Grain Growth Kinetics in Steels

Project Number: RDS 21381
Grain Growth Kinetics in Steels

A Major Qualifying Project Report
Submitted to the Faculty
of the
WORCESTER POLYTECHNIC INSTITUTE
In partial fulfillment of the requirements for the
Degree of Bachelor of Science
in Mechanical Engineering
Submitted by:
Erik Khzouz
________________
Date: April 28, 2011

Approved:
__________________________
Professor Richard D. Sisson Jr.
Abstract
The effects of temperature and time on the grain growth kinetics of selected steels have been
experimentally determined. The steels examined are 1045, 4140, 4340, 8620, 9310 and 52100. Samples
were heat treated at temperatures ranging from 850C to 1050C in increments of 50C and held for 30
minutes, 2, 4, and 9 hours. Using the standard ASTM test methods to measure grain size it was found
that grain growth exhibited parabolic behavior and the activation energy for grain growth ranged from
175.2 to 353.4 KJ/mol.
II
Acknowledgements
I would like to thank Professor Richard D. Sisson Jr. for his advice and guidance throughout the
duration of this project. I would also like to thank Dr. Boquan Li, Adam Sears for their assistance in
ensuring that I had the necessary equipment and training to complete this project. In addition I would
like to thank George F. Vander Vort for his assistance with the etchant for revealing prior austenite grain
boundaries. Lastly, I would like to thank the following graduate research students: Danielle Belsito,
Chun-Min Chou, Guannan Guo, Zhijia Jin, Wendi Liu, Sidath Wijesooriya and Lei Zhang for their
experimental and analytical support.
III
Table of Contents
Abstract ......................................................................................................................................................... II
Acknowledgements...................................................................................................................................... III
List of Figures .............................................................................................................................................. VII
List of Tables .............................................................................................................................................. VIII
List of Equations ........................................................................................................................................... IX
1 Introduction ............................................................................................................................................... 1
2 Literature Review ....................................................................................................................................... 2
2.1 Heat Treatment ................................................................................................................................... 2
2.1.1 Austenitizing................................................................................................................................. 2
2.1.2 Tempering .................................................................................................................................... 4
2.2 Grain Size and Growth ........................................................................................................................ 5
2.2.1 What is Grain Growth?................................................................................................................. 5
2.2.2 Factors Affecting Grain Growth ................................................................................................... 6
2.3 Materials ............................................................................................................................................. 7
2.3.1 AISI 1045 ...................................................................................................................................... 7
2.3.2 AISI 4140 ...................................................................................................................................... 7
2.3.3 AISI 4340 ...................................................................................................................................... 8
2.3.4 AISI 8620 Steel............................................................................................................................. 8
2.3.5 AISI 9310 Steel ............................................................................................................................. 8
2.3.6 AISI 52100 .................................................................................................................................... 8
2.3.7 Material Composition .................................................................................................................. 8
3 Methodology ............................................................................................................................................ 10
3.1 Furnace Calibration ........................................................................................................................... 10
3.1.1 Temperature Mapping ............................................................................................................... 10
3.1.2 Temperature Calibration............................................................................................................ 10
3.2 Heat Treatment Procedure ............................................................................................................... 11
3.3 Sample Preparation .......................................................................................................................... 13
3.4 Optical Microscopy Measurements .................................................................................................. 13
3.4.1 Hyen Intercept Method ............................................................................................................. 13
IV
3.4.2 Jefferies Method ........................................................................................................................ 14
4 Results and Discussion ............................................................................................................................. 17
4.1 Gain Size Evolution............................................................................................................................ 17
4.2 Average Grain Diameters .................................................................................................................. 18
4.3 ASTM Grain Size ................................................................................................................................ 19
4.4 Effective Time ................................................................................................................................... 19
4.5 Ideal Grain Growth ............................................................................................................................ 21
4.5.1 Evaluating K and D0 .................................................................................................................... 21
4.5.2 Evaluating Activation Energy ..................................................................................................... 23
5 Conclusions & Recommendations ........................................................................................................... 25
5.1 Heat Treatment ................................................................................................................................. 25
5.2 Sample Preparation .......................................................................................................................... 25
5.3 Average Grain Size Measurements ................................................................................................... 25
5.4 Growth Kinetics ................................................................................................................................. 26
Works Cited ................................................................................................................................................. 27
Appendix 1: Isothermal Transformation Diagrams..................................................................................... 29
Appendix 2: Sample Grinding & Polishing Procedures ............................................................................... 32
Mark V CS600 - Sectioning ...................................................................................................................... 32
Beuhler Simplimet II Mounting ............................................................................................................ 33
Appendix 3: Sample Etching Procedures .................................................................................................... 34
Appendix 4: Jefferies Planimetric Method Calibration Studies .................................................................. 35
Calibration Study #1 ................................................................................................................................ 35
Calibration Study #2 ................................................................................................................................ 37
Appendix 5: Average Grain Diameters........................................................................................................ 39
Appendix 6: Effective Time Results ............................................................................................................. 44
Appendix 7: D2 vs. Effective Time Graphs ................................................................................................... 60
AISI 1045 ................................................................................................................................................. 60
AISI 4140 ................................................................................................................................................. 63
AISI 4340 ................................................................................................................................................. 66
AISI 8620 ................................................................................................................................................. 69
AISI 9310 ................................................................................................................................................. 72
V
AISI 52100 ............................................................................................................................................... 75
Appendix 8: Log(K) vs. 1/T Graphs .............................................................................................................. 78
Appendix 9: Micrographs ............................................................................................................................ 81
AISI 1045 ................................................................................................................................................. 81
AISI 4140 ................................................................................................................................................. 92
AISI 4340 ............................................................................................................................................... 103
AISI 8620 ............................................................................................................................................... 114
AISI 9310 ............................................................................................................................................... 125
AISI 52100 ............................................................................................................................................. 134
VI
List of Figures
Figure 1 - Temperature vs. Time Plot of Solution and Precipitation Heat Treatments [4] ........................... 2
Figure 2 Fe3C Phase Diagram [2] ................................................................................................................ 3
Figure 3 - Isothermal Transformation Diagram Fe-C Alloy of Eutectiod Composition [1] ............................ 4
Figure 4 - Comparison of Thermocouple Connections [12] ........................................................................ 11
Figure 5 - Heating Rate of 8620 to 900C ..................................................................................................... 12
Figure 6 Time-Temperature Graph of 900C Heat Treatment ..................................................................... 12
Figure 7 - Heyn Intercept Method at 200x Magnification: 1045 850C 9Hr ................................................ 14
Figure 8 - Jefferies Method at 200x Magnification: 1045 850C 4Hr ........................................................... 15
Figure 9: Variation in Grain Size of AISI 4140 with Time at 1050C ............................................................ 17
Figure 10: Variation of Grain Size of AISI 4140 with Temperature at 2 Hours ........................................... 18
Figure 11: Plot of Average Grain Diameter squared vs. Effective Time ...................................................... 21
Figure 12 - Log(Kp) vs. 1/T Comparison ...................................................................................................... 23
VII
List of Tables
Table 1 - Material Composition Obtained via OES ........................................................................................ 9

Table 2: Functions of Alloying Elements [12] ................................................................................................ 9
Table 3: Average Grain Diameter (mm) for AISI 8620 Steel ....................................................................... 19
Table 4: Comparison of K and D0 for Various Alloys ................................................................................... 22
Table 5 - Comparison of Activation Energy and Pre-exponential constant ................................................ 24
VIII
List of Equations
Equation 1- Hall-Petch Equation ................................................................................................................... 5

Equation 2 - Ideal Grain Growth Law ............................................................................................................ 5
Equation 3 - General Grain Growth Law ....................................................................................................... 6
Equation 4 - Relationship between K and Heating Temperature T .............................................................. 6
Equation 5: Zener Equation [10] ................................................................................................................... 7
Equation 6: ASTM Grain Size Equation ....................................................................................................... 19
Equation 7: Heating Time Equation ............................................................................................................ 20
Equation 8: Effective Time Equation........................................................................................................... 20
IX
1 Introduction
Steels are utilized in a wide variety of applications ranging from automobiles, bolts, to structural
components, etc. The addition of alloying elements within low, medium and high carbon steels leads to
enhanced mechanical properties over traditional plain carbon steel. Alloying elements that are added
within the steel can include: chromium, manganese, molybdenum, nickel, phosphorous, sulfur and
silicon. [1] In the past, researchers have noted significant changes in the microstructure of steels that
undergo alloy element addition to enhance the desired mechanical properties. As grain size increases,
the strength, hardness and fatigue life of the steel decrease. [3] It was observed that the prior austenite
grain size is directly influenced by the temperatures and the various time durations of exposure.
Austenite grains grow at elevated temperatures which can affect mechanical properties. Grain growth is
dependent upon heat treatment time and temperature as well pinning effects of second phase
precipitates within the steel.
The goal of this project is to investigate the effect of temperature and time upon the grain
growth kinetics of selected steels. The steels examined included 1045, 4140, 4340, 8620, 9310 and
52100. Heat treatment temperature and time were varied ranging from 850C to 1050C in increments
of 50C and held for 30 minutes, 2, 4, and 9 hours. Utilizing the standard ASTM test methods, average
grain size measurements could be determined using the Jefferies Planimetric Method to further
examine the growth kinetics.
1
2 Literature Review
2.1 Heat Treatment

Heat Treatment is a process commonly utilized to obtain desired properties within steels. [4]
This is done by controlling the heat treatment temperature, its holding time and the rate at which it is
cooled. A typical temperature vs. time plot for a heat treatment schedule can be seen in Figure 1. In
most cases, a process consists of a two-part heat treatment, Solution Heat Treating or Austenitizing and
Tempering or Precipitation Heat Treating.
Figure 1 - Temperature vs. Time Plot of Solution and Precipitation Heat Treatments [4]
2.1.1 Austenitizing
Austenitizing is the first step heat treatment and involves transforming the initial microstructure
to an austenitic structure. [3] By observing the Fe-C phase diagram in Figure 2 the phase transformation
can be seen.
2
Figure 2 Fe3C Phase Diagram [2]
To transform the microstructure to austenite, the sample is heated above the eutectoid
temperature (727C). If the material is a hypoeutectoid alloy (contains less than 0.76 weight % C), the
ferrite will start to transform into austenite and continue to do so as the temperature rises above the
eutectoid temperature. If the material is a hypereutectoid alloy (contains between 0.76 and 2.14 weight
% C), the cementite will transform into austenite and continue to do so as the temperature increases.
The temperature at which the microstructure is completely austenite depends upon the amount of
carbon within the alloy. [4]
After being held for the desired time, the steel can be rapidly quenched from the austenitic
region. The resulting microstructure is dependent on the rate of cooling as well as the concentration of
alloying elements within the steel. The Isothermal Transformation Diagram for a steel with a eutectoid
composition is presented in Figure 3, additional ITT diagrams for each steel examined within this study
can be seen within Appendix 1.
3
Figure 3 - Isothermal Transformation Diagram Fe-C Alloy of Eutectiod Composition [1]
By referencing the appropriate ITT diagrams, the final microstructure can be controlled to produce
desired microstructures and properties. A rapid quench may avoid the formation of Pearlite or Bainite
and allow martensite to form.
2.1.2 Tempering
Generally the microstructure of steel in its post-quenched state is undesirable due to internal
stresses, brittleness and hardness. . Tempering is generally utilized for martensitic steels as their
ductility and toughness are not optimal for most applications. [1] The process of tempering steel is
utilized to relieve the internal stresses and remove other undesirable properties that may have arisen in
previous heat treatment. The microstructure of tempered martensite consists of carbide particles
embedded within a ferrite matrix leading to a substantially enhanced ductility and toughness.
Martensite (BCT, single phase) Tempered Martensite ( +Fe3C and other carbides)
Tempering is normally carried out at temperatures between 250 and 650C, but stress relief can be
accomplished at temperatures as low as 200C. [4]
4
2.2 Grain Size and Growth
The grain size within steels largely contributes to bulk material properties such as strength,
creep, and fatigue resistance, electrical and magnetic properties.[5] The Hall-Petch equation relates
yield strength, , to the average grain diameter, d, where 0 and k are constants as seen in the equation
below. [7]
Equation 1- Hall-Petch Equation
The relationship introduced in Equation 1 can be explained via dislocation theory which assumes that
grain boundaries act as obstacles to slip dislocations, causing dislocations to pile up on their slip planes
behind the grain boundaries. Dislocations that attempt to pass from one grain to the adjacent grain will
have to change its direction of motion due to crystallographic misorientation. [4] An increase in the
number of dislocations is assumed with increasing grain size and magnitude of applied stress. [3] Thus a
fine grained material possess a higher yield strength compared to a coarse grained material as a greater
applied stress would be needed to cause slip to pass through the boundary. In order to estimate
material properties as a function of heat treatment, the kinetics of grain growth must be understood.
2.2.1 What is Grain Growth?

The driving force for grain growth is the surface energy of the grain boundaries. As growth
occurs at elevated temperatures the number overall number of grains decreases as larger grains
consume smaller grains. As some grains begin to shrink, their area diminishes and the total surface
energy is lowered. [2] It has been generally recognized that the decrease of surface energy as a result of
grain growth is the driving force for grain growth. [7] As grains are continually growing and shrinking
over time, the mean grain size increases. The mean grain diameter is utilized as a measure of the grain
size of an alloy. The Ideal Grain Growth Law relates average grain diameter to initial grain size, and time
as seen below.
Equation 2 - Ideal Grain Growth Law
D is the average grain diameter, D0 is the initial grain size, K is a constant of proportionality that relates
heating temperature and activation energy for grain growth, and t is the holding time. The Ideal Grain
Growth Law is commonly written in a more general form by substituting the exponent as the variable m.
5
Equation 3 - General Grain Growth Law
Equation 4 - Relationship between K and Heating Temperature T
Early theories of grain growth are based upon the proportionality of the growth rate to the
interfacial free energy per unit volume or based on the inverse proportionality of the rate of boundary
migration to the boundary curvature predict a value of m to be 2. [8] Experimentally it has been shown
that values of m lie within the range of 2 to 5. The kinetic exponent, m, within an ideal system controlled
by diffusion, has a value of 2, meaning that the system has no defects or precipitates. A value of 3
indicates several phenomena such as precipitate phases with diffusion in the produced grains. If a value
of 4 is determined, it means there is an effect of the precipitate with diffusion along the grain boundary.
[9]
2.2.2 Factors Affecting Grain Growth
2.2.2.1 Heating Rate

The heating rate of the steel has been determined to have a significant influence upon the
growth kinetics in Equation 3. Slower heating rates have been shown to result in a larger initial grain
size, D0. Experimentally A36 steel has shown to possess varying initial grain sizes based upon the rate of
heating. Slowly heated specimens were heated to 1100C at 100C/s reveals initial grain sizes of 47m.
Rapidly heated specimens were heated in a stepped heating cycle and were heated initially at 5C/s to
900C and held for 120 seconds, then heated at 100C/s to 1100C. The initial grain size of the rapidly
heated samples was 88m in size. [9] The difference in initial grain size can be explained by grain growth
during heating. As the sample is heated from its austenite transition temperature to the target
temperature grains are growing; the sample with a slower heating rate took more time to reach the
target temperature compared to the faster heating rate and thus had more time for grain growth.
6
2.2.2.2 Zener Pinning
Grain growth can be inhibited in the presence of second phase particles which pin grain
boundaries in place. The restraining forces exerted on grain boundaries are called Zener forces. [9] A
grain of critical radius Rcr is the radius where the driving force is equivalent to the pinning force exerted
by second phase particles on grain boundaries. The limiting size for which grain growth can occur can be
seen in the Zener Equation. [10]
Equation 5: Zener Equation [10]
A is a constant, r is the mean second phase particle radius, and f is the volume fraction of second phase
particles. Second phase particles which can inhibit grain growth include very small oxide, sulfide, carbide
or silicate particles. [2] Zener pining can be observed at lower temperatures where second phase
particles are present, but not at elevated temperatures the particles dissolve. [11]
2.3 Materials
The following steels were used throughout the duration of this project. Each of the steels
utilized have distinct chemical and physical properties which allow them to be used in a variety of
applications.
2.3.1 AISI 1045

AISI 1045 steel is a widely used medium carbon steel with various engineering applications
ranging from bolts, gears, axels spindles, crankshafts, connecting rods and guide rods. [13] This steel has
a carbon content generally within the range of 0.43 to 0.5 wt% which results in increased strength in the
steel. [15]
2.3.2 AISI 4140

AISI 4140 is a low cost chromium-molybdenum alloy with uses in the oil and gas sector. [9] This
steel possesses desirable properties such as wear resistance, toughness and ductility in the quenched
and tempered conditions. Additionally it is easy to machine in the heat treated condition allowing for
use in a variety of applications such as axels and structural applications. [17] AISI 4140 typically
possesses a carbon content in the range of 0.38 to 0.43 wt%. [15]
7
2.3.3 AISI 4340
AISI 4340 is a nickel chromium-molybdenum steel alloy known for its toughness and ability of
developing a high strength in the heat treated condition while retaining good fatigue strength. This alloy
is utilized in structural applications such as aircraft landing gear, power transmission gears and shafts.
AISI 4340 possesses a carbon content generally within the range of 0.38 to 0.43 wt%. [18]
2.3.4 AISI 8620 Steel

AISI 8620 is a Chromium-Molybdenum-Nickel low alloy steel, often used in carburizing to
develop a hard case resulting in good wear resistance. Applications of this steel include transmission
components in a wide variety of vehicles as well gears, ring gears, shafts and crankshafts. [14] Typical
carbon content within this steel is within the range of 0.18 to 0.23 wt% carbon. [15]
2.3.5 AISI 9310 Steel

AISI 9310 is a Nickel-Chromium-Molybdenum steel utilized widely in vehicle transmission gears,
track rod pins, roller bearing rings and small arms parts. [14] Typical carbon content for this steel is in
the range of 0.08 to 0.13 wt% carbon. [14]
2.3.6 AISI 52100

AISI 52100 is a high carbon chromium alloy steel utilized for ball bearings. This alloy is a tool
steel which is capable of cutting a wide range of materials due to its combination of toughness, wear
resistance and hardness. Low quantities of manganese and chromium are utilized to improve hardening
characteristics. AISI 52100 possesses a low corrosion resistance compared to other chromium steels due
to low chromium levels. This steel typically has a carbon concentration within the range of 0.95 to 1.05
wt%. [19]
2.3.7 Material Composition
Optical Emission Spectrometry (OES) was used to determine the chemical composition of the
steels. The average readings of three measurements are shown in Table 1. The addition of each element
within the steel provides a specified role in determining the properties of the alloy. The function of each
element can be seen within Table 2. [1]
8
Table 1 - Material Composition Obtained via OES
C Cr Fe Mn Mo Ni P S Si
1045 0.484 0.1195 Bal. 0.745 0.0225 0.081 0.00435 0.0135 0.215
4140 0.377 1.025 Bal. 0.695 0.1505 0.1565 0.0071 0.011 0.2265
4340 0.417 0.79 Bal. 0.76 0.2283 1.71 0.00893 0.021 0.241
8620 0.2135 0.56 Bal. 0.805 0.1535 0.4525 0.00645 0.014 0.2355
9310 0.121 1.3 Bal. 0.605 0.141 3.49 0.0053 0.0098 0.2405
52100 0.975 1.57 Bal. 0.316 0.029 0.102 0.00625 0.0075 0.2045
Table 2: Functions of Alloying Elements [1]
Alloying Element Function
C To Control Strength Level and Hardenability
Cr Hardenability & Oxidation Resistance
Mn Hardenability
Mo Hardenability & to Improve Creep Strength
Hardenability & to Improve Notch Toughness at

Ni
Low Temperatures
Ferrite Strengthening & to Improve Corrosion

P
Resistance
S To Improve Machinability
As a Deoxidizer or to Reduce Core Losses in

Si
Electrical Sheets
By observing the chemical composition of each element in relation to the function of the element grain
growth rates can be compared due to Zenner Pinning Effects.
9
3 Methodology
Steels were received from Peterson Steel Corporation and A.M. Castle Metals in a rod stock
form. With assistance from the machinists at WPIs Haas Technical Education Center, these rods were
turned down to 46, 1cm thick disks. The process of furnace calibration, heat treatment, sample
preparation, and analysis are outlined within this chapter.
3.1 Furnace Calibration

In order to ensure the entire sample reached a specified temperature, the temperature of both
the furnace and the core of the sample were monitored closely. The process of temperature mapping
was utilized to view the temperature variation profile of the furnace. By temperature mapping the
furnace as well as measuring the samples core temperature, uniform heating can be achieved.
3.1.1 Temperature Mapping

The furnace initially utilized for heat treatment was a Thermolyne 1300 Furnace. This furnace
was utilized for lower temperature heat treatments, while the Thermolyne 48000 Furnace, model
number F48015 was utilized for temperatures exceeding 1000C. Temperature variation profiles from a
number of locations inside the furnace chamber were monitored in a process called temperature
mapping, to identify potential cold or hot spots that can cause deviations from the anticipated uniform
heating of the samples.
The temperature of each furnace was mapped using an Omega brand K-type thermocouple and
an Omega HH111 data-logger. To ensure the thermocouple and the datalogger were functioning within
specifications, a container of water was set to boil on a hotplate, and the temperature was measured.
The furnace was heated to a set temperature, and held for several minutes. The thermocouple was then
placed within the furnace at set locations to determine if a variance in temperature existed with respect
to location within the chamber.
3.1.2 Temperature Calibration

To monitor the core temperature of the samples, a 1 cm deep hole was drilled into the side of
each sample with a 1.6 mm drill bit. An Omega K-type grounded thermocouple was press fit into the
hole. A grounded thermocouple was utilized since the wires are physically attached to the interior of the
sheathing, thus eliminating possible air-gaps produced by ungrounded thermocouples. Exposed
10
thermocouples were not utilized as the bead of the bimetal could become easily damaged resulting in
inaccurate readings as seen in Figure 4 below.
Figure 4 - Comparison of Thermocouple Connections [12]
The core temperature of the disks was measured at fifteen minute intervals to ensure the samples did
not deviate from the specified heat treatment temperature.
3.2 Heat Treatment Procedure

The samples were heat treated in 50C increments from 850C to 1050C and held for 0.5 to 9
hours. The temperature and time values were chosen through consideration of the austenitizing
temperatures for medium carbon steels. Two identical samples were heat treated under identical
conditions to ensure redundancy.
The furnace was heated to the desired temperature; once this temperature was achieved the
samples were placed within the furnace. One of these samples contained the thermocouple, which
would monitor the internal core temperature. The time temperature curve for the heating rates can
be observed by recording the temperatures at 10 second intervals until the samples are within 10 C of
the target temperature. Once the core temperatures reached 10C of the target temperature, the heat
treatment process began with temperature measurements at 15 minute intervals to ensure thermal
stability. A time-temperature curve can be seen in Figure 5 & Figure 6.
11
8620 Heating Rate to 900C
1000
900
800
Temperature (C) 700
600
500
400
300
200
100
0
0 100 200 300 400 500
Time (s)
Figure 5 - Heating Rate of 8620 to 900C
Heat Treatment: 900C 2 Hours

1000
900
800
Temperature (C)
700
600
500
400
300
200
100
0
0 2000 4000 6000 8000 10000
Time (S)
Figure 6 Time-Temperature Graph of 900C Heat Treatment
Once the samples reached the prescribed length of heat treatment, they were immediately quenched
within a bath of ice water which was vigorously stirred.
12
3.3 Sample Preparation
Once the samples were quenched, they were sectioned and mounted via standard
metallographic procedures using a Mark V CS600 cutting wheel and a Buehler Simplimet II mounting
press. The samples underwent a grinding process using a Buehler Metaserv 2000 grinding wheel with
progressively finer grits of sandpaper. After achieving uniform directional wear with 600 grit sandpaper,
the samples were finely polished via a combination of the Buehler Vibromet I polisher and Century E-
plus polishers to produce a mirror finish. A Picric Acid Etchant was used in order to observe the
microstructure of the samples. Detailed instructions regarding sample preparation can be seen within
Appendix 2 and 3.
3.4 Optical Microscopy Measurements

Once the samples were etched, digital optical micrographs were taken using a Nikon Epiphot
Optical Microscope attached to a Nikon Digital Sight DS-U1 image acquisition system. Average grain size
measurements were conducted manually using the Hyen Intercept Method and Jefferies Planimetric
Method for each sample. While there are a number of image analysis software packages available to
measure the grain sizes, there have been a number of occasions where the level of accuracy of the
analysis was questioned. Hence, the analysis was conducted manually. The image processing program
ImageJ was utilized to overlay necessary features upon the micrographs for analysis.
3.4.1 Hyen Intercept Method

The first widely used methodology for measuring the average grain size is the Hyen Intercept
Method. The Intercept method utilizes a randomly positioned line of a known length that is overlaid on
the micrograph. In order to ensure accuracy the line must be long enough that it produces 50 to 150
intersections or interceptions at the micrographs magnification. Once the line is drawn, a set of rules
are utilized to count the intercepts along the line. [8] Seen below in Figure 7 is an example of the
Intercept Method for one of the samples with a line length of 0.23 mm. By calibrating the software
ImageJ with the micrographs scale bar, the line length can be measured within the program.
13
Figure 7 - Heyn Intercept Method at 200x Magnification: 1045 850C 9Hr
A set of rules are utilized to count the number of intersections and interceptions across the
length of the line. If the ends of the line end within a grain boundary, each end is counted as one-half
interception. Grain boundary intersections are counted as one point, triple-point intersections are
counted as 1.5 points and tangent hits are counted as one-half point. [8] Once the intersections along
the line have been tallied up, the mean intercept length, L3, can be determined:
[ ]
where NL is the tallied intercept count. With the mean intercept length, the ASTM grain size, G, can be
determined and further correlated to the average grain diameter via ASTM E112. [9]
3.4.2 Jefferies Method

The second methodology widely utilized to determine grain size is the Jefferies Planimetric
Method. The Jefferies Method has become the preferred methodology for measuring grain with
industry size due to its ease of use. This methodology utilizes a circle or rectangle of known area that has
been overlaid on top of the micrograph. The number of full grain boundaries within the area and partial
grain boundaries intersected by the shape are tallied and used to calculate the average grain diameter.
14
During this analysis, it is suggested that a standard circle of 79.8 mm in diameter (5000 mm2) be drawn
on the micrograph obtained at 100x. Figure 8 shows an example of the Jefferies Method on one of the
samples. By calibrating the software ImageJ with the micrographs scale bar, an accurate value of the
circles area can be determined for non-standardized sizes.
Figure 8 - Jefferies Method at 200x Magnification: 1045 850C 4Hr
A set of rules are also utilized for the Jefferies Method, but are much simpler in comparison to
the Heyn Intercept Method. A grain that is within the area of interest counts as a full point, where a
grain that intersects the boundary counts as a half point. [8] The grain area and diameter can be
determined via the following equations:
While the Jefferies Method provides slower results, the results were observed to be more accurate. This
was seen when multiple measurements were taken along the same micrograph, consistent values were
observed via the Jefferies Method, but a spread could be seen using the Heyn Intercept Method.
To achieve a more representative value for the average grain diameter, it was decided that the
Jefferies Method would be utilized with a total of fifteen measurements per sample. To remove bias
15
within the measurements, several graduate students assisted in calculating the grain sizes. A calibration
study was performed on a known sample to further measure the bias of each individual with results
seen in Appendix 4. Each individual performed three distinct measurements at different locations within
the sample. Outlying data was discarded by utilizing the Inter-Quartile Range (IQR) and the average of
the remaining data was taken as the representative average grain diameter for the sample.
16
4 Results and Discussion
4.1 Gain Size Evolution

By utilizing the Nikon Epiphot Optical Microscope, digital optical micrographs could be obtained.
By observing samples with respect to time and temperature, a visual indication of grain growth can be
seen. The following series of micrographs of AISIS 4140 were held at 0.5, 2, 4, and 9 hours at 1050C as
well as 850, 900, 950, 1000 and 1050C for 2 hours. All micrographs are at 100x magnification. These
micrographs visually indicate in average grain size with both heat treating time and temperature.
0.5 Hours 2 Hours
4 Hours 9 Hours
Figure 9: Variation in Grain Size of AISI 4140 with Time at 1050C
17
850C 900C
950C 1000C
1050C
Figure 10: Variation of Grain Size of AISI 4140 with Temperature at 2 Hours
4.2 Average Grain Diameters

The average grain diameter for each of the samples was determined using the procedure
outlined in Section 4.4.2. Fifteen measurements were taken per sample and the Inter-Quartile Range
(IQR) was utilized to filter out the outlying results. [19] The IQR calculation method, a representative
average of the grain diameter can be taken for each sample. Average grain diameters (mm) for AISI 8620
with respect to holding temperature and time can be seen within Table 3, additional steels can be seen
within Appendix 5.
18
Table 3: Average Grain Diameter (mm) for AISI 8620 Steel
0.5 Hours 2 Hours 4 Hours 9 Hours

850C 0.0112 0.0108 0.0106 0.0118
900C 0.0121 0.0142 0.0145 0.0157
950C 0.0140 0.0167 0.0165 0.0244
1000C 0.0172 0.0204 0.0219 0.0313
1050C 0.0230 0.0345 0.0382 0.0515
From observed values of the average grain diameter, grain size increased with both holding temperature
as well as time. Variance within measurements at lower temperatures can be attributed to minimal
grain growth resulting in consistent diameters.
4.3 ASTM Grain Size

Different methodologies can be utilized to calculate the ASTM Grain Size Number including use
of an eyepiece graticules for optical microscopes and conversion from either the Hyen Linear Intercept
Method or Jefferies Planimetric Method. As data was collected via the Jefferies Method, a conversion
was utilized.
[ ]
Equation 6: ASTM Grain Size Equation
Equation 6 was utilized to calculate the ASTM Grain Size Number for each sample where NA is the
number of grains per square millimeter. Calculated ASTM Grain Size Numbers for each steel can be seen
within Appendix 5.
4.4 Effective Time

It has been shown through previous work that the heating rate affects the grain size of steels. To
account for this within the results the effective heating time had to be determined by observing the
recorded heating rates.
19

Equation 7: Heating Time Equation
Equation 8: Effective Time Equation
Through the use of Equation 7 and Equation 8, the effective heating time and time grains were allowed
to grow can be calculated. The effective heating time was taken to be the amount of time the steel took
to go from the eutectoid temperature of 727C, where austenite initially forms to the lower extreme of
the holding temperature tolerance, 10C from the holding temperature. Detailed as well as tabulated
calculations for the total heating time each steel can be seen in Appendix 6.
20
4.5 Ideal Grain Growth
4.5.1 Evaluating K and D0
The grain growth kinetics of Equation 3 can be observed for each steel by plotting values of
average grain diameter squared vs. effective time. In doing so an assumption is made that ideal grain
growth is present, thus the value of the exponent m is 2.
A comparison of D2 vs. time for 8620 can be seen within Figure 11. At lower temperatures grain growth
is minimal; at elevated temperatures substantial growth can be seen. Plots of each steel can be seen in
Appendix 7.
8620 Comparison
0.003
Average Grain Diameter2 (mm2)
0.0025
850C
0.002
900C
0.0015
950C
0.001
1000C
0.0005 1050C
0
0.00 100.00 200.00 300.00 400.00 500.00 600.00
Effective Time (min)
Figure 11: Plot of Average Grain Diameter squared vs. Effective Time
The proportionality constant, K, and initial grain size D0 were determined from the slope and intercept
of the trend line. Calculated values of K and D0 for each steel can be seen within Table 4.
21
Table 4: Comparison of K and D0 for Various Alloys
Alloy Temperature K (mm2/min) D0 (mm)

(C)
850 6.65E-08 0.0107
900 2.31E-07 0.0116
1045 950 2.58E-07 0.0148
1000 2.19E-06 0.0312
1050 3.73E-06 0.0401
850 2.73E-08 0.0109
900 6.61E-08 0.0125
4140
950 5.64E-08 0.0136

1000 1.28E-07 0.0173
1050 7.26E-07 0.0341
850 3.13E-08 0.0107
900 4.55E-08 0.0114
4340
950 1.28E-07 0.0133

1000 2.82E-07 0.0184
1050 9.90E-07 0.0304
850 3.39E-08 0.0107
900 1.65E-07 0.0128
8620
950 7.65E-07 0.0124

1000 1.33E-06 0.0147
1050 3.95E-06 0.0221
900 7.62E-08 0.0111
950 8.75E-08 0.0125
9310
1000 5.47E-07 0.0163

1050 1.46E-06 0.0346
900 2.49E-08 0.0139
52100
950 1.28E-07 0.0133

1000 3.96E-07 0.0221
1050 1.65E-06 0.0270
An increase in initial grain size, D0, as well as the constant K can be seen with increasing temperature as
growth occurs at an accelerated rate at elevated temperatures.
22
4.5.2 Evaluating Activation Energy
For grain growth to occur, a number of barriers must be surpassed, one of which is the
necessary activation energy must be supplied to the steel. The activation energy, Q, is related to grain
growth via Equation 4.
By plotting the inverse of absolute temperature against the proportionality constant K, the activation
energy was determined from the slope of a linear trend line.
Comparison of Alloys
-10.5
1045
-11
4140
-11.5
4340
-12
Log(Kp)
8620
-12.5
9310
-13
-13.5 52100
-14
0.00074 0.00076 0.00078 0.0008 0.00082 0.00084 0.00086 0.00088 0.0009
1/T
Figure 12 - Log(Kp) vs. 1/T Comparison
The relation between the slope of the trend line and the activation energy needed for grain growth can
be seen below where R is the gas constant. Plots of individual alloys with accompanying linear trend
lines can be seen within Appendix 8.
Values obtained for the activation energy as well as the pre-exponential constant, k0 for each alloy can
be seen in Table 5 below:
23
Table 5 - Comparison of Activation Energy and Pre-exponential constant
Steel Q (KJ/mol) K0
1045 253.3 6.165E-04
4140 175.2 5.409E-08
4340 213.7 3.392E-06
8620 287.9 1.747E-02
9310 273.4 1.352E-03
52100 353.4 4.061E-01
24
5 Conclusions & Recommendations
5.1 Heat Treatment

The rate of heat treatment of samples was significantly improved through the use of the
Thermolyne 48000 due to its large chamber size. The presence of a larger chamber allowed for all
samples at a prescribed holding temperature to be heat treated simultaneously in single batch. This
significantly decreased the amount of time spent heat treating as 0.5, 2, 4 and 9 hour samples could
undergo this process within a single day.
Recommendations for further heat treatment include the use of a Data Acquisition System
(DAQ) to record temperature measurements over time. Without the use of a DAQ, measurements had
to be recorded by hand for the course of the heat treatment cycle. Implementation of such a system
would provide an accurate temperature profile during quenching to ensure a martensitic microstructure
was obtained.
5.2 Sample Preparation

The process of sample preparation faced minimal challenges in terms of cutting and mounting
samples. Grinding and polishing proved to be a challenging process at first as it required producing a
mirror finish, free from scratches. A completely flat samples is critical to obtain high quality micrographs
with the optical microscope. In order to achieve a flat surface, pressure must be applied uniformly on
the samples surface during the grinding and polishing procedures.
Etching the grain boundaries proved to be the most challenging portion of this project. Due to
the varying chemical composition between each of the steels, they had to be immersed within the
etchant for varying amounts of time. In addition, each batch of etchant provided varying grain boundary
visibility as the etchant concentration changed over time on the hot plate. Additionally, samples
behaved differently to the etchant within clear grain boundaries outlined in all steels but 1045.
5.3 Average Grain Size Measurements

Average grain size measurements were calculated utilizing the Jefferies Planimetric Method as it
proved to be a more reliable methodology compared to the Hyen Intercept Method. While
measurements did take substantially longer it was much easier to distinguish between a full and partial
25
grain of Jefferies Method compared to an intersection, triple point and tangent in the Intercept Method.
Even though the Jefferies Method proved to produce more reliable results, the quality of the etchant
strongly impacted visibility of the grain boundaries. If grain boundaries are not well defined, it is
recommended to outline the boundaries on the micrograph to aid in further analysis.
By performing an IQR analysis of a total of fifteen measurements between five individuals at

different locations within the sample provided a representative average grain diameter for each sample.
To ensure grains were being counted correctly, a calibration study was performed and the numbers of
grains within a known sample were counted and compared. Determining grain boundaries proved
difficult if they were not well defined through the etchant process which led to multiple iterations of
measurements.
As expected, average grain sizes increased with both holding time and temperature, as
predicted from the grain growth equations. An increase in temperature was found to have a larger
effect on grain size than an increase in holding time as temperature is exponentially dependent
compared to times linear dependence. At lower temperatures, grain growth was minimal or severely
restricted due to grain pinning effects. By utilizing the Energy Dispersive Spectroscopy (EDS) function of
an SEM, the chemical composition of the grain boundaries can be analyzed indicating if carbides or
other inclusions are present within the sample. The addition of pinning mechanisms within the sample
alter the growth kinetics as the growth exponent, m, is no longer equal to 2. In order to predict a value
of m for non-ideal growth, an iterative algorithm would have to be developed which solves for values of
m, k and d0.
5.4 Growth Kinetics

In determining the grain growth kinetics of each of the steels, the average grain size (squared)
was plotted against time. In doing so, values of K and D0 can be determined and utilized to find the
activation energy for grain growth; Q. Values of K and D0 were specific to each steel and temperature,
while Q is specific to each steel. The calculated activation energy for grain growth was compared to the
activation energy for diffusion of iron in iron, 284 KJ/mol. [4] Observed values of activation energy lie
within the range of 175 to 353 KJ/mol. While the calculated values for Q, K and D0 pertain to ideal grain
growth, further work must be done to determine if pinning effects are present and how they affect
growth kinetics.
26
Works Cited
[1] Seco / Warwick, Heat Treating Data Book, 10th ed. Meadville, PA: Seco / Warwick Corporation,
2011.
[2] Reza Abbaschian, Lara Abbaschian, and Robert E. Reed-Hill, Physical Metallurgy Principles.
Stamford, CT: Cengage Learning, 2009.
[3] William D. Callister Jr., Materials Science and Engineering an Introduction. York: Wiley, 2007.
[4] Advanced Cast Products. The Austempering Process. [Online].

http://www.advancedcast.com/austempering-process.htm
[5] A.K. Giumelli, M. Militzer, and E.B Hawbolt, "Analysis of the Austenite Grain Size Distribution in
Plain Carbon Steels," The Iron and Steel Institute of Japan, vol. 39, no. 3, pp. 271-280, 1998.
[6] J. W. Morris, Jr., "The Influence of Grain Size on the Mechanical Properties of Steel," Berkeley, 2001.
[7] Chongxiang Yue, Liwen Zhang, Shulun Liao, and Huiju Gao, "Kinetic Analysis of the Austenite Grain
Growth in GCr15 Steel," Journal of Materials Engineering and Performance, vol. 19, no. 1, pp. 112-
115, February 2009.
[8] S. Illescas, J. Fernandez, and J.M. Guilemany, "Kinetic Analysis of the Austenitic Grain Growth in
HSLA Steel with a Low Carbon Content," Materials Letters, vol. 62, pp. 3478 - 3480, March 2008.
[9] Alan Giumelli, "Austenite Grain Growth Kinetics and the Grain Size Distribution," University of
British Columbia, Vancouver, M.A.Sc. Thesis 601896139, 1995.
[10] J Rudnizki, B Zeislmair, U Prahl, and W Bleck, "Prediction of Abnormal Grain Growth During High
Temperature Treatment," Computational Materials Science, vol. 47, pp. 209-216, April 2010.
[11] P. A. Manohar, D. P. Dunne, T. Chandra, and C. R. Killmore, "Grain Growth Predictions in

Microalloyed Steels," The Iron and Steel Institute of Japan, vol. 36, no. 2, pp. 194-200, September
1995.
[12] P. A. Beck, M. L. Holzworth, and P. Sperry, "Effect of a Dispersed Phase on Grain Growth in Al-Mn
Alloys," AIME Transactions, vol. 180, no. 163, 1949.
[13] Tata Steel International Ltd. Medium Tensile Steel - AISI 1045. [Online].
http://www.corusnz.com/downloads/MeduimTens_AISI1045.pdf
[14] Granta Design. (2010) CES EduPack - Low Alloy Steel, AISI 9310. Software v. 5.2.0.
27
[15] West Yorkshire Steel Company Ltd. West Yorkshire Steel: UK Special Steel Stockholders. [Online].
http://www.westyorkssteel.com/AISI_4140.html
[16] Short Run Pro: Custom Machines Parts. [Online].

http://www.shortrunpro.com/Machining/General_eng_guidelines.aspx
[17] Metal Suppliers. (2009) Material Property Data Alloy Steels 4340. [Online].
http://www.suppliersonline.com/propertypages/4340.asp
[18] Metal Suppliers Online. (2009) Alloy Steels 8620. [Online].

http://www.suppliersonline.com/propertypages/8620.asp
[19] Sullivan Steel Service. Applications of 52100 Alloy Steel Tubing. [Online].
http://www.52100steel.com/about.html
[20] Omega. Introduction to Thermocouples. [Online].

http://www.omega.com/techref/themointro.html
[21] George F Vander Voort, Metallography: Principles and Practice. New York: ASM International, 2004.
[22] ASTM International, ASTM E112 - 10: Standard Test Methods for Determining Average Grain Size.:
ASTM International, 2010.
[23] Joseph D Petruccelli, Applied Statistics for Engineers and Scientists. Upper Saddle River, N.J., United
States of America: Prentice Hall, 1999.
[24] American Society for Metals, Atlas of Isothermal Transformation and Cooling Transformation
Diagrams.: ASM, Metals Park, Ohio, 1977.
[25] Key to Metals: The World's Most Comprehensive METALS Database. [Online].
http://www.keytometals.com/page.aspx?ID=CheckArticle&site=kts&NM=62
[26] Mike Meier. (2004, September) UC Davis: Department of Chemical Engineering and Materials
Science. [Online]. http://chms.engineering.ucdavis.edu/students/undergraduates/labs/files/HT-
Steel.pdf
[27] C.S Smith,. Cleveland, United States of America: ASM International, 1952, p. 65.
[28] Mid-Atlantic Casting Services. (2005, Feburary) A Guide to Mechanical Properties of Cast Carbon
and Low Alloy Steels. [Online]. http://www.mid-atlanticcasting.com/cast-steel-guide_FEB05.pdf
28
Appendix 1: Isothermal Transformation Diagrams
Isothermal Transformation Diagram for AISI 1045 Steel [4]
Isothermal Transformation Diagram for AISI 4140 Steel
29
30
31
Appendix 2: Sample Grinding & Polishing Procedures
The following details instructions on how to section and mount a sample utilizing the Mark V CS600
cutting wheel and Buehler Simplimet II mounting press.
Mark V CS600 - Sectioning

1) Select the appropriate blade based on the hardness of your sample, a chart is posted within the
lab. An incorrect choice of blade will lead to damage of the blade and or sample.
a. If the blade is damaged, it must be replaced. Utilize the correct combination of
wrenches within the supply drawers to remove and replace the blade.
2) Check lubricating fluid levels within the fluid bay, refill if necessary.
3) Secure the sample within the vice on the cutting table.
4) Rotate the stop to allow for the cutting table to pivot.
5) Press On/Off, followed by Start to start the Mark V. Slowly lower the cutting table until contact
is made with the sample.
6) Allow for the weight of the sample to drive the sectioning process, do not apply pressure to the
sample as it leads to a non-uniform cutting face and could damage the blade.
7) Once the sample is bisected, press the On/Off button to power down the Mark V. Raise the
protective enclosure, replace the stop and remove the sample.
8) Utilize a paper towel to remove chips, powder or excess fluid that has deposited within the
machine.
Mark V CS600
32
Beuhler Simplimet II Mounting
1) Power on the Mounting Press via the On button located on the display panel.
2) Turn on the water from the flow control valve located on the wall behind the press.
3) Ensure both the metallic stopper on the underside of the handle as well as the ram are clear of
debris.
4) Place the desired sample on the center of the ram with the face of interest faced down.
5) Lower the ram via the down arrow on the display. Pour/place the mounting powder or disk on
top of the sample.
6) Once the sample has been lowered to the bottom of the chamber, press the metallic stopper
into the chamber and lock by rotating.
7) To start the mounting process, press Start on the display panel. Once completed, the press
will beep.
8) Unlock the stopper and press the Up arrow to raise the ram. Remove the sample as well as any
present residual polymer flakes on the ram or stopper.
9) Lower the ram to just below the top of the machine, stop the flow of water, and power off the
machine.
Beuhler Simplimet II Mounting Press
33
Appendix 3: Sample Etching Procedures
The following details the procedure for creating the Picric Acid etchant utilized to reveal the
microstructure of 1045 samples. The following dictates how to prepare 300 mL of etchant.
1. Measure 12g of Picric Acid into a beaker and mix with 300mL of water to create an aqueous
solution.
2. Place a magnetic stir rod within the beaker and utilize a stirring plate to dissolve the majority of the
Picric Acid, creating a saturated solution.
3. Add two tablespoons of Nacconal 90G, a wetting agent made of sodium dodecyl benzene sulfonate.
4. Excess Picric Acid and wetting agent are filtered out via a funnel and wetted cotton to create a seal.
5. The filtered solution is heated between 80 and 90C underneath a hood.
6. If the samples to be etched contain > 0.5% Cr, 18 drops of HCl are added to the solution (6 drops per
100mL).
7. Samples are submerged within the etchant sample facing up for initially 30 seconds.
8. Once the time has elapsed, samples are washed under running warm water, rinsed with acetone
and blown dry.
9. The quality of the procedure is observed via an Optical Microscope, if the grains are faint further
time within the etchant is required. If the sample is dark, it has been over-etched and must be back-
polished with figure eight motions to remove smut build up.
10. A blue hue will be visible on the samples surface, providing a visual clue that it has been etched
sufficiently.
34
Appendix 4: Jefferies Planimetric Method Calibration Studies
The following details the calibration methods utilized for the Jefferies Planimetric Method. The
Jefferies method was performed on known micrographs in order to compare measured values of
inscribed and partial grains. The calibration studies were also utilized to determine the impact of the
number of full and partial grains on calculated grain size.
Calibration Study #1
The first micrograph utilized below is of an austenitic manganese steel that was solution
annealed at 1038C and aged at 621C. The micrograph is taken at 100x magnification and the area is
approximately 5000 mm2. [8]
Value of both the inscribed and partial grains were counted by each individual and compared to the
known values. As seen in the following tables, a discrepancy of 12.27% in determining full and partial
grains results in a 1.34% difference in average grain diameter.
35
Results: Calibration Study #1
Measured Actual % Difference
Full Grains 43 44 -2.27

Chunmin
Partial Grains 23 25 -8.00

Erik
Partial Grains 25 25 0.00
Full Grains 44 44 0.00

Lei

Sidath

Zhijia
Average Grain Measured Actual ASTM % Difference

Diameter (mm) ASTM Grain # Grain #
Chunmin 0.01354 3.818 3.87 -1.34
Erik 0.01342 3.845 3.87 -0.66
Lei 0.01348 3.832 3.87 -0.99
Sidath 0.01348 3.8315 3.87 -0.99
Zhijia 0.01336 3.8575 3.87 -0.32
36
Calibration Study #2
The second micrograph utilized below is of low-carbon sheet steel taken at 500x magnification
and an area of approximately 5000 mm2. [8]
Value of both the inscribed and partial grains were counted by each individual and compared to the
known values. The second calibration study is a closer representation to micrographs of 1045 steel due
to the faint grain boundaries. As seen in the following tables, a discrepancy of 18.15% in determining full
and partial grains results in a 1.77% difference in average grain diameter.
37
Results: Calibration Study #2
Measured Actual % Difference

Chunmin

Erik
Partial Grains 33 30 10.00

Lei

Sidath

Zhijia
Average Grain Measured Actual ASTM

% Difference
Diameter (mm) ASTM Grain # Grain #
Chunmin 0.00237 8.844 8.94 -1.08
Erik 0.00236 8.854 8.94 -0.96
Lei 0.00239 8.813 8.94 -1.42
Sidath 0.00242 8.7816 8.94 -1.77
Zhijia 0.00235 8.8640 8.94 -0.85
38
Appendix 5: Average Grain Diameters
AISI 1045
Temperature Effective Time ASTM Grain Size Avg Grain Diameter Kp (mm^2 / D0
(C) (min) # (mm) min) (mm)
850 34 10.263 0.0103 6.65E-08 0.0107
850 124 9.815 0.0120 6.65E-08 0.0107
850 244 10.090 0.0109 6.65E-08 0.0107
850 544 9.743 0.0123 6.65E-08 0.0107
900 34.67 9.905 0.0116 2.31E-07 0.0116
900 124.67 9.560 0.0131 2.31E-07 0.0116
900 244.67 9.418 0.0138 2.31E-07 0.0116
900 544.67 8.968 0.0161 2.31E-07 0.0116
950 35.42 9.130 0.0152 2.58E-07 0.0148
950 125.42 8.895 0.0165 2.58E-07 0.0148
950 245.42 9.025 0.0158 2.58E-07 0.0148
950 545.42 8.450 0.0192 2.58E-07 0.0148
1000 44.92 7.226 0.0294 2.19E-06 0.0311
1000 134.92 6.590 0.0367 2.19E-06 0.0311
1000 254.92 6.200 0.0420 2.19E-06 0.0311
1000 554.92 5.963 0.0456 2.19E-06 0.0311
1050 42.08 6.645 0.0360 3.73E-06 0.0400
1050 132.08 5.951 0.0457 3.73E-06 0.0400
1050 252.08 5.279 0.0577 3.73E-06 0.0400
1050 552.08 5.279 0.0577 3.73E-06 0.0400
39
AISI 4140
Temperature Effective ASTM Grain Size Avg Grain Diameter Kp (mm^2 / min) D0
(C) Time (min) # (mm) (mm)
850 33.33 10.188 0.0105 2.73E-08 0.0109
850 123.33 10.027 0.0111 2.73E-08 0.0109
850 243.33 9.893 0.0117 2.73E-08 0.0109
850 543.33 9.978 0.0113 2.73E-08 0.0109
900 33.83 9.768 0.0122 6.61E-08 0.0125
900 123.83 9.658 0.0127 6.61E-08 0.0125
900 243.83 9.351 0.0141 6.61E-08 0.0125
900 543.83 9.462 0.0135 6.61E-08 0.0125
950 35.83 9.511 0.0133 5.64E-08 0.0136
950 125.83 9.428 0.0137 5.64E-08 0.0136
950 245.83 9.160 0.0150 5.64E-08 0.0136
950 545.83 9.287 0.0144 5.64E-08 0.0136
1000 43.83 8.824 0.0169 1.28E-07 0.0173
1000 133.83 8.584 0.0184 1.28E-07 0.0173
1000 253.83 8.471 0.0191 1.28E-07 0.0173
1000 553.83 8.597 0.0183 1.28E-07 0.0173
1050 42.83 6.784 0.0343 7.26E-07 0.0341
1050 132.83 6.375 0.0395 7.26E-07 0.0341
1050 252.83 6.658 0.0358 7.26E-07 0.0341
1050 552.83 6.576 0.0368 7.26E-07 0.0341
40
AISI 4340
850 33.33 10.126 0.0108 3.13E-08 0.0107
850 123.33 10.044 0.0111 3.13E-08 0.0107
850 243.33 10.112 0.0108 3.13E-08 0.0107
850 543.33 9.923 0.0115 3.13E-08 0.0107
900 32.33 9.924 0.0115 4.55E-08 0.0114
900 122.33 10.127 0.0108 4.55E-08 0.0114
900 242.33 9.614 0.0128 4.55E-08 0.0114
900 542.33 9.772 0.0122 4.55E-08 0.0114
950 35.67 9.318 0.0142 1.28E-07 0.0133
950 125.67 9.626 0.0128 1.28E-07 0.0133
950 245.67 9.225 0.0147 1.28E-07 0.0133
950 545.67 9.017 0.0158 1.28E-07 0.0133
1000 40.58 8.542 0.0186 2.82E-07 0.0184
1000 130.58 8.529 0.0187 2.82E-07 0.0184
1000 250.58 8.068 0.0220 2.82E-07 0.0184
1000 550.58 8.187 0.0211 2.82E-07 0.0184
1050 43.58 7.364 0.0280 9.90E-07 0.0304
1050 133.58 6.739 0.0348 9.90E-07 0.0304
1050 253.58 6.670 0.0357 9.90E-07 0.0304
1050 553.58 6.523 0.0375 9.90E-07 0.0304
41
AISI 8620
850 34.25 10.008 0.0112 3.39E-08 0.0107
850 124.25 10.122 0.0108 3.39E-08 0.0107
850 244.25 10.161 0.0106 3.39E-08 0.0107
850 544.25 9.864 0.0118 3.39E-08 0.0107
900 33.75 9.782 0.0121 1.65E-07 0.0128
900 123.75 9.320 0.0142 1.65E-07 0.0128
900 243.75 9.257 0.0145 1.65E-07 0.0128
900 543.75 9.044 0.0157 1.65E-07 0.0128
950 34.50 9.364 0.0140 7.65E-07 0.0124
950 124.50 8.864 0.0167 7.65E-07 0.0124
950 244.50 8.887 0.0165 7.65E-07 0.0124
950 544.50 7.770 0.0244 7.65E-07 0.0124
1000 44.42 8.768 0.0172 1.33E-06 0.0146
1000 134.42 8.282 0.0204 1.33E-06 0.0146
1000 254.42 8.082 0.0219 1.33E-06 0.0146
1000 554.42 7.050 0.0313 1.33E-06 0.0146
1050 43.75 7.931 0.0230 3.95E-06 0.0220
1050 133.75 6.768 0.0345 3.95E-06 0.0220
1050 253.75 6.474 0.0382 3.95E-06 0.0220
1050 553.75 5.610 0.0515 3.95E-06 0.0220
42
AISI 9310
900 33.00 10.135 0.0107 7.62E-08 0.0111
900 123.00 10.322 0.0101 7.62E-08 0.0111
900 243.00 9.320 0.0142 7.62E-08 0.0111
900 543.00 9.806 0.0120 7.62E-08 0.0111
950 35.25 9.683 0.0125 8.74E-08 0.0125
950 125.25 9.590 0.0130 8.74E-08 0.0125
950 245.25 9.469 0.0135 8.74E-08 0.0125
950 545.25 9.317 0.0142 8.74E-08 0.0125
1000 41.50 9.012 0.0158 5.47E-07 0.0163
1000 131.50 8.511 0.0188 5.47E-07 0.0163
1000 251.50 8.193 0.0210 5.47E-07 0.0163
1000 551.50 7.884 0.0234 5.47E-07 0.0163
1050 38.58 7.131 0.0304 1.46E-06 0.0346
1050 128.58 6.406 0.0391 1.46E-06 0.0346
1050 248.58 6.067 0.0439 1.46E-06 0.0346
1050 548.58 6.151 0.0427 1.46E-06 0.0346
AISI 52100
Temperature Effective ASTM Grain Size Avg Grain Diameter Kp (mm^2 / D0

(C) Time (min) # (mm) min) (mm)
850 33.85 9.564 0.0131 -7.90E-08 0.0119
850 123.85 10.478 0.0095 -7.90E-08 0.0119
850 243.85 10.050 0.0110 -7.90E-08 0.0119
850 543.85 10.270 0.0102 -7.90E-08 0.0119
900 35.58 9.162 0.0150 2.49E-08 0.0139
900 125.58 9.554 0.0131 2.49E-08 0.0139
900 245.58 9.485 0.0134 2.49E-08 0.0139
900 545.58 9.204 0.0148 2.49E-08 0.0139
950 35.67 9.318 0.0142 1.28E-07 0.0133
950 125.67 9.626 0.0128 1.28E-07 0.0133
950 245.67 9.225 0.0147 1.28E-07 0.0133
950 545.67 9.017 0.0158 1.28E-07 0.0133
1000 41.50 7.999 0.0225 3.96E-07 0.0221
1000 131.50 7.913 0.0232 3.96E-07 0.0221
1000 251.50 7.518 0.0266 3.96E-07 0.0221
1000 551.50 7.765 0.0244 3.96E-07 0.0221
1050 44.83 7.599 0.0258 1.65E-06 0.0268
1050 134.83 7.145 0.0302 1.65E-06 0.0268
1050 254.83 6.398 0.0392 1.65E-06 0.0268
1050 554.83 6.551 0.0371 1.65E-06 0.0268
43
Appendix 6: Effective Time Results
The effective time was calculated via Equation 7 & Equation 8 to determine the total amount of
time that austenite grains were allowed to grow. Tabulated results are listed below for both effective
heating time as well as the effective time that grains were allowed to grow. Following the tabulated
results are the accompanying Mathcad calculations.
Tabulated Effective Time for AISI 1045
Sample Temperature Holding Time Heating Time

# C (min) (min) Effective Time (min)
131 850 30 3.74 33.74
112 850 120 3.74 123.74
111 850 240 3.74 243.74
114 850 540 3.74 543.74
132 900 30 4.60 34.60
105 900 120 4.60 124.60
106 900 240 4.60 244.60
109 900 540 4.60 544.60
133 950 30 5.00 35.00
118 950 120 5.00 125.00
117 950 240 5.00 245.00
120 950 540 5.00 545.00
123 1000 30 13.48 43.48
124 1000 120 13.48 133.48
125 1000 240 13.48 253.48
126 1000 540 13.48 553.48
127 1050 30 11.01 41.01
128 1050 120 11.01 131.01
129 1050 240 11.01 251.01
130 1050 540 11.01 551.01
44
Temperature Holding Time Heating Time

Sample # C (min) (min) Effective Time (min)
234 850 30 3.04 33.04
215 850 120 3.04 123.04
214 850 240 3.04 243.04
217 850 540 3.04 543.04
235 900 30 3.39 33.39
208 900 120 3.39 123.39
209 900 240 3.39 243.39
212 900 540 3.39 543.39
236 950 30 5.37 35.37
221 950 120 5.37 125.37
220 950 240 5.37 245.37
224 950 540 5.37 545.37
226 1000 30 12.49 42.49
227 1000 120 12.49 132.49
229 1000 240 12.49 252.49
228 1000 540 12.49 552.49
230 1050 30 11.78 41.78
231 1050 120 11.78 131.78
232 1050 240 11.78 251.78
233 1050 540 11.78 551.78
45

610 850 30 3.01 33.01
611 850 120 3.01 123.01
612 850 240 3.01 243.01
613 850 540 3.01 543.01
614 900 30 1.57 31.57
615 900 120 1.57 121.57
616 900 240 1.57 241.57
617 900 540 1.57 541.57
618 950 30 5.21 35.21
619 950 120 5.21 125.21
620 950 240 5.21 245.21
621 950 540 5.21 545.21
601 1000 30 9.68 39.68
602 1000 120 9.68 129.68
604 1000 240 9.68 249.68
603 1000 540 9.68 549.68
605 1050 30 12.37 42.37
606 1050 120 12.37 132.37
609 1050 240 12.37 252.37
608 1050 540 12.37 552.37
46

331 850 30 4.00 34.00
317 850 120 4.00 124.00
319 850 240 4.00 244.00
321 850 540 4.00 544.00
332 900 30 3.46 33.46
310 900 120 3.46 123.46
313 900 240 3.46 243.46
314 900 540 3.46 543.46
333 950 30 4.15 34.15
304 950 120 4.15 124.15
306 950 240 4.15 244.15
308 950 540 4.15 544.15
323 1000 30 13.54 43.54
324 1000 120 13.54 133.54
325 1000 240 13.54 253.54
326 1000 540 13.54 553.54
327 1050 30 12.71 42.71
328 1050 120 12.71 132.71
329 1050 240 12.71 252.71
330 1050 540 12.71 552.71
47

423 900 30 2.70 32.70
406 900 120 2.70 122.70
411 900 240 2.70 242.70
408 900 540 2.70 542.70
424 950 30 4.94 34.94
401 950 120 4.94 124.94
403 950 240 4.94 244.94
405 950 540 4.94 544.94
413 1000 30 10.55 40.55
414 1000 120 10.55 130.55
416 1000 240 10.55 250.55
415 1000 540 10.55 550.55
417 1050 30 7.83 37.83
422 1050 120 7.83 127.83
421 1050 240 7.83 247.83
420 1050 540 7.83 547.83
*Note AISI 9310 was not heat treated at 850C as the selected temperature was to close in proximity to
the austenitizing temperature for this steel.
48
Temperature Holding Time Heating Time

C (min) (min) Effective Time (min)
850 30 3.36 33.36
850 120 3.36 123.36
850 240 3.36 243.36
850 540 3.36 543.36
900 30 5.22 35.22
900 120 5.22 125.22
900 240 5.22 245.22
900 540 5.22 545.22
950 30 5.16 35.16
950 120 5.16 125.16
950 240 5.16 245.16
950 540 5.16 545.16
1000 30 11.67 41.67
1000 120 11.67 131.67
1000 240 11.67 251.67
1000 540 11.67 551.67
1050 30 7.61 37.61
1050 120 7.61 127.61
1050 240 7.61 247.61
1050 540 7.61 547.61
*Note AISI 52100 did not possess sample numbers as they could not be engraved via the Haas MiniMill,
instead a methodology of sample bags was adopted to differentiate between samples.
49
At T = 850 Celsius Ttarget 850 10
1045 Steel
2 6.73 10 4 x xmin 240 xmax 480

f ( x) 6.16 10 e
x
max 5
Area f ( x) d x 1.886 10
x
min
Area
effective 224.494
Ttarget
4140 Steel
2 7.43 10 4 x xmin 190 xmax 385

f ( x) 6.34 10 e
x
max 5
Area f ( x) d x 1.532 10
x
min
Area
effective 182.388
Ttarget
4340 Steel
0.0008 x
f ( x) 622.9 e xmin 180 xmax 375
x
max 5
Area f ( x) d x 1.518 10
x
min
Area
effective 180.729
Ttarget
8620 Steel
2 5.76 10 4 x xmin 185 xmax 440

f ( x) 6.60 10 e
x
max 5
Area f ( x) d x 2.017 10
x
min
Area
effective 240.087
Ttarget
50
9310 Steel
2 8.96 10 4 x xmin 165 xmax 340

f ( x) 6.29 10 e
x
max 5
Area f ( x) d x 1.382 10
x
min
Area
effective 164.478
Ttarget
52100 Steel
2 6.84 10 4 x
f ( x) 6.31 10 e xmin 215 xmax 430
x
max 5
Area f ( x) d x 1.693 10
x
min
Area
effective 201.549
Ttarget
51
1045 Steel
2 9.05 10 4 x xmin 165 xmax 450

f ( x) 6.51 10 e
x
max 5
Area f ( x) d x 2.457 10
x
min
Area
effective 276.12
T target
4140 Steel
2 7.43 10 4 x xmin 150 xmax 380

f ( x) 6.46 10 e
x
max 5
Area f ( x) d x 1.811 10
x
min
Area
effective 203.521
Ttarget
4340 Steel
2 1.62 10 4 x
f ( x) 5.80 10 e xmin 140 xmax 280
x
max 4
Area f ( x) d x 8.401 10
x
min
Area
effective 94.395
T target
8620 Steel
2 9.52 10 4 x xmin 180 xmax 405

f ( x) 6.21 10 e
x
max 5
Area f ( x) d x 1.849 10
x
min
Area
effective 207.801
Ttarget
52
9310 Steel
2 1.20 10 3 x xmin 140 xmax 315

f ( x) 6.27 10 e
x
max 5
Area f ( x) d x 1.444 10
x
min
Area
effective 162.284
Ttarget
52100 Steel
2 6.32 10 4 x
f ( x) 6.77 10 e xmin 155 xmax 490
x
max 5
Area f ( x) d x 2.786 10
x
min
Area
effective 313.02
T target
53
1045 Steel
2 8.20 10 4 x xmin 145 xmax 470

f ( x) 6.72 10 e
x
max 5
Area f ( x) d x 2.819 10
x
min
Area
effective 299.859
Ttarget
4140 Steel
2 7.16 10 4 x xmin 155 xmax 505

f ( x) 6.82 10 e
x
max 5
Area f ( x) d x 3.031 10
x
min
Area
effective 322.46
T target
4340 Steel
2 7.46 10 4 x
f ( x) 6.63 10 e xmin 205 xmax 540
x
max 5
Area f ( x) d x 2.94 10
x
min
Area
effective 312.784
Ttarget
8620 Steel
2 9.47 10 4 x xmin 195 xmax 465

f ( x) 6.33 10 e
x
max 5
Area f ( x) d x 2.342 10
x
min
Area
effective 249.197
Ttarget
54
9310 Steel
2 7.78 10 4 x xmin 120 xmax 440

f ( x) 6.98 10 e
x
max 5
Area f ( x) d x 2.784 10
x
min
Area
effective 296.214
Ttarget
52100 Steel
2 7.62 10 4 x
f ( x) 6.93 10 e xmin 125 xmax 460
x
max 5
Area f ( x) d x 2.909 10
x
min
Area
effective 309.476
Ttarget
55
1045 Steel
2 3.17 10 4 x xmin 185 xmax 1070

f ( x) 7.39 10 e
x
max 5
Area f ( x) d x 8.006 10
x
min
Area
effective 808.657
Ttarget
4140 Steel
2 3.48 10 4 x xmin 200 xmax 1020

f ( x) 7.29 10 e
x
max 5
Area f ( x) d x 7.417 10
x
min
Area
effective 749.153
Ttarget
4340 Steel
2 4.47 10 4 x
f ( x) 7.34 10 e xmin 145 xmax 780
x
max 5
Area f ( x) d x 5.751 10
x
min
Area
effective 580.867
Ttarget
8620 Steel
4
2 2.63 10 x xmin 125 xmax 990
f ( x) 8.01 10 e
x
max 5
Area f ( x) d x 8.04 10
x
min
Area
effective 812.132
Ttarget
56
9310 Steel
4
2 3.97 10 x xmin 180 xmax 870
f ( x) 7.35 10 e
x
max 5
Area f ( x) d x 6.266 10
x
min
Area
effective 632.96
T target
52100 Steel
4
2 3.75 10 x
f ( x) 7.07 10 e xmin 250 xmax 1020
x
max 5
Area f ( x) d x 6.932 10
x
min
Area
effective 700.163
Ttarget
57
1045 Steel
4
2 4.25 10 x xmin 145 xmax 870
f ( x) 7.61 10 e
x
max 5
Area f ( x) d x 6.872 10
x
min
Area
effective 660.812
Ttarget
4140 Steel
0.0004 x xmin 160 xmax 930

f ( x) 765.41 e
x
max 5
Area f ( x) d x 7.358 10
x
min
Area
effective 707.527
Ttarget
4340 Steel
2 3.77 10 4 x
f ( x) 7.32 10 e xmin 265 xmax 1080
x
max 5
Area f ( x) d x 7.718 10
x
min
Area
effective 742.079
Ttarget
8620 Steel
2 3.30 10 4 x xmin 115 xmax 940

f ( x) 8.05 10 e
x
max 5
Area f ( x) d x 7.928 10
x
min
Area
effective 762.354
Ttarget
58
9310 Steel
2 5.96 10 4 x xmin 135 xmax 650

f ( x) 7.48 10 e
x
max 5
Area f ( x) d x 4.887 10
x
min
Area
effective 469.865
Ttarget
52100 Steel
2 5.89 10 4 x
f ( x) 6.68 10 e xmin 190 xmax 730
x
max 5
Area f ( x) d x 4.75 10
x
min
Area
effective 456.703
Ttarget
59
Appendix 7: D2 vs. Effective Time Graphs
AISI 1045
1045 Comparison
4.00E-03
3.50E-03
850C
3.00E-03
2.50E-03 900C
2.00E-03 950C
1.50E-03 1000C
1.00E-03
1050C
5.00E-04
0.00E+00
0 100 200 300 400 500 600
1045 850C
1.60E-04
1.40E-04
1.20E-04
1.00E-04
8.00E-05
y = 6.65E-08x + 1.14E-04
6.00E-05
R = 4.79E-01
4.00E-05
2.00E-05
0.00E+00
0 100 200 300 400 500 600
60
1045 900C
3.00E-04

2.50E-04
2.00E-04
1.50E-04
y = 2.312E-07x + 1.337E-04
1.00E-04 R = 9.843E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
1045 950C
4.00E-04
3.50E-04
3.00E-04
2.50E-04
2.00E-04
y = 2.583E-07x + 2.190E-04
1.50E-04
R = 8.544E-01
1.00E-04
5.00E-05
0.00E+00
0 100 200 300 400 500 600
61
1045 1000C
2.50E-03
Average Grain Diameter2 (mm2) 2.00E-03
1.50E-03
y = 2.192E-06x + 9.717E-04
1.00E-03 R = 8.624E-01
5.00E-04
0.00E+00
0 100 200 300 400 500 600
1045 1050C
4.00E-03
3.50E-03
3.00E-03
2.50E-03
2.00E-03
1.50E-03 y = 3.728E-06x + 1.605E-03
R = 6.849E-01
1.00E-03
5.00E-04
0.00E+00
0 100 200 300 400 500 600
62
AISI 4140
4140 Comparison
1.80E-03
1.60E-03
1.40E-03 850C
1.20E-03
900C
1.00E-03
8.00E-04 950C
6.00E-04 1000C
4.00E-04
1050C
2.00E-04
0.00E+00
0 100 200 300 400 500 600
4140 850C
1.60E-04
1.40E-04
1.20E-04
1.00E-04
8.00E-05
y = 2.733E-08x + 1.184E-04
6.00E-05
R = 3.324E-01
4.00E-05
2.00E-05
0.00E+00
0 100 200 300 400 500 600
63
4140 900C
2.50E-04
2.00E-04
1.50E-04
y = 6.612E-08x + 1.570E-04
1.00E-04
R = 4.300E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
4140 950C
2.50E-04
2.00E-04
1.50E-04
y = 5.639E-08x + 1.863E-04
R = 3.365E-01
1.00E-04
5.00E-05
0.00E+00
0 100 200 300 400 500 600
64
4140 1000C
4.00E-04
3.50E-04
3.00E-04
2.50E-04
2.00E-04
1.50E-04 y = 1.275E-07x + 2.992E-04
R = 7.413E-01
1.00E-04
5.00E-05
0.00E+00
0 100 200 300 400 500 600
4140 1050C
1.80E-03
1.60E-03
1.40E-03
1.20E-03
1.00E-03
8.00E-04 y = 7.257E-07x + 1.166E-03
R = 9.872E-01
6.00E-04
4.00E-04
2.00E-04
0.00E+00
0 100 200 300 400 500 600
65
AISI 4340
4340 Comparison
1.60E-03
1.40E-03
850C
1.20E-03
1.00E-03 900C
8.00E-04 950C
6.00E-04
1000C
4.00E-04
1050C
2.00E-04
0.00E+00
0 100 200 300 400 500 600
4340 850C
1.35E-04
1.30E-04
1.25E-04
1.20E-04 y = 3.128E-08x + 1.148E-04

R = 7.527E-01
1.15E-04
1.10E-04
0 100 200 300 400 500 600
66
4340 900C
1.60E-04
1.40E-04
1.20E-04
1.00E-04
8.00E-05 y = 4.552E-08x + 1.299E-04
6.00E-05 R = 2.316E-01
4.00E-05
2.00E-05
0.00E+00
0 100 200 300 400 500 600
4340 950C
3.00E-04
2.50E-04
2.00E-04
1.50E-04
y = 1.277E-07x + 1.778E-04
1.00E-04
R = 6.374E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
67
4340 1000C
5.00E-04
4.00E-04
3.00E-04
y = 2.822E-07x + 3.376E-04
2.00E-04 R = 8.566E-01
1.00E-04
0.00E+00
0 100 200 300 400 500 600
4340 1050C
1.60E-03
1.40E-03
1.20E-03
1.00E-03
8.00E-04 y = 9.897E-07x + 9.267E-04
R = 6.731E-01
6.00E-04
4.00E-04
2.00E-04
0.00E+00
0 100 200 300 400 500 600
68
AISI 8620
3.00E-03
8620 Comparison
2.50E-03
850C
2.00E-03
900C
1.50E-03
950C
1.00E-03
1000C
5.00E-04 1050C
0.00E+00
0 100 200 300 400 500 600
8620 850C
1.60E-04
1.40E-04
1.20E-04
1.00E-04
8.00E-05
y = 3.394E-08x + 1.154E-04
6.00E-05 R = 4.216E-01
4.00E-05
2.00E-05
0.00E+00
0 100 200 300 400 500 600
69
8620 900C
3.00E-04
2.00E-04
1.50E-04
y = 1.647E-07x + 1.626E-04
1.00E-04
R = 8.082E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
8620 950C
7.00E-04
6.00E-04
5.00E-04
4.00E-04
3.00E-04
y = 7.647E-07x + 1.542E-04
2.00E-04
R = 9.339E-01
1.00E-04
0.00E+00
0 100 200 300 400 500 600
70
8620 1000C
1.20E-03

1.00E-03
8.00E-04
6.00E-04
4.00E-04 y = 1.329E-06x + 2.148E-04

R = 9.728E-01
2.00E-04
0.00E+00
0 100 200 300 400 500 600
8620 1050C
3.00E-03
2.50E-03
2.00E-03
1.50E-03
1.00E-03 y = 3.945E-06x + 4.889E-04

R = 9.796E-01
5.00E-04
0.00E+00
0 100 200 300 400 500 600
71
AISI 9310
9310 Comparison
2.50E-03
2.00E-03
900C
1.50E-03 950C
1.00E-03 1000C
5.00E-04 1050C
0.00E+00
0 100 200 300 400 500 600
9310 900C
2.50E-04
2.00E-04
1.50E-04
1.00E-04
y = 7.622E-08x + 1.229E-04
R = 1.424E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
72
9310 950C
2.00E-04
1.50E-04
1.00E-04
y = 8.745E-08x + 1.570E-04
5.00E-05 R = 9.764E-01
0.00E+00
0 100 200 300 400 500 600
9310 1000C
6.00E-04
5.00E-04
4.00E-04
3.00E-04
y = 5.473E-07x + 2.659E-04
2.00E-04
R = 9.249E-01
1.00E-04
0.00E+00
0 100 200 300 400 500 600
73
9310 1050C
2.50E-03

2.00E-03
1.50E-03
1.00E-03 y = 1.457E-06x + 1.200E-03

R = 5.142E-01
5.00E-04
0.00E+00
0 100 200 300 400 500 600
74
AISI 52100
52100 Comparison
0.0018
0.0016
0.0014 850C
0.0012 900C
0.001
950C
0.0008
0.0006 1000C
0.0004 1050C
0.0002
0
0.00 100.00 200.00 300.00 400.00 500.00 600.00
52100 850C
1.80E-04
1.60E-04
1.40E-04
1.20E-04
1.00E-04
8.00E-05
6.00E-05
y = -7.897E-08x + 1.408E-04
4.00E-05
R = 2.515E-01
2.00E-05
0.00E+00
0 100 200 300 400 500 600
75
52100 900C
2.50E-04

2.00E-04
1.50E-04
1.00E-04
y = 2.490E-08x + 1.936E-04
5.00E-05 R = 4.175E-02
0.00E+00
0 100 200 300 400 500 600
52100 950C
3.00E-04
2.50E-04
2.00E-04
1.50E-04
1.00E-04 y = 1.277E-07x + 1.778E-04

R = 6.374E-01
5.00E-05
0.00E+00
0 100 200 300 400 500 600
76
52100 1000C
8.00E-04

7.00E-04
6.00E-04
5.00E-04
4.00E-04
y = 3.956E-07x + 4.894E-04
3.00E-04
R = 9.974E-01
2.00E-04
1.00E-04
0.00E+00
0 100 200 300 400 500 600
52100 1050C
1.80E-03
1.60E-03
1.40E-03
1.20E-03
1.00E-03
8.00E-04 y = 1.648E-06x + 7.286E-04
R = 8.271E-01
6.00E-04
4.00E-04
2.00E-04
0.00E+00
0 100 200 300 400 500 600
77
Appendix 8: Log(K) vs. 1/T Graphs
y = -13244x - 3.2101
1045 R = 0.9307
-13
-13.5
-14
Log(Kp)
-14.5
-15
-15.5
0.00072 0.00076 0.0008 0.00084 0.00088 0.00092
1/T
4140 y = -9161.7x - 7.2669

R = 0.8173
-13.8
-14
-14.2
-14.4
Log(Kp)
-14.6
-14.8
-15
-15.2
-15.4
-15.6
0.00072 0.00076 0.0008 0.00084 0.00088 0.00092
1/T
78
y = -11174x - 5.4695
4340 R = 0.9576
-13.5
-14
-14.5
Log(Kp)
-15
-15.5
-16
0.00072 0.00076 0.0008 0.00084 0.00088 0.00092
1/T
y = -15054x - 1.7578
8620 R = 0.9828
-13
-13.5
-14
Log(Kp)
-14.5
-15
-15.5
0.00072 0.00076 0.0008 0.00084 0.00088 0.00092
1/T
79
9310 y = -14295x - 2.8691
R = 0.9059
-13.4
-13.6
-13.8
-14
Log(Kp)
-14.2
-14.4
-14.6
-14.8
-15
-15.2
0.00074 0.00076 0.00078 0.0008 0.00082 0.00084 0.00086
1/T
y = -18483x - 0.3912
52100 R = 0.9967
-13
-13.5
-14
Log(Kp)
-14.5
-15
-15.5
0.00074 0.00076 0.00078 0.0008 0.00082 0.00084 0.00086
1/T
80
Appendix 9: Micrographs
AISI 1045
Micrograph 1-1
Microstructure of AISI 1045 Steel, austenized at 850C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-
Picral Acid solution. Magnification is 200x.
81
Micrograph 1-2
Microstructure of AISI 1045 Steel, austenized at 850C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-
Micrograph 1-3
82
Micrograph 1-4
Micrograph 1-5
83
Micrograph 1-6
Micrograph 1-7
84
Micrograph 1-8
Micrograph 1-9
85
Micrograph 1-10
Micrograph 1-11
86
Micrograph 1-12
Micrograph 1-13
87
Micrograph 1-14
Micrograph 1-15
88
Micrograph 1-16
Micrograph 1-17
89
Micrograph 1-18
Micrograph 1-19
90
Micrograph 1-20
91
AISI 4140
Micrograph 2-1
92
Micrograph 2-2
Micrograph 2-3
93
Micrograph 2-4
Micrograph 2-5
94
Micrograph 2-6
Micrograph 2-7
95
Micrograph 2-8
Micrograph 2-9
96
Micrograph 2-10
Micrograph 2-11
97
Micrograph 2-12
Micrograph 2-13
98
Micrograph 2-14
Micrograph 2-15
99
Micrograph 2-16
Micrograph 2-17
100
Micrograph 2-18
Micrograph 2-19
101
Micrograph 2-20
102
AISI 4340
Micrograph 3-1
103
Micrograph 3-2
Micrograph 3-3
104
Micrograph 3-4
Micrograph 3-5
105
Micrograph 3-6
Micrograph 3-7
106
Micrograph 3-8
Micrograph 3-9
107
Micrograph 3-10
Micrograph 3-11
108
Micrograph 3-12
Micrograph 3-13
109
Micrograph 3-14
Micrograph 3-15
110
Micrograph 3-16
Micrograph 3-17
111
Micrograph 3-18
Micrograph 3-19
112
Micrograph 3-20
113
AISI 8620
Micrograph 4-1
114
Micrograph 4-2
Micrograph 4-3
115
Micrograph 4-4
Micrograph 4-5
116
Micrograph 4-6
Micrograph 4-7
117
Micrograph 4-8
Micrograph 4-9
118
Micrograph 4-10
Micrograph 4-11
119
Micrograph 4-12
Micrograph 4-13
120
Micrograph 4-14
Micrograph 4-15
121
Micrograph 4-16
Micrograph 4-17
122
Micrograph 4-18
Micrograph 4-19
123
Micrograph 4-20
124
AISI 9310
Micrograph 5-1
125
Micrograph 5-2
Micrograph 5-3
126
Micrograph 5-4
Micrograph 5-5
127
Micrograph 5-6
Micrograph 5-7
128
Micrograph 5-8
Micrograph 5-9
129
Micrograph 5-10
Micrograph 5-11
130
Micrograph 5-12
Micrograph 5-13
131
Micrograph 5-14
Micrograph 5-15
132
Micrograph 5-16
133
AISI 52100
Micrograph 6-1
134
Micrograph 6-2
Micrograph 6-3
135
Micrograph 6-4
Micrograph 6-5
136
Micrograph 6-6
Micrograph 6-7
137
Micrograph 6-8
Micrograph 6-9
138
Micrograph 6-10
Micrograph 6-11
139
Micrograph 6-12
Micrograph 6-13
140
Micrograph 6-14
Micrograph 6-15
141
Micrograph 6-16
Micrograph 6-17
142
Micrograph 6-18
Micrograph 6-19
143
Micrograph 6-20
144

Grain Growth Kinetics in Steels

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Grain Growth Kinetics in Steels

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Project Number: RDS 21381

Grain Growth Kinetics in Steels

Date: April 28, 2011

Table 1 - Material Composition Obtained via OES ........................................................................................ 9

Equation 1- Hall-Petch Equation ................................................................................................................... 5

2.1 Heat Treatment

Equation 1- Hall-Petch Equation

2.2.1 What is Grain Growth?

Equation 2 - Ideal Grain Growth Law

Equation 4 - Relationship between K and Heating Temperature T

2.2.2 Factors Affecting Grain Growth

2.2.2.1 Heating Rate

Equation 5: Zener Equation [10]

2.3.1 AISI 1045

2.3.2 AISI 4140

2.3.4 AISI 8620 Steel

2.3.5 AISI 9310 Steel

2.3.6 AISI 52100

2.3.7 Material Composition

Table 2: Functions of Alloying Elements [1]

Alloying Element Function

C To Control Strength Level and Hardenability

Cr Hardenability & Oxidation Resistance

Mo Hardenability & to Improve Creep Strength

Hardenability & to Improve Notch Toughness at

Ferrite Strengthening & to Improve Corrosion

As a Deoxidizer or to Reduce Core Losses in

3.1 Furnace Calibration

3.1.1 Temperature Mapping

3.1.2 Temperature Calibration

Figure 4 - Comparison of Thermocouple Connections [12]

3.2 Heat Treatment Procedure

Figure 5 - Heating Rate of 8620 to 900C

Heat Treatment: 900C 2 Hours

Figure 6 Time-Temperature Graph of 900C Heat Treatment

3.4 Optical Microscopy Measurements

3.4.1 Hyen Intercept Method

3.4.2 Jefferies Method

Figure 8 - Jefferies Method at 200x Magnification: 1045 850C 4Hr

4.1 Gain Size Evolution

0.5 Hours 2 Hours

Figure 9: Variation in Grain Size of AISI 4140 with Time at 1050C

4.2 Average Grain Diameters

0.5 Hours 2 Hours 4 Hours 9 Hours

4.3 ASTM Grain Size

Equation 6: ASTM Grain Size Equation

4.4 Effective Time

Equation 7: Heating Time Equation

Equation 8: Effective Time Equation

Alloy Temperature K (mm2/min) D0 (mm)

950 5.64E-08 0.0136

950 1.28E-07 0.0133

950 7.65E-07 0.0124

1000 5.47E-07 0.0163

950 1.28E-07 0.0133

Figure 12 - Log(Kp) vs. 1/T Comparison

1045 253.3 6.165E-04

4140 175.2 5.409E-08

4340 213.7 3.392E-06

8620 287.9 1.747E-02

9310 273.4 1.352E-03

52100 353.4 4.061E-01

5.1 Heat Treatment