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MatE 25

San Jose State University

Lab Notes

Chapter 7: Steel Processing 1


Processing and Microstructure
1.0 Learning Objectives
After successfully completing this laboratory workshop, including the assigned reading, the lab
worksheets, the lab quizzes, and any required reports, the student will be able to:

List the phases in steel (austenite, ferrite, pearlite, cementite, and martensite), what
temperatures they are stable at, and their mechanical properties.
Describe the influence of tempering, annealing, and quenching on the mechanical
properties of steel.
Identify ductile and brittle fractures.
Use standard heat treating equipment and methods.
Operate the notch-impact testing machine.
Demonstrate the relationship between heat treatment and mechanical properties.

2.0 Resources
[1].
Callister, Materials Science and Engineering: An Introduction 8th edition, (John Wiley
and Sons, New York, 2009), Ch 9.18-9.20, 10.1-10.9.
[2] Industrial Heating articles on Martensite and Retained Austenite
http://www.buehler.com/application_support/MartensiteRetainedAusteniteIHApril2009.pdf

3.0 Materials Applications


Steel is an alloy of iron, carbon, and small additions of a variety of other elements. Steel is one of
the most versatile engineering materials, and is used in a wide variety of structural applications.
There is an abundant supply of iron ore distributed in many locations in the world. Also iron and
steels are readily recyclable, a very important property in material selections. The technology for
reusing iron and steel is making great progress and is a current subject of research in many
universities and industries worldwide.
Some of the key properties that make steel so versatile are high strength and toughness. There
are many alloys of steel, and there are many processes for steel production that enhance the
properties to suit design needs. Processes must be done very carefully to achieve the desired
results, and we will explore one such process in this lab exercise.
One application where steel is used is amusement park rides. This brings us to our accident
investigation.

4.0 The Big Twist Problem


During a recent spring weekend, an accident involving an equipment failure at an amusement
park in Florida set in motion a chain of events that involves you in an investigation to learn the
root cause of the equipment failure and to prevent a reoccurrence of the accident at a similar park
in the local area.
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San Jose State University

Lab Notes

In Florida a new ride called The Big Twist went into service in early spring of 2010. After
about eight weeks of operation, the warming weather and school spring break brought a line of
eager riders resulting in full carloads of riders and full capacity operation of the ride. The Big
Twist raises a car with eight riders to the top of a 60 meter tower from which the car runs down a
twisting and looping track for one and a half minutes. This feature giving the ride its name, Big
Twist, involves a fast descent in a tightly curled helical section of the track involving six
complete circles of 360 degrees each in a path having a diameter of about 7 meters.
On the day of the equipment failure, at about 2:15 p.m. one of the cars separated from the track
about midway down the twist. The car and eight occupants fell to the ground about 30 meters
below. Two of the occupants were killed immediately, two died later at the hospital and the other
four suffered a range of non-fatal injuries, some of which will result in permanent disabilities.
Florida officials immediate shut down the ride and began an investigation to determine the cause
of the car separating from the track. Investigators determined that the sharp descent in the helical
twist would place high side loads on the wheel mechanisms in addition to the normal vertical
loads. Even with the impact damage from the 30+ meter fall, it was determined that the outside
track wheel assembly was inclined at more than 30 degrees from its normal vertical orientation.
This was due to bending of the support bracket rail that connected the wheels to the underside of
the car.
When the Director of Safety for Cal-OSHA received report of the Florida amusement park
accident, she quickly determined that three such rides of similar design had been installed in
California during the winter and all three had been inspected and certified to start operation
within the past three weeks. She immediately issued an order shutting down those three rides.
She ordered another inspection, and ordered the rides closed until there was a determination of a
cause for the equipment failure. Of the three California locations, two were in southern
California and one in the San Jose area. Teams of inspectors were dispatched to each of the sites
with instructions to inspect the cars and all associated equipment. Particular attention was to be
given to the condition of the wheel assemblies and support rails. Within 12 hours the reports
came back from southern California that the inspectors found no problems. However, the team in
northern California reported wheel assemblies tilting 10-15 degrees from the normal orientation
and bending of the support rails on the left side on 3 out of 24 cars at the site.
The park management at the two southern California parks requested lifting of the order shutting
down their rides. They tell the Director of Safety that since the inspection team found no
problems, they should be allowed to resume operations. The Director refuses to lift the stop
order. She still wants to find the root cause of the Florida crash, and her concern escalates when
she receives the report of the problem found on the northern California ride. However, she
mentions in a staff meeting that the pressure to lift the order will intensify as the weekend
approaches and the parks anticipate capacity crowds.

5.0 Failure Investigation


5.1 Your Job
You have been selected by the Cal-OSHA Safety Director to be part of a team of experts to
investigate the wheel assemblies and bent rails discovered both in Florida and California.

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Lab Notes

As a materials engineer, you are asked to determine why the Florida roller coaster failed, and if
the other coasters are at risk. As part of your investigation, you study how the microstructure and
hardness of steel changes with thermal processing. As a first step, you obtain reference samples
of 4140 steel. You austenize, quench, and temper a series of these samples to gain an
understanding of how the microstructure, hardness, and notch-impact toughness change as a
function of quench and tempering temperature. You then need to apply that knowledge to a bent
rail sample to determine if the hardness, toughness, and microstructure match what should be
expected.
5.2 Investigation To Find the Facts
To start in the investigation, you arrange a conference call with representatives of the company
that designed and manufactured the ride. During the call you make notes about the material
details mentioned by the designers. From your notes you plan the tests to be performed once the
suspect rail is received.
1. The designer says that this ride is a new model based on a previous design in use for
several years. The previous model is smaller. It makes loops and turns but less sustained
twisting motion, such as the helical drop that is a new feature introduced for this ride.
2. The designer identified that the wheel assembly could disengage from the track if the rail
bends enough to allow the wheel shaft to tilt more than 15 degrees from its normal
horizontal direction.
3. Calculations made during design, indicate this new ride will generate higher side loading
of the wheel assembly and rail. Because of the higher expected loads a stronger wheel
assembly rail was needed.
4. To handle the higher loads, it was decided to make the rail out of a higher strength
material, keeping the dimensions the same as for the older car design. This avoided a
redesign of other portions of the car.
5. In the previous car design, the rails were made of low carbon steel with commercial
designation of 1018 steel. The material specification called for the finished rail to have a
Rockwell B-scale hardness of HRB 75-85 (which is roughly equal to HRC 2-3).
6. For the new ride design, the design team specified a change to a medium carbon steel
(4140), which gives the material higher strength than the previously used 1018 steel if
processed correctly.
7. This company has now built more than a hundred cars using this design. Manufacturing
the new wheel assembly and rail was complex. After machining to dimensions, rails were
sent out to another shop in batches to be heat-treated. The process involved heating to
844oC for 1 hour followed by water quench, then post-quench tempering for 1 hour at
480oC. Parts were then cleaned of surface scale by grit blasting. The material
specification called for a final Rockwell C-scale hardness of HRc 35-40.
8. The designer and his supervisor say they have rechecked the loading calculations, and
both say the wheels and rail should be safe under the maximum expected loads plus
design margin, provided the rail material is at least 0.40 wt% carbon and the rail received
the specified heat treatment.
9. Your investigation team finds that the first car manufactured with the new design has a
complete record of all the testing done on the materials and components that go into

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Lab Notes

making the car, and everything passed. After that, all the subsequent cars do not have
records of material tests during manufacturing.
10. You participate in an investigation team traveling to Florida, and obtain a small specimen
of the bent rail from the crashed car, and bring it back to your lab in California. The CalOSHA machine shop makes that specimen into a notch-impact toughness Charpy test
sample. You perform hardness tests, and a Charpy test on this sample. You then cut and
polish a section for microscope examination, and take photographs of the microstructure
to document your investigation. A small portion of the retrieved bent rail specimen was
sent to a chemical analysis lab to determine the element content of the steel.
From the data you gather from the reference samples, and the data from the retrieved bent rail
specimen, you are able to piece together the problem. Your data eliminates all other potential
causes, and you are able to determine conclusively the root cause of the. Further, you are able to
recommend additional testing to determine which of the roller coaster cars, if any, should be
allowed to return to operation.
Most importantly, now you need to document your results and send the report to the Director for
her review. She is under pressure to issue a ruling on operational status for the amusement parks,
and needs these results immediately. Also, almost certainly other safety organizations, and
litigation teams will question her ruling. The report must be of high quality and have technical
accuracy.

6.0 Writing Assignment - Engineering Report with Cover Memo


6.1 The Audience
The Cal-OSHA Safety Director, Ms. Irene Huang, has a bachelors degree in Industrial
Engineering, and an MBA. She deals with all types of safety issues and engineering problems,
but is not very familiar with specific materials tests and their interpretation. Assume Irene is
familiar with general engineering concepts, but not necessarily an expert in material properties
and failure modes.
6.2 Length and Time Guidelines
The length should be sufficient to cover the details requested below, and to demonstrate your
understanding of the concepts we discussed in class.
The assignment is to write both a Cover Memo and an Engineering Report.
6.3 Cover Memo (maximum of 1 Page)
It is recommended you write the cover memo after completing the report. That way, you can
select salient points out of the report and write 2-3 sentences on each item shown here. Each of
these should be a separate paragraph.

Introduce your purpose for writing by reminding Irene what you did and why.
Summarize your research and findings.
Explain the significance of the results by stating what caused the failure.
Give a recommendation as to whether the rides can safely be put back in operation. If not,
state what should be tested first to determine if the cars are safe.

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Steel Processing and Microstructure 1

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Lab Notes

6.4 Engineering Report


Write at an appropriate level of detail for your audience. Write in your own words.
6.4.1

Introduction
State why you did the research
Briefly explain relevant materials engineering concepts:
o Amount of carbon in 4140 steel compared to 1018 steel and what effect that has
on strength
o Phases of steel at various temperatures, as shown on the phase diagram, and how
that effects the amount of carbon that can be held interstitially
o The austenite to martensite transition, including the importance of fast quench
o The process of converting martensite to tempered martensite, and the effects on
strength, hardness, and toughness.

6.4.2 Experimental Procedure


Describe what processing you did to prepare some reference samples.
Describe the mechanical tests you performed on the reference samples.
Describe how this compares with the design specifics for the manufactured car.
Describe the tests you performed on the retrieved sample.
Describe what you did to prepare the reference samples and the retrieved sample for
microscope examination.
6.4.3

6.4.4

6.4.5

Results and Discussion


Present your results from the experiments you ran on both the reference and retrieved
samples. Remember to show results in properly formatted tables and/or graphs.
Answer how the retrieved sample compare to the reference samples in hardness and
Charpy tests.
Answer how did the retrieved sample compare to expected results under microscope
examination. What was the microstructure you observed?
What did the chemical analysis indicate, and was that expected. Describe if that indicates
a possible causes of the failure.
Conclusions and Recommendations
From the tests and observations you made, state the processing treatment the suspect rail
received in manufacturing. Explain how that would cause the rail to have the properties it
did and how that caused the failure.
What is your recommendation to the Cal-OSHA Safety Director concerning reopening
the California rides?
If you suspect some cars are safe and some at risk, how do you recommend finding the
cars that are not safe so they can be taken out of service and repaired?
References
List all references you consulted to write this report. Use the proper format.

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Lab Notes

Grading Rubric

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Scoring
Attribute
Writing Mechanics
Assignment Instructions
and Requirements

1
Unacceptable

San Jose State University


1.5

2.5

2
Marginal

Lab Notes
3
Proficient

3.5

4
Excellent
Wt
1

Assignment instructions not


followed

Some assignment
instructions followed

Most assignment
instructions followed

Report fully complies with


instructions & requirements

Grammar, mechanics and


spelling

Consistently inadequate
grammar, mechanics and/or
spelling;
Errors impair meaning

Many errors, which affect


writing clarity

A few errors, which do not


impair meaning

Consistently correct use of


grammar, mechanics and
spelling

Figure and Table Format


and Quality

Figures/tables consistently not


labeled or not referenced in
text

Some figures/tables missing labels, missing descriptive


captions, not referenced and/or not discussed in text

All figures/tables neatly


labeled with title, figure no.
and descriptive caption,
discussed, explained in text

Units and Significant


Figures

No units given for any table


headings, plot labels or
values; or wrong number of
significant figures

Some table headings, plot labels or values missing units


and/or wrong number of significant figures

Tables formatted correctly,


with all table heading;
Plot labels and values given
with correct units and
significant figures

Formulas

All symbols and formulas


written by hand

Some symbols and formulas handwritten or


word-processed

All symbols and equations


written with equation editor
and mathematical notation;
All variables defined, all
equations numbered

Writing Quality
Writing Quality

Originality

Scoring
Attribute

Organization lacks coherency;


Language and sentence
structure is poor;
Report is difficult to read

Writing is plagiarized from


other sources*
1
Unacceptable

Rev. 4.0

Overall organization is
coherent;
Language and sentence
structure is sophisticated;
Report is easy to read and
understand
Author restates or paraphrases ideas from other sources;
Writing is original, shows
Writing does not clearly demonstrate authors
clarity, and demonstrates
understanding
depth of understanding
1.5
2.5
3
3.5
4
2
Proficient
Excellent
Marginal
Organization of some sections is coherent;
Language and sentence structure is average;
Report requires some effort to understand

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Technical Quality
Mastery of Theoretical
and Technical Concepts

San Jose State University

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Wt
3

Author appears to lack


comprehension of subject
matter

Author demonstrates some comprehension of subject


matter

Comprehension of subject
matter is clearly
demonstrated

Methods

Experimental methods not


described

Experimental methods are


difficult to understand

Experimental methods
described using specific
terms and procedures, but
general method is unclear

Experimental methods
described and explained;
Appropriate technical
language and level of detail
is used

Figure(s) of Experimental
Set-up

No figure of experiment
set-up

Generic figure of
experimental setup, but
relevant details omitted

Detailed figure of
experimental setup;
Figure not related to text

Detailed figure of setup,


Figure complements text;

Data,
Presentation, and
Calculation of Results

Result of the work not stated


or unclear;
Calculations not shown;
Results incorrect

Partial or incomplete
results of the work

All required results


present;
Calculations presented

All required results clearly


presented, distinguished
from data, and correct;
Calculations clearly
demonstrate how results
were determined

Discussion of Results

Results presented but not


explained

Results presented and


compared to theoretical or
expected values

Results presented and


compared to theoretical or
expected values;
Appropriate sources of
error are stated

Results interpreted in terms


of theoretical or expected
values;
Sources of error discussed
and explained

Conclusions

No summary given

Results summarized, but


no outcome stated

Report summarized and


outcome stated

Report summarized; opinion


stated concerning outcome
supported by work

References

Sources not cited

Some sources cited;


Common format not used

Sources cited, using


appropriate format (ie IEEE)

Total Rubric Score:__________out of 100


*

Note that any plagiarism will result in a 0 on the entire report. If you are unclear on what constitutes plagiarism, consult our instructor.

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7.0 Background on Steel Processing


The range of properties produced by alloying and by applying various heat treatments is
extensive. The initial step in the heat treatment of steel involves heating to a temperature at
which all of the carbon in the alloy goes into solution by dissolving interstitially in the facecentered cubic (FCC) iron. Austenite is the name of the elevated temperature FCC crystalline
iron. The maximum level of carbon solubility in austenite is about 2.0 wt%. The process of
dissolving carbon in austenite is termed austenitizing. This is shown on the Fe-C phase diagram,
in Callister Figure 9.24. High hardness is then achieved by rapidly cooling the steel to room
temperature by quenching it in water (or oil).
The body centered cubic (BCC) iron is called ferrite, and the solubility limit of carbon in is only
about 0.025 wt%. It is this large difference in carbon solubility between austenite and ferrite that
is primarily responsible for the range of properties available in steels. When there is insufficient
time for the redistribution of carbon in cooling austenite, a metastable phase called martensite
forms. Martensite is a crystalline arrangement intermediate to the FCC and BCC structures; see
Callister Figure 10.20. The carbon, locked in during rapid cooling of austenite, distorts the
martensite lattice. This causes internal stress in the crystal structure. The grain size for martensite
is very small. As a result, martensite formed upon rapid cooling is an extremely hard and brittle
material. Quenched martensite is of limited use as an engineering material because it is so hard
and brittle.
Toughness, and therefore the usefulness, of quenched steel is greatly improved through a process
called tempering. Diffusion of carbon and iron atoms is increased in a controlled manner by
tempering. Some of the distortion of the martensite crystal structure is reduced, and some of the
carbon moves out of the trapped interstitial positions. Since tempering is adjusted by time and
temperature controlling the diffusion, a large range of strength and toughness is possible. The
properties of steel thus can range from extremely hard and brittle (un-tempered martensite) to
very soft and ductile (annealed) which has a predominantly ferrite microstructure. Tempering
never goes above the Eutectoid temperature (727C), where austenite will reform.
7.1 The Heat Treatment of Steel
Alloys are heat-treated to improve or tailor mechanical properties. In steel there are many
potential heat treatments for accomplishing this. In this experiment we examine a few of the
general principles.
Understanding heat treatment processes begins with the concept of an equilibrium state, the state
for which the total free energy of the system is at a minimum, and thus the net change with time
in the system is nil. A phase diagram, such as Callister Figure 9.29, shows the equilibrium phases
predicted at given temperatures and compositions. However, phases not predicted by the
equilibrium diagram can appear during heat treatments. These are metastable phases, and they
will eventually transform to the equilibrium phases, if given sufficient time and/or temperature.
(Diamond at atmospheric pressure and room temperature is an example of a metastable phase
that persists for an extremely long time.) The time and temperature dependent transformation of
martensite to the equilibrium ferrite plus carbide phases provides the engineer a broad range of
mechanical properties from extremely hard and brittle, to very soft and highly ductile.

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7.2 Hardening of Steel


First consider the equilibrium heating and cooling of a 0.77 wt% carbon steel. As shown in the
iron-carbon phase diagram (Callister Figure 9.24), one can see that an alloy of iron and carbon
containing 0.77 wt% carbon heated long enough above 727C will become a single phase solid
solution of carbon in gamma (FCC) iron. Upon slow (equilibrium) cooling, a eutectoid reaction
occurs at 727C. The gamma phase decomposes completely into two new solid phases, alpha
Ferrite (BCC) and Fe3C (cementite). Both phases are stable below 727C. The resulting structure
consists of a lamellar mixture (alternate plates) of the two phases, which is referred to as pearlite.
This is a low strength, soft, ductile structure capable of being machined or shaped relatively
easily. Very slow (many hours) furnace cooling of steel from the austenite region produces
coarse pearlite. If steel is transferred from furnace to air, more rapid cooling occurs and finer
pearlite is produced. This can be seen in Callister Figure 10.15. Aside from being easily
machined and formed, pearlite steel is not used as a structural material because of low strength.
If carbon steel is heated to the fully austenite phase and is rapidly quenched, then there is
insufficient time for the carbon to diffuse out of the FCC interstitial positions, and there is
insufficient time for full conversion of FCC crystal to BCC. The resultant crystal is martensite
with a Body Centered Tetragonal (BCT) structure. If the cooling was rapid enough the structure
is fully martensite, which is a metastable phase, and very little (if any) alpha Ferrite or Fe3C is
formed.
Martensite has very high strength, but is also very brittle with low toughness. This is because the
crystal slip planes have little mobility. Slip plane motion is constrained because Martensite grain
size is small, the carbon is still held in the interstitial sites causing distortions, and the crystal is
BCT, which has fewer slip planes. The as-quenched martensitic structure steel is too hard and
brittle for practical engineering applications.
7.3 Tempering of Steel
A process known as tempering is necessary to restore some ductility and toughness to the rapidly
quenched steel. Heating martensite to some temperature below 727C allows some of the carbon
to diffuse out of interstitial positions, where it combines with iron to form carbides (Fe3C). A
mixture of cementite and ferrite results, with the effect being reduced distortion caused by the
carbon atoms being trapped. At the same time the grain sizes increase, and some of the BCT is
transformed to BCC. All of this increases slip plane mobility in a gradual and controlled manner.
This decreases the strength of the steel, but with a substantial increase in ductility and toughness.
Notice the drop in hardness with tempering shown in Callister, Figure 10.32.
On a microscopic scale the grain size of tempered martensite increases only a small amount and
the appearance is similar to that of un-tempered martensite, if the tempering is done correctly.

8.0 Austenitizing and Tempering Carbon Steel


8.1

Equipment and Materials


Hardening and tempering furnaces
Charpy impact testing machine
Quenching tank
Standard V-notch Charpy impact specimens

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Steel Processing and Microstructure 1

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Lab Notes

Abrasive paper

8.2 Safety Precautions


Do not use Rockwell hardness tester until you have received instructions. Be sure specimen is
firmly seated, and that test and base surfaces are flat and free of scale.
Stand to the side and away from the front of Charpy machine while testing. Eye protection must
be worn, and you must have a second person watching and verifying safety procedures are
followed.
8.3

Procedures
1. Check to see that furnaces are at proper temperatures. The austenitizing furnace
temperature should be at set 844C. Place 6 specimens in the furnace for one hour.
2. Remove 5 specimens from the austenitizing furnace and immediately quench in water.
Remove one specimen and allow to air cool.
3. Set tempering furnaces at 205C, 370C, 482C, and 677C. Place a quenched specimen
in each furnace for one hour. One quenched specimen does not get tempered, but is left as
full martensite.
4. Remove tempered specimens from furnaces and allow cooling. Remove surface scale on
two parallel longitudinal faces that do not have the notch.
5. Measure Hardness Rockwell C Scale (4 places each specimen) on each of the four temper
treatment specimens, the one air-cooled specimen, and the one as-quenched full
martensite specimen. Test hardness on one face only.
6. Perform Charpy Impact Tests for each of the six specimens. For operation of the Charpy
Impact Tester follow these steps:
o Lift pendulum to safety catch.
o Put specimen in place with notch away from pendulum.
o Lift pendulum to uppermost position.
o Manually move pointer to far left reference mark on the scale.
o Release hammer and take reading on scale.
7. Note the appearance of the fracture surfaces, and if available take pictures.

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Steel Processing and Microstructure 1

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Lab Notes

Worksheet 1: Tempering of Steel


Key Member (Encourages all team members to participate, ensures everyone understands the material, and
organizes/divides the tasks amongst the team members):
Other Group Members:
This week you austenize, quench, and temper steel samples to determine hardness and other
properties for reference samples. Next week you will test a retrieved sample of steel from the
wheel assembly failure, and compare with the reference sample results.
Reference Sample Results: Type of Steel ______________
Treatment
Air-Cooled,
No Temper
As-Quenched,
No Temper
Quenched,
205C Temper
Quenched,
370C Temper
Quenched,
482C Temper
Quenched,
677C Temper

HRC#1

HRC#2

HRC#3

HRC#4

Avg.
RC

Impact
Energy (J)

Type of
Fracture

1. What process will result in a Ferrite plus Pearlite microstructure? List the reasons why this
structure will have low strength.
2. What process will result in a Martensite microstructure? List the reasons why this structure
will have high strength.
3. What is happening to the microstructure during the temper process?

4. For 4140 Steel, how many iron atoms per carbon atom are there? Show work neatly on back.
5. What are your sources of error?
6. Did you calibrate the HRC? Did you calibrate the Charpy?

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