Processing of Aerospace

Materials I (ME772)
Lecture 6
Solid solution strengthening, grain boundary
strengthening
Softening
21 Jan 2022
Amol A. Gokhale, Professor, Mechanical Engineering A P Mouritz, Chapter 4.4
Room S05 ME Department, extension 7399 F C Campbell, Appendix B.2
gokhale@iitb.ac.in W D Callister 7.6, 7.8, 7.9, 7.11, 7.12, 7.13
(the best illustrations)
 Solid solution strengthening (alloying)
• In solid solutions, solute atoms create strain fields due to size difference between
parent (solvent) and alloying element (solute) atoms
• Larger substitutionals and all interstitials create compressive strain in the lattice,
while small substitutionals create tensile strain
• Dislocations may be repelled or attracted by solute atoms depending on whether
the solute atoms are in the compressive or tensile strain side of the dislocations
• Interaction between lattice strain and dislocation strain impedes dislocation slip,
requiring greater shear stress for slip to continue
• CRSS = G.b.c. 3/2; c= solute concentration;  = lattice strain

Larger substitutional … and segregate to

elements create tensile strain side of
compressive strain dislocations
Cu
Grain boundary (g.b.) strengthening
• Each grain is a crystal, whose orientation differs in adjoining grains. Grain
boundary is where two/three crystals meet. Grain boundary has energy per
unit area associated with it (due to incomplete bonds)
• Slip in polycrystalline metal occurs via the following steps:
• It starts with dislocation slip within the grain
• Slip is resisted by the grain boundary because of change in crystal
orientation and also because of loss of crystallinity at the g.b.
• Dislocations pile up at the grain boundary. If the applied stress exceeds
a critical level, it triggers crossover of slip (or initiates slip freshly in the
adjoining grains)
• If the grain size is small, more grain boundaries need to be crossed,
increasing the stress requirement for slip, causing strengthening
Grain boundary strengthening relationship

Hall-Petch relation
/

Y.S., d = grain dia

K is material constant (slope)
Steel = friction stress/ lattice resistance (intercept)

• This is an empirical relation, works well from 1 µm and 1 mm

• Rapid solidification, grain refiner additions and special thermomechanical processing can
reduce grain size
• Lower limit on grain size (for above relation to be valid) is decided by length of dislocations
(submicroscopic grain size)
 Summary strain hardening, solid solution
strengthening and grain boundary strengthening
Slip lines on the surface of
polycrystalline copper that
was polished and deformed.

• If the dislocation at point A moves to the left, it is blocked by the point defect.
• If the dislocation moves to the right, it interacts with the disturbed lattice near the
second dislocation at point B.
• If the dislocation moves farther to the right, it is blocked by a grain boundary.
 Processing of metallic materials

Alloy
‘Continuous casting’ to
produce standard geometries
Rolling to produce semi-finished (worked or
‘wrought’) products
All mechanical properties improve after the continuously cast forms are ‘rolled’
and ‘heat treated’. Rolling is an important ‘metal working’ process which
introduces heavy amount of plastic deformation. Instead of rolling, the cast forms
can be forged or extruded (terms to be introduced later).
If metals are ‘worked’ at high temperatures
• Internal residual stresses, which are elastic, may develop in
metal work pieces due to:
―Non-uniform cooling after fabrication at an elevated temperature
(casting, welding, hot rolling)
―Phase transformation that is induced upon cooling in which parent
and product phases have different densities
• Machining and grinding may also introduce residual stresses
• Distortion and warpage may result if these residual stresses
are not removed.
If metals are ‘cold’ worked at room- or low temperature

Pancaking / flattening of grains Increase in s (from 106 to 1012 lines per cm2),
Thus, the overall crystal energy increases ‘twins’ (another mode of plastic deformation in
due to increase in strain energy and grain non-fcc metals) and shear bands. This increases
boundary energy. strength and reduces ductility.
 Restoration of microstructure (‘coming back’) to
the pre-worked (‘ground’) state
• Cold working cannot impart large strains required in processing
unless the microstructural changes are reversed in between.
• However, it cannot happen at room temperature, and thermal energy
is needed for atoms for restorative processes to operate.
• Higher the cold work, higher is the driving force for restoration and
faster is the kinetics of restoration.
• Such restoration of the microstructure occurs in four stages at
elevated temperatures:
⁻ Elastic stress relief Typical annealing thermal cycle
⁻ Recovery
holding in furnace
⁻ Recrystallisation
slow
⁻ May be followed by grain growth. Heating cooling

Annealing is generic term to describe heat

treatment done for any or more of the
above processes to occur.
 Recovery (RV)
High strain energy • At high temperature, s of opposite sign
annihilate each other, hence there is small
reduction in  density
• s rearrange in certain fashion to reduce overall
energy. Low angle boundaries are formed dividing
the grain into sub-grains
• Yield strength reduces and ductility increases by a
small %
• Definition: Recovery refers to that part of
annealing which does not involve the migration
Low angle boundaries
of high-angle grain boundaries. Hence the grain
Low strain energy structure does not change during recovery.
• It occurs at
a. high temperatures after cold working,
(static RV) or
b. during hot working (dynamic RV)

High angle grain boundaries

Low angle grain boundaries

(sub-grain boundaries)
 Recrystallisation (RX) and Grain Growth (GG)
• Definition: "... the formation of a new grain structure in a deformed material by the formation
and migration of high angle grain boundaries driven by the stored energy of deformation.
[Doherty 1997]
• These new grains are strain free (substantially lower  density), thus they reduce strain energy
of the grains.
• RX occurs at high temperature exposures after cold working (static RX). In many metals, it can
occur during hot working also (Dynamic RX). It reduces strength.
• The new grains form as very small nuclei and grow until they completely consume the parent
material. Grain growth (which reduces grain boundary area) may be followed.
• They involves short-range atomic diffusion
(g.b.: grain boundary)
• RX reduces strength
since  density reduces
substantially
• Grain growth reduces
strength because grain
boundary area reduces
Grains with large New  -free (104-5 The entire Grain growth
 density, low lines per cm2) microstructure is (actually
angle g.b.’s grains nucleate occupied by new ‘coarsening’)
(preferably at g.b.’s  -free grains
RX kinetics (time to 100% RX) depends on
• alloy composition: pure metals recrystallise at lower temperatures than alloys (see
later),
• annealing temperature: higher the temperature, higher is the diffusion rate and
shorter the time it takes to complete RX. RX temperature is roughly = 0.4 (m.p. of
metals, TM)
• level of work hardening: higher the % cold work (work hardening), lower is the RX
temp.
• Smaller initial grain size accelerates RX, i.e. it reduces RX temperature. This happens
because grain boundaries are preferred nucleation sites for new grains to form

Since RX is a diffusion-controlled Temperature at which the Tensile Strength drops

process, the RX temperature is roughly sharply defines the RX temperature for given
proportional to 0.4TM (TM in kelvin). duration
Effect of RV, RX and GG on grain size and
properties
 Vacancy- dependent atomic diffusion
(sometimes called “vacancy diffusion”)
• Diffusion is the phenomenon of
species transport by atomic
motion (there can be ionic
diffusion in some other solids)
• The process by which atoms of
one metal diffuse into another is
termed inter-diffusion
• Diffusion also occurs for pure
metals, but all atoms exchanging
positions are of the same type;
this is termed self-diffusion.

Self diffusion
Inter-diffusion
 Vacancy-dependent atomic diffusion (contd)

Vacancy diffusion: There must be

an empty adjacent site, as in self
diffusion and inter diffusion

Vacancy-independent
atomic diffusion
Interstitial diffusion: diffusion of
small atoms like H, C, N and O
does not depend on vacancies. It
is faster than vacancy diffusion.
 ‘Activation energy’ for diffusion
Original state (stable) Final state (stable)

Vacancy
diffusion
Intermediate state
(Unstable)

―Atoms must have sufficient energy

(‘activation energy’) to break bonds with
neighbour atoms and cause lattice
distortion during the displacement
Interstitial ―Diffusion is insignificant at low
diffusion
temperatures because of lack of sufficient
energy in atoms to overcome the
‘activation energy’ barrier.

•High temperature provides sufficient energy for atoms to ‘cross over’ the
activation energy barrier.
• The fraction of total number of atoms capable of diffusive motion increases with
temperature
Fick’s first law of diffusion

• One dimensional steady state diffusion:

• J = flux, kg/(m2.s)
• D = diffusion coefficient, m2/s
• = concentration gradient along x direction

Steady -state
diffusion
no net accumulation
of diffusing species
in the plate
 Fick’s second law of diffusion
• Nonsteady-state diffusion
• The diffusion flux and the concentration gradient at a given location
in a solid vary with time, with a net accumulation or depletion of the
diffusing species Solution to concentration profile

1) C = C0 for all 𝑥, at t = t0 and for 𝑥 ∞

2) at t = t0 C𝑥 = 0 𝑖𝑠 𝑟𝑎𝑖𝑠𝑒𝑑 𝑡𝑜 CS and remains at
CS, for all 𝑡
Tracking penetration of iso-concentration surface
Cs C1 into the interior

Second law
Cx

C1 This concept will be used later when we discuss

‘homogenisation’ of alloys after casting.
C0
Also, many coating processes rely on diffusion.
 Factors affecting diffusion
 Species
• The diffusing species and the host material influence the diffusion
coefficient D, which is a measure of diffusion rate
• For example, C atoms diffuse much faster (D = 1.4 x 10-12 m2/s) in bcc
iron than self diffusion of Fe (D = 3.0 x 10-21 m2/s) (inters. vs subs)
 Temperature
• D (Fe in Fe) increases from 3.0 x 10-21 to 1.8 x 10-15 m2/s by raising
temperature from 500 C to 900 C

D0 = a temperature-independent pre-exponential (m2/s)

Qd = the activation energy for diffusion (J/mol)
R = the gas constant, 8.31 J/molK
T = absolute temperature (K)
Substitutional elements added to Ni in turbine blades for
strengthening have very low diffusion coefficients to
minimise diffusion and related deformation.
 Hot working (= thermo-mechanical working)
• Hence annealing can partly or completely revert the effects of
strain hardening; i.e. it reverts the increase in strength and
reduction in ductility which accompanies cold working)
• Mechanical working and annealing can be combined by doing
mechanical working at high temperature to facilitate large
amounts of strains to be imparted for shape change and cause
structural restoration (reversion to pre-deformation stage) and
refinement (since RX reduces grain size)
Assignment 6
1. Describe in your own words, the principles behind strengthening
by grain size reduction, elemental addition (alloying), and strain
hardening. Explain how dislocations are involved in each of the
strengthening techniques.
2. From the plot of yield strength versus (grain diameter)1/2 for a 70
Cu–30 Zn cartridge brass in figure, determine values for the
constants 0 and ky in the Hall-Petch relation.
Now predict the yield strength of this alloy when the average grain
diameter is 2 x 10-3 mm.
 Assignment 8 (there was no assignment 7)
3. Carbon is allowed to diffuse through a steel plate 10-mm thick. The concentrations
of carbon in Fe at the two faces are 0.85 and 0.40 kg/cm3, which are maintained
constant. If the pre-exponential and activation energy are 5.0 * 10-7 m2/s and 77,000
J/mol, respectively, compute the temperature at which the diffusion flux is 6.3 x 10-10
kg/m2. s.

4. Describe the changes that occur during recovery (RV), recrystallisation (RX) and
grain growth (GG) with respect to dislocation density, grain size and yield strength
compared to the cold worked stage (for RV) or the preceding stage (for RX and GG).
You may answer in a tabular form given below:
Structure/property Cold worked After recovery After After grain growth
condition recrystallisation

Dislocation density High

Grain size / shape Large and flat

Yield strength High

Definitions
• Recovery (RV): A high temperature treatment during which
dislocations assume low-energy configurations and dislocation
density reduces though not significantly. Some material properties
revert back to their pre-cold-worked values..
• Recrystallization (RX): A medium-temperature annealing heat
treatment designed to eliminate all of the effects of the strain
hardening produced during cold working.
• Recrystallization (RX) temperature: A temperature above which essentially
dislocation-free new grains emerge from the cold worked material.
• Grain growth (GG): is the increase in average grain size of
polycrystalline materials, which proceeds by grain boundary motion.
There is concomitant reduction in number of grains

CW RV RX GG