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Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20081 Characterisation of Microstructure.

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Presentation on theme: "Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20081 Characterisation of Microstructure."— Presentation transcript:

1 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20081 Characterisation of Microstructure in model ODS Alloys Arup Dasgupta Physical Metallurgy Division Indira Gandhi Centre for Atomic Research Kalpakkam – 603102, INDIA A collaborative work between IGCAR, Kalpakkam and International Advanced Research Centre for Powder Metallurgy and New Materials, Hyderabad

2 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20082 SCHEME The Issue –What kind of alloy is under development –Processing Scheme –Importance of microstructure and microchemistry investigations in alloy development This Talk –Types of samples studies so far –Results and Discussion –Summary

3 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20083 The Alloy under development 9Cr-0.12C-2W-0.2Ti-0.35Y 2 O 3 Ferritic/Martensitic steel chosen because of advantages over austenitic stainless steels: Higher thermal conductivity Lower thermal expansion Lower void swelling during irradiation Excellent high temperature creep resistance W  Mo replacement for solid solution strengthening; reduced activation Ti  Helps to get finer dispersoids Mandate: Clad Tubes (6.6mm OD, 0.45mm thick, 2.65 m long)

4 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20084 Processing Scheme Courtesy: IGCAR ODS Task force, ARCI - Hyderabad Extr. Rods Mother Tubes Clad Tubes Mult. Pass CW Int. Heat Trtmt. Machining

5 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20085 Importance of Microstructural & Microchemical Investigations MA systems Grain morphology Phase stability Microstructural Uniformity Mechanical Interdiffusion (Microchemical Uniformity) Milling process + Subsequent Annealing Steps Dispersoid  Large strain fields Shape Size Distribution Interface with matrix Dislocations, other defects Impurities  Microstr.  Mech. Prop. Microstructure / Microchemistry Purity of feed powders, containers, milling conditions

6 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20086 Samples Studied #ODS 0: 48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1: Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

7 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20087 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

8 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20088

9 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 20089 3 size ranges: (a)large, facetted (Fe-Co) (b)50 – 75 nm (Fe-Ti) (c)sub-10 nm (Fe) Fe Co Courtesy: Institute Nano- science Initiative IISc, Bangalore - Tecnai F-30

10 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200810 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

11 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200811

12 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200812 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

13 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200813

14 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200814 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

15 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200815 Porosity ~ 1%

16 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200816 SADP Selection Rule FCC : (h k l) all odd / even BCC : h + k + l even

17 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200817 DF

18 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200818 IMPURITY

19 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200819 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

20 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200820 ElementWt. % Ti0.57 Cr9.78 Fe87.18 W2.46

21 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200821 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.16C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.16C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

22 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200822 Av. Particle Size (XRD) : 42 nm

23 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200823 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

24 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200824

25 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200825 Samples Studied #ODS 0:48h Milled Fe-0.2Ti-0.35Y 2 O 3 Powder #ODS 1:Fe-0.35Y 2 O 3 Fe (150µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vacuum, double compacted, double sintered at 1323K / H2 #ODS 2: Fe-0.2Ti-0.35Y 2 O 3 Fe (150µm), Ti (105µm) and Y 2 O 3 (1.33µm) ball milled / 30h, annealed at 973K / vac., double compacted, double sintered at 1323K / H2 #ODS 3: Fe-0.2Ti-0.35Y 2 O 3 - Forged Fe (150µm), Ti (105µm) and Y 2 O 3 (10-20nm) attritor milled / 20h, degassed at 723K & sealed. Can hipped/ forged at 1323K/ 1000MPa #ODS 4: Fe-0.12C-9Cr-2W-0.2Ti – Pre-alloyed Powder – SEM Only #ODS 5: Yttria Powder #ODS 6: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Milled Powder #ODS 7: Fe-9Cr-2W-0.2Ti-0.35Y 2 O 3 -0.12C – Extruded at 1050 o C B1-ODS-S150-Z04-C46-D04-E1050-ER09

26 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200826 Pore Density ~0.3% aligned along Extrusion direction  Tears

27 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200827 Y L : 0.63 % Ti K : 0.36 % Cr K : 8.95 % Fe K : 87.6 % W L : 2.44 %

28 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200828 0

29 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200829 Summary Seven sets of model materials studied ( powders, milled, compacted products ) Higher Milling Duration  Agglomeration The sintered products were porous, 14-20% but forged material had a porosity ~1%. Extruded material had porosity ~0.3% only! Yttria  bcc with a=10.6 Å Forged sample  fine bcc yttria particles with an av. size ~ 10-20 nm; some were ~ 5-7 nm and some were agglomerated; there appeared to be an orientation between the Yttria and the rextallised ferrite grains Prealloyed powder & yttria powder  desired sizes + quite pure The extruded ODS steel  desired composition, fine martensite laths (~100 nm wide) within the elongated grains, very fine (~ 3nm) yttria.

30 Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102, India WS&FT-08 Physical Metallurgy Division, PMD 22 July 200830 Contributors IGCAR, KalpakkamARCI, Hyderabad Arup Dasgupta*, R Divakar, S Saroja, E Mohandas, M Vijayalakshmi, PV Sivaprasad, KBS Rao & Baldev Raj R Vijay, S Sudhakara Sarma, A Venugopala Reddy

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