Metal processing research overview

Metal Processing with Lap
MSE 4202
Introduction
Filimon Hadish, Ph.D.
Assistant Professor of Materials Science and Engineering
Adama Science and Technology (ASTU)
Email: filimon.hadish@astu.edu.et
hadfili2005@gmail.com
Phone: +251 900740162
1

Anterenga
Buda
• https://johangerrits.com/travel/ethiopia/north_ethiopia/143_-_A_blacksmith_in_Harar_-
_Ethiopia/
• https://www.mediastorehouse.com.au/worldinprint/africa/ethiopia-abyssinia-ethiopia-
heritage-sites-aksum/portrait-blacksmith-work-town-axoum-axum-1150420.html
• https://www.superstock.com/asset/metal-objects-blacksmith-workshop-axoum-axum-tigre-
region-ethiopia-africa/1890-44473
• https://www.mediastorehouse.co.uk/fine-art-finder/artists/luca-giordano/blacksmiths-shop-
1885-oil-canvas-28649531.html
• https://www.npr.org/2021/06/29/1011043968/united-airlines-is-buying-270-new-planes-in-
massive-bet-on-future-of-travel
• https://newsghana.com.gh/zambia-starts-impounding-dubiously-imported-heavy-
duty-vehicles
• https://www.nswrailmuseum.com.au/
• https://www.usamm.com/blogs/news/u-s-navy-ship-classes-a-close-
look-at-classifications
2

Luke Shaw
https://www.sportzcraazy.com/worst-football-injuries/ 3

Luke Shaw
https://www.sportzcraazy.com/worst-football-injuries/ 4

https://www.drfragomen.com/knock-knees 5

https://www.drfragomen.com/knock-knees 6

A. Photograph shows two sizes of the
eight-Plate Guided Growth System:
12 and 16 mm. The eight-Plate kit
includes three sizes of cannulated
screws (16, 24, and 32 mm).
B. Photograph shows the complete
eight-Plate set (clockwise from top):
a 3.2-mm cannulated drill bit, a 21-
gauge needle, two 1.5-mm wires with
1.2-mm threaded tips, a screwdriver,
four eight-Plates, ten cannulated
screws, and a drill-guide. New
instrumentation kits include a 3.2-
mm cannulated step drill and a guide
to limit penetration to 5 mm.
C. Guide wires, 21-gauge needle,
cannulated screws, and an eight-
Plate. The cannulated screws are
inserted over the guide wires. The
21-gauge needle provides temporary
fixation.
D. Photograph shows that the screws
are able to pivot within the eight-
Plate (greater than 45 of rotation is
possible)
Rolf D. Burghardt et.al., J Child Orthop (2008) 2:187–197
7

Stainless steel small fragment screws and Orthopedic plate
https://www.shutterstock.com/image-
photo/surgical-plates-osteosynthesis-case-
bone-fractures-2086757179
https://naileditortho.com/heres-what-med-
students-should-know-about-orthopedic-
plates-and-screws-part-1/
https://www.dreamstime.com/orthopaedic-plate-
screw-image225183093
8

• 316L stainless steel
• cobalt base alloys
• Bioceramics
• titanium alloys
• pure titanium
• composite materials and
• polymers (non-resorbable and bioresorbable).
Property
Bioinert
 Wear
 corrosion and
 heat resistances
The biocompatible materials used for bone plates are:
9

https://www.xometry.com/resources/materials/alloy-steel-
vs-stainless-steel/
Binary Alloys
Mg-9Gd-4Y-2Zn-0.5Zr(wt.%) alloy aged
Galvanically Induced Intergranular
Corrosion of AA5083-H131
10

Matsumoto, K. et.al.; Nat. Commun v(2022).
Inter-element miscibility driven stabilization of ordered pseudo-binary
alloy Z3-FePd3
• Multi component phases
• thermodynamically-stable phases?
F. Cao, B. Xiao, Z. Wang et al. Journal of Magnesium and Alloys
(2021)
Journal of Magnesium and Alloys
zinc-water
system and
magnesium-
water
system
at 25 oC
Corrosion behavior
of Mg64Zn36 in
3.5 wt.% NaCl
11

Advanced Aluminum Armor Alloys 5083-H131
https://www.lightmetalage.com/news/industr
y-news/flat-rolled-sheet/article-advanced-
aluminum-armor-
alloys/#:~:text=Based%20on%20their%20balli
stic%20characteristics,preferred%20alloys%20
for%20armored%20vehicles.
12

Eutectic compound Mg21Zn25 + Mg51Zn20.
Mg–12 wt.%Zn binary alloy
13

https://www.neetprep.com/section/chapter/650?sectionId=325
Thermodynamic
First law of thermodynamics
• Heat (Q);
• Internal energy (U)
• Exact and inexact differentials
• Enthalpy (H)
• Joule-Thompson expansion
• Heat Capacities (Cp)
14

First law of thermodynamics
• Internal energy (U)
• Heat (Q)
• Enthalpy (H): heat content of the system
 –ve, the system losses its heat content to the surrounding
 +ve, system absorbs heat from surrounding
• Exact and inexact differentials
∆ +ve
∆ -ve
∆ +ve
∆ -ve
Exact differential
• State functions
• path independent
• Eg. U, p, V, H
Inexact differential
• Not state functions
• path dependent
• Eg. W, Q
15

• Joule-Thompson expansion
• Intensive and Extensive properties
https://www.mechanicalbooster.com/2016/04/difference-between-
intensive-and-extensive-properties.html#google_vignette
It is a useful relation for relating the heat capacities at constant pressure
and volume and for the liquefaction
of gases
Where is the Joule-Thompson
coefficient and is defined as
Cooling by isenthalpic
expansion is now
called the Joule- Thomson
effect.
16

Heat capacities (solid and liquid)
Subsequently, the enthalpy H and the entropy S can be obtained as:
• Heat Capacities (Cp)
https://thesis.library.caltech.edu/2237/3/chapter_2.pdf
Second Law of Thermodynamics. Entropy
• Heat always is transferred
spontaneously from a warmer to a
colder body ( )
• The revers process is possible only if
work or energy is supplied
• i.e.
Spontaneous
Non-Spontaneous
17

Carnot cycle
• A theoretical description of a machine that represents the process of
heat transfer into mechanical work.
• Four steps of figurative representations are
 Isothermal expansion (at )
 Adiabatic Expansion (from )
 Isothermal Compression (at )
 Adiabatic Compression (back from )
From the general relation of
The efficiency ( )of a Carnot cycle is
18

Entropy (S): measure of the disturbance of a system.
• thermodynamically defined as
A general useful relation for the validation of a process of system is
• If a process is reversible the entropy change is zero.( )
• The entropy increases in all irreversible processes.( )
Entropy of mixtures
Entropy Change at Mixing Two Liquids or Solids (molar entropy of mixing)
Entropy and probability (statistical thermodynamic expression)
Entropy Change during Solidification
19

Gibbs’ Free Energy (G)
For the change of a system at constant temperature
Thermodynamics of Single-Component Systems
• A single-component system may consist of only one phase, f(eg. a solid, a
liquid or a gas) depending on the temperature.
• Even phase transformation occurs, only single-component systems (pure
metals only is considered).
Clausius–Clapeyron’s Law
Taking into consideration 1st and 2nd laws of TDs, we get
For an arbitrary phase equilibrium condition
Clausius--Clapeyron’s law
20

 An ancient Chinese medicine-based approach (2,500 years)
 Stimulate nerve-rich areas of the skin surface in order to influence
tissues, gland, organs, and various functions of the body.
Acupuncture
•allergies
•anxiety and depression
•osteoarthritis
•chronic pain, often in the neck, back, knees,
and head
•hypertension
•insomnia
•menstrual cramps and PMS
•migraines
•morning sickness
•sprains
•Strokes
https://www.healthline.com/health/acupuncture-how-does-it-work-scientifically#what-are-the-benefits
21

(a) AN (b) AuNPs/AN and (c)rGO/AuNPs/AN
(a) PMB/P[Bvim]Br/rGO/AuNPs/AN
(b) P[Bvim]Br/PMB/P[Bvim]Br/rGO/AuN
Ps/AN
(c) MI/PMB/P[Bvim]Br/rGO/AuNPs/AN
(c) and MI/PMB/P
[Bvim]Br/rGO/AuNPs/AN + SARS-
CoV-2-S protein
23

Nucleation and
Crystal Growth in Vapour
MSE 4202
Phone: +251 900740162
24

The formation of crystals (influenced by the number of crystals growing in the
melt).
Nucleation
intermediate phases
Pure Metals
Homogeneous nucleation (HN):
very high supersaturation is needed before any crystals form
Supersaturation
• Clusters
• Nucleation rate
• Nuclei (Critical size)
• Embryos (Sub-critical size)
Theory of Homogeneous Nucleation of Solid
Crystals from Liquids
• Nucleation Rate
• HN as a Function of Undercooling. Nucleation Temperature
• HN as a Function of Concentration in Binary Alloys
• Influence of Variable Surface Energy on HN
• HN of Non-Spherical Embryos. Nucleation of Faceted Crystals
25

Schematics of nucleation mechanisms 26

Secondary Nucleation:
• The presence of the crystal
seed of parent solution acts
as catalysts for the formation
of nuclei.
• Reduced
27

Secondary Nucleation:
• The presence of the crystal seed of parent solution acts as catalysts for the
formation of nuclei.
• Reduced the required energy for nucleation less super-saturation will be
necessary.
• Van der Waals force of the seed crystals in a supersaturated solution
attracts the
solute clusters or embryos.
• By increasing these embryos in the near crystals rapid coagulation occurs, so
the creation of nuclei bigger than critical size happens.
• The crystal seed of parent solution operates as the origin of nuclei, either by
micro-attrition because of the fluid shear or needle breeding.
• Since the impact force brings a bigger disturbance to the adsorbed layer and
transfers a greater number of nuclei to the bulk.
• contact is more effective in the creation of secondary nucleation relative to
bulk fluid shear. 28

• if r< the system can lower its free
energy by dissolution of the solid
• Unstable solid particles with r<r* are
known as clusters or embryos
• if r> the free energy of the system
decreases if the solid grows
• Stable solid particles with r> are
referred to as nuclei
• Since ∆G = 0 when r = r* the critical
nuclei is effectively in (unstable)
equilibrium with the surrounding liquid
Cluster and Nuclei
29

• At optimal concentrations: surface reduction of Ag ions occurs on the
surface of formed AgNPs owing to the reduction potential of the citrate
adsorbed onto the surface.
• At low concentrations, coalescence of smaller silver NP clusters occurs.
Experiment on seed solution of AgNPs and adding further Ag precursor
and reducing electrons to check how the seed particles affected.
32

• Many different crystal morphologies (shape and structure) can be observed
during crystal growth from a vapour phase.
• Experiments show that the morphology is strongly related to the growth
conditions, i.e. the supersaturation of thewater vapour as well as the growth
temperature. This is a general observation, valid for all sorts of crystals.
• Eg. Thin film Crystals growth models
Crystal Morphologies
Frank Vander
Stansky Chrstanove
Volmer
34

Prachi Sharma et.al. Journal of Materials Science: Materials
in Electronics volume 28, pages3891–3896 (2017)
https://www.sciencedirect.com/topics/chemic
al-engineering/vacuum-deposition
35

1. Chemical transport methods
2. Vapor decomposition methods
3. Vapor synthesis methods
Chemical Vapor deposition
CVD is a chemical process to produce high quality solid materials. The precursor
gases are delivered into the reaction chamber at approximately ambient
temperature. As they pass over or come into contact with heated substrate,
they react and decompose to form a solid phase which are deposited onto
substrate.
36

Lindberg Blue M Mini-Mite-Roll to roll (R2R) CVD
Chemical vapor deposition (CVD)
Polsen et.al. (2015) 37

Gases cylinder
Flow meter
controller
Concentric Tube/Quartz tube
Pump
Oven
Oven
Sample holder
Gas out
CVD Instrumentation
www.kejiafurnace.com
Ethylene,
Methane,
Hydrogen, and
Ar
Zhengzhou Kejiafurnace Co., LTD
38

https://www.mks.com/n/cvd-physics
Substrates: metals, alloys, and
pure elements:
Eg; Cu and Ni
https://is.muni.cz/el/sci/podzim2007/C7780/um/L24_CVD.pdf
39

• Oxygen
• Halides: H2SiCl2, HSiCl3, TiCl4, WF6, etc.
• Hydrides: SiH4, GeH4, AlH3(NMe3)2, NH3, etc.
• Organometallics: AlMe3, Ti(CH2tBu)4, etc.
• Metal Alkoxides: TEOS, Tetrakis Dimethylamino Titanium (TDMAT),
Ti(OiPr)4, etc.
• Metal Dialkylamides: Ti(NMe2)4, etc.
• Metal Diketonates: Cu(acac)2
• Metal Carbonyls: Ni(CO)4
https://www.mks.com/n/cvd-physics
Typical precursors for CVD processes include:
40

• Horizontal chemical vapour deposition (CVD) and vertical CVD
• Low-pressure CVD and atmospheric pressure CVD
• Hot-wall CVD and cold-wall CVD
• Plasma-enhanced CVD, photo-assisted CVD and laser-assisted CVD
• Metal–organic CVD (MOCVD)
• Hot filament/wire CVD
• Initiated CVD
• Oxidative CVD
• Atomic layer deposition and molecular layer deposition
CVD categories and variants
https://www.nature.com/articles/s43586-020-00005-y 41

Natural diamond
• Diamond stability field
• P & T are just right for
diamonds to form
43
https://sciencequery.com/structure-of-diamond/
Artificial Diamond
 CVD
 2 weeks
 Hydrocarbon gases
120 - 200 km
https://gemscience.net/geological-origin-of-natural-diamonds/
https://www.jewellerybusiness.com/features/synthetic-
gemstones-where-knowledge-is-power/
Diamond

Faceted and Dendrite
MSE 4202
Phone: +251 900740162
44

Gallium antimonide (GaSb):
• high thermal conductivity and low latent heat and vapor pressure
• zinc-blende single-crystal structure used
 mid-infrared-emitting diodes and
 thermophotovoltaic cells
Crystal–melt interfaces during the directional solidification of molten GaSb
• stoichiometric composition, and
• the formation of dendrite structures 45

Crystal–melt interfaces formed during the directional solidification of GaSb
were observed using system consisting
• A furnace (suited with a thermocouples) and
• A digital microscope with a zoom lens having a long working distance
• Because GaSb
o has the high thermal conductivity
o low latent heat
o vapor pressure
• The growth of crystals with a low dislocation density is not very difficult.
• During the single-crystal growth of GaSb is the formation of twin
boundaries is important.
• The formation of twin boundaries gives rise to
 Polycrystallization
 Dendrite growth.
46

GaSb crystal–melt interface
• Dendrite growth was initiated as the planar crystal–melt interface became
unstable with increases in growth velocity
• Dendrites having {111} facets were found to grow in either the 110 or 112
directions
• A pair of twin boundaries was identified at the center of a dendrite.
• Thus, the growth of dendrites in GaSb is associated with nucleation at twin-
related reentrant corners.
47

Electron backscatter diffraction (EBSD) used to determine GaSb dendrites
crystallographic orientations
48

Color coded inverse pole figures (IPFs) for a plane cut perpendicular to the
112 growth direction
• Here, A1 and A2 are the axes parallel to the growth direction and the
normal direction of the top surface of the dendrite, respectively.
• Two {111} twin planes parallel to the top surface of the dendrite and
• The existence of two twin boundaries in the dendrite provides evidence
• The dendrite growth in GaSb is associated with reentrant corners.
49

Molar Gibbs’ Free Energy of a Pure Metal
Metals and alloys also have crystalline structures (Scanning electron microscope)
Faceted crystals and faceted growth Dendrite crystals and dendritic
growth
Two crystal structures
• The shape is determined by the
growth of the surfaces
• The driving force of a faceted
crystal
o the surface tension
o the growth rate (the kinetics)
o the mass transport
time
• Most metals solidify by a primary
precipitation of dendrites.
Geometric structures
• Grooves (reentrant corners)
• Ridges
steel
ingots
50

Dendrite propagation in silicon based on reentrant corners at twin boundaries
K. Shiga et al. / Scripta Materialia 168 (2019) 56–60
• The equilibrium form bounded by {111} facet planes contains two twin boundaries
(Figure (a)).
• Two morphologies can be present at a crystal–melt interface associated with a twin
boundary:
o A reentrant corner with an external angle of 141° and
o A ridge structure with an external angle of 219°.
51

Thomas A. Griffiths, Journal of Petrology, 2023, Vol. 64, No. 1
• (a) Typical microstructure of high
aspect ratio dendritic domains,
• (b) Transition from faceted to high
aspect ratio dendritic morphology (right
to left)
52

• IPF color-coded EBSD maps of the orientation of branching Cpx indicates for
each pixel the crystal direction that is parallel to a fixed reference direction
in sample coordinates,
• According to the IPF color key the reference direction for
• (a) is the sample Z direction and for (b) the sample Y direction
Thomas A. Griffiths, Journal of Petrology, 2023, Vol. 64, No. 1 53

Dynamics at crystal/melt interface
during solidification of multi-
crystalline silicon
High Temperature Materials and Processes 2022; 41: 31–47
Kozo Fujiwara*, Lu-Chung Chuang, and Kensaku Maeda
Institute for Materials Research, Tohoku University,
Sendai, 980-8577, Japan,
54

(a) conventional directional solidification method,
(b) dendritic casting method, where dendrite growth is promoted along the
bottom wall of the crucible to create a grain structure with large grains,
(c) mono casting method, where a single crystal is preset on the bottom wall of
the crucible to grow a single crystal ingot in the crucible, and
(d) HP mc-Si growth, where tiny beads are preset on the bottom wall of the
crucible to enhance nucleation to obtain a grain structure with small grains.
Directional solidification processes in various methods for producing mc-Si
ingots for solar cells:
Kozo Fujiwara et al. https://doi.org/10.1515/htmp-2022-0020
55

(a) the case of a rough plane. The flat interface is transformed to a zigzag
interface with increasing growth rate due to the interface instability and
(b) the case of a smooth plane (facet plane). The flat interface is maintained
even at a higher growth rate.
Transformation of microscopic interface shape for atomically rough and
smooth planes
56

actual images of the interface at the point of interface instability for a Si
single crystal.
Process of interface instability:
57

Eutectic and Peritectic Solidification
MSE 4202
Phone: +251 900740162
58

T3
Temp
(
o
C)
Time (sec)
Cooling Curve
T1
T2
d e m o d e m o d e m o d e m o
Liquid
ES of a liquid: a simultaneous precipitation of two or more phases via a
eutectic reaction
Eutectic solidification (ES)
Liquid
• = pure liquid of phase (brick red)
• = between liquid and solid of phase
(light blue)
• = composition below solid of phase
(yellow line) all down to
solidification process
Solidification process before Solid
Solubility Limit (Single Phase Alloy)
https://www.southampton.ac.uk/~pasr1/eutectic.htm
59

T3
Temp
(
o
C)
Time (sec)
Cooling Curve
T1
T2
Liquid
eutectic reaction
Liquid
Solidification Beyond Solid
Solubility Limit (Joule Phase Alloy)
phase precipitates
𝜷
𝜶
60

Liquid
eutectic reaction
Liquid
Solidification at Eutectic point
(Eutectic point alloys)
𝜷
𝜶
• There is a solidification at a single
temperature (Thermal arrest)
• Formation of lamellar plates
Temp
(
o
C)
Time (sec)
Cooling Curve
Thermal Arrest
61

Liquid
eutectic reaction
Liquid
liquid
Solidification at Near Eutectic
point (Near Eutectic alloys)
,
𝜷
𝜶
𝑬
Primary
,
,
;
Temp(
O
C)
Time(sec)
Cooling Curve
Thermal
Arrest
62

Classification of Eutectic Structures
Irregular plate-like eutectic
structure in Al-Si
Rod-like and plate-like
eutectic structures in Cu-Ag
Spiral eutectic structure in
ZnMg-Zn2
Irregular plate-like eutectic
structure in Cd-Bi
Irregular eutectic structure in
Co-TaC
Rod-like eutectic structure
in FeFe2B 63

Alloys with out Eutectic
Homogenous grain
• Low strength
• High ductility
• High corrosion resistance
• Low brittleness
Lamellar
• High strength
• Low ductility
• High brittleness
• Low corrosion resistance
Alloys with Eutectic
https://www.youtube.com/watch?v=K9pZZ3DjvCU 64

P. Lü & H. P. Wang | 6:22641 | DOI: 10.1038/srep22641 www.nature.com/scientificreports
65

• Peritectic reaction, in which the primary phase reacts with a liquid phase at
a triple junction on cooling to produce the peritectic phase.
• Observed in many binary alloys systems, such as Ti-Al, Fe-Co, Fe-Ni, etc.
• Terminates once the primary phase is enwrapped by the peritectic phase.
• Then, the primary phase transforms to the peritectic phase by peritectic
transformation.
Peritectic reaction
at 1573K
• Peritectic phase grows equiaxially at a cooling rate of 0.167K/s
• . . alloy is a typical peritectic composition in Ni-Zr binary alloy
system.
• The primary phase and peritectic
phase are both intermetallic
compounds.
• Phase selections between primary
phase and peritectic phase have great
influence on the final solidified
microstructures, which directly relate
to the materials characteristics.
66

Average volume fractions of peritectic
phase Ni5Zr versus droplet diameter
Average cooling rate andundercooling
versus droplet diameter.
liquid
≫
liquid
P.
Lü
&
H.
P.
Wang
|
6:22641
|
DOI:
10.1038/srep22641
www.nature.com/scientificreports
67

Solidified microstuctures of 𝑵𝒊𝟖𝟑.𝟐𝟓𝒁𝒓𝟏𝟔.𝟕𝟓 peritectic droplets with different diameters
0.167 K/s
Cooling rate
at DSC
2.8× 103 K/s
Cooling rate
in the drop
tube
68

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