Investigation of Primary Recrystallization and Decarbonization with Different Heating Rates of Intermediate Annealing Using Nb-Containing Grain-Oriented Silicon Steel
Round 1
Reviewer 1 Report
The paper was nicely constructed and read well. The graphics and tables were clear and well done in terms of getting at the data and understanding the trends. (With that said the scale markers on many of the figures were submerged in the figure making them hard to read. Also, rule in Figure 9a was shadowed significantly.) The last paragraph in the Introduction was a bit long, making getting at the objective of the research a bit difficult. I had to revisit to make sure I was following the conclusions correctly. These are minor to non-consequential issues but thought I would mention given the high quality of the rest of the manuscript.
Author Response
The paper was nicely constructed and read well. The graphics and tables were clear and well done in terms of getting at the data and understanding the trends. (With that said the scale markers on many of the figures were submerged in the figure making them hard to read. Also, rule in Figure 9a was shadowed significantly.) The last paragraph in the Introduction was a bit long, making getting at the objective of the research a bit difficult. I had to revisit to make sure I was following the conclusions correctly. These are minor to non-consequential issues but thought I would mention given the high quality of the rest of the manuscript.
Response: The last paragraph of the introduction has been revised to make the objectives of the study clearer. We have optimized the images, especially the scale markers.
Reviewer 2 Report
- Clearly state the novelty aspects of the paper;
- Materials and methods. What was the heating and cooling rate of samples annealed at 1200°C?
- More details referring EBSD are necessary. What about post-processing of EBSD data? What kind of clean-up procedures were applied? What size of area for each sample was investigated? Step size? Which values of grain tolerance angle and minimum grain size were applied?
- The role of high energy grain boundaries (HEGB) and explanation of separating them from high angle grain boundaries should be presented in point 3.1. Currently, this description is included in the chapter 2.3. It should be moved to 3.1.
- In Fig. 1 HAGBs cover whole areas (blue colors). Does not it result from the lack of indexation in the EBSD method caused by severe plastic deformation in these areas? This should be added to the description. This result is very doubtful.
- There is no information on the methodology of determining the average grain size. It has to be added to the methods.
- On which section of the sample the grain size and grain aspect ratio were determined?
- Where are the results that confirm the statement “The micro- structure of first cold-rolled plate along the thickness direction is known to be the banded structure, so the grain aspect ratio is much less than 1”?
- From which area (dimensions) the texture content presented in Table 3 was determined?
- Add the results of the phase identification of the particles investigated by TEM. Moreover, the role of these particles in the structural changes is not well documented and described. It should be completed.
- There is no information on the methodology of determining the average particle size regarding the results presented in Fig. 8f. It has to be added to the methods. Moreover it should be average particle size instead of average grain size.
- There are some flaws, for instance: “recrystallzation” (also in the title), “permeameter”, “intermediateannealing”,
- In conclusions please underline the new findings of the paper compared to the state of the art. For instance it is well known that “As the heating rate increases, the average grain size decreases gradually, and the aspect ratio of the grains tends to be smaller.”
Author Response
- Clearly state the novelty aspects of the paper;
Response: The last paragraph of the introduction has been revised to clarify the novelty aspects.
- Materials and methods. What was the heating and cooling rate of samples annealed at 1200°C?
Response: The information of the heating and cooling rate has been added in the materials and methods section.
- More details referring EBSD are necessary. What about post-processing of EBSD data? What kind of clean-up procedures were applied? What size of area for each sample was investigated? Step size? Which values of grain tolerance angle and minimum grain size were applied?
Response: The clean-up procedures is: the clearnup type is grain dilation, the grain tolerance angle is 2, minimum grain size is 3. The EBSD analysis of each sample is all calculated based on the data of more than 400 grains. And the information of step size has been added in the materials and methods section.
- The role of high energy grain boundaries (HEGB) and explanation of separating them from high angle grain boundaries should be presented in point 3.1. Currently, this description is included in the chapter 2.3. It should be moved to 3.1.
Response: It has been revised in the manuscript as suggested.
- In Fig. 1 HAGBs cover whole areas (blue colors). Does not it result from the lack of indexation in the EBSD method caused by severe plastic deformation in these areas? This should be added to the description. This result is very doubtful.
Response: Because of the internal stress of cold-rolled microstructure, the confidence index of EBSD collected in the area with large internal stress is low and the boundaries of these points with lower confidence indices are marked as HEGB and HAGB as shown in the lower right corner of Figure 1(c), which is inaccurate. It has been revised in the manuscript.
- There is no information on the methodology of determining the average grain size. It has to be added to the methods.
Response: As suggested, the information on methodology of determining the average grain size has been added in the materials and methods section.
- On which section of the sample the grain size and grain aspect ratio were determined?
Response: The thickness direction of the rolling, e.g. Fig. 1.
- Where are the results that confirm the statement “The micro- structure of first cold-rolled plate along the thickness direction is known to be the banded structure, so the grain aspect ratio is much less than 1”?
Response: “The grain aspect ratio is much less than 1” was shown in Figure 1. Additional notes have been added to the manuscript.
- From which area (dimensions) the texture content presented in Table 3 was determined?
Response: The textural content listed in Table 3 was determined by EBSD from a count of approximately 400 grains.
- Add the results of the phase identification of the particles investigated by TEM. Moreover, the role of these particles in the structural changes is not well documented and described. It should be completed.
Response: The EDSs of inhibitors Nb(C,N), AlN and MnS have added in Figure 8. The role of these particles in the structural changes is described in 3.2.4 section.
- There is no information on the methodology of determining the average particle size regarding the results presented in Fig. 8f. It has to be added to the methods. Moreover it should be average particle size instead of average grain size.
Response: As suggested, the information on the average particle size has been added in the materials and methods section. The words “grain size” has been changed to “particle size” in Figure 8.
- There are some flaws, for instance: “recrystallzation” (also in the title), “permeameter”, “intermediateannealing”,
Response: We have checked and revised the manuscript as suggested.
- In conclusions please underline the new findings of the paper compared to the state of the art. For instance it is well known that “As the heating rate increases, the average grain size decreases gradually, and the aspect ratio of the grains tends to be smaller.”
Response: The conclusions have been revised as suggested.
Reviewer 3 Report
This excellent paper describes how a Nb-containing grain-oriented silicon steel was produced by double-stage cold rolling to investigate the effect of heating rate during intermediate annealing on primary recrystallization and decarburization behaviour. The results indicate that a higher heating rate during intermediate annealing contributes to excellent microstructure and magnetic properties. The literature in this field is thoroughly surveyed in the Introduction. The scientific work reported in this paper would appear to have been competently executed. The equations are clear and accurate. How are the percent texture types in Table 3 determined? Is there any problem with hydrogen embrittlement during intermediate annealing? What does W/kg signify? Define what Sigma3, 5, 9 and 11 boundaries mean. What is the ideal microstructure for a silicon steel and how close does the present work come to this? The authors could add an extra conclusion which states exactly how their results will lead to a better product. The English is very poor and in need of thorough proof reading. I have provided corrections to some of the worst examples below:-
A Nomenclature at the beginning of the paper would be helpful.
Page 1, Abstract, Line 14: …optical… -> …an optical…
Page 1, Abstract, Line 14: Transmission… -> A transmission…
Page 1, Abstract, Line 15: Decarburization… -> The decarburization…
Page 1, Abstract, Line 20: …and distribute… -> …are distributed…
Page 1, Abstract, Line 22: …helps obtain the… -> …contributes to an…
Page 1, Line 26: …recrystallzation; -> …recrystallization;
Page 2, Line 45: …similar feathers… -> …similar features
Page 2, Line 78: Give unit for carbon content.
Page 2, Lines 90/91: …primary recrystallzation, -> …primary recrystallization,
Page 3, Line 116: The microstrcutures… -> The microstructures…
Page 3, Line 121: …CuKa… -> …CuK-alpha…
Page 4, Line 166: Figure 1. microstructure… -> Figure 1. Microstructure
Page 9, Line 329 : …f value corresponded… -> …the f value corresponding…
Page 9, Line 338: …where is K0… -> where K0 is…
Page 9, Line 362: …which meet the… -> …which meets the…
Page 12, Line 414: …being reserved at… -> …being preserved at…
Page 12, Line 464: …the highest, -> …is the highest,
Author Response
This excellent paper describes how a Nb-containing grain-oriented silicon steel was produced by double-stage cold rolling to investigate the effect of heating rate during intermediate annealing on primary recrystallization and decarburization behaviour. The results indicate that a higher heating rate during intermediate annealing contributes to excellent microstructure and magnetic properties. The literature in this field is thoroughly surveyed in the Introduction. The scientific work reported in this paper would appear to have been competently executed. The equations are clear and accurate. How are the percent texture types in Table 3 determined? Is there any problem with hydrogen embrittlement during intermediate annealing? What does W/kg signify? Define what Sigma3, 5, 9 and 11 boundaries mean. What is the ideal microstructure for a silicon steel and how close does the present work come to this? The authors could add an extra conclusion which states exactly how their results will lead to a better product. The English is very poor and in need of thorough proof reading.
- How are the percent texture types in Table 3 determined?
Response: The texture analysis of each sample was all calculated from EBSD.
- Is there any problem with hydrogen embrittlement during intermediate annealing?
Response: The grain-oriented silicon steel mainly takes advantage of its magnetic properties and pays less attention to its mechanical properties such as hydrogen embrittlement.
- What does W/kg signify?
Response: Iron loss refers to the sum of hysteresis loss and eddy current loss per unit mass of ferromagnetic material in alternating and pulsating magnetic fields, and the unit is W/kg.
- Define what Sigma3, 5, 9 and 11 boundaries mean.
Response: The define of Sigma3, 5, 9 and 11 boundaries.
Imagine that two adjacent crystals with the same structure but different orientations will expand in phase according to their lattice periods, or that one part of the same crystal will rotate an angle relative to the other part with a certain crystallographic direction as the axis. At this time, the two crystals will penetrate each other. In the penetration region, the atoms of the two lattices will periodically appear in the position phase focus according to a certain law to form a new periodic lattice, It is called a multiple bit lattice. The proportion of heavy site bursts is called coincidence position density, which is defined as 1/Σ. Σ can also be understood as the ratio of CSL cell volume to origin array cell volume.
- What is the ideal microstructure for a silicon steel and how close does the present work come to this?
Response: The ideal microstructure of silicon steel is a single Goss oriented microstructure. In the present work, most of the grains in the steel are Goss oriented grains.
- The English is very poor and in need of thorough proof reading.
Response: According to the suggestions, the wording and grammatical errors were revised.
Round 2
Reviewer 2 Report
- Correction is required: “with the heating rate of 50/h” on with the heating rate of 50°C/h
- The following response should be added to the materials and methods section ”The clean-up procedures is: the clearnup type is grain dilation, the grain tolerance angle is 2, minimum grain size is 3. The EBSD analysis of each sample is all calculated based on the data of more than 400 grains. And the information of step size has been added in the materials and methods section.”
- EDS measurements are not used for phase identification by TEM. Electron diffraction patterns are required to confirm the presence of the following particles: Nb(C,N), AlN and MnS. These results should be added to the paper.
Author Response
- Correction is required: “with the heating rate of 50/h” on with the heating rate of 50°C/h
Response: Revised as required.
- The following response should be added to the materials and methods section ”The clean-up procedures is: the clearnup type is grain dilation, the grain tolerance angle is 2, minimum grain size is 3. The EBSD analysis of each sample is all calculated based on the data of more than 400 grains. And the information of step size has been added in the materials and methods section.”
Response: Revised as required.
- EDS measurements are not used for phase identification by TEM. Electron diffraction patterns are required to confirm the presence of the following particles: Nb(C,N), AlN and MnS. These results should be added to the paper.
Response: Revised as required.
Round 3
Reviewer 2 Report
The sentence "And the in- formation of step size has been added in the materials and methods section." should be removed from the paper.
I accept the manuscript after this correction.
Author Response
- The sentence "And the in- formation of step size has been added in the materials and methods section." should be removed from the paper.
Response: Revised as required.
