MICROMAGNETIC AND MULTIPARAMETER MEASUREMENT FOR MICROSTRUCTURAL MATERIAL PROPERTIES CHARACTERIZATION By Shuo Zhang A THESIS Michigan State University in partial fulfillment of the requirements Submitted to for the degree of Electrical Engineering – Master of Science 2018 ABSTRACT MICROMAGNETIC AND MULTIPARAMETER MEASUREMENT FOR MICROSTRUCTURAL MATERIAL PROPERTIES CHARACTERIZATION By Shuo Zhang Magnetic Barkhausen noise (MBN) is measured in low carbon steels, and the relationship between microstructural properties and parameters extracted from MBN signal has been characterized. In the present study, the relationship between the number of turns of pick-up coils and MBN signals in both time-domain and frequency-domain is studied for the sensor coil optimization. With optimized pick-up coil, the characteristics of MBN are investigated for various mild steels with different grain sizes, carbon contents and hardness. To investigate the relationship between profiles of MBN signals and carbon contents of samples, the parameter has been extracted experimentally by fitting the original profiles with two Gaussian curves. The gap between two peaks (∆G) of fitted Gaussian curves shows a better linear relationship with carbon contents of samples in the experiment. The peak positions of MBN signal’s frequency response profiles have been observed decreasing with the increase of grain sizes. The fact is related to the length of two pinning sets reduces with the increase in the grain size. As a result, the frequency increases for the decrease of the time interval between two impulses. Due to the mechanical properties, such as hardness, are closely related to the grain size of the mild steels, the relationship can be described by Hall-Petch relation. The hardness can be predicted with the parameter MBN frequency peak position. To ensure the sensitivity of measurement, advanced multi-objective optimization algorithm Non-dominant sorting generic algorithm III (NSGA III) has been used to fulfill the optimization of the magnetic core of sensor [1]. The relationship between the properties of samples and Magneto-Acoustic Emission (MAE) signals has also been investigated. Multi-features have been extracted and selected to fit a linear regression model to predict the hardness and grain size of the samples. ACKNOWLEDGEMENTS I want to express my appreciation for Professor Yiming Deng, my adviser, who give me patient instruction for the research and my academic work. And I would like to thanks for the tremendous support of my family and friends throughout my time at school. This work is partially supported by the U.S. Department of Transportation CAAP Research Grant: DTPH5615HCAP03L. I wish to thank project manager Dr. J. Merritt, J. Arnold and J. Prothro for their support. The sample heat-treatment was processed by Hansen Balk steel treatment company. I would like to show my thanks for the manager Martin Balk for the support. iii TABLE OF CONTENTS LIST OF TABLES . LIST OF FIGURES . CHAPTER 1 1.1 Motivation . . 1.2 Background . vi . . . . . . . . . . . . . . . . INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vii 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.2.1 Review of micro-magnetic and magnetic method . . . . . . . . . . . . . . 2 2 1.2.1.1 Hysteresis loop . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.2.1.2 Magneto-Acoustic Emission . . . . . . . . . . . . . . . . . . . . 1.2.1.3 Magnetic Barkhausen Noise . . . . . . . . . . . . . . . . . . . . 7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11 . . . . . . . . . . . . . . . . . . 1.3 Contributions . 1.4 Summary . . . CHAPTER 2 METHODOLOGY . . 2.1 Sample preparation . . 2.1.1 Sample heat treatment 2.2 Properties measurement . . 2.2.1 Microstructure 2.2.2 Vickers hardness test 2.3 Optimization algorithm . 2.4 Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 . 17 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.1 Schematic . . 3.1.1 Hall sensor 3.1.2 CHAPTER 3 EXPERIMENT SET-UP FOR MBN . . . . . . . . . . . . . . . . . . . . . . 21 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Sensor Holder design and sensor coil connection . . . . . . . . . . . . . . 23 3.2 Data acquiring and storing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 3.3 Data processing and parameter extraction . . . . . . . . . . . . . . . . . . . . . . 25 3.3.1 Root mean square . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 3.3.2 MBN profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 Frequency spectrum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 3.3.3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 3.4 Optimization program . . 3.5 Summary . . . . . . . . . . . 4.1 Schematic and sensor of MAE experiment 4.2 Data processing . CHAPTER 4 EXPERIMENT SET-UP FOR MAE . . . . . . . . . . . . . . . . . . . . . . 33 . . . . . . . . . . . . . . . . . . . . . . 33 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35 4.2.1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35 4.2.2 Linear regression . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 4.2.3 Data preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37 . Package tsfresh . 4.3 Summary . . . . . . . . . . . iv . . . . CHAPTER 5 RESULTS . . 5.1 Optimization results . Sensor optimization with NSGA III . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38 5.1.1 MBN signals for different of pick-up coils . . . . . . . . . . . . . . . . . . 38 5.1.2 . . . . . . . . . . . . . . . . . . . . . 40 5.2 Carbon content effect on the MBN signal . . . . . . . . . . . . . . . . . . . . . . . 41 . 43 5.3 Grain size effect on MBN frequency spectrum . . . . . . . . . . . . . . . . . . . 5.3.1 Grain size effect on MBN frequency spectrum . . . . . . . . . . . . . . . . 43 5.3.2 Excitation signal effect on MBN frequency spectrum . . . . . . . . . . . . 47 Predict hardness with parameter frequency peak position . . . . . . . . . . 49 5.3.3 . . . . . . . . . . . . . . . . . . 51 . 52 5.4 Predict grain size and hardness with MAE signal 5.5 Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . CHAPTER 6 CONCLUSION AND FUTURE WORK . . . . . . . . . . . . . . . . . . . 54 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55 6.1 Conclusion . 6.2 Future work . . . . . . . . . . . . . BIBLIOGRAPHY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 v LIST OF TABLES Table 21: Carbon content, grain size, Vickers hardness and heat treatment of steel samples 18 Table 51: Decision making with L2 norm with different weight . . . . . . . . . . . . . . . 40 Table 52: Predicted hardness and corresponding error of steel samples . . . . . . . . . . . 51 vi LIST OF FIGURES Figure 11: B-H Curve and parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . Figure 12: Diagrams illustrating measurements of MAE signal . . . . . . . . . . . . . . . Figure 13: Principle of Magnetic Barkhausen Noise . . . . . . . . . . . . . . . . . . . . . 3 6 8 Figure 21: Iron carbon phase diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Figure 22: Annealing process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Figure 23: Normalizing process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Figure 24: Microstructure of steel samples with magnefication of 1000X . . . . . . . . . . 16 Figure 25: The diagram for Vickers hardness test . . . . . . . . . . . . . . . . . . . . . . 17 Figure 26: Vickers hardness tester . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Figure 27: Pareto-front for cost and comfort of the car . . . . . . . . . . . . . . . . . . . 19 Figure 28: NSGA II algorithm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 Figure 31: The schematic and physical prototype for the experimental setup . . . . . . . . 21 Figure 32: Printed circuit board to hold the hall senor . . . . . . . . . . . . . . . . . . . . 22 Figure 33: Transfer characteristics of Hall sensor . . . . . . . . . . . . . . . . . . . . . . 22 Figure 34: Transfer characteristics of Hall sensor . . . . . . . . . . . . . . . . . . . . . . 23 Figure 35: Transfer characteristics of Hall sensor . . . . . . . . . . . . . . . . . . . . . . 24 Figure 36: Transfer characteristics of Hall sensor . . . . . . . . . . . . . . . . . . . . . . 24 Figure 37: The schematic of the Labview program . . . . . . . . . . . . . . . . . . . . . 25 Figure 38: The front panel of the Labview program . . . . . . . . . . . . . . . . . . . . . 26 Figure 39: Magnetic Barkhausen Noise periodic signal . . . . . . . . . . . . . . . . . . . 27 Figure 310: Magnetic Barkhausen Noise signal for one period . . . . . . . . . . . . . . . . 28 vii Figure 311: Magnetic Barkhausen Noise signal for one period . . . . . . . . . . . . . . . . 28 Figure 312: Magnetic Barkhausen Noise profile . . . . . . . . . . . . . . . . . . . . . . . 29 Figure 313: Frequency spectrum, frequency profile and fitted curve of sample 1008 . . . . . 30 Figure 314: Flowchart of optimization and ANSYSEM models . . . . . . . . . . . . . . . . 31 Figure 315: Variables and objectives for optimization . . . . . . . . . . . . . . . . . . . . . 31 Figure 41: Schematic for the MAE experiment set-up . . . . . . . . . . . . . . . . . . . . 34 Figure 42: physical prototype for the sensor . . . . . . . . . . . . . . . . . . . . . . . . . 34 Figure 43: Wide-band AE sensor and frequency response . . . . . . . . . . . . . . . . . . 34 Figure 44: schematic of tsfresh . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 Figure 51: Normalized MBN profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39 Figure 52: Normalized MBN frequency response . . . . . . . . . . . . . . . . . . . . . . 39 Figure 53: Pareto front in objective field . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 Figure 54: Measured MBN profiles fitted with two Gaussian curves . . . . . . . . . . . . . 42 Figure 55: The gaps between two peaks for both simulated and experimental results as a function of carbon contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Figure 56: Fitted MBN frequency profiles of different samples . . . . . . . . . . . . . . . 45 Figure 57: MBN frequency response peak position as a function of grain size . . . . . . . 45 Figure 58: MBN frequency response peak position as a function of grain size (grain size larger than 15 µm) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46 Figure 59: MBN frequency response peak position and grain size for each samples (high amplitude excitation signal) . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46 Figure 510: Fitted MBN frequency response peak profile for samples with different exci- tation signal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 . . . . Figure 511: MBN frequency response peak position as a function of grain size (high amplitude excitation signal) . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 viii Figure 512: Hardness as a function of grain size . . . . . . . . . . . . . . . . . . . . . . . . 50 Figure 513: Predicted hardness and hardness measured by Vickers hardness tester . . . . . . 50 Figure 514: Predicted grain size with different datasets . . . . . . . . . . . . . . . . . . . . 51 Figure 515: Predicted grain size with MAE signal and actual grain size . . . . . . . . . . . 52 Figure 516: Predicted hardness with MAE signal and hardness measured by Vickers hard- . . . . ness tester . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 ix CHAPTER 1 INTRODUCTION 1.1 Motivation Over the next decade, the demand for energy is projected to reach record levels. The United States has a golden opportunity to become a powerhouse in global energy markets, to truly achieve full energy independence and to use natural gas to power our economy. The pipeline infrastructure forms a critical aspect of US economy. The United States system for natural gas pipelines consists of 210 systems overall running through the different states. This makes the accurate pipe property determination crucial, especially in the field of oil and natural gas transportation. At the present date, 63 percent these pipelines contain too many twists and turns that do not allow the conventional methods of inspection such as pipeline inspection gauge (PIG), or automatic robots to be used in such situations. And those pipelines, which have been laid down for decades of years, usually lack reliable information for the property and microstructure changing and then issues in the concern for the safety and integrity of the whole system. Therefore, accurate and efficient pipeline properties determination and evaluation is crucial for maintaining the healthy and long-lasting system. However, to characterize the piping materials for better understanding the microstructure properties, state-of-the-art techniques relying on microscopes often involve destructive procedures (polish and etch) for microstructure observation and identification of chemical constituents to estimate material properties accurately which is impossible for in-situ inspection. Due to various gaps that exist in pipe properties measurement, the desire for novel techniques provides the impetus for the development of Micromagnetic method, such as Magnetic Barkhausen Noise (MBN) and Magneto-Acoustic Emission (MAE), which are sensitive to the multi-properties of ferromagnetic materials. This M.S. Thesis work is to involve estimation of the basic material properties, microstructure, composition, etc. with the use of electromagnetic and acoustic sensors and Several major tasks are proposed to address the above-mentioned M.S. Thesis work objectives. 1 New parameters have been extracted and new methods have been developed for properties charac- terization. Experimental testing, advanced data analysis, and probabilistic methods are integrated into the proposed tasks. 1.2 Background 1.2.1 Review of micro-magnetic and magnetic method For the ferromagnetic materials, they consist of small, finite and magnetic regions called domains which are randomly oriented in the virgin state. In the peacetime its direction desultorily, magnetic mutual offset, the whole object does not show magnetism. When the magnetic field H applied, the magnetization vectors inside the domain would rotate into the direction of the applied field and convert the multi-domain state into a single domain. This process is performed by moving the domain walls, the so-called Bloch wall, stepwise [2] [3]. Those discontinuous pulses due to movement of domain wall can be measured in the form of both magnetic signal and acoustic signal. 1.2.1.1 Hysteresis loop Among different kinds of magnetic inspection, the measurement of the hysteresis loop of steel is the most common way to get information about the microstructural changes and material properties. Fig. 11 shows the graph of typical hysteresis loop and the definition of various parameters derived from hysteresis loops such as coercive force and remanence. For ferromagnetic material, the coercivity is the intensity of the applied magnetic field required to reduce the magnetization of that material to zero after the magnetization of the sample has been driven to saturation. And the remanence or remanent magnetization or residual magnetism is the magnetization left behind in a ferromagnetic material after an external magnetic field is removed. Those paramters have been investigated to measure the hardness, residual stress, and plastic deformation. The effect of stress on the magnetic hysteresis properties of different kinds of steels have been investigated by various of authors. K.J. Stevens measures the uni-axial stress by the magnetic properties such as maximum magnetization, remanence, and coercive field get from hysteresis 2 Figure 11: B-H Curve and parameters loops [4].An experimental investigation was carried out to study the effect of stresses that approach and exceed the yield point, on the magnetic properties of ground samples of medium carbon steel upon surface grinding by M. Vashista et al.. It shows that maximum magnetization and permeability derived from hysteresis loop increase with residual stress but starts to decrease when tensile residual stress exceeds yield strength of material [5]. H. Kwun et al. shows the hysteresis loops in specimens of AISI 410 stainless and SAE 4340 steels were sensitive to both hardness and stress. Qualitatively, for all the specimens investigated, tensile stress increased the magnetic induction (B) and the slope of the sides of the hysteresis loops; compressive stress did the opposite [6]. The magnetic hysteresis loop is also sensitive to the plastic deformation of the steels. Few investigators have demonstrated their results in the papers. Plastic deformation affects the hysteretic magnetic properties of steels because it changes the dislocation density, which affects domain-wall movement and pinning. J.M. Makar et al. report measurements of the bulk magnetic properties of pearlitic steels recorded in-situ during plastic deformation. Remnant magnetization was found to increase at lower tension levels, but higher stress levels produced a decrease in value that was attributed to stress induced changes in magnetic anisotropy. The high field magnetization decreased 3 monotonically with stress in both the pre-yield and plastically deformed regions [7]. Martin J. Sablik et al. modify the model to study the effect of plastic tensile deformation on hysteresis loops with the same Bmax .With increasing residual tensile strain Hc increase, the slope of the hysteresis loop decreases, whereas with increasing elastic tensile strain, the slope increases [8]. The influence of microstructure transformation of the steel after room temperature rolling is also an essential part of the magnetic hysteresis loop. The detection of α martensite phase in austenitic stainless steel after 15 to 55% reduction in thickness was investigated by K. Mumatz et al. Saturation magnetization was increased with the increasing percent reduction in thickness for the increasing volume percent of α martensite. Whereas coercive force and remanence ratio decreased with the increasing percent reduction in thickness. These results were attributed to the shape magnetic anisotropy due to formation of a different shape of martensite [9]. Low carbon steel specimens cold rolled at ratios of 0–40% have been examined comprehensively by H. Kikuchi et al.. the coercive force and the magnetizing current at peak in rms voltage increase monotonically due to the increase in dislocation density below 10% and the formation of cell structure; these microstructural changes enhance the intensity of interaction between pinning site and domain wall [10]. Other microstructural or mechanical properties, such as grain size, hardness and even aging of steels also have an impact on the magnetic hysteresis loop. JW Wilson et al. have established the correlations between electromagnetic properties and hardness of power generation steel (P9 and T22) with the different microstructural state through major and minor B-H loop measurement [11]. F.J.G. Landgraf et al. show how the hysteresis curve is changed with variables such as the second phase, grain size, texture and deformation. The growth of a second phase (as in aging) or the decrease in grain size show changes in the domain wall movement region (coercive force) and the domain annihilation region with little change in the domain nucleation region. In the case of the effect of texture and deformation, a larger amount of domain rotation can explain the decrease in remanence and high-induction permeability [12]. J.N. Mohapatra et al. recorded and analyzed for 5Cr–0.5Mo steel after aging at 600 ℃ for various lengths of time. A decrease in coercivity at the initial stage of aging, extending up to 200 h of aging, was found due to the interstitial carbon 4 diffuses towards the grain boundary making the matrix magnetically softer. Beyond 200 h of aging the precipitation of alloy carbides attains subsequent growth, making the material magnetically harder [13]. However, there are some drewbacks for the hystersis loop. The hystersis loop of the steel is influenced by multiproperties of the steel and can hardly find a linear relationship for properties characterization. 1.2.1.2 Magneto-Acoustic Emission Magneto-Acoustic Emission (MAE) is acoustic emission pulses driven by local sources of mag- netostriction strain due to the irreversible displacement of domain walls which is similar to the Magnetic Barkhausen Noise (MBN). Whereas, MAE only responses to the non-180 degree domain wall, for the reason that 180-degree domain wall will not influence the magneto-elastic energy. The MAE signals with low amplitude and high frequency (50KHz-1MHz) can be detected by high sensitivity acoustic emission sensor with wide operating frequency band. Therefore the MAE effect is determined by both magnetic and elastic properties of ferromagnets. Fig. 12 illustrates the shape of MAE signal when the triangular magnetic field applied. The peak of the MAE signal is happened near the coercivity points of the hysteresis loop. Due to the mechanism of MAE, it is sensitive to multi-properties of the ferromagnetic materials and carries information of changes in microstructure and mechanical properties. Based on analysis of some typical features of MAE signal [14] [15] [16] in time domain such as the root-mean-square (RMS) value, the peak value, position and number of the pulse during a period, the relationship between MAE signal and crystallographic texture, plastic and elastic stress has been investigated. D. O’Sullivan et al. found that MAE absolute energy is linearly inversely proportional to hardness for both the plastically strained and heat treated samples. With high measurement depth than MBN, MAE can be used as an efficient tool to evaluate the information along depth direction [17]. John W. Wilson et al. used MAE and MBN for case depth measurement in En36 5 Figure 12: Diagrams illustrating measurements of MAE signal gear steel. The overall amplitudes for both MBE and MAE exhibit a good correlation with case depth [18]. K. Praveena et al. investigated the MAE signal for sample nanocrystalline Mn-Zn ferrites and found that the MAE activity along hysteresis loop is proportional to the hysteresis losses during the same loop and the domain wall creation or annihilation processes are the origins of the MAE [19]. R. Ranjan et al. had dealt with the effects of grain size and carbon content on the magnetic properties of steel. And the MAE had shown an increase in the number of pulses and average pulse height with the grain size [20]. Miriam Rocío Neyra Astudillo et al. had studied the MBN and MAE for A508 Class II forged steel used for pressure vessels in nuclear power stations and showed that the MBN and MAE signal is sensitive to the crystallographic texture and microstructure [21]. D.H.L Ng et al. reported that MAE is capable of detecting the direction of the stress axis for mild steel and nickel bars [22]. Whereas, there are some drawbacks for MAE measurement. At first, the technique is sensitive 6 to disturbing noise in the environment. As a result, it has a low signal to noise ratio. Secondly, the MAE signal only response to non-180 degree domain walls. So investigations with this technique are of interest for comprehensive interpretation studies and their interaction with the microstructure is observed. 1.2.1.3 Magnetic Barkhausen Noise MBN is a promising nondestructive electromagnetic method for detecting properties of the ferro- magnetic materials. The simple principle of the Magnetic Barkhausen Noise shows as following: a) Magnetic domains show random orientation without the external magnetic field. b) Those domains with moments aligned most closely with the applied field will increase in volume at the expense of the other domains. c) The move of the domain wall is discontinuous. The irreversible jump of domain wall energy for encountering pinning sites will lead to uneven and discontinuous change in magnetization. d) This uneven change will lead to the tiny impulse in the hysteresis curve like (d) show in figure 13. With the principle showing above, the MBN signal shows excellent performance in evaluating mechanical characterizations and electromagnetic properties of steel, and this is due to the sen- sitivity of MBN signals to microstructural changes. The relationship between MBN signal and microstructure (grain boundary [23], grain size [23], composition [24]), hardness [25], applied and residual stress [26], fatigue and damage [27], and the plastic and elastic deformation [28] have been investigated based on the analysis of typical features of MBN signal in time domain (such as the root-mean-square (RMS) value, the peak value, position and half-width value of profile curve). The effect of microstructure on the MBN signal has been widely investigated for different aspects and different samples in details. Ktena et al. compared interlaboratory results about the relationship of MBN and grain size and the strain showed that MBN decreases with increasing grain size and increases with strain, consistently [29]. H. Sakamoto et al. described the theoretical relationships between RMS values of MBN and the microstructures of carbon steels. It showed 7 1/2 g in ferrite grains and RMS =Cp*d2 that RMS = Cg*d p in cementite-dispersed ferrite grains, where dg and dp are ferrite grain size and cementite particle diameter, respectively. Cg and Cp are constant [30]. S. Yamaura et al. also got the same relationship between MBN RMS value and the grain size for pure iron samples with different heat treatment [23]. MBN signal is also sensitive to the grain phase and composition fraction. L. Clapham et al. presented that the pearlite content of plain carbon steels has a significant effect on MBN signal. The MBN pulse height distribution for fully pearlitic steels is highly asymmetrical, exhibiting a tail. Conversely, samples containing no pearlite generated a comparatively narrow and symmetrical pulse height [31]. The characteristics of the Barkhausen noise phenomenon were investigated for various crystalline microstructures of plain steels by O. Saquet et al., including ferrite, pearlite, and martensite, which enabled us to get a better understanding of the dependency of MBN signal on complex microstructure [24]. (a) (b) (c) (d) Figure 13: Principle of Magnetic Barkhausen Noise Another application for MBN signal is to measure the hardness of the steel and the depth of case hardened or decarburized steel. Franco et al. showed linear correlations between different MBN parameters and hardness measurements in the steel SAE 4140 and SAE 6150 with different excitation signal frequency [32]. M. Blaow et al. concluded in the paper that the shape and position of the MBN profile are significantly affected when a gradient in microstructure is induced by a gradient in carbon content [33]. V. Moorthy et al. analyzed the MBN signal with a number of narrow ranges of low frequencies to give useful insights into the microstructural gradient through the depth of the case. This type of analysis might also be used to evaluate steels with different case depths, as it would indicate the approximate depth at which the transition from the hard to the softer 8 region takes place [25]. O. Stupakov et al. investigated the applicability of the BN technique for evaluation of the decarburization depth of the industrial spring steel. The classical number of BN counts and especially the alternative second-peak-based parameter U2, were shown to be perfect indicators of the sand blasting treatment having perfect sensitivity with the decarburization depth of up to 150-200 µm [34]. MBN is also a very promising method for non-destructive, fast and accurate prediction of residual stresses. Stewart et al. analyzed the different parameters of MBN with applied stress, including tension and compression, and determined residual stress near the edge of the weld with the conclusion [35]. J. Anglada-Rivera showed that the peak amplitude of the Barkhausen voltage increases with the applied stress, reaching a maximum value and then beginning to decrease at higher tensile stress for 1005 commercial steel [26]. H.Ilker Yelbay developed an MBN stress calibration set-up and a residual stress measurement system with scanning ability to determine the residual stresses in the welded steel plates by MBN technique [36]. MBN is also an efficient tool to detect the damage of plastic deformation and fatigue load. A. Dhar et al. measured the MBN signal on hot-rolled mild steel samples uniaxially deformed to differing magnitudes of plastic strain to study the dependence of MBN activity on the plastic strain. Angular MBN had been implied to monitor the deformation induced magnetic anisotropy [37]. C.- G. STEFANITA et al. performed a study to differentiate the effects of elastic and plastic deformation on MBN signal. Elastic strain effects on the MBNenergy were determined to be far more significant than plastic strain effects [28]. The various stages of fatigue damage in low carbon structural steel had been characterized using MBE signal analysis technique during high cycle fatiguing by S. Palit Sagar et al. The observed trends in the variation in MBE peak voltage showed an initial increase followed by a decrease. After that, a sharp increase was found during online monitoring of fatigue till failure [27]. 9 1.3 Contributions It is known that the frequency response of the pick-up coils would change with the number of turns winded. The peaks of frequency response move to the lower frequency with the increase of the number of turns of pick-up coil [38]. In this paper, the relationship between the MBN profile and frequency response and pick-up coils with turns number 80, 200, 400 have been investigated as guidance for the choice of pick-up coils for the experiment. Other than those conventional parameters mentioned in previous work, new parameters have been introduced and related to significant microstructural properties. Pérez-Benitez et al. presented a numerical model to fit the original experimental results and showed that the carbon content was linear to define a parameter “overlapping factor” which is the gap between two peaks of theoretical fitting curves [39]. Vashista et al. used two Gaussian curves to fit the two peaks of 18NiCrMo5 steel with different treatments and extracted parameters of two peaks include peak height, peak position and the full width of half maximum [40]. In present work, two methods have been combined. Parameter gap between two peaks (∆G) extracted from the fitting curve fitted by two Gaussian curves shows a linear relationship with the carbon content of samples. Other than those parameters extracted in the time domain, it is also important to study the results from the frequency response of the MBN signal, which provides a wealth of information. S. Yamaura et al. derived a new parameter, P60/P3, to study the effect of grain size of pure iron specimens on the Barkhausen noise, where P60 and P3 are the spectrum intensities at 60 kHz and 3 kHz respectively [23]. M. Vashista et al. showed that the frequency response of the pick-up coils would change with the number of turns of the coil. The peaks of frequency response move to the lower frequency with the increase of the number of turns of pick-up coil [38]. In this study, the relationship between the MBN frequency response and grain size and hardness of samples in the experiment. For frequency response for different samples, in contrast to the description in the previous paper [38] that the frequency response of a pick-up coil does not change significantly with the different microstructure of test material, as grain size decreases, the position of peaks of frequency profiles increases. For mild steels, the grain size of the steels and the their hardness exist 10 the hall-petch relationship. Therefore, we can predict the hardness with the parameter Fpp. Similar to MBN, MAE is due to the displacement of domain wall during magnetization. Whereas, MAE is acoustic emission signal detected by the acoustic sensor. Even though, the sensor we are using is a highly sensitive wide-band acoustic sensor, tremendous acoustic noise in the environment will have an influence on the signal measured. Therefore, the signal to noise ratio of MAE signal is relatively smaller than MBN signal’s, making it difficult for parameter extraction. As a result, for signal processing of MAE signal, we introduce the machine learning method for feature extraction and linear regression. The hardness and grain size have been predicted in the network and the results show good accuracy. Considering the sensitive, weak and noise-like properties of the MBN signal, a suitably effi- cient sensor is indispensable to achieve accurate measurement of the microstructure of materials. Previous work has investigated the relationship between the magnetic field with different single objectives like material of the core, the shape of core tips and distance between two poles [41]. These kinds of studies are important as the guidance for designing the experiment but are still not enough when there is a trade-off between two objectives. To ensure the sensitivity of the measurement, a detailed parametric study of sensor core design is conducted with multi-objective optimization algorithm NSGA III [42] and ANSYSEM simulation. An optimized sensor which is suitable for various diameter pipes is developed. 1.4 Summary The principle and application of traditional magnetic and micro-magnetic method has been reviewed in the behind section. The Magnetic Barkhausen Noise method with wide application and sensitivity has been chosen as the main method for investigation. Contributions for this paper has been summarized and described. 11 CHAPTER 2 METHODOLOGY 2.1 Sample preparation 2.1.1 Sample heat treatment Parallelepiped samples were prepared from various types of mild steels obtained commercially, which include 1008, A36 and 1018 with different carbon contents of 0.04 wt%, 0.12 wt% and 0.19 wt% respectively. As Fig. 21 showing, those steels using in the experiment whose carbon contents less than 0.83% mainly consist of ferrite and pearlite. To change the microstructure of steels obtained off-the-shelf and investigate the influence of heat treatment to the Barkhausen noise signals, each kind of steels were normalized and annealed by heating the samples above the Ac3 around 50 ◦F to 150 ◦F to austenitize the original grains. The carbon contents of the samples are from 0.04 wt% to 0.19 wt %, according to the Fig. 21, the corresponding austenitizing temperature are from 1600 ◦F to 1650 ◦F. Considering all the samples, we set the temperature with 1706 ◦F as shown in the Fig. 22 and Fig. 23. The heat rate for the heat treatment also has an influence on the austenitize temperature, the samples have been heated with a related slow ramp rate of 300 ◦F/ h to make sure a low austenitize temperature. To make the sample heated sufficiently, according to the thickness of the sample, the samples have been held at the temperature for one hour. The cooling rate, which is the only difference between annealing process and normalizing process, is the most import procedure to control the grain size and grain phase of the steel. For annealing, the steels are cooled in the furnace with a relatively slow rate of 225 ◦F / h to around 800 ◦F. This process will lead to a coarse-grain structure of the steel. The grain size will become smaller with the increase of the cooling rate. For normalizing, the samples are cooling in the air which has a relative higher cooling rate and leads to a fine-grain structure. The grain phase of the steel after annealing and normalizing are still ferrite and pearlite. Whereas, martensite will present when the cooling rate 12 increase further, such as cooling in water or oil, which is known as quenching. Each kind of steels was normalized to get samples 1008 N, A36 N and 1018 N and annealed to get the samples 1008 A, A36 A and 1008 A with the vacuum furnace. To make the samples fully saturated, all steels were cut into small pieces with dimensions of 100mm × 30mm × 4.76mm. Specially, steel 1026 pipeline with outside diameter of 152.4 mm and a wall thickness of 4.57 mm is introduced to be examed the relationship between carbon content and the MBN signal and to be used in optimization of the sensor geometry. Figure 21: Iron carbon phase diagram 2.2 Properties measurement 2.2.1 Microstructure To observe the microstructure on the surface of each sample, small pieces of the samples were cut and polished with diamond paste (6 µm and 0.2 µm).The metallographic structure was revealed by etching with the 4% Nital solution. Fig. 24 shows the microstructure observed under an optical microscope with the magnification of 1000X. Bright regions in the majority of the picture represent 13 Figure 22: Annealing process Figure 23: Normalizing process 14 the ferrite grains and the dark ones spread in between are pearlite grains, which can be taken as the second phase particles. With the graph obtained from the microscope and the scale bar marked on the bottom right corner of the picture, we can predict the area for the whole picture. The grain number can be counted from the picture and the average grain size for ferrite grain can be calculated. The grain size, grain shape, Vickers hardness and second phase percentage drastically changed after heat treatment. From the Fig. 24, we can find that the grain size for annealed sample is larger than normalized one, which is consisted with the conclusion before. And the second phase (pearlite, dark particles) proportion will change a lot during heat treatment. The samples 1018, 1018 annealed, 1018 normalized, A36 and A36 normalized all have a large propertion of pearlite grains. 2.2.2 Vickers hardness test The Vickers hardness test method is very useful for testing on a wide type of materials, but test samples must be perfectly polished to enable measuring the size of the impressions. It consists of indenting the test material with a diamond indenter, in the form of a right pyramid with a square base and an angle of 136 degrees between opposite faces subjected to a load of 1 to 100 kgf. The full load is normally applied for 10 to 15 seconds. After loading, when we move the indenter away, there is a small impression with the shape of rectangular pyramid under the microscope. The Fig. 25 shows the diagram for the Vickers hardness test and the top view of the impression. By using screw micrometer, the diagonal lengths, which are the d1 and d2 in Fig. 25, can be measured accordingly. The HV number is determined by the ratio F/A, where F is the force applied to the diamond in grams-force (gf) or kilograms-force (kgf) and A is the surface area of the resulting indentation in square micrometers mm2 or square millimeters µm2. A can be determined by the formula 2.2 : d = d1 + d2 2 15 (2.1) (a) 1008 (b) 1008 annealed (c) 1008 normalized (d) 1018 (e) 1018 annealed (f) 1018 normalized (g) A36 Figure 24: Microstructure of steel samples with magnefication of 1000X (h) A36 annealed (i) A36 normalized d2 d2 ≈ HV = F A ≈ 1.8544 • F d2 A = 1.8544 2 • sin(136◦ 2 ) mm2] ≈ 1854.4 • F [ kg f d2 (2.2) (2.3) [ g f µm2] The F in equation 2.3 stands for the load force, which is set by yourself. The d represents the average of two the diagonal line of the indent. Vickers hardness values are generally independent of the test force. And Fig. 26 shows the tester we are using. On the top of the machine, there are screw micrometers to measure the diagonal lengths through the microscopes. On the middle of the 16 picture, it is the main part of the machine, which includes the diamend indenter, microscope and the platform to fix and control the position of samples. On the bottom of the device, there is a green button on the panel to start loading of the force. Figure 25: The diagram for Vickers hardness test The micro-hardness of the samples are obtained with Vickers hardness tester with load 200g f . According to equation 2.1 and 2.3, we can calculate the Vickers hardness for different samples. The tests have been conducted on every sample for five times, and the final hardness is obtained by taking the average of results of five times.The details of the chemical composition, heat treatment process and microstructure are summarized in Table 21. From the table we can see, the Vickers hardness of the samples increase with the increase of the carbon content and decrease with the increase of the grain size. 2.3 Optimization algorithm To optimize the magnetic core of the sensor, algorithm NSGA III has been adopted and implemented. NSGA III is an advanced optimization algorithm to search the Pareto-front (optimal solution set) for multi-objective problems. For each point on the Pareto-front, we cannot find any 17 Figure 26: Vickers hardness tester Table 21: Carbon content, grain size, Vickers hardness and heat treatment of steel samples Without heat treatment Vickers hardness Heat treatment 110.21 172.19 185.33 256.84 95.06 116.33 118.81 99.71 120.7 133.43 Annealing: 1706◦F, 1hr, 4hrs cool to 800◦F Normalizing: 1700◦F to 1750◦F, 1hr, cool in air Samples 1008 A36 1018 1026 1008 A A36 A 1018 A 1008 N A36 N 1018 N Carbon Content (CC wt%) Grain Size(GS) (d/µm) 0.04 0.12 0.19 0.25 32 11 10 15 40 22.5 25 34 16.5 22 18 point which is better than it in the objective space. The Fig. 27 shows a typical Pareto-front for cost and comfort of the car. The comfort of the car will be limited by the cost of the car. The red line from point 1 to point 2 describes the set of the optimal points in the objective field when we try to minimize the cost and maximize the comfort coefficient of the car. The points in Pareto-front mean that the most comfortable car we can get with the same price. Figure 27: Pareto-front for cost and comfort of the car The procedure for NSGA II is shown bellow: 1. Pt/Qt : the parents/offspring of generation t Pt+1 : the parents of generation t+1 2. All elements in Pt and Qt compete with each other for non-domination. 3. The elements in the optimal-front F1 (if ||F1|| ≤ ||Pt+1||) are selected into the next generation. 4. This procedure repeats until ||F1|| + ||F2|| + . . . + ||Fk|| ≥ ||Pt+1||. 5. If ||F1|| + ||F2|| + . . . + ||Fk|| > ||Pt+1||, extra elements are rejected based on the crowding distance sorting. NSGA III is more effecient than the previous version NSGA II for the reson that it introduces reference direction to get a good distribution. 19 Figure 28: NSGA II algorithm 2.4 Summary In this chapter, we focus on the information obtaining and analysis about the basic steel prop- erties. At first, the process for heat-treatment of the samples has been introduced and detailed described. Samples with different grades has been annealed and normalized with vacuum furnace to change the grain size of samples. Following this, the steel microstructure analysis have been performed to obtain the grain structure images using optical microscopy. Imaging analysis will be performed to obtain the statistical information and metrics about the pipe steel microstructure, such as grain size distribution. Next, surface hardness measurements have been performed using Vickers hardness testers. And the optimization algorithm has been introduced. 20 CHAPTER 3 EXPERIMENT SET-UP FOR MBN 3.1 Schematic Fig. 31 shows the schematic and physical prototype for the experiment setting. The MBN signal is generated by discontinuous movements of domain walls when low-frequency sinusoidal or triangular signal magnetic field (5Hz) is applied. Pick-up coils attached near the surface of samples with the different number of turns (80 turns, 200 turns, 400 turns) are flexibly connected with other parts of the experimental apparatus and are used to detect Barkhausen signals. Filtering and amplifying circuit with passband 0.5 to 200 kHz is used to filter out the low-frequency excitation signal, harmonic and high-frequency background noise and to amplify the MBN signal to millivolt level. Barkhausen noise signals detected by the coil and applied signal measured from resistance in series with excitation coils were captured by the data acquiring card with the sampling rate of 200 kHz/s. Figure 31: The schematic and physical prototype for the experimental setup 21 (a) (b) Figure 32: Printed circuit board to hold the hall senor 3.1.1 Hall sensor To get the corresponding relationship between the realistic magnetic field the sample experienced and the timing when Magnetic Barkhausen Noise generated, we introduce one hall sensor which can measure the magnetic flux directly. To hold the small sensor, we design a simple PCB and connect the components to the circuit (Fig. 32). The chip with three pins is our linear hall-effective sensor SS39ET from Honeywell. With supplied voltage amplitude 5 V, the relationship of the output voltage and magnetic flux with the units gauss has been shown in Fig. 33. The sensor can measure a wide range of magnetic flux density that between -1000 gauss to 1000 gauss and with a high sensitivity 1.4 mv/gauss. With the hall sensor, we can know the magnetic field between two poles directly. Figure 33: Transfer characteristics of Hall sensor 22 3.1.2 Sensor Holder design and sensor coil connection Based on the original experiment setup, to keep the relative position of excitation core and pick-up coil consistently, we design a holder to integrate the excitation part and pick up part. The model of the holder is designed with software Auto CAD. Fig. 34 shows the schematic and physical prototype for the holder. The hollow quadrangular prism on the left-hand side is used to fasten the holder to the pole of the magnetic core. The size of the hollow prism is designed to fit the magnetic core. On the right-hand side, there is a sensor holder to hold the cylinder like pick up coil. On the top of the sensor holder, one hole is designed to allow the wire to reach out. Figure 34: Transfer characteristics of Hall sensor To investigate the influence of pickup sensor, pickup coils with the different number of turns (Fig. 36) has been introduced in the experiment. From the Fig. 35, the sensor and other parts of the experiment are flexibly connected for easy replacement. 3.2 Data acquiring and storing The processed analog signal can be acquired by NI PCI device combining with LABVIEW sampling program to convert the analog signal into the digital signal for further processing in the 23 Figure 35: Transfer characteristics of Hall sensor Figure 36: Transfer characteristics of Hall sensor computer. The maximal sampling rate for the NI card is 500 kHz/s. The LABVIEW program diagram is shown in Fig. 37. The sampling program consists of the establishment of the physical channel, setting of the sample clock, reading the sample data and writing the data to file. At first, we should set the pysical channel of the input signal. For the NI card we are using, it can support multi-channel input and output simultaneously. And then, due to the signal type we are measuring is voltage, we set the acquisition mode as continuous voltage input. For the part of the setting of the sample clock, considering the maximum frequency of the signal and the speed of reading and writing of the data acquisition equipment, we choose the frequency of 200 kHz as the sampling rate. For sample mode, we choose the continue sampling mode to get continue image on the front panel until we turn off the button. The data acquisition is done in a while loop and the recarded data is saved in a lvm file for postprocessing in MATLAB. To get the frequency spectrum of the signal directly from the front panel, we can carry on the FFT transformation on the original signal. 24 Fig. 38 shows the front panel when the input is a 100Hz sin signal. In the front panel, there are some buttons to control the maximum and minimum value for input voltage. We set the limitation for input voltage to 10 V and -10 V separately. And we can choose the acquisition channel with the button the DAQmx Pythsical channel. The maximal number of channels for the device is two considering the maximal sampling rate of the NI card and the sampling rate we choose for acquisition. One is for our excitation signal, and another is for the Magnetic Barkhausen Noise. Both of the two channels wavelets would show at the same time on the time waveform window, and their corresponding frequency spectrums would show on the spectrum window. The front panel can show the waveform simultaneously as the data acquired. Figure 37: The schematic of the Labview program 3.3 Data processing and parameter extraction 3.3.1 Root mean square The value of root-mean-square as the most popular methods to show the intensity of the Barkhausen noise is intimately linked with the properties of metals. The expression for calculating the RMS of the noise is shown in below. RMS = X2 i (3.1) (cid:118)(cid:117)(cid:116) 1 n N i=1 25 Figure 38: The front panel of the Labview program For some experiment, they are using RMS voltage meter to get the parameter directly. We can also get the value by MATLAB function rms for the Magnetic Barkhausen Noise signal acquired. 3.3.2 MBN profile MBN signals repeat every half period and usually occur around the zero cross point of the excitation signal, as shown in the Fig. 39. The blue triangular waveform is the excitational signal measured by hall sensor and the orange signal is the MBN signal. To remove the noise in the signal, an average of ten half-periods of MBN signals have been taken for subsequent data processing and analysis. To determine the start points for one period, we introduce the minimal point of excitation magnetic field measured by hall sensor as the indicator for start of the period. It is easy to find the zero cross point of the excitation signal with MATLAB program and the minimum point of the periodic signal can be obtained by adding 1/4 period after zero cross point. From Fig. 310, we can find that the original signal measured from hall sensor is not smooth enough to check the zero cross point. It is better to filter the original signal with moving average with window size 50 points. The 26 signal processed (red line) overlaps with the original one and is smoother than before. Fig. 311 shows the averaged Magnetic Barkhausen Noise and corresponding excitation signal plot against time. In consideration of the randomness of MBN, to get relative robust and reliable parameters, parameters are obtained from averaged MBN signals. Figure 39: Magnetic Barkhausen Noise periodic signal The profile of the MBN signal is extracted as a plot of RMS calculated with the adjustable window size of 1/40 of the points per period as a function of the magnetic field measured by hall sensor. The output signal for the hall sensor is voltage signal. With the transfer characteristics of the Hall sensor, we can get the B, magnetic flux density, describes the field felt by objects. With the formula H=B/µ0, we can calculate the magnetic strength which is the same when the hall sensor is close to the surface of the sample. Fig. 312 shows the Magnetic Barkhausen Noise profile and the peak position and value detected. The peak value and the position are detected by MATLAB code to feed back the maximum point of the profile and corresponding position for the point. 27 Figure 310: Magnetic Barkhausen Noise signal for one period Figure 311: Magnetic Barkhausen Noise signal for one period 28 Figure 312: Magnetic Barkhausen Noise profile 3.3.3 Frequency spectrum The frequency spectrum of the MBN signal has been determined from the Fast Fourier Transfor- mation (FFT) of the time-domain signals. Fig.313 shows the frequency spectrum of the sample 1008, the frequency profile and fitted profile correspondingly. The profile of the intensity of the frequency response has been extracted by moving average with the window size of 1000 data points. To extract the parameter peak of frequency intensity, a smooth profile has been obtained by fitting the original one with a 15-degree polynomial. 3.4 Optimization program To optimize the magnetic core of the sensor, advanced optimization algorithm NSGA III has been adopted and implemented. Fig. 314 shows the procedure of the optimization. To calculate the magnetic field at the center of two poles, a 3D model has been built in the ANSYSEM software. To reduce the simulation time it takes, half model with one symmetric boundary has been used to gain the same result. The python code as an interface between MATLAB code and simulation 29 Figure 313: Frequency spectrum, frequency profile and fitted curve of sample 1008 software ANSYSEM, can call ANSYSEM project and feed the population points into the variables to change the shape of the core in the model. And then the magnetic field value can be obtained from one text file saved after simulation procedure. Three objectives which are important for the design of the sensor for a special sample. One is to maximize the magnetic field at the center of two poles for the pick-up coil to gain a relatively strong signal. The second one is to minimize the overall effective area of the magnetic core to obtain a good spatial resolution. Also, the sample shape should be taken into consideration. The large gap between poles of the magnetic core and the pipeline sample can affect magnetic coupling and result in the lower magnetic field inside the sample. To design a sensor which is good for both the worse situation, the pipeline sample with outside diameter 6 inches and the best situation, the flat sample, two models have been built. A, b, c defined in Fig. 315 are important variables which can control the shape of the core directly. a and b as the length and width of poles have an influence on the contact area between core and samples. c determines the distance between two poles and is related to the number of turns of excitation coils winded around. As a result, in the model, the excitation signal is set linear to the parameter c. The height of the magnetic core is not taken into 30 012345678910Frequency /Hz10400.511.522.5Intensity10-3Frequency specturmFrequency profileFitted line consideration in the optimization and keeps it as a constant. Figure 314: Flowchart of optimization and ANSYSEM models Figure 315: Variables and objectives for optimization 3.5 Summary In this chapter, the detail of experiment set-up has been introduced, including the physical prototype for the excitation part as well as the software design for the data acquisation and storage. And then the basic parameters for MBN signal have been introduced and explained, like root mean square, MBN profile, and MBN frequency spectrum. All of those parameters are extracted by MATLAB code. Next, the process for optimization of the magnetic core with NSGA III has been 31 described. We introduce ANSYSEM software to calculate the magnetic field with finite element method. And the objects and variables have been presented. 32 CHAPTER 4 EXPERIMENT SET-UP FOR MAE 4.1 Schematic and sensor of MAE experiment The schematic of the MAE experiment is quite the same with the experiment set-up of MBN including signal generator, power amplifier, sensor, signal filter and amplifier and data acquisition card as shown in the Fig. 41. What is special for the MAE experiment is that, instead of magnetic coil, the MAE signal is obtained by a wide-band acoustic emission sensor made by piezoelectric materials. The structure of the acoustic emission sensor is shown in the Fig. 43 (a). Piezoelectric material is a kind of smart material which exsists the linear electromechanical interaction between the mechanical and the electrical state in crystalline materials. The acoustic emission sensor employs the reverse piezoelectric effect which is the internal generation of electrical charge resulting from an applied mechanical force. The movement of the domain wall during magnetization would generate acoustic waves with low amplitude and high-frequency (50 kHz-1 MHz). Those acoustic waves can be detected by piezoelectric crystal inside the acoustic emission sensor which give rise to structure deformation of the crystal lattice and occurrence of electric dipole moments in solids. And this can generate electrical current changing with the magnitude of mechanical stress. The Fig. 43 (b) shows a flat sensitivity from 100 kHz to 1 MHz, which is a wide-band acoustic emission sensor. An essential requirement in mounting a sensor is sufficient acoustic coupling between the sensor surface and the structure surface. The first thing is to make sure that the sensor’s surface is smooth and clean, allowing for maximum couplant adhesion. What is more, application of a thin layer couplant can fill gaps caused by surface roughness and eliminate airgaps to ensure good acoustic transmission. 33 Figure 41: Schematic for the MAE experiment set-up Figure 42: physical prototype for the sensor (a) (b) Figure 43: Wide-band AE sensor and frequency response 34 4.2 Data processing 4.2.1 Package tsfresh Tsfresh is a python package. It automatically calculates a large number of characteristics of time series signals, the so called features, including simple statistical features such as min, max and mean and frequency spectrum features. Further the package contains methods to evaluate the explaining power and importance of such characteristics for regression or classification tasks. In the process of feature extaction, there are three dictionaries predefined to selection. The ComprehensiveFCParameters includes all 788 features without parameters and with parameters. The MinimalFCParameters can be used for quick tests including around 8 features which have the "minimal" attribute. The E f f icientFCParameters contains almost the same features as in ComprehensiveFCParameters except those features are marked with the "high_comp_cost" attribute. This can save the runtime and memory of the process and is selected in our experiment. The all-relevant problem of feature selection is the identification of all strongly and weakly relevant attributes. This problem is especially hard to solve for time series classification and regression in industrial applications. To limit the number of irrelevant features, tsfresh deploys the algorithem for feature selection. It is an efficient, scalable feature extraction algorithm, which filters the available features in an early stage of the machine learning pipeline with respect to their significance for the classification or regression task, while controlling the expected percentage of selected but irrelevant features. The procedures for feature selection follow three steps and are skeched with Fig. 44. At first, a comprehensive and well-established feature cluster has been extracted to discribe the raw time series signals. In the second step, each feature vector is individually and independently evaluated with respect to its significance for predicting the target under investigation. The results of the tests is the vector of p-values, quantifying the significance of each feature for predicting the target. And then the vector of p-values is evaluated on basis of Benjamini-Yekutieli procedure [43] to determine which features to keep. 35 Figure 44: schematic of tsfresh 4.2.2 Linear regression In statistics, Linear regression is a regression analysis of the relationship between a scalar dependent variable and one or more explanatory variables using a least-squares function. The case of one explanatory variable is called simple linear regression. For more than one explanatory variable, like the situation in our experiment, the process is called multiple linear regression. In our experiment, the goal is to predict the hardness and grain size with features extracted from MAE signals. In this case, linear regression can be trained to fit a predictive model to an observed data set of hardness and grain size values of the sample and corresponding features. 4.2.3 Data preparation Data preparation is done by MATLAB code to segment the periodic MAE signal into one period signal. For each periods of signal contains 20,000 points. And for each samples, we are using 100 signals as the datasets. So there is 900 signals and around 18,000,000 points. It is a large 36 dataset, to improve the efficiency and save the run time, the E f f icientFCParameters dictionary has been used for feature extraction. The data is integrated and rearranged into the format of data input required for the package. 4.3 Summary The experiment set-up, priciple of the sensor and data processing procedure for MAE signal has been introduced in this section. Instead of magnetic coils, the MAE signal is measured by acoustic emission sensor made by piezoelectric materials which has flat frequency response over a wide-band. Data processing of the MAE signals is done by using the python package tsfresh. It is a package special for extracting and selecting features of time series signals. And then a linear regression model is followed to predict the hardness and grain size of the samples. 37 CHAPTER 5 RESULTS 5.1 Optimization results 5.1.1 MBN signals for different of pick-up coils To investigate the influence of the different number of turns of pick-up coils to the MBN signal, three different coils (80 turns, 200 turns, 400 turns) have been prepared in NDE Lab to measure the MBN emission with the same excitation signal. Fig. 51 shows the normalized MBN profiles, which have been divided by the peak values of each original profile. There is no obvious shift in the peak positions of profiles for signals detected with different pick-up coils. All peaks overlap with each other, whereas with the increase of the number of turns, the signal-to-noise ratio (SNR) has improved dramatically. The noise can be defined as the area below the minimal value of the MBN profile. Fig. 52 shows the normalized MBN frequency spectrum profile over bandwidth 0 to 100 kHz obtained from the time-domain signals above. The frequency spectrum profile is used to show the intensity changes along the bandwidth. Considering that the intensity changes with the number of turns of pick-up coils, normalized profiles can put them on the same scale and make them comparable. For the same MBN signal, it is obvious that the sensor with the larger number of turns is more sensitive to the low frequency. The coil of 400 turns has a higher intensity in bandwidth from 20 kHz to 60 kHz. The high-intensity frequency response of the coil with 200 turns shifts to bandwidth from 60 kHz to 100 kHz. For the 80-turn coil, the frequency response is almost flat over the whole bandwidth, except for some impulses related to noise. 38 Figure 51: Normalized MBN profile Figure 52: Normalized MBN frequency response 39 -3000-2500-2000-1500-1000-5000500100015002000Magnetic field H/(A/m)00.10.20.30.40.50.60.70.80.91Normalized intensity80 turns200 turns400 turnsNoise012345678910Frequency/Hz1040.750.80.850.90.951Normalized intensity80 turns200 turns400 turns 5.1.2 Sensor optimization with NSGA III (cid:118)(cid:117)(cid:116) m 3 i=1 The following Fig. 53 shows the Pareto fronts gotten from the NSGA III algorithm. The points on the surface is a set of optimal points in the objective field. For decision-making, the L2 norm method with idea point as the reference point is used to find one adequate point in the Pareto front. The defination of L2 norm method can be destribed as the formula: fi − zi − f min m is the number of objectes and z is the idea point. wi, f max d = min( f max i wi( i=1 i )2) i − f min and f min are the weight, maximal value and minimal value for the ith object. The values for each of the objects are normalized by deviding f max . By slightly changing the weight, different combinations of objectives have been gotten and shown in Table 52. Compared with the original design, the effective areas of point 1, 2, 3 decrease a lot at small sacrifices for the magnetic field. Performance improvement ratios defined as: i i i (5.1) m = optimizedi − originali originali (5.2) It is calculated by summing up the improvement ratio for each objectives. From the result, it suggests that the optimized points are better than the original design. Table 51: Decision making with L2 norm with different weight Point 3 Original design Point 1 Point 2 (1,3,3) (1,2,2) (1,1,1) Wight Effective area (mm2) 2377.17 876.60 1634.14 465.59 461.04 383.61 Magnetic field of pipeline H (A/m) 831.19 691.05 Magnetic field of flat sample H (A/m) 537.21 22.65 14.10 21.89 a (mm) 23.48 20.04 17.6 b (mm) 21.49 55.91 37.74 c (mm) 11.97% 17.23% 6.36% Performance improvement ratio 2500 490.7 780 25 25 50 40 Figure 53: Pareto front in objective field 5.2 Carbon content effect on the MBN signal Profiles of MBN signals are plotted against the real-time field measured by integrated Hall sensor. Due to the nonlinearity during the magnetization and different magnetic permeability of various samples, there are differences of positive and negative Hmax for the same and different samples. Profiles of MBN signal of samples 1008, A36 and 1018 in Fig. 24 show obvious slope changes in the high magnetic field strength which can be taken as second peaks. For steel 1026, even though there is no sharp slope change from the profile, it can be explained by the reason that the second peak merged with the first one depending on the distribution of pinning strength of microstructural obstacles in response to a given range of magnetization which has been described in previous studies [44]. For the property observed in the figure, two Gaussian curves have been used to fit two peaks in MBN profiles separately. The first peak in low magnetic field strength is related 41 (a) 1008 (b) A36 (c) 1018 (d) 1026 Figure 54: Measured MBN profiles fitted with two Gaussian curves to the nucleation and annihilation of domain walls in grain boundaries of ferrite and the second peak at higher amplitude position indicates the displacement of domain walls due to the second phase particles which are harder pearlites in samples [40]. It is obvious that the shapes of profiles for different samples change slightly with the change of the relative position of two peaks. From (a) to (d) in Fig. 54, the gaps between two peaks (∆G) defined as the difference of mean values of two Gaussian distributions become smaller with the increase of the carbon content. A plot of the parameter (∆G) and carbon content for four samples is given in Fig. 58. Most of the experimental results collected by multiple measurements lie around the fitted line suggests the reliability of the data. 42 -2000-1500-1000-500050010001500H/(A/m)00.010.020.030.040.050.060.07Voltage/V1008 MBN profilefitted curveGaussian 1Gaussian 2262.259-2500-2000-1500-1000-500050010001500H/(A/m)00.010.020.030.040.050.060.070.080.090.1Voltage/VASTM-36 MBN profilefitted curveGaussian 1Gaussian 2189.81-2500-2000-1500-1000-5000500100015002000H/(A/m)00.010.020.030.040.050.060.070.080.09Voltage/V1018 MBN profilefitted curveGaussian 1Gaussian 276.69-2500-2000-1500-1000-500050010001500H/(A/m)00.010.020.030.040.050.060.07Voltage/V1026 MBN profilefitted curveGaussian 1Gaussian 2-10.6 Figure 55: The gaps between two peaks for both simulated and experimental results as a function of carbon contents 5.3 Grain size effect on MBN frequency spectrum 5.3.1 Grain size effect on MBN frequency spectrum Grain size as a significant microstructural property has an important influence on the MBN signals. A Hall-Petch type relationship between the grain-size and the MBN power observed for polycrys- talline iron was found. The relationship can be described by the formula MBN =Cg • d−1/2 [23]. Grain size also has an influence on the frequency spectrum of the MBN signal. The relationship between the length of the wall displacement between pinning obstacles and the local magnetic moment is described as the following formula: g δ (cid:174)m = (cid:174)β((cid:174)S · δ(cid:174)l) (5.3) (cid:174)β is a coefficient related to the type of domain wall and atomic magnetic moment. (cid:174)S is the face of moving Bloch wall. δ(cid:174)l is the length between two pinning obstacles associated with microstructure morphology closely, which can be further expressed as δ(cid:174)l = (cid:174)v· δt. (cid:174)v is the average wall velocity and 43 δt is the time interval between two pinned states. Frequency content can roughly be characterized by f=1/δt [24]. With the decrease of the grain size, there are more pinning sets around grain boundaries, and this fact results in the short displacement length δ(cid:174)l, which further leads to the increase of the frequency content. Fig. 56 shows the fitted frequency spectrum profile of samples with the excitation voltage of 700 mv generated by the signal generator. The lines in the same color stand for the same samples with different heat treatment processes. Steel 1008 groups with large grain sizes from 32 µm to 40 µm have obvious sharp peaks in the low-frequency regions. Whereas, the peak positions of steel A36 and 1018 with fine grains are moving to the high-frequency ranges. From Table 21 and Fig.24, the grain size for each kind of samples with different heat treatment processes is following the same trend where samples after normalizing are larger than samples without heat treatment and smaller than samples after annealing. When we take a look at lines with the same color, the peak positions are increasing with the decrease of the grain size from annealed samples to samples without heat treatment. The relationship between grain size and main frequency content has been plotted in the Fig. 57. Each point in Fig. 57 is obtained by taking the average of results from multiple measurements to get reliable parameters. The relationship between grain size and frequency peak position are perfectly fitted by the power function. Fpp = 1.0022E + 06 ∗ Gs−1.349 (5.4) (Fpp stands for frequency peak position of MBN signal and Gs is grain size of the sample). The sensitivity of the parameter, frequency peak position, increases when the grain size of samples decreases. For those samples with fine grain, small changes in grain size will result in a large shift of the frequency peak, whereas those samples with the coarse grain (larger than 15 µm), the frequency peak position has good linearity with grain size. Fig. 58 shows the linear relationship between frequency peak position and samples with the grain size larger than 15 µm. 44 Figure 56: Fitted MBN frequency profiles of different samples Figure 57: MBN frequency response peak position as a function of grain size 45 012345678910Freq/Hz1044.555.566.577.588.59Intensity10-41008A10081008N1018A10181018NA36AA36A36N Figure 58: MBN frequency response peak position as a function of grain size (grain size larger than 15 µm) Figure 59: MBN frequency response peak position and grain size for each samples (high amplitude excitation signal) 46 5.3.2 Excitation signal effect on MBN frequency spectrum It has been showed that the MBN time-domain profile would show two peaks for steels with two- phase of particles when the applied magnetic field is high enough. The first peak in low magnetic field strength is related to the nucleation and annihilation of domain walls in grain boundaries of ferrite and the second peak at higher amplitude position indicates the displacement of domain walls due to the second phase particles [40]. The intensity of the second peak will increase as the applied magnetic field increases [45]. The excitation signal also influences the frequency spectrum. Previous works show the results with the excitation signal of 700 mV. When increasing the excitation signal from signal generator to 1.2 V, the frequency peak of samples normalized A36, annealed 1018 and normalized 1018 have been shifted to a higher frequency from the original position (Fig.59). Frequency profiles in Fig.510 are from the same sample with different excitation signal amplitudes. They show two peaks for both profiles and the second peak intensity increases a lot with the increase of excitation signal. It is because that when the excitation voltage increases, the MBN signal that comes from the second phase particles, which are harder pearlites for low carbon samples, has been increased. Pearlite is a two-phase, lamellar structure composed of alternating layers of ferrite (88 wt%) and cementite (12 wt%). It usually has more pins and is difficult for magnetization. As a result, the frequency response for pearlite is in high-frequency regions, and this is consistent with previous works [24]. This fact results in the increase of the second peak of the frequency profile for samples with large proportions of second phase particles. It can be further confirmed by the fact that samples normalized A36, annealed 1018 and normalized 1018 all have large proportions of second phase particles. The second peaks of the frequency spectrum are in the region from 40 kHz to 50 kHz, and this overlaps with the frequency region of samples 1018 and A36. This explains why samples 1018 and A36 do not show a small frequency peak shift when excitation signal increases. 47 (a) 1018 annealed (b) 1018 normalied Figure 510: Fitted MBN frequency response peak profile for samples with different excitation signal (c) A36 normalized 48 012345678910Freq/Hz1045.45.65.866.26.46.6Intensity10-41018A 700mv1018A 1.2vFirst peakSecond peak012345678910Freq/Hz1046.66.877.27.47.67.888.2Intensity10-41018N 700mv1018N 1.2vFirst peakSecond peak012345678910Freq/Hz1045.85.966.16.26.36.46.56.66.76.8Intensity10-4A36N 700mvA36N 1.2vSecond peakFirst peak Figure 511: MBN frequency response peak position as a function of grain size (high amplitude excitation signal) 5.3.3 Predict hardness with parameter frequency peak position The grain size has a strong effect on the mechanical behavior of the materials. For mild steel, the grain refinement can enhance the hardness. This grain-size dependence is described by the Hall-Petch relation. H = H0 + K • Gs−1/2 (5.5) Where H0 is the hardness of an indefinitely large, error-prone grain, and K is the Hall-Petch constant, which describes the grain boundary structure. Gs is the average grain size, and H is the hardness of a different kind of steel. The relationship between hardness measured by Vickers hardness tester and grain size has been plotted in Fig. 512. The parameter H0 and K can be predicted from Fig. 512, which are 10.237 and 531.32 respectively for mild steel. With combination equation 5.4 and equation 5.5 mentioned before, it is easy to obtain a relationship between hardness H and parameter frequency peak position Fpp. The relationship can be described by the following equation: 49 Figure 512: Hardness as a function of grain size H = H0 + K • (Fpp/1E + 06)0.371 (5.6) Therefore, with the equation 5.6, the hardness of the mild steel can be predicted, and Fig. 513 shows values for predicted hardness and hardness measured by Vickers hardness tester. The results show good accuracy for prediction and the errors are less than 10%. Figure 513: Predicted hardness and hardness measured by Vickers hardness tester 50 Table 52: Predicted hardness and corresponding error of steel samples Samples Vickers hardness Predicted hardness 1008 A36 1018 1008 A A36 A 1018 A 1008 N A36 N 1018 N 105.99 179.92 181.98 97.08 116.27 117.68 102.72 130.82 121.05 110.21 172.19 185.33 95.06 116.33 118.81 99.71 120.7 133.43 error -3.8% 4.5% -1.8% 2.1% -0.05% -0.9% 3.0% 8.3% -9.3% 5.4 Predict grain size and hardness with MAE signal Fig. 514 shows the result for predited grain size with different datasets. The coefficient of determination (R2) for those three samples are 0.49, 0.91 and 0.94 respectly, which means that the accuracy for prediction increases with the increase of the number of datasets. With the increase of the dataset, the training of the network would be better for finding the relationship between features and the properties of steels. To make sure the data train well and considering the computitional time for training, we are using 900 samples in our dataset. (a) 99 samples (b) 270 samples (c) 900 samples Figure 514: Predicted grain size with different datasets Fig. 515 and Fig. 516 show the results for predicted grain size and hardness with MAE signals. Compared with (a) and (b) in both figures, they show that the accuracy for prediction would increase a lot when the irrelevant features are eliminated. Because those irrelevant features like noise which can disturb the prediction. After feature selection, the total number of features is droped to 229 51 10152025303540Actual grain size/um1020304050Predicted grain size/um (a) Predicted grain size without feature selection (b) Predicted grain size with feature selection Figure 515: Predicted grain size with MAE signal and actual grain size (a) Predicted hardness without feature selection (b) Predicted hardness with feature selection Figure 516: Predicted hardness with MAE signal and hardness measured by Vickers hardness tester from 788, which could slim the network, save the computional cost and accelerate the speed. It is very important when the number of samples increase dramatically. And the final predicted results with coefficient of determination (R2) 0.94 are well trained to predict the properties of sample steels. 5.5 Summary In this chapter, the results for research have been described detailedly. At first, the optimizations of the pick-up coil and magnetic core have been introduced. Secondly, some new parameters of MBN siganl have been extracted and the relationship between those parameters and properties of 52 10152025303540Actual grain size/um1020304050Predicted grain size/um100120140160180Actual hardness80100120140160180200Predicted hardness steel has been investigated. Thirdly, the machine learning method has been introduced for MAE signal feature extraction and steel sample properties’ prediction. 53 CHAPTER 6 CONCLUSION AND FUTURE WORK 6.1 Conclusion In this thesis, Magnetic Barkhausen Noise (MBN) measurements were conducted on various mild steels with different heat-treatments. New parameters were introduced to quantificationally characterize the influence of microstructural and mechanical properties, including carbon content, grain size, and hardness, of sample steels and following conclusions were obtained: 1. Sensor optimization has been introduced in the present study. Three coils with the different number of turns have been compared for sensitivity. The result shows that pick-up coils with a larger number of turns have higher SNR and are sensitive to lower frequency response. 2. For the optimization for the magnetic core, NSGA III has been introduced and applied to design a magnetic core with small size, high magnetic field, and suit for different diameter pipelines. 3. In the experiment, the shape of profiles of MBN signals is changed with carbon content. By extracting parameter with two fitted Gaussian curves, a linear relationship has been revealed between gaps and carbon content of samples. 4. The experimental work shows that the peaks of frequency responses of the MBN signals move to higher frequency with the decrease of grain size, which results from the decrease of the length between two obstacles with the decrease of grain size. The relationship can be perfectly fitted by the function Fpp = 1E + 06 ∗ Gs−1.349. As a result, with the information of MBN frequency spectrum, the grain size of the sample can be inferred. 5. The grain size has a strong effect on the mechanical properties of the steels. The grain size dependence of hardness of steels can be described by Hall-Petch relationship. Therefore, the Fpp can also be an efficient parameter to predict the hardness of the steels. 6. The influence of the excitation signal also has been investigated. With the increase of the excitation signal, the part of MBN signal that comes from the second phase particles has been 54 increased and this results in the increase of the second peak of the MBN frequency spectrum for samples with a large portion of pearlite. The frequency peak position of those samples moves to a higher frequency. As a result, the parameter Fpp is good to predict the grain size of ferrite with a smaller applied magnetic field. 7. By using the package tsfresh, multi-features of MAE signal have been calculated and relevent features have selected to predict the hardness and grain size of the samples. The result shows a good accuracy. 6.2 Future work According to previous works, MBN and MAE is a powerful tool to study and characterize microstructural properties of low carbon steels. As for practical application, estimation of the basic material properties, such as microstructure, composition as well as various surface mechanical properties with the usage of acoustic and electromagnetic sensors can be fused and correlated to a multimodal system to integrate these and obtain a probabilistic strength and toughness with a high degree of accuracy. Therefore, it is important to link the parameters of MBN and MAE signal to more microstructural properties of aging steel and tailor the MBN and MAE system for multi- parameter microstructural properties study through sensor optimization, advanced data processing, and statistical modeling. What is more, existing techniques focus on the single modality deterministic estimation of pipe strength and ignores inhomogeneousity and uncertainties. In view of this, a novel information fusion framework using multimodality diagnosis for pipe materials is proposed for accurate probabilistic strength and toughness estimation under uncertainties. Advanced data analysis using Gaussian Processing model will be performed for surrogate modeling and uncertainty quantification. A generalized Bayesian network methodology is proposed to fuse multiple sources of information from the multimodality diagnosis results. Probabilistic pipe strength and toughness estimation is inferred based on the posterior distribution after information fusion. If successful, this study can help to accurately and effectively assess the reliability of pipeline systems, and eventually help the 55 decision making process to balance the pipeline safety and economical operations. 56 BIBLIOGRAPHY 57 BIBLIOGRAPHY [1] S. Zhang, X. Shi, L. Udpa, and Y. Deng, “Micromagnetic measurement for characterization of ferromagnetic materials’ microstructural properties,” AIP Advances, vol. 8, 5 2018. [2] D. Jiles, Introduction to magnetism and magnetic materials. CRC press, 2015. [3] J. P. Liu, E. Fullerton, O. Gutfleisch, and D. J. Sellmyer, Nanoscale magnetic materials and applications. Springer, 2009. [4] K. Stevens, “Stress dependence of ferromagnetic hysteresis loops for two grades of steel,” NDT & E International, vol. 33, no. 2, pp. 111–121, 2000. [5] M. Vashista and S. Paul, “Correlation between surface integrity of ground medium carbon steel with barkhausen noise parameters and magnetic hysteresis loop characteristics,” Materials & Design, vol. 30, no. 5, pp. 1595–1603, 2009. [6] H. Kwun and G. Burkhardt, “Effects of grain size, hardness, and stress on the magnetic hysteresis loops of ferromagnetic steels,” Journal of applied physics, vol. 61, no. 4, pp. 1576– 1579, 1987. J. Makar and B. Tanner, “The effect of plastic deformation and residual stress on the per- meability and magnetostriction of steels,” Journal of Magnetism and Magnetic Materials, vol. 222, no. 3, pp. 291–304, 2000. [7] [8] M. J. Sablik, T. Yonamine, and F. J. Landgraf, “Modeling plastic deformation effects in steel on hysteresis loops with the same maximum flux density,” IEEE transactions on magnetics, vol. 40, no. 5, pp. 3219–3226, 2004. [9] K. Mumtaz, S. Takahashi, J. Echigoya, Y. Kamada, L. Zhang, H. Kikuchi, K. Ara, and M. Sato, “Magnetic measurements of martensitic transformation in austenitic steel after room temperature rolling,” Journal of Materials Science, vol. 39, no. 1, pp. 85–97, 2004. [10] H. Kikuchi, K. Ara, Y. Kamada, and S. Kobayashi, “Effect of microstructure changes on barkhausen noise properties and hysteresis loop in cold rolled low carbon steel,” IEEE Trans- actions on Magnetics, vol. 45, no. 6, pp. 2744–2747, 2009. [11] N. Karimian, J. Wilson, W. Yin, J. Liu, C. Davis, and A. Peyton, “Magnetic sensing for microstructural assessment of power station steels: Differential permeability and magnetic hysteresis,” vol. 450, no. 1, p. 012042, 2013. [12] F. Landgraf, M. Emura, J. Teixeira, and M. De Campos, “Effect of grain size, deformation, ag- ing and anisotropy on hysteresis loss of electrical steels,” Journal of magnetism and magnetic materials, vol. 215, pp. 97–99, 2000. [13] J. Mohapatra, A. Panda, M. Gunjan, N. Bandyopadhyay, A. Mitra, and R. Ghosh, “Ageing behavior study of 5cr–0.5 mo steel by magnetic barkhausen emissions and magnetic hysteresis loop techniques,” NDT & E International, vol. 40, no. 2, pp. 173–178, 2007. 58 [14] E. Gorkunov, A. Ul’yanov, and V. Khamitov, “Magnetic acoustic emission in ferromagnetic materials. 3: Effect of structural changes on magnetic acoustic emission,” Russian journal of nondestructive testing, vol. 38, no. 5, pp. 376–397, 2002. [15] E. Gorkunov, Y. N. Dragoshanskii, and V. Khamitov, “Magnetoelastic acoustic emission in ferromagnetic materials. ii. effect of elastic and plastic strains on parameters of magnetoelastic acoustic emission,” Russian journal of nondestructive testing, vol. 37, no. 12, pp. 835–858, 2001. [16] E. Gorkunov, Y. N. Dragoshanskii, V. Khamitov, and V. Shevnin, “Magnetoelastic acous- tic emission in ferromagnetic materials. i. effect of crystal anisotropy,” Russian journal of nondestructive testing, vol. 37, no. 3, pp. 163–180, 2001. [17] M. O Sullivan, D Cotterell, S. Cassidy, D. A. Tanner, and I. Mészáros, “Magneto-acoustic emission for the characterisation of ferritic stainless steel microstructural state,” Journal of Magnetism and Magnetic Materials, vol. 271, no. 2-3, pp. 381–389, 2004. [18] J. W. Wilson, G. Y. Tian, V. Moorthy, and B. A. Shaw, “Magneto-acoustic emission and mag- netic barkhausen emission for case depth measurement in en36 gear steel,” IEEE Transactions on Magnetics, vol. 45, no. 1, pp. 177–183, 2009. [19] K. Praveena and S. Murthty, “Magneto acoustical emission in nanocrystalline mn–zn ferrites,” Materials Research Bulletin, vol. 48, no. 11, pp. 4826–4833, 2013. [20] R. Ranjan, D. Jiles, and P. Rastogi, “Magnetic properties of decarburized steels: an investiga- tion of the effects of grain size and carbon content,” IEEE transactions on magnetics, vol. 23, no. 3, pp. 1869–1876, 1987. [21] M. R. N. Astudillo, M. I. L. Pumarega, N. M. Núñez, A. Pochettino, and J. Ruzzante, “Magnetic barkhausen noise and magneto acoustic emission in pressure vessel steel,” Journal of Magnetism and Magnetic Materials, vol. 426, pp. 779–784, 2017. [22] D. Ng, J. Jakubovics, C. Scruby, and G. Briggs, “Effect of stress on magneto-acoustic emission from mild steel and nickel,” Journal of Magnetism and Magnetic Materials, vol. 104, pp. 355– 356, 1992. [23] S. Yamaura, Y. Furuya, and T. Watanabe, “The effect of grain boundary microstructure on barkhausen noise in ferromagnetic materials,” Acta materialia, vol. 49, no. 15, pp. 3019–3027, 2001. [24] O. Saquet, J. Chicois, and A. Vincent, “Barkhausen noise from plain carbon steels: analysis of the influence of microstructure,” Materials Science and Engineering: A, vol. 269, no. 1-2, pp. 73–82, 1999. [25] V. Moorthy, B. Shaw, and J. Evans, “Evaluation of tempering induced changes in the hardness profile of case-carburised en36 steel using magnetic barkhausen noise analysis,” Ndt & E International, vol. 36, no. 1, pp. 43–49, 2003. 59 [26] J. Anglada-Rivera, L. Padovese, and J. Capo-Sanchez, “Magnetic barkhausen noise and hysteresis loop in commercial carbon steel: influence of applied tensile stress and grain size,” Journal of magnetism and magnetic materials, vol. 231, no. 2-3, pp. 299–306, 2001. [27] S. P. Sagar, N. Parida, S. Das, G. Dobmann, and D. Bhattacharya, “Magnetic barkhausen emission to evaluate fatigue damage in a low carbon structural steel,” International journal of fatigue, vol. 27, no. 3, pp. 317–322, 2005. [28] C.-G. Stefanita, D. Atherton, and L. Clapham, “Plastic versus elastic deformation effects on magnetic barkhausen noise in steel,” Acta materialia, vol. 48, no. 13, pp. 3545–3551, 2000. [29] A. Ktena, E. Hristoforou, G. J. Gerhardt, F. P. Missell, F. J. Landgraf, D. L. Rodrigues, and M. Alberteris-Campos, “Barkhausen noise as a microstructure characterization tool,” Physica B: Condensed Matter, vol. 435, pp. 109–112, 2014. [30] H. Sakamoto, M. Okada, and M. Homma, “Theoretical analysis of barkhausen noise in carbon steels,” IEEE transactions on magnetics, vol. 23, no. 5, pp. 2236–2238, 1987. [31] L. Clapham, C. Jagadish, and D. Atherton, “The influence of pearlite on barkhausen noise generation in plain carbon steels,” Acta metallurgica et materialia, vol. 39, no. 7, pp. 1555– 1562, 1991. [32] F. A. Franco, M. González, M. De Campos, and L. Padovese, “Relation between magnetic barkhausen noise and hardness for jominy quench tests in sae 4140 and 6150 steels,” Journal of Nondestructive Evaluation, vol. 32, no. 1, pp. 93–103, 2013. [33] M. Blaow, J. Evans, and B. Shaw, “Effect of hardness and composition gradients on barkhausen emission in case hardened steel,” Journal of magnetism and magnetic materials, vol. 303, no. 1, pp. 153–159, 2006. [34] O. Stupakov, O. Perevertov, I. Tomáš, and B. Skrbek, “Evaluation of surface decarburiza- tion depth by magnetic barkhausen noise technique,” Journal of magnetism and magnetic materials, vol. 323, no. 12, pp. 1692–1697, 2011. [35] D. Stewart, K. Stevens, and A. Kaiser, “Magnetic barkhausen noise analysis of stress in steel,” Current Applied Physics, vol. 4, no. 2, pp. 308–311, 2004. [36] H. I. Yelbay, I. Cam, and C. H. Gür, “Non-destructive determination of residual stress state in steel weldments by magnetic barkhausen noise technique,” NDT & E International, vol. 43, no. 1, pp. 29–33, 2010. [37] A. Dhar, L. Clapham, and D. Atherton, “Influence of uniaxial plastic deformation on magnetic barkhausen noise in steel,” NDT & E International, vol. 34, no. 8, pp. 507–514, 2001. [38] M. Vashista and V. Moorthy, “Influence of applied magnetic field strength and frequency response of pick-up coil on the magnetic barkhausen noise profile,” Journal of magnetism and magnetic materials, vol. 345, pp. 208–214, 2013. 60 [39] J. A. Perez-Benitez, J. Capó-Sánchez, J. Anglada-Rivera, and L. Padovese, “A model for the influence of microstructural defects on magnetic barkhausen noise in plain steels,” Journal of magnetism and magnetic materials, vol. 288, pp. 433–442, 2005. [40] M. Vashista and V. Moorthy, “On the shape of the magnetic barkhausen noise profile for better revelation of the effect of microstructures on the magnetisation process in ferritic steels,” Journal of Magnetism and Magnetic Materials, vol. 393, pp. 584–592, 2015. [41] N. P. Gaunkar, Magnetic hysteresis and Barkhausen noise emission analysis of magnetic materials and composites. PhD thesis, Iowa State University, 2014. [42] K. Deb, A. Pratap, S. Agarwal, and T. Meyarivan, “A fast and elitist multiobjective genetic algorithm: Nsga-ii,” IEEE transactions on evolutionary computation, vol. 6, no. 2, pp. 182– 197, 2002. [43] Y. Benjamini and D. Yekutieli, “The control of the false discovery rate in multiple testing under dependency,” Annals of statistics, pp. 1165–1188, 2001. [44] V. Moorthy, S. Vaidyanathan, T. Jayakumar, and B. Raj, “On the influence of tempered microstructures on magnetic barkhausen emission in ferritic steels,” Philosophical magazine A, vol. 77, no. 6, pp. 1499–1514, 1998. [45] V. Moorthy, “Important factors influencing the magnetic barkhausen noise profile,” IEEE Transactions on Magnetics, vol. 52, no. 4, pp. 1–13, 2016. 61