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Nuclear Engineering and Technology 50 (2018) 724e730
Contents lists available at ScienceDirect
Nuclear Engineering and Technology
journal homepage: www.elsevier.com/locate/net
Original Article
Effect of CrN barrier on fuel-clad chemical interaction
Dongkyu Kim a, b, Kangsoo Lee b, **, Young Soo Yoon b, *
a
b
U.C. San Diego, Department of Mechanical and Aerospace Engineering, 9500 Gilman Dr, La Jolla, CA, 92093, USA
Gachon University, Department of Environment and Energy Engineering, Seongnamdaero 1342, Gyeonggi-do, 461-710, Republic of Korea
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 29 November 2017
Received in revised form
2 February 2018
Accepted 12 February 2018
Available online 28 March 2018
Chromium and chromium nitride were selected as potential barriers to prevent fuel-clad chemical
interaction (FCCI) between the cladding and the fuel material. In this study, ferritic/martensitic HT-9 steel
and misch metal were used to simulate the reaction between the cladding and fuel fission product,
respectively. Radio frequency magnetron sputtering was used to deposit Cr and CrN films onto the
cladding, and the gas flow rates of argon and nitrogen were fixed at certain values for each sample to
control the deposition rate and the crystal structure of the films. The samples were heated for 24 h at
933 K through the diffusion couple test, and considerable amount of interdiffusion (max. thickness:
550 mm) occurred at the interface between HT-9 and misch metal when the argon and nitrogen were
used individually. The elemental contents of misch metal were detected at the HT-9 through energy
dispersive X-ray spectroscopy due to the interdiffusion. However, the specimens that were sputtered by
mixed gases (Ar and N2) exhibited excellent resistance to FCCI. The thickness of these CrN films were only
4 mm, but these films effectively prevented the FCCI due to their high adhesion strength (frictional force
1,200 mm) and dense columnar microstructures.
© 2018 Korean Nuclear Society, Published by Elsevier Korea LLC. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Keywords:
CrN
Fuel-Clad Chemical Interaction Barrier
Interdiffusion
Scratch Test
1. Introduction
The majority of nuclear industry uses pressurized water reactors, but many people think that sodium-cooled fast reactor (SFR)
will become the next generation nuclear reactor because of its
ability to recycle spent nuclear fuels such as uranium, plutonium,
and lanthanide through pyroprocessing [1]. SFR has many advantages over pressurized water reactor. SFR has high thermal conductivity, which creates a reservoir that prevents overheating [2].
Also, the neutrons in SFR lose less energy compared to hydrogen
and oxygen atoms found in water when atoms collide due to the
weight difference. SFR is energy efficient, but the drawback of sodium is its chemical reactivity. When the temperature of the fuelcladding interface reaches 650 C (923 K), the interdiffusion occurs between actinide elements (nuclear fission products) and the
cladding [1,2]. This phenomenon is called fuel-clad chemical
interaction (FCCI), and this lowers the melting point of the cladding
through eutectic reaction [3e7]. The FCCI causes the thickness of
* Corresponding author.
** Corresponding author.
E-mail address: benedicto@gachon.ac.kr (Y.S. Yoon).
the cladding to become thinner, which end up weakening the
mechanical strength of the cladding.
One of the common methods to prevent diffusion is coating the
inner cladding tube with a thin layer [8e12]. So far, many researchers conducted experiments with Zr barriers in the nuclear
industry. However, Zr-based coatings are not efficient diffusion
barriers compared to Cr-based coatings. Lee et al. deposited Zr film
onto HT-9 clad using radio frequency magnetron and tested its
performance as a FCCI barrier. However, the barrier did not entirely
prevent the interdiffusion between the misch metal and the HT-9,
so they had to add a 25 mm-thick Zr foil, which made the FCCI
barrier thicker overall [1]. Jee et al. created Zr film FCCI barriers at
multiple temperatures using hydrothermal crystallization. The
barriers did not perfectly prevent the interdiffusion from occurring,
and the experiment gave inconsistent results at various temperatures [13].
In this study, Cr-based coatings were considered as a substitute
for Zr-based coatings. Among Cr-based coatings, the CrN coatings
particularly have good mechanical and chemical properties, such as
high adhesion strength, high hardness, good conductivity, and
excellent chemical, thermal, and wear resistance [14e21]. To deposit Cr and CrN layers, radio frequency magnetron sputtering was
chosen due to its high deposition rate and good uniformity
[22e24]. HT-9 was used as cladding and went through diffusion
https://doi.org/10.1016/j.net.2018.02.008
1738-5733/© 2018 Korean Nuclear Society, Published by Elsevier Korea LLC. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).
D. Kim et al. / Nuclear Engineering and Technology 50 (2018) 724e730
725
couple test to assess the FCCI behavior [25e28]. HT-9 (Table 1) was
chosen as a candidate for SFR cladding due to its excellent irradiation resistance [29]. The misch metal was used to simulate the
nuclear fuel due to its high content of cerium and lanthanum. The
gas flow rate of nitrogen and argon were adjusted differently for
each sample to find the best CrN barrier during sputtering. The
interdiffusion between the misch metal and HT9 was evaluated
through diffusion couple tests.
2. Experimental procedure
2.1. Material and preparation
HT-9, a ferritic/martensitic steel, is a commonly used material in
nuclear facilities as a fuel cladding. The HT-9 disk was used to test
the FCCI through the diffusion couple test. The diameter of the HT-9
is 8 mm, and its thickness is 1.9 mm. The specific composition of the
HT-9 that was used for the experiment is shown in Table 1. Before
the sputtering process, the HT-9 disks were chemically etched by
ultrasonication in a mixture composed with 95 mL of deionized (DI)
water, 2 mL of hydrogen fluoride, and 3 mL of nitric acid (HNO3) for
30 s to increase the adhesion. Once the etching was done, the Zr
plate, HT-9, and the silicon wafer inside the acetone were cleaned
by ultrasonication for 15 minute. The Cr and CrN film was deposited
on these cleaned materials at 100 W under the pressure of 5 m torr
for a certain amount of time depending on its gas composition as
shown in Table 2. Total of four types of samples were made using
the mass flow controller. The ratio of the argon and nitrogen
changed for each sample, but the total flow rate was kept at 40
sccm. The substrate plate rotated at a speed of 40 rpm during the
process to create an even deposition layer.
Table 1
Chemical properties (wt %) of the HT-9 steel.
Fe
Cr
Mo
Si
Ni
W
V
C
Other
84.4
11.9
1.03
0.69
0.62
0.48
0.30
0.21
0.37
Fig. 2. XRD spectra of Cr and CrN films with different nitrogen flow rate. (A) 100% N2
(B) 70% N2, (C) 30% N2, (D) 0% N2.
XRD, X-ray diffraction.
2.2. Diffusion couple test
The diffusion couple test was conducted to measure Cr and CrN
barriers' ability to prevent FCCI between the HT-9 and the rare
earth element. The misch metal, which mainly consisted of Ce: 75%
and La: 25%, is a good candidate to simulate the interdiffusion
behavior between rare earth material and the clad. The HT-9 and
the misch metal were inserted into a screw jig as shown in Fig. 1,
and then these materials were covered with tantalum foil (thickness 0.25 mm, 99.9%, Aldrich) to prevent the reaction between
the jig and the misch metal. Once they were clamped, the samples
were put into the furnace inside argon (purity: 99.999%)-filled
glove box maintained at humidity level below 2 ppm to prevent the
misch metal from oxidizing. The samples were heated for 24 h at
933 K, which is the peak inner cladding wall temperature for SFR
[30,31].” After heating, the samples were taken out to be cooled.
2.3. Material characterization
Table 2
Deposition parameters under a constant total gas flow rate of 40 sccm and the
properties of each sample.
Sample
N2 (%)
Ar (%)
N2 (sccm)
Ar (sccm)
Time (min.)
Thickness (mm)
1
2
3
4
0
30
70
100
100
70
30
0
0
12
28
40
40
28
12
0
144
289
442
562
4.18
4.16
4.14
3.85
The glass substrates deposited with Cr and CrN film were prepared to analyze the crystal structures of the Cr and CrN film on the
HT-9 using X-ray diffraction (XRD, Rigaku RINT). To characterize the
FCCI through field-emission scanning electron microscope (FESEM, Hitachi S-4200), the HT-9 samples were cut into half, and the
cross sections of the samples were polished by silicon carbide paper. The images of the cross section and the surface of the Cr and
Fig. 1. Schematic illustration of the specimen for the diffusion couple test. (A) Diagonal view. (B) Enlarged diagonal view.
726
D. Kim et al. / Nuclear Engineering and Technology 50 (2018) 724e730
Fig. 3. FE-SEM images of Cr and CrN films deposited by RF magnetron sputtering. (A) For surface, 0% N2. (B) Cross section, 30% N2. (C) Surface, 30% N2. (D) Cross section, 70% N2. (E)
Surface, 70% N2. (F) Cross section, 100% N2. (G) Surface, 0% N2. (H) Cross section, 100% N2.
FE-SEM, field-emission scanning electron microscope; RF, radio frequency.
CrN film were captured as shown in Fig. 3 during the FE-SEM
analysis. To test the adhesion of barriers, the zirconium plates
deposited with Cr and CrN films were scratched by the nano scratch
tester (CSM Instruments). The frictional forces onto the Cr and CrN
barriers were drawn as graphs along the grind marks of these
coatings. Critical loads for each samples were detected from sharp
peaks of the frictional force graphs, and these loads assessed the
coating adhesion [32]. The critical loads were collated into a graph
as shown in Fig. 4.
3. Results and discussion
3.1. Structural characterization
The crystalline structures of the four samples at Table 2 were
determined by XRD. The main purpose of XRD was to determine
whether the barriers are composed of CrN or Cr2N. The XRD patterns of Cr and CrN films for each sample are shown in Fig. 2. The
peaks of Cr foil (N2 0%) in the diffraction patterns clearly correspond
D. Kim et al. / Nuclear Engineering and Technology 50 (2018) 724e730
Fig. 4. Scratch test images and graph of Cr and CrN film with different N2 flow content.
(A) 0% N2. (B) 30% N2. (C) 70% N2. (D) 100% N2. (E) The frictional force of Cr and CrN
films with different N2 coated by RF magnetron sputtering.
RF, radio frequency.
Fig. 5. Magnified FE-SEM images of cross section of the Sample 1 after diffusion couple
test. (A) At low magnification (50). (B) Enlarged image of (A) at 200 magnification.
(C) EDS line profiles for elements content (500).
EDS, energy dispersive X-ray spectroscopy; FE-SEM, field-emission scanning electron
microscope.
to crystal system of cubic structure (JCPDS, No. 01-085-1336).
Sample 3 and 4 (N2 70%, N2 100%) clearly have four peaks that
correspond to the crystal system of cubic system (JCPDS, No. 65-2899),
but Sample 2 (N2 30%,) does not have a peak at 43.594 at the horizontal axis of Fig. 2. Also, unlike the other two samples, the intensity of
the remaining peaks for Sample 2 also does not match the cubic
system (JCPDS, No. 65-2899). The CrN may have not been formed
completely due to its lack of N2 gas compared to other two samples.
727
Fig. 6. Magnified FE-SEM images of cross section of the Sample 2 after diffusion couple
test. (A) At low magnification (50). (B) Enlarged image of (A) at 500 magnification.
(C) EDS line profiles for elements content (500).
EDS, energy dispersive X-ray spectroscopy; FE-SEM, field-emission scanning electron
microscope.
Fig. 7. Magnified FE-SEM images of cross section of the Sample 3 after diffusion couple
test. (A) At low magnification (50). (B) Enlarged image of (A) 500 magnification. (C)
EDS line profiles for elements content (500).
EDS, energy dispersive X-ray spectroscopy; FE-SEM, field-emission scanning electron
microscope.
The FE-SEM analysis of Cr and CrN thin films for each sample is
shown in Fig. 3. The images of the surface and the cross section of
Cr and CrN barriers for different specimens are shown in Fig. 3.
Fig. 3B shows thick columnar microstructures of the Cr barrier,
and it does not have any major defects such as pinholes. However,
the columnar microstructures are very thick, and they are not
exactly perpendicular to the silicon wafer. Owing to the thickness
and shape of the microstructures, the top (surface) of the Cr layer
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D. Kim et al. / Nuclear Engineering and Technology 50 (2018) 724e730
is very rough, and the microstructures are not very compact as
shown in Fig. 3A. This is mainly due to the fast deposition rate of
Cr film. It took less than ~2.5 h to deposit 4.18 mm of Cr film, but
the surface was rough due to its high speed. There is a noticeable
difference between samples with Cr and CrN barriers. Adding
nitride significantly decreased the deposition rate. In Fig. 3D, F, H,
the columnar microstructures of the films are much thinner
compared to the ones in Fig. 3B. The CrN barriers became denser
and the surfaces became smoother as the deposition rate went
down.
The adhesion strength of the Cr and CrN barriers were analyzed
by comparing the frictional forces during the scratch test. Fig. 4AeD
show the images of the scratched plates and the location of the
measured frictional forces. Fig. 4E compares the frictional forces of
the specimens with different nitrogen flow content from Table 2 as
a graph. Overall, samples with CrN films had higher adhesion
strengths compared to the Cr film. The frictional force the CrN film
can withstand went up significantly when the nitrogen flow content was 30% but went down as the nitrogen flow content
increased. Sample 4 only used nitrogen for sputtering, but its
adhesion strength was similar to Sample 1, which did not use any
nitrogen. As a result, it has been found that proper ratio of nitride
and argon increases the adhesion strength.
3.2. Reaction between misch metal and HT-9
Figs. 5e8 exhibit the results of the diffusion couple test for each
specimen from Table 2 at 933 K. Fig. 5 shows the cross-sectional FESEM image of misch metal and HT-9 with Cr barrier (sample 1: Ar
100%). In Fig. 5A, most of the Cr barrier got destroyed by the interdiffusion that occurred throughout most parts of the HT-9. As shown
in Fig. 5B, the thickness of the interdiffusion layer is 292.5 mm, which
is more than 70 times the thickness of the Cr barrier. In Fig. 3C,
energy dispersive X-ray spectroscopy (EDS) is used for more accurate analysis. The elemental content of the misch metal and HT-9
throughout the interdiffusion is drawn as a graph. Between 100
and 150 mm, there is a Cr peak, which indicates the Cr barrier.
However, a lot of the Ce and La content can be seen at the side of HT9 on the graph. Although there was a Cr barrier, many of the Ce and
La content moved from the misch metal to HT-9 and the Fe content
moved from HT-9 to misch metal due to the interdiffusion. However,
the Cr within the HT-9 did not move over to misch metal. Instead,
some Cr peaks with high intensity appeared at the side of the HT-9.
When the diffusion occurred, the chromium that fell apart from the
HT-9 formed clusters at some points of the HT-9. As shown in Fig. 2A
and B, the columnar gaps of the Cr film are thick, and their surface is
rough. The element content of misch metal and HT-9 may have
pierced through the columnar gaps within the Cr film.
Figs. 6 and 7 demonstrate the cross-sectional FE-SEM images of
misch metal, Sample 2 (Ar 70%, N2 30%), and Sample 3 (Ar 30%, N2
70%). Unlike the Cr barrier in Fig. 5A, there are no signs of interdiffusion in Figs. 6A and 7A. As shown in the EDS graphs of Figs. 6C
and 7C, none of the Ce and La content moved from misch metal to
HT-9, and the Fe content remained at the side of HT-9 as well. The
CrN films of the two specimens successfully prevented the interdiffusion from occurring at SFR operation temperature of 933 K. In
Figs. 6B and 7B, the thin CrN films are clearly visible between the
misch metal and HT-9. The Cr peaks of the CrN films are confirmed
at Figs. 6C and 7C, but the nitrogen is not included in the graphs.
Unfortunately, nitrogen's atomic number is 7, and FE-SEM cannot
detect elements with atomic number lower than the oxygen
(atomic number: 8). However, this was not a major issue since the
nitrogen content of the CrN barriers were confirmed from the XRD
at Fig. 2. The dense CrN films, formed by thin columnar microstructures, were effective barriers for diffusion.
Fig. 8 shows the cross-sectional FE-SEM image of misch metal
and HT-9 with CrN barrier (Sample 1: N2 100%). In Fig. 8A, almost
half of the Cr barrier got destroyed by interdiffusion. As shown in
Fig. 8B, the thickness of the interdiffusion layer is 549.4 mm, which
is almost twice the thickness of the Cr barrier at Fig. 5A. On top of
that, the CrN film was not even visible in Sample 4, so it was
necessary to analyze where the elements were distributed through
EDS. In Fig. 8C, the peaks for each element are all over the place.
Unlike the Ce content, which diffused equally throughout the Line
EDS, most of the La content was detected at the side of HT-9. As
expected, some of the Fe peaks are detected at the misch metal
because of interdiffusion. Unfortunately, the location of CrN film
was not detected through EDS analysis. It is very likely that the CrN
barrier got destroyed completely because of interdiffusion. Not only
the CrN film was not visible but also there were multiple Cr peaks
detected at the side of HT-9. There is a high chance that the Cr
diffused throughout HT-9 as the CrN film dispersed.
Among all the samples listed in Table 2, only Sample 1 allowed
interdiffusion to occur throughout the entire interface of misch
metal and HT-9, as shown in Fig. 5A. To strengthen the Cr barrier, a
Cr foil (thickness: 25 mm, purity 99.99%, Goodfellow) was inserted inside the steel jig between misch metal and HT-9 (Sample 1)
shown in Fig. 1A during the diffusion couple test. However, cutting
chromium foil into the shape of HT-9 was very difficult because it
was very brittle. As shown in Fig. 9A, the Cr foil had multiple cracks
before it was cut, and these cracks are clearly visible through the
optical microscope image in Fig. 9B. Fig. 9C demonstrates the crosssectional FE-SEM images of misch metal, Sample 1 (Ar 100%), and
Cr foil, and the Cr foil completely was clearly visible in the image
because of its thickness. However, the Cr foil was not visible at the
bottom part of the interface of HT-9 and misch metal. It was presumed that the portion of the chromium foil fell off because of the
compression force of the bolts as they got clamped to the steel jig.
As expected, the interdiffusion occurred in this region, and the EDS
analysis had to be done. The line EDS was drawn at the selected
location in Fig. 9D, and the distribution of the elements were drawn
as a graph in Fig. 9E. In Fig. 9E, cerium, lanthanum, and iron were
Fig. 8. Magnified FE-SEM images of cross section of the Sample 4 after diffusion couple
test. (A) At low magnification (50). (B) Enlarged image of (A) at 200 magnification.
(C) EDS line profiles for elements content (500).
EDS, energy dispersive X-ray spectroscopy; FE-SEM, field-emission scanning electron
microscope.
D. Kim et al. / Nuclear Engineering and Technology 50 (2018) 724e730
729
(Sample 2: Ar 70%, N2 30%/Sample 3: Ar 70%, N2 30%) that successfully prevented FCCI had high adhesion strength, and these
specimens used mixed gases (N2 and Ar) for magnetron sputtering. As the nitrogen flow rate of the samples increased, the
deposition rate went down and the barriers became denser and
smoother. Owing to different N2 flow rates, the microstructures of
the samples were all different, and this affected the adhesion
strength of the specimens. These results indicate that the gas
ratios of N2 and Ar during sputtering affect the adhesion strength,
and the adhesion strength affects the performance of FCCI barrier.
These results suggest that the CrN thin film has the potential to
serve as an effective diffusion barrier for cladding with careful
adjustment of the gas ratio.
Conflicts of interest
The authors do not have any conflicts of interest to declare.
Acknowledgments
The authors would like to thank the support by Basic Science
Research Program through the National Research Foundation of
Korea(NRF) funded by the Ministry of Science, ICT & Future Planning (NRF-2016R1A5A1013919).
Appendix A. Supplementary data
Supplementary data related to this article can be found at
https://doi.org/10.1016/j.net.2018.02.008.
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Fig. 9. Images of Cr foil. (A) Digital image. (B) Optical microscope (40 magnification).
Magnified FE-SEM images of cross section of the Sample 1 with Cr foil after diffusion
couple test. (C) At low magnification (50). (D) Enlarged image of (C) at 300
magnification. (E) EDS line profiles for elements content (500).
EDS, energy dispersive X-ray spectroscopy; FE-SEM, field-emission scanning electron
microscope.
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4. Conclusion
The diffusion couple test was conducted to experiment the
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