IBP1292_19

CHARACTERIZATION BY NON-DESTRUCTIVE
TECHNIQUES OF AISI 317L AUSTENITIC
STAINLESS STEEL AGED AT DIFFERENT
TEMPERATURES
Moacir C. da Silva1, Humberto N. Farneze 2, Juan M. Pardal3,
Leosdan F. Noris4, Sérgio S. M. Tavares5
Copyright 2019, Brazilian Petroleum, Gas and Biofuels Institute - IBP
This Technical Paper was prepared for presentation at the Rio Pipeline Conference and Exhibition 2019, held
between 03 and 05 of September, in Rio de Janeiro. This Technical Paper was selected for presentation by the
Technical Committee of the event according to the information contained in the final paper submitted by the
author(s). The organizers are not supposed to translate or correct the submitted papers. The material as it is
presented, does not necessarily represent Brazilian Petroleum, Gas and Biofuels Institute’ opinion, or that of its
Members or Representatives. Authors consent to the publication of this Technical Paper in the Rio Pipeline
Conference and Exhibition 2019.

Abstract

The austenitic stainless steels are corrosion resistance alloys with good mechanical properties,
mainly toughness at low temperatures. In this family stands out the AISI 317L steel due to its
greater resistance to localized corrosion when compared to traditional grades AISI 304L and
AISI 316L. Some applications of AISI 317L steel in oil refineries are clads, vessels, tubes,
valves and accessories whose service temperature can reach 450°C or higher. However,
microstructural changes in prolonged exposure above 450°C, promote the progressive
formation of intermetallic phases, causing embrittlement and deterioration of corrosion
resistance of metal. Thus, there will be a considerable decrease of the above-mentioned
properties, making attractive the application of non-destructive techniques that aim to
characterize the microstructure of this material. In this respect, this work evaluated the effects
of the microstructural changes produced in this material, when thermal
aged at 450°C, 550°C and 650°C for periods up to 400 hours, using non-destructive
techniques of electromagnetic measurements by use of feritscope and magnetic Barkhausen
noise conventional, being performed a comparative characterization of these inspection
techniques in order to correlate with the microstructural changes. The results of
electromagnetic measurements indicate reductions in the percentage of ferrite δ, with the
increase of temperature and period of thermal aging, converging with the microstructural
aspects presented under the analyzed conditions. These results will contribute to consolidate
the microstructural characterization by non-destructive techniques of this stainless steel
family, so that these techniques can be used in the quality control and inspection of pipes and
process equipments.

Keywords: AISI 317L, Non-destructive testing, Microstructural characterization.

______________________________
1
Mechanical Engineer - Master student of the Program in Mechanical Engineering and Materials Technology of
CEFET / RJ
2
Doctor of Mechanical Engineering – DEMEC / CEFET / RJ
3
Doctor of Mechanical Engineering – TEM / UFF
4
Doctoral student in Mechanical Engineering – PGMEC / UFF
5
Doctor of Materials and Metallurgical Engineering – TEM / UFF
 Rio Pipeline Conference and Exhibition 2019

1. Introduction

Austenitic stainless steels form the largest group of stainless steels in use, accounting
for about 65 to 70% of the total produced. Among the properties that stand out in these types
of steels is the good mechanical and corrosion resistance at high temperatures, which allows
their use at temperatures considerably higher than the maximum service temperatures of low
alloy steels or martensitic and ferritic stainless steels. These characteristics are mainly
achieved in austenitic stainless steels alloyed with Mo or Si (Mcguide, 2008).
AISI 317L austenitic steel, which has a carbon content limited to 0.03% and Mo
content between 3.00 and 4.00%, is required due to its better resistance to creep and
naphthenic corrosion when compared to other classes of austenitic stainless steels (Yae Kina
et al., 2008). Currently, AISI 317L is being used extensively in petroleum refineries, having
wide application in the manufacture of tubes, pressure vessels, valves and clad coatings. For
some of these applications, the service temperature can reach 450°C or higher.
Despite of the inherent qualities of AISI 317L steel, its use in the process industry
encounters metallurgical problems, due to changes in microstructure caused by high
temperatures, together with the precipitation of deleterious intermetallic phases, such as sigma
(σ) and chi (χ), leading to the degradation of the properties of this material, especially in
applications exposed to high service temperatures (Villanueva et al., 2006, Eckstein et al.,
2011).
The use of non-destructive characterization, determining the presence of deleterious
phases, is of great use for the evaluation of the integrity of this material, since the results of
the segregation and precipitation processes, mainly the submicroscopic phases can be detected
by such techniques (O'Sullivan et al., 2004; Vértesy et al., 2005).
Thus, is relevant to seek a better orientation on the integrity of AISI 317L steel when
subjected to high temperatures, through the application of non-destructive techniques such as
electromagnetic measurements and to correlate them with analysis by microscopy techniques,
contributing to a better consolidation of the use of this steel in equipment and components
applied in the petroleum industry.

2. Materials and Methods

For the development of this research, samples of AISI 317L austenitic stainless steel
were used. Table 1 shows the chemical composition of the stainless steel studied, according to
the manufacturer's data.

Table 1. Chemical composition of AISI 317L steel (wt.%).

Material C Mn Si S P Cr Ni Mo
AISI 317L 0.024 1.34 0.47 0.003 0.031 18.13 11.41 3.02

The thermal aging was carried out in a muffle furnace at temperatures of 450°C (E4),
550°C (E5) and 650°C (E6), for periods of 200 hours (E42, E52, E53), 300 hours (E43, E53,
E63) and 400 hours (E44, E54, E64) for each temperature condition, with subsequent cooling
in water. It is emphasized that these conditions were compared to the condition of the “as-
received” (AR) sample, that is, without aging treatment. Aging was carried out at these
temperatures because they can be achieved in some applications of AISI 317L steel.

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The microstructures were analyzed by scanning electron microscopy (SEM) and X-ray
dispersive energy (EDS) spectroscopy. To reveal the microstructural characteristics, the
chemical attack with the Behara's reagent (20ml HCl + 80 ml H2O + 0.3g potassium
metabissulfite) was used. Due to the small dimensions of the intermetallic phases present, the
results obtained by energy dispersive X-ray spectroscopy (EDS) are considered as qualitative.
Non-destructive microstructural characterizations based on electromagnetic measurements
were performed using the Helmut Fisher® feritscope, which is based on the magnetic
permeability of the ferritic phase, and by measurements of Magnetic Barkhausen Noise
(MBN), using a portable device called "BarkTech" (Helmut Fisher, 2018; DENG et al., 2018;
Noris et al. 2018). Figure 1 shows the main components of this equipment. The measurements
were made by using a sinusoidal magnetic wave of 40Hz, an excitation amplitude of 3.5 A.
The reel reader was responsible for the detection of the MBN signal. The MBN sensor output
was amplified and band pass filtered (1 to 150 kHz). In order to reduce environmental noise,
the magnetizing yoke, reel reader and samples were placed in a grounded copper box.
Constructed by winding wire around a small cylindrical plastic bobbin, the reel reader
measured the normal component of the MBN signal (Noris et al., 2018; Harter and Grijalba,
2013).

Figure 1. Experimental setup for acquisition of MBN. (Noris, et al., 2019).

3. Results and Discussion

Figure 2 shows the microstructural aspect of the AISI 317L, observed by scanning
electron microscopy (SEM), in the “as-received” (AR) condition, in the mode of secondary
electrons (SE), using the Behara reagent to reveal the δ-ferrite and γ-austenite. Table 2 shows
the chemical composition, obtained qualitatively by microanalysis, through EDS, from the
reference points indicated in Figure 2. It is observed that in the “as-received” condition, the
microstructure of the base metal consists of γ-austenite and δ-ferrite, free from the
precipitation of intermetallic phases (IP).

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Figure 2. Microstructural aspect of the study material in the AR condition observed by SEM. Attack: Behara.

Table 2. Chemical composition of the phases identified by EDS in Figure 3 (wt.%).

Points Fe Cr Ni Mo Mn Si Phase
1 64.84 18.49 10.56 3.75 1.54 0.82 γ
2 63.90 19.92 9.13 4.85 1.52 0.68 δ
3 63.20 23.58 6.53 3.94 1.31 1.40 δ

Microstructural aspects obtained by SEM of the samples aged at 450°C, 550°C and
650°C during the 400h period are shown in Figures 3 (a-c), respectively. Tables 3, 4 and 5
show the chemical composition, obtained qualitatively by microanalysis, through EDS, from
the reference points indicated in Figures 4 (a-c).
In the sample aged at 450ºC, the γ-austenite and δ-ferrite phases (points 1 and 3), and
the presence of intermetallic phases (IP) inside the δ-ferrite are observed. The analysis by
EDS, presented in Table 3, indicates the possible existence of differentiated regions,
considering the presence of higher levels of Cr and Mo (points 2 and 4) in relation to the
matrix γ. It is also visible the decomposition of δ-ferrite in very fine precipitates. The analysis
of the sample treated at 550ºC shows a growth of the intermetallic phase inside the δ-ferrite
(point 3), occurring an increase of the Mo content (Table 4) in relation to the results found in
the sample aged by 450ºC. This fact is due to the effect of temperature increase, leading to the
growth of the diffusion rate of Mo in δ-ferrite (Villanueva et al., 2006, Escriba et al., 2007).
The microstructure observed in the sample aged at 650°C shows a great evolution of
the intermetallic phases (IP) in δ-ferrite (point 2), leading to an almost complete
decomposition of δ-ferrite, by virtue of a drastic reduction of the ferritic regions (point 3).

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(a) (b)

(c)
Figure 3. Images obtained by MEV from the microstructure of the study material thermally aged for 400 h. (a)
450°C, (b) 550°C and (c) 650°C. Attack: Behara.

Table 3. Chemical composition of the phases identified by EDS in Figure 3 (a) (wt.%).

Points Fe Cr Ni Mo Mn Si Phase
1 65.62 18.29 10.25 3.65 1.40 0.79 γ
2 62.52 23.23 6.09 6.09 1.19 0.88 IP
3 64.04 20.49 8.25 4.86 1.47 0.89 δ
4 64.41 21.62 7.00 5.08 1.33 0.58 IP

Table 4. Chemical composition of the phases identified by EDS in Figure 3 (b) (wt.%).

Points Fe Cr Ni Mo Mn Si Phase
1 66.19 18.01 11.20 2.54 1.32 0.74 γ
2 63.97 23.69 5.84 4.86 1.18 0.46 δ
3 60.16 22.47 6.12 8.94 1.27 1.05 IP

Table 5. Chemical composition of the phases identified by EDS in Figure 3 (c) (wt.%).

Points Fe Cr Ni Mo Mn Si Phase
1 66.53 18.34 10.18 3.01 1.40 0.54 γ
2 59.63 27.32 3.90 7.21 1.00 0.93 IP
3 63.25 26.77 4.41 3.63 1.68 0.26 δ
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Figure 4 shows the variation of the δ-ferrite content of the base metal with the aging
time at the temperatures of 450°C, 550°C and 650°C as measured by the feritscope. It is
observed the reduction of δ-ferrite content due to the precipitation of intermetallic phases with
increasing temperature and aging time. These phases are paramagnetic and modify the
magnetic permeability of the material. The highest variation is observed at the temperature of
650ºC, in agreement with the microstructural aspect presented in Figure 3 (c).

Figure 4. Variation of the δ-ferrite content of the AISI317L steel with aging time at 450ºC, 550ºC and 650ºC.

It is observed in Figure 5 the results of the measurements found from the Magnetic
Barkhausen Noise (MBN) measurements, establishing a relation between RMS (V) and the
thermal aging conditions. It is possible to verify the drop of the RMS signal of Magnetic
Barkhausen Noise (RMSMBN) with the increase of the temperature and time of aging. This
occurrence is associated to the possible decomposition of δ-ferrite and the precipitation of
paramagnetic intermetallic phases, which may correspond to sigma (σ), chi (χ) and M23C6
carbide, converging with the results presented by the measurements performed with the
feritscope (Hualpa et al., 2016).
A small rise of the RMS (V) signal of E42 sample in relation to AR sample is
observed, the peak value of RMS (V) may be associated with the possible precipitation of the
α' phase, which is ferromagnetic. The presence of α' phase suggests the occurrence of the
embrittlement phenomenon at 475ºC, which is more common in duplex stainless steels and
ferritic steels, in the temperature range between 300ºC and 550ºC (Lo et al., 2009).
Microstructural aspect by SEM of the sample aged at 450°C during the 200h period is
shown in Figure 6. Table 6 shows the chemical composition, obtained qualitatively by
microanalysis, through EDS, from the reference points indicated in Figure. It is observed that
the intermetallic phases (IP), compared to the EDS results of Figure 6, have higher levels of
Cr and Mo, indicating that these phases can correspond to the α' e and chi (χ) phases (Farneze
et al., 2017).

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Figure 5. RMS values of the samples analyzed.

.

Figure 6. Images obtained by MEV of the microstructure of the study material thermally aged at 450°C for
200h. Attack: Behara.

Table 6. Chemical composition of the phases identified by EDS in Figure 6 (wt.%).

Points Fe Cr Ni Mo Mn Si Phase
1 65.13 18.08 11.54 3.23 1.30 0.72 γ
2 62.69 22.99 6.01 6.30 1.17 0.56 IP
3 62.50 23.15 6.50 6.08 1.23 0.49 IP

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4. Conclusions

The aim of the present study was to evaluate the effects of microstructural changes
produced on AISI 317L stainless steel when aged at 450°C, 550°C and 650°C for periods of
up to 400 hours using non-destructive techniques through electromagnetic measurements,
revealed that:
- The variations of the δ-ferrite contents, measured in the feritscope, indicate the percentage
reduction of δ-ferrite due to the precipitation of intermetallic phases (IP) with increasing
temperature and aging time.
- The decrease in the value of RMS (V) is related to the lower δ-ferrite content, the reduction
would also be associated to the precipitation of paramagnetic intermetallic phases (IP), such
as chi (χ), sigma (σ) and M23C6 carbide, converging with the results obtained by SEM.
- The peak value of RMS (V), observed in E42 sample, may be associated with the possible
precipitation of the α' phase which is ferromagnetic.
- Magnetic measurements through the use of the Barkhausen Magnetic Noise technique and
the feritscope as a non-destructive evaluation were relevant as complementary analyzes, in
order to have a more accurate interpretation of the microstructure existing in each condition
analyzed, showing the possible use of these techniques for analysis of pipes and process
equipments manufactured in austenitic stainless steels.

5. Acknowledgments

The authors thank the Institutions for the support provided in the execution of this
work: To the INT - National Institute of Technology for the experimental support; CAPES,
CNPq for financial support.

6. References

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