Thermodynamics and Phase Diagram of the Ni-Sb-Sn System
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1 Thermodynamics and Phase Diagram of the Ni-Sb-Sn System Ratikanta Mishra & Herbert Ipser Department of Inorganic Chemistry / Materials Chemistry, University of Vienna, Austria
2 Traditional Solder Materials As examples: Sn-Pb (62/38 wt.%) C 183 C 232 C High-lead solders (up to 90 % Pb) for high-temperature soldering (90/10) eutectic (38/ 62) Pb Sn
3 Search is on for possible lead-free alloys with melting point between 250 and 400 C. It is now widely agreed that there is no drop-in replacement for the standard tin-lead solders Sn-Sb alloys with additional alloying elements Ag, Cu, Ni can be a possible candidate for new hightemperature solders. The present work deals with the phase diagram and thermodynamic studies Ni-Sb-Sn system
4 Overview Thermal analysis of Sn-rich corner Phase Diagram Ni-Sb Sb-Sn Sn system at 900 C Thermodynamics of Ni-Sb Sb-Sn Sn system
5 Thermal analysis of Sn-rich corner Samples : 20 Ni: 0-25 at % Sb: 0 to 25 at % Sn: at % Heat Treatment: 3h 7d 12h RT 1050 C 1050 C 200 C 21d quench 200 C 200 C RT Isothermal sections at 200C. DTA XRD EPMA High resolution microscope Isopleths Scheil diagram Liquidus projection
6 EPMA & XRD Results
7 DTA results of 80% Sn alloys At % Sb Invariant Temperature ( C) Other Temperature ( C) , , , , , , , 242, , , 243, , , 244, , , 243, , , 243, , 388 Isopleth for 80 % at Sn 200 C
8 DTA results of 85% Sn alloys At % Sb Invariant Temperature ( C) Other Temperatur e ( C) , --, -- --, , 243, -- --, , 244, , , 242, , , 243, , , 242, Isopleth for 85 % at Sn 200 C
9 Experimental Results: Scheil Diagram Sn-rich corner
10 Liquidus projection
11 Phase diagram Ni-Sb-Sn system at 900 Samples : 30 Heat Treatment: RT RT 3h 1050 C 3h 1050 C 7d 2h 1050 C RT Grinding & pelleting 96h 6h 2weeks quenching 1050K 900 C 900 C RT Samples were analyzed by (XRD and EPMA)
12 XRD data Ni3Sn2-NiSb tie line a ( A) (c) (a) Mole frac. NiSb c ( A) c/ /a c/a plot Ni 3 Sn 2 phase as a function of composition Mole frac. NiSb
13 Phase diagram Ni-Sb-Sn system at 900 C L1 2 The liquidus phase boundary is being determined by DTA
14 Thermodynamic Investigation of Ni-Sb-Sn Sn system by Isopiestic Vapor Pressure Method
15 pure Sb p Sb (T R ) Isopiestic Vapor Pressure Measurement Of Ni-Sn-Sb Sb system Ni-Sn alloys Before equilibration Conditions for Ni-Sn-Sb system fulfilled: pure Sb p Sb (T R ) After equilibration Temp. Reservoir, T R (T S > T R ) pni, p Sn << p Sb an alloy NixSn y Sb z p Sb (T S ) In equilibrium: p Sb (T S ) = p Sb (T R )
16 Quartz seal Isopiestic Apparatus Ni 3 Sn Quartz outer tube Ni-Sb-Sn alloy Ni 3 Sn 2 Ni 3 Sn 4 (up to 36 crucibles 12 each) Quartz crucible Quartz thermo-well Quartz crucible holder Quartz spacer Quartz reservoir Sb
17 Two-zone furnace for equilibration S-type thermocouple Stepper motor arrangement for controlled raising of thermocouple Two zone gradient furnace PC based DAS (Data acquisition system)
18 Furnace characteristics & Temperature profile Sample Temp. (K) 1300 Isopiestic apparatus ~ 600 mm K 1000 height of the furnace 1200 mm Distance (mm) Sample Temp. (K) Tr= 979 K Tr=1090 K Tr=1017 K Tr=939 K Tr=1072 K Distance (mm)
19 After equilibration quenching of the entire apparatus in cold water
20 Isopiestic equilibrium curves For Ni3Sn-Sb, Ni3Sn2-Sb and Ni3Sn4-Sb systems Ni 3 Sn-Sb system Ni 3 Sn 2 -Sb system Tr = 979 K Tr = 1090 K Tr = 939 K Tr = 1072 K Tr = 979 K Tr = 1090 K Tr= 1017 K Tr = 939 K Tr = 1072 K Ts (K) 1125 Ts, K At. frac. Sb Tr=1017 K Tr= 939 K Tr = 1072 K At. fraction Sb TS(K) Ni 3 Sn 4 -Sb system At. Fraction Sb
21 lnp(sbx, Atm) l Vapour pressures antimony Results Ni-Sb-SnSn System evaluation psb psb2 psb /T, K a ( T ) = Sb p = p + Sb, total S K = p p p Sb 2 Sb 4 2 Sb Sb p p 2 4 Sb o Sb ( T ( T S S ) ) a = Sb 4 p p Sb 0 Sb 4 4
22 Results Ni-Sn-Sb Sb System Partial enthalpies of antimony H Sb can be obtained from the slope of ln(a Sb ) vs. 1/T plot at a fixed Composition. Then the activities are converted into to one common temperature
23 Ln(a, Sb) Results Ni3Sn2-SbSb System xsb=0.55 xsb=0.60 x Sb=0.65 xsb=0.70 XSb=0.75 xsb= /T, K Natural logarithm of Sb activity vs. reciprocal temperature for selected compositions in the liquid phase as an example. Composition (At % Sb) ln 1 a P = H ( T ) R Partial Molar Enthalpy of Sb (kj/mol) P Similar results were also obtained for Ni3Sn And Ni3Sn4 alloys
24 Integrated Gibbs-Helmholtz Equation: = ) ( ln ) ( ln T T R H T a T a P P P Natural logarithm of the antimony activity as a function of composition for Ni 3 Sn 2 in the liquid phase at 1150 K; standard state: liquid Sb.
25 Summary The thermal analysis Sn-rich corner in the Ni-Sb-Sn System was carried out The diagram for 80 and 85 at Sb% isopleth was delineated The Scheil Diagram and the liquidus projections for Sn-rich corner of Ni-Sb-Sn system were determined. The phase diagram for ternary Ni-Sn-Sn system at 900 C is presented Thermochemical data on Ni-Sb-Sn system is being obtained by isopiestic method
26 Acknowledgements This research is part of the European Research Actions COST 531 and COST MP0602 Financial Support: Marie Curie Foundation (FP7-PEOPLE-IIF-2008, Project No ) and the European Union (COST) for networking.
27 27
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