Journal of Materials Engineering and Performance

Use of Hardness and Electrical Conductivity Testing to

Evaluate Heat Damage and Sensitization in 5083-H116 Al-
Mg Alloys

Journal: Journal of Materials Engineering and Performance

Manuscript ID JMEP-20-06-20877.R1

Manuscript Type: Technical Paper

Date Submitted by the

n/a
Author:

Complete List of Authors: Tzeng, Yu-Chih ; Department of Power Vehicle and Systems Engineering,
Chung-Cheng Institute of Technology, National Defense University
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Lu, Cheng-Yu ; Department of Naval Architecture and Ocean
Engineering, Nation Kaohsiung University of Science and Technology
Kaliyaperumal, Kaliyaraj; Senior Structural Naval Architect, Naval and
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Commercial Ship Design
Chen, Renyu; Department of Marine Mechanical Engineering, R.O.C.
Naval Academy
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Keywords: Aluminum, Corrosion, Nondestructive Testing, Heat Treatment

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Page 1 of 28 Journal of Materials Engineering and Performance

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Dear Editor and Reviewers,
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7 Thank you for your letter and for the reviewer’s helpful comments concerning our
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9 manuscript entitled “Use of Hardness and Electrical Conductivity Testing to Evaluate
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11 Heat Damage and Sensitization in 5083-H116 Al-Mg Alloys” (ID: JMEP-20-06-20877).
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14 Those comments have proved invaluable for revising and improving our paper, as well
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16 as giving us some suggestions for further research. We have studied the comments
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18 carefully and have made correction which we hope will meet with your approval. The
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20 changes and additions are marked in red in the revised paper. The main revisions to
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23 the paper and specific responses to the reviewer’s comments are outlined below.
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 Journal of Materials Engineering and Performance Page 2 of 28

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4 Responses to the comments of Reviewer #1
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6 1. Improvement with regard to the standard of English is a must. For example, “The
7 results show there to be a ..(Abstract)”. Page 3 – “At present ... are desirable [42]”-
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9 Incomplete statement.
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11 Response:
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Thank you for allowing us the opportunity to correct the grammar problems and
14 the content of the paper. The paper has been proofread by a native English
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speaker with a background in science as requested. We have revised the whole
17 manuscript carefully and tried our best to correct grammar and syntax errors.
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We have also revised incomplete statements to improve the clarity. The revised
20 statements are also provided below:
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I. Abstract – The findings indicate a strong relationship between the hardness,
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23 electrical conductivity, and degree of sensitization (DoS).
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II. Page 3 – At present, the development of better non-destructive methods
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26 (NDT), for example, ultrasonic methods [41, 42], eddy current testing [16, 43],
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and new detection methods [44-50] is desirable for the fast evaluation of
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29 mechanical strength and corrosion resistance in the aluminum alloys.

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31
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32 2. Page 2 “... due to elevated temperature [5]” What is elevated temperature in ship
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structures? Page 3 - “..reflected in the pile by the..” Not clear.
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37 We have revised the description of what we mean by elevated temperatures and
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39 what might cause them. We hope that the modification clarifies the meaning. The
40 revisions are provided below:
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42 I. Page 2 – However, the major design issue encountered when using the
43 wrought 5XXX aluminum-magnesium alloys for ship structures is degradation
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45 of the mechanical properties due to elevated temperatures [5], which can be
46 causes by welding, flame straightening, and/or thermal exposure.
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48 II. Page 3 – Reduction in the corrosion resistance is reflected in the degree of β
49 phase precipitation and a general increase in conductivity [22, 36]. This
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51 occurs due to changes in the concentration of solute Mg atoms in the Al
52 matrix [3, 37], changes in the microstructure (grain size, dispersoids,
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54 recrystallisation) which develop during heat treatments (different
55 sensitization times, sensitization temperatures) [8], and changes in the
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57 intensity of the precipitation [22, 36, 38-40].
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Page 3 of 28 Journal of Materials Engineering and Performance

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3. Page 4 – Why microhardness not macrohardness was selected when annealing
5 and sensitization treatments made the microstructure more inhomogeneous?
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Even in microhardness testing, the selected load (150 g) appears too low for
8 present purpose. Proper justification or fresh testing is required.
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10 Response:
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12 Thank you for pointing this out. We conducted the hardness experiment again.
13 The revised statements are provided below:
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15 Vickers hardness testing was conducted to quantify the strength and determine
16 the extent of softening caused by annealing. The hardness measurements were
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18 executed using a Struers Duramin-A300 hardness tester operating with a 1 Kg load.
19 The hardness values reported in this study are the average of ten measurements
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21 for each sample.
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24 4. Page 5- Why red coloured statement? The ‘solid’ and ‘open’ symbols should be a
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25 part of the figure caption. In general, figures captions are not detailed enough.
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27 Consider through revision.
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29 Response:
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We have corrected the symbol definitions in the figure captions.
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5. Page 5 – “These results indicate that ... solute Mg atoms precipitating out of alpha-
35 Al matrix does not affect the hardness...”- How does it possible considering
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metallurgical phenomena?
38 Response:
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40 The results of the metallographic investigation and hardness measurements of the
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42 as-annealed and as-sensitized alloys are presented below. The results indicate
43 that there is not much difference in the hardness of the as-annealed and as-
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45 sensitized alloys. It seems that the hardness of the alloy is not affected by the β
46 phase. Therefore, we conclude that the loss in the concentration of solute Mg
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48 atoms precipitating out the α-Al matrix does not affect the hardness of sensitized
49 alloys.
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51 As-annealed As-sensitized
52 450°C/30min 450°C/30min+175°C /168h
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 Journal of Materials Engineering and Performance Page 4 of 28

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13 Hardness: 74.3 HV Hardness: 74 HV
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16 6. What is ‘LS surface’? Please explain.
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Response:
19 Thank you for pointing out this omission. We have explained the abbreviation in
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21 the revised manuscript:
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22 The as-received specimen displays a marked fibrous rolling deformation

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24 organization (Fig. 1(a)) in the longitudinal-short transverse (L-ST) orientation
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27 7. Page 6 – “.. continuous films ... continuous network ..” The concerned
28 micrographs do not support ‘continuous’ term. Similarly, explain the
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30 “homogenous” term in “...lead to the formation of a “homogeneous” structure..”
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32 Response:
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34 I. Thank you for pointing out to us the lack of clarity in the micrographs in figure
35 1. We have replaced them with a new set of SEM micrographs; see Figs. 1(e)-
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37 (d). The SEM micrographs clearly show a continuous network of β phase
38 precipitates along the grain boundaries.
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40 II. According to the Al-Mg binary phase diagram shown below, annealing of the
41 alloys at an elevated temperature (~250°C) exceeding the solubility limit of
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43 Mg in aluminum leads to re-dissolving of the β-phase precipitates in the α
44 matrix so they do not form a continuous network along the grain boundaries.
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This means that annealing at temperatures of around 250°C tends to create
47 a more “low-sensitized” structure.
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Page 5 of 28 Journal of Materials Engineering and Performance

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26 The revised statements are provided below:
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According to the Al-Mg binary phase diagram, β-phase precipitation can be
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29 re-dissolved into the α matrix by annealing the alloys at elevated

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temperatures (~250°C) exceeding the solubility limit of Mg in aluminum so
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32 that they do not form a continuous network along the grain boundaries.
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Therefore, annealing the alloy at a temperature between 200-250°C led to
35 the formation of a more “low-sensitized” structure making the alloy less
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susceptible to IGC because of the absence of precipitation of the β phase.
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8. Page 6 – “ Hence, .. was closely related not only.. and ageing time but also to
41 orientation..” – Neither ageing time not orientation was varied in this study.
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43 Response:
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45 Thank you for pointing this out. We have revised the description to improve the
46 clarity:
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48 Hence, the DoS of the tested alloy was closely related to microstructure and β
49 phase distribution.
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52 9. Page 8 –“The results showed... than the increasing dislocation density..” Not clear.
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54 Response:
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56 We have revised the description and hope that the modification will be clearer:
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58 Miljana and Endre [15] also demonstrated that the increase in electrical
59 conductivity due to the β phase precipitation was more enhanced than the
60 increasing dislocation density.
 Journal of Materials Engineering and Performance Page 6 of 28

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5 10. Fig. 1 – Micrographs are hard to follow with the concerned text. Authors should
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also include a new set of SEM micrographs, both annealed and sensitized samples
8 (prior to their corrosion tests).
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10 Response:
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12 We have replaced the SEM micrographs in Figs. 1(e)-(d). The SEM micrographs
13 clearly show a continuous network of β phase precipitate along the grain
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15 boundaries.
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18 11. Fig. 4 – Precipitate appears to be too high and too many within the grains in Fig.
19 4(e).
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21 Response:
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23 We have done our best to correct the mistakes throughout the revised manuscript
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and in Fig. 4(e).
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12. Explain how Fig. 5 was constructed. What are the meaning of DoS < 3 and > 90
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29 mg/cm2 (in absence of experimental data)?

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31 Response:
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33 In order to establish the relationship between the hardness, electrical conductivity,
34 and degree of sensitization (DoS) from the test results obtained in this study we
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36 produced a contour plot using the origin@ Pro software based on the data for the
37 hardness, electrical conductivity, and DoS at 150, 200, 250, 300, 350, 400, and
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39 450°C and sensitization treatment at 175°C for 168 hours. In addition, the NAMLT
40 test results show that the DoS of the as-annealed and as-sensitized samples were
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42 about 2.1-4.1 mg/cm2 and 30.8-89.4 mg/cm2, respectively. Therefore, the contour
43 plot demonstrates the trend from low DoS (3 mg/cm2) to high DoS values (90
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45 mg/cm2).
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48 13. Following refs (Corrosion 72 (2016) 221-241; Materials Science and Engineering:
49 A 792 (2020) 139792; Journal of Materials Engineering and Performance 28 (2019)
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51 2764-2778; Corrosion Science 169 (2020)108618; Materials and Corrosion 70
52 (2019) 2052-2063; Journal of Materials Research and Technology 9 (2020) 1005-
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54 1024) may be included.
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56 Response:
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Thank you for providing the valuable research information. We have read the
59 papers and included the additional references in the revised manuscript.
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Page 7 of 28 Journal of Materials Engineering and Performance

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5 Responses to the comments of Reviewer #2
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7 1. How the authors measured weight loss, a method of weight loss measurement is
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9 not mentioned in the article.
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11 Response:
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Weight loss measurements of the specimens were conducted per ASTM G67
14 (NAMLT, nitric acid mass loss test) to examine the intergranular corrosion
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susceptibility. The NAMLT Testing method is discussed in Section 2.3.
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2. What is the brand and model of the optical microscope used?
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22 The missing information has been proved in the revision as follows:

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24 The metallographic investigation was carried out using optical microscopy (OM,
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25 Olympus BX60M).
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28 3. There are some previous studies between electrical conductivity and corrosion
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30 behaviour. I recommend the authors to read and benefit from these works.
31 Publication links:
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33 https://onlinelibrary.wiley.com/doi/full/10.1002/maco.201709497
34 https://onlinelibrary.wiley.com/doi/full/10.1002/maco.201810436
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38 Thank you for providing the valuable research information. We have read these
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papers and added the references to the revised manuscript .
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46 Special thanks to the referees for their detailed and valuable comments. We hope
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48 that the revisions in the manuscript and our accompanying responses will be sufficient
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50 for publication of our manuscript in JMEP.
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 Journal of Materials Engineering and Performance Page 8 of 28

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4 Use of Hardness and Electrical Conductivity Testing to Evaluate Heat
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6 Damage and Sensitization in 5083-H116 Al-Mg Alloys
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Yu-Chih Tzeng1, Cheng-Yu Lu2, Kaliyaraj Kaliyaperumal3, Ren-Yu Chen4,*
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11 Department of Power Vehicle and Systems Engineering, Chung-Cheng Institute of
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13 Technology, National Defense University, Taoyuan City, 33551, Taiwan
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15 2 Department of Naval Architecture and Ocean Engineering, Nation Kaohsiung University
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of Science and Technology, Kaohsiung City, 81157, Taiwan
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19 3 Senior
20 Structural Naval Architect, Naval and Commercial Ship Design, K2L4E6, Canada.
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4 Department of Marine Mechanical Engineering, R.O.C. Naval Academy, Kaohsiung City,

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24 81345, Taiwan
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26 *Corresponding author: renyu.tw@gmail.com
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Abstract
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32 Detecting heat damage and eliminating the susceptibility to sensitization of wrought

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34 5xxx series aluminum-magnesium alloys is of practical importance for the remediation of
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36 field structures. Electrical conductivity and hardness testing were employed to provide
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indirect evidence to assess the microstructural evolution of 5083-H116 alloys after
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39 annealing treatment at 150, 200, 250, 300, 350, 400, and 450°C and sensitization treatment
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41 at 175°C for 168 h. The findings indicate a strong relationship between the hardness,
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43 electrical conductivity, and degree of sensitization (DoS). This methodology can be used
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as a simple guide to quickly determine whether heat damage or sensitization exists.
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48 Keywords: 5083-H116, Hardness, Electrical Conductivity, Mg2Al3, Sensitization, Heat
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50 Damage
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1 Introduction
5 Alloys of the wrought 5XXX aluminum-magnesium series, such as 5086, 5083, 5383,
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7 5456, and 5059 alloys with H116 and H321 tempering, are attractive for use in the hulls
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9 and decks of ship structures owing to their outstanding properties, including high strength-
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to-weight ratio, good corrosion resistance performance, and weldability [1,2]. The 5xxx
12 aluminum-magnesium alloys are the strongest non-heat-treatable aluminum alloys and
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14 significant strengthening effects can be achieved through cold working and solid solution
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16 strengthening by the addition of magnesium [2-4]. However, the major design issue
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encountered when using the wrought 5XXX aluminum-magnesium alloys for ship
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19 structures is degradation of the mechanical properties due to elevated temperatures [5],
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21 which can be causes by welding, flame straightening, and/or thermal exposure. The main
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23 reduction in mechanical properties is caused by recrystallization upon annealing at high
24 temperatures (250-350°C), which leads to the destruction of grain structures. [5,6]. The
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26 mechanical behavior at elevated temperatures of several 5xxx aluminum-magnesium alloy
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28 has been well researched [5-12], and design guides (Eurocode 9 [13]) outlining the
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structural behavior of aluminum during fires have been developed. The microstructures and
31 electrical conductivity of aluminum alloys are sensitive to a decline in the mechanical
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33 properties. [14, 15]. The reduction in mechanical properties is dependent on changes in the
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35 distribution, size, shape, and coherency strain of the precipitate intermetallic phases in heat-
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treated alloys [16].
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38 Another particular issue with using wrought 5XXX aluminum-magnesium alloys in
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40 ship structures is their corrosion resistance degradation because of the sensitization
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42 phenomenon [17-19]. The exposure of 5XXX aluminum-magnesium alloys at temperatures
43 from 65°C to 200°C over a long period of time can result in the continuous precipitation of
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45 intermetallic β phases (Mg2Al3) along the grain boundaries to form a mesh [19-26]. Because
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47 the intermetallic β phase works as a sacrificing anode to the Al-matrix in corrosive seawater
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environments, galvanic corrosion very easily leads to the creation of common sites for
50 intergranular corrosion (IGC) and stress corrosion cracking (SCC) nucleation of the β phase
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52 [27-32]. This microstructural sensitivity phenomenon leading to corrosion of the 5XXX
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54 aluminum-magnesium alloy is termed sensitization [17] and is usually assessed by the nitric
55 acid mass loss test (NAMLT) [33]. The NAMLT test is an accelerated corrosion test used
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57 to compare the degree to which the alloy has been sensitized by the formation of the β
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59 phase. The degree of sensitization (DoS) is measured by taking the mass loss per unit of
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3 surface area (mg/cm2) after a specimen has been immersed in nitric acid at 30 °C for 24
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5 hours. An alternate method for DoS quantification is the electrochemical method which
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7 measures the electrochemical response of the β phase synthesized in the bulk form in situ
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[34,35]. Reduction in the corrosion resistance is reflected in the degree of β phase
10 precipitation and a general increase in conductivity [22,36]. This occurs due to changes in
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12 the concentration of solute Mg atoms in the Al matrix [3,37], changes in the microstructure
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14 (grain size, dispersoids, recrystallisation) which develop during heat treatments (different
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sensitization times, sensitization temperatures) [8], and changes in the intensity of the
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17 precipitation [22,36, 38-40].
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19 At present, the development of better non-destructive methods (NDT), for example,
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21 ultrasonic method [41,42], eddy current testing [16,43], and new detection methods [44-50]
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22 is desirable for the fast evaluation of mechanical strength and corrosion resistance in the
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24 aluminum alloys. The use of NDT methods to evaluate the effects of heat treatment on the
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26 microstructure, mechanical properties, and DoS of the 5xxx aluminum-magnesium alloy is
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gradually increasing, but the overall relationship between softening and sensitizing is often
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29 ignored. This study examines the effects of heat treatment (150-450°C) on the
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31 microstructures and the DoS evolution, and identifies the relationship between electrical
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33 conductivity and hardness for the various DoS. The identified relationships will assist in
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determining whether heat damage or sensitization exists in 5xxx aluminum-magnesium
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40 2 Experimental procedures
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42 2.1 Materials and Heat Treatment
43 The experiments were conducted on 6mm thick commercial grade 5083-H116
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45 aluminum alloy plates (as-received). The chemical composition of the as-received 5083-
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47 H116 alloy is given in Table 1. The procedure for the seven heat treatments designed in this
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study is as follows: the 5083-H116 specimens were placed in an air furnace for the
50 application of heat treatment at 150, 200, 250, 300, 350, 400, and 450°C for 30 min,
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52 followed by water quenching (as-annealed). The as-annealed specimens were then
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54 artificially aged at 175°C for 168 h to allow for sensitization (as-sensitized). A temperature
55 of 175°C was found to be favorable for the Al and Mg atoms to diffuse together to form the
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57 precipitates of the β phase [12]. This temperature was high enough to accelerate β phase
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59 precipitation from the supersaturated solid solution but not so high as to introduce a new
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Page 11 of 28 Journal of Materials Engineering and Performance

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3 phase.
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7 2.2 Microhardness Testing
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Vickers hardness testing was conducted to quantify the strength and determine the
10 extent of softening caused by annealing. The hardness measurements were executed using
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12 a Struers Duramin-A300 hardness tester operating with a 1 Kg load. The hardness values
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14 reported in this study are the average of ten measurements for each sample.
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17 2.3 NAMLT Testing
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19 The NAMLT test was conducted as per ASTM G67 specifications to examine the IGC
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21 susceptibility of the as-annealed and as-sensitized specimens. The specimens were cut into
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22 50 mm × 6 mm × 6 mm (Length (L) × Width (W) × Thickness (T)) pieces and prepared as

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24 per ASTM G67. The prepared test specimens were immersed in a 70% nitric solution at
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26 30°C for 24 h to determine the mass loss per unit area (mg/cm2) as a measure of the DoS.
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All experiments were conducted three times and the average values were reported along
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29 with the standard deviation. The tested specimens were considered to be resistant to IGC
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31 when the DoS was less than 15 mg/cm2. Specimens with DoS values greater than 25 mg/cm2
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33 were considered susceptible to IGC. For intermediate DoS, metallographic examination is
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required to determine the IGC resistance.
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38 2.4 Electrical Conductivity
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40 Electrical conductivity tests were carried out to examine the change in intensity of β
41 phase precipitation of the as-annealed and as-sensitized specimens. A Fisher’s Sigmascope
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43 SMP10 conductivity meter, an eddy current instrument, was used for this test. The change
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45 in electrical conductivity was measured at room temperature as the percent of the
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international annealed copper standard (%IACS). Electrical conductivity was measured at
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48 three different positions on each test specimen and the average value reported. To ensure
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50 the accuracy of the measurements, the equipment was calibrated before the tests according
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52 to the calibration standards using a material with a known conductivity.
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55 2.5 Microstructure
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57 The metallographic investigation was carried out using optical microscopy (OM,
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Olympus BX60M). The specimen’s surface was first polished with an 0.05 alumina
60 suspension followed by electro-etching in Barker’s reagent. To clarify the distribution and
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3 extent of the β phase precipitates, as-sensitized specimens were polished to a 0.05-micron
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5 surface finish and etched with a 5% hydrofluoric acid solution. Scanning electron
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7 microscopy (SEM; Hitachi S-3000N) analysis was utilized to observe the morphology of
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the specimens after NAMLT testing. The microstructure of the precipitated phases was
10 analyzed using transmission electron microscopy (TEM; JEOL JEM-ARM200FTH). The
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12 TEM samples were prepared by a double beam focused ion beam system (FIB; FEI Versa
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14 3D Dual Beam).
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17 3 Results
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19 3.1 Hardness Profiles
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21 The hardness values of the tested 5083-H116 alloy, as-annealed (marked as squares)
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23 and as-sensitized (marked by circles), presented in Fig. 1, are closely associated with the
24 characteristics of the deformed microstructures. The hardness distribution was similar to
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26 some tensile test results reported in previous studies [5,6,9,11,22]. The hardness distribution
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28 curve shows that annealing at temperatures ranging between 150 ° C to 250 ° C reveals the
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recovery of the alloy structure resulting in a slight decrease in hardness. Significant changes
31 in hardness were caused by the occurrence of recrystallization between 250°C and 450°C.
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33 Accordingly, the basic softening process occurred in the temperature range from 250-450°C.
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35 In addition, the plotted data showed no significant difference in hardness values between
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the as-annealed and as-sensitized specimens. These results indicate that the hardness and
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38 strength of the as-annealed 5083-H116 alloys are not affected by the β phase and that the
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40 corresponding loss of the concentration of solute Mg atoms precipitating out the α-Al
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42 matrix does not affect the hardness properties of sensitized alloys. The microstructural
43 evolution of the as-received 5083-H116 alloy after annealing for 30 min at temperatures of
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45 150, 300, and 450 °C is shown in Figs. 1(a)-(d). The as-received specimen displays a
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47 marked fibrous rolling deformation organization (Fig. 1(a)) in the longitudinal-short
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transverse (L-ST) orientation. As can be seen in Fig. 1 (b) when the annealing temperature
50 is below 250°C, the grains are distributed in an elongated fibrous structure along the rolling
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52 direction, indicating that there are no remarkable changes in the microstructure. This is
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54 predictable, since low-temperature annealing does not provide enough activation energy for
55 grain boundary migration. Compared with Fig. 1 (b), we can see the appearance of partial
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57 recrystallization structures containing equiaxial grains in the matrix after annealing at
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59 300°C for 30 min (as shown in Fig. 1(c)). As the annealing temperature is further increased
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Page 13 of 28 Journal of Materials Engineering and Performance

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3 to 450 °C, the existence of fine and nearly equiaxed grains in the matrix suggests that the
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5 alloy has been completely recrystallized, as shown in Fig. 1(d). Microstructural
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7 examination was also performed to evaluate the effect of the annealing treatment on β phase
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precipitation in the sensitized state.
10 The evolution of the microstructure of the as-sensitized 5083-H116 alloys, with and
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12 without the application of various annealing treatments, is shown in Figs. 1(e)-(h). Fig. 1(e)
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14 illustrates the typical microstructure of the 5083-H116 alloy, consisting of uniformly
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dispersed β phase precipitates. For the non-sensitized alloy, there is no obvious indication
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17 of any precipitation at the grain boundaries, and all other particles are distributed uniformly
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19 within different grains. After sensitization for 168 h at 175°C, continuous films of the β
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21 phase formed. Figs. 1(f)-(h) show that the continuous network of the β phase tends to
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24 microstructure of a sensitized alloy depends primarily on the morphology of the grain
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26 structure.
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29 3.2 NAMLT Profiles

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31 The DoS of the as-annealed and as-sensitized samples after undergoing NAMLT are
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33 summarized in Fig. 2. The results show that the DoS of the as-annealed samples were about
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2.1-4.1 mg/cm2. The resistance of these as-annealed alloys to intergranular corrosion (DoS
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36 <15 mg/cm2) after annealing at temperatures up to 450°C was primarily due to having a
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38 discrete β phase precipitates at the grain boundaries.
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40 In contrast, there was a dramatic increase in mass loss in the as-sensitized specimens,
41 which made them susceptible to intergranular corrosion (DoS > 25 mg/cm2). The increase
42
43 in the DoS was contributed to by the increase in the β phase fraction, although the
44
45 morphology and distribution also affect the DoS. As can be seen in Figs. 2(a)-(d), the cross-
46
section surface morphology of the as-sensitized specimens after NAMLT depend primarily
47
48 on the morphology of the grain structure. Hence, the DoS of the tested alloy was closely
49
50 related to microstructure and β phase distribution.
51
52 The DoS of the recrystallized structure (80.0-89.4 mg/cm2) is greater than that of the
53 recovered structure (30.8-57.1 mg/cm2). It is worth noting that the DoS of the recovered
54
55 structure for the alloy annealed at 200-250°C (37.93-30.78 mg/cm2) with the single α-Al
56
57 structure is less than that of the alloy annealed at less than 200°C (55.1-57.1 mg/cm2) with
58
59
the dual α+β structure. According to the Al-Mg binary phase diagram, β-phase precipitation
60 can be re-dissolved into the α matrix by annealing the alloys at elevated temperatures
6
 Journal of Materials Engineering and Performance Page 14 of 28

1
2
3 (~250°C) exceeding the solubility limit of Mg in aluminum so that they do not form a
4
5 continuous network along the grain boundaries. Therefore, annealing the alloy at a
6
7 temperature between 200-250°C led to the formation of a more “low-sensitized” structure
8
9
making the alloy less susceptible to IGC because of the absence of precipitation of the β
10 phase. This observation is similar to that made in previous studies [7,9,51,52].
11
12
13
14 3.3 Electrical Conductivity Profiles
15
Fig. 3 shows the electrical conductivity behavior of the as-annealed and as-sensitized
16
17 specimens obtained using various annealing temperatures. The electrical conductivity of
18
19 the as-annealed alloy changed briefly when the annealing temperature was increased from
20
21 100 to 450°C. The electrical conductivity increased substantially from 29.11 to 29.27
Fo

22 %IACS throughout the recovery process (below 250°C) and decreased slightly to 29.07
23
24 %IACS during the recrystallization (300-450°C). The electrical conductivity increased
rP

25
26 significantly, up to 30.03 %IACS, after sensitization at 175°C for 168 h during the recovery
27
28
and recrystallization of the microstructure.
ee

29 The electrical conductivity of 5083-H116 alloys is affected by the dislocation density,

30
31 microstructure, and β phase precipitation during the annealing and sensitization process.
rR

32
33 This can be seen in Figs. 3(a)-(e). The relative changes in electrical conductivity
34
corresponding to the annealing and sensitization were calculated by using the following
35
ev

36 equations:
37
38
iew

39 Δσa=(Cas-annealed-Cas-received)/Cas-received×100% (1)
40
41 Δσs=(Cas-sensitized-Cas-annealed)/Cas-annealed×100% (2)
42
43
44
where Cas-received, Cas-annealed, and Cas-sensitized are the electrical conductivity of the as-received
45 specimens, annealed specimens, and sensitized specimens, respectively.
46
47
48
49 3.3.1 Influence of Annealing on Electrical Conductivity
50
The changes in the relative electrical conductivity between the as-received and as-
51
52 annealed alloys (Δσa) are shown in Fig. 4. The evolution of the microstructure during the
53
54 annealing procedure is illustrated in Figs. 4(a)-(c). The electrical conductivity of the non-
55
56 sensitized alloys was considered as a function of dislocation density and bulk Mg content.
57 During recovery (< 250°C), dislocation configurations are produced with low strain
58
59 energies and their physical properties, such as electrical and thermal conductivities, recover
60

7
Page 15 of 28 Journal of Materials Engineering and Performance

1
2
3 to pre-cold-work states [53]. However, for the 5083-H116 alloys, the 4.5 wt% Mg
4
5 concentration leads to nucleation and growth of the β phase along the grain boundaries due
6
7 to the solubility limits of Mg below 250ºC. Annealing temperatures ranging from 100 to
8
9
250°C can create differences in the β phase morphology and precipitation along the grain
10 boundaries. Phase diagrams can help account for the undissolved β percentage at
11
12 equilibrium. The variations in electrical conductivity due to the β phase precipitation of the
13
14 cold-rolled Al-Mg alloy have already been investigated [28,54]. Miljana and Endre [15]
15
also demonstrated that the increase in electrical conductivity due to the β phase precipitation
16
17 was more enhanced than the increasing dislocation density. Therefore, the electrical
18
19 conductivity increases during the recovery process (< 250°C) contributed to by the β phase
20
21 precipitation.
Fo

22 After the recovery is complete (250-450°C), a new set of strain-free and equiaxed
23
24 grains (Fig. 1(d)) form with low dislocation densities (Fig. 3(d)). The alloy becomes softer
rP

25
26 and weaker, as its mechanical properties are restored to their pre-cold-work values. These
27
28
results, which are consistent with previous studies [15,55], indicate that the dislocation
ee

29 contribution to the total electrical conductivity of the recovered structure is more

30
31 pronounced than that of the recrystallized structure, since the dislocation densities in the
rR

32
33 recrystallized structure are lower. From the phase diagrams, it can be seen that the limiting
34
temperature for stabilization of the 5083-H116 specimens is about 250°C. The Mg solid
35
ev

36 solubility will increase when the annealing temperature is above 250°C and the β phase will
37
38 dissolve into the matrix. Therefore, it is obvious that the electrical conductivity of the
iew

39
40 recrystallized structure will drop lower than the as-received conductivity due to low
41 dislocation densities and Mg solid solute into the Al matrix.
42
43
44
45 3.3.2 Influence of Sensitization on Electrical Conductivity
46
The changes in the relative electrical conductivity between the as-annealed and as-
47
48 sensitized alloys (Δσs) are also shown in Fig. 4. It is well known that high strain energies at
49
50 the grain boundaries lead to the development of precipitation of the β phase along the grain
51
52 boundaries. Consequently, the β phase tends to precipitate continuously along the grain
53 boundaries in both cold-worked and recrystallized structures. The precipitation of the β
54
55 phases in different microstructures is demonstrated in Figs. 4(d)-(f).
56
57 From the experimental data, it can be seen that the Δσ was more pronounced for the
58
59
recovered structure (< 250°C) than for the recrystallized structure (> 250°C). The result is
60 consistent with previous reports [56-59], where β phase precipitation tends to grow
8
 Journal of Materials Engineering and Performance Page 16 of 28

1
2
3 heterogeneously on dislocations/grain boundaries and intermetallic precipitates. In addition,
4
5 some defects remaining in the grains of the recovered structure also act as preferential
6
7 nucleation sites for the precipitation of the β phase. Therefore, the recovery of the structure
8
9
is beneficial to the discontinuous precipitation of the β phase, as shown in Fig. 3(b). After
10 recrystallization, the high strain energy in the structure is relieved. The nucleation sites
11
12 decrease making heterogeneous nucleation of the β phase in the grain interiors difficult.
13
14 The recrystallized grain boundary areas where continuous β phase deposition is easy, are
15
shown in Fig. 3(c).
16
17
18
19 3.4 Relationship between electrical conductivity and hardness and effect on the DoS
20
21 All test results from this study are summarized in a contour plot and presented in Fig.
Fo

22 5, representing a compilation of data collected via NAMLT for various hardness and
23
24 electrical conductivity values. According to ASTM G67, the data can be divided into three
rP

25
26 distinct regions: (I) when the mass loss is less than 15 mg/cm2, the alloy is not sensitive to
27
28
intergranular corrosion; (II) when it is in the range of 15–25 mg/cm2, there is the possibility
ee

29 of intergranular corrosion in the alloy; and (III) when the mass loss exceeds 25 mg/cm2, the
30
31 alloy is sensitive to intergranular corrosion. The cross-linking of electrical conductivity and
rR

32
33 hardness is responsive to the influence of matrix precipitates on the IGC susceptibility.
34
Consequently, the contour plot can be used as a simple guide to quickly determine whether
35
ev

36 heat damage or sensitization exists.

37
38
iew

39
40 4 Conclusions
41
42 As has been experimentally proved in this paper, hardness and electrical conductivity
43 measurements can be employed as indirect evidence to evaluate changes in the material
44
45 properties and corrosion resistance of an alloy. This method can be used as a guide by
46
47 fabricators and in repair facilities to quickly determine whether the material is sensitized or
48
49
not. This will assist in the accurate planning and execution of fabrication and maintenance
50 work, avoiding unnecessary expensive tests or additional work, thereby significantly
51
52 reducing the cost of maintenance and fabrication. However, it should be noted that sound
53
54 engineering judgment and proper interpretation of the data are vital for accurate
55 interpretation of the results accurately and to determine whether the material has been heat
56
57 damaged or not, and then to make recommendations based on these predictions.
58
59
60

9
Page 17 of 28 Journal of Materials Engineering and Performance

1
2
3
4
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19
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21
Fo

22
23
24
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25
26
27
28
ee

29
30
31
rR

32
33
34
35
ev

36
37
38
iew

39
40
41
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43
44
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47
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49
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52
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 Journal of Materials Engineering and Performance Page 22 of 28

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4
5
Table 1 Chemical composition of 5083-H116 alloy (wt%)
6 Mg Mn Cr Si Fe Cu Zn Ti Zr Al
7 4.51 0.54 0.07 0.11 0.29 0.05 0.12 0.01 0.07 Bal.
8
9
10
11
12
13
14
15
16
17
18
19
20
21
Fo

22
23
24
rP

25
26
27
28
ee

29
30
31
rR

32
33
34
35
ev

36
37
38
iew

39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
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Page 23 of 28 Journal of Materials Engineering and Performance

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3 Figure 1. Results from the hardness test of as-annealed and as-sensitized specimens.
4
5 Microstructures of cross-sections under various annealing temperatures (a-d) and
6
7 then sensitization at 175°C for 168 h (e-h).
8
9
10 Figure 2. NAMLT results of the 5083-H116 alloy annealed at various annealing
11
12 temperatures. SEM micrographs of (a) as-received, (b) 150°C, (c) 250°C, (d)
13
14 300°C, (e) 450°C after G67 mass loss test.
15
16
17 Figure 3. Electrical conductivity results of the 5083-H116 alloy annealed at various
18
19 annealing temperatures. SEM and TEM micrographs of β phase precipitation: (a)
20 as-received, (b) 150°C and (c) 400°C after sensitization at 175°C for 168 h. TEM
21
Fo

22 images of the 5083-H116 alloy annealed at (d) 450°C, and then (e) sensitization
23
24 at 175°C for 168 h.
rP

25
26
27 Figure 4. The relative electrical conductivity changes of the as-annealed (Δσa) and as-
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Figure 5. Correlation between hardness and electrical conductivity (% IACS) via NAMLT.
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 Journal of Materials Engineering and Performance Page 24 of 28

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Page 25 of 28 Journal of Materials Engineering and Performance

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 Journal of Materials Engineering and Performance Page 26 of 28

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Page 27 of 28 Journal of Materials Engineering and Performance

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 Journal of Materials Engineering and Performance Page 28 of 28

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