In-situ Scattering Study of Phase Transformation Kinetics

Xun-Li Wang Neutron Scattering Science Division Oak Ridge National Laboratory

Outline
• Why are phase transformations of interest? • Why kinetics? • How are neutrons used to study phase transformations? • Future opportunities

OAK RIDGE NATIONAL LABORATORY
U. S. DEPARTMENT OF ENERGY

The structure of a material at various length scales

Graphite

Diamond

Metallic Glass

TRIP Steel
OAK RIDGE NATIONAL LABORATORY Nanocrystalline Ni Nanoscale clusters
U. S. DEPARTMENT OF ENERGY

S. DEPARTMENT OF ENERGY .Structure Affects Properties OAK RIDGE NATIONAL LABORATORY U.

S. Acta Cryst. DEPARTMENT OF ENERGY ..Structural change during curing of cement (Chakomakous et al. 1992) OAK RIDGE NATIONAL LABORATORY U.

S. Nature Mat. crystalline amorphous? OAK RIDGE NATIONAL LABORATORY U. DEPARTMENT OF ENERGY .Structure of metallic glass? Miracle.

DEPARTMENT OF ENERGY . S.The structure of a material at various length scales Graphite Diamond Metallic Glass TRIP Steel OAK RIDGE NATIONAL LABORATORY Nanocrystalline Ni Nanoscale clusters U.

DEPARTMENT OF ENERGY .OAK RIDGE NATIONAL LABORATORY U. S.

S. OAK RIDGE NATIONAL LABORATORY U.NANOCLUSTERS IN IRON MATRIX 4nm 2nm The nanoclusters were estimated to be 2-3 nm in diameter with a spacing of 12 nm in agreement with APT. DEPARTMENT OF ENERGY 14YWT 1 h at 1000°C .

S.000 0 5 10 15 Particle Size Radius (nm) and thermally stable up to 1400 C OAK RIDGE NATIONAL LABORATORY U.020 0.015 0.025 Particle Size Distribution Function (N*v) 0. DEPARTMENT OF ENERGY .Small Angle Neutron Scattering showed a bi-modal size distribution 0.005 0.010 0.

. DEPARTMENT OF ENERGY .Microstructure Cross-section of a friction stir weld showing distinct microstructure zones generated by heat and mechanical work Hardness profile through the different microstructure zones reflects the changes in microstructure Wang et al.Structure Determines Properties . 1999 OAK RIDGE NATIONAL LABORATORY U. S.

DEPARTMENT OF ENERGY endurance .Microstructure of TRIP Steel • TRansformation Induced Plasticity steels • Retained austenite transforms into martensite (a hard phase) during deformation • Hard martensite delays the onset of necking resulting in high total elongation OAK RIDGE NATIONAL LABORATORY • Extremely high fatigue U. S.

DEPARTMENT OF ENERGY . S.Why Kinetics? • Because we must ! − Mechanisms of nucleation − Mechanisms of growth − Nature of intermediate and meta-stable phase −… − Ultimate goal is achieve structure control − Effect on properties • Because we can ! − In-situ time-resolved measurements OAK RIDGE NATIONAL LABORATORY U.

What we are interested in are evolution of the structures at multiple length scales Length & Time OAK RIDGE NATIONAL LABORATORY U. DEPARTMENT OF ENERGY . S.

Examples • Kinetic study of order-disorder phase transformation in Ni3Mn (1986) • Kinetic study of α→β phase transformation in Mn (1999) • Fatigue-induced phase transition (on-going) • Transient behavior during welding • Crystallization of bulk metallic glass OAK RIDGE NATIONAL LABORATORY U. S. DEPARTMENT OF ENERGY .

S.error | peak position (220) (211) (210) (111) (110) (200) (100) Grain morphology and size distribution Ni Fe Al OAK RIDGE NATIONAL LABORATORY U. Dwide angle diffraction EPARTMENT OF ENERGY . Fe) + data -.How are neutrons used to determine structures? small angle scattering Ni (Al.refined -.

S. DEPARTMENT OF ENERGY .Order-disorder phase transformation in Ni3Mn • Very difficult to study with X-ray − Mn Z=25 − Ni Z=28 • Ideal for neutrons − Ni b=10.8 fm • Tc=510 C OAK RIDGE NATIONAL LABORATORY U.3 fm − Mn b=-3.

S. DEPARTMENT OF ENERGY .Real-time measurements – peak width (211) reflection OAK RIDGE NATIONAL LABORATORY U.

DEPARTMENT OF ENERGY .Kinetic study of α→β phase transformation in Mn OAK RIDGE NATIONAL LABORATORY U. S.

DEPARTMENT OF ENERGY . S.Kinetic study of α→β phase transformation in Mn • Experiments done on HRPD at ISIS − 100 m instrument − Very high Δd/d resolution of ~ 4 × 10-4 • Time resolution: 5 minutes per data set OAK RIDGE NATIONAL LABORATORY U.

Multiphase Rietveld analysis to yield volume fraction OAK RIDGE NATIONAL LABORATORY U. DEPARTMENT OF ENERGY . S.

DEPARTMENT OF ENERGY . S.Multiphase Rietveld analysis to yield volume fraction Tremendous difference in growth rates OAK RIDGE NATIONAL LABORATORY U.

S. DEPARTMENT OF ENERGY .Growth behavior follows scaling by Johnson-Mehl-Avrami theory OAK RIDGE NATIONAL LABORATORY U.

Phase transformation induced by cyclic loading (fatigue) The Case of ULTIMET 54Co-26Cr-9Ni-5Mo-3Fe-2W (wt%) fcc hcp OAK RIDGE NATIONAL LABORATORY U. OH. S.1. ASM. DEPARTMENT OF ENERGY *Source: Binary Alloy Phase Diagrams. p. 759. vol. . Metals Park. 1986.

DEPARTMENT OF ENERGY .In-situ Neutron Diffraction Incident Neutron Beam Axial Detector Bank • ENGIN-X at the ISIS facility. • Pulsed neutron source. RIDGE et al. S. • 40 minute count times. Transverse Detector Bank Specimen Load Frame OAKBenson NATIONAL LABORATORY 2005 M. Co scatters poorly. UK. Powder Diffraction U. • Sampling volume: ~120 mm3..

tension-compression (R is the ratio of the minimum strain to maximum strain). 24 mm gage length. M12 threaded ends. Δε = 2. DEPARTMENT OF ENERGY .In-situ Neutron Diffraction Collimator Specimen • Strain-controlled fatigue: R = -1. S. f = 0. Powder Diffraction U.5 Hz. OAKBenson NATIONAL LABORATORY 2005 M.. • Total strain range. • Cycling frequency. Extensometer • Cylindrical specimens of 8 mm gage diameter.5 %. RIDGE et al.

” 500 cycles 250 cycles 100 cycles 75 cycles 50 cycles 30 cycles 12 cycles 8 cycles 4 cycles 1 cycle 0 cycles 111 311 103 220 102 200 101 1.000 X 0 0. S.5 -500 fcc OAKBenson NATIONAL LABORATORY 2005 M.5 500 0 -1.000 -1. RIDGE et al.5 1 1. DEPARTMENT OF ENERGY hcp -1.5 -1 σ -0.500 1.500 ε ..Evolution of the hcp phase during fatigue test Overlay of the axial detector bank diffraction patterns measured at “point 1. Powder Diffraction U.

Brooks. • Similar trends in both the axial and transverse detector banks. • Attributed to the interaction of stacking faults during low cycle fatigue. K Liaw. • Demonstrates the incubation period found in austenitic stainless steels during low cycle fatigue*. Jiang. . OAK RIDGE NATIONAL LABORATORY Rawn. A. R. R. C. 1997. Dunlap. ASM International. P.** Axial Detector Bank Transverse Detector Bank * Source: ASM Handbook. Peascoe. C. U. S. Vol. **Source: L.Increase in the HCP Peak Intensity as a Function of Fatigue Cycles Increase in intensity of the hcp (101) peak. L. 18. and D. DEPARTMENT OF ENERGY Klarstrom. J. • Demonstrates increase in volume fraction as fatigue progresses and strain accumulates. Met Trans A (2004) 35 3 785-796. J.

Bulk Metallic Glass Materials Exhibit Unconventional Properties • Excellent mechanical properties • Controllable magnetic properties Nd-Fe-Co-Al 15 10 M (kAm kg ) -1 2 5 0 -5 -10 -2000 -1000 0 1000 -1 as-cast 723 K 748 K Ribbon 2000 H (kAm ) OAK RIDGE NATIONAL LABORATORY U. DEPARTMENT OF ENERGY . S.

g. upon isothermal annealing • Density 1023-1024 m-3 • Crystallite size ~10-50 nm • Even for temperatures close to Tg OAK RIDGE NATIONAL LABORATORY U..Partially Crystallized Bulk Metallic Glass Contains High-density Nanometer Sized Crystallites • e. S. DEPARTMENT OF ENERGY .

Letter... S. DEPARTMENT OF ENERGY Wang et al.. 2003 Wang et al. unpublished Ti m e (s ec ) . Phys. Rev.Simultaneous Diffraction and Small Angle Scattering in Bulk Metallic Glass Show Concurrent Structural and Chemical Ordering amorphous crystalline Structural changes in two length scales Diffraction SAXS (s ec ) e Ti m Q (A-1) Q (A-1) OAK RIDGE NATIONAL LABORATORY U.

DEPARTMENT OF ENERGY . S.In-situ Neutron Diffraction Measurements Revealed for the first time Stress and Temperature Profiles during Friction Stir Welding x z y OAK RIDGE NATIONAL LABORATORY U.

2×108 in high-int. mode • Wide angle detector coverage. DEPARTMENT OF ENERGY . mode − 1.2% • λ ~ 0.01 – 0.5 Å • Flux on sample (n/s/cm2/Å) − 3×107 in high-reso.VULCAN Technical Data • Flight paths − Incident ~ 43. 60-150° • SANS Q-range − 0.2 Å-1 OAK RIDGE NATIONAL LABORATORY U. S.5 m − Scatting ~ 2 m • Satellite building • Resolution ~ 0.9-3.

with high flux. the control of structural evolution in materials. DEPARTMENT OF ENERGY .Summary • Next generation neutron scattering instruments. ultimately. S. will lead to major breakthroughs in our understanding and. OAK RIDGE NATIONAL LABORATORY U.

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