Informations: microstructure
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1 Informations: microstructure Crystallite sizes, anisotropic, distribution Microstrain (III kind), distribution, dislocation or point defects density Antiphase domains (intermetallics ) Stacking and deformation faults probability, intrinsic, extrinsic
2 Crystallites distribution Name Definition Mean length M = Length weighted or area-length D = Area weighted or volume-area D a = Volume-weighted D V = Ni=1 n i d i Ni=1 n i Ni=1 n i d 2 i Ni=1 n i d i Ni=1 n i d i 3 Ni=1 n i d i 2 Ni=1 n i d i 4 Ni=1 n i d 3 i
3 Line broadening methods! Are based on profile analysis: Crystallites and microstrain have a different broadening behavior in 2theta! Several methods available: Scherrer equation (1918): Williamson-Hall plot Warren-Averbach or Fourier analysis...! Instrumental broadening must be subtracted! Two reflections are needed to separate crystallite and microstrain broadening! More reflections for anisotropic broadening! Planar defects analysis was developed by Warren (see book)
4 The Warren-Averbach analysis Warren treatment for a 00l peak: S 2 = S S 2 z S I z dz (Stokes treatment: A=A S A I ) Fourier coefficients: A n = A S n AD n = N n N 3 cos 2 lz n inf A S n = N n = 1 i n p i N 3 N 3 i= n ( ) da S n = 1 dn N 3 n 0 is the fraction of columns having leng
5 Get the profiles for Fourier transform We need two peaks of different order, same hkl direction
6 W-A continue...
7 Planar faults No faults assumed Stacking and deformation faults
8 Order-disorder transition in intermetallic! Applications: High temperature structural material Oxidation resistance Blade material for Gas turbine! Main problem: Ductility (forming and shaping) Brittle at low temperature! Disordered phase is more ductile! Materials: FeAl, Ni3Al, NiAl, TiAl...
9 Disordering FeAl by ball-milling Intensity- 1 / 2 [counts- 1 / 2] h 150 6h 100 3h 1.5 h h 0 0h ! [degrees]
10 Faults effect Anisotropic size model Faulting model (Warren) Intensity (counts) a) b) ! (degrees) ! (degrees)
11 Defect analysis on ball-milled FeAl Long Range Order LRO Deformation faulting (intrinsic) Deformation faulting (extrinsic) Twin faulting Antiphase domain Milling time [h] Deformation faulting probability Crystallite size [nm] Crystallite size Microstrain Milling time [h] Microstrain
12 FeAl annealing (neutron-xrd meas.) LRO XRD (RT measurments) LRO neutron Deformation faults Microstrain Antiphase LRO Defects Temperature [ C]
13 Quantitative phase analysis I j k = I f j V j 2 L k F k, j 2 Pk, j A j! Methods: Polymorph method RIR Rietveld...! Crystallinity determination f 1 f 2 = I 1 An external or internal standard is needed Traditional methods are based on the change in intensity of the crystallized fraction adding a crystalline standard Method without standard: Rietveld + pseudo amorphous model (Le Bail) k I 2 s V 1 2 L s F s,2 2 V 2 2 L k F k,1 2
14 Cermet: Ni-Al2O3! Alumina is quite inexpensive as high temperature structural material! Lack of toughness! Ductile metal inclusions! Ni, Ag, FeAl, NiAl.! Nickel is very ductile (relatively low temperature applications)
15 Cermet production (Ni-Al2O3)! Powder metallurgy! Forming and sintering! Cold Isostatic Pressing and sintering! Hot Pressing! Active binder Binder + powder Al2O3 - Ni Polimerization and forming Thermal treatment (decomposition) + sintering
16 SEM: Al2O3-40 % Ni
17 Mechanical properties! Toughness: SENB-S modified! Elastic modulus three point bending
18 Density and Hardness
19 Toughness and R-curve KIC (MPa!m) a (mm)
20 Quantitative phase analysis
21 Quantitative phase analysis: problems! High contrast in absorption between Ni and alumina No Correction Brindley Cubic Corr. Brindley Spheric Corr. %Al 2 O 3 VOL %Ni VOL %Al 2 O 3 VOL %Ni VOL %Al 2 O 3 VOL %Ni VOL Al 2 O % VOL Ni Powders 72.1 (2) 27.9 (2) 61.3 (2) 38.7 (2) 63.8 (2) 36.2 (2) Pure Al 2 O 3 F1 100 (0) 0 (0) 100 (0) 0 (0) 100 (0) 0 (0) Al 2 O % VOL Ni F (1) 5.34 (1) 89.9 (1) 10.1 (1) 91.2 (1) 8.8 (1) Al 2 O % VOL Ni F (1) 11.9 (1) 79.9 (1) 20.1 (1) 82.0 (1) 18.0 (1) Al 2 O % VOL Ni F (2) 19.3 (2) 70.4 (2) 29.6 (2) 72.9 (2) 27.1 (2) Al 2 O % VOL Ni F (3) 29.9 (2) 59.2 (3) 40.8 (2) 61.7 (3) 58.1 (2) Pure Al 2 O 3 F1C (0) 0 (0) 100 (0) 0 (0) 100 (0) 0 (0) Al 2 O % VOL Ni F1C (1) 8.6 (1) 84.6 (1) 15.4 (1) 86.4 (1) 13.6 (1) Al 2 O % VOL Ni F1C (1) 11.8 (1) 79.8 (1) 20.2 (1) 82.0 (1) 18.0 (1) Al 2 O % VOL Ni F1C (2) 20.2 (2) 69.4 (2) 30.6 (2) 71.9 (2) 28.1 (2) Al 2 O % VOL Ni F1C (3) 29.4 (3) 60.4 (3) 39.6 (3) 62.9 (3) 37.1 (3) Al 2 O % VOL Ni HP (b) 88.4 (1) 11.6 (1) 80.4 (1) 19.6 (1) 82.4 (1) 17.6 (1) Al 2 O % VOL Ni HP (w) 88.4 (1) 11.6 (1) 80.3 (1) 19.7 (1) 82.4 (1) 17.6 (1) Al 2 O % VOL Ni HP (Mo) 89.7 (1) 10.3 (1) 78.8 (1) 21.2 (1) 81.4 (1) 18.6 (1) Al 2 O % VOL Ni HP (b) 73.8 (2) 26.2 (2) 63.1 (2) 36.9 (2) 65.6 (2) 34.4 (2) Al 2 O % VOL Ni HP (w) 70.2 (2) 29.8 (2) 59.2 (2) 40.6 (2) 61.9 (2) 38.1 (2) Al 2 O % VOL Ni HP (Mo) 76.1 (3) 23.9 (2) 61.5 (3) 38.5 (2) 64.7 (3) 35.3 (2) Use neutron
22 Pseudo-amorphous approximation! Le Bail, A., J. Non-Cryst. Solids, 183, pp , 1995
23 Corundum+amorphous silica mixed
24 Result of the Rietveld analysis using the pseudo-amorphous approx.
25 Sanitary ware (>60% silica glass)
26 Ceramics for high temperature
27 Results
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