January 2023 Term Laboratory Report Book

MME 444
Heat Treatment and
Microstructure Sessional
Name: Masuma Akther Lovely

Student Number: 1811016

Experiment No : 03

Experiment name: Design of hardening treatment and tempering of hardened steel

to obtain different hardness of that of as quenched steel

Group no: A3
 PLAGIARISM STATEMENT (to be signed by student)

Using someone else's ideas or phrasing and representing those ideas or phrasing as my own,
either on purpose or through carelessness, is a serious offense known as plagiarism.
Plagiarism is an examination offence and may carry heavy penalties.

I declare that apart from properly referenced quotations, this report is my own work and
contains no plagiarism; it has not been submitted previously for any other assessed work on
this course.

I further declare that the report in any way does not resemble cheating and attempted
cheating, lying, and stealing.

Student Name: Masuma Akther Lovely

Student Number: 1811016

Course Number: MME 444 Heat Treatment and Microstructure Sessional

Student Signature:

Date: 08/08/2023
Table of Contents
ABSTRACT: ..........................................................................................................5

INTRODUCTION: .................................................................................................5

EXPERIMENTAL PROCEDURE: ........................................................................6

CALCULATION: ...................................................................................................7

RESULT:.................................................................................................................9

DISCUSSION:......................................................................................................12

QUESTION and ANSWERS: ..............................................................................13

REFERENCES.........................................................................................................21
Table of Figures:
Figure 1 : Heating and cooling cycles for hardening and tempering ……………………… 5
Figure 2: Rockwell Hardness (HRB) vs. Brinell Hardness Number (BHN) ................................ 10
Figure 3: Rockwell Hardness vs. Tempering Temperature (℃).................................................... 10
Figure 4: Rockwell Hardness vs. Tempering Temperature ............................................................11
Figure 5: Standard Microstructure of tempered martensite and observed tempered martensite .. 13
Figure 6: Standard microstructure of spheroidized steel .............................................................. 14
Figure 7: Microstructure of the spheroidized high-carbon steel ................................................... 16
Figure 8: Annealed high-carbon steel microstructure ................................................................... 16
Figure 9: Microstructure of normalized high carbon steel............................................................ 17
Figure 10: The hardness of martensite as a function of carbon content ....................................... 18
Figure 11: Cooling rate effect on martensite................................................................................. 19
Figure 12: Relationship between hardness, carbon content and amount of martensite ................ 19

List of Tables:
Table 1: The OES composition of the sample of group-3............................................................... 9
Table 2: Comparison between measured BHN and converted BHN from HRB ............................ 9
Table 3: Comparison between tempering temperature (℃) and HRC .......................................... 10
Table 4: Comparison among wt% of carbon, tempering temperature and hardness after tempering
........................................................................................................................................................11
Table 5: Ultimate Tensile Strength from BHN ............................................................................. 12
ABSTRACT:
This report explores the microstructure and hardness of plain carbon steel that contains less than
or equal to 1.2% carbon through hardening and spheroidization. By applying heat treatment
processes appropriately, the steel's hardness, strength, and toughness can be adjusted to fit various
engineering and manufacturing applications. The report investigates the optimization of the
hardening and tempering processes to achieve different levels of hardness in hardened steel
compared to its initial state. Samples were heated at 920℃ for 1 hour and 20 minutes, quenched,
and tempered at 540℃ for 30 minutes according to the heat treatment design. To develop the
hardening and tempering procedures, Optical Emission Spectroscopy (OES) was used for steel.
The hardness was measured using the Brinell (1500 kgf) and Rockwell C and B scales before and
after heat treatment, while the microstructure was analyzed before hardening and after tempering.

INTRODUCTION:
Hardening involves heating a steel component to a high temperature within the austenite zone. It
is then held at this temperature for a specific duration before being rapidly cooled. This rapid
cooling prevents the usual formation of ferrite and pearlite phases and instead promotes the
creation of a metastable martensitic structure within the steel. Following complete austenitization,
this stage involves rapidly cooling the heated part using suitable cooling agents to attain
martensitic structures.

Figure 1 : Heating and cooling cycles for hardening and tempering

There are two distinct approaches for converting austenite into martensite, known as isothermal
cooling and transformation through continuous cooling. This transformation leads to a substantial
enhancement in hardness.

During the hardening procedure, steel undergoes heating within the hardening range, which
surpasses the higher critical point by 30°C to 50°C or lies between the upper critical temperature
(A3) and the lower critical temperature (A1) for hypo eutectoid steels. The steel is maintained at
this temperature for a suitable duration to achieve an austenitic structure. Rapid cooling is then
executed through quenching in an appropriate medium like water, oil, or salt.

Throughout the hardening process, the steel is meticulously managed, ensuring rapid quenching
prevents transformation at the lower critical point. This deliberate strategy compels the
transformation to occur at a notably lower temperature. The rapidness of cooling limits the time
accessible to the metal, thereby hindering transformation at the lower critical temperature.

A hardened steel piece, due to martensitic structure, is extremely hard and brittle, due to which it
is found unsuitable for most practical purposes. So, subsequent treatment is required to obtain the
desired degree of toughness at the cost of some strength and hardness to make it suitable for use.
Tempering entails enhancing the qualities of a metal, particularly steel, by subjecting it to elevated
temperatures, below its melting point, followed by subsequent cooling, often within an ambient
environment. This procedure results in increased toughness through the reduction of brittleness
and the alleviation of internal stresses. Appropriate tempering temperatures exhibit significant
variation, depending upon the steel's composition and its intended purpose. [1]

Heating high-hardness steel, between 100℃ to 200℃, removes carbon and creates epsilon carbide
leading to the restoration of the BCC structure in the matrix. Further heating, between 200℃ to
400℃, transforms the structure into ferrite and cementite. Above 400℃ to 550℃, weaker but more
ductile ferrite is created. If the temperature exceeds 550℃, the cementite is spheroidized. The
structure returns to stable martensite with continued heating. [2]

EXPERIMENTAL PROCEDURE:
1. The Rockwell hardness on the B scale and the Brinell hardness of the sample were taken.
2. OES was used to determine the chemical composition of the sample.
3. The microstructure of the specimen was observed
 4. Specimens from group-1,2, and 3 were placed in the furnace at a pre-determined
temperature and time.
5. After the hardening treatment procedure, the sample was taken out to quench in water
within less than 1 second.
6. The Rockwell hardness on the B scale of the sample was then measured.
7. The sample was then tempered for 30 minutes at 540℃.
8. The specimens were cooled in water after tempering.
9. The Rockwell hardness on the both B scale and C scale and the Brinell hardness of the
specimens were measured again.

CALCULATION:
Rockwell Hardness Calculation:

Average Rockwell hardness value before hardening treatment and tempering,

70.2+72.1+74.2
HRB1 = 3

= 72.17

110+108+109
Average Rockwell hardness value after hardening treatment, HRB2 = 3

= 108

96+95+97
Average Rockwell hardness value after tempering, HRB3 = 3

= 95

The average rockwell hardness value after tempering, HRC = 17.26

Brinell Hardness Calculation:

Brinell Hardness value for the specimen (before hardening treatment and tempering):

2𝑃×0.102
BHN=
𝜋𝐷(𝐷−√𝐷2 −𝑑 2 ))

BHN = Brinell hardness number

P = the load on the indenting tool (kgf) = 1500kgf = 14700N

D = the diameter of the steel ball (mm) = 10mm

d1 = measure diameter at the rim of the impression (mm) = 54 division = 4 mm

d2 = measure diameter at the rim of the impression (mm) = 55 division = 4.07 mm

d3 = measure diameter at the rim of the impression (mm) = 53.5 division = 3.96 mm

2 ×14700 ×0.102
BHN1 = = 114.34 MPa
𝜋 ×10 (10−√(10)2 −(4)2 ))

2 ×14700 ×0.102
BHN2 = = 110.26 MPa
𝜋 ×10 (10−√(10)2 −(4.07)2 ))

2 ×14700 ×0.102
BHN3 = = 116.76 MPa
𝜋 ×10 (10−√(10)2 −(3.96)2 ))

𝐵𝐻𝑁1 + 𝐵𝐻𝑁2 + 𝐵𝐻𝑁3 114.34+110.26+116.76

Average BHN = BHNavg = = = 113.85 MPa
3 2

Brinell Hardness value for the specimen (after tempering):

2 ×14700 ×0.102
BHN, after tempering= = 208.73 MPa
𝜋 ×10 (10−√(10)2 −(3.44)2 ))

Temperature and time taken for hardening and tempering:

The temperature for hardening is taken at 920 ℃

The temperature for tempering is taken at 540 ℃

Holding time for hardening was 1hr 20min

RESULT:
Table 1: The OES composition of the sample of group-3

Elements Content (wt%) Elements Content (wt%)

Fe 98.05 Si 0.199

C 0.131 Mn 0.57

P 0.013 Cr 0.23

S 0.013 Ni 0.174

The hardness data of the specimen of group -3 before hardening, after hardening and tempering:
Average Rockwell Hardness, HRBbefore hardening = 72.17
Average Brinell Hardness, BHNbefore hardening = 113.85 MPa
Average Rockwell Hardness, HRBafter hardening = 108
Average Rockwell Hardness, HRBafter tempering = 95
Average Rockwell Hardness, HRCafter tempering = 17.26
Average Brinell Hardness, BHNbefore tempering = 208.73 MPa

Table 2: Comparison between measured BHN and converted BHN from HRB

Test Condition HRB Converted to BHN (Conversion table) Measured BHN

(MPa)
Before Hardening 72.17 127 113.85

After Hardening 108 322 -

After Tempering 95 212 208.73

 Relation between BHN and HRB
120 108
95
Rockwell Hardness (HRB)
100

80 72
60

40

20

0
127 322 212
Brinell Hardness Number(BHN)

Figure 2: Rockwell Hardness (HRB) vs. Brinell Hardness Number (BHN)

Table 3: Comparison between tempering temperature (℃) and HRC

Group No Tempering Temp HRC

A-1 315 30.13

A-2 430 22.17
A-3 540 17.26

Tempering Temperature Vs HRC

35 30.13
Rockwell C Hardness

30
25 22.17
20 17.26
15
10
5
0
315 430 540
Tempering Temperature, ̊C

Figure 3: Rockwell Hardness vs. Tempering Temperature (℃)

Table 4: Comparison among wt% of carbon, tempering temperature and hardness after tempering

Group Wt% of Carbon Tempering Hardness After

Temperature Tempering (HRC)
1 0.131 315 30.133
2 430 22.17
3 540 17.26
4 0.945 315 51.76
5 430 48.30
6 540 47.89
7 0.542 315 57.27
8 430 57.20
9 540 44.20

Figure 4: Rockwell Hardness vs. Tempering Temperature

Table 5: Ultimate Tensile Strength from BHN

Sample Condition BHN UTS (psi) = BHN × 500

Before Hardening 127 63500

After Hardening 322 161000

After Tempering 212 106000

DISCUSSION:
To assess the material's response to the hardening and tempering processes, we conducted hardness
tests and obtained the Brinell hardness number (BHN) and Rockwell hardness value (HRB). These
tests provided quantitative measurements of the material's hardness at different stages of the
experiment. From the table no. 4, we can see, with the increase of carbon percentage, the hardness
data also increase which matches with the theoretical value. The increase in the tempering
temperature results in a reduced hardness value. During tempering, solid-state reactions occur and
the as-quenched martensite is transformed into tempered martensite, which, at higher tempering
temperatures, is composed of highly dispersed spheroids of cementite (carbides) dispersed in a soft
matrix of ferrite, resulting in reduced hardness and increased toughness.

After examining the microstructure, it was discovered that the plain carbon steel specimen
contained two distinct phases: ferrite and pearlite. Ferrite was soft and ductile, while pearlite had
a lamellar structure made up of alternating layers of ferrite and cementite. If the specimen is
hardened at 920°C for 1 hour and 20 minutes, followed by water quenching, it will likely show the
formation of martensite. This will appear as a distinct, needle-like, or lath-like pattern in
micrographs, indicating its characteristic crystal structure. After tempering the hardened sample at
540°C for 30 minutes, followed by water cooling, the microstructure analysis is expected to reveal
changes in the martensitic structure formed during the initial hardening process. We observed a
refinement of the martensitic structure with a reduction in the needle-like patterns. This indicates
a partial transformation of the hard martensite into a more ductile structure. Additionally, the
tempering process causes fine carbides to precipitate within the microstructure, which impedes
crack propagation and increases toughness.
QUESTION and ANSWERS:
1. How do your tempered structures compare with standard microstructures of tempered
martensite and spheroidized steel?

Answer:

Comparison of tempered structure with standard microstructure of tempered martensite:

My observed microstructure shows carbide precipitate, retained austenite, ferrite, disappeared

boundary along with needle shaped martensite. The standard microstructure of tempered
martensite shows uniform distribution of needle shaped martensite, the shape of martensite is
sharper than my observed martensite.

Figure 5: Standard Microstructure of tempered martensite and observed tempered martensite

Comparison of tempered structure with standard microstructure of spheroidized steel:

The standard microstructure of spheroidized steel shows small globules of cementite distributed
all over the ferrite matrix where my microstructure shows martensite all over the matrix. No
presence of martensite is in the spheroidized steel.

Figure 6: Standard microstructure of spheroidized steel

2. Give the physical and mechanical changes that occur during the above phase
transformation

Answer:

During the phase transformation of hypo eutectoid steel:

i. The rapid cooling of austenite results in the formation of martensite which is hard and
brittle. It appears needle-like shaped and because of the formation of martensite, the
hardness and wear resistance of the steel increases.
ii. The tempering of the specimen reduces the residual stress resulting in the formation of
tempered martensite and retained austenite. The steel becomes more ductile and toughness
increases and hardness decreases. So, the machinability increases.
3. Explain the nature of pearlite and cementite phases in spheroids steel?

Answer:

Spheroidized steel is characterized by the presence of small globules of cementite and carbide
within the ferrite matrix.

This type of steel exhibits a less noticeable pearlite phase, which is an alternating layer of ferrite
and cementite, due to the transformation of the original lamellar pearlite structure into rounded
shapes of cementite on the ferrite matrix.

4. Why is tempering preceded by converting the steel into martensite phase?

Answer:

The martensite phase is essential before tempering as it provides a foundation of high initial
hardness. Tempering then benefits from this initial hardness by allowing controlled reduction,
resulting in improved toughness and a balanced combination of mechanical properties in the steel.
This brittleness of martensite can cause issues in many applications, so tempering is necessary to
improve the steel's toughness and ductility. By controlling how long the tempering process lasts,
it's possible to adjust the steel's hardness and create small carbide particles that make the
microstructure more even. Additionally, tempering helps reduce the internal stress that builds up
during quenching.

5. Which steel will be tougher, tempered high carbon steel or hardened medium carbon steel?

Answer:

Hardened medium carbon steel has toughness superior to tempered high carbon steel. Very higher
austenitizing temperatures increase the carbon content of the austenite but the bulk hardness is
reduced due to retained austenite and a lower resultant martensite content. So, the toughness of the
hardened medium carbon steel is more than tempered high carbon steel.
6. What is the nature of the microstructure in Spheroidized high-carbon steel, normalized high-
carbon steel, and annealed high-carbon steel?

Answer:

The microstructure of the spheroidized high-carbon steel contains tiny rounded cementite particles
that make up the microstructure.

Figure 7: Microstructure of the spheroidized high-carbon steel

An annealed high-carbon steel microstructure consists of a thick and continuous cementite

network. The coarse lamellar pearlite areas remain surrounded by a network of pro eutectoid
cementite along with its grain boundary.

Figure 8: Annealed high-carbon steel microstructure

The normalized high carbon steel consists of broken continuity of cementite networks. The
normalized structure consists of refined ferrite and pearlite grains with pro-eutectoid cementite.

Figure 9: Microstructure of normalized high carbon steel

7. How does hardness vary with % carbon content in steels? Explain.

Answer:

The increase of carbon in steel yields a proportional increase in cementite composition. Cementite,
a material renowned for its hardness, consequently renders the steel harder. Specifically, this
association holds for unalloyed steel, with carbon content levels up to 0.8%. Cementite's
microstructure in steel creates fine-lamellar formations, which hinder dislocations, thereby
amplifying the steel's hardness. The fine lamellas act as barriers to dislocation migration, which in
turn results in more hardness. As the carbon content increases, the volume of cementite formation
also increases, resulting in more fractions of fine lamellar pearlite structures, and hence, harder
steel.
When the concentration of carbon in steel reaches 0.8%, cementite precipitates at the grain
boundaries, leading to embrittlement and reduced hardness. Elevated surface carbon content arises
from a high carbon potential, which can result in excessive amounts of retained austenite or free
carbides. These factors have a negative impact on the distribution of residual stress in the steel,
ultimately leading to decreased hardness. [3]

Figure 10: The hardness of martensite as a function of carbon content

 8. Why it is necessary to be quick in transferring the specimen from the austenitizing furnace to
the water bath during quenching?

Answer:

It is necessary to be quick in transferring the specimen from the austenitizing furnace to the water
bath during quenching to produce a martensite transformation. The more time needed to transfer
the specimen to the water bath, the slower the cooling rate becomes, ferrite pearlite or ferrite-
pearlite-bainite also appear in the microstructure and the percentage of martensite becomes low
and the hardness decreases.

Figure 12: Relationship between hardness, carbon

Figure 11: Cooling rate effect on martensite
content and amount of martensite

9. How does the hardness of the specimen tempered at 700℃ compares with that of the furnace-
cooled specimen? A Steel given such a tempering treatment is preferred to a furnace-cooled
specimen for good machinability. Can you explain this based on the difference in microstructure?

Answer:

After cooling a specimen in a furnace, it is dominated by martensite, which creates a highly

hardened material. However, if tempered at 700°C, some of the martensite transitions into more
ductile phases, reducing the overall hardness. The resulting microstructures and hardness of a
tempered and furnace-cooled specimen differ significantly at this temperature. To make it easier
to machine the material into desired shapes without damaging the workpiece, it's preferable to use
the tempered specimen. Machinability refers to the ease of machining a material without causing
tool wear. The tempered steel has more ductile phases and reduced hardness, making it easier to
machine than the hard and brittle martensite present in the furnace-cooled specimen. Therefore,
it's recommended to temper at 700°C to achieve tempered martensite and ferrite, resulting in softer
steel than the furnace-cooled specimen.

10. What is the significance of this experiment? How is it related to your course of study?

Answer:

The transformation that occurred in this experiment led to increased strength, improved wear
resistance, and suitability for demanding applications. We can employ this process to enhance steel
components' performance, resulting in more dependable and enduring products across various
industrial sectors. This experiment enables us to have an insight into how the carbon percentage,
tempering temperature, and cooling rate control the final microstructure. To achieve controlled
ductility and toughness, tempering plays a great role. The study of this experiment helps us later
in our study of the surface hardness of the steel
REFERENCES

[1] "Heat Treatment, Hardening, Annealing," [Online]. Available: Tempering | Heat Treatment,
Hardening, Annealing | Britannica. [Accessed 7 8 2023].

[2] "DE-1: Lesson 6. Heat treatment processes: hardening, tempering, annealing, and
normalizing," [Online]. Available: DE-1: Lesson 6. Heat treatment processes: hardening,
tempering, annealing, and normalizing (iasri.res.in). [Accessed 7 8 2023].

[3] "Influence of carbon on hardness and strength of steels," [Online]. Available: Influence of
carbon on hardness and strength of steels - tec-science. [Accessed 7 8 2023].