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A1 Paper Revised Materials Characterization
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Abstract
The entrainment of the surface oxide layer of aluminum alloy melts is currently a mostly
inevitable process during the melt handling and processing techniques of the foundry industry.
As a consequence, a large number of double oxide films (bifilms) are often incorporated into
the melts, which bifilms can act as initiation sites for pore formation during the solidification
of the alloy. In this study, this relationship between bifilms and pores was examined in the
case of an Al-Si-Mg-Cu based alloy. The entrained oxide film content of the melts was
measurement and X-ray computed tomography (CT) of reduced pressure test (RPT) samples,
which can be considered as a new method of melt quality characterization. It was found that
the number of oxide films found on the fracture surfaces of K-mold specimens is proportional
to the number density of pores found in RPT samples. Investigations with scanning electron
microscopy (SEM) revealed that oxide films can be found on the inner surface of the pores in
RPT samples, which confirms the theory, that pores and bifilms are interconnected
phenomenon. Based on the results, the bifilm content and so the quality of aluminum melts
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
1. Introduction
Aluminum casting alloys are widely used in automotive and aerospace industries for their
high strength to weight ratio, good castability and excellent corrosion resistance [1-3].
fatigue life, etc.) of cast parts, the number of structural defects like porosity and inclusions
must be minimized [4-8]. Porosity is one of the most common defects, which can lead to
inadequate mechanical properties and premature failure of cast parts. In the case of aluminum
and the rejection of dissolved hydrogen during the solidification of the alloy [9, 10]. However,
it was proposed by Campbell [11], that double oxide films (bifilms) take a central role in pore
formation as they can easily open up and inflate into pores due to hydrogen diffusion into
their inner atmosphere and pressure drop in the mushy zone caused by the volumetric
shrinkage during solidification (Fig. 1). This hypothesis is supported by experimental results
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Bifilm formation during the melt handling and processing techniques of aluminum alloys is
mostly an unavoidable process as any disturbance of the melt surface leads to the entrainment
of the surface oxide layer. In this way, numerous bifilms are introduced to the melts during
common foundry activities like melting, alloying, fluxing and pouring [25-27]. In order to
produce high-quality castings, it is essential to assess and control the melt quality. The
determination of the bifilm content of melts is an important but especially hard task since
oxide films are usually extremely thin (often a few nanometers in thickness) [11, 26].
However, as revealed by Fox and Campbell [28, 29], reduced pressure test (RPT) can be an
effective tool in the assessment of melt quality. During solidification under reduced pressure,
the entrained air between the oxide layers is expanded [12]. Besides that, due to a lower
partial pressure, the solubility of hydrogen in the metal is lower and the H2 precipitation
process inside the bifilms is accelerated [30]. In this way, the bifilms inside RPT samples are
expanded and they can be more easily detected by X-ray radiography or quantitative image
analysis on a polished section [31]. Dispinar and Campbell [32] introduced a metric called the
Bifilm Index (BI) which can be used to quantify the bifilm content of the molten metal based
on the length of pores found on the polished section of RPT samples. However, the BI value
is only based on one section of the RPT sample, thus the spatial distribution of bifilms inside
the samples cannot be characterized with it. Besides that, the bifilm index values have a
significant degree of variation, therefore several RPT samples need to be analyzed to get
In order to address these issues, during our investigations, besides BI measurements, the
bifilm quantity of different melts was characterized by computed tomography (CT) of RPT
samples, which method can be used to characterize the full volume of the given sample
instead of only one section. The aim of this study was to investigate the described relationship
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
between bifilms and pores, as well as to get information about the possible utilization of it in
2. Experimental
2.1 Materials
During our experiments, an Al-Si-Mg-Cu casting alloy was used, which is widely used in
the automotive industry for cylinder head castings (A356 alloy with an additional 0.5 % Cu).
Si Fe Cu Mn Mg Ti Sr
6.5 - 7.5 < 0.2 0.45 - 0.58 < 0.1 0.36 - 0.45 < 0.2 0.017 - 0.030
Melt treatments consisting of rotary degassing with N2 gas and flux addition were executed
on the alloy melts using two different fluxes (A and B), which are commercially available
granular fluxes. Based on previously made X-ray powder diffraction measurements, Flux A
mainly consists of NaCl, Na2SO4, and CaF2, the identified components of flux B are KCl,
CaF2, K2SiF6, and Ca3Al2(SiO4)3. Each flux was used in 3 treatment cycles. The quantity of
metal treated in one cycle was approximately 1000 kg. The metal was melted in a stack
smelter then transported by a transport ladle to a resistance heated holding furnace where the
melt treatments were performed (Fig. 2). The treatment parameters and the quantity of flux
added (400 g) were the same in each cycle. The N2 gas flow rate was 20 L/min; the rotor
revolution was 500 RPM during vortex formation and 250 RPM in the degassing phase. The
treatment time was 10 minutes in each case. The molten metal temperature in the holding
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 2. The stages of melt preparation: (a) pouring from melting furnace, (b) melt transport to
2.2 Methods
The bifilm content of the melts was investigated by the evaluation of K-mold specimens
and X-ray computed tomography (CT) of reduced pressure test (RPT) samples. The K-mold
specimen itself is a flat plate with four notches that act as fracture points (Fig. 3 (a)). The
fracture surface of samples (such as the ones in Fig. 3 (b) and (c)) can be examined either by
Fig. 3. (a) K-mold sample, (b) fracture surfaces indicating good and (c) poor melt quality
Based on the number of inclusions found on the fracture surfaces, a K-value can be
determined which can be used for the quantitative characterization of the melt purity (Eq. 1).
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
𝑆
𝐾= (1)
𝑛
where 𝐾 is the K-mold value (dimensionless number), 𝑛 is the number of examined fracture
surfaces, and 𝑆 is the total number of inclusions found in 𝑛 pieces [33]. During each melt
preparation, specimens were cast two times. Samples were prepared from the melt in the
holding furnace before and after the melt treatment. At each sampling step, 5 K-mold and 1
RPT specimens were cast. The fracture surface of K-mold specimens was inspected with a
For the casting of RPT samples, steel cups preheated to 200 °C were used. The specimens
stayed in the vacuum chamber of the RPT machine at 80 mbar pressure for 6 minutes. The
porosity analysis of RPT samples was executed with computed tomography (CT). The
radiographic images were made with GE Seifert X-Cube Compact 225kV apparatus, the
acceleration voltage was 135 kV, the tube current was 0.8 mA. During one rotation of the
samples, 900 images were acquired. The image reconstruction and processing were conducted
dimensional geometry of an analyzed sample and three different sections of the same
Fig. 4. CT section of an RPT sample in (a) the xy, (b) the xz and (c) the yz planes, (d) shows
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
For the detection of pores, the VGDefX algorithm was used which is a part of the porosity
analysis module of the software. Based on the grey level of the voxels, which is proportional
to the local rate of attenuation of X-rays, the algorithm decides which voxels represent the
material and which of them corresponds to porosity defects. For each pore, a probability value
is determined which depends on the local contrast (the difference between the grey level of
voxels). During the analysis objects with a volume smaller than 0.05 mm3 and pores with a
probability value lower than 0.9 were ignored. The visual representation of the results of
porosity analysis conducted on the sample shown in Fig. 4 can be seen in Fig. 5. Based on the
results of the CT analysis, the volume fraction and total surface area of pores, as well as the
volumetric pore density (which is expressed in mm-3, and refers to the number of pores found
Fig. 5. (a-c) CT sections and (d) volumetric view of an RPT sample with the detected pores
After CT analysis, the samples were cut in half and were ground with SiC grinding papers
with a grit size of 80, 120, 180 and 240 (with average grain sizes of 201, 125, 82 and 58.5 μm,
respectively). A scanner was used to scan the cross-section of the samples at 600 dpi. After
contrast and brightness enhancement, the scans were converted to 8-bit greyscale images.
After that, image analysis was executed with MATLAB® Image Processing ToolboxTM
software. The segmentation of pores was realized based on the grey level of pixels. In order to
avoid the detection of noise and imperfections of the images, individual objects with an area
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
smaller than 0.05 mm2 were not considered. The sum of the maximum length of pores was
𝐵𝐼 = ∑ 𝐿𝑚𝑎𝑥 (2)
where 𝐵𝐼 is the Bifilm-Index [mm] and 𝐿𝑚𝑎𝑥 is the maximum length (major axis length) of
pores [mm]. Besides BI, the areal number density of pores was also determined for each
sample. For this purpose, during another image analysis step, the cross-sectional area of the
RPT specimens was also determined. The inner surface of pores found in the RPT samples
was investigated with Zeiss EVO MA 10 scanning electron microscope (SEM) equipped with
The results of the K-value evaluation are shown in Fig. 6, and some examples of inclusions
Fig. 6. Average K-values determined before and following the melt treatments
As can be seen in Fig. 6, each treatment resulted in the reduction of the K-values, however,
a significant amount of inclusions could be found on the fracture surfaces, even after melt
treatments, so the melt quality was far from optimal in each case. Melt processing conducted
with flux A resulted in considerably lower average K-values, which indicates that flux A is
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 7. Two sides of bifilm defects found on the fracture surfaces of the K-mold samples
In each case, crumpled, creased, film-like inclusions were found on the fracture surfaces.
Generally, the two distinct layers of the bifilm defects could be distinguished on the opposing
fracture surfaces (Fig.7), which confirms the theory that bifilms are the most common
Fig. 8. shows two examples of the reconstructed three-dimensional view of the RPT
samples before and following the melt treatments, including the pores found within them
during CT analysis. As seen in Fig. 8, the spatial- and size distribution of pores inside the
RPT samples is significantly different before and after the treatments. The RPT specimens
cast previously to melt processing have evenly distributed relatively moderate-sized pores,
while the samples made following the treatments, on the other hand, have one central, large-
sized pore and numerous other small-sized pores throughout the whole volume of the
samples. The mentioned large-sized pores are obviously the results of shrinkage, which -
based on the CT images- has a strong effect on pore growth in the RPT samples cast after
melt treatments.
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 8. Reconstructed CT image of RPT samples cast before and after melt treatments
The average pore number density and pore volume fraction results determined following
Fig. 9. (a) Average volumetric pore number density and (b) pore volume fraction results
Based on the pore formation mechanism proposed by Campbell [11], the number of pores
found in the samples is about the same as the number of bifilms which can act as pore
initiation sites during solidification. In this way, the volumetric pore density can be used to
quantify the bifilms suspended in the molten metal. This is supported by the fact, that the
results shown in Fig. 9 (a) are highly similar to the results of the K-value evaluation shown in
Fig. 6; the treatments executed with both fluxes resulted in the reduction of pore density
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
values and thus, the bifilm quantity of the melt. The application of flux A however, can be
considered more effective regarding bifilm removal, since it resulted in a greater reduction of
pore density values than the treatments executed with flux B. Pore volume fraction, on the
other hand, gives information about the total size of the pores and thus, the ability of pores to
grow during solidification. Based on the results shown in Fig. 9 (b), it can be said, that the
pore volume fraction values were significantly decreased during melt processing, which is
certainly the result of effective solute hydrogen removal during the rotary degassing
treatments. Due to lower solute hydrogen concentration, the pores inside the RPT samples
taken after melt processing are small-sized except the central large-sized pores, which are the
results of shrinkage. Fig. 10 (a) shows the average values of the total pore surface area
determined with CT analysis. Considering the fact, that bifilms are expanded during the
solidification of RPT specimens, the total surface area of pores can be used as a good
approximation of the total bifilm area and thus, the area of unbounded interfaces present in
the melt. These unbounded interfaces are the initiation sites of pores, hot tears, and cracks
[34], in this way they heavily influence mechanical properties of cast parts, thus the total pore
surface area inside an RPT sample can be considered as an important metric of liquid metal
quality. The total pore surface area and pore volume fraction results follow the same tendency
as it is showed by the linear regression in Fig. 10 (b). Despite the relationship between the
mentioned quantities, it should be mentioned, that pore surface area can be considered as a
more critical factor which can alter the mechanical properties of cast parts since pores which
have the same volume can reduce the properties at a different degree depending on the shape
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 10. (a) Total pore surface area results and (b) the relationship between pore volume
The results of image analysis of the cross-section of RPT samples are shown in Fig. 11,
and two examples of the scanned images of samples cast before and after melt processing are
shown in Fig. 12. Both BI (Fig. 11 (a)) and areal pore number density values (Fig. 11 (b))
were excessively reduced due to melt treatments. As seen in Fig. 12, the RPT samples cast
following melt processing contain only a few, rather small-sized pores in the cross-sectional
area, which resulted in low BI and pore density values. In the case of treatments with flux B,
the average BI value achieved an exceptionally low BI value of 8, which refers to a high-
quality melt according to Uludaǧ et al. [35]. This clearly contradicts the results of the K-value
evaluation and CT analysis which suggested that the application of flux B results in worse
Fig. 11. (a) Average BI values and (b) areal pore number density results
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 12. Examples of cross-sectional images of RPT samples cast before and after melt
treatments
As it was mentioned above, the average K-values and the volumetric pore density values
determined by CT analysis are following the same tendency. This relationship is visualized by
the linear regression line in Fig. 13 (a). As it is represented by large error bars in the graph, K-
values have a large degree of variation, which is most likely the result of the non-uniform
spatial distribution of bifilms inside the melt. Despite the low coefficient of determination
(R2) of the linear regression, the relationship between K-values and pore density values
indisputably indicates that bifilm quantity is proportional to the pore density values
whether the results are influenced by the strong tendency to shrinkage driven pore growth in
the case of samples taken from a degassed melt (as can be seen in Fig. 8).
characterization of the bulk melt, which is obviously only an approximation. The accuracy of
this estimation can be determined from the comparison of areal and volumetric pore number
density values, which is shown in Fig. 13 (b). Based on the results, it can be said that the pore
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
number density values follow the linear tendency with a great extent of uncertainty (R2 value
of linear regression is only 0.57), which is the result of the non-uniform spatial distribution of
pores inside the RPT samples. In addition, characterization of the cross-sectional area can lead
to inaccurate results because of the fact that one pore can appear to be multiple separate pores
on a section.
Fig. 13. Comparison of (a) average K-values and volumetric pore number density results, (b)
the volumetric and areal pore number density values determined by CT and image analysis
According to Campbell [11], rotary degassing treatments are only effective in reducing the
solute hydrogen content and removing larger oxide film inclusions of aluminum alloy melts.
In this work, despite the fact, that fluxes were employed during melt treatments, it is evident
from the K-value and volumetric pore density results, that significant amount of bifilms
remained in the melts after the treatments, which could not be detected due to their small size
during the image analysis of the cross-section of RPT samples. As it was highlighted by
Riestra et al. [36], in the case of well-degassed melts, low BI values can be misleading, as, in
the absence of hydrogen, bifilms can only expand to a limited degree. In this way, because of
their small size, they cannot be detected during image analysis. This explains the relatively
low BI and areal pore number density values showed in Fig. 11 (a-b), which suggest that BI
measurement can give inaccurate results when the solute hydrogen concentration of the melt
is substantially low. Dispinar et al. [5, 37-39] carried out several comprehensive works about
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
the correlation between Bifilm Index and mechanical properties of cast parts, which clearly
prove that BI measurement is a valuable method of melt quality evaluation, which can aid in
the production of high-quality cast components. However, as reported in [5] and [32],
ultimate tensile strength and elongation to fracture results at lower BI values can scatter
significantly, which indicate that the sensitivity of the BI analysis to melt quality changes at
The results of BI evaluation were compared with pore volume fraction and total pore
Fig. 14. Comparison of BI values with (a) pore volume fraction and (b) total pore surface area
results
As can be seen in Fig. 14 (a), there is a strong relationship between BI and pore volume
fraction values. Uludaǧ et al. [35] also observed a direct correlation between BI and
volumetric porosity when the BI was higher than 50 mm. However, it is evident from the data
given in Fig. 14 (a), that the correlation is inaccurate at lower BI values. The same
interpretation can be made regarding the total pore surface area results, which are given in
Fig. 14 (b). This also suggests that at lower bifilm concentrations the accuracy of CT analysis
is better, than that of BI evaluation, as some presumably small-sized bifilms could be detected
with the aid of CT, and were taken into account during pore volume fraction and pore surface
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Besides solute hydrogen concentration and pressure drop due to shrinkage, there is another
important factor which can alter the ease of bifilm unfurling and inflation. The flexibility of
the parts of the oxide films can be significantly different from each other due to the
differences in the time available for the thickening of the sections of the oxide layers during
the oxidation process. As a result, bifilms have parts which inflate more easily because of the
thinness and flexibility of the oxide film. In contrast, other parts of the bifilms cannot open
significantly due to hydrogen diffusion and/or shrinkage, as the thick oxide films which form
these parts are rigid [11, 20, 27, 40]. This phenomenon has a significant effect on the shape of
pores, as can be seen in Fig. 15; some parts of the bifilm were excessively inflated during
solidification, while other parts could not open and expand due to the rigidity of the local
oxide film section. The described difficulties in unfurling and inflation of bifilms may be
another reason why volumetric pore number density and bifilm content do not appear to
Based on the pore formation mechanism illustrated in Fig. 1, it can be suggested that the
bifilms which act as pore initiation sites can be detected on the inner surface of the pores. This
is supported by the published experimental results [14-18] and the findings of the
investigations made by SEM during this research. Fig. 16 shows a pore found in the cross-
section of an RPT sample and the results of EDS analysis made in two separate areas. EDS
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
analysis was made on the base matrix of the alloy (Area 1) and on the inner surface of the
pore (Area 2). The oxygen concentration measured inside the pore is significantly higher,
which indicates that a relatively thick oxide layer covers the inner surface of the pore. The
oxygen concentration measured on Area 1 on the other hand, is substantially low, which
implies that only a thin oxide layer covers the base metal, which is the product of solid-state
oxidation.
Fig. 16. SEM image of pore found in an RPT sample and the results of EDS analysis
Besides higher oxygen concentration, at higher magnifications, wrinkles and creases could
be detected inside the investigated pores (as indicated by the arrows in Fig. 17), which are
additional signs of the presence of bifilms, as wrinkles and creases are common
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
4. Conclusion
In this study, the relationship between double oxide films and pore formation was
investigated in the case of an aluminum casting alloy. Based on the results, the following
• Computed tomography aided porosity analysis of RPT samples can be used for the
the quantity of entrained bifilms within the melt. Pore volume fraction, on the other hand,
gives information about the ability of bifilms to inflate into pores, while pore surface area
may be utilized in the determination of the total area of unbounded interfaces present in the
melts.
• In the case of well-degassed melts, Bifilm-Index and areal pore density determinations can
give inaccurate results, because at low solute hydrogen concentrations, small-sized bifilms,
which usually remain suspended in the melts after degassing treatments, cannot inflate to
sizes at which they can be easily detected during the image analysis of the cross-section of
RPT samples.
• With the aid of SEM, oxide films could be detected on the inner surface of pores within
RPT samples, which confirms the theory of bifilm initiated pore formation.
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Acknowledgments
The described study was carried out as part of the EFOP-3.6.1-16-2016-00011 “Younger and
framework of the Szechenyi 2020 program. The realization of this project is supported by the
The raw/processed data required to reproduce these findings cannot be shared at this time due
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Figure Captions
Fig. 2. The stages of melt preparation: (a) pouring from melting furnace, (b) melt transport to
Fig. 3. (a) K-mold sample, (b) fracture surfaces indicating good and (c) poor melt quality
Fig. 4. CT section of an RPT sample in (a) the xy, (b) the xz and (c) the yz planes, (d) shows
Fig. 5. (a-c) CT sections and (d) volumetric view of an RPT sample with the detected pores
Fig. 6. Average K-values determined before and following the melt treatments
Fig. 7. Two sides of bifilm defects found on the fracture surfaces of the K-mold samples
Fig. 8. Reconstructed CT image of RPT samples cast before and after melt treatments
Fig. 9. (a) Average volumetric pore number density and (b) pore volume fraction results
Fig. 10. (a) Average pore surface area results and (b) the relationship between pore volume
Fig. 11. (a) Average BI values and (b) areal pore number density results
Fig. 12. Examples of cross-sectional images of RPT samples cast before and after melt
treatments
Fig. 13. Comparison of (a) average K-values and volumetric pore number density results, (b)
the volumetric and areal pore number density values determined by CT and image
analysis
Fig. 14. Comparison of BI values with (a) pore volume fraction and (b) total pore surface area
results
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Materials Characterization Vol. 157. 2019. 109925. DOI: 10.1016/j.matchar.2019.109925
Fig. 16. SEM image of pore found in an RPT sample and the results of EDS analysis
Table Captions
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