Non-destructive monitoring microstructure and properties changes of 35CrMo steel cylinder using magnetic Barkhausen noise and hysteresis loop techniques

doi:10.21203/rs.3.rs-2102605/v1

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Non-destructive monitoring microstructure and properties changes of 35CrMo steel cylinder using magnetic Barkhausen noise and hysteresis loop techniques

https://doi.org/10.21203/rs.3.rs-2102605/v1

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Background

An important subject during the inspection and quality control of heat-treated steel components is the accurate determination of their microstructure and properties through efficient methods. Traditional laboratory-based techniques, such as optical microscope and mechanical test, are expensive and require a lot of time for samples preparation. Among the various inspection methods for ferromagnetic materials, magnetic non-destructive testing technology is very suitable for on-line detection of product quality, because it is convenient and sensitive to changes in microstructure.

Objective

The main task of this work is to develop a reliable magnetic method of nondestructive testing of the heat treatment quality of steel components from high strength alloy steel. More specifcally, the relationship between magnetic properties and mechanical properties is provided for rapid on-site inspection of product quality.

Methods

Based on hysteresis loop and Barkhausen noise method, the microstructure characterization and residual stress evaluation of 35CrMo steel cylinders under different heat treatment processes are studied. Simultaneously, microstructure observation and hardness measurement are also carried out for the experimental validation. Finally, based on the destructive mechanical test, the linear relationship between the magnetic properties of the cylinder material and its main mechanical properties is fitted.

Results

The quenching and tempering heat treatment processes result in significant variations in the coercive force and the RMS value of the MBN voltage of the 35CrMo steel cylinders, respectively. The surface hardness is in good agreement with coercive force, and the residual stresses levels are evaluated quantitatively via the calibration curve of stress-RMS value. In particular, the coercivity has a good fit with the hardness and strength, the corresponding correlation coefficients are 0.92 and 0.98, respectively.

Conclusion

To avoid destructive testing, magnetic hysteresis loop and Barkhausen noise techniques could be a better tool for the evaluation of quality of heated steel products.

Coercive force

Barkhausen noise

hardness

residual stress

mechanical test

35CrMo steel has good hardenability, strength and toughness. It can serve in the range of -100℃ཞ500℃ for a long term, and the cost is lower than that of Cr-Ni steel, so it is widely used in the construction machinery, automobile and petrochemical industry [1]. Generally, the original 35CrMo steel available in the market has poor mechanical properties and cannot be directly used for applications. Especially for high-load structural components, the 35CrMo steel needs to undergo precise heat treatment to ensure that its mechanical properties meet the requirements. The heating and cooling process determine the microstructure of the steel, such as phase transformations, growth of grain boundary and grain refinement. Microstructural changes have a direct effect on the mechanical properties of the steel. Besides, the common problem is the occurrences of residual stresses, which may weaken the structure and lead to poor mechanical and metallurgical properties, lower corrosion resistance. At this movement, the quality control and evaluation are essential parts in the heat treatment process [2–3]. In the manufacturing industry, traditional techniques are still employed to study the metallurgical changes that take place during the heat treatment process. Apparently, these laboratory-based techniques (e.g., optical microscope) are expensive and require a lot of time for samples preparation, which are not suitable for online inspection in large scale. Although a variety of residual stress measurement methods are currently available, most are destructive and cannot detect all residual stresses in a specimen or component. Therefore, new magnetic non-destructive techniques such as Barkhausen noise (BN) and hysteresis loop (HL) have great advantages for quantitative assessment of microstructure and residual stress changes during heat treatment. Sufficient information on the physical, mechanical properties and stress-strain conditions of different types and sizes of steel structures can be obtained based on these non-destructive control methods.

Barkhausen noise and hysteresis loop measurements are essentially the preferred and advanced techniques for materials characterization at a specific depth [4–5]. BN signal parameters (e.g., root mean square value, amplitude and peak position) and HL properties (e.g., permeability, coercivity and remanence) are sensitive to changes in microstructure, microhardness, grain size and residual stresses. Numerous studies have demonstrated the ability of BN and HL techniques to assess microstructural and properties changes in heat-treated steels. For instance, Henager Jr., et al. [6] assessed microstructure effects on micro-magnetics measurements (Barkhausen noise emission, magnetic hysteresis measurements) for heat-treated HT-9 alloy samples, and discussed the possibility of non-destructive testing of radiation damage and microstructural changes using magnetic signatures. Tam, et al. [7] evaluated the case depth of the induction-hardened camshaft using magnetic Barkhausen noise (MBN) method, and described the experimental results through a physical model. Yelbay, et al. [8] determined the residual stresses in the welded steel plates by MBN method, and the MBN results were verified by the hole-drilling method. Raja, et al. [9] characterized the properties of IS 2062 steel plates after friction stir welding with hysteresis loop characteristics, the magnetic responses of welded samples with base metal were compared at different frequency range. Besides, BN and HL were utilized to qualitative assess the fatigue damage in structural steel [10], the deformation behavior of tensile samples [11], and the stress-strain state of structural components [12]. Even in terms of theoretical modeling, Jiles and Kiarie [13] successfully developed an integrated model of magnetic hysteresis, the Barkhausen effect and the magneto-mechanical effect. The model parameters can be directly linked to the measured magnetic properties of materials.

From the literature review, most of the existing research focus on the magnetic properties of the destructive specimens under applied loading, there are few reports on the estimation of microstructural features and residual stresses of heat-treated steel products with nondestructive techniques. Apparently, the magnetic properties of heat-treated steels are more complex, because they are not only affected by changes in the dislocation density of the material, but also by the grains and their phase composition. Hence, the effect of heat treatment on the microstructural and mechanical properties of 35CrMo steel cylinders was studied with the typical BN and HL parameters, providing technical reference for on-line quality inspection of steel products.

2.1 Materials

The original material is 35CrMo seamless steel pipe (AISI 4135) with the specification of φ219mm×12mm, the main chemical composition is shown in Table 1. Tube specimen were cut from the pipe components with a length of 250mm, and two groups of cylindrical shells with both ends closed were processed by hot spinning. Referring to the heat treatment conditions listed in Fig. 2, one group (2# cylinder) was taken for heat treatment by a continuous heating furnace to promote various microstructural features, the other (1# cylinder) remained its virgin state.

Table 1 Chemical composition of the 35CrMo steel

C	Si	Mn	P	S	Cr	Ni	Mo	Cu	Fe
0.38	0.24	0.56	0.009	0.005	0.98	0.04	0.21	0.04	Bal.

2.2 Magnetic testing and Characterization

After the heat treatments, the magnetic properties of two cylinders were examined respectively and non-destructively. As shown in Fig. 3, four meridional lines marked by numbers 1–4 were drawn parallel to each other on the surface of the cylindrical shells, in which these scan lines were distributed at 0^°, 90^°, 180^° and 270^° on the circumference. Four representative measure points were located in each scanning line, and the distance between two adjacent points is d = 10mm.

The HL analysis were carried out by a commercially available digital ferromagnetic material structure analyzer (KRC-M2) and its software developed in Ukraine. The main magnetic parameter of this instrument is the coercivity, the measurement range is 1∼40A/cm, and the relative error is 2.5∼5%. As displayed in Fig. 4, the size of the magnetic core poles in the magnetic sensor was 18×32 mm, and a distance of 26mm was placed between the two poles. This sensor is a magnetic system with the hall transducer, which is closed with tested sample. The coils at the sensor were used for magnetization of samples and compensation of the field of residual induction. During magnetic preparation, the area of tested samples between the pole pieces are periodically magnetized up to saturation of current pulses with amplitude not less 2.0 A. Then an automatic compensation of the residual magnetization field is performed. The coercivity is automatically calculated from the value of the magnetic field compensation current. During the measurement, the applied field was parallel to the axis direction of the cylinder. Local magnetization of the cylinder wall before and after heat treatment was conducted by scanning its surface along the meridional lines, and the normal components of the stray magnetic field of the local magnetization at the measure points were recorded. The final value of the coercivity H_c was obtained by averaging those three measurements. A quick quantitative assessment of the state and properties of the cylinders can be achieved without surface grinding or using couplant, according to established coercivity measurement procedures [14].

Simultaneously, the stress levels of two cylinders were evaluated with a Barkhausen noise analyser designed and constructed at the laboratory. As revealed in Fig. 5, the MBN analyser is generally composed of excitation circuit, detection probe, signal conditioning and signal processing modules. The external magnetic field is generated by a non-magnetic yoke made of a 300-turn coil wound around a U-shaped core. The induction signal within the pickup coil is obtained in the form of voltage pulse by integration according to the induction law, while the tangential magnetic field strength is measured using a Hall probe placed on the sample surface. The depth and amount of information of MBN analysis depends on the excitation frequency. In this work, MBN measurements were carried out with a low-frequency excitation signal of 50Hz, and the induced signal was amplified and filtered with a band-pass filtering of 1∼400kHz. Throughout the entire measurement procedure, the probe was in full contact with the surface (four meridional lines) of the cylinder. It should be noted that MBN emission data is usually analyzed by the root mean square (RMS) value, which depends significantly on the microstructure and the stress state of the material [15]. That is,

$$RMS=\sqrt{\frac{1}{n}\sum _{i=1}^{n}{x}_{i}^{2}}$$

where x_i is the i-th sampled MBN signal data, n is the total number of acquired points. The resulting BN envelope can be used to calculate various characteristics of the component under observation. When MBN analysis is used to determine stress in ferromagnetic materials, careful calibration of the test system through the uniaxial tension is necessary [16–20]. During the calibration stage, the 35CrMo specimen was only subjected to the elastic deformation at a constant velocity at room temperature, using an MTS® universal testing machine. At a strain rate less than 10^− 1 s^− 1, the specimen was deformed at various predetermined stress levels, and the resulting MBN voltage due to each load condition was recorded. After that, the calibration curve of stress-RMS value can be established, allowing performing stress determination in components of the same material.

Next, all measuring points were ground and polished, and the surface hardness of the cylindrical shell was measured with a MH 660 portable Leeb hardness tester. The test force is 5 N, and the relative error is ± 6 HL. Further, these two cylinders were partially etched with 3% nitric acid alcohol solution to distinguish the grain boundaries. After washing and drying, the microstructure was observed with an JXD-Pro field optical microscope.

2.3 Destructive mechanical testing

In final, an attempt is made to compare the test data of specimens and components, with the aim of examining whether the magnetic properties obtained from structural components are meaningful for evaluating the true mechanical properties of actual steels. As illustrated in Fig. 6, the above two test cylinders (1# and 2#) were cut and manufactured into the smooth cuboid plates for magnetic and hardness measurement at the room temperature (Stage ϕ), then these cuboid plates were processed into standard specimens for mechanical test (Stage κ). In detail, three sets of rings were cut from different locations on each cylinder, and three cuboid plates with dimensions of 120mm×30mm×10mm were made with each ring.

3.1 Microstructure and hardness

The original 35CrMo seamless steel pipe is generally produced by the hot rolling, which will generate a large amount of residual stress during the forming and crystallization process. In order to improve the uniformity of the microstructure and reduce the level of internal residual stress, the steel pipe is often subjected to quenching and tempering heat treatment. Based on the effect of structural continuity on magnetic and mechanical properties, the magnetic coercivity parameter of HL analysis at room temperature can be used for steel grade classification and even evaluation of quenching, tempering and annealing effects [21].

Figure 7 is the contour diagram of the coercive force on the surface (four meridional lines) of two 35CrMo cylinders in different state. Due to the original 35CrMo steel in the hot rolled state without any heat treatment, as shown in Fig. 7a, the original cylinder has a coercivity that ranges from 9.2A/cm to 11.5A/cm. It is obvious that the microstructure of 1# cylinder is not uniform, and there may be stress concentration zones (marked in Fig. 7a) locally. After quenching illustrated in Fig. 7b, the overall coercivity level is greatly improved to 19.6∼20.87A/cm. Although the variation range is narrowed, the distribution of coercivity is also uneven, there are still some areas of high stress in the cylinder (marked in Fig. 7b). This is due to the martensitic transformation by the quenching of 2# cylinder, resulting in a decrease in grain size and an increase in dislocation density. The interlacing of "needle" grain boundaries increases the resistance of the magnetic domain movement, so the coercivity level reaches the highest. After tempering at high temperature in Fig. 7c, the internal stress of 2# cylinder is released fully, so the coercive force level dropped to 12ཞ12.9A/cm, corresponding to a uniform microstructure with grain refinement. It should be emphasized that the coercivity of steels is strongly related to the microstructure. The above results are also validated by metallographic investigation of two cylinders investigated here.

Table 2 Microstructural features

No.	Ferrite content/%	Grain size/mm	State
1# cylinder	96.4~97.4	0.03	Original
2# cylinder	89.5~90.1	0.16	Heated/Cooled

As seen in Table 2, the coarse-grained ferrite and pearlite microstructure are observed clearly in the original cylinder (Fig. 8a). In the microstructure of 2# cylinder at quenched and tempered state, microstructural changes are clearly observed in comparison with as-received one. Due to the precipitation of supersaturated carbides, the tempered sorbite phase in Fig. 8b is a mixture of ferrite and cementite essentially. However, due to large number of grain boundaries and dispersion of carbides, the movement of magnetic domain wall is still restricted, higher magnetic fields are required to overcome strong pinning sites and move domain walls [22-23], the coercivity level of 2# cylinder is still higher compared to that of the original cylinder. Moreover, the coercivity values determined using digital measurements were compared with the results obtained by the traditional HL method [24,34], a very good correlation was found between the two techniques (Fig. 9).

After achieving the mean values from the hardness and magnetic coercivity measurements, Fig. 10 shows the coercivity and hardness distributions of 35CrMo cylinder in different states. As the most structure-sensitive magnetic parameter, coercivity is determined by the grain, inclusions, dislocation, inhomogeneities and defects of the crystal lattice [25]. For the as-quenched state, the hardness of the cylinder is characterized by the martensite hardness in the 35CrMo steel. Furthermore, the grain refinement, the phase hardening, the formation of supersaturated non-solid solutions and high dislocation density result in the difficulty of magnetic domain wall motion, the coercivity achieves its maximum. In some extent, the high coercivity of martensite has contributed by the higher magnetic anisotropy, due to the magnetic lattice structure and magnetoelastic effects [26]. Once tempered at high temperature, the hardness of the cylinder drops significantly, because the decay process of the martensite and residual austenite becomes more rapid. As the carbide particles merges, the pinning of large-angle boundaries is weakened. Moreover, the redistribution of dislocations, the smaller distortions of the lattice and the lower levels of internal stress lead to lower coercivity values [27]. Likewise, the formation of alloyed carbides can lead to secondary hardening phenomena, resulting in hardness peak compared to the original material.

The relationship between the hardness and coercivity of 35CrMo cylinders at each stage of its heat treatment is quantitatively characterized in Fig. 11. Compared to the original, the hardness and coercivity in quenching process increased by 90.7% and 90.4%, respectively. Although decreasing dramatically after tempering, the final increases in hardness and coercivity are 17.98% and 19.9%. Evidently, the level of coercive force is directly proportional to the hardness, which is agreed with previous researches [28–29]. Even, a reliable correlation between the hardness and the coercivity measurement can be established for nondestructive testing of mechanical properties.

3.2 Residual Stress

The potential energy barrier caused by residual stress or stress concentration can hinder the movement of magnetic domains, thereby causing significant changes in the magnetic BN signals [30]. One of the most important information from the envelope of the BN signal is the root mean square (RMS) value, which is strongly related to domain wall motion. By measuring the RMS values of the sample material with a known applied stress, a calibration curve can be obtained to evaluate the residual stresses of the components [31]. Fig. 12 shows the elastic stress dependency of the RMS values, and an increasing trend is observed. Therefore, the MBN values could be converted to the residual stress values indirectly via the calibration curve. Consequently, the magnitudes of the residual stresses of two cylinders during heat treatment were evaluated quantitatively on the BN measurement. Fig. 13 shows the residual stresses of the original, quenched and tempered states of the 35CrMo cylinders. Although the BN signals at different points fluctuate greatly, the variation trend of residual stresses is generally clear. In the hot rolling process of 35CrMo steel pipe, uneven forming or cooling generates large internal stress. If it is not normalized or annealed, the grains are usually coarse, and the homogeneity of the structure is poor, the initial residual stress level of the original cylinder is about 101.5 MPa. While quenching in water produces the martensitic transformation and hardening of the steels, resulting in a signiﬁcant increase in the overall stress level (~171.68 MPa). The rapid cooling effect leads to finer grains, dislocation immobilization and local increased strain. Finally, tempering at high temperature releases the internal stress mostly, the magnitude of residual stresses decreases to the lowest level of 41.46 MPa. As expected, the almost uniform residual stress in the tempered cylinder obtained by the MBN analysis is consistent with the coercivity measurement in Fig. 6c. It is known that the microstructure and properties of the 35CrMo steel (AISI 4135) are similar to those of the AISI 4340 steel. Earlier studies [32] showed that residual stress values of AISI 4340 steel samples obtained by XRD measurements decrease with increasing tempering temperature. From Fig. 14, when the tempering temperature exceeded 450°C, the stress relief was significant and the stresses nature was reversed, resulting in compressive residual stress in both directions. Apparently, MBN and XRD methods gave the same tendency, the residual stresses behaviour of the 35CrMo steel cylinders is in good agreement with that of the AISI 4340 steel samples, except for some variation in stress magnitudes. This difference is mostly due to the different information depth of these two techniques, some additional factors such as microstructure changes, also affect the domain wall movements during MBN measurements [33-34]. Thus, the nondestructive MBN method has a fairly high sensitivity to estimate residual stresses in heat-treated steel cylinders. Further in production lines, the simultaneous use of coercive force and MBN method can adequately monitor the microstructure and properties changes of steel components after hardening heat treatment, avoiding significant costs for destructive testing and ensuring that all components can be checked quickly.

As shown in Fig. 6, a total of 18 test plates were manufactured into 18 sets of round bar tensile specimens. The round rod specimens of φ8mm×120mm were used for tensile testing. All the test results are shown in Table 3.

Table 3

Magnetic and mechanical properties of 35CrMo specimens
Specimen	Magnetic	Mechanical
Specimen	Coercive force H_c/A·cm^− 1	Hardness /HL	Tensile strength σσ_s /MPa	Yield strength σ_y /MPa	Elongation A/%
s-b-1	9.15	395	715	400	24
s-b-2	9.525	401	730	368	26
s-b-3	9.425	412	705	410	22
s-b_mean	9.367	402.7	716.7	392.7	24
s-a-1	11.535	503	984	932	17.5
s-a-2	11.525	505	1023	905	16
s-a-3	11.5	499	980	890	15.5
s-a_mean	11.52	502.3	995.7	909	16.33
Variation	+ 22.98%	+ 24.73%	+ 38.93%	131.47%	-31.96%
Note: s-b represents the original state, s-a represents the heat treated state.

Studies have shown that oxides or rust on the surface of the material can form air gaps, which can increase magnetoresistance in the magnetic measurement [35]. In this work, although the magnitudes of values for coercivity and hardness of the polished steel plates are slightly decreased as compared with those of the cylinders for on-line test, the relative errors are all below 10%. Table 3 gives the results of relative deviation of the magnetic and mechanical properties of 35CrMo specimens cut from two test cylinders. The average hardness in the original condition of the steel plates is 402.7 HL, a target hardness of 502.3 HL is obtained after heat treatment. The average increment in hardness for the plates is 24.73%, the corresponding average increment in coercivity is 22.98%. This observation is in agreement with that of the test cylinders (17.98% and 19.9%) basically. We use the data in cylinders and plates to find a relation between the hardness and coercivity for the 35CrMo steel. As presented in Fig. 15a, this relation can be approximated by linear equations of the form

$$HL=39.42{H}_{\text{c}}+35.72, {R}^{2}=0.92$$

Where HL represents the Leeb hardness, H_c represents the coercivity, R² is the coefficient of correlation. The high reliability (R² ≈ 0.92) of this correspondence is a prerequisite for estimating the hardness of 35CrMo steel products using only the measured coercivity. For the ultimate tensile strength σ_s and the yield strength σ_y of steels in Fig. 15b and Fig. 15c, the similar results are described by the following expressions

$$\left\{\begin{array}{c}{\sigma }_{s}=128.46{H}_{\text{c}}-485.37, {R}^{2}=0.98\\ {\sigma }_{y}=236.65{H}_{\text{c}}-1820.6, {R}^{2}=0.98\end{array}\right.$$

However, for the steel plasticity illustrated in Fig. 15d, it is seen that the higher coercivity results in the great reduction in elongation. This correspondence is given below

$$A=-3.49{H}_{\text{c}}+50.6, {R}^{2}=0.84$$

The reason behind the decreasing trend could be the increasing resistance to deformation associated with the grain boundaries [36]. Hence, the magnetic coercivity can serve as a qualitative indicator for the mechanical characteristics of the 35CrMo steel components after heat treatment.

In this paper, quantitative prediction of the microstructure and properties changes of different heat-treated 35CrMo steel products was presented by hysteresis loop and Barkhausen noise technology. The microstructure of the original 35CrMo cylinder is coarse, the corresponding coercive force is 9.2∼11.5 A/cm, and there is a significant local stress concentration in the cylinder according to the measured MBN signals. The grains of the quenched 35CrMo cylinder are refined, the residual stress determined by MBN reaches the highest level, and the coercive force increases by 90.4%. The final tempering process at high temperature results in the homogenization of the microstructures and the release of residual stresses. Although the coercivity is also greatly reduced, the final increment is about 19.9%. Combined with the verification of destructive tests, the magnetic properties of the 35CrMo cylinders are in good agreement with the hardness, and the analytical representations of the relation between coercivity and main mechanical parameters are obtained. It is shown that the mechanical properties of the steels can be determined from the coercive force, which is measured using a nondestructive method.

Ethics approval and consent to participate

Not applicable.

Availability of data and material

All data sets will be provided on request, but only in the existing format.

Funding

The authors would like to thank Zhejiang Basic Public Welfare Research Project (LGF21E040003) for their financial supporting this present work.

Authors' contributions

Jun-hui Chai: Writing- Reviewing and Editing. Zhong-jie Lv: Conceptualization, Investigation. Bo Xu: Data Curation. Zi-jiang Zhang: Resources, Validation. Zheng-xiang Shen: Methodology, Writing- Original draft preparation. Jian-min Shen: Data Curation, Formal analysis.

Xiao-long Zhang: Investigation, Data Curation.

Acknowledgements

MBN testing equipment is provided by China Special Equipment Testing Research Institute, and we would like to express our special thanks to the team of electromagnetic acoustic nondestructive testing.

Conflict of interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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No competing interests reported.

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Non-destructive monitoring microstructure and properties changes of 35CrMo steel cylinder using magnetic Barkhausen noise and hysteresis loop techniques

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Abstract

Background

Objective

Methods

Results

Conclusion

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1. Introduction

2. Experimental Procedure

2.1 Materials

2.2 Magnetic testing and Characterization

2.3 Destructive mechanical testing

3. Results And Discussion

3.1 Microstructure and hardness

3.2 Residual Stress

4. Mechanical Test And Validation

5. Conclusions

Declarations

References

Additional Declarations

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