MSE 3331 Module 1 Lecture Metals Processing AU23

MSE 3331 - Autumn Semester 2023
Materials Science and Engineering Lab I

Module 1: Thermomechanical Processing
Lecture 1. Introduction to Metals Processing
Alan A. Luo
Professor of Materials Science & Engineering
Professor of Integrated Systems Engineering (Manufacturing)
The Ohio State University, Columbus, OH, USA
luo.445@osu.edu 1
My introduction
 Joined OSU in 2013, as MSE and ISE Professor
 25 years of industrial R&D experience including 15 years at General Motors
Global R&D Center, Warren, MI
 Research in lightweight metallic materials (Al, Mg, Ti, high entropy alloys,
and metal matrix composites), advanced manufacturing processes, and
integrated computational materials engineering (ICME)
 Feel free to e-mail me (luo.445@osu.edu) for meetings or discussions
2
Outline
 Why metals? automotive examples
 Introduction to metals processing
 What is thermomechanical processing (TMP)?
3
Metals: automotive example
4
Manufacturing processes
Manufacturing
How is the input
Processes material changed?
Sheet Polymer
Deformation Casting Metal Processes Machining Finishing Assembly
Extrusion Centrifugal Bending Blow molding Boring Anodizing Automated

Forging Die casting Blanking Casting Drilling Honing Bonding
Rolling Investment Drawing Compression molding Facing Painting Brazing
Bar drawing Permanent mold Punching Extrusion Grinding Plating Manual
Wire drawing Sand casting Shearing Injection Molding Milling Polishing Riveting
Spinning Thermoforming Planing Soldering
Transfer molding Turning Welding
Sawing
ECM, EDM 5
Classification of materials processing
- by material
Metals processing Plastic processing

 Metal casting  Extrusion
 Powder metallurgy  Injection Molding
 Rolling  Blow Molding
 Forging  Vacuum Forming
 Sheet forming  Compression Molding
 Heat-treating  Calendering
Ceramic processing  Strip Heating
 Glass forming  Rotational Molding
 Particulate forming
 Cementation
6
Metal casting processes
 Continuous casting processing – steel and non-ferrous slabs and plates
 Expendable mold processing – the molds are not re-usable
 Sand casting
 Evaporative pattern casting
 Investment casting
 Permanent mold processing – the molds can be re-used
 Die casting (gravity or under pressure)
 Centrifugal casting
 Semi-solid casting
 MSE 5451 in SP24 – Molten Metal Processing (please sign up if interested)
design pattern pouring casting 7

MSE 5451 / ISE 5502 in SP24:
Molten Metal Processing
Chapter 1. Ferrous Extractive Metallurgy (two weeks)
Chapter 2. Non-ferrous Extractive Metallurgy (three weeks)
Chapter 3. Solidification (one week)
Chapter 4. Continuous Casting (one week)
Chapter 5. Cast Alloys (one week)
Chapter 6. Shape Casting (one week)
Chapter 7. Casting Processes (one week)
Chapter 8. Other solidification processing (one week)
Chapter 9. Casting Simulation - MagmaSoft (two weeks)
8
Experimental foundry at Center for Design
and Manufacturing Excellence (CDME)
2,000 sf capable of casting ferrous and non-ferrous metals

PVT vacuum induction furnace with a water-cooled copper
crucible for titanium and high-entropy alloy casting
9
High pressure die casting machine at CDME
 280 ton LK Die Casting Cell – Al and Mg

 Fondarex Highvac vacuum system for super vacuum die casting
10
Advanced Casting Research Center (ACRC)
 ACRC is dedicated to collaborative research in metal processing and manufacturing through a

consortium of ~40 corporate members.
 Our focus is metal casting, alloys and processes, recovery and recycling, & digital
manufacturing.
 We hire undergraduate research assistants at ACRC to do industry-sponsored research.
Material Producers Casters

 AlmexUSA
Alcoa ACRC  ATEK
Aluminum Rheinfelden Gmbh
Audubon Metals
Members  Linamar Light Metals
IBC Advanced Alloys  Magna International
Materion  NEMAK
NioCorp  WBTL
End Users
Suppliers  General Motors Corp.
CPC Machines  Harley-Davidson Motor Co. National Labs/Associations
Fehrmann Alloys GmbH  Honda?  AFS
Inductotherm Group  Mercury Marine  Aluminum Association
Intrepid Automation  Oshkosh  CANMET
MAGMA  Pratt & Whitney  LANL
Persimmon  Schnitzer  NADCA
QuesTek Innovations LLC  Space X  PNNL?
SPEE3D  Stellantis  Sandia Camino
Thermatool  Tesla
VJ Technologies
11
Student chapter
 A very active AFS (American Foundry Society) student
chapter (28 members at this time)
 Known as “The Foundry Club” on campus
 Regular meetings and activities (including those with
local industry and AFS Central Ohio Chapter)
 Please visit club website (https://u.osu.edu/afsatosu/)
& email Michael Moodispaw (.4) to join the club
12
FEF students
 Foundry Educational Foundation (FEF) supports metal casting educational programs
at colleges and universities, offering scholarship & employment opportunities.
 OSU is a certified FEF school. Please register at https://www.fefinc.org/students.html.
 5 or 6 students attending FEF College Industry Conference (CIC) every year
 As FEF Key professor, I’m selecting students to attend CIC on Nov. 16-18 in Chicago.
 Please email me (luo.445@osu.edu) if you are interested in attending (expenses paid).
13
How is a casting made?
Die
Bottom
mold plate
Feed tube
system
Furnace
14
Thermomechanical processing (TMP)
 Thermomechanical Processing (TMP) is solid-state metals

processing which includes:
 TMP = Thermomechanical processing
 TMP = Thermal processing (no mechanical force)
 TMP = Mechanical processing (no heat)
 TMP – applicable to multiple processing methodologies
including
 Rolling
 Forging
 Extrusion
 Hydroforming
 etc…
15
TMP: classification by workpiece
Metal Forming Processes
Bulk Forming Processes Sheet Forming Processes
• Spatial workpieces (3 dimensional) • Planar workpieces (2 dimensional)

• Large changes in cross-section - sheets, plates
& large changes in thicknesses • Hollow pieces with almost constant
• Material flows in all directions wall thickness
• Generally multi-axial compressive • Generally two-axial stress states:
stress states tensile-tensile/tensile-compressive
• Larger relative forces
16
TMP: classification by temperature
Forging , Rolling, Extrusion, Drawing

Hot forming (T > 0.55 Tmelting)
- lower strength and recrystallization
- bigger shape changes
- poorer finish
Warm forming (0.35 Tm < T < 0.55 Tm)
- recovery not recrystallization
Cold forming (T ~ Room T)
- strengthen through work hardening
- smaller shape changes
- better finish 17
TMP: recrystallization temperatures
Recrystallization Recrystallization
Material Material
Temperature Temperature
C-Steel 550oC tin 0 to 40oC
Pure-Al 290 to 300oC zinc 50 to 100oC
Dur-Al 360 to 400oC Mo 870oC

200oC
Cu (changes drastically with alloying W 900-1000oC
elements)
Lead -50 to 50oC Ni 400-600oC
18
First law of metal forming:
volume constancy
 The volume of the formed body remains constant during the plastic
deformation (experimental finding)
Before forming After forming
V  a0  b0  c0  a1  b1  c1  const dV
    0
Ausgangsvolumen
Initial volume Endvolumen
Final volume dt
19
Closed-die forging: crankshaft
 From ancient blacksmith to modern forging operations
20
Extrusion: I-beam production
 Extrusion is a process used to create objects of a fixed cross-sectional profile.
A material (metals, polymers, ceramics, concrete) is pushed or drawn through
a die of the desired cross-section.
21
Sheet metal drawing: stamping
 Drawing is a sheet metal forming operation used to make cup-shaped, box-shaped, or
other complex-curved, hollow-shaped parts. It is performed by placing a piece of sheet
metal over a die cavity and then pushing the sheet into the opening with a punch. The
blank is held down flat against the die by a blankholder.
Punch ram
Punch
Blank
holder
Clamp
Die force
Blank
Drawn 22
part
Sheet metal drawing: stamping
23
The door can also be made
by casting process
GM-OSU research collaboration
24
Large aluminum die castings by Tesla:
Giga press and giga casting
 Largest die casting machines in the world: 5,600 ton in CA & 9,000 ton in TX
25
Rolling
 Rolling is a metal forming process in which metal stock is passed through one
or more pairs of rolls, at room (cold roll) or elevated temperatures (warm or
hot roll) to reduce the thickness and to make the thickness uniform.
26
Summary…Questions?
Metals are essential to industrialization and global economy.
Manufacturing is transformation of materials, and metals processing is
critical part of manufacturing.
Thermomechanical processing (TMP) is a highly efficient solid-state
metals process, which is widely used to make a variety of components.
34.6 40
AX51 (Mg-5Al-1Ca)
AX52 (Mg-5Al-2Ca)
AX53 (Mg-5Al-3Ca)
950K
26.0 30
C14 - Mg2Ca
900K
A)
(C
17.3 20 850K
w%
790K 800K
800K
C36 - (Mg,Al)2 Ca
AX53
8.7 10
850K -Mg
AX52
AX51
900K
750K Mg17 Al12
0
0.0 922K 711K
00 10
10 20
20 30
30 40
40
MG w%(AL)
w%(AL)
Contact: luo.445@osu.edu 27
College of Engineering
Dept. of Materials Science & Engineering
Module 1: Themomechanical Processing
Rolling, Heat Treating, Hardness
MATSCEN 3331
Autumn Semester 2023
August 17, 2023 1

Thermomechanical Processing College of Engineering
• Definition: “THERMOMECHANICAL PROCESSING (TMP) refers to various metal forming

processes that involve careful control of thermal and deformation conditions to achieve
products with required shape specifications and good properties.”
- ASM Handbook, Volume 14A: Metalworking: Bulk Forming S.L. Semiatin, editor, p286-296 DOI: 10.31399/asm.hb.v14a.a0003995
• THERMOMECHANICAL PROCESSING (TMP) refers to various metal forming processes that

involve careful precise, accurate control of thermal and deformation conditions to achieve
products with required that meet shape specifications and good and have material properties
that are suitable for the application.
• Thermal Processes:
• Deformation Processes:
August 17, 2023 2

Rolling Processes College of Engineering
• Cast metals undergo TMP to

become wrought metals.
• Various rolling processes are
shown in the figure on the right.
Continuous casting
or
Ingot
August 17, 2023 3

Hot Rolling (HR) and Cold Rolling (CR) College of Engineering
https://www.manufacturingguide.com/en/hot-rolling-sheets https://www.manufacturingguide.com/en/cold-rolling-sheets
August 17, 2023 Link: Roll Forming Processes 4

Comparison of HR & CR Processes College of Engineering
HOT ROLLING COLD ROLLING

Advantages Advantages
• Large reductions are possible • Smooth, shiny surface finish
• Grain structure is equiaxed and smaller than
original • Closer tolerances can be met
• Lower cost • Lower thickness possible relative to HR
• Lower residual stress due to slow cooling • Work hardening results in higher strength
after coiling
Disadvantages
Disadvantages
• Elongated & oriented grains
• Lower tolerance control
• Materials properties are directional
• Oxidation of the surface
• CR requires more power to the rolling mill
• Rougher surfaces
• Uniform mechanical properties, but lower
strength and stiffness than CR
August 17, 2023 5

Variables in Flat Rolling Process College of Engineering
August 17, 2023 6

Considerations in Flat Rolling Processes College of Engineering
• Camber occurs when rolls are not ground properly.

• Strip widening may occur when large reductions are
made in materials with low width/thickness ratios.
August 17, 2023 7

Flat Rolling Defects College of Engineering
Wavy Edge
Edges Cracking
Zipper Alligatoring
Cracks
August 17, 2023 8

Residual Stress in Materials after Rolling College of Engineering
• The upper schematics show the material undergoing reduction.

• The lower diagram shows the qualitative sign and magnitude of the stress in the resulting
material.
• In (a) small rolls and/or small reductions per pass were used
• In (b) large rolls and/or large reductions per pass were used (note reversal of stresses)
August 17, 2023 9

Types of Mills College of Engineering
• Two high roll is what we will use in lab; however, we will not use reversing action.
• Four high rolls are common in industrial tandem mills.
• Cluster mills are used for higher strength or tight tolerance (i.e. high cost) steels.
August 17, 2023 10

Tandem Roll College of Engineering
• Used in both hot rolling and cold rolling operations.
https://thelibraryofmanufacturing.com/metal_rolling.html
August 17, 2023 https://www.tmeic.com/application/cold-mill-systems 11

Fe-C Phase Diagram College of Engineering
• Steels are in the low carbon range of

the phase diagram with less than 1%
carbon.
• Focus on this today. Cast irons
would require an additional session
to cover.
• Need to define some critical
temperatures for heat treating.
• A1 – lower critical temperature
• A3 – upper critical temperature
Heat treating is a critical process step in

materials processing. Understanding
the effects of heat treating processes is
critical for all types of materials; steel is ASM Handbook Volume 11
just the example we are working with.
August 17, 2023 12

TTT Diagram (Isothermal Transformation) College of Engineering
• Time-temperature-transformation
diagrams.
• Also referred to as isothermal
transformation diagrams.
• Useful if on needs to develop a specific
mixed microstructure or single phase.
• Example if you were tasked to create a
fully martensitic steel, how could you do
that here?
• If you wanted to create a bainitic steel,
how would you do that? 1045 Steel
880°C austenitization temperature
• These type of processes require
specialized equipment such as molten
salt baths to perform the heat treatment.
• Many industrial processes rely on more
continuous cooling processes.
ASM Handbook Volume 11
August 17, 2023 13

CCT Diagram College of Engineering
• Continuous-Cooling-Transformation
diagram.
• Processes where the component or
material is cooled in a continuous
manner at some slower rate.
• Furnace cooling, air cooling, or mild
quenching are used to achieve these
rates.
• CCT diagrams are useful to design
more economical processes than
using isothermal hold types of heat 1045 Steel
treating. 880°C austenitization
temperature
• Common in steel processing where
cost is always an issue.
ASM Handbook Volume 11

August 17, 2023 14
Heat Treating Processes College of Engineering
• Normalizing (Steels)
• A homogenizing and/or grain refining heat treatment.
• This is an austenitizing heat treatment followed by cooling in still or slow moving air.
• Normalizing is done to cast ingots before working and to cast steel parts or forged steel
parts prior to hardening heat treatments.
• Temperature for normalizing should be 55°C (100°F) higher than the upper critical
temperature (Ac3). 870°C (1600°F) is a typical normalizing temperature; however, the alloy
content of the steel may require higher or lower temperatures.
• Homogenization (Non-ferrous Alloys)

• Similar to a normalizing heat treatment, but this is the language applied to non-ferrous
alloys
• Aluminum alloy ingots are homogenized after casting and before any additional work is
done for example.
• Similar process, alloys are heated to a temperature where a single phase solid solution
exists (quite near melting temperature typically) and then slowly cooling
August 17, 2023 15

• Annealing
• Generic term referring to a heat treatment mainly used to soften metals.
• Full Annealing: material is heated above the upper critical temperature and slowly cooled
back to room temperature. Times for full anneal depend on desired final properties.
• Stress-Relief Annealing: material is heated below the lower critical temperature for a
relatively short period of time and slowly cooled back to room temperature
• Spherodizing Annealing: material is heated near the lower critical temperature and held
for a significant period of time before slow cooling back to room temperature.
August 17, 2023 16

Annealing Conditions
(typical ranges, many special
cases)
- Full Anneal
- Stress Relief Anneal
- Spherodizing Anneal
August 17, 2023 17

• Hardending (specifically austenitizing and quenching) – not surface hardening
• Heating the material above A3 and holding to fully convert to austenite

• Rapidly quenching to form martensite in steel.
• The selection of austenitizing temperature, time, transfer to quenchant, type of quenchant

used, and the agitation all need to be considered.
• Maximum hardness of the material in the as-quenched state, typically requires another heat
treatment (tempering) to recover some toughness or ductility.
• For non-ferrous alloys (aluminum as an example here) similar processes are done to harden
the alloys.
• Solution heat treating to form a single phase, followed by quenching to maintain the single
phase microstructure is performed regularly.
• In these alloys a precipitation (aging) heat treatment is required to increase the strength
August 17, 2023 18

Quenching College of Engineering
• Example of an austentizing and quenching process where the part is dropped directly into the
quench tank.
• Quenchant agitation is a key component to achieve a uniform quench.
August 17, 2023 19

• Tempering
• Process where previous hardened (sometimes normalized, but mainly hardened) steel is
heated to a temperature below A1 and held for a period of time and cooled at a suitable
rate to increase:
• Toughness
• Ductility
• Increase the grain size
• Tempering temperatures range from 200°C up to 600°C depending on the desired final
properties.
• Temper embrittlement can be a concern for some steels.
• 200 - 400°C, martensite with excess carbon can form cementite, retained austenite will
transform into ferrite and cementite and the cementite phase can be quite coarse leading
to a decrease in toughness.
• Processes need to be developed and adhered in order to prevent this.
• Tempering may be repeated two or three times to improve the microstructure for certain
applications. Double tempers have been found to lower the ductile-to-brittle transformation
temperature in some steels for example and minimize or eliminate residual austenite.
August 17, 2023 20
Surface Hardening Processes College of Engineering
• Generic term is case hardening when referring to a heat treating process that increases the
hardness of a steel surface.
• Numerous processes: carburizing, nitriding, carbo-nitriding, flame hardening, induction
hardening.
• Some processes are gas, some use fluidized beds, others even pack them in carbon/charcoal.
The goal is to drive in more carbon and/or nitrogen to create a case or hard layer at the
surface.
• Flame and induction hardening use rapid heating at the surface followed by quenching to
develop a hard surface layer. Faster processes than heat treatments that rely on diffusion to
drive carbon and nitrogen into the surface.
• The goal of all of these processes is to create a hard surface on the material while
maintaining the internal toughness of the part.
• Too many processes and too many important details for each to cover these processes in any
substantial depth here. We’ll include some case studies where surface hardening heat
treatments played a role later in the class.
August 17, 2023 21

Heat Treating Jargon College of Engineering
• Carbide: cementite (Fe3C)
• Ramp: heating or cooling rate in a heat treating process
• Soak: dwell time or the time at a given temperature
• Draw: tempering temperature or time

• Double Draw, Triple Draw
• Slack Quench: incomplete quench, often cause by the vapor barrier during quenching
• Scale: iron oxide that forms on the surface of steel during high temperature processing in air
• Decarb: decarburization or the loss of carbon at or near the surface in steel
August 17, 2023 22

Decarburization College of Engineering
• Decarburization is simply the loss of carbon

on the surface or the surface adjacent region
of steel.
• Decarb happens when there is sufficient
temperature, time, and reactive species in
the atmosphere.
Scale
• Reactive Species
• Typical Processes where this is Decarb

important
• When oxygen is present (in air) there is

some competition between oxidation and
decarburization; however, if there is both
oxidizing and reducing species present then
oxide can actually increase the http://www.raysteeltube.com/Decarburization-of-steel-tube-heat-treatment-surface-and-
preventive-measures-id6746046.html
decarburization rate during annealing.
August 17, 2023 23

Example – Batch Annealing Steel Coils College of Engineering
• Batch annealing is used

frequently on cold rolled
steel.
• The environment contains
hydrogen to reduce any
light oxidation that has
developed on the surface.
• Process environment must
be carefully controlled.
• Steel that goes into this
process cannot have
significant scale.
https://www.eurotherm.com/heat-treatment-articles/single-and-multi-stack-batch-annealing/
• Why is heavy scale not compatible with batch annealing?

Shouldn’t H2 (gas) reduce the scale?
Fe3O4 + 4H2 = 3Fe + 4H2O (g)
FeO +H2 = Fe + H2O(g)
Fe3O4 + Fe = FeO
• Water is also bad news in a batch annealing furnace.
https://dev.worthingtonindustries.com/Expertise/Processing-Capabilities/Steel-Annealing
August 17, 2023 24
Extreme Decarburization Example College of Engineering
• These samples were intentionally

decarburized, to show how important
process control is.
• Pickled, then cold rolled steel, 0.2mm
thick, ~ 0.15 wt% C.
• Annealed at 800°C for 1, 3, 5, and 10
minutes.
• Dry hydrogen (a – d)
• Wet hydrogen (e – h)
𝐶𝐶 + 𝐻𝐻2 𝑂𝑂(𝑔𝑔) → 𝐶𝐶𝑂𝑂 + 𝐻𝐻2
𝐶𝐶 + 2𝐻𝐻2 → 𝐶𝐶𝐻𝐻4
• Water is bad.
• Need to tune process to have just
enough, but not too much hydrogen.
August 17, 2023 Y-A. Jing et. al. 25

Hardness Testing College of Engineering
• “Hardness is a somewhat imprecise term. It is essentially a measure of a material’s

resistance to surface penetration by an indenter with a force applied to it.” T. H. Courtney
• Hardness is a characteristic of a material, not a fundamental physical property.
• Some hardness tests can be directly related to the

strength of a material while others cannot. Mechanical Behavior of Materials
T. H. Courtney
• Hardness testing is much easier and faster to carry McGraw-Hill, New York
out than tensile testing and has found widespread 1990
industrial use. ISBN: 0-07-013265-8
• Microhardness testing is also used in research &

development applications regularly. Indentations
on the scale of the microstructure can be made and
this technique is useful for multiphase materials and
materials joining.
August 17, 2023 26

Brinell Hardness Dept. of Materials Science & Engineering
F
• Brinell hardness test are commonly
used to test materials that have a
structure that is too coarse or that
have a surface that is too rough to be
tested using another test method, D
e.g., castings and forgings.
• Brinell testing often use a very high
test load (3,000 kgf) and a 10mm
diameter indenter so that the
resulting indentation averages out
most surface and sub-surface
inconsistencies d
• Standard: ASTM E10-18
• Nomenclature
2𝐹𝐹 * Units are stress
• BHN (Brinell Hardness Number) 𝐵𝐵𝐻𝐻𝐵𝐵 = (N/mm2), but often
• HBW (Hardness, Brinell, WC 𝜋𝜋𝜋𝜋 𝜋𝜋 − 𝜋𝜋 − 𝑑𝑑 reported as load/area
(kg/mm2).
indenter)
• HB (Hardness Brinell) BHN: Brinell Hardness Number
• Telebrinell test uses hammer and F: applied load (Force)
indenter to make measurements. Still D: indenter diameter
useful in some applications.
d: diameter of the indentation
August 17, 2023 27
Microindentation Hardness Testing Dept. of Materials Science & Engineering
• Vickers
• Macro Vickers (30 kgf loads)
• Vickers microindentation hardness testing (5 gf to 2 kgf)
• Symmetrical (4 sided pyramidal) diamond indenter
• Most commonly used and reported microindentation hardness scale
• Load can have significant affect on accuracy.
• Reported as HV0.3 (hardness Vickers, 300gf)
• Knoop
• Microindentation Hardness Testing (5 gf to 2 kgf) HV HK
• Asymmetric diamond indenter (7:1 aspect ratio)
• Commonly used for coatings or when less space
between microindentations is required
• Similar reporting, HK0.5 (hardness Knoop, 500 gf)
Image Source: https://www.emcotest.com/en/the-world-of-hardness-testing/hardness-know-

how/theory-of-hardness-testing/knoop-51/comparison-between-knoop-and-vickers-methods-244/
August 17, 2023 28

Microindentation Hardness Testing College of Engineering
• Standard for microindentation hardness testing
• ASTM E384-17
• ASTM E92-17 (Vickers) is also frequently cited
• Spacing between microindentations is critical so the previous indentation does not
influence the next.
• Minimum 2 diagonals between each indent (for HK in thin direction means indents can
be placed closer together).
• Lighter loads result in lower accuracy.
• Indentation becomes strongly influenced by the surface condition
and interacts with a very thin layer on the surface.
• Below 50gf load, microindentation hardness should be used for
qualitative comparison, not quantitative analysis.
• Microindentation hardness is extremely useful in materials
joining and multiphase materials research.
• Modern equipment can create hardness “maps” using large
arrays if microindentations.
Image Source: https://www.struers.com/en/Knowledge/Hardness-testing/Knoop#application
August 17, 2023 29

Rockwell Hardness College of Engineering
• “A hardness test commonly used in the United States is the Rockwell hardness test. Various combinations
of load and indenter can be used in the Rockwell series of tests.” T.H. Courtney
• “In contrast to Brinell and Vickers hardness previously described, the Rockwell hardness number is
dimensionless, and it does not relate directly to material yield strength. In fact the Rockwell hardness
number correlates with the inverse of the indentation depth. The test is easy to perform and rapidly
accomplished. As a consequence it is used widely in industrial applications, particularly in quality control
situations.” T.H. Courtney
• Rockwell hardness has a HUGE number of scales for different applications. There is a standard set of
Rockwell scales that use 60, 100, 150 kg loads, and a set called superficial that use 15, 30, an 45 kg loads.
• Indenters can be conical diamond indenters, carbide ball indenters, or hardened steel indenters. The
diameter of the indenters ranges from 1/16” up to 1/2“.
• Note Rockwell hardness uses mixed units! Loads are in SI units, indenter dimensions are in standard
units. The Rockwell hardness number is unitless.
• As noted, the numbers are dimensionless (unitless) and do not directly relate to yield strength. Some tables
relate hardness to ultimate tensile strength, these are estimates only and should not be reported as
quantitative values.
August 17, 2023 30

Rockwell Hardness College of Engineering
• Two scales in Rockwell hardness testing are used in the vast majority of testing.
• Rockwell B Scale: 100 kg load, 1/16” hardened steel ball indenter
• Rockwell C Scale: 150 kg load, conical diamond indenter
• Nomenclature
• The proper term used in specifications for a Rockwell hardness number is HRB, HRC, etc.
• Often one will see it reported as RB or RC , particularly in industrial labs.
• The current ASTM standard for Rockwell hardness testing is ASTM E18-22.
• Rockwell hardness measurements are accomplished by placing the sample on an anvil, applying
a small preload, then applying full load for 10 – 15 seconds, and measuring the depth between
the preload position and the full load position.
• Materials properties and thickness

determine the scale that should be used
for hardness testing.
• In this lab we will use both HRB and
HRC indenters and measurement scales.
August 17, 2023 31

Rockwell Hardness Testers, Indenters, Anvils, College of Engineering
Hardness Test Blocks Dept. of Materials Science & Engineering
• There are two main types of Rockwell hardness testers

• Dead weight testers and load cell based testers (we will discuss load cells later).
• Dead weight systems have the advantage of being simple and difficult to damage or
“knock out of calibration”.
• Load cell based system are more accurate but require frequent calibration and more
care in handling to prevent damage to the load cell.
• The anvil is what the sample is tested on. Typically it is hardened steel and the smallest
area that can be used to support the sample results in the most accurate measurement.
https://www.hardness-testblocks.com/
August 17, 2023 https://www.buehler.com/
Converting Hardness to Tensile Strength College of Engineering
• There are tables available that report conversions between hardness scales and relate Rockwell
hardness to tensile strength. Tensile strength values may be highly inaccurate for a particular
application and a correlation must be developed for the particular material of interest.
• ASTM E140-12b provides accepted conversion methods between hardness scales which may be
useful if a report is using a different hardness scale than one is used to or one does not have the
capability to perform.
• An example of a hardness conversion table is

provided to the right.
• Notice there is no conversion between HRB and
HRC. When the hardness is greater than or equal
to 100 HRB, one needs to change to HRC scale.
• Note some testers extrapolate to 105 HRB,
these values are incorrect and should never
be reported, 100 is the end of the HRB range.
August 17, 2023 33

Key Points for your Lab Work College of Engineering
• Differences in the grain structure of hot rolled and cold rolled metal.
• Observe and note the differences in surface finish between HR & CR samples.
• Cold rolling requires several small reductions to achieve the final thickness while hot rolling
will be require fewer reductions, but time for static recrystallization in between each
reduction.
• Note hardness changes as reduction increases in CR vs. HR steel samples.
• Compare the hardness and grain structure of annealed steel samples after 80% reduction by
cold rolling to original annealed samples.
• Document your annealing data if your team is responsible for an annealed sample this week.
• Understand how to use the Rockwell hardness tester
• Rockwell Hardness B-scale (HRB): 1/16” ball indenter, 100kgf load, range is 20 – 100 HRB
• Rockwell Hardness C-scale (HRC): conical diamond indenter, 150kgf load, range is 20 – 70
HRC.
• Note any errors that can be introduced by the person doing the test, and the accuracy of
hardness testing measurements based on data collected.
August 17, 2023 34

Steel Microstructures
MATSCEN 3331
Autumn Semester 2023
August 17, 2023 1

Updates College of Engineering
• Lab sessions will meet in 0158 Fontana Lab (basement lab).

• This week’s labs will cover mounting, grinding, and polishing samples.
• Each group will make two (2) mounts with two (2) samples in each mount.
• Documents with the metallographic mount information and the metallography procedures
are posted on Carmen.
• We will etch and examine the mounted samples using optical microscopy next week.
• No lecture scheduled next week (Week 5), labs conducted at regularly scheduled times.
August 17, 2023 2

Metallography College of Engineering
• Definition:
• Process steps in metallography

1. Sectioning (cutting)
2. Mounting
3. Grinding
4. Polishing
5. Etching
6. Microscopic Examination*
* We often examine specimens after polishing and before etching. There may be
microstructural features (e.g. inclusions, cracks, voids, etc.) that may be obscured or destroyed
by the etchant.
August 17, 2023 3

Sectioning College of Engineering
• Sectioning (cutting a sample from the larger part) is a very important part of the
metallographic process.
• Saw selection and damage to the sample need to be considered carefully.
• Bulk cuts may be done with a torch or band-saw, but final cuts should be made with a
metallographic cut-off wheel or precision saw with coolant.
Diamond or Boron Nitride

coated blade.
Slower, smaller samples,
but very precise cuts
possible.
Abrasive (ceramic grit)

cut-off wheel.
Fast & able to cut
large samples.
August 17, 2023 4

Mounting College of Engineering
• Hot (melting) mounting and cold (epoxy resin) mounting.

• Hot mounting is fast and creates solid mounts, sample has to be able to withstand
temperatures and pressures without deforming during mounting.
• Cold mounting is versatile and can accommodate soft samples. Often has poor edge
retention and often takes 1 – 24 hours to cure completely.
• Cold mounting can be done under vacuum to help fill pores.
• Mounting makes holding the sample easier, allows for automation, and protects the sample
edge during grinding and polishing
August 17, 2023 5

Grinding College of Engineering
• Grinding is used to remove damage and scratches from the sectioning process.
• Often the mounted sample is ground on a belt sander with 60 or 120 grit abrasive paper and
flowing water.
• The sample is then ground on strips or a rotating wheel with progressively smaller grit
abrasive starting at 240, 320, 400, 600, 800, and 1200 grit. Procedures vary by material and
every metallographer has their own system that works for them.
• The abrasive paper (sandpaper) used in metallographic grinding is typically silicon carbide.
August 17, 2023 https://www.doitpoms.ac.uk/tlplib/optical-microscopy/preparation.php 6

Polishing College of Engineering
• Polishing is done with diamond pastes or slurries on soft clothes and is intended to remove all the scratches
remaining from grinding. A polished surface will have a mirror like appearance and few to no scratches visible
when observed in an optical microscope at 100 – 200x magnification.
• Typical diamond particle size in polishing media are 9μm, 6μm, 3μm, and 1μm.
• We will polish with 6, 3, and 1 micrometer diamond pastes.
• Polishing cloths have a range of what is referred to as napped fabrics.
• A napped fabric is a process to raise woven or knit fibers in a cloth, then shearing them off to make them even.
A high napped cloth will hold a lot of polishing compound and is good to remove heavy scratches; however, it
will round the edges of your sample. A low napped cloth will hold enough diamond to polish but will not
damage sample edges as much.
• Final polishing is often one using colloidal silica with a particle size of 0.05μm or less, but not in all cases.
• Grinding and polishing can be semi-automated, once a process is developed and proven for a material.

Etching College of Engineering
• Etching is a technique that highlights features and creates contrast for the microscopy technique used
(optical or electron).
• There are different types of etchants
• Attack etches: controlled corrosion, often attack grain boundaries preferentially.
• Stain etches: the etchant creates a chemical reaction with a certain phase or element creating
contrast in the image
• Electrolytic etches: can be used as an attack etch or to form a thin layer on the surface (typically and
oxide) that creates contrast in the image
• We will use an attack etch called Nital (nitric acid (2 – 5%) + ethanol) to show the grain boundaries in
our samples.

Optical Microscopy College of Engineering
• We will use brightfield optical microscopy to examine the surface of our steel samples.
• Brightfield means the optical ray paths are set such that the reflected light from the bulk or majority
phase will appear bright in the images. This is the typical mode used in optical microscopy.
• Dark field, differential interference contrast, polarized light, and polarized light with color tint filters can
also be used in special circumstances.
August 17, 2023 9

Directions in Rolled Steel College of Engineering
• Rolled steel has three primary directions

• The rolling direction (RD), also called the longitudinal direction
• The transverse direction (TD)
• The normal direction (ND)
• An assembly of micrographs taken in each direction is shown below.
• We will look at cross-sections along the rolling direction; the direction of maximum
elongation.
August 17, 2023 https://www.scielo.br/j/mr/a/fxLR8kTVZ5jhVzCS78GcMbS/?lang=en# 10

Steel Phases & Optical Microscopy College of Engineering
• The remaining slides will talk about steel phases and how we observe them in the optical
microscope.
August 17, 2023 11

Heat Treating (Mini-Review) College of Engineering
• Critical temperatures, temperature ranges for
heat treating steels shown on Fe-C phase
diagram.
• Phases resulting from various cooling
practice shown on the right.
August 17, 2023 Figure reproduced from reference 1, chapter 11. Figure reproduced from reference 2. 12
Eutectoid Steel (equilibrium cooling) College of Engineering
August 17, 2023 Figures reproduced from reference 1, chapter 10. 13

Hypoeutectoid Steel Microstructures College of Engineering
• Near equilibrium cooling

1010, equilibrium cooling
• Relatively equiaxed ferrite & pearlite
Figure reproduced from reference 3, chapter 1.
Figure reproduced from reference 1, chapter 10. Figure reproduced from reference 3, chapter 1.
August 17, 2023 14
Widmanstätten ferrite College of Engineering
• Non-equilibrium cooling in a hypoeutectoid steel results in the formation of Widmanstätten

ferrite.
• Widmanstätten ferrite is regularly found in welds of hypoeutectoid steels.
Figure reproduced from reference 5.
Figure reproduced from reference 1, chapter 10. Figure reproduced from reference 5.
August 17, 2023 15

Hypereutectoid Steel Microstructure College of Engineering
• Note this is equilibrium cooling, hypereutectic steels are have high hardenability due to high
carbon content and are often used in a hardened form (e.g. blades).
August 17, 2023 16

Pearlite College of Engineering
• Hypoeutectoid steel microstructure shown on the left. In the optical microscope, at low
magnification the pearlite colonies may appear brown/black and no lamellar structure is
visible after Nital etching.
• Higher magnification can reveal the lamellar structure and the size of the lamella help
determine the temperature range where the pearlite was formed (i.e. fine vs. coarse).
Figures reproduced from reference 4.
500x magnification images of pearlite, Nital etched.

Figure reproduced from reference 5. Left: coarse pearlite formed at 700°C.
Right: fine pearlite formed at 600°C.
August 17, 2023 17
Bainite College of Engineering
• Bainite has two forms, upper and lower bainite. The
mechanisms of bainite formation are beyond the scope of this
class.
• TTT diagram that shows separation of the pearlite and bainite
regions.
• Detailed heat treating history is required to identify bainite in the
optical microscope.
• 4340 is a good example, it will appear 100% martensitic, there is
some bainite in the microstructure.
Figure reproduced from reference 5. Figure reproduced from reference 4.

August 17, 2023 18
Bainite College of Engineering
• !! IMPORTANT !!
• It is not possible to distinguish between bainite and martensite in an optical microscope
unless you have detailed knowledge of the heat-treating history.
• On an unknown steel it is nearly impossible to distinguish bainite from tempered
martensite visually. The identifying features are too fine to be resolved in an etched
sample with an optical microscope.

Figures reproduced from reference 4.

August 17, 2023 19
Martensite College of Engineering
• BCT phase, magnetic.
• Displacive phase transformation (no
diffusion).
• a/c ratio depends on carbon content.
• Note the midrib in the lower figure, helps
distinguish between lath and plate
martensite.
August 17, 2023 Figures reproduced from reference 4. 20

Martensite College of Engineering
August 17, 2023 Figure reproduced from reference 4. 21

Rolled Steel Grain Structure Examples College of Engineering
• 1018 after 60%reductions cold rolling (left), and hot rolling (right).
August 17, 2023 22

References College of Engineering
1. Elements of Metallurgy and Engineering Alloys, F.C. Campbell, ASM International, 2008, ISBN: 978-1-62708-251-8.
2. Atlas of Isothermal and Continuous Cooling Diagrams, G. Vander Voort (editor) ASM International, 1991, ISBN: 0-
87170-415-3.
3. Metallographer’s Guide: Irons and Steels, ASM International, 2002, ISBN:
4. Carbon Steel Handbook, Electric Power Research Institute (EPRI), Document 1014670, 2002.
5. Interpretation of the Microstructure of Steels, H.K.D.H. Bhadeshia, Link.
August 17, 2023 23

1018 and 4140 Microstructures

&
Lab Report 1 Discussion
MATSCEN 3331, AU23
September 18, 2023
Elvin Beach
Samples & Expected Microstructures College of Engineering
• Two types of steel

• AISI 1018 steel – low carbon steel
• AISI 4140 steel – low alloy (Cr & Mo), medium carbon steel
• Five unique thermomechanical processing conditions for each steel

• Annealed
• (samples of rolled 6.35mm nominal thickness steel purchased, annealed at OSU)
• Cold Rolled to a target of 40% reduction in thickness
• Cold Rolled to a target of 80% reduction in thickness
• Cold Rolled to a target of 80% reduction in thickness, then annealed
• Hot Rolled to a target of 40% reduction in thickness
• Hot Rolled to a target of 80% reduction in thickness
• Ten microstructures available for comparison
September 18, 2023 2

Expected Phases: 1018 & 4140 College of Engineering
• 1018
• Ferrite
• Pearlite
• 1018 is a low carbon steel so there should be more ferrite than pearlite
• What do you expect to see in Cold Rolled vs. Hot Rolled Samples?
• 4140
• Ferrite
• Pearlite
• Martensite
• 4140 is a medium carbon steel, it may have more pearlite than ferrite in some conditions
• Where would you expect to see Martensite in our set of samples?

Review: Hypoeutectoid Steel Microstructures College of Engineering
• Near equilibrium cooling

• Relatively equiaxed ferrite & pearlite
September 18, 2023 Reproduced from Elements of Metallurgy and Engineering Alloys . Images reproduced from Metallographer’s Guide: Irons and Steels, ASM International, 2002 4
Scale College of Engineering
• Why do we collect images at 200x, 500x, and 1,000x in this project?

• Set of optical micrographs from 1018 Annealed samples below.
200x original magnification 500x original magnification 1,000x original magnification

1018 Steel – Compare Annealed and CR µstructures College of Engineering
• Top row of micrographs is 200x and bottom row is 500x original magnification
Annealed Cold Rolled 40% Cold Rolled 80% Cold Rolled 80% + Anneal

• All micrographs are 1,000x original magnification

1018 Steel – CR & HR microstructures College of Engineering
• All images are 500x original magnification.
Hot Rolled 80%

Hot Rolled 40%
Cold Rolled 40% Cold Rolled 80%

1018 Steel – Annealed & HR microstructures College of Engineering
• All images are 1,000x original magnification
Annealed Hot Rolled 40% Hot Rolled 80%

• Top row of micrographs is 200x and bottom row is 500x original magnification

4140 Steel – Compare Annealed and CR µstuctures College of Engineering
• All micrographs are 1,000x original magnification

4140 Steel – CR & HR microstructures College of Engineering
• All images are 500x original magnification.
Hot Rolled 80%

Hot Rolled 40%
Cold Rolled 40% Cold Rolled 80%

4140 Steel – Annealed & HR microstructures College of Engineering
• All images are 1,000x original magnification
Annealed Hot Rolled 40% Hot Rolled 80%

Reporting & Writing College of Engineering
• Look through:
• Report Rubric
• Report Template
• Figure Template (not always, provided. Might be useful for this report though)
• Technical Writing Common Mistakes
• Time for Questions & Answers

What is Corrosion?
Corrosion occurs via two coupled electrochemical half cell reactions:
1. Anodic Reaction (oxidation): metal loses electrons

Fe  Fe2+ + 2e-
2. Cathodic Reaction (reduction): A species gains electrons

hydrogen/water reduction: 2H+ + 2e-  H2(g) (in acidic soln.)
typical
2H2O + 2e-  H2 + 2OH- (in basic soln.)
cathodic rxns
in natural
oxygen reduction: O2 + 4H+ + 4e- 2H2O (in acid soln.)
environments
O2 + 2H2O + 4e- 4OH- (in acidic soln.)
Corrosion of iron in acidic water, a simple example:

oxidation of iron: Fe = Fe2+ + 2e-
reduction of hydrogen ions: 2H+ + 2e- = H2 (g)
overall corrosion reaction: Fe + 2H+  Fe2+ + H2 (g)
3
Who Cares? Cost of Corrosion
• National Association for Corrosion Engineers (NACE) IMPACT study estimated

2013 global cost of corrosion to be US$ 2.5 trillion annually (3.4% of GDP)
• Use of available corrosion control practices could reduce cost by 15 to 35%
Corrosion costs cut by

300% by improving
corrosion control
strategies!
4
http://impact.nace.org/economic-impact.aspx
Who Cares? Our Nuclear Waste Legacy
spent
nuclear fuel
interim
storage
Yucca
Mountain
plutonium production
Repository,
waste tanks at Hanford
NV
Nuclear Reservation, WA
5
Who Cares? Oil and Gas
Sissonville, WV
Other components or structures susceptible to

catastrophic corrosion failures:
• Boilers • Turbine blades
• Submarines • Aircraft
• Power plants • Medical implants
• Bridges • Water lines
6
Who Cares? Columbus, Ohio
https://www.dispatch.com/news/20170728/photo-appears-to-show-crack-on-
rides-arm-grew-to-catastrophic-break 7
Who Cares? Flint, MI
• April 2014 Flint began using
Flint River as water source
without corrosion inhibitor
• Supply of improperly treated
water until 2015
• Elevated Pb levels in resident
blood and tap water
EPA action
level, 15 µg/L
http://www.materialsperformance.com/articles/material-selection-design/2016/06/the-science-
8
behind-it-corrosion-caused-lead-tainted-water-in-flint-Michigan
What is Corrosion?
4 Essential Elements of an
1. Anode
Electrochemical Cell
O2
2. Cathode Na+
OH-
Cl- e-
3. Electronic Path (metal) Cu+
Cu
4. Ionic Path (electrolyte)
9
Location of Anode and Cathode Areas and Relationship to Corrosion
Attack Patterns
The anodic reaction is most likely to occur

at the highest energy site.
This principle means that corrosion can

occur in different morphologies.
McCafferty Fig 2.5
uniform
Jones, Fig 1.4
Intergranular
pitting
dealloying
10
Jones, Fig 1.4
Electrode Potential: The Driving Force for Corrosion
The spontaneous separation of

charge across the metal/electrolyte
electrical double layer
interface, called the electrical double
- + layer, creates an electrostatic
- + potential difference across the
interface:
+ - + +
Electrode
+ - -
+ - + - -
+ - + + This potential difference is called the
+ -
electrode potential, E.
- + -
Bulk solution is
electrically neutral
~109 V/m!!
over 1 nm
11
Electrode Potential: The Driving Force for Corrosion
The electrode potential

( 𝑴 - 𝒔 ) is a driving force
for electrochemical reactions
Electrode Electrolyte charge
+
Each electrochemical ½ cell reaction has
a unique potential.
12
Standard Electrode Potentials: The Electromotive Force Series
The standard electrode potential, Eo, is a reversible half cell potential of a redox reaction
under standard state conditions*
*[redox ion species] = 1 M, P= 1 atm, T = 298 K 13

Measuring Electrode Potential
high impedance
voltmeter
E (V) ? E( - -
( - )
measured E
DL
Not feasible to measure

absolute electrode potential We can, however, measure relative
(potential drop): 𝑴- 𝒔 electrode potential:
Emeas = 𝑴𝟏 - 𝒔𝟏 𝑴𝟐 − 𝒔𝟐
- -( - ) 14
Measuring Electrode Potential: Reference Electrodes
Reference electrodes with a known electrode potential (fixed by a ½ cell reaction) are
used to measure the unknown potential of another electrode. -
Schematic of Ag/AgCl Reference Electrode

E (Vref) reference AgCl(s) +e−= Ag +Cl−
electrode
EAg/AgCl = +0.199 VSHE

E
measured
voltage or
potential metal/solution AgCl coated
potential drop
Ag wire
4 M KCl
solution
metal
porous frit
electrode
15
Electrode potential of a Freely Corroding Metal (Ecorr)
Corrosion potential (Ecorr): electrode potential of a metal that is corroding
freely* in solution
Ecorr (Vreference)
+ -
Corrosion potential is
R dependent on both
e environment and material
f factors:
e Na O
Na • chemistry (pH, composition)
r + 2
+
O • temperature
e
n Cl- Cl- H- e- • flow conditions
c • oxygen levels
Ecorr Cu+
e • material condition (e.g.,
strain, microstructure)
Cl-
Na Cu
+
17
*there is no net current flowing into or out of the electrode
Corrosion Potential: Tendency for Corrosion
Is this shipwreck in danger of corroding away?
Perth, Australia Uncovered area of wreck
James Mathews reclaimer Pre-1918 Pourbaix Diagram
Wreck Site dredge shoreline Fe-H2O, 298K
Fe3+
Fe2O3
Fe2+
Passive
Fe 2+
Corrosion
Fe3O4
Fe Immunity
Fe HFeO2-
Intern 
buried wreck location
19
Corrosion Potential: Tendency for Galvanic Corrosion
galvanic corrosion is corrosion damage resulting from connection of two dissimilar metals
Statue of Liberty:
Iron Armature, Copper Skin
Hot Water Heater
https://www.corrosion-doctors.org/Definitions/Galvanizing.htm
galvanized steel
20
Galvanic Series: Predicting Tendency for Galvanic Corrosion
Galvanic Corrosion Requirements:
1. dissimilar metals
2. electrically connected
3. ionically connected (share electrolyte)
Galvanic Series
Ordered list of corrosion potentials in a particular
environment (e.g., stagnant seawater at STP).
Golden Rule:
21
Module 3: Corrosion
Week 2
• What is localized corrosion?
• Passivity
• Passive film breakdown
• Forms of localized corrosion (pitting, intergranular)
• What microstructural features can cause local passive film breakdown?

• micro-galvanic precipitates, segregation of passivating elements, passive film
interruption
• How does localized corrosion propagate?

• Microstructural role (galvanic, passivating element segregation)
• Geometry role (pits and maintenance aggressive pit chemistry)
• Intergranular corrosion
• How does alloy composition and condition impact localized corrosion attack pathways
and severity?
1
Passivity
Passivity is a loss of electrochemical reactivity (drastic decrease in
corrosion rate) that many engineering alloys exhibit under certain
environmental conditions.
Passivation is typically the result of the presence of a thin protective oxide

or oxy-hydroxide passive film on the metal surface.
Sometimes a
Barrier oxide porous layer on
top
metal metal
Passive films are an oxide or precipitate layer that act as a mass transport
and charge transfer barrier between the metal and environment.
However, passive metals are susceptible to local breakdown and

accelerated localized attack. Cl- is a common catalyst for breakdown.
3
Passivity: Aluminum
Al-H2O Pourbaix Diagram
– Passive oxide layer (~1 - 10 nm)

forms spontaneously when Al is on
contact with water or water vapor
– Provides an excellent barrier to

metal dissolution.
4
Localized Corrosion  Localized Passive Film Breakdown
Localized corrosion is dissolution of small areas of a metal surface while other
areas remain intact (fixed anode). It is the result of local breakdown of an
otherwise protective passive film. Attack can occur at a rapid rate and be
extremely difficult to detect, with risk of catastrophic failure.
Some Forms of Localized Corrosion

Pitting – local dissolution leaving behind craters in the
metal surface.
Intergranular corrosion- preferential attack of grain

boundaries
Exfoliation- special type of IGC occurring between

elongated grains of extruded or rolled Al alloys
Effects of Localized Corrosion

Corrosion attack acts as stress concentrator;
lowers strain to failure, impact resistance
2
Microstrucural Heterogenieties can Interrupt Protective
Oxide Film and/or Create Microgalvanic Cells
Birbilis, 2006
Pitting around Al7Cu2Fe

inclusion in aluminum
7075-T651 matrix.
Inclusion is more noble
than surrounding matrix
(microgalvanic effect).
Goswami, 2012
A bright-field TEM
image showing
the β phase at the triple
point and grain
boundaries in AA 5083
after 90 days at 100oC.
Fe and Si rich inclusions interrupt
passive oxide film and serve as
preferential cathodes in
commercially pure aluminum
5
Pitting Corrosion
Pitting –local dissolution leaving behind craters in the metal surface. More
noble intermetallics in aluminum serve as preferential cathode areas that
support oxygen and water reduction reactions.
7
Pit Propagation Occurs by Maintenance of Aggressive Chemistry
Galvele, 1978 Al-H2O Pourbaix Diagram

pit depth, X
Men+ + H2O = Me(OH)(n-1)++H+

Me = Men+ + ne- Acidic Conditions
Extreme solution condition develops and
maintained inside “occluded” area
8
Localized Corrosion  Localized Passive Film Breakdown
Localized corrosion is dissolution of small areas of a metal surface while other
areas remain intact (fixed anode). It is the result of local breakdown of an otherwise
protective passive film. Attack can occur at a rapid rate and be extremely difficult
to detect, with risk of catastrophic failure.
Some Forms of Localized Corrosion

Pitting – local dissolution leaving behind craters in the
metal surface.
Intergranular corrosion- preferential attack of grain

boundaries
Exfoliation- special type of IGC occurring between

elongated grains of extruded or rolled Al alloys
Effects of Localized Corrosion

Corrosion attack acts as stress concentrator;
lowers strain to failure, impact resistance
10
Intergranular Corrosion
For most passive alloys, grain boundaries (GBs) are usually only slightly more
reactive than the matrix and general pitting corrosion results. However, under certain
conditions, corrosion of the GB region exceeds that of the matrix and intergranular
corrosion (IGC) occurs.
IGC is caused by heterogeneities at the GB’s:

– impurities or particles at GBs
– enrichment or depletion of an alloying element at GBs
Why care about IGC?
• extremely rapid rates of material

loss because of undermining and
falling-out of grains
• Significant loss in residual strength
• crack initiation – IG stress corrosion
cracking can occur in presence of
tensile stress
11
Al Alloy Exfoliation Corrosion
 Exfoliation is a form of IGC that occurs in wrought Al alloys, which have grains
elongated parallel to the surface.
 IGC can occur on the elongated grain boundaries.
 The corrosion product is more voluminous than the matrix and forces the layers
apart.
 Exfoliation is a form of self-induced SCC.
16
Localized Corrosion in Al-Cu Alloys: 2xxx
2xxx - Al-Cu
• Used for aircraft, rivets, hardware, truck
wheels where good strength and fatigue
performance required.
• Can handle elevated temperatures to 250 oC
• Heat treatable- precipitation hardened
Starke, 1996
Principal strengthening precipitates are Cu rich:

2024 • Guinier-Preston (G-P) zones
• Al2CuMg (S phase)
• Al2Cu (ϴ phase)
12
Localized Corrosion in Al-Cu Alloys: 2xxx
Copper-rich precipitates tend to
nucleate at dislocation structures Davis, 1999
(e.g., grain boundaries)
Grain boundary precipitates form in

the early stages of thermal treatment,
quenching or aging
Given the following corrosion potential ordering

(Ecorr), what phase is expected to dissolve?
EAl2Cu > EAl2CuMg > Ematrix > ECu-DZ
13
IGC in Al-Cu Alloys: Effect of Microstructure/Condition
2024
T351 uncorroded:
σy= 285 MPa Time and temperature of heat
σTS = 395 MPa
treatment, quench rate and
deformation processes, strongly affect
corrosion resistance and attack
morphology.
T42 uncorroded:
σy= 276 MPa
Processing that produces finer,
σTS = 427 MPa uniformly distributed precipitates is
generally favorable over production of
T851 uncorroded:
σy= 395 MPa
larger, contiguous precipitates.
σTS = 460 MPa
Davis, 1992 14
IGC in Al-Cu Alloys: Effect of Microstructure/Condition
2024
S-phase becomes coarser, more

contiguous with aging time.
15
Localized Corrosion in Al-Zn Alloys: 7xxx
7xxx - Al-Zn (-Mg-Cu)
• Some of the highest strength Al alloys. Used
in high performance applications for
• aircraft, vehicles, rivets, hardware, truck
wheels where good strength and fatigue
performance required.
• Corrosion and stress corrosion cracking is an
issue for certain tempers (e.g., T6)
Starke, 1996
Principal strengthening precipitates:

MgZn2 or Mg(Zn, Cu, Al)2 (η phase)
7075
Other typical constituent particles:
Mg2Si (7075)
Al2CuMg (S phase)
Al2Cu (ϴ phase)
10
Localized Corrosion in Al-Zn(-Mg-Cu) Alloys: 7xxx
Like 6xxx, can undergo pitting and/or IGC,
depending on processing conditions. η decorating grain boundaries in T6 condition
For 7075 T6 – pitting transitions to IGC with
slowing quench rates.
IGC associated with η (MgZn2 or Mg(Zn, Cu,
Al)2) and Cu-rich precipitates along grain
boundaries. Zn, Cu depletion in grain
boundary zones. Mechanism similar to 2xxx
Meng, J. Electrochem.
11 Soc., 2004
Localized Corrosion in Al-Mg-Si Alloys: 6xxx
6xxx – Al-Mg-Si
• Excellent corrosion resistance and moderate
strength. Used in marine, automotive,
aerospace, structural extrusions and other
applications where corrosion resistance,
weldability, machinability desired
• Heat treatable- precipitation hardened
• Si is added to promote Mg2Si. Small
amounts Cu added to further strengthen
Principal strengthening precipitates:

Mg2Si
6061
Other typical constituent particles:
Si (when Si in excess of Mg2Si mg/Si ratio)
Al5Cu2Mg8Si6 (Q phase), 0.8 wt% Cu
AlFeSi(Mn,Cu)
12
Mg2Si is anodic to the matrix Corrosion mode is temper dependent. Pitting is
in neutral chloride solutions: favored over IGC in material with finer and more
Ematrix > EMg2Si uniformly distributed second phase particles.
Other typical phases are cathodic Pitting IGC
to the matrix:
• Si
• Al5Cu2Mg8Si6
• AlFeSi(Mn,Cu)
Zander, Mat. & Des., 2015
13
Al–0.92Si–0.80Mg–0.001Cu (wt%)
small excess Si, negligible Cu
Corrosion morphology and < 5 μg/cm2/day < 5 μg/cm2/day
corrosion rates (mass loss) after
14 days exposure in 0.1 M NaCl
natural peak
Corrosion resistance
dependent on amount of Cu Al–1.26Si–0.37Mg–0.30Cu
and Si and aging condition. large excess Si, moderate Cu
10 μg/cm2/day 10 μg/cm2/day 6 μg/cm2/day
natural peak over

Al–1.05Si–0.53Mg–0.89Cu
large excess Si, high Cu
< 5 μg/cm2/day 7 μg/cm2/day
Liang et al., Corr Sci, 2013

under over 14
Environment Assisted Cracking (EAC) = corrosion + stress
For many structural alloys like Al, Ti, steel, and Mg; the environment (air
around us, salt water, wet winter roads, etc.) can cause corrosion to occur...
pitting intergranular exfoliation
AND cracks initiate and grow when not normally expected =

Environment Assisted Cracking (EAC)
A brittle fracture process that results from simultaneous exposure to stresses and
environments (electrolytes or gases) cause failure at stress/strain levels much lower than
expected → if environment was never present, there would be no cracking at given
stress(es)!
main issues when corrosion + stress: Stress Mat’l
1) Corrosion site → concentrate stress → crack to ini ate

2) ↓ me to ini ate a crack Environment
3) ↑ crack propaga on rates 15
EAC of Al-Zn-Mg-Cu Alloys: 7xxx
7079-T6 (now obsolete),

7075-T6, and 2024-T3 have
contributed to over 90% of
EAC service failures of
aluminum alloy products
https://airwaysmag.com/airlines/32-years-aloha-flight-243-accident/
16
Types of EAC
2 categories of EAC:
SCC CF
Static (either applied or residual) or very slowly Fatigue style stresses (cyclic or undulating through
rising stress a max and min that can vary)
Cracking at loads/stresses never expected and Crack growth below mechanical fatigue threshold
can be far below KC, σYS and σUTS when never expected
Crack growth at higher rates than expected for just
mechanical fatigue
CRACKING WHEN NEVER EXPECTED ACCELERATES MECHANICAL FATIGUE
DAMAGE
• Multiple stages: 1) crack initiation, 2) microscopic propagation, 3) macroscopic propagation

• Environment causes surface corrosion (pits or IGC fissures) which act as a stress concentrator
and can initiate a crack when mechanically a crack is not predicted
• Environment causes crack to propagate at an accelerated rate
• Time dependent
• Lower bound thresholds exist
• The two can interact with each other and occur in tandem
• Mechanisms driving argued and likely not just one (HEAC, anodic dissolution, film rupture)
***Note CF is different than corrosion followed by fatigue 17
A Note on Lab Tests versus Service
At what rate and to what extent will corrosion damage propagate?
Sun,Cor. Sci., 2011
Field
O3 RH Exposure
T Cl- years
NOx SOx Lab

Exposure
Environmental Corrosion
weeks Damage
Parameters
limited prediction capability, mechanistic insight lacking; development of

realistic accelerated tests and predictive models is a grand challenge
25

MSE 3331 Module 1 Lecture Metals Processing AU23

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MSE 3331 - Autumn Semester 2023

Materials Science and Engineering Lab I

Lecture 1. Introduction to Metals Processing

 Introduction to metals processing

 What is thermomechanical processing (TMP)?

Extrusion Centrifugal Bending Blow molding Boring Anodizing Automated

Metals processing Plastic processing

design pattern pouring casting 7

2,000 sf capable of casting ferrous and non-ferrous metals

 280 ton LK Die Casting Cell – Al and Mg

 ACRC is dedicated to collaborative research in metal processing and manufacturing through a

Material Producers Casters

 Thermomechanical Processing (TMP) is solid-state metals

Metal Forming Processes

Bulk Forming Processes Sheet Forming Processes

• Spatial workpieces (3 dimensional) • Planar workpieces (2 dimensional)

Forging , Rolling, Extrusion, Drawing

C-Steel 550oC tin 0 to 40oC

Pure-Al 290 to 300oC zinc 50 to 100oC

Dur-Al 360 to 400oC Mo 870oC

Lead -50 to 50oC Ni 400-600oC

Before forming After forming

Module 1: Themomechanical Processing

Rolling, Heat Treating, Hardness

August 17, 2023 1

• Definition: “THERMOMECHANICAL PROCESSING (TMP) refers to various metal forming

• THERMOMECHANICAL PROCESSING (TMP) refers to various metal forming processes that

August 17, 2023 2

• Cast metals undergo TMP to

August 17, 2023 3

August 17, 2023 Link: Roll Forming Processes 4

HOT ROLLING COLD ROLLING

August 17, 2023 5

August 17, 2023 6

• Camber occurs when rolls are not ground properly.

August 17, 2023 7

August 17, 2023 8

• The upper schematics show the material undergoing reduction.

August 17, 2023 9

August 17, 2023 10

• Used in both hot rolling and cold rolling operations.

August 17, 2023 https://www.tmeic.com/application/cold-mill-systems 11

• Steels are in the low carbon range of

Heat treating is a critical process step in

just the example we are working with.

August 17, 2023 12

August 17, 2023 13

ASM Handbook Volume 11

• Homogenization (Non-ferrous Alloys)

August 17, 2023 15

August 17, 2023 16

- Stress Relief Anneal

August 17, 2023 17

• Hardending (specifically austenitizing and quenching) – not surface hardening

• Heating the material above A3 and holding to fully convert to austenite

• The selection of austenitizing temperature, time, transfer to quenchant, type of quenchant

August 17, 2023 18

August 17, 2023 19

August 17, 2023 21

• Carbide: cementite (Fe3C)

• Ramp: heating or cooling rate in a heat treating process

• Soak: dwell time or the time at a given temperature