at x(Au)-x(In)=0.1 Vertical section at x(Sn)-2/3x(In)=0.1 8 Final Meeting COST Action 531 Vienna 17-18 May 2007

  15. Au-In-Sn systemSurface properties Wetting behaviour IT 2-5Consiglio Nazionale Ricerche , Genova- I E. Ricci, D. Giuranno, F. Gnecco, S. Amore, T. Lanata, R. Novakovic Surface Tension + modelling: Binary systems Au-Sn Au-In In-Sn Wetting behaviour: Ternary systems: Au-In-Sn/Cu Binary sub-systems: Au-In/Cu Au-Sn/(Cu,Ni) In-Sn /(Cu,Ni) Final Meeting COST Action 531 Vienna 17-18 May 2007

  16. Bi-In-Sn system. Thermodynamic Properties IT 2-4 Università di Roma La Sapienza – Roma- I D.Gozzi , V.Piacente, B.Brunetti IT 2-1 University of Genova – I, G.Zanicchi, N.Parodi and G.Borzone • Aim…… • Thermodynamic description • DSC MEASUREMENTS • (liquidus surface) • BISMUTH ACTIVITY • MEASUREMENTS Final Meeting COST Action 531 Vienna 17-18 May 2007

  17. IT 2-4 Università di Roma La Sapienza – Roma- I D.Gozzi EXPERIMENTAL effusion holes • effusion flow–rate, Je, generates the torsion of W–wire. • torsion is measured through deviation of the beam light. • the torsion angle  Je • Je = pe(2 mKT)–1/2 At 1000 K Bi/In = 200 Bi/Sn = 3x105 xBi variable xSn/xIn = 0.85

  18. Bi-In-Sn systemSurface properties Wetting behaviour IT 2-5Consiglio Nazionale Ricerche , Genova- I E. Ricci, D. Giuranno, F. Gnecco, S. Amore, T. Lanata, R. Novakovic Surface Tension + modelling: Binary systems Bi-In In-Sn Wetting behaviour: Ternary systems: Bi-In-Sn/Cu Binary sub-systems: Bi-In/Cu In-Sn /(Cu,Ni) Final Meeting COST Action 531 Vienna 17-18 May 2007

  19. Table 1. Au-In-Sn alloys. Experimental data. Ag-In-Sn-Zn system FR 2-3Marseille-F, J.P.Bros, M.Gambino, A.Sabbar,AZrineh,J.M.Miane Ag Liquidus temperatures Points 3 and 5: 289°C Point 4 : 315°C Eutectic surface: 114°C Section xAg= 0.045 Zn In Section xIn/xSn = 1.1 xZn = 0.10 Sn Section xIn/xSn = 0.25

  20. Table 1. Au-In-Sn alloys. Experimental data. Ag-In-Sn-Zn system FR 2-3Marseille-F, J.P.Bros and M.Gambino Ag-In-Sn-Zn Liquidus xIn/xSn = 0.25 section T/°C xAg= 0.09 xAg= 0 xZn xAg= 0.05 xAg= 0 T/°C xZn Ag-In-Sn-Zn Liquidus xIn/xSn = 1.1 section Final Meeting COST Action 531 Vienna 17-18 May 2007

  21. Electrochemical measurements Potentiodynamic polarization curves recorded in 0.1 M NaCl solution using a saturated calomel electrode (SCE) as a reference Copper addition enhances the corrosion resistance of Sn-Ag solder alloys which show more passive behaviour than Sn73.9Pb26.1 one. Increasing the copper content from 0.8 to 6.7 wt % results in a significant improvement of the corrosion behaviour of Sn-Ag solders. Final Meeting COST Action 531 Vienna 17-18 May 2007

  22. Pd-X (X= In, Sn, Zn) HT drop calorimetry IT 2-1 Università di Genova– I, S.Amore, N.Parodi and G.Borzone Our data ,dir. reaction cal, 298K Final Meeting COST Action 531 Vienna 17-18 May 2007

  23. Thank you for your attention Final Meeting COST Action 531 Vienna 17-18 May 2007

  24. Final Meeting COST Action 531 Vienna 17-18 May 2007

  25. H. Flandorfer (2002) Final Meeting COST Action 531 Vienna 17-18 May 2007

  26. Final Meeting COST Action 531 Vienna 17-18 May 2007

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