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Abstract: Mild steel is one of the most commonly used materials in the construction industry throughout the world, but it is also very
vulnerable to corrosion in aggressive environments. There is little research on how corrosion and the hydrogen released from the corrosion
process affect the mechanical properties of the corroded steel. The intention of this paper is to present results produced from a comprehensive
experimental program designed to investigate the effects of corrosion and corresponding hydrogen on the degradation of mechanical proper-
ties of mild steel in corrosive soil environments. Both microstructural analysis and mechanical tests on corroded steel are undertaken at
different exposure times and conditions of corrosion. The effects of corrosion and the released hydrogen on steel are examined phenom-
enologically and analyzed quantitatively at the microstructural level in terms of constituent elements and phase changes, and at the macro-
structural level in terms of mechanical properties of strength and ductility. From the analysis of test results, a relationship of cause and effect
of corrosion, hydrogen release, and strength reduction is established. The results and their analysis presented in the paper can contribute to the
body of knowledge related to the degradation of mild steel, which helps in determining its service life prediction under corrosive environ-
ments. DOI: 10.1061/(ASCE)MT.1943-5533.0002560. © 2018 American Society of Civil Engineers.
Author keywords: Mild steel; Corrosion; Hydrogen; Mechanical properties; Microstructural analysis.
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(a)
(b) (c)
Fig. 1. Experimental setup: (a) dimensions of test specimen (filled area indicates protected area from corrosion); (b) wrapped test specimens; and
(c) specimens in test containers.
6 0 pH (1M)
-0.48 pH (3M) and 5 pH solutions, respectively, after 28 days as shown in Fig. 4.
5 Meanwhile on their 7th day, the corrosion rates were 5.32, 3.02,
and 0.145, and 0.056 mm=year, respectively, as shown in Fig. 4.
4
From these results, it can be inferred that the corrosion rates are
3
nearly doubled on the 28th day to those on the 7th day of the speci-
men in −0.48 pH and 0 pH solution, which indicates the severity of
2 the corrosive environment. The high corrosion rates can be attrib-
uted to the coupled effect of chloride and hydrogen ions, which can
1 decrease pH and the passivity of steel with time. Therefore, it is
possible to have a lower pH in the corroded areas of specimens
0 as compared to the surrounding pH environment.
0 5 10 15 20 25 30
Based on the results of corrosion rates and hydrogen concentra-
Time (days) tion, an empirical relation can be derived using the statistics soft-
ware SPSS with R2 ¼ 0.72 and a very high statistical significance
Fig. 3. Hydrogen concentration of specimens in various solutions.
i.e., p ≪ 0.05, as follows:
Fig. 5. Change in mechanical property of specimens in various solutions: (a) failure strains; (b) yield strength; and (c) ultimate strength.
The percentage reduction after 28 days was 38% and 18% in the ft ¼ −10.366 × CR − 1.139 × T þ 443.456 ð4Þ
−0.48 and 0 pH solutions, respectively. However, the decline in
yield strength in the other two soil solutions was not that significant where f t is yield strength in MPa. Eqs. (3) and (4) can be used to
due to their relatively high pH (2.5 and 5) as compared to the −0.48 predict the residual strength of mild steel in highly aggressive envi-
and 0 pH (HCl) solutions. It was found that the coupled effect of Cl ronments, which can be very useful for predicting the failures of
and Hþ resulted in more decline of the yield strength of specimens steel structures.
in HCl solutions.
The results of reduction of ultimate strength of specimens in
different solutions are presented in Fig. 5(c). As can be seen, Microstructural Analysis
the ultimate strength of the specimens at the 7th day of corro-
X-ray fluorescence (XRF) was used to determine the constitutent
sion shows a similar trend as that from the yield strength results,
element variation of steel specimens due to the corrosion process.
i.e., not a significant change in the ultimate strength. However, after
The results were compared with the uncorroded specimen to deter-
28 days of corrosion, the ultimate strength of the specimens in
mine the reduction or inclusion of elements during the corrosion
−0.48 pH solutions was significantly reduced from 426.84 MPa
process. A scanning electron microscope (SEM) and electronic
to 214.8 MPa, indicating the severity of the corrosive environment.
back-scattered diffraction (EBSD) mapping of the corroded spec-
The change in mechanical properties of the specimens in the 2.5
imens for various corrosive environment solutions were taken at 7,
and 5 PH solutions was small because of the low acidity of these
14, and 28 days. The EBSD measurements were performed with an
solutions as compared to the −0.48 and 0 pH solutions. Corrosion
FEI Nova NanoSEM with the Aztec software suite. The purpose of
is a slow process that takes time to occur. In the current research,
using EBSD in this research was to quantify any microstructural
the duration of testing is 28 days, which probably is not enough to
degradation and phase transformation due to the corrosion process
cause mechanical change for a pH of 2.5 and 5 in this short period
with time. The results of the corroded specimens from different
of time. The average change in mechanical properties of failure
environments were compared with each other and also with the un-
strain, yield strength, and ultimate strength of the specimens in vari-
corroded steel specimens to determine any microstructural changes
ous solutions is shown in Table 4.
due to corrosion over time.
corrosion process continues, the liberation of Fe ions from the steel These microcracks appear to be hydrogen embrittlement cracks
surface continues, and consequently reduces the percentage of Fe due to the existence of hydrogen blisters, which are signs of
in the steel with time. The reduction in Fe was highest in the hydrogen accumulations (Jin et al. 2010). High hydrogen concen-
−0.48 pH solution, being subjected to the severest corrosive envi- tration favors rapid initiation of cracks, as there were more cracks
ronment, then it was followed by 0, 2.5 and 5 pH solution. discovered in the −0.48 pH solution (hydrogen concentration of
Pickering (1971) has developed empirical equations for yield 5.97 ppm) compared with 0 pH HCl (hydrogen concentration of
(fy ) and tensile (f t ) strength of ferrite-pearlite steel under 5.03 ppm). The pits and cracks were clearly visible in specimens
0.25% C content that relate to contents of constituent elements immersed in the −0.48 and 0 pH solutions that could have caused
and grains diameter as follows: strength reduction (Jakubowski 2011). Pits and cracks were not
visible in specimens of the 2.5 and 5 pH solutions even after 28 days
fy ¼ 53.9 þ 32.34ðMnÞ þ 83.2ðSiÞ þ 354.2ðNfÞ þ 17.4ðd1=2 Þ of corrosion.
ð5Þ
Phase Analysis
f t ¼ 294.1 þ 27.7ðMnÞ þ 83.2ðSiÞ þ 3.9ðPÞ þ 7.7ðd−l=2 Þ ð6Þ
To further authenticate the grain sizes and phases of the corroded
where Mn is manganese, Si is silicon, Nf is nitrogen, and d is the areas and the surrounding regions, the EBSD technique was used
grain size of Fe and P is pearlite. All elements are given in percent- for analysis. Operating at 20 kV and using 6 spot sizes, EBSD maps
age while the diameter is in micrometers. of the corroded areas of various samples were taken. The purpose
As shown in Table 5 and Fig. 6, those elements that are prone to was to find which phase of steel had the maximum corrosion and
corrosion have increased and those that contribute to the strength then its subsequent hydrogen effect. After EBSD analysis of several
have been reduced. In Table 5, the percentage of large grains of Fe samples, the software Channel 5 (Oxford Instrument), an EBSD
in specimens was successively reduced with corrosion progress. postprocessing software, was used to calculate the phases and grain
From Figs. 6(a and c–e), it can be seen that the contents of elements sizes of EBSD maps. Using this software, the average of selected
iron (Fe), manganese (Mn), silicon (Si), and chromium (Cr) all de- larger grains was found to be 12.65 μm while the average of
crease over time with the progress of corrosion, in particular in the selected smaller grains was 5.73 μm.
more acidic solutions, i.e., 1 M (0 pH) and 3 M (−0.48 pH) solu- Moreover, from the EBSD map data of uncorroded samples, it
tions. From Figs. 6(b and f), it can be seen that contents of oxygen became evident that 98.15% was the ferrite phase, and the remain-
(O) and chloride (Cl) both increase successively with time, again ing percentage was cementite. Further, from the analysis of EBSD
more obvious in the 1 M (0 pH) and 3 M (−0.48 pH) solutions. maps of severely corroded areas of various test specimens, it was
These are the causal factors for strength reduction of corroded established that most of this central area was dominated by the fer-
steel. rite phase (Fe) and the other phases were cementite (Fe3 C) and iron
oxide (Fe2 O3 ). Ferrite is more prone to corrosion as it quickly
oxidizes, while cementite provides the resistance to corrosion
Microcracks and Blisters
(Syugaev et al. 2008). Fig. 8 represents the morphology and phase
From SEM analysis of specimens immersed in the 0 and −0.48 pH maps analysis of corroded specimens immersed in −0.48, 0, and
HCl solutions, microcracks can be observed as shown in Fig. 7. 2.5 pH solution near the pit areas after 28 days of corrosion.
Fig. 6. Change of elemental composition of specimens in various solutions: (a) iron; (b) oxygen; (c) manganese; (d) silicon; (e) chromium; and
(f) chloride.
Fig. 7. SEM image of micro cracks at the 28th day of corrosion: (a) 0 pH (1 M); and (b) −0.48 pH (3 M).
Fig. 8. Phases of surrounding corroded area of various specimens at the 28th day (SEM images and EBSD phase maps): (a) 0 pH, 28 days
(SEM image on the left and EBSD phase map on the right); and (b) −0.48 pH, 28 days (SEM image on the left and EBSD phase map on the right);
and (c) 2.5 pH, 28 days (SEM image on the left and EBSD phase map on the right).
The selected areas for the EBSD are shown on the left-side images Moreover, by using EBSD, accurate percentages of phases of
of Fig. 8, while the right-side images of this figure represent the specimens can be determined as shown in Fig. 9. As it can be seen
EBSD phase analysis of these areas. From visual inspection of from the EBSD analysis, ferrite, cementite, and iron oxide contents
these maps, a fair estimation of the phase percentage can be made of 71.76%, 0.92%, and 27.32% were obtained, respectively, after
without doing calculations. For instance, from Fig. 8(a) (right side), 28 days of corrosion from specimen immersed in the −0.48 pH
it can be seen that the red color, as labeled iron bcc (body-centered solution. These phases were determined to be 76.44%, 1.56%,
cube, i.e, ferrite), dominates the whole image with few visible and 22% in specimens of 0 pH solution, while 81.8%, 2.98%,
yellow-colored Fe2 03 , i.e., iron oxide and tiny blue-colored dots and 15.22% of ferrite, cementite, and iron oxide were obtained, re-
of FeC3 (cementite). Similarly in Figs. 8(b and c), the ferrite phase spectively, from the 2.5 pH solution (Fig. 9). These results are
is prevalent in specimens of 0 and 2.5 pH [red color in (b) and green found in agreement to the XRF results, which also showed a similar
in (c), respectively]. trend of Fe (ferrite) reduction due to the corrosion process when