Next Article in Journal
TERESA Target Area at ELI Beamlines
Next Article in Special Issue
In Situ Observation for Deformation-Induced Martensite Transformation during Tensile Deformation of SUS 304 Stainless Steel by Using Neutron Diffraction PART II: Transformation and Texture Formation Mechanisms
Previous Article in Journal / Special Issue
Measurement of the X-ray Elastic Constants of Amorphous Polycarbonate
 
 
Article
Peer-Review Record

Characterization of Dislocation Rearrangement in FCC Metals during Work Hardening Using X-ray Diffraction Line-Profile Analysis

by Koutarou Nakagawa 1, Momoki Hayashi 1, Kozue Takano-Satoh 2, Hirotaka Matsunaga 2, Hiroyuki Mori 2, Kazunari Maki 2, Yusuke Onuki 3, Shigeru Suzuki 4 and Shigeo Sato 1,*
Reviewer 1:
Reviewer 2: Anonymous
Reviewer 3:
Submission received: 14 September 2020 / Revised: 9 October 2020 / Accepted: 9 October 2020 / Published: 11 October 2020
(This article belongs to the Special Issue Analysis of Strain, Stress and Texture with Quantum Beams)

Round 1

Reviewer 1 Report

This work on deriving characteristics of dislocations in metals (of specific symmetry) via X-ray diffraction line profile analysis is thoroughly done albeit mostly empirical. The conclusions are plausible and I believe useful to enhance confidence in using X-ray line profile analysis in this context. I enjoyed reading this manuscript.

Author Response

Please see the attached file.

Author Response File: Author Response.pdf

Reviewer 2 Report

The manuscript "Characterization of dislocation rearrangement in FCC metals during work hardening using X-ray diffraction line-profile analysis" by Nakagawa and coworkers discusses how the dislocations modify and rearrange in crystals of metals (alloys) when they undergo tensile stress. The basic analysis was carried out using X-Ray diffraction and the dislocation density and the dislocation arrangement were obtained from the measured pattern using the CMWP fitting method, besides the descriptor M, that quantify the interaction between the dislocations. Very interestingly, these quantities have proved to play a role in the conversion between an elastic and a plastic phase. The article is well written and organized, and I recomment publication, after minor issues are fixed:

1) Please give a reference for the Hall-Perch strengthening

2) A couple of typos

exoression

becomes is stronger

3) "a simple and well-known relationship with the dislocation density and the mean travel distance of dislocations, x̅ , which is expressed as:...". Altough the relation is well-known, please reference it. 

4) Generally speaking, when reviewing one has often to "fight" against, but in this case the number of references is (rather) small.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Reviewer 3 Report

“Characterization of dislocation rearrangement in FCC metals during work hardening using X-ray diffraction line-profile analysis” by Koutarou Nakagawa et al. is an interesting manuscript, which describes the dislocation density and their rearrangement in FCC metals during tensile deformation by XRD line-profile analysis.The line-profile analysis of experimental patterns is performed by using the convolutional multiple whole profile (CMWP) method. Within the CMWP method, the dislocation density and the dislocation arrangement parameter M values were evaluated by fitting theoretical Voight profiles to the experimental peaks of the XRD pattern. Furthermore, the effects of grain size, stacking fault energy (SFE) and solute elements on the extent of dislocation rearrangement were evaluated by determining M values during tensile deformation. It was found that M values decreased as the dislocation density increased. By contrast, grain size and SFE did not exhibit a significant influence on the obtained M values. The influence of solute species and concentration of solute elements on M changes were also determined.

 

Even though the manuscript is well motivated and interesting, the manuscript contains some flaws, which prohibit the publication in the present state. The main concern I have, is related to the instrumental correction of XRD line profiles, which was not properly performed by using the XRD pattern of a typical standard material. The use of the Cu “standard” for performing the instrumental correction is wrong and makes doubtful all microstructural parameters determined in the following. However, the microstructure analysis performed in this manuscript may be accepted only after clarify this aspect. Accordingly, I suggest that the manuscript could become suitable for publication in Quantum Beam Science after major revisions.

 

Below are listed point-by-point comments that should help authors to further improve their manuscript.

 

Sect. 2 Materials and Methods, line 75-76:

“An instrumental broadening correction was made using the diffraction pattern of fully recrystallized copper.”

Authors are asked to explain the reason for performing the instrumental broadening correction by using the XRD pattern of the fully recrystallized Cu instead of that of an appropriate certified standard diffraction material with similar mass absorption coefficient (just for example: NIST 640c Si, NIST 660a LaB6, NIST 674b CeO2 or NIST 675 Mica). The use of this Cu “standard” with unknown XRD peak profiles is wrong and results not only in questionable values of the corrected physical broadening of all peak profiles in the experimental pattern(s), but more important in doubtful values of all microstructural parameters derived in the following by using them. However, by using another standard for the instrumental correction as usual, authors have to show its XRD pattern and to discuss it in respect with the XRD pattern of one of the typical standard materials.

 

Sect. 2 Materials and Methods, line 85:

In Figure 1, authors show the indexed experimental and simulated XRD patterns of the Cu-30%Zn sample. However, I would like to ask you authors to add the difference plot, i.e. (Iexp – Isim) as function of K, to this figure. This plot directly shows, how well the simulated XRD pattern fits the experimental one and, eventually, regions where the fit is not so precise. Related to that, authors have to characterize in the manuscript the overall quality of the XRD line profile fit with analytical Voigt functions within the CMWP method by using the goodness of fit, for example.

 

Sect. 2 Materials and Methods, line 85:

In Figure 1, authors show the indexed experimental and simulated XRD patterns of the Cu-30%Zn sample. However, the diffraction peak located just after the (311) one is not indexed and not analyzed. Authors are asked to comment on that.

The experimental XRD pattern of the fcc Cu-30%Zn sample shown in Figure 1 indicates the (110)-preferred orientation of the sample. This suggests that crystallite are quite inhomogeneous in shape. In this context, authors are asked to comment the meaning of the crystallite size of 70.3 nm.

 

Sect. 3.1 Variations in M values during tensile deformation in nickel and AISI 310S stainless steel, line 111:

“Figure 5a shows the variations of FWHM and ?L/WG ratio as a function of true strain.”

Authors are asked to indicate, to which reflection belongs the FWHM and the WL/WG shown in Figure 5. It may be of interest to show some of the experimental XRD patterns of the two materials and to discuss their fit with theoretical Voight functions.

Authors are asked to comment the reason of the WL/WG increase with the increasing of the true strain. In fact, a decrease of the WL/WG ratio with increasing the true strain would be expected, at least due to the increase of the WG value.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Round 2

Reviewer 3 Report

Within the revised version of the manuscript “Characterization of dislocation rearrangement in FCC metals during work hardening using X-ray diffraction line-profile analysis”, authors added suitable explanations, which answer the questions from my previous report and result in an improvement of data interpretation. All these make the manuscript, in my opinion, suitable for publication in Quantum Beam Science.

 

With my best regards,

 

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Back to TopTop