Characterization of Superplastic Deformation Behavior for a Novel Al-Mg-Fe-Ni-Zr-Sc Alloy: Arrhenius-Based Modeling and Artificial Neural Network Approach

Round 1

Reviewer 1 Report

Interesting work dealing with the development of mathematical model for predicting the superplastic flow behavior of the novel Al-Mg-Fe-Ni-based alloy, demonstrating high strain-rate superplasticity and strain softening during the deformation, using ACE and ANN approaches comparing accuracies. I recommend publication. Nevertheless, first it is necessary:

• Complete the introduction, adding more references.
• To avoid the use of "bold" in equations and parameters.
• It is necessary to fill "author contributions" and "institution review board statement" sections.
• In line 332 ("conclusions") there is a "point" that it is not necessary.

 

Author Response

Dear Reviewer,

Thank you very much for your time and consideration of the manuscript. We thank the reviewer for his/her insightful comments and very helpful recommendations to improve our manuscript. We have taken all your comments into consideration and marked changes to the manuscript with blue-colored text. Our answers are below.

 

1. Complete the introduction, adding more references.

• The introduction was modified by adding more references.
• Zhang, W.; Gao, Y.; Feng, Z.; Wang, X.; Zhang, S.; Huang, L.; Huang, Z.; Jiang, L. Ductility limit diagrams for superplasticity and forging of high temperature polycrystalline materials. Acta Mater. 2020, 194, 378–386.
• Williams, J.C.; Boyer, R.R. Opportunities and issues in the application of titanium alloys for aerospace components. Metals (Basel). 2020, 10.
• Aksenov, S.; Sorgente, D. Determination of biaxial stress–strain curves for superplastic materials by means of bulge forming tests at constant stress. CIRP J. Manuf. Sci. Technol. 2020, 31, 618–627.
• Aksenov, S.; Mikolaenko, V. The effect of material properties on the accuracy of superplastic tensile test. Metals (Basel). 2020, 10, 1–18.
• Jarrar, F.; Sorgente, D.; Aksenov, S.A.; Enikeev, F. On the Challenges and Prospects of the Superplastic Forming Process. Sci. Forum 2019, 941, 2343–2348.
• Fereshteh-Saniee, F.; Fakhar, N.; Mahmudi, R. Influence of Combined Severe Plastic Deformation and Sheet Extrusion Process on the Superplastic Formability of AA 5083 Aluminum Alloy Assessed by Free Bulge Test. Mater. Eng. Perform. 2019, 28, 6682–6691.
• Dunwoody, B.J. The Production of Automotive Body Panels in 5083 SPF Aluminium Alloy. Sci. Forum 2001, 357–359, 59–64.
• Hefti, L.D. Commercial Airplane Applications of Superplastically Formed AA5083 Aluminum Sheet. Mater. Eng. Perform. 2007, 16, 136–141.
• Wang, X.G.; Li, Q.S.; Wu, R.R.; Zhang, X.Y.; Ma, L. A Review on Superplastic Formation Behavior of Al Alloys. Mater. Sci. Eng. 2018, 2018.
• Sorgente, D.; Tricarico, L. Characterization of a superplastic aluminium alloy ALNOVI-U through free inflation tests and inverse analysis. J. Mater. Form. 2014, 7, 179–187.
• Kudo, T.; Goto, A.; Saito, K. High Strain Rate Blow Formability of Newly Developed Al-Mg-High-Mn Alloy. Sci. Forum 2013, 735, 271–277.
• Bate, P. The effect of deformation on grain growth in Zener pinned systems. Acta Mater. 2001, 49, 1453–1461.
• Maeng, D.Y.; Lee, J.H.; Hong, S.I. The effect of transition elements on the superplastic behavior of Al–Mg alloys. Sci. Eng. A 2003, 357, 188–195.
• PENG, Y.; YIN, Z.; NIE, B.; ZHONG, L. Effect of minor Sc and Zr on superplasticity of Al-Mg-Mn alloys. Nonferrous Met. Soc. China 2007, 17, 744–750.
• Chuvil’deev, V.N.; Shadrina, I.S.; Nokhrin, A. V; Kopylov, V.I.; Bobrov, A.A.; Gryaznov, M.Y.; Shotin, S. V; Tabachkova, N.Y.; Chegurov, M.K.; Melekhin, N. V An investigation of thermal stability of structure and mechanical properties of Al-0.5Mg–Sc ultrafine-grained aluminum alloys. Alloys Compd. 2020, 831, 154805.
• Sitdikov, O.; Garipova, R.; Avtokratova, E.; Mukhametdinova, O.; Markushev, M. Effect of temperature of isothermal multidirectional forging on microstructure development in the Al-Mg alloy with nano-size aluminides of Sc and Zr. Alloys Compd. 2018, 746, 520–531.
• Sitdikov, O.S.; Avtokratova, E. V; Mukhametdinova, O.E.; Garipova, R.N.; Markushev, M. V Effect of the Size of Al3(Sc,Zr) Precipitates on the Structure of Multi-Directionally Isothermally Forged Al-Mg-Sc-Zr Alloy. Met. Metallogr. 2017, 118, 1215–1224.
• Michi, R.A.; Toinin, J.P.; Seidman, D.N.; Dunand, D.C. Ambient- and elevated-temperature strengthening by Al3Zr-Nanoprecipitates and Al3Ni-Microfibers in a cast Al-2.9Ni-0.11Zr-0.02Si-0.005Er (at.%) alloy. Sci. Eng. A 2019, 759, 78–89.
• Mochugovskiy, A.G.; Mikhaylovskaya, A. V; Zadorognyy, M.Y.; Golovin, I.S. Effect of heat treatment on the grain size control, superplasticity, internal friction, and mechanical properties of zirconium-bearing aluminum-based alloy. Alloys Compd. 2021, 856, 157455.
• Nokhrin, A.; Shadrina, I.; Chuvil’deev, V.; Kopylov, V. Study of Structure and Mechanical Properties of Fine-Grained Aluminum Alloys Al-0.6wt.%Mg-Zr-Sc with Ratio Zr:Sc = 1.5 Obtained by Cold Drawing. 2019, 12.
• Ma, Z.Y.; Mishra, R.S.; Mahoney, M.W.; Grimes, R. High strain rate superplasticity in friction stir processed Al–Mg–Zr alloy. Sci. Eng. A 2003, 351, 148–153.
• Mochugovskiy, A.G.; Mikhaylovskaya, A. V; Tabachkova, N.Y.; Portnoy, V.K. The mechanism of L12 phase precipitation, microstructure and tensile properties of Al-Mg-Er-Zr alloy. Sci. Eng. A 2019, 744, 195–205.
• Kotov, A.D.; Mikhaylovskaya, A. V; Portnoy, V.K. Effect of the solid-solution composition on the superplasticity characteristics of Al-Zn-Mg-Cu-Ni-Zr Alloys. Met. Metallogr. 2014, 115, 730–735.

2. To avoid the use of "bold" in equations and parameters.

• Were corrected

3. It is necessary to fill "author contributions" and "institution review board statement" sections.

• Were added

4. In line 332 ("conclusions") there is a "point" that it is not necessary.

• Were corrected

Author Response File: Author Response.pdf

Reviewer 2 Report

The manuscript applsci-1123354 entitled Characterization of superplastic deformation behaviour for a novel Al-Mg-Fe-Ni-Zr-Sc based alloy: Arrhenius-based modelling and artificial neural network approach; describes the modelling and structural analysis of superplastic deformation effect of Al-based alloy (Al–4.9Mg–0.9Fe–0.9Ni–0.2Zr–0.1Sc). The presented research is important for many branches i.e. automotive, aerospace in the aspect of forming elements, where high strength, stiffness and lightweight are desirable. Authors based on the structural characterization of the produced alloy try to verify its superplastic behaviour during forming using model approach I. Arrhenius-type constitutive hyperbolic equation (ACE) and II. Artificial neural network (ANN).  By comparing these models Authors will try to optimize the best solution to predict alloy’s superplastic behaviour. Understanding such a process and setting the parameters according to the simulation results will finally give the Authors and in perspective engineers possibilities to produce the ready-made complex elements. An important stage of the article was the structural characterization and tensile tests of the novel Al-Mg-Fe-Ni-Zr-Sc alloy. Analyses of microstructure, grain size, grain boundaries and the precipitation mechanism of phases (Al₉FeNi, L1₂ Al₃Zr) taking place in the alloy during heat treatment at temperature range 420-540 °С were documented using LM, SEM, SEM-EDS, TEM. I appreciate the use of more than one research method however, I suggest that grain size and microstructure observation before and after plastic deformation should be upgraded using i.e. SEM-EBSD mapping. It would be valuable to assess grains orientation, their plastic deformation and observation effects going on through the grain boundaries (Euler’s map of phase precipitation). Using such methods may give a much deeper insight into the mechanisms of superplasticity of investigated Al-based alloys. For superplasticity effect verification Authors also realized tensile tests. The elongation above 500% (ca. 560±30%) was observed at temperatures of 460 °C / strain rate 0.8×10^-2s^-1 and 540 °C / strain rate 2×10^-3s^-1. However, the primary objective of the manuscript was to investigate the model of mentioned Al-based alloy superplastic behaviour based on ACE and ANN simulation. When fitting and approximating the hot deformation behaviour of the investigated alloy, the constructed models demonstrated well performance. Results showed that for higher strain rates the ACE model demonstrated a lower deviation from the experiments than that of the ANN model and has better predictability. The proposed models were verified correctly and might be very useful for the superplastic forming process simulation and the prediction of Al-based alloys forming parameters and are of great importance for the optimization of superplastic forming regimes and processed high-quality complex shape parts from the investigated alloy and other Al-based alloys. The authors cite past literature accordingly. To sum up I can state the aim of the investigation was reached. However, considering the strengths above, though, as I read the manuscript I found some minor errors which I would be appreciated when correcting by the Authors:

1. The Introduction section of the article might be It is only a presentation of the research results. I think the main assumptions of choosing and developing the composition of Al-based alloy should also be highlighted here and finally confirmed by the Authors. I want the Authors to try to answer the question. Why did the Authors finally choose such a composition? (with Zr and Sc). It would be also good to present some more information on the SPF technique in the introduction.

Some sentences are unclear please re-edit the fragments and sentences:

1. Line 28: is – constrictions should be – constructions
   
   
2. Line 33: is–…Al-Mg-based alloys are attractive for transportation in the industry….
   better to say – …Al-Mg-based alloys are attractive for implementation / transferring into the industry…– please re-edit
   
   
3. Line 68: 85% Al, 99.5% Mg – please add space between % and element name
4. Line 72: Ingot size is – 30×120×250 mm3 should be – 30×120×250 mm
5. Line 73: cooling rate unit should be written according to the temperature unit in the whole article is – K/sec should be – °C/s
   the second unit is sec, should be s / also Line 85
6. Please add space between the units: e. Line 75 400±10°C; Line 309 – please check the whole article
7. Line 78: is – scanning electron (SEM) microscopy
   should be –  scanning electron microscopy (SEM)
   
   
8. Line 81: is – in SiC papers
   should be – with (or using) SiC papers
   
   
9. Line 83: optical microscopy – OM, better to say light microscopy – LM
   
   
10. Line 90: Please correct the name of the thinning device / should be TenuPol-5
    
    
11. Line 91: is – (0±2) °C should be – 0±2 °C
    
    
12. Please add the spaces between the Figures abbreviation / should be – Fig. 1. a,b also lines 111, 121, 122, 125, 136, 140, 146 is ok., 182 is ok. 280, 297, 299, 
13. Figure captions: please add the name of the investigated alloy: Figure 1. (Al-Mg-Fe-Ni-Zr-Sc alloy), Figure 2. Please write the name of the alloye. Grain structure of investigated Al-Mg-Fe-Ni-Zr-Sc alloy…..
    The pictures 2c and 2d should be upgraded for better quality, (sharpness, resolution)
    Figure 3. Please include the name of the alloy in the figure caption Al-Mg-Fe-Ni-Zr-Sc alloy
    
    
14. Line 192: Table 2. Please correct the kJ/mol unit
    Is – KJ/mol, should be – kJ/mol

11. Line 204: Please correct the number of equations (Eq. 17, 2018, 21).

12. Line 213: Please correct the activation energy unit; should be 75-90 kJ/mol

13. Line 293: Please correct the unit in Table 5. Superscript in strain rate 1×10^-2s^-1

14. Line 313: It would be better to write results in A., B., C. schedule

15. Line 332: is – …with a. lower error level.
    should be – …with a lower error level.

16. Line 334: Please complete the Author Contributions, Institutional Review Board Statement, Informed Consent Statement, Data Availability Statement.

I have no more comments that I would like to point out. Generally, the article is well-written but requires editorial refinement and proofreading at some points. The manuscript after corrections should be a great interest to readers. The issues presented in the article are essential in the field of superplastic forming technique and suitable for publication in the Journal Applied Sciences (ISSN 2076-3417), but to increase the scientific value, the article requires corrections and should be re-edited by the Authors. I recommend the paper for publication after minor revisions.

Author Response

Dear Reviewer,

 

Thank you very much for your time and consideration of the manuscript. We thank the reviewer for his/her insightful comments and very helpful recommendations to improve our manuscript. We have taken all the comments into consideration and marked changes to the manuscript with blue-colored text. Our responses to the reviewer’s comments are detailed below. Please contact us if any further clarification is required.

Comments:

1.  The Introduction section of the article might be It is only a presentation of the research results. I think the main assumptions of choosing and developing the composition of Al-based alloy should also be highlighted here and finally confirmed by the Authors. I want the Authors to try to answer the question. Why did the Authors finally choose such a composition? (with Zr and Sc). It would be also good to present some more information on the SPF technique in the introduction.

• Answer, Thank you very much for your valuable comment. More information and details were added in the introduction part
•  
• Among the different types of aluminum alloys, Al-Mg-based alloys are attractive for transferring into the industry owing to their lower density, good mechanical properties, and high corrosion resistance [8]. The Al-Mg-based AA5083-type alloys are widely used for SPF [9–14]. The main disadvantage of this alloy is a low forming rate of about 10^-3 s^-1, which limits SPF productivity [9–11,15]. Kishchik et al. [16] improved the Al-Mg- based alloy’s superplasticity by adding Fe, Ni (about of 2 wt% total), and a small amount of Sc and Zr (0.3 wt.% total) to the base alloy. Iron and nickel lead to form the coarse particles of the Al₉FeNi phase [16–23]. Such coarse particles provide the particle stimulated nucleation (PSN) effect during recrystallization [24–28] . The alloying with complex addition of Zr and Sc provides high-dense distributed nanoscale precipitates (dispersoids) of the L1₂-structured Al₃(Sc,Zr) phase that has a strong Zener pinning effect [26,29–34]. Due to lower cost of Zr and improvement of the coarsening resistance of L1₂ precipitates, partial replacement of Sc by Zr is an effective way to provide a fine grain structure at elevated temperature deformation [35–41]. As the result, bimodal particle size distribution with coarse and fine particles help to provide a fine-grained structure with a limited effect of the dynamic grain growth, leading to excellent superplasticity at the strain rates up to 1 × 10⁻¹ s⁻¹ [16,42,43] . It should be noted that a high strain rate superplasticity is provided by a simple thermomechanical treatment including homogenization annealing, hot and cold rolling with low reduction.
•  

Some sentences are unclear please re-edit the fragments and sentences:

1. Line 28: is – constrictions should be – constructions

• Was corrected

1. Line 33: is–…Al-Mg-based alloys are attractive for transportation in the industry better to say Al-Mg-based alloys are attractive for implementation/transferring into the industry please re-edit

• Was re-edited

1. Line 68: 85% Al, 99.5% Mg – please add space between % and element name

• Were added

1. Line 72: Ingot size is – 30×120×250 mm3 should be – 30×120×250 mm

• Was modified

1. Line 73: cooling rate unit should be written according to the temperature unit in the whole article is – K/sec should be – °C/s the second unit is sec, should be s / also Line 85

• Were corrected

1. Please add space between the units: e. Line 75 400±10°C; Line 309 – please check the whole article

• Were checked and modified

1. Line 78: is – scanning electron (SEM) microscopy should be – scanning electron microscopy (SEM)

• Was modified

1. Line 81: is – in SiC papers should be – with (or using) SiC papers

• Was modified

1. Line 83: optical microscopy – OM, better to say light microscopy – LM

• Was modified

1. Line 90: Please correct the name of the thinning device / should be TenuPol-5

• Was corrected

1. Line 91: is – (0±2) °C should be – 0±2 °C

• Was corrected

1. Please add the spaces between the Figures abbreviation / should be – Fig. 1. a,b also lines 111, 121, 122, 125, 136, 140, 146 is ok., 182 is ok. 280, 297, 299, 

• Was added

1. Figure captions: please add the name of the investigated alloy: Figure 1. (Al-Mg-Fe-Ni-Zr-Sc alloy), Figure 2. Please write the name of the alloy. Grain structure of investigated Al-Mg-Fe-Ni-Zr-Sc alloy. The pictures 2c and 2d should be upgraded for better quality, (sharpness, resolution) Figure 3. Please include the name of the alloy in the figure caption Al-Mg-Fe-Ni-Zr-Sc alloy

• Figure and captures were modified

1. Line 192: Table 2. Please correct the kJ/mol unit Is – KJ/mol, should be – kJ/mol

• Were corrected

1. Line 204: Please correct the number of equations (Eq. 17, 2018, 21).

• It is right, Equation 17 is mentioned in L198

1. Line 213: Please correct the activation energy unit; should be 75-90 kJ/mol

• Was corrected

1. Line 293: Please correct the unit in Table 5. Superscript in strain rate 1×10-2s-1

• Was corrected

1. Line 313: It would be better to write results in A., B., C. schedule

• Was re-written

1. Line 332: is – …with a. lower error level. should be – …with a lower error level.

• The point was deleted.

1. Line 334: Please complete the Author Contributions, Institutional Review Board Statement, Informed Consent Statement, Data Availability Statement.

• Were completed.

 

Author Response File: Author Response.pdf