Two Cycle Heat Treatment (Austempering + Tempering) Of

Low C Equivalent Ductile Iron

THESIS

Submitted as a part of final year project, for the degree of

Bachelor Of Technology

By

Anirudh Kshemendranath (BT09MME018)

Piyush Patil (BT09MME045)

Priyanshu Bajaj (BT09MME053)

Vinayak Poddar (BT09MME070)

Under the guidance of:

Dr. S.U. Pathak Dr. A.A. Likhite

Professor Associate Professor

Department Of Metallurgy Department Of Metallurgy
And Materials Engineering And Materials Engineering

DEPARTMENT OF METALLURGICAL AND MATERIALS

ENGINEERING
VISVESVARAYA NATIONAL INSTITUTE OF TECHNOLOGY
NAGPUR – 440010

2012-13

1
 DEPARTMENT OF

METALLURCIGAL AND MATERIALS ENGINEERING

VISVESVARAYA NATIONAL INSTITUTE OF TECHNOLOGY

CERTIFICATE

This is to certify that the project work embodied in the thesis entitled “Two
Cycle Heat Treatment (Austempering + Tempering) of Low C
equivalentDuctile Iron” is genuine and has not been submitted to any other
university for any other degree. This bonafide work has been carried out by

Anirudh Kshemendranath (BT09MME018)

Piyush Patil (BT09MME045)

Priyanshu Bajaj (BT09MME053)

Vinayak Poddar (BT09MME070)

In partial fulfillment of the requirements for the award of the Degree of

Bachelor of Technology (Metallurgical and Materials Engineering) from
Visvesvaraya National Institute of Technology, Nagpur during 2012-13

Dr. S.U. Pathak Dr. A.A. Likhite

(Guide & Professor) (Guide & Professor)

Dr. S.G. Sapate

(Professor and Head of Department of Metallurgical & Materials Engineering)

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 ACKNOWLEDGEMENT

We wish to thank Dr. T. Srinivasan Rao, Director Visvesvaraya National

Institute Of Technology Nagpur, Dr. S.G. Sapate, Head of the Department of
Metallurgical and Materials Engineering, Dr. S.U. Pathak, Professor at
Department of Metallurgical and Materials Engineering and Dr. A.A. Likhite,
Associate Professor at Department of Metallurgical and Materials Engineering for
providing us an opportunity to work and study at VNIT Nagpur. We are extremely
grateful to Dr. S.U. Pathak and Dr. A.A. Likhite for guiding and encouraging us
throughout this project.

We are also obliged to Dr. D.R. Peshwe, Professor at Department of

Metallurgical and Materials Engineering, VNIT Nagpur. We would like to thank
Mr. Sunil Patil, Associate professor at Government College of Engineering,
Aurangabad for valuable support and previous testing parameters. The samples
which were used were obtained by the courtesy of M/s AB Castings, Butibori
Nagpur.

We are also very thankful to Mr. Vinayak Dakre, Post Doctorate student
at Department of Metallurgical and Materials Engineering, who has been a
constant pillar of support throughout the entire course of our work and has given
us all the help required. We would also like to make a special mention for Mr.
Aavishkar Rathod, Post Doctorate student at Department of Metallurgical and
Materials Engineering and Mr. Shrushrupal, Post Graduate student at
Department of Metallurgical and Materials Engineering.

We wish to express our gratitude to staff of Metallurgical and Materials

Engineering Of VNIT especially to Mrs. M D Jawale in-charge of the
Engineering Physical Metallurgy Laboratory; Mr. S L Gadge, in-charge of the
Chemical Characterization laboratory and the wear testing laboratory; Mrs. V A
Patankar, in-charge of the testing of Materials laboratory. We are extremely
grateful to all the faculty and staff of the Department of Metallurgical and
Materials Engineering for providing us unwavering guidance and support for the
entire four years of our bachelor‟s degree course

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 Abstract
The undiscovered pasture in the field of ductile iron, especially in
austempered ductile iron was the major reason which motivated all of us to choose
this topic. Our work is based on low C equivalent ductile iron. We referred to
research papers and ASM handbooks to get started on the topic and to gain some
vital information on the relevant topics.

Our main aim was focused on establishing a structure-property co-

relationship in the material provided to us i.e. Low C equivalent ductile iron. We
initially cut the samples into 3 parts and each was subjected to austenitizing
(850°C, 900°C and 950°C for 1 hr.) and austempering at 250°C for 2 hr. Thus we
obtained 3 samples of ADI and observed their microstructures. To provide the
aspect of physical properties, we even calculated the hardness (Rockwell hardness
tester) and wear properties (Pin Abrasion Test) of these samples. The next stage
was cutting two samples from each of the above three samples for tempering,
separately at two temperatures of 215°C and 336°C (decided on the basis of peaks
obtained in the DSC). The hardness and wear properties of these austempered +
tempered samples were also calculated.

Our results and discussions are focused on comparing this hardness and
wear results with a normal ADI (900°C 1 hr., 250°C 2 hr.) and even with a normal
ductile iron and thereby comment on material usage depending on these two
properties. We have also tried to establish a structure-property co-relationship for
the samples to explain the values of our hardness and wear.

We have tried our level best to give justification to the project with the
provided infrastructure and the basic knowledge in the field of Metallurgy &
Materials engineering. We have also included some suggestions in the end to carry
out some future work pertaining to this topic.

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 CONTENTS

Page No.

Cover Page 1

Certificate 2

Acknowledgement 3

Abstract 4

Contents 5

List Of Figures 7

List Of Tables 9

Chapter 1 – Introduction 10 - 20

1.1 Ductile Cast Iron 11 - 12

1.2 Composition of Ductile Iron 12
1.3 Applications of Ductile Iron 12 - 14
1.4 Structure of Ductile Iron 14 - 15
1.5 Types of Ductile Iron 15
1.6 Heat Treatment of Ductile Iron 15 - 18
1.7 Properties of ADI 19 - 20

Chapter 2 – Literature Review 21 - 31

2.1 Effect of Austenitizing temperature & time 23 - 25

2.2 Effect of Austempering temperature & time 26 - 28
2.3 Dual Stage Austempering treatment of ductile iron 28 – 30
2.4 Low carbon equivalent ductile iron. 30 - 31

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Chapter 3 – Experimental Details 32 - 51
3.1 Planning of experiment 33 - 34
3.2 Procedure 34 - 41

Chapter 4 – Results and discussions 42 – 53

4.1 Observations 43 – 52
4.2 Conclusion
o Microstructure Analysis, comparisons & discussions
o Comparison of properties & discussions 53
o Structure – Property Co-relationship

Chapter 5 – Suggestions 54 - 55

*References 56 - 58

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 List of Figures
1. Microstructures of ductile iron
2. Optical micrographs of ductile iron
3. It diagram of a processing sequence for austempering, with the ms and
mf decreasing as the γ is enriched with carbon during stage
4. Tensile strength versus elongation of ductile iron
5. Micrographs of ductile iron treated at different austempering
temperatures
6. Section of the fe-c-2% si equilibrium phase diagram showing a
metastable projection of the α +γ two phase field into the bainitic
transformation temperature range
7. Time to 5% transformed for a low-alloy ductile iron austenitized at 870
and 925 °C (1600 and 1700°F)
8. I T Diagram Illustrating the effect of Austenitizing Temperature
9. Measured carbon concentrations and volume fractions in ausferrite
together with calculated volume fractions assuming a two phase α+γ
ausferrite
10. Comparison of average properties of as-cast, single-step austempering
and two-step austempering materials.
11. EDM Cutting Machine
12. Polishing Wheel
13. Microstructures. A) Etchant: Picral B) Etchant: Sodium Metabisulphite
14. Optical Microscope
15. DSC Equipment
16. Furnace used for tempering.
17. ROCKWELL Hardness Tester
18. WEAR Test Machine

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19. Microstructure of the sample. Treatment given is 850°c 1 hr. and 250°c
2 hr. Etchant: 2% Nital, 500X
20. Microstructure of the sample a) 900°C 1hr. 250°C 2hr. b) 950°C 1hr.
250° 2hr. Etchant used: 2% Nital, 500X
21. Microstructure of the sample: a) 850°C 1hr. 250°C 2hr. b) 900°C 1hr.
250° 2hr. Etchant used: Picral, 500X
22. Microstructure of the sample, 950°C 1hr. 250° 2hr. Etchant used: Picral,
500X
23. Microstructure of the sample: a) 850°C 1hr. 250°C 2hr. b) 900°C 1hr.
250° 2hr. c) 950°C 1hr. 250° 2hr
24. Microstructure of the sample: a) 850°C 1hr. 250°C 2hr. b) 900°C 1hr.
250° 2hr. Etchant used: Sodium meta bilsulphite, 500X
25. Microstructure of the sample: 950°C 1hr. 250°C 2hr. Etchant used:
Sodium Meta bilsulphite, 500X
26. FIG 26: DSC Curves a) 850°C b) 900°C c) 950°C. All austempered at
250°C
27. FIG 27: Bar Graph Showing Wear Properties. (Wt. Loss in grams on X
axis)
28. FIG 28: Graph Showing Wear Properties (Wt. Loss % on Y axis)

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 List of tables
1. GENERAL COMPOSITION OF DUCTILE IRON

2. HARDNESS, TOUGHNESS, AND TENSILE PROPERTIES AT ROOM

TEMPERATURE FOR AUSTEMPERED DUCTILE IRON GRADES

SPECIFIED IN ASTM A 897 AND A 897M (METRIC)

3. COMPOSITION OF THE SAMPLE

4. COMPOSITION OF A NORMAL ADI SAMPLE

5. HARDNESS VALUES AFTER AUSTEMPERING AT 3

TEMPERATURES, ALSO AS-CAST SAMPLE WITH NO HEAT

TREATMENT

6. HARDNESS VALUES AFTER TEMPERING

7. DSC ANALYSIS TABLE

8. WEAR TEST RESULTS – WEIGHT LOSS

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Introduction

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 1. Introduction
1.1 DUCTILE CAST IRON

Previously known as nodular iron or spheroidal-graphite (SG) cast iron (the

international term is ductile iron), is cast iron in which the graphite is present as
tiny spheres (nodules) In ductile iron, eutectic graphite separates from the molten
iron during solidification in a manner similar to that in which eutectic graphite
separates in gray cast iron. However, because of additives introduced in the molten
iron before casting, the graphite grows as spheres, rather than as flakes of any of
the forms characteristic of gray iron. Cast iron containing spheroidal graphite is
much stronger and has higher elongation than gray iron or malleable iron. It may
be considered as a natural composite in which the spheroidal graphite imparts
unique properties to ductile iron. [17]

a b

FIG 1. MICROSTRUCTURES OF DUCTILE IRON.

(a) As-cast ferritic. (b) As-cast pearlitic; hardness, 255 HB. (c) Ferritic, annealed 3h
at 700 °C (1290 °F). (d) Pearlitic ductile iron oil quenched and tempered to 255 HB.
All etched in 2% nital. 100×

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 The relatively high strength and toughness of ductile iron give it an
advantage over gray iron or malleable iron in manystructural applications. Also,
because ductile iron does not require heat treatment to produce graphite nodules
(as does malleable iron to produce temper-carbon nodules), it can compete with
malleable iron even though it requires a treatment and inoculation process. The
mould yield is normally higher than with malleable iron. Ductile iron can be
produced to x-ray standards because porosity stays in the thermal centre.
Malleable iron cannot tolerate porosity because voids migrate to the surface of hot
spots such as fillets and appears as cracks.

In recent years, considerable interest has been shown in the property

improvements obtained in ductile iron by austempering heat treatments.
Austempered ductile iron (ADI) has a matrix that is a combination of acicular
(bainitic) ferrite and stabilized austenite. As the matrix structure is progressively
varied from ferrite to ferrite plus pearlite to pearlite to bainite and finally to
martensite, hardness, strength, and wear resistance increase, but impact resistance,
ductility, and machinability decrease. However, these structures results in an
exceptional combination of strength, ductility, and wear resistance. The following
is the general composition of ductile iron [17]

1.2 Composition Of Ductile Iron

Composition, %
TC Mn Si Cr Ni Mo Cu P S Ce Mg
3.6- 0.15- 1.8- 0.03- 0.05- 0.01- 0.15- 0.03 0.002 0.005- 0.03-
3.8 1.00 2.8 0.07 0.2 0.1 1.00 max max 0.02 0.06
TABLE 1: GENERAL COMPOSITION OF DUCTILE IRON [17]

1.3 Applications Of Ductile Iron

Some of the applications for austempered ductile iron include:

• Gears (including side and timing gears)
• Wear-resistant parts
• High-fatigue strength applications
• High-impact strength applications
• Automotive crankshafts
• Chain sprockets
• Refrigeration compressor crankshafts
• Universal joints
• Chain links
• Dolly wheels

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 Ductile iron castings are used for many structural applications, particularly
those requiring strength and toughness combined with good machinability and low
cost. The selection of casting, instead of mechanical fabrication, as the production
process oftenallows the designer to:
• Use to best advantage the combination of properties that is unique to ductile iron
• Combine several functions (or component shapes) in a single integrated
configuration
• Realize the economic advantages inherent in casting, which is the simplest and
most direct of the various production processes.

Casting is like forming with a homogenous liquid that can flow smoothly
into a wide variety of thicknesses, shapes, andcontours. The material is consistent
piece to piece, day after day because it is made from a pattern that has very low
wear anddimensional change and that is produced to a specification. The
microstructure is uniform, with neither directional flow lines norvariations from
weld junctions or heat-affected zones. Any porosity is predictable and remains in
the thermal centre. Machiningcosts are low because there is less material to
remove and to dispose of, castings are easier to machine, and cutting tools
aresubjected to less tool wear.Properties unique to ductile iron include the ease of
heat treating because the free carbon in the matrix can be redissolved toany
desired level for hardness and strength control. Free carbon can be selectively
hardened by flame, induction, laser, or electronbeam. A 650 °C (1200 °F) anneal
for 3 h can produce high toughness at low temperatures. Ductile iron can be
austempered tohigh tensile strength, high fatigue strength, high toughness, and
excellent wear resistance. Second, lower density makes ductileiron weigh 10%
less than steel for the same section size. Third, the graphite content provides
damping properties for quiet running gears. Also, the low coefficient of friction
produces more efficient gear boxes. Furthermore, ductile iron has fewer tendencies
to gear seizures from the loss of lubricant.Experience has proved that ductile iron
works in applications in which experience and handbook data say it should not.
This isbecause data in the literature do not describe the true properties of ductile
iron, whereas it is very easy to make a prototypecasting and try it in the field. This
practice has resulted in very large cost savings and superior performance
compared to thematerial it replaces. A ductile iron casting can be poured and
shipped the same day. As-cast ductile iron castings are consistent indimensions
and weight because there is no distortion or growth due to heat treatment.

Austempered ductile iron has resulted in many new applications for ductile
iron. It is a high-strength, wear-resistant,heat-treated material. It has more than
double the strength of conventional ductile iron for a given level of ductility.
Austempered ductile iron gets its remarkable properties from a special
austempering heat treatment. The resultant strengthproperties can be varied by
controlling the heat treat cycle. Inthe austempering process, good-quality ductile

13
iron can be transformed into a superior engineering material. It cannot
transformpoor-quality iron into a good-quality material. [17]

1.4 Structure [18]

The microstructure of ductile iron constitutes of: the morphological forms
taken by carbon and the metal matrix in which the carbon and/or carbide particles
are dispersed. The following important microstructural components are found in
ductile iron.
Graphite:
Graphite is the most stable form of pure carbon in cast iron. Some of the
physical properties of graphite are as follows: low density, low hardness, high
thermal conductivity & Lubricant.
In cast iron graphite shape may vary from flake to spherical. In ductile iron all of
its graphite occurs in spheroidal form microscopically and it constitutes about 10%
by volume of ductile iron.
Ferrite:
This is an interstitial solid solution of carbon in Alpha Iron and also the
purest iron phase in a cast iron. Ferrite offers lower strength and hardness, but it is
very ductile in nature which gives high ductility and toughness. Austempered
Ductile Iron (ADI) contain acicular ferrite (very fine grained), which provides a
good combination of strength with ductility and toughness. In ferritic ductile iron
the strength properties are generally increased by the elements, which go into the
solution.
Pearlite:
Pearlite is a eutectoid mixture of cementite and ferrite produced by the
eutectoid reaction. It provides higher strength but at the expense of reduction in
the ductility which meets the requirements of many engineering applications.
Martensite:
It is a supersaturated solid solution of carbon in iron produced by rapid
cooling or “quenching”. It is very hard and brittle but ductility is very low. To
increase the ductility it is normally “tempered” i.e. heat treated which reduces the
carbon content by the precipitation of carbides.
Austenite:
It is a high temperature phase consists of carbon dissolved in iron. Nickel
stabilizes the austenitic irons and the amount of Ni should be in the range of 18 to
36%. In austempered ductile irons, austenite is produced by a combination of rapid
cooling, suppress the pearlite formation. Supersaturation of carbon during
austempering, depresses the start of the transformation of the austenite to
martensite far below room temperature. The austenite matrix provides ductility
and toughness at all temperatures corrosion resistance and good high temperature
properties, especially under thermal cycling conditions.

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Bainite:
Bainite is a mixture of ferrite and carbide (Fe3C, Fe2.4C) produced by heat
treatment or alloying. [18]

1.5 Types of ductile iron [19, 20]

The different types of ductile iron are as follows:
Ferritic Ductile Iron
Ferritic ductile iron is formed when graphite spheroids are present in a matrix
of ferrite. It provides an iron with good ductility and impact resistance with a
tensile and yield strength equivalent to low carbon steel. It can be produced as-cast
and an annealing heat treatment may be given to assure maximum ductility and
low temperature toughness.
Ferrito- Pearlitic Ductile Iron
These are the most common grade of ductile iron where the graphite spheroids
are present in a matrix containing both ferrite and pearlite. It is produced as-cast
and its properties are intermediate between ferritic and pearlitic grades along with
good machinability and low production costs.
Pearlitic Ductile Iron
In these type of ductile iron the graphite spheroids are present in a matrix of
pearlite which results in high strength, good wear resistance, and moderate
ductility and impact resistant. It also shows good machinability.
Martensitic Ductile iron
The graphite spheroids are present in a matrix of martensite. Sufficient alloy
additions to prevent pearlite formation, and a heat treatment (quench and
tempered) produces this type of ductile iron.This type of ductile iron develops
very high strength and wear resistance but with lower levels of ductility due to
tempered martensite matrix.
Austenitic Ductile Iron
When the iron is alloyed to produce an austenitic matrix this type of ductile
iron is produced. It offers good corrosion and oxidation resistance good strength
and dimensional stability at elevated temperatures.

1.6 Heat Treatment Of Ductile Iron [1]

DUCTILE CAST IRONS (also known as nodular or spheroidal graphite

iron), are primarily heat treated to create matrixmicrostructures and associated
mechanical properties not readily obtained in the as-cast condition. As-cast
matrixmicrostructures usually consist of ferrite or pearlite or combinations of both,
depending on cast section size and/or alloycomposition.

15
The most important heat treatments and their purposes are:
 Stress relieving, a low-temperature treatment, to reduce or relieve internal
stresses remaining after casting.
 Annealing, to improve ductility and toughness, to reduce hardness, and to
remove carbides.
 Normalizing, to improve strength with some ductility.
 Hardening and tempering, to increase hardness or to improve strength and
raise proof stress ratio.
 Austempering, to yield a microstructure of high strength, with some
ductility and good wear resistance.
 Surface hardening, by induction, flame, or laser, to produce a locally
selected wear-resistant hard surface.

The normalizing, hardening, and Austempering heat treatment, which involve

austenitization followed by controlled cooling or isothermal reaction, or a
combination of the two, can produce a variety of microstructures and greatly
extend the limits on the mechanical properties of ductile cast iron. These
microstructures can be separated into two broad classes:
 Those in which the major iron-bearing matrix phase is the
thermodynamically stable body-centered cubic (ferrite) structure.
 Those with a matrix phase that is a metastable face-centered cubic
(austenite) structure

The former are usually generated by the annealing, normalizing, normalizing

and tempering, or quenching and tempering processes. The latter are generated by
Austempering, an isothermal reaction process resulting in a product called
Austempered ductile iron (ADI) [1]

FIG. 2. OPTICAL MICROGRAPHS OF DUCTILE IRON WITH

(a) A ferritic matrix in an annealed casting, (b) fine pearlitic matrix in a normalized
casting, and (c) a martensitic matrix in a quenched casting. Etched in nital;
approximate magnifications shown
[1]

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FIG 3. GIVEN BELOW IS THE IT DIAGRAM OF A PROCESSING SEQUENCE
FOR AUSTEMPERING, WITH THE MS AND MF DECREASING AS THE Γ IS
ENRICHED WITH CARBON DURING STAGE. [1]

17
 _

FIG 4. TENSILE STRENGTH VERSUS ELONGATION OF DUCTILE

IRON. (a) Minimum values given in various standards. (b) Minimum values
of austempered ductile iron grades specified in ASTM A 897. (c) Range of
tensile strength and elongation values with different heat treatments [1]

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 1.7 Properties Of ADI [1]

It is obvious from Fig. 4(b) And 4(c) that ADI is a unique cast iron material
with tensile properties attributable to γH with the fine dispersion of ferrite. As
outlined above, Austempering is accomplished by heating the casting to a
temperature in the austenite-phase range (usually 815 to 925 °C, or 1500 to 1700
°F), holding for the time required to saturate the austenite with carbon, cooling to a
temperature above the Ms temperature at a rate sufficient to avoid the formation of
pearlite or other mixed structures, and then holding at that Austempering
temperature for the time required to produce the optimum structure of acicular
ferrite and carbon-enriched austenite. [1]

The properties of ADI can be varied by changing the Austempering

temperature. A lower transformation temperature (260 °C, or 500 °F) produces a
fine, high strength, wear-resistant structure (Fig. 5a). A higher transformation
temperature (370 °C or 700 °F) results in a coarser structure that exhibits high
fatigue strength and good ductility.(Fig. 5b)

TABLE 2: HARDNESS, TOUGHNESS, AND TENSILE PROPERTIES AT ROOM

TEMPERATURE FOR AUSTEMPERED DUCTILE IRON GRADES SPECIFIED
IN ASTM A 897 AND A 897M (METRIC) [1]

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 FIG. 5 MICROGRAPHS OF DUCTILE IRON TREATED AT DIFFERENT
AUSTEMPERING TEMPERATURES.
(a) Ductile iron austempered at 260 °C (500 °F) exhibits a fine acicular structure
with the following properties: tensile strength, 1585 MPa (230 ksi); yield strength,
1380 MPa (200 ksi); elongation, 3%; unnotched impact, 54 J (40 ft · lbf);
hardness, 475 HB. (b) Same iron as in (a) austempered at 370 °C (700 °F) exhibits
a coarse acicular structure with the following properties: tensile strength, 1035
MPa (150 ksi); yield strength, 825 MPa (120 ksi); elongation, 11%; unnotched
impact, 130 J (95 ft · lbf); hardness, 321 HB. Both etched with 3% nital. 300×. [1]

20
Literature Review

21
2 Literature Study
A lot of work has been done in the field of Austempered ductile iron and lot of
literature is thus available on this.

Our study was focused mainly on:

 Effects of various processing parameters on microstructure and engineering

properties –
o Effect of Austenitizing temperature
o Effect of Austenitizing time
o Effect of Austempering temperature
o Effect of Austempering time
 Two step Austempering treatment of ductile iron
 Works in the field of low carbon equivalent ductile iron.
 Structure property co-relationship

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2.1 Effect of Austenitizing temperature and time:

Fig 6: Section of the Fe-C-2% Si equilibrium phase diagram showing a metastable

projection of the α +γ two phase field into the bainitic transformation temperature
range [1]

23
 Karl B. Rundman, Department of Metallurgical and Materials Engineering,
Michigan Technological University in his article Heat Treating of Ductile Iron [1]
gives the 2% Si section of the iron-carbon-silicon phase diagram (Figure 6), he
explains that as the austenitizing temperature is increased the carbon content of the
austenite phase increases. Now, since the carbon concentration of the austenite
increases the martensitic transformation start temperature or Ms Temperature
decreases as the austenitising temperature increases.Here, he also mentions that
Austenitizing time should be decided on the basis of alloy content, the original
microstructure, and the section size. Austenitizing time of 2 hours is usually
sufficient.

In year 1990, D.J. Moore, B.S. Shugart, K.L. Hayrynen, and K.B.
Rundman, studied the transformation rates during Austempering process of low
alloy ductile iron at various Austempering temperatures, for samples austenitized
at two different temperatures (8700C and 9250C). They found that as the
Austenitizing temperature is increased the rate of ausferrite reaction decreases. [2]
In figure 7, it can be seen that the rate of ausferrite reaction is higher for higher
austenitizing temperature at all austempering temperatures.

Fig 7: Time to 5% transformed for a low-alloy ductile iron austenitized at

870 and 925 °C (1600 and 1700°F) [2]

24
 T.N. Rouns and K.B. Rundman studied the kinetics of Austempering
reactions. They showed that the increase in transformation rate on decreasing
Austenitizing temperature is attributed to an increased thermodynamic driving
force for the reaction. They also noted that with decreasing austenitizing
temperature the fineness of ferrite needles increased. [3]

Thus it can be said that change in Austenitizing temperature effects final

product of Austempering (ausferrite product) in two ways; as explained by K. B.
Rundman. [4] Rundman explains that decreasing austenitizing temperature effects
austempering reaction in ways (figure 8):

 Rate of ausferrite reaction is increased.

 Ms Temperature increases, as the carbon content of the austenite phase
decreases with decreasing austenitizing temperature.

These effects result in finer acicular ferrite needles which improves hardness
and strength of the ADI.

Fig 8: I T Diagram illustrating the effect of Austenitizing Temperature [4]

25
2.2 Effect of Austempering temperature and time:

In 1988, K. B. Rundman, D.J.Moore, K.L.Hayrynen, W.J. Dubensky, T.N.

Rouns showed a massive study on structure property correlation of ADI. They
made measurements of the metastable carbon content in ductile iron austempered
at different temperatures. Their results showed that as austempering temperature
decreases, the metastable carbon content in the matrix austenite increases. [ 5 ]
This can be explained by the phase diagram shown below (Figure 9). Clearly the
carbon content of austenite formed at 3160C is greater than austenite formed at
3710C

In 1985, W. Dubensky conducted a massive electron microscope study of

ADI; his aim was to study carbide formation during Austempering process. With
this study he showed that at low austempering temperatures (< 3710C) iron carbide
was present in the ausferrite product. [6]

In the year 2003, J.R. Parolini and D. J. Moore studied the effect of
Austempering temperature on the amount of austenite present in ausferrite phase.
They worked on samples with same initial composition austempered at 3710C and
3160C. it was found that as the Austempering temperature decreases the relative
amount of austenite in ausferrite also decreases. They compared their results with
the results expected on the basis of phase diagram (Figure 9), and noted that the
actual decrease in amount of austenite was much higher than expected. Also the
deviation from the phase diagram increases as the temperature is lowered. [7]The
reason for high variation from lever rule at lower temperatures (< 3710C) may be
the formation of carbides at these temperatures.

26
Fig 9: Measured carbon concentrations and volume fractions in ausferrite together
with calculated volume fractions assuming a two phase α+γ ausferrite. [7]

S. S. Umale1, P. P. Parhad, Ajay Likhite and S. U. Pathak, in 2012 studied

hardness and microstructures of ductile iron austempered at 2500C and 5000C, and
Austempering time from 1 hour to 8 hours. They found that hardness of ADI
decreases with increasing Austempering temperature or increasing Austempering
time at a same temperature. Their microstructural study showed an increase in
amount of ferrite needles and austenite, and a decrease in that of martensite with
increasing austempering time. [8] Their results also indicated that for
Austempering time less than 3 hours, higher hardness was obtained at lower
Austempering temperatures for the same alloy and same Austempering time.

In 1986, Doong J. L., Ju F. C., Chen H. S. and Chen L. W. studied fracture

of ADIs austempered at different temperatures; they found that ADIs austempered
at low temperatures show higher fracture toughness than those austempered at
higher temperatures. [ 9 ]

27
 In 1995, Putatunda S. K. and Singh I. related facture toughness of
Austempered Ductile Iron to the yield strength and some microstructural features
by the following relationship [ 10 ]:

Klc2 = σYS (XyCy)1/2

Where, Klc is the fracture toughness,
σYS is the yield strength,
Xy is the volume fraction of the stabilized austenite
Cy is the carbon content of the stabilized austenite

Now, as Xy and Cy depend on Austempering temperature and time, we can

also relate fracture toughness with these parameters.

Also, it was noted that Xy increases as Austempering temperature is

increased and Cy increases when it is decreased. Thus to get maximum fracture
toughness work started in dual stage Austempering. [12]

2.3 Dual stage Austempering:

In this treatment the metal is subjected to two temperatures during

Austempering treatment before it is cooled down to room temperature.

In 2001, CHENG-HSUN HSU and TAO-LIANG CHUANG studied effect

of two stage Austempering process on fracture toughness of Austempered Ductile
Iron. They compared the fracture toughness and hardness of a sample subjected to
two stage Austempering (3600C, 8 min. followed by 3000C, 172 min.) with a
sample austempered at higher temperature (3600C, 1 to 3 hours) and a sample
austempered at lower temperature (3000C, 1 to 3 hours). [11] Their results showed
that two-stage ADI possesses both high fracture toughness (77.8 MPam1/2) and
high hardness (331 BHN). Microstructural analysis also showed that ADI
subjected to two stage Austempering has higher amount of retained austenite and
the more-inter- woven and less-sharp ferrite needles in the ausferrite matrix.Their
results are shown below (Figure 10)

28
Fig 10: Comparison of average properties of as-cast, single-step austempering and
two-step austempering materials. [11]

29
 In the same year Putatunda S claimed to have developed Austempered
Ductile Iron having high strength and fracture toughness by a similar two stage
Austempering treatment. He reported a significant improvement in mechanical
properties and fracture toughness of the material as result of the two-stage
austempering process. [12]

In 2008, Ravishankar K.S., K. Rajendra Udupa and P. Prasad Rao studied

the effect of varying step time in two stage Austempering of ductile iron. They
subjected the samples to two stage Austempering with first stage at 3000C and
time ranging from 10 min to 60 min; and second stage at 4000C for 2 hours. They
compared these samples with samples subjected to conventional single step
Austempering for 2 hours at temperatures ranging from 2800C to 4000C. [13]
Their results showed that the retained austenite content decreases with increasing
time in the first stage (First stage being at lower temperature), while the carbon
content of the retained austenite increases. This was reflected in an increased in
tensile and yield strength and a decrease in ductility and tensile toughness.They
also found an improvement in fracture toughness which they attributed to
reduction in ferrite needle size and increase in carbon content of retained austenite
leading to more stability.

2.4 Low carbon austempered cast iron:

Not much work has been done in this direction, and hence very little
information is available.

John R. Keough, Bela V. Kovacs and Douglas M. Pramstaller were granted

patent in 1991 for a method of producing high Si, low C Austempered Cast Iron.
[14] This was a method for preparing an austemperable cast iron which produces
an ausferritic matrix, the cast iron had a silicon content of from about 1.6 to about
2.4 weight percent (preferably 1.8 weight percent) and a carbon content of from
about 1.6 to about 2.2 weight percent (preferably 2.0 weight percent), such that the
carbon equivalent of the cast iron is from about 2.1 to about 3.0 weight percent.
Most desirable compositions would have a carbon equivalent of about 2.6 weight
percent. Manganese content is preferably kept between 0.1 and 0.8 weight percent.

30
 In 2012, S. S. Umale1, P. P. Parhad, Ajay Likhite and S. U. Pathak
compared hardness and microstructures of a low CE ductile iron (CE = 2.58) with
a normal Ductile Iron (CE = 4.38) austempered at 2500C and different
austempering times (2 hours to 8 hours). They found that ADI with low CE exhibit
higher hardness than that of conventional ADI after austempering. [8]

In 2008, SinivasmurthyDaber and P. Prasad Rao studied the effect of

microstructure on the formation of strain induced martensite in Austempered
Ductile Iron. It was found that strain hardening behavior improved with increasing
austempering temperature in single step austempering and by reducing time at first
step (low temperature) in two stage austempering. It was also concluded that
propensity of strain induced martensite is greater in samples containing more of
blocky austenite. [16]

31
Experimental Work

32
3 Experimental Work
3.1 Planning Of Experiment

In the ductile iron family not much work has been done on low C
equivalent ductile iron and it would be an interesting proposition to observe the
microstructural changes and the corresponding changes in the physical properties
of this material. Our experiment focuses on dual heat treatment cycle to this low C
equivalent ductile iron and then establishing a structure property co relation based
on the changes observed in the microstructure and in the mechanical properties of
hardness and wear resistance.

The sample was taken and initially subjected to austenitizing at three

different austenizing temperatures and then they were subsequently held at a
temperature (Austempering). The microstructures, hardness and wear properties of
this ADI was taken and were carefully examined various etchants to observe
distinct phases. These samples were further subjected to tempering to study the
improvement in their properties. The temperature for tempering was decided based
upon the peaks observed in the DSC.

The sample chosen for the experiment is:

Low carbon equivalent ductile cast iron

Element C Si Mn S P Cr Cu Ni C
Equivalent

% 2.16 1.42 0.83 0.013 0.027 - 0.6 0.57 2.64

TABLE 3: COMPOSITION OF THE SAMPLE

33
 The thing to note about the given sample is that there is a clear absence of
carbide forming elements barring iron carbides which will be discussed later.

This sample was cut into 3 parts and each was subjected to different
austenitizing temperatures. The quenching media used for Austempering these
samples was a salt bath which will also be discussed in detail. After Austempering
in the salt bath, the samples were allowed to cool till room temperature and then
subsequent investigations were carried out.

Comparison of the results obtained formed an integral part of the experiment. The
As- Cast sample, a normal ADI sample and our sample i.e. low C equivalent
ductile iron were compared based on their hardness and wear properties.

3.2 Procedure:

3.2.1 Austenitizing and Austempering Treatment

The usual objective of austenitizing is to produce an austenitic matrix with as

uniform a carbon content as possible prior to thermal processing. For a typical
hypereutectic ductile cast iron, an upper critical temperature must be exceeded so
that the austenitizing temperature is in the two-phase (austenite and graphite) field.
This temperature varies with alloy content, the "equilibrium" austenite carbon
content in equilibrium with graphite increases with an increase in austenitizing
temperature. This ability to select (within limits) the matrix austenite carbon
content makes austenitizing temperature control important in processes that
depend on carbon in the matrix to drive a reaction.
The austenitizing treatment was decided to be carried out at three different
temperatures 850°C, 900°C and 950°C. The samples were held at the respective
austenitizing temperature for 1 hour.
The samples were then given austempering treatment by quenching in a salt
bath (Hot Oil Quench, Meta quench 44) maintained at 250°C for 2 hours and then
cooled in air to room temperature.
This austempering temperature is in lower ranges, also austempering time
was short and hence a mixed phase of martensite and ausferrite is expected. [8]

34
 3.2.2 Sample Cutting

The samples were procured from a runner from a foundry. The parts were
cut using a Wire Cut- Electric discharge machining (EDM). The workpiece and
the wire represent positive and negative terminals in a DC electrical circuit, and
are always separated by a controlled gap, constantly maintained by the machine.
This gap, filled with a dielectric fluid, acts as an insulator and cooling agent.
Sparks are formed through a sequence of rapid electrical pulses, generated by the
machine‟s power supply thousands of times per second. Each spark forms an
ionization channel under extremely high heat and pressure, in which particles flow
between the wire electrode and the workpiece, resulting in vaporization of
localized sections, thus cutting the sample. [21]

Fig 11: EDM Cutting Machine

35
 3.2.3 Sample Preparation for metallographic studies

The surfaces of the samples were flattened on a bench grinder. These

flattened samples were then prepared for metallographic studies under
microscopes and image analyzer by following steps:-

FIG 12: Polishing Wheel

1. The samples were first rough grinded on belt sander. The rough grinding
process was carried out till sample surface became flat and free of nicks,
burrs etc. and all the scratches due to bench grinder wheel were no longer
visible.
2. Now the samples were subjected to intermediate polishing on emery papers
containing successively finer abrasives. These papers are generally 1/0, 2/0,
3/0 4/0 respectively according to the fineness of the abrasive increasing
from 1/0 to 4/0. Roughly ground samples were rotated by 90o before
polishing them on paper 1/0. This is done in order to be able to clearly
distinguish between scratches due to rough grinding and those due to paper
1/0. Every time switching between the papers the sample was rotated by
90o. The pressure applied goes on decreasing as we go from 1/0 to 4/0 so
that the scratches become more and more finer. The operation has to be
carried out very carefully. Care was taken so that no scratches from any
earlier paper or that od rough grinding were present after polishing on paper
4/0. Only scratches due to 4/0 were present.
3. Now the samples were subjected to fine polishing. The final approximation
to flat scratch free surface is obtained by use of a wet rotating wheel
covered with a special cloth that is charged with carefully sized abrasive

36
 particles. The abrasives used polishing ADI samples are gamma form of
aluminum oxide. After fine polishing on cloth, the polished sample was
scratch free when observed under optical microscope.
4. After polishing was done the sample were washed under tap water. After
that they were given alcohol treatment i.e. few drops of methyl alcohol
were put on the polished surface and held till the alcohol dries out. This
treatment allowed the removal of water marks that were present during
washing under tap water.
5. The samples were etched by the etchants prepared and the resulting
microstructures were viewed under an Light optical Microscope.

3.2.4 Etchant Preparation and Microstructural Imaging [22]

In order to view the different microstructural aspects of the samples, several

etchants were prepared and the microstructures of the samples were viewed under
the optical microscope.

1. NITAL
This is the most common etchant whose composition is 96- 98 ml ethanol
with 2 ml nitric acid. It reveals the alpha grain boundaries and constituents.
It is used by immersion of the sample in the solution for 60s.
2. PICRAL
The etchant is recommended for structures consisting of ferrite and
carbides, since it is used to delineate the structure. The composition is 2g of
picric acid added to 100 ml of ethanol.
3. SODIUM META BISULFITE (SMB)
This etchant is used to detect the presence of untempered martensite. The
composition consists of 10 g sodium pyrosulfite (Na2S2O5) added to 100
mL distilled water. Tints as-quenched martensite into brown; Acicular
ferrite into blue; carbides and residual austenite are left unaffected. We
need to immerse sample in etchant solution for approximately 20 s.
4. ALKALINE SODIUM PICRATE (ASP)
2 g picric acid ((NO2)3C6H2OH)) is mixed with 25 g sodium hydroxide in
100 ml distilled water. Immerse sample in solution at 60–70 °C (140–
160°F) for 1–3 min.

37
 Etched with 4% picral. 1000×
AF- acicular ferrite; PM- plate
martensite

Etched with 10% Sodium Metabisulfite.

1000X
PM -plate martensite; FM-
fine martensite; and AF + A -acicular
ferrite and austenite.

FIG 13: Microstructures. A) Etchant: Picral B) Etchant: Sodium Metabisulphite [22]

Austempered ductile iron (Fe-3.6%C-2.5%Si-0.056%P-0.052%Mg-0.7%Cu).
Austenitized at 900 °C, 2 hr., Austempered at 360 °C, 2 min., and air cooled.

38
 Carl Zeus POB 4041, D 37030

Model: PL-A662

Lamp: Super pressure mercury

lamp, HBO 103 W/2

FIG 14: Optical Microscope

3.2.5 Differential Scanning Calorimetric Analysis

Differential scanning calorimetry or DSC is a thermo analytical technique in

which the difference in the amount ofheat required to increase the temperature of a
sample and reference is measured as a function of temperature. The peaks in the
DSC curve determine the temperature at which transition would take place, thus
by carrying out the DSC test we see that two peaks are obtained, one at 215°C and
the other at 336°C.

FIG 15: DSC Equipment

39
 3.2.6 Tempering

As martensite was obtained in the microstructure, the material was unfit for use
in any engineering application, as martensite being brittle reduces the fracture
toughness of the material. Thus it was important to carry out tempering process to
retain toughness in the material. Now, since we were developing the material for
wear application we wanted to keep the decrease in hardness to minimum, while
improving its toughness. Hence low temperatures were selected for tempering
where most of the residual stresses would be relieved and hardness would also be
retained.

We carried out a DSC test to correctly select the tempering temperature. Based
on the DSC peaks obtained, we decided to carry out tempering at 215 oC, and 336
o
C.

FIG 16: Furnace used for tempering

3.2.7 Hardness

The Bulk hardness values of the Austempered samples were measured

using a Rockwell Hardness tester. The range of the hardness fell between 56-
62 HRC.

40
FIG 17: ROCKWELL Hardness Tester

3.2.8 Wear Resistance Test - pin abrasion test [23]

The 9 samples obtained; 3 austemepered samples, 3 austempered and tempered

at 215 oC, 3 austempered and tempered at 336 oC, were tested for wear
resistance using the pin abrasion test. For the pin abrasion test method, the
sample pin is positioned perpendicular to the abrasive surface (Emery paper
150 No.), which is usually mounted on a flat curricular disk. The initial and
final weights were taken in the test and weight loss were calculated. The
following were the wear specifications used by us: RPM: 400 Load: 2kg and
Time: 1hr. 40 min

FIG 18: WEAR Test

Machine

ASTM Standard
Used: G 132-96
(Reapproved 2001)

41
Results & Discussions

42
4.1 Observations

Element C Si Mn S P Cr Cu Ni C
Equivalent

% 2.86 2.5 0.88 0.01 0.02 - 0.59 0.55 3.69

TABLE 4: COMPOSITION OF A NORMAL ADI SAMPLE

Austenizing Temperature Hardness Values

850 62 – 63 HRC

900 58 – 62 HRC

950 58 – 60 HRC

Normal ADI 51-53 HRC

As Cast 45 – 48 HRC

TABLE 5: HARDNESS VALUES AFTER AUSTEMPERING AT 3

TEMPERATURES, ALSO AS-CAST SAMPLE WITH NO HEAT TREATMENT

FIG 19: Microstructure of

G
the sample.Etchant: 2%
Nital, 500X
Treatment given is 850°c 1
hr., 250°c 2 hr.

C- Carbide
G- Graphite nodule
A- Austenite
N N- Intermixed needles
A of ferrite and martensite

43
 G

N
A

b
FIG 20: Microstructure of the sample,Etchant: 2% Nital, 500X.
a) 900°C 1hr, 250°C 2hr. b) 950°C 1hr, 250° 2hr.
C- Carbide, G- Graphite nodule, A- Austenite, N- Intermixed needles of ferrite
and martensite
44
 G

C
A N

a)

G
A

b)
FIG 21: Microstructure of the sample,Etchant: 2% Picral, 500X.
a) 850°C 1hr, 250°C 2hr. b) 900°C 1hr, 250° 2hr.
C- Carbide, G- Graphite nodule, A- Austenite, N- Intermixed needles of
ferrite and martensite
45
 G

FIG 22: Microstructure of the sample, 950°C 1hr. 250° 2hr. Etchant: Picral, 500X
G- Graphite nodule, A- Austenite, N- Intermixed needles of ferrite and martensite

C
C
G

a) b)

FIG 23: Microstructure of the

sample,Etchant: Sodium Picrate,
500X
a) 850°C 1hr, 250°C 2hr. b)
G
900°C 1hr, 250° 2hr. c) 950°C
1hr, 250° 2hr
G- Graphite
C- Carbide 46
c)
 C

F
A

a)

M G

b)
FIG 24: Microstructure of the sample, Etchant: Sodium meta-bilsulphite,
500X
a) 850°C 1hr. 250°C 2hr. b) 900°C 1hr. 250° 2hr. 47
A- Austenite, C- Carbide, F- Accicular Ferrite, G- Graphite, M- Martensite
 G

M
F

FIG 25: Microstructure of the sample,Etchant: Sodium Meta-bilsulphite, 500X

950°C 1hr., 250°C 2hr.
A- Austenite, F- Accicular Ferrite, G- Graphite, M- Martensite

Austenizing Tempering Temperature Hardness Values

Temperature

850 215 & 336 60 – 61 HRC

900 215 & 336 58 – 60 HRC

950 215 & 336 57 – 59 HRC

TABLE 6: HARDNESS VALUES AFTER TEMPERING

48
^e xo

->->850 1 hr 250 2hr

850 1 hr 250 2hr, 21.5000 mg

Integral 33.15 mJ
normalized 1.54 Jg^-1 Integral 260.58 mJ
Onset 194.97 °C normalized 12.12 Jg^-1
Peak 215.12 °C Onset 258.29 °C
Endset 248.13 °C Peak 337.17 °C
Endset 384.46 °C

5
mW

60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 °C
A)
2 4 6 8 10 12 14 16 18min

La b: METTLER STAR e SW 9 .20

^e xo

900 1hr 250 2 hr

55.1000 mg
Integral 6.70 mJ
normalized 0.12 Jg^ -1
Onset 263.59 °C
Peak 273.67 °C
Endset 290.72 °C

1
mW
Integral 135.44 mJ
normalized 2.46 Jg^ -1
Onset 298.50 °C
Peak 351.00 °C
Endset 389.32 °C

60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 °C

2 4 6 8 10 12 14 16 min

L a b : ME TT L E R S TAR S W 9 .2 0
e
B)
49
^e xo

Integral 191.35 mJ
|->950 1 hr 250 2 hr-line ->950 1 hr 250
normalized 2.72 Jg^-1
950 1 hr 250 2 hr, 70.3000 mg
Onset 301.26 °C
Peak 356.00 °C
Endset 385.54 °C
Integral 15.18 mJ
normalized 0.22 Jg^-1
Onset 203.27 °C
Peak 241.33 °C
Endset 258.44 °C

2
mW

60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 °C

2 4 6 8 10 12 14 16 min

L a b : ME TT L E R S TAR e S W 9 .2 0 C)

FIG 26: DSC Curves a) 850°C b) 900°C c) 950°C. All austempered at 250°C
Ist peak IIst peak

Sample Peak Integral Onset End set Peak Integral Onset End set
(0c) (0c) (0c) (0c) (0c) (0c)
(mJ) (mJ)

850c 1hr 250c 215 33.15 194.9 248.13 337 260.58 258.29 384.46
2hr

900c 1hr 250c 273 6.7 263 290 351 135 298 389
2hr

950c 1hr 250c 241 15.1 203 258 356 191.35 301 385
2hr

TABLE 7: DSC ANALYSIS TABLE

50
 Heat Treatment Of Initial Weight Final Weight Weight Loss
The Material (g) (g) (g)
850°C (1 hr.), 250°C 14. 4002 14.2699 0.1303
(2 hr.),
Un-tempered
850°C (1 hr.), 250°C 13.7899 13.641 0.1489
(2 hr.),
Tempered215°(1hr.)
850°C (1 hr.), 250°C 14.8575 14.7136 0.1439
(2 hr.),
Tempered336°(1hr.)
900°C (1 hr.), 250°C 14.5243 14.4186 0.1057
(2 hr.),
Un-tempered
900°C (1 hr.), 250°C 14.4267 14.2766 0.1501
(2 hr.),
Tempered215°(1hr.)
900°C (1 hr.), 250°C 14.3767 14.2395 0.1372
(2 hr.),
Tempered336°(1hr.)
950°C (1 hr.), 250°C 14.2403 14.1632 0.0771
(2 hr.),
Un-tempered
950°C (1 hr.), 250°C 14.4746 14.3766 0.098
(2 hr.),
Tempered215°(1hr.)
950°C (1 hr.), 250°C 14.9797 14.8789 0.1008
(2 hr.),
Tempered336°(1hr.)

TABLE 8: WEAR TEST RESULTS – WEIGHT LOSS

**NOTE: Weight loss of a normal ADI sample (Same heat treatment) was found to
be 0.2366

51
Low C eq. ADI (Tempered 336°C)

Low C eq. ADI (Tempered 215°C)

950°C
900°C
850°C
Low C eq. ADI (Untempered)

Normal ADI

0 0.05 0.1 0.15 0.2 0.25

FIG 27: Bar Graph Showing Wear Properties. (Wt. Loss in grams on X axis)

1.2

0.8

850°C
0.6
900°C
950°
0.4

0.2

0
Untempered Tempered 215°C Tempered 336°C

FIG 28: Graph Showing Wear Properties (Wt. Loss % on Y axis)

52
4.2 Conclusions

 In untempered condition, higher hardness was observed in samples

austenitized at lower temperatures (Table 5), this is because of the finer
needles observed in their microstructure (Figures 19-22 ).
 Ferrite nucleates on grain boundaries and graphite nodules [4]. Since, at
lower austenitizing temperature the grain size is smaller and the grain
boundary area is larger, hence larger area is available for nucleation and
nucleation rates are higher giving finer needles.
 On tempering (Table 6 ), the hardness decreases as tempering temperature
increases. This is because on increasing the tempering temperature more
amount of carbon diffuses out of the martensite and a higher degree of
relief in residual stresses is observed. [15]
 As the austenitizing temperature is increased the amount of carbides
decreases and no carbide was observed in the sample austenitized at 9500C.
This is because as the temperature increases, diffusion rate also increases
resulting in rates of dissolution of carbides. (Figure 23 )
 By the use of 10% sodium Metabisulfite etchant (Figures 24-25), which
tints as quenched martensite into brown and ferrite needles into blue [22]; it
was found that the microstructure consisted of a mixed interwoven
martensite and ferrite needles. One of the reasons cited is the lower
austempering temperature and less time (2500C, 2 hours).
 In untempered condition, higher wear resistance was observed in samples
austenitized at higher temperatures (Figure 27). One of the reasons cited is
the higher amount and blocky austenite present in these samples (Figures
21-22) as the presence of blocky austenite in austempered ductile iron
improves strain hardening behavior by the formation strain induced
martensite [16].
 On tempering the wear resistance of the material decreases, this is because
on tempering carbon diffuses out of the martensite reducing hardness.
 On increasing the tempering temperature the decrease in wear resistance is
less(Figure 28), as at higher tempering temperatures the carbon diffusing
out of the martensite forms fine carbide precipitates [15]. These precipitates
may be responsible for better wear properties.
 The hardness and wear properties of low C equivalent ductile iron were
found to be much better than those of normal ADI.

53
Suggestions

54
 5.1 Suggestions

 Physical properties of fatigue, fracture toughness and tensile strength

should also be studied for the same material giving it the same treatment
 Different Austempering temperatures should be used and a structure
property co-relationship should be established.
 Different time for austenitizing and austempering should be used to
establish a more concurrent result on the usability of the material.
 The major comparison was whether this material can replace normal ADI in
the industry, however without establishing results of the above mentioned
features we cannot come to a strong consensus.

55
 References
1) Karl B. Rundman „Heat Treatment of Ductile Iron‟ ASM Handbook
Volume 4, Heat Treating (ASM International), Pages 682-692 (1990)
2) D.J. Moore, B.S. Shugart, K.L. Hayrynen, and K.B. Rundman, Published a
paper titled „Microstructural Determination of Isothermal Transformation
Diagrams in a Low Alloy Ductile Iron‟ Trans. AFS., (1990)
3) T.N. Rouns and K.B. Rundman, „Constitution of Austempered ductile Iron
and the Kinetics of Austempering‟ AFS Transactions Volume 95, Page 851
- 874 (1987)
4) Karl B. Rundman “It‟s About Austenite and Carbon, Mate” -A Story of the
Physical Metallurgy of ADI - Part II (2006).
5) K. B. Rundman, D.J.Moore, K.L.Hayrynen, W.J. Dubensky, T.N. Rouns
“The Microstructure and Properties of ADI” Journal of Heat Treating,
Volume 5, no.2, Page 79 - 95 (1988)
6) W. Dubensky, K. B. Rundman “An Electron Microscope Study of Carbide
Formation in Austempered ductile Iron” AFS Transactions, Volume 93,
Page 389 – 394 (1985)
7) J.R. Parolini, D. J. Moore, and K. B. Rundman “On the Kinetics of
Austempered Gray Iron” AFS Transactions, Volume 110 pp(2003)
8) S. S. Umale1, P. P. Parhad, Ajay Likhite and S. U. Pathak “Austempering
Heat Treatment of Low Carbon Equivalent Ductile Irons” Indian Foundry
Journal, Vol. 58, No. 5 (May 2012)
9) Doong J. L., Ju F. C., Chen H. S. and Chen L. W., J. Mater. Sci. Letter,
Voume. 5, Page. 555 (1986)
10) Putatunda S. K. and Singh I., J. Test. Eval., Volume 23, Page 325 (1995)
11) CHENG-HSUN HSU and TAO-LIANG CHUANG “Influence of Stageped
Austempering Process on the Fracture Toughness of Austempered Ductile

56
 Iron”, Metallurgical and Materials Transactions A, Volume 32 A (Oct
2001)
12) Putatunda S “Development of Austempered Duc-tile Iron with
Simultaneous High Yield Strength and Fracture Toughness by Novel Two-
stage Aus-tempering Process”, Material Science, Volume 315, Page 70-80
(2001)
13) Ravishankar K.S., K. Rajendra Udupa and P. Prasad Rao “Development of
Austempered Ductile Iron for High Tensile and Fracture toughness by Two
Stage Austempering Process.”, 68th WFC - World Foundry Congress 7th -
10th February, 2008, Page. 35-40 (2008)
14) John R. Keough, Bela V. Kovacs and Douglas M. Pramstaller „Method for
preparing high silicon, low carbon austempered cast iron‟ (US 5139579 A)
(1991)
15) Sidney H. Avner, Introduction to Physical Metallurgy, second edition, Page
305-313 (2009)
16) Srinivasmurthy Daber, P. Prasad Rao, „Formation of Strain Induced
Martensite in Austempered Ductile Iron‟, Journal of Material Science,
Volume 43, Issue 1, Page357-367 (Jan, 2008)
17) ASM Handbook, Volume 1, Properties and Selection: Irons, Steels, and
High Performance Alloys, Section: Cast Irons, Ductile Iron. Revised by
Lyle R. Jenkins, Ductile Iron Society; and R.D. Forrest, Pechiney
Electrometallurgie, Division Fonderie. (ASM International), Pages 65-67,
70-72, 74
18) Ductile Iron society, ductile Iron Data for Design Engineers.
http://www.ductile.org/didata/ pdf/didata2.pdf, 9.
19) Batra Uma, Ray S. and Prabhakar S.R., Impact properties of copper alloyed
and nickel copper alloyed ADI, JMEPEG, vol. 13 (2004) pp 64-68
20) Swine S., Effect of Chemistry and Processing Variables on the Mechanical
Properties of Thin-wall Ductile iron castings, M.Tech thesis.

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21) Company Website (www.machine821.com)
22) M. Radzikowska, Metallography and Microstructures of Cast Iron,
Metallography and Microstructures, Vol9, ASM Handbook, ASM
International, 2004, p. 565–587
23) Standard Test Method for Pin Abrasion Testing, designation G132-96
(Reapproved 2001), (ASTM International), Page 563-567

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