Thermodynamic and thermal analysis of Mg cast alloys

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1 Thermodynamic and thermal analysis of Mg cast alloys Jožef Medved, Primož Mrvar, Maja Vončina University of Ljubljana, Faculty of natural science and engineering Department of materials and metallurgy Aškerčeva 12, Ljubljana, Slovenia

2 Purpose: Complex investigation of Mg - alloys Topics: -Thermodynamic calculation -Thermal analyses (ETA, DSC, TG) - Non-metallic inclusions characterization, mechanical properties - High temperature corrosion resistance

3 Isopleth phase diagram Mg Al Mn at 6,28 mass.% Al 0,3056 mass. % Mn, 0,0294 mass. % Si and 0,0032 mass. % Fe. AL11MN4#1 STATUS ENTERED Number of moles 8,3785E-03, Mass 2,8853E-01 Mass fractions: AL 5,74581E-01 MG 0,00000E+00 MN 4,25419E-01 ZN 0,00000E+00 HCP_A3#1 STATUS ENTERED Number of moles 9,9162E-01, Mass 2,4262E+01 Mass fractions: MG 9,44096E-01 ZN 2,02378E-03 AL 5,38805E-02 MN 2,55276E-07

4 Measuring cell Measuring card PC A new eequipment with the measuring cell for»in situ«thermal analyses of Mg and Al alloys.

5 University of Ljubljana - NTF - Department for materials and metallurgy Experimental - ETA

6 Cooling curves and microstructures of Mg and 5,7 K/s 5,7 K/s alloy MgAl4 5,7 K/s 604 C C 438 C 0 T [ C] dt/dt [K/s] Cooling curve (T) Cooling rate (dt/dt) t [s]

7 700 T L =611,4 C 1, T E =511,2 C T E2 =431 C T S =426 C 0,5 Cooling curve and isoplet phase diagram of AM T [ C] ,0-0,5 dt/dt [ C/s] , t [s]

8 Cooling curve, microstructure and phase diagram of AM T L =607,6 C 1,0 600 T E =509,4 C 0,5 T [ C] T E2 =432,9 C T S =428,1 C 0,0-0,5 dt/dt [ C/s] 300-1, t [s]

9 700 University of Ljubljana Faculty of material science and engineering Department for materials and metallurgy T L =581,4 C T E =510,7 C 1 Cooling curve and phase diagram of AZ T E2 =424,1 C T [ C] 500 T S =410,8 C 0 dt/dt [ C/s] 400 Cooling curve of AE t [s] 700 T L =619,3 C 1 T E =598,2 C 600 T S =566,5 C 0 T [ C] dt/dt [ C/s] t [s]

10 DSC mesurements of Mg-alloys Crucibles material: platinum. Heating and cooling speed: 10 K/min. Max. temp.: 720 C Atmosphere: vacuum, nitrogen.

11 STA heating curve of the AM50 alloy L α Mg L (αmg+mg17al12)

12 STA cooling curve of the AM60 alloy L α Mg L (αmg+mg17al12)

13 DSC analysis of solidification of Mg- alloys

14 DSC analysis of solidification of Mg- alloys

15 DSC analysis as melt control method Comparison of melting Enthalpy ) Enthalpy (J/g) Material 1. Hydro 2. Elektron 3. Mimet 4. Gold River

16 Conclusion AM60 T [ C] 1: α Mg 2: Al 4 Mn 3: Tekoče 4: Al 11 Mn 4 5: Mg 2 Si 6: Al 8 Mn 5 7: Cu 2 Al 9: Mg 17 Al 12 AM 60 mass. % Al T [ C] 800 T L =610 C T S =569 C T E =418 C 0-4 dt/dt [K/s] 200 Cooling curve (T) Cooling rate (dt/dt) t [s]

17 Non-metallic inclusions characterization Stehiometric compositions of inclusions and Gibbs free energies ( G). Zap. Št. Spojine Temperatura razpada G(kJ/mol) 1 2MgO*2Al 2 O 3 *5SiO CaO*Al 2 O 3 *3SiO CaO*MgO*3SiO K 2 O*4SiO CaO*Al 2 O 3 *2SiO CaO*Al 2 O 3 *SiO CaO*MgO*2SiO CaO*Al 2 O 3 *SiO CaO*MgO*2SiO MgO*Al 2 O CaO*SiO MgO*SiO CaO*MgO*SiO CaO*Fe 2 O MnO*Al 2 O Al 2 O MgO*SiO MgO*MoO CaO*MoO CaO*MgO MgCO SiO CaCl MoO MgCl MgO CaO MoO CaS KCl NaCl FeCl MgS SiS

18 1) 2) 3) 2 mm Microstructure of AM60 alloy in a HDC as-cast sate; a) primary dendrite α Mg (1), inter-metallic compound Mg 17 Al 12 (2) and Al 4 Mn (3), b) Macro photo of specimen. 9 mm

19 Kem. At. % Mas. % el O 76,767 65,161 Mg 1,013 1,306 Si 21,583 32,156 SEM micro photo of SiO 2 particle in AM 60 alloy. Probable source of SiO 2 particles: - Silicon-thermal reduction: T >1200 C..4MgO + Si Mg 2 SiO 2 + 2Mg - Mg 2 SiO 2 can not be reduce by Si under 1500 C. - If MgO in magnesium silicate is replaced by CaO (dolomite can be used): 2CaMgO 2 + Si 2Mg + Ca 2 SO 4

20 Kem. el. At. % Mas. % O 37,052 24,600 Mg 52,349 52,798 Al 2,342 2,622 Ca 5,525 9,188 Mo 2,681 10,675 SEM micro photo of inclusion on base of Mo, Ca, Mg and O. Probable source of inclusion: -Possible compounds are: MgO MoO 3, CaO MoO 3, MoO 3 in MoO 2 -According to the lowest value of G, inclusion can be compound CaO MoO 3 + MgO.

21 High temperature corrosion resistance Although magnesium alloys are used at room temperatures, they can be putted out to the high temperatures and oxidizing atmospheres in different stages of processing, such as: overheating of charge, melting, pouring, heat treatment and mechanical processing, recycling etc. The results are undesirable effects that change chemical properties and deteriorate structural properties of surface layers. For this reason, the knowledge of oxidation of Mg-alloys at different temperatures is important for optimization of technological processes. Protective oxide layer The growth of oxide flowers

22 Experimental work Cylindrical samples with diameter 4.0 mm and height 2,0 mm were prepared. The samples were searched by TG on STA 449 Jupiter Instrument (NETZSCH). The samples were heated in protective gas (nitrogen) till oxidation temperatures (200, 400, 450 and 500 C), with the heating speed of 20 K/min. The samples were then held in oxygen atmosphere for 12 h. Then cooling with 20 K/min followed till room temperature. Chemical composition of tested alloy Alloy Mg (mass %) Al (mass %) Si (mass %) Mn (mass %) Zn (mass %) AE42 Ost. 4,2 0,03 0,29 0,15 1,5 RE AM50 94,7 4,7-0,40 0,12 AM60 93,7 5,84 0,028 0,33 0,05 AZ91 Ost. 8,5-9,5-0,17-0,4 0,45-0,9

23 University of Ljubljana Faculty of material science and engineering Department for materials and metallurgy Results 450 C 200 C TG curves and structures for AE42 alloy

24 University of Ljubljana Faculty of material science and engineering Department for materials and metallurgy 450 C 400 C TG curves and structures for AZ91 alloy

25 University of Ljubljana Faculty of material science and engineering Department for materials and metallurgy 450 C 400 C TG curves and structures for AM50 alloy

26 University of Ljubljana Faculty of material science and engineering Department for materials and metallurgy 450 C 400 C TG curves and structures for AM60 alloy

27 Mass changes for all samples at 200 C

28 Mass changes for all samples at 450 C 450 C m AM50 = 99, ,00222 t m AE42 = 99, , t m AM60 = 99, ,00712 t - 1, t 2 + 1, t 3 m AZ91 = 121, ,74693 t + 0,0083 t 2-3, t 3 + 5, t 4-3, t 5

29 Calculated polythermal phase diagram Mg-Al-Mn (a) and b) binary phase diagram Al-Mg. a) b) T [ C] 800 T L =610 C T S =569 C T E =418 C dt/dt [K/s] 200 Cooling curve (T) Cooling rate (dt/dt) t [s] Microstructure and cooling curve of Mg-alloy at 5,7 K/s cooling rate

30 The results of heating and cooling DSC curves indicate the course of melting and solidification of Mg-Al alloys. The addition of Al decreases liquidus temperature. DSC curves show that alloys with 5 or more mass % of Al have another peak of solidification. Optical microscopy reveals that this is due to cooling with nonequilibrium eutectic crystallization; It has been proved that on all examined alloys during heating at oxidation temperature, a thin oxide layer appears which has a protective nature. The alloys that have eutectic in microstructure are protected by the oxide layer up to the first incipient fusion (equilibrium up to 437 C, practically up to 400 C). In alloys without eutectic the protective oxide layer exists up to higher temperatures. It is evident that the most stable alloy at high temperatures is AE 42 and the most unstable is AZ 91. Alloys with bigger Al addition have lower corrosion stability.

31 Thank You for your attention Hvala za pozornost

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