Professional Documents
Culture Documents
October 2016
Pages 151-161
Acoustic Emission Techniques in Corrosion Monitoring
Summary
Fe C Mn Si P S Cr Ni
0.00
Balance 0.13 0.43 0.29 0.02 1 12.18 0.21
•
Acoustic Emission Techniques in Corrosion Monitoring
Specimens tested in open circuit potential condition under tensile stress
by means of a dead weight type machine.
𝜎
𝑡𝑒𝑛𝑠𝑖𝑙𝑒 = 80% of 0.2% Yield Stress .
Experimental Method
• The open circuit potential of the specimens after 5 min from immersion was
measured at approximately −0.600 VAg/AgCl.
• At the end of the test the open circuit potential was more anodic and stabilized at
approximately −0.540 VAg/AgCl.
Acoustic Emission Techniques in Corrosion Monitoring
• Acoustic emission signals were recorded by a 10-channel Vallen AMSY-5 measurement system for duration
of the experiment.
• The AE sensors were VS150-M type piezoelectric transducers suitable for metal integrity
testing operating within the 100–450 kHz frequency range with resonance at 150 kHz.
Thresholds of amplitude and rise-time parameters were set at 26.7 dB and 0.4 μs
respectively.
The rearm time was fixed at 3.2 ms.
The duration discrimination time was set at 400 μs,
The amplification was set at 34 dB with a bandwidth (−3 dB) from 2.5 kHz to 1 MHz.
• Several experimentations were performed under the described condition, showing similar
outcomes; however, the results of only a few experiments were reported.
• Several experiments were intentionally stopped after 200–250 h in order to evaluate the
extension of corrosion damage at an intermediate stage .
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• Pitting corrosion was observed on the stainless steel sample under tensile load.
Experimental Results
End of Test
t = 250h
(Failure)
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• AE monitoring allowed to distinguish different damage mechanisms
characterized by specific AE parameters.
Cumulative AE hits plot versus time evidencing the quiescence phase between 200 and 300 h.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• Hit duration, hit rise time, burst average frequency, crack index and hit
energy were identified as the most relevant parameters in damage
mechanism identification.
• FeS scale build up and hydrogen evolutions were the most energetic
AE sources during the first stage of corrosion test.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• Localization of AE events
along specimen length vs
time. Position values were
calculated starting from the
top AE sensor.
Experimental Results
Bubble diameters and bubble colour code refer to d) hit average frequency
normalized values; (e) hit crack-index normalized values.
Acoustic Emission Techniques in Corrosion Monitoring
Conclusions
• Higher duration and energy hits have been related to crack opening
mechanisms anticipating the final failure.
Acoustic Emission Techniques in Corrosion Monitoring
September 2016
Summary
• Current density and applied load were monitored during corrosion tests.
• Austentitic stainless AISI 304L steel rods with a diameter = 6 mm and an
active length = 40 mm.
• Steel wires were chosen to allow comparison with results from AE literature.
Acoustic Emission Techniques in Corrosion Monitoring
Materials
• Silicon carbide paper was used to wet grind all specimens up to 4000 grit ,
before specimens were cleaned with de-ionized water and then rinsed
with acetone.
• A stress ring was used to perform stress corrosion cracking, consisting of a tensile strength
apparatus that facilitated a fixed tensile load.
• The tensile stress applied by the stress ring in the beginning of the test is
fixed at .
• Electrochemical tests were carried out using a Parstat 2273 potentiostat equipped with a frequency
response analyser.
• A settling time of 15 min was observed to allow stabilisation of the open circuit potential prior to
straining. Samples were then exposed at the desired potential, waiting for the currents to reach stability.
During the experiment, the current and load evolution was recorded until sample failure occurred.
• After each CSCC test, both the corroded surfaces and the fracture surfaces were observed by optical
microscopy and SEM.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Method: Acoustic Emission Setup
• The transducers used were resonant R15D type from PAC (Piezo-electric disks), which have high
sensitivity suitable for metal integrity testing, operating in a bandwidth of 20–1000 kHz.
• The acquisition system was computer-controlled by a computer, with the waveforms and the
characteristic acoustic parameters (events, amplitude, rise time, counts number, duration) were
computer-controlled upon detected. The obtained signals were analyzed with Noesis™ 5.0
software
Experimental Results
• The analysis and classification of signals shows that the amplitude and rise time are the most relevant
parameters of the acoustic signature associated with this damage phenomenon.
• The coupling of acoustic emission and electrochemical measurements revealed a good correlation
between acoustic activity and corrosion and made it possible to characterize the degradation of the
material.
• The results of the novel accelerated test carried out on AISI 304L show the presence of various stages
of corrosion as in conventional accelerated CSCC tests, that can lead to the validation of this novel
laboratory test.
• The study of current density and of stress evolution during CSCC tests confirms the presence of
various stages in the corrosion process.
• Microscopic observations show that rupture propagation begins in mode I and evolves towards a
mixed I–II mode before failure.
• The stress evolution during the test can be linked to the current density evolution. The various stages
observed in the curves are due to the creation of pitting initiation sites, and to the pits and cracks
propagation.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
Evolution of the amplitude of the AE signals as a function of time in 3 wt% NaCl at 60 °C for a steel wire
stretched to 80% of UTS.
Acoustic Emission Techniques in Corrosion Monitoring
Evolution of acoustic activity and current density (above) and Amplitude in dB (below) during immersion in 3 wt% NaCl at 60 °C for a
steel wire stretched to 80% of UTS
Acoustic Emission Techniques in Corrosion Monitoring
• Typical AE waveforms associated with stages:
I (a)
II (b)
III (c)
breakdown (d)
Evolution of the amplitude of the AE signals as a function of time in 3 wt% NaCl at 60 °C
Acoustic Emission Techniques in Corrosion Monitoring
Conclusions
• The analysis and classification of signals showed that the amplitude and rise time
are the most relevant parameters of the acoustic signature associated with this
damage phenomenon. The coupling of acoustic emission and electrochemical
measurements revealed a good correlation between acoustic activity and corrosion
and made it possible to characterize the degradation of the material.
Acoustic Emission Techniques in Corrosion Monitoring
April 2016
Pages 8-16
Acoustic Emission Techniques in Corrosion Monitoring
Summary
• Kaige et al. analysed acoustic emission (AE) energy to monitor the pitting
process on a vertically positioned 304-stainless steel.
• Two AE clusters with different energy levels were suggested from a scatter plot of
the duration and energy.
• Hydrogen bubble evolution and pit covers rupturing were separately monitored by
AE.
• An in-situ analysis of the AE energy evolution provided thorough insight into the
corrosion process vis-à-vis the specimen position.
Acoustic Emission Techniques in Corrosion Monitoring
Materials and specimen preparation
• A commercial sheet of 304 stainless steel was used for this investigation, of the following
composition:
0.07 mass% C, 0.55 mass% Si, 2.00 mass% Mn, 18.19 mass% Cr, 8.07 mass% Ni,
0.02 mass% P, and 0.03 mass% S.
• The specimens’ dimensions were 75 mm × 15 mm × 2 mm and all were wet-ground using
up to No. 1500 sand paper, followed by polishing from 6 to 1 μm using a diamond gel.
• The surface of each specimen was masked with tape (3 M electroplating/anodizing Tape
484 L) so as to provide a desired exposed surface area of 12 mm × 12 mm.
• To prevent crevice corrosion, a fast-curing epoxy was applied to expose a surface area of
10 mm × 10 mm
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Procedure
• A salt bridge was utilised to eliminate the effect of the H2 gas bubbling on the
counter electrode during the test via placing the counter electrode in a neighbouring
corrosion test cell.
• The AE signal and various parameters were collected using an acquisition device.
• An anodic polarization using the potentiodynamic method was applied to control the
pitting corrosion process at room temperature.
• Scanning electron microscopy was used to inspect the pit morphology before and
after the corrosion testing.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• Integrated pit morphologies of
the specimens after the anodic
polarization testing in (a) the low-
and (b) high-concentration
solutions.
Experimental Results
Experimental Results
Experimental Results
• Typical AE waveforms for the low- and high-energy clusters detected
during the tests in different solutions are shown.
• Therefore, the signals from the pitting corrosion in the 0.5 mass%
NaCl solution shared the same source as the low-energy signals from
the pitting corrosion in the 2.5 mass% NaCl solution .
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• To identify the AE source and match the
detected AE signals to the different
pitting stages, the AE signals of the low-
and high-energy clusters in the 2.5
mass% NaCl solution were tracked
separately.
Experimental Results
• AE stage I: the period of the time
delay.
Experimental Results
Conclusions
1. The pitting shape on vertically positioned 304 SS electrodes was asymmetric and elongated under the
disturbance of gravity. AE signals were detected a short time after the pitting commenced. The AE
signals signals increased as the pitting progressed.
2. Two clusters of AE signals were detected based on the absolute energy. The AE signals of the
low-energy cluster (0.031–6.46 × 10−18 J) were predominantly continuous signals, whereas those of
the high-energy clusters (7.93–11.50 × 10−18 J) were predominantly burst signals.
3. The low-energy signals were believed to originate from the hydrogen-bubble evolution inside the pits,
and the high-energy signals were attributed to the rupturing of the pit covers during the pit growth.
4. The AE parameter of absolute energy seemed to effectively classify different pitting steps. The
correlation between the AE signals and pitting progress for a vertically positioned specimen was well
founded based on separately monitoring the low- and high-energy AE signals. Thus, the potential of
the in-situ evaluation of the pitting mechanism by monitoring the AE-energy was verified.
Acoustic Emission Techniques in Corrosion Monitoring
Detection and characterization of stainless steel SCC by the analysis of crack related ac
oustic emission
Jaka Kovač, Andraž Legat, Bojan Zajec, Tadeja Kosec and Edvard Govekar
Ultrasonics, Volume 62
September 2015
Summary
• In the paper the results of the acoustic emission (AE) based detection and characterization of stress-
corrosion cracking (SCC) in stainless steel are presented.
• Based on the defined qualitative and quantitative time and power spectra characteristics of the AE
bursts, a manual and an automatic procedure for the detection of crack related AE bursts were
introduced.
• The results of the analysis of the crack related AE bursts indicate that the AE method is capable of
detecting large scale cracks, where, apart from intergranular crack propagation, also some small
ductile fractures occur.
• The sizes of the corresponding ductile fracture areas can be estimated based on a relative
comparison of the energies of the detected AE bursts. It has also been shown that AE burst time and
power spectra features can be successfully used for the automatic detection of SCC.
Acoustic Emission Techniques in Corrosion Monitoring
Materials and specimen preparation
• The specimens were made of austenitic stainless steel of type AISI 304.
• The plates had a thickness of 2 mm, and were 12 mm wide and 280 mm long. For the purpose of crack
initiation and location, they had semi-circular notches with a radius 8 mm at the mid-length.
• The distance between the notch centre and the centre of each AE sensor was approximately 100 mm.
The material was sensitised prior to specimen production in order to increase the susceptibility of the
material to intergranular stress corrosion cracking.
• For this purpose the steel was heated to 1050 °C in a vacuum, maintained at this temperature for 1 h,
and then quenched in oil. It was then re-heated to 650 °C in a vacuum, maintained at this temperature
for 24 h, and cooled down to room temperature in the open air.
Acoustic Emission Techniques in Corrosion Monitoring
Materials and specimen preparation
• The obtained microstructure of the material was austenitic, with no dominant orientation of the crystal
structure, after sensitisation.
• The yield stress of the tested material was determined to be 230 MPa; the ultimate tensile stress was
650 MPa.
• In order to develop to intergranular stress corrosion cracking, the specimen was sealed inside the
corrosion cell, which was filled with an aqueous solution of 0.5 M sodium thiosulphate (Na2S2O3) at
20 °C.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Procedure
• The corrosion cell, shown opposite, was
designed for the detection of AE during SCC
degradation processes on the specimen.
Experimental Procedure
• The sensors were fixed in a symmetrical
fashion to the semi-circular notch out of the
corrosion cell, one to the top and the other to
the bottom of the specimen, Amplification of
the detected signals was set to 40 dB.
Experimental Procedure
• For a comprehensive SCC characterisation
and interpretation of SCC-related AE signals,
the corrosion cell was equipped with a set of
two auxiliary reference electrodes for
electrochemical noise (EN) measurements.
Experimental Procedure
Experimental Procedure
Experimental Procedure
• The performed experiments, with the applied load levels expressed as a percentage of the specimens’
tensile strength, are shown here:
List of the performed experiments, the applied load levels, and the time of the specimen failure.
Experimental Results
• Examples of different detected AE
signals detected:
Experimental Results
• Frequency Spectra:
Experimental Results
• AE bursts were presumed to have been caused by events related to SCC and
were hence selected to analyse and characterise the SSC process.
Experimental Results
• The left branch of the block • The right branch of the
diagram presents manual block diagram an
filtering of the AE signals, automatic, a method for AE
based on the visually signal amplitude and
observed AE waveform average frequency based
characteristics. filtering is presented.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
Experimental Results
e) Energy.
f) Duration.
g) Average frequency.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
Experimental Results
• Analysis showed that the fracture surface of the specimen was approximately 60% predominantly
intergranular, caused by SCC (a).
• The rest of the final fracture surface was ductile, caused by overloading of the specimen due to the
reduced cross-section.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• In the predominantly intergranular part of the fracture surface some small ductile areas were also observed (b).
• It was suggested that these areas developed due to the ductile fracture of ligaments which stayed behind the
intergranular advancing crack tip, at more resistant grain boundaries.
• There was indication that these AE signals could be related to the ductile fracture process , as the number of small
ductile areas observed were roughly the same as the number of AE signals detected during the post filtering
procedure.
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• The energy of the detected AE signals EAE was used for estimation of the size of the ductile
fracture area.
• In the case of considered herein, the average energy of the AE signals was estimated to be 1.2
10−1 pJ.
• The sum of the energy of all the AE signals captured during specimen failure was approximately
1 nJ.
• The size of the ductile area of the final fracture surface was estimated to be 3 mm 2 – taken from
the SEM analysis of the fracture surface.
• The average size of an individual ductile fracture area was then estimated as:
Acoustic Emission Techniques in Corrosion Monitoring
Experimental Results
• This estimate was in approximate agreement with the sizes of individual ductile
areas observed by SEM analysis.
• The average size of an individual ductile fracture area was estimated as between
1 x 10−4 mm 2 to 1 x 10−3 mm 2.
• Thus, the results demonstrated the ability to use AE to estimate the size of the
ductile fracture areas.
Acoustic Emission Techniques in Corrosion Monitoring
Conclusions
• It was shown that there are noteworthy differences between the characteristics of SCC
related and crack non related AE signals, apparent in the waveforms and in the
corresponding power spectra characteristics of the detected AE signals.
• Analysis of the SCC-related AE signals showed that the AE method is able to detect larger
cracks in the case when some small ductile fractures also occur (not including intergranular
propagation). It was shown that these ductile fractures are the source of the detected
acoustics emission waves.
• The size of corresponding ductile fracture area can be estimated based on a relative
comparison of the energies of the detected AE signal.
• Based on the presented results it can be concluded that AE can be successfully used for
SCC detection and characterization in the later phase of this process.