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grain growth

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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

________________

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 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 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

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]

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.

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.

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

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]

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]

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.

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]

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]

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]

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]

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]

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

Mn Hardenability

Ni

Low Temperatures

P

Resistance

S To Improve Machinability

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.

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.

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.

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.

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.

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)

1000

900

800

Temperature (C)

700

600

500

400

300

200

100

0

0 2000 4000 6000 8000 10000

Time (S)

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.

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.

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]

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.

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

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.

4 Hours 9 Hours

17

850C 900C

950C 1000C

1050C

Figure 10: Variation of Grain Size of AISI 4140 with Temperature at 2 Hours

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

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.

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 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.

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

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

(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

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

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

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

1050 1.46E-06 0.0346

900 2.49E-08 0.0139

52100

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

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

24

5 Conclusions & Recommendations

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.

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.

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.

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.

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.

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.

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

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

http://www.suppliersonline.com/propertypages/8620.asp

[19] Sullivan Steel Service. Applications of 52100 Alloy Steel Tubing. [Online].

http://www.52100steel.com/about.html

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

29

Isothermal Transformation Diagram for AISI 4340 Steel

30

Isothermal Transformation Diagram for AISI 52100 Steel

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.

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.

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

Chunmin

Partial Grains 23 25 -8.00

Erik

Partial Grains 25 25 0.00

Lei

Partial Grains 22 25 -12.00

Sidath

Partial Grains 22 25 -12.00

Zhijia

Partial Grains 24 25 -4.00

Diameter (mm) ASTM Grain # Grain #

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

Chunmin

Partial Grains 28 30 -6.67

Erik

Partial Grains 33 30 10.00

Lei

Partial Grains 27 30 -10.00

Sidath

Partial Grains 28 30 -6.67

Zhijia

Partial Grains 28 30 -6.67

% Difference

Diameter (mm) ASTM Grain # Grain #

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

Temperature Effective ASTM Grain Size Avg Grain Diameter Kp (mm^2 / min) D0

(C) Time (min) # (mm) (mm)

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

Temperature Effective ASTM Grain Size Avg Grain Diameter Kp (mm^2 / min) D0

(C) Time (min) # (mm) (mm)

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

Temperature Effective ASTM Grain Size Avg Grain Diameter Kp (mm^2 / min) D0

(C) Time (min) # (mm) (mm)

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

(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.

# 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

Tabulated Effective Time for AISI 4140

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

Tabulated Effective Time for AISI 4340

# C (min) (min) Effective Time (min)

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

Tabulated Effective Time for AISI 8620

# C (min) (min) Effective Time (min)

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

Tabulated Effective Time for AISI 9310

# C (min) (min) Effective Time (min)

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

Tabulated Effective Time for AISI 52100

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

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

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

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

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

At T = 900 Celsius Ttarget 900 10

1045 Steel

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

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

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

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

At T = 950 Celsius Ttarget 950 10

1045 Steel

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

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

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

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

At T = 1000 Celsius Ttarget 1000 10

1045 Steel

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

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

At T = 1050 Celsius Ttarget 1050 10

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

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

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

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

Average Grain Diameter2 (mm2)

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

Effective Time (min)

1045 850C

1.60E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

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

Effective Time (min)

1045 950C

4.00E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

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

Effective Time (min)

1045 1050C

4.00E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

62

AISI 4140

4140 Comparison

1.80E-03

1.60E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

4140 850C

1.60E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

63

4140 900C

2.50E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

4140 950C

2.50E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

64

4140 1000C

4.00E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

4140 1050C

1.80E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

65

AISI 4340

4340 Comparison

1.60E-03

1.40E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

4340 850C

1.35E-04

Average Grain Diameter2 (mm2)

1.30E-04

1.25E-04

R = 7.527E-01

1.15E-04

1.10E-04

0 100 200 300 400 500 600

Effective Time (min)

66

4340 900C

Average Grain Diameter2 (mm2) 1.80E-04

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

Effective Time (min)

4340 950C

3.00E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

67

4340 1000C

Average Grain Diameter2 (mm2) 6.00E-04

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

Effective Time (min)

4340 1050C

1.60E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

68

AISI 8620

3.00E-03

8620 Comparison

Average Grain Diameter2 (mm2)

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

Effective Time (min)

8620 850C

1.60E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

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

Effective Time (min)

8620 950C

7.00E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

70

8620 1000C

1.20E-03

1.00E-03

8.00E-04

6.00E-04

R = 9.728E-01

2.00E-04

0.00E+00

0 100 200 300 400 500 600

Effective Time (min)

8620 1050C

3.00E-03

Average Grain Diameter2 (mm2)

2.50E-03

2.00E-03

1.50E-03

R = 9.796E-01

5.00E-04

0.00E+00

0 100 200 300 400 500 600

Effective Time (min)

71

AISI 9310

9310 Comparison

2.50E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

9310 900C

2.50E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

72

9310 950C

Average Grain Diameter2 (mm2) 2.50E-04

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

Effective Time (min)

9310 1000C

6.00E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

73

9310 1050C

2.50E-03

2.00E-03

1.50E-03

R = 5.142E-01

5.00E-04

0.00E+00

0 100 200 300 400 500 600

Effective Time (min)

74

AISI 52100

52100 Comparison

0.0018

0.0016

Average Grain Diameter2 (mm2)

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

Effective Time (min)

52100 850C

1.80E-04

Average Grain Diameter2 (mm2)

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

Effective Time (min)

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

Effective Time (min)

52100 950C

3.00E-04

Average Grain Diameter2 (mm2)

2.50E-04

2.00E-04

1.50E-04

R = 6.374E-01

5.00E-05

0.00E+00

0 100 200 300 400 500 600

Effective Time (min)

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

Effective Time (min)

52100 1050C

1.80E-03

Average Grain Diameter2 (mm2)

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

Effective Time (min)

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

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-

Picral Acid solution. Magnification is 200x.

Micrograph 1-3

Microstructure of AISI 1045 Steel, austenized at 850C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

82

Micrograph 1-4

Microstructure of AISI 1045 Steel, austenized at 850C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 1-5

Microstructure of AISI 1045 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

83

Micrograph 1-6

Microstructure of AISI 1045 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 1-7

Microstructure of AISI 1045 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

84

Micrograph 1-8

Microstructure of AISI 1045 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 1-9

Microstructure of AISI 1045 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

85

Micrograph 1-10

Microstructure of AISI 1045 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 1-11

Microstructure of AISI 1045 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

86

Micrograph 1-12

Microstructure of AISI 1045 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 1-13

Microstructure of AISI 1045 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

87

Micrograph 1-14

Microstructure of AISI 1045 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

Micrograph 1-15

Microstructure of AISI 1045 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

88

Micrograph 1-16

Microstructure of AISI 1045 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

Micrograph 1-17

Microstructure of AISI 1045 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

89

Micrograph 1-18

Microstructure of AISI 1045 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

Micrograph 1-19

Microstructure of AISI 1045 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

90

Micrograph 1-20

Microstructure of AISI 1045 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

91

AISI 4140

Micrograph 2-1

Microstructure of AISI 4140 Steel, austenized at 850C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

92

Micrograph 2-2

Microstructure of AISI 4140 Steel, austenized at 850C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-3

Microstructure of AISI 4140 Steel, austenized at 850C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

93

Micrograph 2-4

Microstructure of AISI 4140 Steel, austenized at 850C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-5

Microstructure of AISI 4140 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

94

Micrograph 2-6

Microstructure of AISI 4140 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-7

Microstructure of AISI 4140 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

95

Micrograph 2-8

Microstructure of AISI 4140 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-9

Microstructure of AISI 4140 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

96

Micrograph 2-10

Microstructure of AISI 4140 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-11

Microstructure of AISI 4140 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

97

Micrograph 2-12

Microstructure of AISI 4140 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-13

Microstructure of AISI 4140 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

98

Micrograph 2-14

Microstructure of AISI 4140 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-15

Microstructure of AISI 4140 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

99

Micrograph 2-16

Microstructure of AISI 4140 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 2-17

Microstructure of AISI 4140 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

100

Micrograph 2-18

Microstructure of AISI 4140 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 2-19

Microstructure of AISI 4140 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

101

Micrograph 2-20

Microstructure of AISI 4140 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

102

AISI 4340

Micrograph 3-1

Microstructure of AISI 4340 Steel, austenized at 850C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

103

Micrograph 3-2

Microstructure of AISI 4340 Steel, austenized at 850C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-3

Microstructure of AISI 4340 Steel, austenized at 850C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

104

Micrograph 3-4

Microstructure of AISI 4340 Steel, austenized at 850C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-5

Microstructure of AISI 4340 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

105

Micrograph 3-6

Microstructure of AISI 4340 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-7

Microstructure of AISI 4340 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

106

Micrograph 3-8

Microstructure of AISI 4340 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-9

Microstructure of AISI 4340 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

107

Micrograph 3-10

Microstructure of AISI 4340 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-11

Microstructure of AISI 4340 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

108

Micrograph 3-12

Microstructure of AISI 4340 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-13

Microstructure of AISI 4340 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

109

Micrograph 3-14

Microstructure of AISI 4340 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-15

Microstructure of AISI 4340 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

110

Micrograph 3-16

Microstructure of AISI 4340 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 3-17

Microstructure of AISI 4340 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

111

Micrograph 3-18

Microstructure of AISI 4340 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 3-19

Microstructure of AISI 4340 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

112

Micrograph 3-20

Microstructure of AISI 4340 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

113

AISI 8620

Micrograph 4-1

Microstructure of AISI 8620 Steel, austenized at 850C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

114

Micrograph 4-2

Microstructure of AISI 8620 Steel, austenized at 850C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 4-3

Microstructure of AISI 8620 Steel, austenized at 850C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

115

Micrograph 4-4

Microstructure of AISI 8620 Steel, austenized at 850C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 4-5

Microstructure of AISI 8620 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

116

Micrograph 4-6

Microstructure of AISI 8620 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 4-7

Microstructure of AISI 8620 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

117

Micrograph 4-8

Microstructure of AISI 8620 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 4-9

Microstructure of AISI 8620 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

118

Micrograph 4-10

Microstructure of AISI 8620 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 4-11

Microstructure of AISI 8620 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

119

Micrograph 4-12

Microstructure of AISI 8620 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 4-13

Microstructure of AISI 8620 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

120

Micrograph 4-14

Microstructure of AISI 8620 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 4-15

Microstructure of AISI 8620 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

121

Micrograph 4-16

Microstructure of AISI 8620 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 4-17

Microstructure of AISI 8620 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

122

Micrograph 4-18

Microstructure of AISI 8620 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 4-19

Microstructure of AISI 8620 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

123

Micrograph 4-20

Microstructure of AISI 8620 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 50x.

124

AISI 9310

Micrograph 5-1

Microstructure of AISI 9310 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

125

Micrograph 5-2

Microstructure of AISI 9310 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 5-3

Microstructure of AISI 9310 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

126

Micrograph 5-4

Microstructure of AISI 9310 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 5-5

Microstructure of AISI 9310 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

127

Micrograph 5-6

Microstructure of AISI 9310 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 5-7

Microstructure of AISI 9310 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

128

Micrograph 5-8

Microstructure of AISI 9310 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 5-9

Microstructure of AISI 9310 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

129

Micrograph 5-10

Microstructure of AISI 9310 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 5-11

Microstructure of AISI 9310 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

130

Micrograph 5-12

Microstructure of AISI 9310 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 5-13

Microstructure of AISI 9310 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

131

Micrograph 5-14

Microstructure of AISI 9310 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

Micrograph 5-15

Microstructure of AISI 9310 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

132

Micrograph 5-16

Microstructure of AISI 9310 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

133

AISI 52100

Micrograph 6-1

Microstructure of AISI 52100 Steel, austenized at 850C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

134

Micrograph 6-2

Microstructure of AISI 52100 Steel, austenized at 850C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 6-3

Microstructure of AISI 52100 Steel, austenized at 850C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

135

Micrograph 6-4

Microstructure of AISI 52100 Steel, austenized at 850C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 6-5

Microstructure of AISI 52100 Steel, austenized at 900C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

136

Micrograph 6-6

Microstructure of AISI 52100 Steel, austenized at 900C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 6-7

Microstructure of AISI 52100 Steel, austenized at 900C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

137

Micrograph 6-8

Microstructure of AISI 52100 Steel, austenized at 900C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 500x.

Micrograph 6-9

Microstructure of AISI 52100 Steel, austenized at 950C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

138

Micrograph 6-10

Microstructure of AISI 52100 Steel, austenized at 950C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 6-11

Microstructure of AISI 52100 Steel, austenized at 950C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

139

Micrograph 6-12

Microstructure of AISI 52100 Steel, austenized at 950C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 6-13

Microstructure of AISI 52100 Steel, austenized at 1000C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

140

Micrograph 6-14

Microstructure of AISI 52100 Steel, austenized at 1000C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 6-15

Microstructure of AISI 52100 Steel, austenized at 1000C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

141

Micrograph 6-16

Microstructure of AISI 52100 Steel, austenized at 1000C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 6-17

Microstructure of AISI 52100 Steel, austenized at 1050C for 0.5 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

142

Micrograph 6-18

Microstructure of AISI 52100 Steel, austenized at 1050C for 2 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 200x.

Micrograph 6-19

Microstructure of AISI 52100 Steel, austenized at 1050C for 4 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

143

Micrograph 6-20

Microstructure of AISI 52100 Steel, austenized at 1050C for 9 Hours then water quenched. Etchant utilized is an aqueous HCl-

Picral Acid solution. Magnification is 100x.

144

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