STRUCTURE OF MATERIALS The Key to its Properties A Multiscale Perspective
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1 STRUCTURE OF MATERIALS The Key to its Properties A Multiscale Perspective Anandh Subramaniam Materials and Metallurgical Engineering INDIAN INSTITUTE OF TECHNOLOGY KANPUR Kanpur anandh@iitk.ac.in Jan 2009
2 Properties of Materials The Scale of Microstructures Crystal Structures + Defects Microstructure OUTLINE With Examples from the Materials World
3 PROPERTIES Structure sensitive E.g. Yield stress, Fracture toughness Structure Insensitive E.g. Density, Elastic Modulus Structure Microstructure
4 What determines the properties? Cannot just be the composition! Few 10s of ppm of Oxygen in Cu can degrade its conductivity Cannot just be the amount of phases present! A small amount of cementite along grain boundaries can cause the material to have poor impact toughness Cannot just be the distribution of phases! Dislocations can severely weaken a crystal Cannot just be the defect structure in the phases present! The presence of surface compressive stress toughens glass [1] Composition Phases & Their Distribution Defect Structure Residual Stress [1] Metals Handbook, Vol.8, 8 th Edition, ASM, 1973
5 Length Scales Involved Nucleus Atom Crystal Microstructure Component Defects Angstroms Dislocation Stress fields Nanometers Microns Unit Cell * Crystalline Defects Microstructure Component Grain Size Centimeters *Simple Unit Cells
6 Crystal Thermo-mechanical Treatments Casting Metal Forming Welding Powder Processing Machining Atom Structure Microstructure Component Electromagnetic Phases + Defects Avoid Stress Concentrators Good Surface Finish Crystalline Quasicrystalline Amorphous Ferromagnetic Ferroelectric Superconducting Structure based Property based Vacancies Dislocations Twins Stacking Faults Grain Boundaries Voids Cracks + Residual Stress Processing determines shape and microstructure of a component
7 Crystal Thermo-mechanical Treatments Casting Metal Forming Welding Powder Processing Machining Atom Structure Microstructure Component Electromagnetic Crystalline Quasicrystalline Amorphous Ferromagnetic Ferroelectric Superconducting Phases + & their distribution Structure based Property based Defects Vacancies Dislocations Twins Stacking Faults Grain Boundaries Voids Cracks Avoid Stress Concentrators Good Surface Finish + Residual Stress Processing determines shape and microstructure of a component
8 METAL SEMI-METAL SEMI-CONDUCTOR INSULATOR BAND STRUCTURE ATOMIC STATE / VISCOSITY GAS SOLID LIQUID LIQUID CRYSTALS STRUCTURE AMORPHOUS QUASICRYSTALS RATIONAL APPROXIMANTS CRYSTALS SIZE NANO-QUASICRYSTALS NANOCRYSTALS
9 Crystal Atom Structure Microstructure Component Electromagnetic Why is BCC Iron the stable form of Iron at room temperature and not the FCC form of Iron? 1 Atm G vs T showing regions of stability of FCC and BCC Iron (Computed using thermo-calc software and database developed at the Royal Institute of Technology, Stockholm) The Structure of Materials, S.M. Allen & E.L. Thomas, John Wiley & Sons, Inc. New York, 1999.
10 This functional definition of microstructure includes all lengthscales Microstructure Phases + Defects Vacancies Dislocations Twins Stacking Faults Grain Boundaries Voids Cracks + Residual Stress
11 Microstructure Phases + Defects + Residual Stress Vacancies Dislocations Twins Stacking Faults Grain Boundaries Voids Cracks
12 Microstructure Phases + Defects + Residual Stress Vacancies Dislocations Twins Stacking Faults Grain Boundaries Voids Cracks Defects (Crystalline) Microstructural Vacancies Dislocations Phase Transformation Voids Cracks Component Stress corrosion cracking + Residual Surface Compressive Stress
13 CRYSTAL STRUCTURES
14 Crystal = Lattice (Where to repeat) + Motif (What to repeat) + = Unit cell of BCC lattice Crystal = Space group (how to repeat) + Asymmetric unit (Motif : what to repeat)
15 Progressive lowering of symmetry amongst the 7 crystal systems Increasing symmetry Cubic Hexagonal Tetragonal Trigonal Orthorhombic Monoclinic Triclinic Arrow marks lead from supergroups to subgroups
16 1. Cubic Crystals a = b= c = = = 90º Simple Cubic (P) Body Centred Cubic (I) BCC Face Centred Cubic (F) - FCC [2] Point groups 23, 43m, m3, 432, 4 m 3 2 m Vapor grown NiO crystal Tetrakaidecahedron (Truncated Octahedron) Pyrite Cube [1] [1] Garnet Dodecahedron [1] Fluorite Octahedron [1] [2] L.E. Muir, Interfacial Phenomenon in Metals, Addison-Wesley Publ. co.
17 Crystals and Properties (The symmetry of) Any physical property of a crystal has at least the symmetry of the crystal Crystals are anisotropic with respect to most properties The growth shape of a (well grown) crystal has the internal symmetry of the crystal Polycrystalline materials or aggregates of crystals may have isotropic properties (due to averaging of may randomly oriented grains) The properties of a crystal can be drastically altered in the presence of defects (starting with crystal defects)
18 CLASSIFICATION OF DEFECTS BASED ON DIMENSIONALITY 0D (Point defects) 1D (Line defects) 2D (Surface / Interface) 3D (Volume defects) Vacancy Dislocation Surface Twins Impurity Disclination Interphase boundary Precipitate Frenkel defect Dispiration Grain boundary Faulted region Schottky defect Twin boundary Stacking faults Voids / Cracks Thermal vibration Anti-phase boundaries
19 0D (Point defects)
20 Non-ionic crystals Vacancy Impurity Interstitial Substitutional 0D (Point defects) Ionic crystals Frenkel defect Schottky defect Other ~ Imperfect point-like regions in the crystal about the size of 1-2 atomic diameters
21 Vacancy Missing atom from an atomic site Atoms around the vacancy displaced Tensile stress field produced in the vicinity Tensile Stress Fields
22 Impurity Interstitial Substitutional Relative size Compressive Stress Fields Compressive stress fields SUBSTITUTIONAL IMPURITY Foreign atom replacing the parent atom in the crystal E.g. Cu sitting in the lattice site of FCC-Ni INTERSTITIAL IMPURITY Foreign atom sitting in the void of a crystal E.g. C sitting in the octahedral void in HT FCC-Fe Tensile Stress Fields
23 Interstitial C sitting in the octahedral void in HT FCC-Fe r Octahedral void / r FCC atom = r Fe-FCC = 1.29 Å r Octahedral void = x 1.29 = 0.53 Å r C = 0.71 Å Compressive strains around the C atom Solubility limited to 2 wt% (9.3 at%) Interstitial C sitting in the octahedral void in LT BCC-Fe r Tetrahedral void / r BCC atom = 0.29 r C = 0.71 Å r Fe-BCC = Å r Tetrahedral void = 0.29 x = Å But C sits in smaller octahedral void- displaces fewer atoms Severe compressive strains around the C atom Solubility limited to wt% (0.037 at%)
24 Equilibrium Concentration of Vacancies Formation of a vacancy leads to missing bonds and distortion of the lattice The potential energy (Enthalpy) of the system increases Work required for the formaion of a point defect Enthalpy of formation ( H f ) [kj/mol or ev/defect] Though it costs energy to form a vacancy its formation leads to increase in configurational entropy above zero Kelvin there is an equilibrium number of vacancies G = H T S SConfig kln( ) Crystal Kr Cd Pb Zn Mg Al Ag Cu Ni kj / mol ev / vacancy
25 G (perfect crystal) T (ºC) n/n G (Gibbs free energy) G min Equilibrium concentration H f x x x x 10 3 = 1 ev/vacancy = 0.16 x J/vacancy n (number of vacancies) Certain equilibrium number of vacancies are preferred at T > 0K Vacancies play a role in: Diffusion Climb Electrical conductivity Creep etc.
26 1D (Line defects)
27 The shear modulus of metals is in the range GPa m G 2 The theoretical shear stress will be in the range 3 30 GPa Actual shear stress is MPa I.e. (Shear stress) theoretical > 100 * (Shear stress) experimental!!!! DISLOCATIONS Dislocations weaken the crystal
28 DISLOCATIONS EDGE MIXED SCREW Usually dislocations have a mixed character and Edge and Screw dislocations are the ideal extremes
29 Conservative (Glide) Motion of dislocations On the slip plane Motion of Edge dislocation Non-conservative (Climb) Motion of dislocation to the slip plane For edge dislocation: as b t they define a plane the slip plane Climb involves addition or subtraction of a row of atoms below the half plane +ve climb = climb up removal of a plane of atoms ve climb = climb down addition of a plane of atoms
30 Mixed dislocations b t b Pure screw Pure Edge
31 Role of Dislocations Slip Fracture Fatigue Creep Diffusion (Pipe) Structural Creep mechanisms in crystalline materials Cross-slip Dislocation climb Vacancy diffusion Grain boundary sliding Incoherent Twin Grain boundary (low angle) Semicoherent Interfaces Disc of vacancies ~ edge dislocation
32 2D (Surface / Interface)
33 Grain Boundary The grain boundary region may be distorted with atoms belonging to neither crystal The thickness may be of the order of few atomic diameters The crystal orientation changes abruptly at the grain boundary In an low angle boundary the orientation difference is < 10º In the low angle boundary the distortion is not so drastic as the high-angle boundary can be described as an array of dislocations Grain boundary energy is responsible for grain growth on heating ~ (>0.5T m ) Large grains grow at the expense of smaller ones The average no. of nearest neighbours for an atom in the grain boundary of a close packed crystal is 11
34 Type of boundary Energy (J/m 2 ) Grain boundary between BCC crystals 0.89 Grain boundary between FCC crystals 0.85 Interface between BCC and FCC crystals 0.63 Grain boundaries in SrTiO 3
35 Twin Boundary The atomic arrangement on one side of the twin boundary is related to the other side by a symmetry operation (usually a mirror) Mirror twin boundaries usually occur in pairs such that the orientation difference introduced by one is restored by the other The region between the regions is called the twinned region Annealing twins (formed during recrystallization) Twin [1] Annealing twins in Austenitic Stainless Steel Deformation twins (formed during plastic deformation) [1] Transformations in Metals, Paul G. Shewmon,McGraw-Hill Book Company, New York, 1969.
36 Twin boundary in Fe doped SrTiO 3 bicrystals (artificially prepared) High-resolution micrograph Mirror related variants Twin plane [1] S. Hutt, O. Kienzle, F. Ernst and M. Rühle, Z Metallkd, 92 (2001) 2
37 Grain size and strength y k i d Hall-Petch Relation y Yield stress i Stress to move a dislocation in single crystal k Locking parameter (measure of the relative hardening contribution of grain boundaries) d Grain diameter
38 Defects: Further Enquiry
39 DEFECTS Based on origin Random Structural Vacancies Dislocations Ledges The role played by a random defect is very different from the role played by a structural defect in various phenomenon
40 Low Angle Grain Boundaries b 2 2h
41 ~8º TILT BOUNDARY IN SrTiO 3 POLYCRYSTAL No visible Grain Boundary Å Dislocation structures at the Grain boundary Fourier filtered image
42 DEFECTS Based on position Random Ordered Vacancies Stacking Faults Ordered defects become part of the structure and hence affect the basic symmetry of the structure
43 Crystal with vacancies Vacancy ordering E.g. V 6 C 5, V 8 C 7
44 Effect of Atomic Level Residual Stress Yield Point Phenomenon y (Å) x (Å) (GPa) Interaction of the stress fields of dislocations with Interstitial atoms
45 3D (Volume defects) & MICROSTRUCTURES
46 Bright field TEM micrograph of an Al- 3.3% Cu alloy, aged at room temperature for 100 days, showing the GP-I zones. HAADF micrographs of the GP zones: (a) Intercalated monatomic Cu layers several nm in width are clearly resolved, (b) a GP-zone two Cu layers thick can chemically be identified. T.J. Konno, K. Hiraga and M. Kawasaki, Scripta mater. 44 (2001)
47 b Precipitate particle b Hardening effect Increase in surface area due to particle shearing Part of the dislocation line segment (inside the precipitate) could face a higher PN stress
48 Pinning effect of the precipitate Can act like a Frank-Reed source ~ Gb 2r
49 Controlling microstructures: Examples
50 Fe-Cementite diagram Eutectic L + Fe 3 C Peritectic L ºC L + L Fe 3 C ºC Eutectoid + Fe 3 C T + Fe 3 C Austenite ( ) FCC 723ºC Ferrite ( ) BCC Cementite (Fe 3 C) Orthorhombic [1] Fe Fe 3 C 6.7 %C [1] rruff.geo.arizona.edu/doclib/zk/vol74/zk74_534.pdf
51 Time- Temperature-Transformation (TTT) Curves Isothermal Transformation Eutectoid steel (0.8%C) Eutectoid temperature Austenite Pearlite Coarse Fine 500 Pearlite + Bainite Metals Handbook, Vol.8, 8 th edition, ASM, Metals Park, Ohio T 400 [2] Bainite M s Austenite 348 C [1] 100 M f Martensite t (s) [2] Introduction to Physical Metallurgy, S.H. Avner, McGraw-Hill Book Company, 1974 [2] 278 C [1] Physical Metallurgy for Engineers, D S Clark and W R Varney, Affiliated EastWest Press Pvt. Ltd., New Delhi, 1962 [1]
52 Time- Temperature-Transformation (TTT) Curves Isothermal Transformation Eutectoid temperature Austenite + Fe 3 C Eutectoid steel (0.8%C) Pearlite Pearlite + Bainite T Bainite M s M f Martensite t (s)
53 Different cooling treatments Eutectoid steel (0.8%C) M = Martensite 600 P = Pearlite 500 T 400 Water quench Normalizing Full anneal Oil quench M M + P Fine P Coarse P t (s)
54 Hardness (R c ) % Carbon Harness of Martensite as a function of Carbon content Properties of 0.8% C steel Constituent Hardness (R c ) Tensile strength (MN / m 2 ) Coarse pearlite Fine pearlite Bainite Martensite 65 - Martensite tempered at 250 o C
55 Cooling C 1 C 2 C 3 + Fe 3 C + + Fe 3 C T Fe 0.02 %C Eutectoid + Fe 3 C 0.8 Pro-eutectoid Cementite Pearlite 1.4%C [1] [1] Materials Science and Engineering, W.D.Callister, Wiley India (P) Ltd., 2007.
56 3.4%C, 0.7% Si, 0.6% Mn White CI 0% Heat Treatment Fe3C 2.5% C, 1.0% Si, 0.55% Mn Graphite Nodules Malleable CI 12% Ferrite (White) Grey CI 0.5% Change Composition 3.4% C,1.8% Si, 0.5% Mn Nodular CI Graphite (black) 10 m Fully Malleabilized Ductile 18% 3.4% C, 0.1% P, 0.4% Mn,1.0% Ni, 0.06% Mg Graphite nodules L ( Fe3C) FeC 3 ( FeC 3 ) Ledeburite Pearlite 10 m Ferritic Matrix Ferrite
57 Anisotropy in Material Properties: an example Texture can reintroduce anisotropy in material properties Cubic Crystal (3 Elastic Moduli) Texture Polycrystal Rolling/ Anisotropic Isotropic Extrusion Anisotropic E 12 E 11 1 E 44 2 E11 E12 Moly Permalloy: 4% Mo, 79% Ni, 17% Fe Cold Worked Elongated [1] Textured samples Equiaxed Annealed [1] [1] Metals Handbook, Vol.8, 8 th Edition, ASM, 1973
58 CONCLUSION To understand the properties of materials the structure at many different lengthscales must be viewed
59
60 Ionic Crystals Overall electrical neutrality has to be maintained Frenkel defect Cation (being smaller get displaced to interstitial voids E.g. AgI, CaF 2
61 Schottky defect Pair of anion and cation vacancies E.g. Alkali halides
62 Other defects due to charge balance If Cd 2+ replaces Na + one cation vacancy is created Defects due to off stiochiometry ZnO heated in Zn vapour Zn y O (y >1) The excess cations occupy interstitial voids The electrons (2e ) released stay associated to the interstitial cation
63 FeO heated in oxygen atmosphere Fe x O (x <1) Vacant cation sites are present Charge is compensated by conversion of ferrous to ferric ion: Fe 2+ Fe 3+ + e For every vacancy (of Fe cation) two ferrous ions are converted to ferric ions provides the 2 electrons required by excess oxygen
64 Progressive lowering of symmetry amongst the 7 crystal systems Increasing symmetry Cubic 48 Hexagonal 24 Tetragonal 16 Trigonal 12 Orthorhombic 8 Monoclinic 4 Triclinic 2 Arrow marks lead from supergroups to subgroups Superscript to the crystal system is the order of the lattice point group
65 A semimetal is a material with a small overlap in the energy of the conduction band and valence bands. However, the bottom of the conduction band is typically situated in a different part of momentum space (at a different k- vector) than the top of the valence band. One could say that a semimetal is a semiconductor with a negative indirect bandgap, although they are seldom described in those terms. Schematically, the figure shows A) a semiconductor with a direct gap (like e.g. CuInSe 2 ), B) a semiconductor with an indirect gap (like Si) and C) a semimetal (like Sn or graphite). The figure is schematic, showing only the lowest-energy conduction band and the highest-energy valence band in one dimension of momentum space (or k-space). In typical solids, k-space is three dimensional, and there are an infinite number of bands. Unlike a regular metal, semimetals have charge carriers of both types (holes and electrons), so that one could also argue that they should be called 'double-metals' rather than semimetals. However, the charge carriers typically occur in much smaller numbers than in a real metal. In this respect they resemble degenerate semiconductors more closely. This explains why the electrical properties of semimetals are partway between those of metals and semiconductors. As semimetals have fewer charge carriers than metals, they typically have lower electrical and thermal conductivities. They also have small effective masses for both holes and electrons because the overlap in energy is usually the result of the fact that both energy bands are broad. In addition they typically show high diamagnetic susceptibilities and high lattice dielectric constants. The classic semimetallic elements are arsenic, antimony, and bismuth. These are also considered metalloids but the concepts are not synonymous. Semimetals, in contrast to metalloids, can also be compounds, such as HgTe, and tin and graphite are typically not considered metalloids. Graphite and hexagonal boronnitride (BN) are an interesting comparison. The materials have essentially the same layered structure and are isoelectronic, which means that their band structure should be rather similar. However, BN is a white semiconductor and graphite a black semimetal, because the relative position of the bands in the energy direction is somewhat different. In one case the bandgap is positive (like case B in the figure), explaining why BN is a semiconductor. In the other case the conduction band lies sufficiently lower to overlap with the valence band in energy, rendering the value for the bandgap negative (see C).
66
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