Practical 1

The Effect of Heat Treatment on the Structure

and Mechanical Properties of Steel

Theoretical introduction
A STEEL is usually defined as an alloy of iron and carbon with carbon content between a
few hundreds of a percent up to about 2 wt%. Other alloying elements can amount in total
to about 5 wt% in low-alloy steels and more in high alloyed steels such as tool steels and
stainless steels. Steels can exhibit a wide variety of properties depending on composition
as well as the phases and microconstituents present, which in turn depend on the heat
treatment.
The basis for the understanding of the heat treatment of steels is the metastable Fe-Fe3C
phase diagram.
It shows which phases are to be expected at metastable equilibrium for different
combinations of carbon concentration and temperature.

Important metallurgical phases and microconstituents

Phase Crystal structure
(microconstituent) of phases Characteristics
Ferrite (-iron) bcc Relatively soft low-temperature phase; stable equilibrium
phase
Austenite (-iron) fcc Relatively soft medium-temperature phase; stable
equilibrium phase
Cementite (Fe3C) Complex Hard metastable phase
orthorhombic
Pearlite Metastable microconstituent; lamellar mixture of ferrite
and cementite
Martensite bct (supersaturated Hard metastable phase; lath morphology when <0.6 wt%
solution of carbon C; plate morphology when >1.0 wt% C and mixture of
in ferrite) those in between
Bainite ... Hard metastable microconstituent; nonlamellar mixture
of ferrite and cementite on an extremely fine scale; upper
bainite formed at higher temperatures has a feathery
appearance; lower bainite formed at lower temperatures
has an acicular appearance. The hardness of bainite
increases with decreasing temperature of formation.
 Definitions of transformation temperatures in iron and steels
Transformation temperature. The temperature at which a change in phase occurs. The term is
sometimes used to denote the limiting temperature of a transformation range. The following
symbols are used for iron and steels.
Accm. In hypereutectoid steel, the temperature at which dissolution of cementite in austenite is
completed during heating.
Ac1. The temperature at which austenite begins to form during heating, with “c” being derived from
the French chauffant.
Ac3. The temperature at which transformation of ferrite to austenite is completed during heating.
Arcm. In hypereutectoid steel, the temperature at which precipitation of cementite starts during
cooling, with “r” being derived from the French refroidissant.
Ar1. The temperature at which transformation of austenite to ferrite or to ferrite plus cementite is
completed during cooling.
Ar3. The temperature at which austenite begins to transform to ferrite during cooling.
Ar4. The temperature at which delta ferrite transforms to austenite during cooling.
Ms . The temperature at which transformation of austenite to martensite starts during cooling.
Mf. The temperature at which martensite formation finishes during cooling.

If alloying elements are added to the steel, the position of the A1, A3 and Acm boundaries
and the eutectoid composition are changed. It suffices here to mention that (1) all the
important alloying elements decrease the eutectoid carbon content, (2) the austenite-
stabilizing elements manganese and nickel decrease A1, and (3) the ferrite-stabilizing
elements chromium, silicon, molybdenum, and tungsten increase A1.

Transformation Diagrams
The kinetic aspects of phase transformations are as important as the equilibrium diagrams
for the heat treatment of steels. The metastable phase martensite and the morphologically
metastable microconstituent bainite, which are of extreme importance to the properties of
steels, can generally form with comparatively rapid cooling to ambient temperature, that is,
when diffusion of carbon and alloying elements is suppressed or limited to a vary low
level. Bainite is a eutectoid decomposition, which is a mixture of ferrite and cementite.
Martensite, the hardest constituent, forms during severe quenches from supersaturated
austenite by a shear transformation. Its hardness increases monotonically with carbon
content up to about 0.7 wt%. If these unstable metastable products are subsequently heated
to a moderately elevated temperature, they decompose to create a more stable distributions
of ferrite and carbide. The reheating process is sometimes known as tempering or
annealing.
One can conveniently describe what is happening during transformation by means of
transformation diagrams. Four different types of such diagrams can be distinguished.
These include:
 Isothermal transformation diagrams describing formation of austenite, which will be referred to as
ITh diagrams

 Isothermal transformation (IT) diagrams, also referred to as time-temperature-transformation (TTT)

diagrams, describing decomposition of austenite

 Continuous heating transformation (CHT) diagrams

  Continuous cooling transformation (CCT) diagrams

The goal of heat treatment of steel is very often to attain a satisfactory hardness. The
important microstructural phase is then normally martensite, which is the hardest
constituent in low-alloy steels. The hardness of martensite is primarily dependent on its
carbon content as is shown in Fig 1. If the microstructure is not fully martensitic, its
hardness is lower. In practical heat treatment, it is important to achieve full hardness to a
certain minimum depth after cooling, that is, to obtain a fully martensitic microstructure to
a certain minimum depth, which also represents a critical cooling rate. If a given steel does
not permit a martensitic structure to be formed to this depth, one has to choose another
steel with a higher hardenability.

Fig. 1. Relationship between hardness, carbon content, and amount of martensite.

QUENCHING refers to the process of rapidly cooling metal parts from the austenitizing
or solution treating temperature, typically from within the range of 815 to 870 °C for steel.
Stainless and high-alloy steels may be quenched to minimize the presence of grain
boundary carbides or to improve the ferrite distribution but most steels including carbon,
low-alloy, and tool steels, are quenched to produce controlled amounts of martensite in the
microstructure. Successful hardening usually means achieving the required microstructure,
hardness, strength, or toughness while minimizing residual stress, distortion, and the
possibility of cracking.
The selection of a quenchant medium depends on the hardenability of the particular alloy,
the section thickness and shape involved, and the cooling rates needed to achieve the
desired microstructure. The most common quenchant media are either liquids or gases. The
liquid quenchants commonly used include:
 Oil that may contain a variety of additives

 Water

 Aqueous polymer solutions

  Water that may contain salt or caustic additives

The most common gaseous quenchants are inert gases including helium, argon and
nitrogen. These quenchants are sometimes used after austenitizing in vacuum.
The ability of a quenchant to harden steel depends on the cooling characteristics of the
quenching medium. Quenching effectiveness is dependent on the steel composition, type
of quenchant or the quenchant use conditions. The design of the quenching system and the
thoroughness with which the system is maintained also contribute to the success of the
process.

Cooling Media and Quench Intensity

The depth of hardness at a given work-piece dimension is determined by the chemical
composition of the steel, the austenite grain size as established during the austenitizing
treatment, and the cooling rate. The steel is normally chosen on the basis of hardenability.
The choice of cooling medium, on the other hand, is less exact and crude rules are
normally applied (unalloyed steel is quenched in water, alloy steels in oil, and high-alloy
steels in air). Molten salt is often used for bainitic hardening of medium-carbon steels and
martempering of carburized parts (salt temperature above Ms for the case). Judicious
selection of cooling medium is critical for obtaining optimum mechanical properties,
avoiding quench cracks, minimizing distortion (to be discussed below), and improving
reproducibility in hardening. Of most interest are the liquid quenching media, and they also
show the most complicated cooling process.

Quenching Media
Many different media are used for quenching. Most are included in the list that follows:

 Water

 Aqueous brine solutions

 Oils

 Molten salts

 Molten metals

 Gases

TEMPERING OF STEEL is a process in which the previously hardened steel is usually

heated to a temperature below the lower critical temperature and cooled at a suitable rate,
primarily to increase ductility and toughness, but also to increase grain size of the matrix.
Steels are tempered by reheating after hardening to obtain specific values of mechanical
properties and also to relieve quenching stresses and to ensure dimensional stability.
Tempering usually follows quenching from above the upper critical temperature; however,
tempering is also used to relieve the stresses and reduce the hardness developed during
welding and to relieve stresses induced by forming and machining.
Martensite is a very hard phase in steel. However, except at low carbon contents,
martensitic steels have insufficient toughness for many applications. Tempering of
martensitic steels, by heating for a certain time at temperatures below the A1, is therefore
introduced to exchange some of the strength for greater ductility through reduction of
carbon supersaturation initially present and replacing it with more stable structures.
Additionally, the retained austenite associated with martensite in steels containing more
than about 0.7 wt% C can be decomposed during the tempering process. In carbon steels
containing small percentages of the common alloying elements, one distinguishes the
following stages during tempering:
 Stage 1 (20 to 100 °C). Short-range diffusion of carbon atoms to dislocations and
martensite plate boundaries; formation of carbon clusters

 Stage 2 (100 to 200 °C). Precipitation of transition carbides, especially -carbide

(Fe2.4C)
 Stage 3 (200 to 350 °C). Transformation of retained austenite to ferrite and
cementite
 Stage 4 (250 to 700 °C). Formation of ferrite and cementite. Spheroidized carbides
in a matrix of equiaxed ferrite grains comprises well-tempered steels, that is,
tempered for long times at temperatures approaching 700 °C.

Variables associated with tempering that affect the microstructure and the mechanical
properties of a tempered steel include:

 Tempering temperature

 Time at temperature

 Cooling rate from the tempering temperature

 Composition of the steel, including carbon content, alloy content, and residual elements

In a steel quenched to a microstructure consisting essentially of martensite, the iron lattice

is strained by carbon atoms, producing high hardness of quenched steels. Upon heating, the
carbon atoms diffuse and react in a series of distinct steps that eventually form Fe3C or an
alloy carbide in a ferrite matrix of gradually decreasing stress level. The properties of the
tempered steel are primarily determined by size, shape, composition and distribution of the
carbides that form, with a relatively minor contribution from solid-solution hardening of
the ferrite. These changes in microstructure usually decrease hardness, tensile strength and
yield strength but increase ductility and toughness.
Under certain conditions, hardness may remain unaffected by tempering or may even be
increased as a result of it. For example, tempering a hardened steel at very low tempering
temperatures may cause no change in hardness but may achieve a desired increase in yield
strength. Also, those alloy steels that contain one or more of the carbide-forming elements
(chromium, molybdenum, vanadium, and tungsten) are capable of secondary hardening;
that is, they may become somewhat harder as a result of tempering.

Thermal Stresses during and Residual Stresses after Heat Treatment

Heat treatment of steel, especially martensitic hardening, is usually accompanied by
evolution of large residual stresses, that is stresses that exist without any external load on
the part considered. Causes for such stresses include:

 Thermal expansion or contraction of a homogeneous material in a temperature

 gradient field
 Different thermal expansion coefficients of various phases in a multiphase material
 Density changes due to phase transformations in the metal
 Growth stresses of reaction products formed on the surface or as precipitates, for
example, external and internal oxidation

Cracking and Distortion due to Hardening

There is a risk for cracking of a workpiece if large tensile stresses, transient or residual, are
combined with the presence of a brittle microstructure (particularly martensite). Thermal
stresses during cooling generally increase with the size of a workpiece. For phase
transformation-induced stresses, geometric dimension, hardenability of the steel and
quench intensity interact in a complicated manner. However, as a general rule it holds that
the use of a more efficient cooling medium, for example, water as compared to oil, will
lead to larger stresses. The presence of geometric stress raisers increases the risk of
cracking.
Hardening is usually accompanied by distortion of a workpiece. The degree of distortion
depends on magnitude of the residual stresses. Hardening procedures that minimize
transient and residual stresses are beneficial as well as the use of fixtures (press hardening).

Overview
Steel can be engineered to display an amazingly wide range of mechanical properties. On
the one hand, it can be made as a soft, ductile material, capable of being stamped into
complex shapes (auto body parts, for example) at room temperature. On the other hand,
steel can be made as a practically unyielding (and yet flexible) material, useful, for
example, as cutlery or springs. The properties of steel not only depend on its composition,
but are determined to a large extent by the relative volume fractions of particular phases
and their dispersion within the material - a result of the material's thermal history. It is this
influence of thermal history on the microstructure and the mechanical properties of steel
that we will investigate.
For this purpose, we will expose a suite of specimens of selected steel to the heat
treatment with different process parameters and then analyze their microstructure and
measure their hardness which is directly related to the mechanical strength. The practical
has two parts (2 h. per each). In part I we will perform the experiment in which we will
simulate industrial practice and its popular faults by adjusting the austenitizing temperature.
In part II we will carry out microscopic examinations and analyze the obtained results.

Part I: Experiment
Objective

The objective of the experiment is to examine the influence of austenitizing temperature

on microstructure and mechanical properties of alloy steel (41Cr4) after quenching and
tempering.

Equipment and Materials

• 6 specimens of steel 41Cr4

• Furnaces set to each of the following temperatures: 750, 850, 1050, 200 and 600°C
• A bucket of water for quenching
• Tongs
• A Rockwell hardness tester

Procedure

1. Heat specimens of steel (2 per each temperature) to 750, 850 and 1050°C for 0.5 h.
2. Quench all specimens in water.
3. Reheat two series (three per each) of the water-quenched specimens for 1 h at 200°C
and 600C, respectively.

4. Measure the Rockwell hardness of each specimen. Use scale "C" when possible.

5. Tabulate measured hardness values against different austenitizing temperature.

Part II: Macroscopic examinations of metallographic cross-sections

Objective

The objective is the same like in the part I.

Equipment and Materials

 6 quenched and tempered specimens of steel 41Cr4

 Polishing and etching equipment
 A light (optical) microscope

Procedure

 Prepare the metallographic cross-sections of specimens by mechanical grinding and

polishing (polish using felt wheels sprayed with suspension of aluminum oxide and
distilled water).
 Etch the polished specimens using a dilute solution of nitric acid in alcohol (Nital),
containing about 5 percent of acid.

Safety Note: Wear a laboratory coat, suitable gloves and eye-protection during this
operation; contact with the solution would cause serious eye damage. Avoid
splashing or spilling the Nital etchant as it is corrosive.

Observations

1. Examine microstructure of each specimen. For all specimens, note the nature and extent
of microstructural changes near the surface. These changes originate from
decarburization. Therefore, you should make sure that the microstructural changes you
report are actually those characteristic of the bulk and not an artifact of surface
decarburization.
2. Describe the microstructure in each case.
3. Prepare a representative photomicrograph for each specimens examined. Be sure to
employ an appropriate magnification, such that the field of view includes all
characteristic features.
4. Comment on your results. How do the microstructure and heat treatment relate to the
mechanical properties of each material? What materials give the highest strength /
greatest hardness / highest ductility? Is there a simple trend in the relationship between
hardness and tensile strength? Explain the reasons for the trends observed in the data.

Questions to be discussed in the report

1. How does the hardness vary with a austenitizing temperature for the specimens studied?
2. How do the microstructures observed compare with the "standard" microstructures of
spheroidite, coarse martensite, fine martensite and tempered martensite?
3. How does the hardness vary with the tempering temperature?
4. How does the measured hardness of the specimen relate to its other mechanical
properties like strength, plasticity etc.?
5. For applications that require suitable toughness, a high tempered steel is preferred to a
low tempered steel. Can you explain this from the observed microstructures?
6. Why is it necessary to effect the transfer from the annealing furnace to the quenching
medium quickly? How quick is quick enough?
7. How do your measured hardness values compare to published data?

Structure of the report

Your report should include the following points:

1. Material
2. Selection of process parameters
3. Technology of heat treatment
4. Hardness measurements
5. Preparation of specimens for macroscopic examinations
6. Macroscopic examinations
7. Conclusions

References
[1] George E. Totten: Steel Heat Treatment Handbook - Metallurgy and Technologies, CRS Press
Taylor&Francis Group, 2 edition, 2007.

[2] George E. Totten: Steel Heat Treatment Handbook - Equipment and Process Design, CRS
Press Taylor&Francis Group, 2 edition, 2007.

[3] ASM Materials Information, ASM Handbooks on-line, vol. 4, 2010.