Outline. Thermodynamic databases. Example: Mg alloy database Ternary parameters Key experiments Quality problems with binary systems / software
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1 1 Thermodynamsche Datenbanken R. Schmd-Fetzer Contrbutons by J. Klngbel, H. Cordes, F. Goesmann, K. Zeng, K. Bhanumurthy, A. Psch, R. Wenzel, G. Fscher, D. Kevorkov, J. Gröbner, T. Studntzky, B. Onderka, S.M. Schnurre, D. Mrkovc, I. Chumak supported by the German Research Councl (DFG), Volkswagenstftung, Federal Mnstry of Educaton & Research (BMBF), European Unon (EU) -clausthal.de/agrsf
2 Outlne 2 Thermodynamc databases Example: Mg alloy database Ternary parameters Key experments Qualty problems wth bnary systems / software Applcatons Developng creep resstant Mg alloys Solderng Al-alloy soldfcaton, mcrosegregaton.met.tu-clausthal.de/agrsfagrsf
3 Mg database: Bnary systems 3 Ag-Al Ag-Ca Ag-Ce Ag-Cu Ag-Gd Ag-L Ag-Mg Ag-Mn Ag-Nd Ag-Sc Ag-S Ag-Sr Ag-Y Ag-Zn Ag-Zr Al-Ca Al-Ce Al-Cu Al-Gd Al-L Al-Mg Al-Mn Al-Nd Al-Sc Al-S Al-Sr Al-Y Al-Zn Al-Zr Ca-Ce Ca-Cu Ca-Gd Ca-L Ca-Mg Ca-Mn Ca-Nd Ca-Sc Ca-S Ca-Sr Ca-Y Ca-Zn Ca-Zr Ce-Cu Ce-Gd Ce-L Ce-Mg Ce-Mn Ce-Nd Ce-Sc Ce-S Ce-Sr Ce-Y Ce-Zn Ce-Zr Cu-Gd Cu-L Cu-Mg Cu-Mn Cu-Nd Cu-Sc Cu-S Cu-Sr Cu-Y Cu-Zn Cu-Zr Gd-L Gd-Mg Gd-Mn Gd-Nd Gd-Sc Gd-S Gd-Sr Gd-Y Gd-Zn Gd-Zr L-Mg L-Mn L-Nd L-Sc L-S L-Sr L-Y L-Zn L-Zr Mg-Mn Mg-Nd Mg-Sc Mg-S Mg-Sr Mg-Y Mg-Zn Mg-Zr Mn-Nd Mn-Sc Mn-S Mn-Sr Mn-Y Mn-Zn Mn-Zr Nd-Sc Nd-S Nd-Sr Nd-Y Nd-Zn Nd-Zr Sc-S Sc-Sr Sc-Y Sc-Zn Sc-Zr S-Sr S-Y S-Zn S-Zr Sr-Y Sr-Zn Sr-Zr Y-Zn Y-Zr Zn-Zr 16 components: 120 bnary systems 16 = from lterature + checked + adapted 37 own modelng + experments 42 mssng systems.met.tu-clausthal.de/agrsfagrsf
4 Mg database: Ternary systems 4 Ag-Al Ag-Ca Ag-Ce Ag-Cu Ag-Gd Ag-L Ag-Mg Ag-Mn Ag-Nd Ag-Sc Ag-S Ag-Sr Ag-Y Ag-Zn Ag-Zr Al-Ca Al-Ce Al-Cu Al-Gd Al-L Al-Mg Al-Mn Al-Nd Al-Sc Al-S Al-Sr Al-Y Al-Zn Al-Zr Ca-Ce Ca-Cu Ca-Gd Ca-L Ca-Mg Ca-Mn Ca-Nd Ca-Sc Ca-S Ca-Sr Ca-Y Ca-Zn Ca-Zr Ce-Cu Ce-Gd Ce-L Ce-Mg Ce-Mn Ce-Nd Ce-Sc Ce-S Ce-Sr Ce-Y Ce-Zn Ce-Zr Cu-Gd Cu-L Cu-Mg Cu-Mn Cu-Nd Cu-Sc Cu-S Cu-Sr Cu-Y Cu-Zn Cu-Zr Gd-L Gd-Mg Gd-Mn Gd-Nd Gd-Sc Gd-S Gd-Sr Gd-Y Gd-Zn Gd-Zr L-Mg L-Mn L-Nd L-Sc L-S L-Sr L-Y L-Zn L-Zr Mg-Mn Mg-Nd Mg-Sc Mg-S Mg-Sr Mg-Y Mg-Zn Mg-Zr Mn-Nd Mn-Sc Mn-S Mn-Sr Mn-Y Mn-Zn Mn-Zr Nd-Sc Nd-S Nd-Sr Nd-Y Nd-Zn Nd-Zr Sc-S Sc-Sr Sc-Y Sc-Zn Sc-Zr S-Sr S-Y S-Zn S-Zr Sr-Y Sr-Zn Sr-Zr Al-Ca-L Al-Ca-S Al-Ce-S Al-Ca-Mg Al-Ca-S Al-Ce-Mg Al-Cu-L Al-Cu-Mg Al-Cu-Nd Al-Cu-S Al-Cu-Zn Al-Gd-Mg Al-L-Mg Al-L-Mn Al-L-S Al-Mg-Mn Al-Mg-Sc Al-Mg-S Al-Mg-Y Al-Mg-Zn Al-Mn-Sc Al-Mn-S Al-S-Y Al-S-Zn Ca-L-Mg Ca-L-S Ca-Mg-S Ce-L-Mg Ce-Mg-Mn Ce-Mg-Sc Ce-Mn-Sc Cu-L-Mg Cu-Mg-S Cu-Mg-Y Cu-Mg-Zn Gd-L-Mg Gd-Mg-Mn Gd-Mg-Sc Gd-Mn-Sc L-Mg-S L-Mg-Zn Mg-Mn-Sc Mg-Mn-Y Mg-Mn-Zr Mg-Y-Zr Mn-Sc-Y Mn-Y-Zr Y-Zn Y-Zr Zn-Zr 16 = possble ternares Exper.+Modell. Lterature&Check Plausblty-Check.met.tu-clausthal.de/agrsfagrsf
5 Mg database: multcomponent systems 5 Ag-Al Ag-Ca Ag-Ce Ag-Cu Ag-Gd Ag-L Ag-Mg Ag-Mn Ag-Nd Ag-Sc Ag-S Ag-Sr Ag-Y Ag-Zn Ag-Zr Al-Ca Al-Ce Al-Cu Al-Gd Al-L Al-Mg Al-Mn Al-Nd Al-Sc Al-S Al-Sr Al-Y Al-Zn Al-Zr Ca-Ce Ca-Cu Ca-Gd Ca-L Ca-Mg Ca-Mn Ca-Nd Ca-Sc Ca-S Ca-Sr Ca-Y Ca-Zn Ca-Zr Ce-Cu Ce-Gd Ce-L Ce-Mg Ce-Mn Ce-Nd Ce-Sc Ce-S Ce-Sr Ce-Y Ce-Zn Ce-Zr Cu-Gd Cu-L Cu-Mg Cu-Mn Cu-Nd Cu-Sc Cu-S Cu-Sr Cu-Y Cu-Zn Cu-Zr Gd-L Gd-Mg Gd-Mn Gd-Nd Gd-Sc Gd-S Gd-Sr Gd-Y Gd-Zn Gd-Zr L-Mg L-Mn L-Nd L-Sc L-S L-Sr L-Y L-Zn L-Zr Mg-Mn Mg-Nd Mg-Sc Mg-S Mg-Sr Mg-Y Mg-Zn Mg-Zr Mn-Nd Mn-Sc Mn-S Mn-Sr Mn-Y Mn-Zn Mn-Zr Nd-Sc Nd-S Nd-Sr Nd-Y Nd-Zn Nd-Zr Sc-S Sc-Sr Sc-Y Sc-Zn Sc-Zr S-Sr S-Y S-Zn S-Zr Sr-Y Sr-Zn Sr-Zr S Mg Y-Zn Y-Zr Zn-Zr Mg RE Mg Al Ca S Al L multcomponent.met.tu-clausthal.de/agrsfagrsf
6 Buldng of multcomponent systems 6 System Gbbs energy data Unary SGTE data, 1991 Dnsdale Bnary Thorough assessment needed Ternary Quaternary & hgher Ternary sold phases? Extrapolaton for soluton phases, careful wth ternary parameters Extrapolaton.met.tu-clausthal.de/agrsfagrsf
7 Key experments 7 Sample selecton Calculated mportant reactons Sample preparaton Levtaton Meltng Arc Meltng Electron Beam Meltng Reacton Snterng Ta capsule Alloy sample Sample analyss Calormetry (Calvet-DSC, drop) Thermal Analyss (DTA, STA) X-ray Dffractometry (XRD, C) Electron Mcroscopy (SEM/EDX/WDX) Metallography, Optcal Mcroscopy.met.tu-clausthal.de/agrsfagrsf
8 Al-Ce-S 8 Temperature, C As-cast, h at 570 C 400 E 1 Al 90 Ce 10 S 0 (Al) L + Al 11 Ce 3 (l) L + τ 1 + Al 11 Ce 3 (l) L + τ 1 coolng; strong peak heatng; strong peak coolng; weak peak heatng; weak peak τ 1 + U 11 (Al) τ 1 + τ 2 + (Al) L + τ 2 + (Al) L + (Al) Al 11 Ce 3 (l) + τ 1 + (Al) τ 2 + (Al) + (S) S S, at.% τ 1 τ 2 E 2 Al 90 Ce 0 S 10 Heat flow n W/g eutectc Calormetry prmary Temperature n C Ce 90 at.% Al Al Thermodynamc calculaton confrms: τ 1 prmary, τ 2 pertectc formaton (transton reacton).met.tu-clausthal clausthal.de/ clausthal.de.de/agrsfagrsf
9 20 at.% Ce constant coolng; strong peak heatng; strong peak coolng; weak peak heatng; weak peak 9 L L + Al 11 Ce 3 (h) Sample 9 Temperature, C L + (S) + τ 1 P C L + (S) + τ 2 E C L + τ 1 U 11 (S) + τ 2 + τ 1 (Al) + (S) + τ 2 (Al) + τ 2 + τ 1 U 6 L + Al 11 Ce 3 (l) + τ 1 (Al) + E 1 Al 11 Ce 3 (l) + τ 1 Al 0 Ce 20 S 80 S Al, at.% Al 80 Ce 20 S 0 Ce 20 at.% Ce Al.met.tu-clausthal.de/agrsfagrsf
10 Impact of ternary parameters 10 extrapolated from bnares, no ternary parameter, L=0 Hg B Sn.met.tu-clausthal.de/agrsfagrsf
11 Impact of ternary parameters 11 Careful wth ternary L-parameters! Fttng tool for phase dagrams? - Check mpact on actvtes! Bnary excess Gbbs energy: E G bn = L x A x B Ternary excess Gbbs energy: E G tern = L x A x B x C a C =x C along the secton x C = 0.5 Because RT ln γ C = L x A x B (1-2 x C ).met.tu-clausthal.de/agrsfagrsf
12 Problems usng frst-generaton software 12 Software does not always fnd stable phase equlbra User may not know all the ntal values Phase dagrams dffer for gven thermodynamc descrpton Relablty problem: Global Gbbs energy mnmum not found automatcally Y. Austn Chang, Shuangln Chen, Fan Zhang, Xnyan Yan, Fanyou Xe, Raner Schmd-Fetzer, W. Alan Oates: Progr. Mater. Scence, 49 (2004) met.tu-clausthal clausthal.de clausthal.de /agrsf/
13 Problems usng frst-generaton software 13 Software problem Assessment problem 1. Inverted mscblty gap 2. Low-T phases stable agan at hgh-t 3. Ordered phases overlooked Calculated constraned phase dagrams (e.g. metastable Fcc) often do not make sense. Publshed assessments contan errors.met.tu-clausthal clausthal.de clausthal.de /agrsf/
14 Inverted mscblty gap: S-Ta 14 Sn-Zr S Ta Calculated by [89Vah] More examples: Error detected by Pandat Co-Mo [99Dav], S-W [89Vah], Al-Mo [97Sau], Al-W [98Ans], Al-N [98Ans], Fe-S [98Ans], Sn-Zr [98Ans], Sn-T [98Ans]: Temp < 3000 K n most of these cases..met.tu-clausthal clausthal.de clausthal.de /agrsf/
15 Low-T phases stable agan at Hgh-T: Co-S 15 Calculated dagram by [92Cho] Error detected by Pandat More examples: Nb-C [97Hua], Mo-C[88Ans], Fe-C [85Gus], N-C [87Gab], Al-Co [98Dup], Cr-Ta [93Cup], N-T [96Bel]..met.tu-clausthal clausthal.de clausthal.de /agrsf/
16 Ordered phases overlooked: Al-Nb 16 Calculated dagram by [98Ans] Error detected by Pandat Other example: Fe-Ta [93Coe].met.tu-clausthal clausthal.de clausthal.de /agrsf/
17 Termnal soluton reappears: Mg-Sn 17 hcp L hcp L T[C] T[C] hcp Mg Calculated dagram [1993Fre] J. Chm. Phys. (1993) 90, Sn hcp : regular soluton L Mg,Sn = *T; L-parameter s too negatve MG SN X[SN] X[SN] Mg Error detected by Pandat Sn.met.tu-clausthal clausthal.de clausthal.de /agrsf/
18 Improbable Constraned Phase Dagram: Cr-Ta Ordered LT stable at hgh T Temp. / K Bcc Lqud Cr 2 Ta_HT Cr 2 Ta_LT Bcc Temp. / K Bcc Cr2Ta_HT Cr 2 Ta_LT Cr 2 Ta_LT Bcc Mol. fracn. Ta Calculated by [93Dup] Mol. fracn. Ta Constraned Phase dagram: Metastable dagram (no Lqud) calculated by Pandat usng the same parameters of [93Dup].met.tu-clausthal clausthal.de clausthal.de /agrsf/
19 Constraned Phase Dagram: Cr-Ta Improved modelng: C15 (LT) & C14 (HT) phases usng Cluster Ste Approxmaton (CSA) wth fewer parameters [2001Zha] 3500 Lqud Cr 2 Ta_HT Temp. / K Bcc Cr 2 Ta_HT Cr 2 Ta_LT Bcc Temp. / K Cr 2 Ta_LT Bcc Mol. fracn. Ta Calculated by [2001Zha] Mol. fracn. Ta Metstable dagram (no Lqud) calculated by [2001Zha] [2001Zha] F. Zhang, S.-L. Chen, Y. A. Chang and W. A. Oates, An Improved Approach for Obtanng Thermodynamc Descrptons of Intermetallc Phases: Applcaton to the Cr-Ta System, Intermetallcs, 2001, 9, met.tu-clausthal clausthal.de clausthal.de /agrsf/
20 Problems usng frst-generaton software 20 These mstakes have been made when the desred answers are known (the expermental bnary phase dagrams). How can we rely on calculatons carred out ths way when the answer s not known (multcomponent phase dagrams)? Example: 27 elements (COST database) 351 bnares 2925 ternares quaternares..met.tu-clausthal clausthal.de clausthal.de /agrsf/
21 Second-generaton: Pandat 21 Fnds automatcally the correct phase dagram gven a thermodynamc descrpton. No user knowledge on demxng or orderng requred. No ntal values requred..met.tu-clausthal clausthal.de clausthal.de /agrsf/
22 Al-Mg-Cu-Zn-Mn-S wth x Mg =x Cu =x Mn =x S = L T[C] fcc 1 +fcc 2 +(S)+σ+τ+Al 4 Mn L+β-AlMnS L+Mn 11 S L+β-AlMnS+δ- AlMnS X[ZN].met.tu-clausthal clausthal.de clausthal.de /agrsf/
23 Outlne 23 Calphad method Thermodynamc databases Example: Mg alloy database Ternary parameters Key experments Qualty problems wth bnary systems Applcatons Developng creep resstant Mg alloys Solderng Al-alloy soldfcaton, mcrosegregaton.met.tu-clausthal.de/agrsfagrsf
24 ADAMIS 24 Alloy Database for Mcro-Solders Elements: Ag, B, Cu, In, Sb, Sn, Zn, Pb Thermodynamc Assessment Surface tenson and vscosty X. J. Lu, I. Ohnuma, R.Kanuma, K. Ishda: Tohoku Unversty, Japan S. L. Chen and Y. A. Chang: CompuTherm & Unversty of Wsconsn, USA
25 ADAMIS Pandat PanEngne 25 Phase dagram calculaton Lqudus projecton ($ 3 components) Soldfcaton smulaton Schel, equlbrum Surface tenson and vscosty calculaton (ternary contours)
26 Surface Tenson and Vscosty at Constant Composton 26 Sn-X Canddate Solders (mostly eutectc composton) Surface Tenson Vscosty
27 Vscosty Contour 27 Lqud Sn-Sb-B Alloys at 900 K X[SB] X[BI] X[BI] X[SB] 0.85mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn mPas Sb B Sn 5 www com www scence.co co.jp jp clausthal.de/.de/agrsf agrsf
28 Surface Tenson and Vscosty Contours 28 Lqud Sn-Cu-Ag alloys at 1000 C Surface Tenson Vscosty 0.87 Cu Cu mn/m mpa.s X[CU] 0.43 X[CU] X[CU] 0.43 X[CU] Sn X[AG] X[AG] Ag Sn X[AG] X[AG] Ag
29 σ = σ + RT S Partal excess Gbbs energes: c = 1 ln Surface Tenson σ xs* = β G Extrapolaton by knowledge of excess Gbbs energy G xs J. A. V. Butler, Proc. Roy. Soc.A, A135 (1935) K. S. Yeum, R. Speser and D. R. Porer, Metall. Trans.B, 20B(1989) T. Tanaka and I. Ida, Steel Research, 65 (1994)p. 21. a a = 1 c components x * = 1 * * RT x 1 σ = σ + ln + β S x S σ S a G surface tenson of pure lqud (), molar surface area n a monolayer of pure lqud () actvty of () n bulk alloy a * actvty of () n "surface phase * " S = bn xs 1/ 3 2 / 3 V ( xs * xs G ( T, x ) G ( T, x )) β = 0.83 for lqud metals b = 91 for close-packed lattce ( = 1...c ) Solve these c+1 equatons for the c+1 unknowns σ and x * 29.met.tu-clausthal.de/agrsfagrsf
30 Vscosty η 30 η = G # hnρ G exp M RT # Gbbs energy of actvaton hn = Js/mol M ρ x ρ ρ densty of pure () = = x M M atomc mass of pure () G # = # x + + G 3RT xx j RT x ln x + < j G # = f(t) Gbbs energy of actvaton of pure () G xs ( T, x ) Extrapolaton by knowledge of excess Gbbs energy G xs H. Eyrng, J. Chem. Phys., 4 (1936) S. Seetharaman and D. Schen, Metall. Mater. Trans. B, 25B (1993)
31 User-Frendly Interface 31 Same as Pandat plus extra buttons
32 Concluson 32 Thermodynamc databases Qualty of data s vtal - scrutnzng publshed datasets Lnk key experments to modelng Applcatons Alloy development Process optmzaton.met.tu-clausthal.de/agrsfagrsf
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