MASTER THESIS
Master Student
Alireza Saeed-Akbari
Matr. –Nr. 268696
Subject:
Alireza S. Akbari
Abstract
In the present work, hardness mapping and dilatometry experiments were
employed as the novel methods for the quantitative and qualitative
assessments of the heterogeneous microstructures in different steels. The
results were initially compared with the optical microscopy images to
show the lack of accuracy in case of handling the heterogeneous
compressive specimens using optical microscopy. It was then
demonstrated that dilatometry and hardness mapping results are
consistent.
In another attempt, a mathematical formula was developed to predict the
fraction of martensite based on the bulk hardness of the investigated
specimens. The formula gave reliable results due to both steels studied.
Surface hardness mapping and optical microscopy methods were also
utilized to study the microstructural phases within the fusion zones and
the heat affected zones of steel welds. Both macro- and microstructures
were examined in this regard. It was concluded that the parallel
application of hardness measurements and optical microscopy was
essential when handling the weld zones.
Table of Contents
1. Introduction 1
2. Fundamentals 3
2.1. Introduction, 3
2.2. Hardness Testing, 4
2.2.1. Background, 4
2.2.2. Microstructural Aspects, 5
2.3. Dilatation Experiment, 7
2.4. Martensitic Transformation and Microstructure, 9
2.5. Bainitic Transformation and Microstructure, 11
2.6. Characterization Difficulties, 15
2.7. Microstructural Aspects of Weld Zones, 16
3. Experimental Procedure 22
3.1. Material Characterization, 22
3.1.1. General Considerations, 22
3.1.2. Chemical Composition, 22
3.1.3. Microstructure, 23
3.2. Isothermal and Non-isothermal Compression Tests, 25
3.3. Execution of Welding, 26
3.4. Hardness Mapping and Metallography, 27
5. Conclusions 58
References i
Chapter 1 – INTRODUCTION 1
CHAPTER
ONE
INTRODUCTION
It has been well established that each single microstructural phase in steel
has its own hardness range. The distribution of such hardness values in
the pre-assumed hardness intervals is interconnected with the
arrangement and amount of different phases within the microstructure.
There are many research works and reports regarding the relationship
among the hardness of each phase, its chemical composition, and its
related mechanical properties [1-3]. In some reports [4,5], hardness
profiles were used to study the homogeneity of microstructures. Some
others [6-8] used surface hardness data to correlate hardness maps and
macrostructure of the entire weld zones, including heat affected zone and
the steel base plate.
It is known that the relative length changes are proportional to the relative
volume changes if the system undergoes a macroscopically isotropic
phase transformation. In the case of anisotropy that may occur in the
specimens exhibiting preferred orientation for the constituent
crystallites/grains, distinction should be made between the length and the
volumetric changes [9]
CHAPTER
TWO
FUNDAMENTALS
2.1. Introduction
In this chapter brief statements are given regarding the concept and the
application of hardness measurement in the materials investigations.
Chapter 2 – FUNDAMENTALS 4
2.2.1. Background
With regard to metallic materials, hardness has always been (and still is) a
subject of much discussion among metallurgists, and material scientists.
Attributes like wear resistance, deformation behavior, tensile strength, as
well as modulus of elasticity are connected with the term hardness.
• fine acicular,
• coarse acicular,
• granular.
The austenite and δ –ferrite phases that form in the FZ and HAZ during
heating will transform to several different low-temperature phases during
cooling. For example, the δ –ferrite in the HAZ may transform back to
austenite, which may then transform to different morphologies of
α –ferrite, namely, allotriomorphic ferrite, Widmanstatten ferrite, and
bainite. At rapid cooling rates, the austenite will transform to martensite.
In the fusion zone during cooling, the liquid solidifies as δ –ferrite, which
then transforms to austenite. With continued cooling, the austenite
transforms to the different α –ferrite morphologies observed in the HAZ
microstructure.
The microstructure obtained as the weld cools from the liquid phase to
ambient temperature is called the as-deposited or primary microstructure.
As stated before, it may consists of allotriomorphic ferrite α ,
Widmanstatten ferrite α W , acicular ferrite α a , and the so-called
microphases, which might include small amounts of martensite, retained
austenite or degenerate pearlite (Figure 2-7).
Bainite is also found in some weld deposits, particularly of the type used
in the power generation industry. Allotriomorphic ferrite is sometimes
called polygonal ferrite or proeutectoid ferrite, but polygonal simply
means many sided (like all ferrite morphologies) and Widmanstatten
ferrite can also be proeutectoid. Widmanstatten ferrite (Figure 2-8) is
sometimes included under the general description 'ferrite with aligned
MAC', the abbreviation referring to martensite, austenite and carbide.
However, bainite plates can also form in a similar shape, although their
thermodynamic and kinetic characteristics are quite different.
The term 'acicular' means shaped and pointed like a needle, but it is
generally recognized that acicular ferrite has in three-dimensions the
morphology of thin, lenticular plates (Figure 2-9).
Chapter 2 – FUNDAMENTALS 19
Hence, the reason why acicular ferrite is not usually obtained in wrought
steels is because they are relatively free of inclusions and because most
commercial heat treatments aim at a small austenite grain size. It is ironic
that bainite when it was first discovered was referred to as acicular ferrite,
and that the terms acicular ferrite and bainite were often used
interchangeably for many year after 1930 [18].
Chapter 3 – EXPERIMENTAL PROCEDURE 22
CHAPTER
THREE
EXPERIMENTAL PROCEDURE
3.1.3. Microstructure
The 22MnB5 steel contains ferrite and pearlite phases (together with
carbide) in as-received condition. Figure 3-1 shows the microstructure of
the 22MnB5 steel in the rolling direction.
The image analysis data shows that the microstructure contains around
78% ferrite besides 22%, combination of pearlite and carbide. Ferrite
grain size was measured to be comparable with 11 ASTM grain size
standard.
Chapter 3 – EXPERIMENTAL PROCEDURE 24
Figure 3-3. Baehr DIL 805 deformation dilatometer, and the sample
set up.
The aforementioned steel sheets (see 3.1), were joint together using arc
welding and laser welding methods. Different parts of a welded structure
Chapter 3 – EXPERIMENTAL PROCEDURE 27
are depicted in Figure 3-5. The caps and roots of fusion zones (FZ) and
heat-affected-zones (HAZ) are plotted as well.
In the current work, the joining sheets were put together before welding
using two methods: either with a simple touching of the two 'V' notched
neighboring sheets, or making a gap between them for further
improvement of the final attachment.
Surface hardness maps of the deformed, cut and mounted samples were
started one millimeter out of the sample, i.e., from the polymeric
mounting material. The hardness of mounting material was recorded as
999 and was ignored. Due to the boundary conditions between the
mounting material and the sample, hardness values of the sample's edge
must not be considered. Accordingly, the quantitative measurements
using surface hardness mapping data were performed by means of the
reliable hardness data which were taken from inside the sample. To
evaluate the consistency of the hardness mapping results regarding the
determination of the present phases, optical microscopy investigation
were also executed on the whole deformed specimens.
The welded sheets were also scanned using hardness mapping method
throughout the fusion zones and heat-affected-zones. Four sets of optical
microscopy images were taken from caps and roots of FZ and HAZ in
every single specimen. In addition, the macrostructures of the welds were
revealed using lower magnification microscopy.
Chapter 4 – RESULTS AND DISCUSSION 30
CHAPTER
FOUR
RESULTS AND DISCUSSION
Figure 4-1. The deformed 22MnB5 sample with ε max =0.1, ε& =0.05s-1,
In the present study, the hardness values of more than 400HV0.8g were
assumed as martensite. The hardness between 200 and 400HV0.8g were
assumed as bainite and below 200HV0.8g as ferrite. These assumptions
were calculated using the CCT diagram, microscopic investigations and
some reports [1-2,19]. Pearlite was not considered because no pearlite
was seen in the final microstructure using LOM and SEM images.
Figure 4-3 shows the relevant microstructures of points 'X' and 'Y'
illustrated in Figure 4-1 using this scanning method.
Chapter 4 – RESULTS AND DISCUSSION 32
0.3
TiD = 850°C
0.0 dε/dt = 0.05 s-1
-0.3
Dilatation (%)
0.15
-0.6 0.1
-0.9
0.0 Martensite (%)
-1.2 εmax Ms(°C) Mf(°C) Dil% (Dilatation Data)
____________________________________________________________
-1.5 0.0 410 230 0.26 100%
0.1 395 292 0.24 92%
0.15 379 258 0.12 46%
-1.8
0 200 400 600 800 1000
Temperature (°C)
These values differ from the previously estimated values using surface
hardness maps up to eight and four percent, respectively. These
discrepancies might be due to the anisotropy of crystal and/or grains. In
Figure 4-6, the results of measurements using these two techniques
corresponding to 26 different specimens are compared.
100
80
% M hardness map
60
40
%Mh = %Md + 3
20
0 20 40 60 80 100
% M dilatation
(H m − H )
κ= .100 (1)
Hm
10
15
κ
20
κ ~ -0.3Mp + 30
25
50%M|22MnB5 ~ κ15
30
35
0 20 40 60 80 100
% Mp
As is seen in Figure 4-7, the equation of the resultant solid trend line is:
κ = 0.3Mp + 30 (2)
The point which should be noted here is that, because of the definition of
κ equation at the beginning, the effect of the hardness of a fully
martensitic microstructure has been almost removed. Therefore, it is
simply possible to compare two specimens (one with higher and one with
lower carbon contents) with exactly the same H value (hardness of the
unknown bulk) and different Hm values (one higher for the higher carbon
content, and one lower, for the lower carbon content).
If one assumes that Hm1>Hm2 and H1=H2, then κ 1 > κ 2 . This can be proved
by putting different numbers within the κ equation.
If κ 1 and κ 2 values are put inside the previous diagram, it is found out
that κ 1 gives a lower martensite fraction. This is true, because the higher
carbon content will increase the hardness of bainite and martensite phases
simultaneously. As the bulk hardness of both specimens is the same, and
it is known that the martensite hardness increases by increasing the
Chapter 4 – RESULTS AND DISCUSSION 40
carbon content, then the only possibility to keep the bulk hardness
constant, is to reduce the fraction of harder martensite and increase the
fraction of less harder bainite.
hardness) values. The plot is given in Figure 4-8. The trend line equation
is:
κ = -0.2 H + 94 (3)
10
20
κ
κ ~ -0.2H + 94
30
40
50
250 300 350 400 450 500
H (HV0.8)
100
90
80
70
60
% MRH
50
40
30 MRH ~ Mp + 6
20
10
0
0 10 20 30 40 50 60 70 80 90 100
% Mp
H = 1.5 M κ + 320
Figures 4-10 and 4-11 gives the hardness maps of differently deformed
MSW1200 specimens. In each case, the fraction of microstructural phases
is shown. In addition the bulk hardness values of specimens are inserted
in the hardness mapping diagrams.
As mentioned in chapter 3, three different steel sheets were chosen for the
study of weld zones microstructure.
The S355 sheets (the lowest carbon content among others) were chosen
with a thickness of 12mm, while EH36 and RQT701 sheets had the
thickness of 20mm. In addition two sets of welding were exerted on
RQT701 sheets one under the condition of making a gap between the 'V'
notched joining parts (called as 'F' specimen) and one without making a
gap (called 'I' specimen).
In each case, the whole surface (including 'HAZ' and 'FZ') was scanned
using hardness mapping method. Moreover, optical microscopy images
were taken from four different locations: a) cap of FZ, b) root of FZ,
c) cap of HAZ, and d) root of HAZ.
Figure 4-12 shows the macrostructure and surface hardness map of the
entire weld zone for S355-12I welded sheets.
Chapter 4 – RESULTS AND DISCUSSION 46
Figure 4-12. Macrostructure (a) and hardness map (b) of S355-12I welded
sheet; the numbers indicate the hardness values in HV0.8.
Chapter 4 – RESULTS AND DISCUSSION 47
Figure 4-13 confirms the hardness mapping data using optical microscopy
images. Due to the presence of inclusions on the FZ cap, the conditions
lead to the formation of acicular ferrite beside bainite (see chapter 2 for
details), while the root mostly shows a ferritic microstructure.
Although not mentioned here, the HAZ cap consists of ferrite (based on
hardness data), while its root is mostly occupied by the mixtures of
bainite and ferrite.
Figure 4-15 and 4-16 gives the microstructures of FZ and HAZ of the
same steel in cap and root zones. As depicted by the mentioned hardness
map, the entire FZ consists of bainite phase with distribution of ferritic
islands in it. This is confirmed by consideration of Figure 4-16. On the
other hands, the whole HAZ (both cap and root) contains ferrite and no
bainite. Looking at the microstructures gives the same information,
besides the fact that the microstructure of HAZ in cap also contains large
fraction of acicular ferrite. It is seen that, although hardness mapping
method can easily distinguish between different phases, it is almost
impossible to find out which morphology is dominant in each case using
Chapter 4 – RESULTS AND DISCUSSION 50
Figure 4-17b, it can be assumed that the optical microscopy image was
taken in the boundary of FZ and HAZ; therefore, left hand side of this
image is strictly bainitic while the rest is martensitic. Based on the same
justification, a wrong capturing zone is the reason for a fully martensitic
microstructure as reported by metallography.
Hence, the finer structure is the major reason for the increase of hardness
in the FZ/HAZ contact zone. Furthermore, it is possible that the change in
grain structure has been also affected the mentioned drop in hardness
when entering HAZ in case of RQT701-20F. However, as said before, the
stable high hardness in the FZ in comparison with the hardness of
FZ/HAZ borderline shows that the present martensite phase has a
dominant effect on the grain structure.
Chapter 1 – INTRODUCTION 58
CHAPTER
FIVE
CONCLUSIONS
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