RWTH Aachen Institute of Ferrous Metallurgy

Master Student Alireza Saeed-Akbari Matr. –Nr. 268696 Subject: Determination of Steels Microstructural Components Based on Novel Characterization Techniques

Supervisors: Univ. Prof. Dr.-Ing. W. Bleck M.Sc. Malek Naderi

To mum and dad, for the whole love they gave me in my life…

The achievements of the current work are the results of helps and supports of all technicians, assistants, and colleagues at the Institute of Ferrous Metallurgy (IEHK), RWTH Aachen University. Among all, I should appreciate Professor Wolfgang Bleck – head of the Institute of Ferrous Metallurgy – for his kind considerations during the project; Mr. Malek Naderi for his invaluable indications, instructions, and cooperation, and IEHK technicians for their quick and accurate experiments. I would like to give special thanks to Mrs. Aida Nonn for her kind devotion to this investigation; without her helps, the examination of weld structures was impossible. The

microstructural and relevant primary hardness data of welds in the current work are parts of her assistance to broaden the discussions of the project.

Alireza S. Akbari

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 2. Fundamentals
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

1 3

3. Experimental Procedure
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


4. Results and Discussion


4.1. Revealing Heterogeneous Microstructures, 30 4.2. Reliability of Dilatometry and Hardness Mapping Methods, 33 4.2.1. Hardness Mapping, 33 4.2.2. Dilatometry Data, 35 4.3. Prediction of Martensite Fraction Using Hardness Criterion, 38 4.3.1. Developing the Formula, 38 4.3.2. Checking the Consistency of Results, 42 4.4. Microstructural Study of Weld Zones, 45

5. Conclusions References

58 i




The fast yet accurate estimation of microstructural phases in steels might be interesting due to both scientific and industrial points of view. In addition, developing the reliable alternative experiments for the calculation of phase distribution and phase fraction which can replace the conventional microscopy techniques is the matter of interest based on its time and cost saving impacts. 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. Phase transformations occur during cooling or heating. Any

transformation results in a specific phase and causes a definite contraction or expansion. For instance, transformation of austenite to martensite during cooling yields a certain dilatation. It should be pointed out that the dilatation term is mainly the magnitude of plastic deformation resulting from martensitic transformation. This dilatation is an invariant plane



strain, which is the combined effect of a uniaxial dilatation and a simple shear. The higher volume fraction of martensite results in higher dilatation magnitudes. 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] In the present work, hardness mapping and dilatometry experiments were employed as the novel methods for the assessment of microstructural phases 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.





2.1. Introduction
Phase transformations can be well studied using quantitative and qualitative microstructural investigations as well as consideration of dilatation data. The first method helps to recognize present phases and fraction of each phase within the microstructure. The latter not only aids to specify the start and finish temperatures of the phase transformations, but also can be used to quantify the volume fraction of the produced phases. Based on the above mentioned reasons, the microstructural investigations using light optical and scanning electron microscopy techniques are carried out. The problem which has to be taken into account is that, the compressive deformation is heterogeneous, i.e. the effective strain and the cooling rate along the horizontal centerline of the samples are varied. Consequently, the distribution of the produced phases is not homogeneous when handling the compression specimens. It means that light optical or scanning electron microscopy investigations on few selected points of the heterogeneously deformed surfaces are not proper techniques for the recognition of the phase fractions inside the experimental specimen. In this chapter brief statements are given regarding the concept and the application of hardness measurement in the materials investigations.



In addition, the dilatometry technique is introduced to measure the temperature and the amount of the possible transformations during cooling from the austenitization temperature. Moreover, the fundamentals of martensitic and bainitic transformations are reviewed. It is shown that similarities between certain bainitic and martensitic microstructures may also reduce the accuracy of the conventional optical microscopy techniques to assess the fraction of microstructural phases in steels. It is then concluded that due to both mentioned problems, i.e. microstructural heterogeneity and distinguishing between fine bainitic and martensitic structures, hardness mapping and dilatometry can be employed as the alternative characterization methods. The chapter is closed by notes regarding the development of microstructures in the weld heat-affected-zone (HAZ) and the weld fusion zone (FZ). It is also shown that in this case, hardness mapping can be utilized as a reasonable method to study the microstructural state.

2.2. Hardness Testing
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. An exact description of the method must be made if one wishes to compare the obtained readings with each other in order to achieve a usable hardness value.



Hardness testing is almost nondestructive and in many cases used for determining parameters to differentiate and describe materials. For example, hardness values can easily provide data on the strength properties of a material. The term hardness is generally understood as being the resistance of a material against the penetration of a body made of a stronger material. Hardness is therefore not a fundamental quantity of a material but always a response of the material to certain load or test method. A hardness value is calculated on the basis of the response of the material to this load [10].

2.2.2. Microstructural Aspects The concept of hardness in steels is divided into two major categories namely hardening capacity, i.e. the maximum achievable hardness level in the selected steel, and hardness penetration, i.e. the change in hardness as dependent on the distance from the surface. While the first item is dependent on the carbon content, the latter is strongly affected by the content of alloying elements [11]. As the hardness penetration is out of the discussions of the current work, the hardening capacity is outlined here. Maximum hardness in steels is obtained by producing a fully martensitic structure. This can be done by austenitizing the steel and then quenching it. During the austenitizing treatment all of the carbides dissolve and the ferrite transforms into austenite. Quenching this structure causes the austenite to transform via a shear mechanism into martensite. This transformation is so fast (martensite needles grow at close to the speed of sound) that there is no time to the carbon to diffuse out of the martensite



grains or to form carbide phases. The martensite, supersaturated with carbon, is very hard and also very brittle. Carbon, being a very effective solid solution strengthening agent, essentially determines the hardness of martensite. Cases where a lesser degree of hardening can be attributed to the presence of other alloying elements, but these elements tend to also make it more difficult to obtain a fully martensitic microstructure. So while maximum hardness in a given steel is dependent on our ability to produce a fully martensitic microstructure, the hardness of the martensite is largely determined by its carbon content [12]. In some instances, especially for hot rolled steels requiring enhanced capability to resist stretching on a blanked edge (as typically measured by hole expansion capacity), the microstructure can also contain significant quantities of bainite [13]. The hardness of bainite also linearly increases with carbon concentration by approximately 190 HV per wt%. This contrasts with a change of about 950 HV per wt% in the case of carbon supersaturated martensite. For mixed microstructures, the hardness depends on the transformation temperature and composition. This is because the stability of the residual austenite to martensitic transformation changes with its carbon concentration, the limiting value of which depends on the transformation temperature [3].



2.3. Dilatation Experiment
Changes in physical properties can be determined through differential thermal analysis, measurement of magnetic or electrical properties, or through measurements using a dilatometer, which is the most prevalently used method. The dilatometer measures the change in length ( ∆L ), which is dependent on temperature and time (Figure 2-1). According to SEP 1681, test evaluation is either isothermal (T=const.) or continuous [11].

Figure 2- 1. Change in length during isothermal and continuous transformation for the determination of TTA and TTT diagrams, after SEP 1681 [11].

Figure 2-2 shows how to evaluate an experiment involving continuous cooling. The beginning of a transformation range is signified by the deviation from a straight line in the graph of change in length over time. If the curve continues into another straight line, then the transformation in that field is finished. If different microstructural components form directly after one another, then a turning point in the curve signifies the boundary between transformation ranges.



Figure 2- 2. Example of how to evaluate experiments using continuous cooling, after SEP 1680 [11].

Finally, the temperature is graphed over the logarithmic time axis in a nonequilibrium diagram. This makes it possible to investigate the transformation behavior of the steel from short to long periods of time. The accuracy of nonequilibrium diagrams varies for temperature by +10K and for time by +10%. Variations due to different chemical compositions and initial states can further increase the range of distribution. All diagrams are valid, in the strictest sense, only for the chemical compositions observed and the conditions given for each specific case (austenitizing temperature and austenitizing time).



In every nonequilibrium diagram, a multitude of transformation points are given along with the specifications for the material and experimental procedures, (SEP 1680). in accordance with the Stahl-Eisen-Prüfblatt 1680

2.4. Martensitic Transformation and Microstructure
Martensitic transformation in steels occurs when austenite is cooled rapidly (quenched) is below Ms temperature Even pure so iron that may diffusional transform



martensitically if the cooling rate is sufficiently high. Crystallographic characteristics of martensite transformation involve shape change, surface relief, internal defects and existence of habit planes. Other characteristics such as athermal transformation,

stabilization and autocatalytic effect also make the mechanism of transformation difficult to understand. The diffusionless transformation accompanies lattice distortion and supersaturation of carbon. Inner microstructure of martensite plates consists of either dislocations or twins and each has differently shaped surface, consequently named as lath martensites and plate martensites. Lath martensite has waved surface whereas plate martensite a flat one as schematically depicted in Figure 2-3 [14].



Figure 2- 3. Schematics



typical by



martensite electron




microscopy. Plate martensite (left) has twins inside the plates of flat boundaries, whereas lath martensite (right) contains dislocations inside the lath of wavy boundaries [14].

The changes in volume and in configuration associated with martensitic transformation cause strong lattice distortions, which naturally counteract the transformation. At high carbon content values (>1.4%) and low transformation temperatures, these distortions can be reduced only to a small degree through gliding and recovery mechanisms, so that the transformation from austenite to martensite does not always fully proceed. Metallographically, martensite forms in plates as seen in Figure 2-4 [11].



Figure 2- 4. Different morphologies of martensite in Fe-C alloys; Left: Plate martensite, and Right: Lath martensite [11].

At lower carbon content values (<<0.5%) and higher transformation temperatures, the elastic lattice stresses can be removed more easily through dislocation movements. Martensite then no longer consists of single crystal plates but rather of lath-shaped crystals that are bunched into blocks and oriented in various directions [11].

2.5. Bainitic Transformation and Microstructure
In contrast to the diffusional characteristics, the surface relief during bainitic transformation is very similar to that of martensitic

transformation. Bainite also forms as isolated plate unlike lamellae of ferrite and cementite in pearlite. The speed of the formation of plates, however, is much lower than that of martensitic transformation.



The morphological characteristics of bainite are divided into two kinds, upper bainite and lower bainite according to the microstructural characteristics of carbides. Upper bainite, on {111} habit planes of austenite, is obtained at a temperature range of 350-550°C and the major microstructural constituent is either needle or laths of ferrite. Carbides, mainly Fe3C, grow at the interface of the ferrite plates. The transformation mechanism of the upper bainite is similar to that of Widmanstatten side plates. Lower bainite, which forms at the lower temperature than upper bainite and on irrational habit planes of austenite, has a similar microstructure to that of tempered martensite. Due to the lower diffusion rate of carbon, carbides, either Fe3C or epsilon carbides grow mostly inside the ferrite plates with a characteristic angle with respect to the ferrite plate and with characteristic habit planes. Schematic features of both types of bainite plates are shown in Figure 2-5 [14].

Figure 2- 5. Two carbide shapes in bainite: left: upper bainite, right: lower bainite. Note that the carbides in the upper bainite form at the plate boundaries and are coarser than those in the lower bainite. Also, the carbides in the lower bainite are aligned along a certain crystallographic direction within the plate [14].



Lower bainite structure that is usually obtained in the temperature range of 250-350°C, shows higher tensile strength than that of upper bainite. This is a consequence of the higher dislocation density in the lower bainite plates. Also, the lower bainite, due to the fine carbide structure, has a higher toughness than upper bainite. Therefore, the ductile transition temperature for the lower bainite is lower than that of upper bainite [14]. It is also possible to distinguish the bainitic structures according to the various metallographic appearances as: • fine acicular, • coarse acicular, • granular. Figure 2-6 gives examples of bainitic microstructures based on this classification.



Figure 2- 6. Optical microscope photos of bainitic microstructures: a) fine acicular bainite, b) coarse acicular bainite, and c) granular bainite [11].



2.6. Characterization Difficulties
The macroscopic mechanical properties of steel are highly dependent upon the microstructure, morphology, and distribution of each phase present [13]. As stated before, there are certain situations where the conventional optical microscopy techniques and/or electron microscopy are not proper or sufficiently accurate methods for the evaluation of steels' microstructures [15]. The examples are the situations where an inhomogeneous distribution of strain and cooling rate along the horizontal centerline of the experimental specimen are varied, thereby influencing the microstructural distribution of phases; also cases where a fine bainitic-martensitic phase mixture makes it impossible to distinguish between the present phases in a precise manner (see Figures 2-4 and 2-6). However, the variations of hardness values when passing through bainitic-martensitic phase boundaries (see section 2.2.2), and the position of sharp dilatation peaks during the dilatometry experiments

(see section 2.3) make it possible to indirectly detect and quantify the present phases, getting precise information from the whole experimental body.



2.7. Microstructural Aspects of Weld Zones
Austenite formation and decomposition in both the weld heat-affected zone (HAZ) and the weld fusion zone (FZ) is a well-studied phenomenon in the welding metallurgy of steels [16]. In the HAZ, the room temperature microstructure transforms to 100% austenite on heating above the Ac3 temperature. This transformation may or may not reach completion depending upon the peak temperature (between Ac1 and Ac3) attained in the HAZ and the time over which the material experiences this temperature. Interestingly, the temperature near the fusion line may be high enough to form the high temperature

δ –ferrite phase.
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. Due to steep temperature gradients and dynamic cooling conditions of welds, the resulting material contains significant microstructural gradients. These microstructural gradients affect the strengths, ductility, toughness, fatigue and creep rupture properties of steel welds. The knowledge of these gradients is well developed and is routinely considered in the design of weldments. However, there is a need to



develop predictive models to describe these gradients as a function of steel composition and weld thermal cycles [17]. 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).

Figure 2- 7. An illustration of the essential constituents of the primary microstructure of a steel weld deposit. The diagram is inaccurate in one respect, that inclusions cannot be expected to be visible in all of the acicular ferrite plates on a planar section of the microstructure. This is because the inclusion size is much smaller than that of an acicular ferrite plates, so that the chances of sectioning an inclusion and plate together are very small indeed [18].



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. Among others, acicular ferrite is a phase most commonly observed as austenite transforms during the cooling of low-alloy steel weld deposits. It is of considerable commercial importance because it provides a relatively tough and strong microstructure. It forms in a temperature range where reconstructive transformations become relatively sluggish and give way to displacive reactions such as Widmanstatten ferrite, bainite and martensite. 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).



Figure 2- 8. (a) Schematic diagrams illustrating the development of microstructures in weld deposits. The hexagons represent cross-sections of columnar austenite grains whose boundaries first become decorated with uniform, polycrystalline layers of allotriomorphic ferrite, followed by the formation of Widmanstatten ferrite. Depending on the relative

transformation rates Widmanstatten ferrite and acicular ferrite, the former can grow entirely across the austenite grains or become stifled by the intragranularly nucleated plates of acicular ferrite. This diagram takes no account of the influence of alloying additions on the austenite grain structure. (b) Actual optical micrographs illustrating the unhindered growth of Widmanstatten ferrite in a weld deposit. (c) Optical micrograph showing how the growth of Widmanstatten ferrite is stifled by the formation acicular ferrite [18].



Figure 2- 9. Replica transmission electron micrograph of acicular ferrite plates in a steel weld deposit [18].

The experimental data to date indicate that acicular ferrite is essentially identical to bainite. Its detailed morphology differs from that of conventional bainite because the former nucleates intragranularly at inclusions within large austenite grains whereas in wrought steels which are relatively free of nonmetallic inclusions, bainite nucleates initially at austenite-austenite grain surfaces and continues growth by the repeated formation of subunits, to generate the classical sheaf morphology. Acicular ferrite does not normally grow in sheaves because the development of sheaves is stifled by hard impingement between plates nucleated independently at adjacent sites. Indeed, conventional bainite or acicular ferrite can be obtained under identical isothermal transformation conditions in the same (inclusion rich) steel. In the former case, the austenite grain size has to be small in order that nucleation from grain surfaces dominates and subsequent growth then swaps the interiors of the austenite grains. For a larger austenite grain size, intragranular nucleation on inclusions dominates, so that acicular ferrite is obtained (Figure 2-10).



Figure 2- 10. An illustration of the effect of austenite grain size in determining whether the microstructure is predominantly acicular ferrite or bainite. A small grain sized sample has a relatively large number density of grain boundary nucleation sites and hence bainite dominates, whereas a large number density of intragranular nucleation sites leads to a microstructure consisting mainly of acicular ferrite [18].

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].





3.1. Materials Characterization
3.1.1. General Considerations Five different steels in shapes of compression specimens and welded sheets were employed. The compression specimens were made of 22MnB5 and MSW1200 steels which were received in form of plates, while the welded sheets were composed of S355, EH36 and RQT701 steels. The S355 sheet had a thickness of 12mm, while EH36 and RQT701 sheets had the thickness of 20mm.

3.1.2. Chemical Composition Chemical compositions of the investigated steels are given in tables 3-1 and 3-2 in case of compression and welded specimens.

Table 3-1. Chemical composition of the compression specimens (wt-%).

C 22MnB5



Cr 0.16 0.55

Ni 0.12 0.06




0.23 0.22 1.18

0.03 0.040 0.002 0.02 0.002 -

MSW1200 0.14 0.12 1.71

Chapter 3 – EXPERIMENTAL PROCEDURE Table 3-2. Chemical composition of the welded sheets (wt-%).


C Si Mn P S Cr Mo Ni Al Nb Cu Ti V B

S355-12 0.054 0.018 1.085 0.011 <0.001 0.015 <0.005 0.019 0.021 0.023 0.010 0.009 0.003 <0.0005

EH36-20 0.121 0.389 1.290 0.012 0.002 0.015 <0.005 0.024 0.037 0.032 0.016 0.001 0.004 <0.0005

RQT701-20 0.144 0.436 1.360 0.012 <0.001 0.016 <0.005 0.021 0.036 0.031 0.014 0.026 0.068 0.002

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.



Figure 3-1.

Microstructure of the as-received 22MnB5 sheets in the rolling direction a) 500X, and b) 1000X.

The microstructures of the base metal of the investigated welded sheets are given in Figure 3-2. As seen in this illustration, in case of S355 and EH36 specimens, the microstructures are predominantly ferritic-pearlitic, while RQT701 has a ferritic-bainitic microstructure.

Figure 3-2.

Microstructure of the base metals: a) S355, b) EH36, and c) RQT701.



3.2. Isothermal and Non-isothermal Compression Tests
The isothermal and non-isothermal compressive deformations were exerted on the 22MnB5 and MSW1200 compression specimens. The whole deformations and dilatometry experiments were carried out using a Baehr 805 dilatometer (Figure 3-3) with a deformation unit designed to perform a simple uniaxial deformation. In all cases, the geometry of the sample used was cylindrical with a length of 10mm and a 5mm diameter (Figure 3-4). In all of the tests, the temperature was measured using a surface mounted Pt/Pt-Rh10% thermocouple located at the mid-length relative to the specimen. Non-isothermal deformations were established through several simultaneous forming and quenching tests at the temperatures between 600°C–850°C and by the strain rates of 0.05s-1–1.0s-1. Regarding the duration of the experiments, the samples were deformed up to the strains of 0.1-0.5 in a single step. All samples were austenitized at 900°C for five minutes and quenched to the compression temperatures at a cooling rate of 50K/s. In case of isothermal experiments, deformations were carried out at the temperature range of 600°C – 850°C by the strain rates of 0.1 s-1 – 10.0 s-1. Due to the technical limitations in the Baehr deformation dilatometer, higher strain rates could not be applied in the simultaneous forming and quenching tests.



Figure 3-3.

Baehr DIL 805 deformation dilatometer, and the sample set up.

Figure 3-4.

Schematic illustration of the cylindrical specimen used during the dilatation experiments.

3.3. Execution of Welding
The aforementioned steel sheets (see 3.1), were joint together using arc welding and laser welding methods. Different parts of a welded structure



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.

Figure 3-5.

Schematic illustration of the welded structure.

3.4. Hardness Mapping and Metallography
In the present study, an innovative surface hardness mapping technique was developed by the Department of Ferrous Metallurgy (IEHK), RWTH Aachen University. In this technique, the surface of the sample is scanned using an indenter which exerts a 0.8g force on the surface of the sample



and records hardness of the points in Vickers or Rockwell hardness scales. Figure 3-6 shows the setup of the mentioned surface hardness mapping device and relevant specimen insertion.

Figure 3-6.

Surface hardness mapping relevant instruments at IEHK, RWTH Aachen University.

Surface hardness measurements were performed on the previously deformed and welded samples. To do this, in case of the deformed samples, they were cut lengthwise. The samples were mounted after cutting. The Vickers hardness of the whole deformed surfaces was measured in 0.3mm steps using an exerted force of 0.8g. In case of welded sheets 0.5mm steps were used. Afterwards, the surface hardness maps of the samples were plotted.



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.





4.1. Revealing Heterogeneous Microstructures
As stated in the previous sections, the compressive deformation results in an inhomogeneous distribution of microstructural components. To clarify this issue, and by consideration of various hardness levels due to different phases in steels, a complete surface hardness map a compressed 22MnB5 specimen deformed up to the strain of 0.1 is plotted in Figure 4-1.

Figure 4-1.

& The deformed 22MnB5 sample with ε max =0.1, ε =0.05s-1,

TiD =750°C; the complete surface hardness map with the scale of 25HV0.8 representing heterogeneity.



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. For further observation of the microstructural state, the whole surface of the investigated specimen was scanned using optical microscopy. The scanning sequence followed a pattern as depicted in Figure 4-2. Red spots demonstrate the approximate positions where an optical image was taken.

Figure 4-2.

The pattern corresponding to scanning the deformed surface using optical microscopy.

Figure 4-3 shows the relevant microstructures of points 'X' and 'Y' illustrated in Figure 4-1 using this scanning method.



Figure 4-3.

Optical microscopy images representing martensite and/or bainite in zones 'X' and 'Y' as mentioned in Figure 4-1.

As seen in Figure 4-3, the microstructure in zone 'X' is fully martensitic while bainite is the dominant phase in zone 'Y'. This proves that the pre-assumed hardness intervals regarding different phases are reliable. In addition, it is clearly seen that one may make a colossal mistake when reporting the phase fractions within the microstructure of the heterogeneously deformed specimens using single selected optical microscopy images.



4.2. Reliability of Dilatometry and Hardness Mapping Methods
4.2.1. Hardness Mapping The complete surface hardness maps of two samples which were deformed by the strain rate of ε& = 0.05s -1 are plotted in Figure 4-4. These samples were austenitized at 900°C for 5min. The initial deformation
& temperature, TiD, was 850°C and the cooling rate, T , was 50K/s. The first

map, Figure 4-4a, exhibits the sample which was deformed up to 10 percent strain ( ε ), while the second, Figure 4-4b, deformed to the maximum strain of 15 percent. As seen in Figure 4-4a, hardness values are greater than 400HV0.8 indicating a fully martensitic microstructure. In the second map, Figure 4-4b, concerning with the hardness values, bainite and martensite phases were distributed almost equally, i.e., 50% martensite and 50% bainite. Besides, the heterogeneity of hardness values in the range of each phase can be well studied. For instance, the hardness values within the fully martensitic microstructure vary between 400 and 550HV0.8. It might be due to the heterogeneous distribution of carbon content during austenization. This fact can be seen even in the bainitic zone.



Figure 4-4.

Surface hardness maps of two 22MnB5 samples deformed non-isothermally, TiD = 850°C , austenization at 900°C for

& & 5min, ε = 0.05s −1 and T = 50 K / s ; a) ε = 0.1 and b)

ε = 0.15 (scale = 25HV0.8).

Another conclusion is that, higher hardness values, i.e. martensite phase, can be detected in the inner parts of the compressed specimen. On the contrary, the phase with lower hardness levels, i.e. bainite, is formed in the outer parts. It is seen that, this technique provides one of the best tools for the physical understanding of the phases' heterogeneity using hardness criterion.



4.2.2. Dilatometry Data It is known that the dilatation observed during martensitic transformation becomes anisotropic if there is variant selection due to stress or strain [20,21]. This makes it difficult to asses the fraction of transformation using one-dimensional dilatometry measurements. However, due to sharp dilatation curves regarding martensitic transformation in all of the experiments, martensite phase percent within the deformed samples were also calculated using the dilatation data. The calculation was based on a simple mathematical method. In this method, the amount of dilatation due to martensitic transformation in one of the samples in the CCT diagram was assumed as a reference. In this case, the sample was cooled down at a cooling rate of approximately 50K/s. A fully martensitic microstructure caused a dilatation of around 0.26 percent. All other calculations – regarding the martensite phase percent resulting from the dilatation data in the rest of the specimens – were completed using this reference value. By using this calculation technique, the amount of martensite in the 10 percent deformed sample is about 92 percent and in the sample which was deformed 15 percent is about 46 percent, Figure 4-5.



TiD = 850°C

0.0 Dilatation (%) -0.3

dε/dt = 0.05 s-1


-0.6 -0.9



Martensite (%)

-1.2 -1.5 -1.8 0





(Dilatation Data)

____________________________________________________________ 0.0 410 230 0.26 100% 0.1 395 292 0.24 92% 0.15 379 258 0.12 46%






Temperature (°C)

Figure 4-5.

Dilatation curves of the previously mentioned samples in Figure 4-4, as well as a fully martensitic sample produced after cooling and without applying any force.

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. These samples were deformed non-isothermally by the strain rates ranging from 0.05s-1 to 1.0s-1, initial deformation temperatures between 600°C to 850°C, and the final strains of 0.05 to 0.5.



100 80
% M hardness map

60 40 20 0 0 20 40 60 80 100
%Mh = %Md + 3

% M dilatation

Figure 4-6.

Comparison of the estimated martensite content in the non-isothermally deformed samples using surface hardness mapping and dilatation data.

It is seen that the mentioned techniques are consistently reliable methods for the quantitative and qualitative assessment of the steels'




4.3. Prediction of Martensite Fraction Using Hardness Criterion
4.3.1. Developing the Formula A dimensionless parameter so-called 'relative hardness' is defined as follows:
(H m − H ) .100 Hm


where κ is the relative hardness, Hm is the average hardness of a fully martensitic microstructure of the same steel in HV10 scale (measured by macrohardness indentation on the known specimen containing almost 100% martensite), and H is the bulk hardness of an unknown specimen in HV10 scale. The Hm value in the case of 22MnB5 steel is amounted to be 473. In this stage, the κ factors of different 22MnB5 steel specimens are calculated. There are reports in which the maximum achievable hardness of steel can be measured using its chemical composition. These methods can be employed as an alternative for the mentioned calculation of the hardness of a fully martensitic specimen. However, in the current work, a direct measurement is used to achieve a higher accuracy in case of the developed formula. The mentioned values are plotted against Mp which is the precise martensite fraction coming from surface hardness mapping data (Figure 4-7).



0 5 10 15

20 25 30 35 0 20 40
% Mp
κ ~ -0.3Mp + 30
50%M|22MnB5 ~ κ15




Figure 4-7.

κ factor against precise martensite fraction of 22MnB5.

As is seen in Figure 4-7, the equation of the resultant solid trend line is:
κ = 0.3Mp + 30


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



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. In another attempt, κ was plotted against different H (unknown bulk hardness) values. The plot is given in Figure 4-8. The trend line equation is:
κ = -0.2 H + 94






κ ~ -0.2H + 94



50 250


H (HV0.8)




Figure 4-8.

κ factor against bulk hardness values of 22MnB5 specimens.

Putting equations (2) and (3) together results in:
H = 1.5M κ + 320


where M κ is the calculated martensite fraction using mathematical method. To show the accuracy of this method in case of 22MnB5 steel, Mp and M κ values were plotted against each other (Figure 4-9).



100 90 80 70 % MRH 60 50 40 30 20 10 0 0 10 20 30 40 50 60 % Mp 70 80 90 100
MRH ~ Mp + 6

Figure 4-9.

Accuracy test of MRH against MP in case of 22MnB5 steel.

As seen in Figure 4-9, there is a +6% tolerance factor regarding the mathematical estimation in comparison with the precise martensite fraction. To expand the application of the presented formula, upper and lower limits of 320 and 470HV10 were set as the states of no martensite and fully martensitic microstructures respectively. These numbers were chosen based on consideration of a large number of differently deformed specimens of the investigated steels. Finally, the whole equation package for the calculation of martensite fraction using hardness of an unknown bulk is as follows: H = 1.5 M κ + 320 H ≤ 320 H ≥ 470 no martensite fully martensitic (5)



4.3.2. Checking the Consistency of Results To check the applicability of this formula in case of other steels, another steel called MSW1200 was employed. The point which must be mentioned here is that, the carbon content of MSW1200 is 0.14%wt (almost half of 0.23%wt carbon content in case of 22MnB5 steel) and there is no boron available in its composition (in comparison with 0.002%wt of boron within the composition of 22MnB5 specimens). 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. Using equation 5, M κ values are calculated. As is easily seen and based on the suggested equation, presented specimens in Figure 4-10 are martensite-free. This is confirmed through both hardness mapping and mathematical estimation methods. In case of the specimens in Figure 4-11, mathematical estimation gives 71% and 60% martensite contents against the actual martensite contents of 76% and 71%, respectively. By this, the equation seems to be reliable. It is concluded that the developed formula is consistently applied for MSW1200 steel with different chemical composition to that of 22MnB5.



Figure 4-10. Hardness maps of ferritic-bainitic MSW1200 specimens;

a) 64% bainite and 36% ferrite , and b) 54% bainite, 46% ferrite, and almost no martensite.



Figure 4-11. Hardness maps of bainitic-martensitic MSW1200 specimens;

a) 24% bainite and 76% martensite , and b) 29% bainite, 71% martensite.



4.4. Microstructural Study of Weld Zones
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.



Figure 4-12. Macrostructure (a) and hardness map (b) of S355-12I welded

sheet; the numbers indicate the hardness values in HV0.8.



Figure 4-13. Microstructure of S355-12I welded sheet; a) cap of FZ, and

b) root of FZ.

Based on the pre-assumed hardness intervals as mentioned in section 4.2.1 and by the evaluation of hardness map of Figure 4-12, it is seen that the FZ cap mostly consists of bainite and ferrite while in the FZ root, ferrite is the dominant phase. 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. It is seen that both methods are consistent when working on a bainitic-ferritic microstructure. Hardness mapping can easily distinguish between ferritic and bainitic zones in an accurate manner. 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 4-14 illustrates EH36-20F specimen based on the same method.



Figure 4-14. Macrostructure (a) and hardness map (b) of EH36-20F

welded sheet; the numbers indicate the hardness values.



Figure 4-15. Microstructure of EH36-20F welded sheet; a) cap of FZ, and

b) root of FZ.

Figure 4-16. Microstructure of EH36-20F welded sheet; a) cap of HAZ,

and b) root of HAZ.

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



single hardness criterion. This is a major deficiency when working on the weld zones which having an idea of the presented morphologies is vital due to their impact on mechanical properties like toughness. Therefore, the parallel utilization of both hardness mapping and optical microscopy methods is suggested in such cases.

Figure 4-17. Macrostructure (a) and hardness map (b) of RQT701-20F,

welded sheets; the numbers indicate the hardness values in HV0.8.



Figure 4-18. Macrostructure (a) and hardness map (b) of RQT701-20I,

welded sheets; the numbers indicate the hardness values in HV0.8.

Figures 4-17 and 4-18 show RQT701-20F and RQT701-20I specimens respectively. It is seen that bainitic-martensitic mixed microstructures are expected in the cap and root of FZ in RQT701-20F sheet. The root has a higher fraction of martensite than cap. The HAZ instead is fully bainitic.



In addition, the RQT701-20I specimen is expected to show a fully bainitic microstructure in both FZ and HAZ parts.

Figure 4-19. Microstructure of RQT701-20F welded sheet; a) cap of FZ,

and b) root of FZ.

Figure 4-20. Microstructure of RQT701-20F welded sheet; a) cap of HAZ,

and b) root of HAZ.

Looking at the microstructures in Figures 4-19 to 4-22 gives contradictory results. Although the cap and root of FZ in RQT701-20F specimens are martensitic-bainitic as expected before, the HAZ seems to be fully martensitic in cap and dominantly martensitic – although partially bainitic - in root. It is in contrast with the hardness mapping results which predict a fully bainitic structure in HAZ. This can be justified by consideration of left hand side of Figure 4-20b. By comparison of this figure and what seen in the relevant hardness map in



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.

Figure 4-21. Microstructure of RQT701-20I welded sheet; a) cap of FZ,

and b) root of FZ.

Figure 4-22. Microstructure of RQT701-20I welded sheet; a) cap of HAZ,

and b) root of HAZ.

As stated before, hardness mapping results show a fully bainitic microstructure for RQT701-20I specimen in both FZ and HAZ sites. However, microstructural investigations (Figures 4-21 and 4-22) give a ferritic-bainitic microstructure. The observed ferritic microstructure is completely acicular particularly in case of FZ parts of the specimen.



Considering the hardness map of RQT701-20I specimen (Figure 4-18b), it is found that in spite of no prediction due to the presence of ferrites, lower hardness values in the center of cap and root of FZ and the increase of hardness till the FZ/HAZ boundary might be an indirect indication of the presence of a softer phase in that areas. In some reports [8,22], the equations were suggested to relate the hardness of each phase to the chemical composition of steel. By this and consideration of thermal profiles from different temperature regimes in the weld zone, also having the hardness map of the specimen, it is possible to have an estimation of the present phases without optical microscopy [8]. However, as described in the current work, due to the fact that the knowledge of phases' morphology in the weld zones is as essential as the distribution of microstructural components based on their influence on mechanical properties, utilization of both hardness mapping and optical microscopy methods is suggested. The linear hardness profiles of RQT701-20F and RQT701-20I specimens are demonstrated in Figure 4-23 and Figure 4-24, respectively. In each case, the profiles are given in three different zones: a) cap, b) middle, and c) root. The black and red colored lines in the diagrams are related to the examination of two closely selected paths within each specific zone. Looking through the linear hardness profiles, it is seen that there is a certain drop in the hardness values when passing across the FZ/HAZ boundary. The reason is however different when talking about RQT701-20F and RQT701-20I specimens. In the case of RQT701-20F samples (Figure 4-23), the FZ consists of bainite and martensite phases as mentioned before by means of optical microscopy. On the contrary, the HAZ is completely bainitic. Passing



through such a boundary reduces the hardness substantially from 400HV0.8 to 280HV0.8 (Figure 4-23).

Figure 4-23. Linear hardness profiles of RQT701-20F specimens: a) cap;

b) middle; and c) root.



Figure 4-24. Linear hardness profiles of RQT701-20I specimens: a) cap;

b) middle; and c) root.



In addition, the hardness values throughout the FZ area is almost stable at around 400HV0.8. Such an average is expected to indicate an almost 50%-50% bainitic-martensitic microstructure using the mathematical estimation method mentioned in 4.3; although an exact estimation is possible only after improvement of the formula based on the chemical composition of the investigated steel welds. Different trends are depicted in Figure 4-24 in case of RQT701-20I specimens. Despite of a sharp drop of hardness values in the borderline of FZ and HAZ (when coming from FZ into HAZ), it is seen that the mentioned drop in hardness values is available on both sides of the boundary. The microstructural images of these zones show a bainitic-ferritic structure in both FZ and HAZ. The average hardness values of 250-350HV0.8 on both sides of the FZ/HAZ boundary can also confirm the presence of a ferrite-bainite mixture. Therefore, the presence of the hardness peak on the borderline of FZ and HAZ – despite of no change in the available microstructural phases - can be justified due to the developed equiaxed structure in the vicinity of FZ. This fact plus the later development of rather coarser structures when going farther from FZ/HAZ boundary, decreases the hardness dramatically. 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.




- Non-isothermal compressive deformation of cylindrical steel samples is heterogeneous, i.e., the effective strain and cooling rate along the horizontal centerline of the samples vary. Consequently, distribution of the produced phases is not homogeneous. This means that light optical or scanning electron microscopy investigations on only a few selected points of the heterogeneously deformed surfaces are not the proper techniques to identify the phase fractions within the experimental specimen. Hence, surface hardness mapping technique as well as dilatation data were used to identify the present phases. It is concluded that these techniques are accurate, applicable, and comparable. - Hardness mapping technique is a powerful method to distinguish between the phases with close microstructural appearances under the optical microscopy. It means that the usual problems regarding discrimination between martensite and bainite can be easily removed. In addition, further works on the field can enhance the possibility for the determination of different morphologies of a single phase, e.g. different ferritic and/or bainitic structures, based on specific hardness intervals. - Despite of various factors affecting the resultant dilatation values, the suggested comparative calculation method in the current work, seems to be reliable due to its consistency with other characterization methods.



- The presented mathematical formula in the current study has been developed based on simple physical assumptions. The results are applicable on two different steels. However, simple improvements might be required – i.e. due to the hardness of a fully martensitic microstructure – when handling the steels with compositions far different from the investigated steels here. - Because of the current deficiencies for the determination of different morphologies of ferrite and bainite using a single hardness criterion, and the importance of those information for the mechanical properties of the weld zone, optical microscopy is still required beside the hardness mapping data.



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